# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Frank Breher' _publ_contact_author_email BREHER@AOC1.UNI-KARLSRUHE.DE _publ_section_title ; Syntheses, structures, and reactivity of poly(pyrazolyl)silanes, -disilanes, and the ambidentate k1Si/k3N-coordinating tris(3,5-dimethylpyrazolyl)silanide ligand [Si(3,5-Me2pz)3]- (MeTpsd) ; loop_ _publ_author_name 'Frank Breher' 'Felix Armbruster' 'Ignacio Fernandez' # Attachment 'B906333A.cif' data_Si2pz6 _database_code_depnum_ccdc_archive 'CCDC 725892' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 N12 Si2' _chemical_formula_sum 'C30 H42 N12 Si2' _chemical_formula_weight 626.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 7.9720(16) _cell_length_b 13.566(3) _cell_length_c 15.596(3) _cell_angle_alpha 76.99(3) _cell_angle_beta 83.98(3) _cell_angle_gamma 83.97(3) _cell_volume 1628.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 12279 _cell_measurement_theta_min 4.04 _cell_measurement_theta_max 25.99 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.151 _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 200(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 'Stoe Stadi 4 with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12279 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.1093 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 25.99 _reflns_number_total 6276 _reflns_number_gt 3549 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0864P)^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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6276 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1736 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.98529(11) 0.92618(7) 0.97878(6) 0.0228(2) Uani 1 1 d . . . N1 N 0.9070(3) 0.8999(2) 0.88498(18) 0.0269(7) Uani 1 1 d . . . N2 N 0.9043(3) 0.9840(2) 0.81649(18) 0.0278(7) Uani 1 1 d . . . Si2 Si 0.45431(11) 0.57295(7) 0.52414(6) 0.0236(2) Uani 1 1 d . . . N3 N 1.0596(3) 0.8071(2) 1.04143(18) 0.0265(6) Uani 1 1 d . . . N4 N 1.1780(4) 0.7520(2) 0.9942(2) 0.0320(7) Uani 1 1 d . . . N5 N 0.7729(3) 0.9505(2) 1.04469(17) 0.0221(6) Uani 1 1 d . . . N6 N 0.8007(3) 1.0310(2) 1.08137(17) 0.0242(6) Uani 1 1 d . . . N7 N 0.3328(3) 0.5991(2) 0.61924(18) 0.0269(7) Uani 1 1 d . . . N8 N 0.3240(3) 0.5134(2) 0.68573(18) 0.0286(7) Uani 1 1 d . . . N9 N 0.5153(3) 0.6922(2) 0.46349(18) 0.0260(6) Uani 1 1 d . . . C10 C 0.8483(5) 0.7148(3) 0.9157(3) 0.0426(10) Uani 1 1 d . . . H10A H 0.9574 0.6752 0.9102 0.064 Uiso 1 1 calc R . . H10B H 0.7599 0.6811 0.8970 0.064 Uiso 1 1 calc R . . H10C H 0.8208 0.7200 0.9773 0.064 Uiso 1 1 calc R . . N10 N 0.5944(3) 0.7446(2) 0.51333(19) 0.0306(7) Uani 1 1 d . . . C11 C 0.8585(4) 0.8182(3) 0.8588(2) 0.0298(8) Uani 1 1 d . . . N11 N 0.2732(3) 0.5548(2) 0.45821(17) 0.0239(6) Uani 1 1 d . . . C12 C 0.8257(4) 0.8524(3) 0.7713(2) 0.0324(9) Uani 1 1 d . . . H12 H 0.7898 0.8135 0.7340 0.039 Uiso 1 1 calc R . . N12 N 0.3406(3) 0.4760(2) 0.41819(17) 0.0245(6) Uani 1 1 d . . . C13 C 0.8554(4) 0.9549(3) 0.7483(2) 0.0322(8) Uani 1 1 d . . . C14 C 0.8393(5) 1.0291(3) 0.6625(3) 0.0475(11) Uani 1 1 d . . . H14A H 0.7199 1.0420 0.6504 0.071 Uiso 1 1 calc R . . H14B H 0.9040 1.0014 0.6150 0.071 Uiso 1 1 calc R . . H14C H 0.8835 1.0929 0.6656 0.071 Uiso 1 1 calc R . . C20 C 0.9341(5) 0.7945(3) 1.1999(2) 0.0338(9) Uani 1 1 d . . . H20A H 0.9625 0.7538 1.2577 0.051 Uiso 1 1 calc R . . H20B H 0.8167 0.7866 1.1912 0.051 Uiso 1 1 calc R . . H20C H 0.9473 0.8661 1.1973 0.051 Uiso 1 1 calc R . . C21 C 1.0500(4) 0.7592(3) 1.1288(2) 0.0273(8) Uani 1 1 d . . . C22 C 1.1602(4) 0.6755(3) 1.1372(3) 0.0359(9) Uani 1 1 d . . . H22 H 1.1818 0.6275 1.1903 0.043 Uiso 1 1 calc R . . C23 C 1.2362(4) 0.6730(3) 1.0527(3) 0.0332(9) Uani 1 1 d . . . C24 C 1.3647(5) 0.5972(3) 1.0241(3) 0.0518(11) Uani 1 1 d . . . H24A H 1.3935 0.6177 0.9603 0.078 Uiso 1 1 calc R . . H24B H 1.3190 0.5306 1.0377 0.078 Uiso 1 1 calc R . . H24C H 1.4666 0.5932 1.0553 0.078 Uiso 1 1 calc R . . C30 C 0.5465(4) 0.8353(3) 1.0534(2) 0.0352(9) Uani 1 1 d . . . H30A H 0.5606 0.8433 0.9891 0.053 Uiso 1 1 calc R . . H30B H 0.4257 0.8357 1.0734 0.053 Uiso 1 1 calc R . . H30C H 0.6051 0.7707 1.0814 0.053 Uiso 1 1 calc R . . C31 C 0.6189(4) 0.9199(3) 1.0782(2) 0.0257(8) Uani 1 1 d . . . C32 C 0.5511(4) 0.9793(3) 1.1365(2) 0.0288(8) Uani 1 1 d . . . H32 H 0.4439 0.9747 1.1694 0.035 Uiso 1 1 calc R . . C33 C 0.6686(4) 1.0466(3) 1.1382(2) 0.0278(8) Uani 1 1 d . . . C34 C 0.6624(5) 1.1250(3) 1.1926(3) 0.0424(10) Uani 1 1 d . . . H34A H 0.7683 1.1180 1.2210 0.064 Uiso 1 1 calc R . . H34B H 0.5671 1.1154 1.2379 0.064 Uiso 1 1 calc R . . H34C H 0.6478 1.1928 1.1545 0.064 Uiso 1 1 calc R . . C40 C 0.2343(5) 0.7873(3) 0.5944(3) 0.0474(11) Uani 1 1 d . . . H40A H 0.3277 0.8239 0.6043 0.071 Uiso 1 1 calc R . . H40B H 0.1263 0.8215 0.6125 0.071 Uiso 1 1 calc R . . H40C H 0.2382 0.7863 0.5316 0.071 Uiso 1 1 calc R . . C41 C 0.2506(4) 0.6819(3) 0.6470(2) 0.0319(8) Uani 1 1 d . . . C42 C 0.1914(5) 0.6479(3) 0.7326(2) 0.0389(9) Uani 1 1 d . . . H42 H 0.1298 0.6874 0.7704 0.047 Uiso 1 1 calc R . . C43 C 0.2386(4) 0.5434(3) 0.7542(2) 0.0322(9) Uani 1 1 d . . . C44 C 0.2040(5) 0.4695(3) 0.8385(3) 0.0487(11) Uani 1 1 d . . . H44A H 0.0874 0.4510 0.8430 0.073 Uiso 1 1 calc R . . H44B H 0.2193 0.5001 0.8881 0.073 Uiso 1 1 calc R . . H44C H 0.2825 0.4086 0.8403 0.073 Uiso 1 1 calc R . . C50 C 0.4407(5) 0.7129(3) 0.3063(2) 0.0382(9) Uani 1 1 d . . . H50A H 0.3170 0.7166 0.3168 0.057 Uiso 1 1 calc R . . H50B H 0.4842 0.6427 0.3055 0.057 Uiso 1 1 calc R . . H50C H 0.4727 0.7572 0.2493 0.057 Uiso 1 1 calc R . . C51 C 0.5135(4) 0.7462(3) 0.3777(2) 0.0294(8) Uani 1 1 d . . . C52 C 0.5900(4) 0.8330(3) 0.3731(2) 0.0343(9) Uani 1 1 d . . . H52 H 0.6083 0.8856 0.3222 0.041 Uiso 1 1 calc R . . C53 C 0.6360(4) 0.8291(3) 0.4580(3) 0.0335(9) Uani 1 1 d . . . C54 C 0.7229(5) 0.9041(3) 0.4908(3) 0.0532(12) Uani 1 1 d . . . H54A H 0.7055 0.8910 0.5554 0.080 Uiso 1 1 calc R . . H54B H 0.6757 0.9730 0.4658 0.080 Uiso 1 1 calc R . . H54C H 0.8443 0.8974 0.4728 0.080 Uiso 1 1 calc R . . C60 C 0.0120(4) 0.6726(3) 0.4566(3) 0.0395(9) Uani 1 1 d . . . H60A H 0.0106 0.6636 0.5208 0.059 Uiso 1 1 calc R . . H60B H -0.1035 0.6727 0.4404 0.059 Uiso 1 1 calc R . . H60C H 0.0575 0.7374 0.4277 0.059 Uiso 1 1 calc R . . C61 C 0.1200(4) 0.5884(3) 0.4278(2) 0.0284(8) Uani 1 1 d . . . C62 C 0.0912(4) 0.5314(3) 0.3683(2) 0.0316(8) Uani 1 1 d . . . H62 H -0.0072 0.5376 0.3374 0.038 Uiso 1 1 calc R . . C63 C 0.2310(4) 0.4644(3) 0.3622(2) 0.0289(8) Uani 1 1 d . . . C64 C 0.2699(5) 0.3880(3) 0.3060(3) 0.0457(11) Uani 1 1 d . . . H64A H 0.3758 0.4017 0.2691 0.069 Uiso 1 1 calc R . . H64B H 0.1776 0.3923 0.2680 0.069 Uiso 1 1 calc R . . H64C H 0.2817 0.3198 0.3437 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0220(5) 0.0233(5) 0.0246(5) -0.0089(4) -0.0005(4) -0.0019(4) N1 0.0272(15) 0.0246(16) 0.0315(17) -0.0108(13) -0.0020(12) -0.0033(13) N2 0.0266(15) 0.0298(17) 0.0278(16) -0.0078(13) -0.0035(12) -0.0020(13) Si2 0.0241(5) 0.0222(5) 0.0253(5) -0.0074(4) -0.0030(4) 0.0007(4) N3 0.0284(15) 0.0220(16) 0.0286(16) -0.0072(13) 0.0026(12) -0.0007(12) N4 0.0320(16) 0.0268(17) 0.0393(18) -0.0151(14) -0.0005(13) 0.0026(13) N5 0.0228(14) 0.0216(15) 0.0239(15) -0.0082(12) -0.0035(11) -0.0026(12) N6 0.0226(14) 0.0214(16) 0.0308(16) -0.0109(12) -0.0015(12) -0.0013(12) N7 0.0268(15) 0.0276(17) 0.0274(16) -0.0098(13) 0.0000(12) -0.0001(13) N8 0.0294(16) 0.0292(17) 0.0284(16) -0.0077(13) -0.0010(13) -0.0057(13) N9 0.0270(15) 0.0233(16) 0.0295(16) -0.0102(13) -0.0032(12) 0.0001(12) C10 0.051(2) 0.033(2) 0.049(3) -0.0188(19) 0.003(2) -0.014(2) N10 0.0281(16) 0.0298(18) 0.0384(18) -0.0163(14) -0.0049(13) -0.0019(13) C11 0.0243(18) 0.032(2) 0.037(2) -0.0167(17) 0.0028(15) -0.0046(16) N11 0.0243(14) 0.0217(16) 0.0255(15) -0.0064(12) -0.0021(12) 0.0016(12) C12 0.032(2) 0.037(2) 0.034(2) -0.0201(17) -0.0038(16) -0.0040(17) N12 0.0266(15) 0.0213(16) 0.0275(16) -0.0096(12) -0.0038(12) 0.0002(12) C13 0.0259(18) 0.042(2) 0.032(2) -0.0173(17) -0.0011(15) 0.0027(16) C14 0.057(3) 0.051(3) 0.035(2) -0.010(2) -0.015(2) 0.004(2) C20 0.040(2) 0.032(2) 0.028(2) -0.0040(16) -0.0037(16) -0.0031(17) C21 0.0284(18) 0.0234(19) 0.031(2) -0.0053(15) -0.0044(15) -0.0055(15) C22 0.034(2) 0.027(2) 0.045(2) -0.0011(17) -0.0121(18) -0.0021(17) C23 0.0298(19) 0.025(2) 0.046(2) -0.0098(17) -0.0075(17) 0.0007(16) C24 0.045(2) 0.038(3) 0.075(3) -0.023(2) -0.007(2) 0.011(2) C30 0.031(2) 0.032(2) 0.044(2) -0.0077(18) -0.0043(17) -0.0104(17) C31 0.0192(17) 0.029(2) 0.0271(19) -0.0014(15) -0.0016(14) -0.0049(15) C32 0.0212(17) 0.034(2) 0.030(2) -0.0074(16) 0.0041(14) -0.0001(15) C33 0.0215(17) 0.033(2) 0.0288(19) -0.0097(16) 0.0023(14) -0.0008(15) C34 0.039(2) 0.049(3) 0.044(2) -0.027(2) 0.0116(18) -0.006(2) C40 0.052(2) 0.036(2) 0.051(3) -0.012(2) 0.008(2) 0.008(2) C41 0.0323(19) 0.030(2) 0.035(2) -0.0150(17) 0.0015(16) 0.0012(16) C42 0.038(2) 0.043(3) 0.040(2) -0.0215(19) 0.0054(17) -0.0037(18) C43 0.0279(19) 0.044(2) 0.029(2) -0.0130(17) -0.0018(15) -0.0092(17) C44 0.057(3) 0.059(3) 0.032(2) -0.009(2) 0.0041(19) -0.019(2) C50 0.049(2) 0.037(2) 0.027(2) -0.0046(17) -0.0023(17) -0.0031(19) C51 0.0249(18) 0.028(2) 0.032(2) -0.0026(16) 0.0015(15) 0.0035(15) C52 0.034(2) 0.026(2) 0.039(2) -0.0013(17) 0.0040(16) -0.0027(16) C53 0.0302(19) 0.023(2) 0.047(2) -0.0098(17) -0.0003(17) -0.0013(16) C54 0.050(3) 0.039(3) 0.078(3) -0.021(2) -0.011(2) -0.013(2) C60 0.030(2) 0.036(2) 0.049(2) -0.0063(19) -0.0016(17) 0.0080(17) C61 0.0212(17) 0.031(2) 0.0283(19) 0.0004(15) 0.0005(14) 0.0008(15) C62 0.0288(19) 0.034(2) 0.032(2) -0.0032(16) -0.0079(15) -0.0054(16) C63 0.0306(19) 0.030(2) 0.0284(19) -0.0074(16) -0.0074(15) -0.0085(16) C64 0.059(3) 0.044(3) 0.041(2) -0.019(2) -0.019(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N3 1.768(3) . ? Si1 N1 1.769(3) . ? Si1 N5 1.924(3) . ? Si1 N6 1.938(3) 2_777 ? Si1 Si1 2.2877(18) 2_777 ? N1 C11 1.368(4) . ? N1 N2 1.376(4) . ? N2 C13 1.323(4) . ? Si2 N9 1.768(3) . ? Si2 N7 1.768(3) . ? Si2 N11 1.925(3) . ? Si2 N12 1.933(3) 2_666 ? Si2 Si2 2.2955(19) 2_666 ? N3 C21 1.370(4) . ? N3 N4 1.395(4) . ? N4 C23 1.319(5) . ? N5 C31 1.352(4) . ? N5 N6 1.388(3) . ? N6 C33 1.334(4) . ? N6 Si1 1.938(3) 2_777 ? N7 C41 1.373(4) . ? N7 N8 1.375(4) . ? N8 C43 1.325(4) . ? N9 C51 1.374(4) . ? N9 N10 1.397(4) . ? C10 C11 1.486(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N10 C53 1.320(5) . ? C11 C12 1.382(5) . ? N11 C61 1.353(4) . ? N11 N12 1.389(4) . ? C12 C13 1.395(5) . ? C12 H12 0.9500 . ? N12 C63 1.342(4) . ? N12 Si2 1.933(3) 2_666 ? C13 C14 1.491(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C20 C21 1.497(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.351(5) . ? C22 C23 1.397(5) . ? C22 H22 0.9500 . ? C23 C24 1.482(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C30 C31 1.479(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.380(5) . ? C32 C33 1.381(5) . ? C32 H32 0.9500 . ? C33 C34 1.496(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C40 C41 1.479(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.361(5) . ? C42 C43 1.400(5) . ? C42 H42 0.9500 . ? C43 C44 1.483(5) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C50 C51 1.483(5) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.367(5) . ? C52 C53 1.400(5) . ? C52 H52 0.9500 . ? C53 C54 1.494(5) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C60 C61 1.481(5) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.384(5) . ? C62 C63 1.372(5) . ? C62 H62 0.9500 . ? C63 C64 1.492(5) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 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 N3 Si1 N1 105.60(14) . . ? N3 Si1 N5 100.75(13) . . ? N1 Si1 N5 98.80(12) . . ? N3 Si1 N6 98.61(13) . 2_777 ? N1 Si1 N6 95.33(13) . 2_777 ? N5 Si1 N6 151.92(12) . 2_777 ? N3 Si1 Si1 121.28(11) . 2_777 ? N1 Si1 Si1 133.01(12) . 2_777 ? N5 Si1 Si1 76.65(9) . 2_777 ? N6 Si1 Si1 75.96(9) 2_777 2_777 ? C11 N1 N2 110.5(3) . . ? C11 N1 Si1 138.2(3) . . ? N2 N1 Si1 111.1(2) . . ? C13 N2 N1 106.4(3) . . ? N9 Si2 N7 105.05(14) . . ? N9 Si2 N11 100.46(13) . . ? N7 Si2 N11 98.90(12) . . ? N9 Si2 N12 98.97(13) . 2_666 ? N7 Si2 N12 95.78(12) . 2_666 ? N11 Si2 N12 151.63(12) . 2_666 ? N9 Si2 Si2 120.74(11) . 2_666 ? N7 Si2 Si2 134.13(12) . 2_666 ? N11 Si2 Si2 76.54(9) . 2_666 ? N12 Si2 Si2 75.80(9) 2_666 2_666 ? C21 N3 N4 109.2(3) . . ? C21 N3 Si1 136.2(2) . . ? N4 N3 Si1 113.8(2) . . ? C23 N4 N3 105.8(3) . . ? C31 N5 N6 107.5(3) . . ? C31 N5 Si1 148.9(2) . . ? N6 N5 Si1 103.07(18) . . ? C33 N6 N5 108.6(3) . . ? C33 N6 Si1 148.2(2) . 2_777 ? N5 N6 Si1 103.11(19) . 2_777 ? C41 N7 N8 110.6(3) . . ? C41 N7 Si2 137.9(3) . . ? N8 N7 Si2 111.4(2) . . ? C43 N8 N7 105.8(3) . . ? C51 N9 N10 110.0(3) . . ? C51 N9 Si2 136.7(2) . . ? N10 N9 Si2 113.2(2) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C53 N10 N9 105.3(3) . . ? N1 C11 C12 106.0(3) . . ? N1 C11 C10 125.0(3) . . ? C12 C11 C10 129.0(3) . . ? C61 N11 N12 108.0(3) . . ? C61 N11 Si2 148.7(2) . . ? N12 N11 Si2 102.89(18) . . ? C11 C12 C13 106.8(3) . . ? C11 C12 H12 126.6 . . ? C13 C12 H12 126.6 . . ? C63 N12 N11 107.9(3) . . ? C63 N12 Si2 148.4(2) . 2_666 ? N11 N12 Si2 103.49(18) . 2_666 ? N2 C13 C12 110.3(3) . . ? N2 C13 C14 120.0(3) . . ? C12 C13 C14 129.7(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N3 107.4(3) . . ? C22 C21 C20 127.7(3) . . ? N3 C21 C20 124.9(3) . . ? C21 C22 C23 106.8(3) . . ? C21 C22 H22 126.6 . . ? C23 C22 H22 126.6 . . ? N4 C23 C22 110.7(3) . . ? N4 C23 C24 120.0(4) . . ? C22 C23 C24 129.4(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 C32 108.3(3) . . ? N5 C31 C30 122.5(3) . . ? C32 C31 C30 129.1(3) . . ? C31 C32 C33 107.1(3) . . ? C31 C32 H32 126.5 . . ? C33 C32 H32 126.5 . . ? N6 C33 C32 108.4(3) . . ? N6 C33 C34 122.2(3) . . ? C32 C33 C34 129.3(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 N7 106.2(3) . . ? C42 C41 C40 127.3(3) . . ? N7 C41 C40 126.4(3) . . ? C41 C42 C43 106.9(3) . . ? C41 C42 H42 126.5 . . ? C43 C42 H42 126.5 . . ? N8 C43 C42 110.4(3) . . ? N8 C43 C44 120.5(4) . . ? C42 C43 C44 129.0(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 N9 106.8(3) . . ? C52 C51 C50 128.5(3) . . ? N9 C51 C50 124.7(3) . . ? C51 C52 C53 106.5(3) . . ? C51 C52 H52 126.8 . . ? C53 C52 H52 126.8 . . ? N10 C53 C52 111.4(3) . . ? N10 C53 C54 119.3(3) . . ? C52 C53 C54 129.4(4) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N11 C61 C62 107.8(3) . . ? N11 C61 C60 122.7(3) . . ? C62 C61 C60 129.5(3) . . ? C63 C62 C61 107.4(3) . . ? C63 C62 H62 126.3 . . ? C61 C62 H62 126.3 . . ? N12 C63 C62 108.8(3) . . ? N12 C63 C64 121.1(3) . . ? C62 C63 C64 130.1(3) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 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 N3 Si1 N1 C11 17.1(4) . . . . ? N5 Si1 N1 C11 -86.8(4) . . . . ? N6 Si1 N1 C11 117.6(3) 2_777 . . . ? Si1 Si1 N1 C11 -166.7(3) 2_777 . . . ? N3 Si1 N1 N2 -157.4(2) . . . . ? N5 Si1 N1 N2 98.7(2) . . . . ? N6 Si1 N1 N2 -56.9(2) 2_777 . . . ? Si1 Si1 N1 N2 18.8(3) 2_777 . . . ? C11 N1 N2 C13 -0.3(4) . . . . ? Si1 N1 N2 C13 175.8(2) . . . . ? N1 Si1 N3 C21 -136.5(3) . . . . ? N5 Si1 N3 C21 -34.0(3) . . . . ? N6 Si1 N3 C21 125.5(3) 2_777 . . . ? Si1 Si1 N3 C21 46.8(4) 2_777 . . . ? N1 Si1 N3 N4 55.1(2) . . . . ? N5 Si1 N3 N4 157.5(2) . . . . ? N6 Si1 N3 N4 -42.9(2) 2_777 . . . ? Si1 Si1 N3 N4 -121.7(2) 2_777 . . . ? C21 N3 N4 C23 0.3(4) . . . . ? Si1 N3 N4 C23 171.8(2) . . . . ? N3 Si1 N5 C31 -58.0(4) . . . . ? N1 Si1 N5 C31 49.9(5) . . . . ? N6 Si1 N5 C31 169.2(4) 2_777 . . . ? Si1 Si1 N5 C31 -177.9(4) 2_777 . . . ? N3 Si1 N5 N6 111.2(2) . . . . ? N1 Si1 N5 N6 -141.0(2) . . . . ? N6 Si1 N5 N6 -21.6(4) 2_777 . . . ? Si1 Si1 N5 N6 -8.68(17) 2_777 . . . ? C31 N5 N6 C33 2.0(4) . . . . ? Si1 N5 N6 C33 -172.1(2) . . . . ? C31 N5 N6 Si1 -175.6(2) . . . 2_777 ? Si1 N5 N6 Si1 10.3(2) . . . 2_777 ? N9 Si2 N7 C41 16.5(4) . . . . ? N11 Si2 N7 C41 -87.0(3) . . . . ? N12 Si2 N7 C41 117.4(3) 2_666 . . . ? Si2 Si2 N7 C41 -166.8(3) 2_666 . . . ? N9 Si2 N7 N8 -159.75(19) . . . . ? N11 Si2 N7 N8 96.8(2) . . . . ? N12 Si2 N7 N8 -58.8(2) 2_666 . . . ? Si2 Si2 N7 N8 17.0(3) 2_666 . . . ? C41 N7 N8 C43 -0.6(3) . . . . ? Si2 N7 N8 C43 176.7(2) . . . . ? N7 Si2 N9 C51 -131.0(3) . . . . ? N11 Si2 N9 C51 -28.7(4) . . . . ? N12 Si2 N9 C51 130.5(3) 2_666 . . . ? Si2 Si2 N9 C51 51.8(4) 2_666 . . . ? N7 Si2 N9 N10 53.1(2) . . . . ? N11 Si2 N9 N10 155.4(2) . . . . ? N12 Si2 N9 N10 -45.4(2) 2_666 . . . ? Si2 Si2 N9 N10 -124.13(19) 2_666 . . . ? C51 N9 N10 C53 1.0(3) . . . . ? Si2 N9 N10 C53 178.0(2) . . . . ? N2 N1 C11 C12 0.4(4) . . . . ? Si1 N1 C11 C12 -174.1(3) . . . . ? N2 N1 C11 C10 179.5(3) . . . . ? Si1 N1 C11 C10 4.9(6) . . . . ? N9 Si2 N11 C61 -60.3(5) . . . . ? N7 Si2 N11 C61 46.9(5) . . . . ? N12 Si2 N11 C61 167.2(4) 2_666 . . . ? Si2 Si2 N11 C61 -179.7(5) 2_666 . . . ? N9 Si2 N11 N12 110.5(2) . . . . ? N7 Si2 N11 N12 -142.3(2) . . . . ? N12 Si2 N11 N12 -22.0(4) 2_666 . . . ? Si2 Si2 N11 N12 -8.86(17) 2_666 . . . ? N1 C11 C12 C13 -0.3(4) . . . . ? C10 C11 C12 C13 -179.3(3) . . . . ? C61 N11 N12 C63 1.8(4) . . . . ? Si2 N11 N12 C63 -173.2(2) . . . . ? C61 N11 N12 Si2 -174.5(2) . . . 2_666 ? Si2 N11 N12 Si2 10.5(2) . . . 2_666 ? N1 N2 C13 C12 0.1(4) . . . . ? N1 N2 C13 C14 180.0(3) . . . . ? C11 C12 C13 N2 0.1(4) . . . . ? C11 C12 C13 C14 -179.7(4) . . . . ? N4 N3 C21 C22 0.2(4) . . . . ? Si1 N3 C21 C22 -168.6(3) . . . . ? N4 N3 C21 C20 -178.7(3) . . . . ? Si1 N3 C21 C20 12.5(5) . . . . ? N3 C21 C22 C23 -0.5(4) . . . . ? C20 C21 C22 C23 178.4(3) . . . . ? N3 N4 C23 C22 -0.6(4) . . . . ? N3 N4 C23 C24 179.3(3) . . . . ? C21 C22 C23 N4 0.7(4) . . . . ? C21 C22 C23 C24 -179.2(4) . . . . ? N6 N5 C31 C32 -1.0(4) . . . . ? Si1 N5 C31 C32 168.0(3) . . . . ? N6 N5 C31 C30 179.8(3) . . . . ? Si1 N5 C31 C30 -11.3(6) . . . . ? N5 C31 C32 C33 -0.4(4) . . . . ? C30 C31 C32 C33 178.8(3) . . . . ? N5 N6 C33 C32 -2.3(4) . . . . ? Si1 N6 C33 C32 173.3(3) 2_777 . . . ? N5 N6 C33 C34 176.9(3) . . . . ? Si1 N6 C33 C34 -7.5(7) 2_777 . . . ? C31 C32 C33 N6 1.6(4) . . . . ? C31 C32 C33 C34 -177.4(4) . . . . ? N8 N7 C41 C42 0.8(4) . . . . ? Si2 N7 C41 C42 -175.5(3) . . . . ? N8 N7 C41 C40 179.4(3) . . . . ? Si2 N7 C41 C40 3.2(6) . . . . ? N7 C41 C42 C43 -0.6(4) . . . . ? C40 C41 C42 C43 -179.3(4) . . . . ? N7 N8 C43 C42 0.2(4) . . . . ? N7 N8 C43 C44 179.7(3) . . . . ? C41 C42 C43 N8 0.3(4) . . . . ? C41 C42 C43 C44 -179.1(4) . . . . ? N10 N9 C51 C52 -0.4(4) . . . . ? Si2 N9 C51 C52 -176.4(3) . . . . ? N10 N9 C51 C50 179.5(3) . . . . ? Si2 N9 C51 C50 3.5(5) . . . . ? N9 C51 C52 C53 -0.3(4) . . . . ? C50 C51 C52 C53 179.8(3) . . . . ? N9 N10 C53 C52 -1.2(4) . . . . ? N9 N10 C53 C54 179.5(3) . . . . ? C51 C52 C53 N10 1.0(4) . . . . ? C51 C52 C53 C54 -179.8(4) . . . . ? N12 N11 C61 C62 -0.4(4) . . . . ? Si2 N11 C61 C62 170.2(4) . . . . ? N12 N11 C61 C60 -179.9(3) . . . . ? Si2 N11 C61 C60 -9.3(7) . . . . ? N11 C61 C62 C63 -1.1(4) . . . . ? C60 C61 C62 C63 178.3(4) . . . . ? N11 N12 C63 C62 -2.5(4) . . . . ? Si2 N12 C63 C62 170.6(4) 2_666 . . . ? N11 N12 C63 C64 177.6(3) . . . . ? Si2 N12 C63 C64 -9.3(7) 2_666 . . . ? C61 C62 C63 N12 2.3(4) . . . . ? C61 C62 C63 C64 -177.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.705 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.087 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_Si2Cl2pz4 _database_code_depnum_ccdc_archive 'CCDC 725893' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Cl2 N8 Si2' _chemical_formula_sum 'C20 H28 Cl2 N8 Si2' _chemical_formula_weight 507.58 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.486(2) _cell_length_b 10.342(2) _cell_length_c 20.670(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.65(3) _cell_angle_gamma 90.00 _cell_volume 2364.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8045 _cell_measurement_theta_min 4.44 _cell_measurement_theta_max 25.99 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.403 _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 200(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 'Stoe Stadi 4 with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8045 _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.44 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2310 _reflns_number_gt 1944 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0672P)^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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2310 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.17252(6) 0.97291(7) 0.05890(4) 0.0297(2) Uani 1 1 d . . . Si2 Si 0.23537(7) 0.78976(8) 0.04935(4) 0.0221(2) Uani 1 1 d . . . N1 N 0.2600(2) 0.7189(2) 0.12924(12) 0.0266(6) Uani 1 1 d . . . N3 N 0.0820(2) 0.7117(2) 0.00425(11) 0.0219(5) Uani 1 1 d . . . N2 N 0.1929(2) 0.7627(2) 0.17201(12) 0.0298(6) Uani 1 1 d . . . C20 C -0.0840(3) 0.7247(3) 0.05903(16) 0.0333(7) Uani 1 1 d . . . H20A H -0.0178 0.7493 0.0980 0.050 Uiso 1 1 calc R . . H20B H -0.1280 0.6513 0.0709 0.050 Uiso 1 1 calc R . . H20C H -0.1393 0.7980 0.0454 0.050 Uiso 1 1 calc R . . C21 C -0.0338(2) 0.6875(3) 0.00247(15) 0.0251(6) Uani 1 1 d . . . C13 C 0.2312(3) 0.6940(3) 0.22729(15) 0.0309(7) Uani 1 1 d . . . C22 C -0.0890(3) 0.6291(3) -0.05829(16) 0.0286(7) Uani 1 1 d . . . H22 H -0.1707 0.6009 -0.0729 0.034 Uiso 1 1 calc R . . C11 C 0.3376(3) 0.6238(3) 0.16032(16) 0.0295(7) Uani 1 1 d . . . C14 C 0.1802(3) 0.7158(4) 0.28576(18) 0.0431(9) Uani 1 1 d . . . H14A H 0.1226 0.7878 0.2757 0.065 Uiso 1 1 calc R . . H14B H 0.2458 0.7366 0.3257 0.065 Uiso 1 1 calc R . . H14C H 0.1387 0.6373 0.2942 0.065 Uiso 1 1 calc R . . C10 C 0.4224(3) 0.5590(3) 0.12789(18) 0.0406(8) Uani 1 1 d . . . H10A H 0.4880 0.6186 0.1265 0.061 Uiso 1 1 calc R . . H10B H 0.3791 0.5337 0.0820 0.061 Uiso 1 1 calc R . . H10C H 0.4563 0.4819 0.1538 0.061 Uiso 1 1 calc R . . C12 C 0.3202(3) 0.6064(3) 0.22229(17) 0.0356(8) Uani 1 1 d . . . H12 H 0.3607 0.5463 0.2555 0.043 Uiso 1 1 calc R . . N4 N 0.1004(2) 0.6684(2) -0.05574(12) 0.0244(5) Uani 1 1 d . . . C23 C -0.0034(3) 0.6195(3) -0.09371(16) 0.0270(7) Uani 1 1 d . . . C24 C -0.0136(3) 0.5721(4) -0.16252(17) 0.0376(8) Uani 1 1 d . . . H24A H -0.0510 0.6390 -0.1951 0.056 Uiso 1 1 calc R . . H24B H -0.0637 0.4940 -0.1709 0.056 Uiso 1 1 calc R . . H24C H 0.0671 0.5520 -0.1672 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 0.0303(4) 0.0269(4) 0.0329(5) -0.0034(3) 0.0104(3) 0.0018(3) Si2 0.0196(4) 0.0258(4) 0.0213(5) -0.0015(3) 0.0061(3) -0.0013(3) N1 0.0248(12) 0.0329(14) 0.0226(13) -0.0015(11) 0.0074(10) -0.0001(10) N3 0.0203(12) 0.0265(13) 0.0202(13) -0.0024(10) 0.0078(10) -0.0015(9) N2 0.0283(13) 0.0416(15) 0.0218(14) 0.0002(12) 0.0108(11) -0.0013(11) C20 0.0265(16) 0.0412(18) 0.0361(19) -0.0038(15) 0.0152(15) -0.0036(13) C21 0.0204(14) 0.0253(15) 0.0302(17) 0.0009(12) 0.0079(13) -0.0006(11) C13 0.0301(16) 0.0403(18) 0.0215(16) -0.0016(14) 0.0054(13) -0.0114(13) C22 0.0182(14) 0.0302(16) 0.0355(18) -0.0029(13) 0.0041(13) -0.0041(12) C11 0.0309(16) 0.0283(16) 0.0257(17) 0.0010(13) 0.0011(13) -0.0011(12) C14 0.045(2) 0.059(2) 0.0278(18) 0.0004(16) 0.0146(16) -0.0082(17) C10 0.046(2) 0.041(2) 0.033(2) 0.0007(15) 0.0067(16) 0.0136(15) C12 0.0412(18) 0.0361(18) 0.0232(17) 0.0071(14) -0.0019(14) -0.0027(14) N4 0.0243(12) 0.0289(13) 0.0209(13) -0.0027(10) 0.0077(10) -0.0017(10) C23 0.0259(15) 0.0233(15) 0.0289(17) -0.0037(12) 0.0023(13) -0.0020(11) C24 0.0334(17) 0.047(2) 0.0298(18) -0.0147(16) 0.0047(14) -0.0045(15) _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 Si2 2.0554(11) . ? Si2 N1 1.758(3) . ? Si2 N4 1.905(2) 7_565 ? Si2 N3 1.933(2) . ? Si2 Si2 2.3067(16) 7_565 ? N1 C11 1.365(4) . ? N1 N2 1.396(3) . ? N3 C21 1.343(3) . ? N3 N4 1.388(3) . ? N2 C13 1.317(4) . ? C20 C21 1.487(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.384(4) . ? C13 C12 1.390(4) . ? C13 C14 1.496(4) . ? C22 C23 1.379(4) . ? C22 H22 0.9500 . ? C11 C12 1.361(5) . ? C11 C10 1.483(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 H12 0.9500 . ? N4 C23 1.337(4) . ? N4 Si2 1.905(2) 7_565 ? C23 C24 1.479(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 N1 Si2 N4 97.12(12) . 7_565 ? N1 Si2 N3 100.01(11) . . ? N4 Si2 N3 152.23(10) 7_565 . ? N1 Si2 Cl1 105.41(9) . . ? N4 Si2 Cl1 98.67(8) 7_565 . ? N3 Si2 Cl1 97.64(8) . . ? N1 Si2 Si2 131.06(10) . 7_565 ? N4 Si2 Si2 76.38(8) 7_565 7_565 ? N3 Si2 Si2 75.89(8) . 7_565 ? Cl1 Si2 Si2 123.53(6) . 7_565 ? C11 N1 N2 109.7(2) . . ? C11 N1 Si2 131.4(2) . . ? N2 N1 Si2 118.87(19) . . ? C21 N3 N4 107.7(2) . . ? C21 N3 Si2 149.0(2) . . ? N4 N3 Si2 103.11(15) . . ? C13 N2 N1 105.2(2) . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 108.3(2) . . ? N3 C21 C20 121.4(3) . . ? C22 C21 C20 130.2(3) . . ? N2 C13 C12 111.5(3) . . ? N2 C13 C14 120.5(3) . . ? C12 C13 C14 127.9(3) . . ? C23 C22 C21 107.2(3) . . ? C23 C22 H22 126.4 . . ? C21 C22 H22 126.4 . . ? C12 C11 N1 107.2(3) . . ? C12 C11 C10 130.3(3) . . ? N1 C11 C10 122.5(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 C12 C13 106.4(3) . . ? C11 C12 H12 126.8 . . ? C13 C12 H12 126.8 . . ? C23 N4 N3 108.7(2) . . ? C23 N4 Si2 146.7(2) . 7_565 ? N3 N4 Si2 104.56(17) . 7_565 ? N4 C23 C22 108.2(3) . . ? N4 C23 C24 121.1(3) . . ? C22 C23 C24 130.7(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 N4 Si2 N1 C11 -51.9(3) 7_565 . . . ? N3 Si2 N1 C11 106.1(3) . . . . ? Cl1 Si2 N1 C11 -153.0(3) . . . . ? Si2 Si2 N1 C11 26.2(3) 7_565 . . . ? N4 Si2 N1 N2 127.4(2) 7_565 . . . ? N3 Si2 N1 N2 -74.5(2) . . . . ? Cl1 Si2 N1 N2 26.3(2) . . . . ? Si2 Si2 N1 N2 -154.47(17) 7_565 . . . ? N1 Si2 N3 C21 54.7(4) . . . . ? N4 Si2 N3 C21 -178.1(3) 7_565 . . . ? Cl1 Si2 N3 C21 -52.6(4) . . . . ? Si2 Si2 N3 C21 -175.3(4) 7_565 . . . ? N1 Si2 N3 N4 -131.88(17) . . . . ? N4 Si2 N3 N4 -4.6(4) 7_565 . . . ? Cl1 Si2 N3 N4 120.91(15) . . . . ? Si2 Si2 N3 N4 -1.83(15) 7_565 . . . ? C11 N1 N2 C13 0.1(3) . . . . ? Si2 N1 N2 C13 -179.4(2) . . . . ? N4 N3 C21 C22 0.0(3) . . . . ? Si2 N3 C21 C22 173.3(3) . . . . ? N4 N3 C21 C20 -178.9(3) . . . . ? Si2 N3 C21 C20 -5.5(6) . . . . ? N1 N2 C13 C12 -0.3(3) . . . . ? N1 N2 C13 C14 179.1(3) . . . . ? N3 C21 C22 C23 -0.5(3) . . . . ? C20 C21 C22 C23 178.2(3) . . . . ? N2 N1 C11 C12 0.2(3) . . . . ? Si2 N1 C11 C12 179.6(2) . . . . ? N2 N1 C11 C10 -179.2(3) . . . . ? Si2 N1 C11 C10 0.2(5) . . . . ? N1 C11 C12 C13 -0.4(3) . . . . ? C10 C11 C12 C13 178.9(3) . . . . ? N2 C13 C12 C11 0.5(4) . . . . ? C14 C13 C12 C11 -178.9(3) . . . . ? C21 N3 N4 C23 0.6(3) . . . . ? Si2 N3 N4 C23 -175.92(19) . . . . ? C21 N3 N4 Si2 178.70(18) . . . 7_565 ? Si2 N3 N4 Si2 2.23(18) . . . 7_565 ? N3 N4 C23 C22 -0.9(3) . . . . ? Si2 N4 C23 C22 -177.6(3) 7_565 . . . ? N3 N4 C23 C24 176.5(3) . . . . ? Si2 N4 C23 C24 -0.2(6) 7_565 . . . ? C21 C22 C23 N4 0.8(3) . . . . ? C21 C22 C23 C24 -176.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.466 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.098 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_Si2Cl4pz2 _database_code_depnum_ccdc_archive 'CCDC 725894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H14 Cl4 N4 Si2' _chemical_formula_sum 'C10 H14 Cl4 N4 Si2' _chemical_formula_weight 388.23 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 C2/m _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.339(3) _cell_length_b 7.4284(15) _cell_length_c 8.6263(17) _cell_angle_alpha 90.00 _cell_angle_beta 108.76(3) _cell_angle_gamma 90.00 _cell_volume 809.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 749 _cell_measurement_theta_min 5.00 _cell_measurement_theta_max 24.98 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 0.873 _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 150(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 'Stoe Stadi 4 with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1874 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 24.98 _reflns_number_total 749 _reflns_number_gt 670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0336P)^2^+0.6383P] 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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 749 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.47694(6) 0.5000 0.36064(9) 0.0179(2) Uani 1 2 d S . . Cl1 Cl 0.45195(4) 0.72255(8) 0.21094(7) 0.0291(2) Uani 1 1 d . . . N1 N 0.34256(19) 0.5000 0.3997(3) 0.0186(6) Uani 1 2 d S . . C12 C 0.1966(2) 0.5000 0.4673(4) 0.0209(7) Uani 1 2 d S . . H12 H 0.1240 0.5000 0.4600 0.025 Uiso 1 2 calc SR . . C10 C 0.1809(3) 0.5000 0.1580(4) 0.0258(7) Uani 1 2 d S . . H10A H 0.1136 0.5646 0.1340 0.039 Uiso 0.50 1 calc PR . . H10B H 0.1674 0.3756 0.1189 0.039 Uiso 0.50 1 calc PR . . H10C H 0.2255 0.5598 0.1027 0.039 Uiso 0.50 1 calc PR . . C11 C 0.2363(2) 0.5000 0.3381(4) 0.0204(7) Uani 1 2 d S . . N2 N 0.37141(19) 0.5000 0.5685(3) 0.0188(5) Uani 1 2 d S . . C13 C 0.2827(2) 0.5000 0.6102(4) 0.0208(7) Uani 1 2 d S . . C14 C 0.2874(3) 0.5000 0.7837(4) 0.0260(7) Uani 1 2 d S . . H14A H 0.3555 0.4506 0.8514 0.039 Uiso 0.50 1 calc PR . . H14B H 0.2298 0.4259 0.7964 0.039 Uiso 0.50 1 calc PR . . H14C H 0.2801 0.6236 0.8184 0.039 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0171(4) 0.0224(5) 0.0147(4) 0.000 0.0057(3) 0.000 Cl1 0.0257(3) 0.0327(4) 0.0292(4) 0.0120(2) 0.0090(2) 0.0024(2) N1 0.0195(13) 0.0237(14) 0.0122(12) 0.000 0.0043(10) 0.000 C12 0.0161(15) 0.0211(16) 0.0262(16) 0.000 0.0080(12) 0.000 C10 0.0229(16) 0.0307(17) 0.0218(16) 0.000 0.0044(13) 0.000 C11 0.0199(16) 0.0188(15) 0.0209(16) 0.000 0.0043(12) 0.000 N2 0.0186(13) 0.0226(13) 0.0148(12) 0.000 0.0050(10) 0.000 C13 0.0224(16) 0.0194(16) 0.0244(16) 0.000 0.0128(13) 0.000 C14 0.0287(17) 0.0295(17) 0.0236(17) 0.000 0.0139(14) 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 Si1 N2 1.916(3) 5_666 ? Si1 N1 1.927(3) . ? Si1 Cl1 2.0579(8) 6_565 ? Si1 Cl1 2.0579(8) . ? Si1 Si1 2.2821(16) 5_666 ? N1 C11 1.345(4) . ? N1 N2 1.382(3) . ? C12 C11 1.379(4) . ? C12 C13 1.388(4) . ? C12 H12 0.9500 . ? C10 C11 1.490(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N2 C13 1.343(4) . ? C13 C14 1.478(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 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 152.90(10) 5_666 . ? N2 Si1 Cl1 98.13(5) 5_666 6_565 ? N1 Si1 Cl1 97.91(5) . 6_565 ? N2 Si1 Cl1 98.13(5) 5_666 . ? N1 Si1 Cl1 97.91(5) . . ? Cl1 Si1 Cl1 106.90(5) 6_565 . ? N2 Si1 Si1 76.40(9) 5_666 5_666 ? N1 Si1 Si1 76.49(8) . 5_666 ? Cl1 Si1 Si1 126.55(3) 6_565 5_666 ? Cl1 Si1 Si1 126.55(3) . 5_666 ? C11 N1 N2 108.5(2) . . ? C11 N1 Si1 148.5(2) . . ? N2 N1 Si1 103.00(16) . . ? C11 C12 C13 107.1(3) . . ? C11 C12 H12 126.4 . . ? C13 C12 H12 126.4 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 108.1(3) . . ? N1 C11 C10 121.2(3) . . ? C12 C11 C10 130.7(3) . . ? C13 N2 N1 108.1(2) . . ? C13 N2 Si1 147.8(2) . 5_666 ? N1 N2 Si1 104.10(16) . 5_666 ? N2 C13 C12 108.1(3) . . ? N2 C13 C14 121.1(3) . . ? C12 C13 C14 130.8(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 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 C11 180.0 5_666 . . . ? Cl1 Si1 N1 C11 -54.20(3) 6_565 . . . ? Cl1 Si1 N1 C11 54.20(3) . . . . ? Si1 Si1 N1 C11 180.0 5_666 . . . ? N2 Si1 N1 N2 0.0 5_666 . . . ? Cl1 Si1 N1 N2 125.80(3) 6_565 . . . ? Cl1 Si1 N1 N2 -125.80(3) . . . . ? Si1 Si1 N1 N2 0.0 5_666 . . . ? N2 N1 C11 C12 0.0 . . . . ? Si1 N1 C11 C12 180.0 . . . . ? N2 N1 C11 C10 180.0 . . . . ? Si1 N1 C11 C10 0.0 . . . . ? C13 C12 C11 N1 0.0 . . . . ? C13 C12 C11 C10 180.0 . . . . ? C11 N1 N2 C13 0.0 . . . . ? Si1 N1 N2 C13 180.0 . . . . ? C11 N1 N2 Si1 180.0 . . . 5_666 ? Si1 N1 N2 Si1 0.0 . . . 5_666 ? N1 N2 C13 C12 0.0 . . . . ? Si1 N2 C13 C12 180.0 5_666 . . . ? N1 N2 C13 C14 180.0 . . . . ? Si1 N2 C13 C14 0.000(1) 5_666 . . . ? C11 C12 C13 N2 0.0 . . . . ? C11 C12 C13 C14 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.405 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.068 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_Sipz4 _database_code_depnum_ccdc_archive 'CCDC 725895' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 N8 Si' _chemical_formula_sum 'C20 H28 N8 Si' _chemical_formula_weight 408.59 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' _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 9.327(2) _cell_length_b 11.782(2) _cell_length_c 20.178(4) _cell_angle_alpha 88.29(3) _cell_angle_beta 84.85(3) _cell_angle_gamma 80.96(3) _cell_volume 2180.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12421 _cell_measurement_theta_min 3.92 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.131 _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 150(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 'Stoe Stadi 4 with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12421 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.1265 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7483 _reflns_number_gt 4153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0518P)^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 7483 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.64983(9) 0.73096(8) 0.07878(4) 0.0225(2) Uani 1 1 d . . . N1 N 0.7056(3) 0.8307(2) 0.12757(13) 0.0232(6) Uani 1 1 d . . . Si2 Si 0.64619(10) 0.73305(8) 0.59310(5) 0.0262(2) Uani 1 1 d . . . N2 N 0.8063(3) 0.7938(2) 0.17357(13) 0.0266(7) Uani 1 1 d . . . N3 N 0.4623(3) 0.7527(2) 0.08379(13) 0.0229(6) Uani 1 1 d . . . N4 N 0.3966(3) 0.7787(2) 0.02450(13) 0.0251(6) Uani 1 1 d . . . N5 N 0.7133(3) 0.5947(2) 0.10634(13) 0.0242(6) Uani 1 1 d . . . N6 N 0.6141(3) 0.5268(2) 0.13482(13) 0.0284(7) Uani 1 1 d . . . N7 N 0.7154(3) 0.7429(2) -0.00285(13) 0.0230(6) Uani 1 1 d . . . N8 N 0.7842(3) 0.8361(2) -0.02466(13) 0.0242(6) Uani 1 1 d . . . N9 N 0.4610(3) 0.7527(2) 0.61075(13) 0.0299(7) Uani 1 1 d . . . N10 N 0.4013(3) 0.6584(2) 0.63903(14) 0.0337(7) Uani 1 1 d . . . C10 C 0.5539(4) 1.0097(3) 0.08793(18) 0.0332(9) Uani 1 1 d . . . H10B H 0.5858 0.9914 0.0413 0.050 Uiso 1 1 calc R . . H10C H 0.5462 1.0927 0.0941 0.050 Uiso 1 1 calc R . . H10D H 0.4586 0.9859 0.0996 0.050 Uiso 1 1 calc R . . N11 N 0.6960(3) 0.7212(2) 0.50938(13) 0.0266(7) Uani 1 1 d . . . C11 C 0.6613(3) 0.9479(3) 0.13142(16) 0.0262(8) Uani 1 1 d . . . N12 N 0.5895(3) 0.7396(2) 0.46491(14) 0.0321(7) Uani 1 1 d . . . C12 C 0.7345(3) 0.9861(3) 0.17931(16) 0.0285(8) Uani 1 1 d . . . H12B H 0.7280 1.0631 0.1934 0.034 Uiso 1 1 calc R . . N13 N 0.7120(3) 0.8497(2) 0.62166(13) 0.0252(6) Uani 1 1 d . . . C13 C 0.2557(3) 0.8018(3) 0.04354(17) 0.0274(8) Uani 1 1 d . . . C23 C 0.8220(3) 0.8882(3) 0.20386(16) 0.0280(8) Uani 1 1 d . . . N14 N 0.7904(3) 0.9132(2) 0.57581(14) 0.0308(7) Uani 1 1 d . . . C14 C 0.9195(4) 0.8830(3) 0.25911(18) 0.0400(10) Uani 1 1 d . . . H14B H 0.9751 0.8055 0.2622 0.060 Uiso 1 1 calc R . . H14C H 0.8604 0.9014 0.3012 0.060 Uiso 1 1 calc R . . H14D H 0.9869 0.9387 0.2502 0.060 Uiso 1 1 calc R . . N15 N 0.7201(3) 0.6056(2) 0.62969(13) 0.0258(7) Uani 1 1 d . . . N16 N 0.7856(3) 0.6070(2) 0.68912(13) 0.0273(7) Uani 1 1 d . . . C20 C 0.4007(4) 0.7409(3) 0.20630(16) 0.0380(9) Uani 1 1 d . . . H20A H 0.3126 0.7514 0.2372 0.057 Uiso 1 1 calc R . . H20B H 0.4644 0.7955 0.2166 0.057 Uiso 1 1 calc R . . H20C H 0.4522 0.6623 0.2108 0.057 Uiso 1 1 calc R . . C21 C 0.3600(3) 0.7613(3) 0.13775(16) 0.0255(8) Uani 1 1 d . . . C22 C 0.2290(4) 0.7916(3) 0.11282(17) 0.0287(8) Uani 1 1 d . . . H22A H 0.1365 0.8036 0.1376 0.034 Uiso 1 1 calc R . . C24 C 0.1501(4) 0.8384(3) -0.00667(18) 0.0425(10) Uani 1 1 d . . . H24A H 0.1764 0.7909 -0.0463 0.064 Uiso 1 1 calc R . . H24B H 0.1523 0.9192 -0.0190 0.064 Uiso 1 1 calc R . . H24C H 0.0519 0.8293 0.0121 0.064 Uiso 1 1 calc R . . C30 C 0.9785(3) 0.5846(3) 0.07189(18) 0.0344(9) Uani 1 1 d . . . H30A H 1.0671 0.5277 0.0728 0.052 Uiso 1 1 calc R . . H30B H 0.9876 0.6508 0.0986 0.052 Uiso 1 1 calc R . . H30C H 0.9648 0.6099 0.0259 0.052 Uiso 1 1 calc R . . C31 C 0.8513(3) 0.5322(3) 0.09975(16) 0.0251(8) Uani 1 1 d . . . C32 C 0.8389(4) 0.4254(3) 0.12446(17) 0.0318(9) Uani 1 1 d . . . H32A H 0.9157 0.3626 0.1271 0.038 Uiso 1 1 calc R . . C33 C 0.6926(4) 0.4254(3) 0.14520(17) 0.0318(9) Uani 1 1 d . . . C34 C 0.6199(4) 0.3290(3) 0.1750(2) 0.0469(11) Uani 1 1 d . . . H34A H 0.5292 0.3606 0.2009 0.070 Uiso 1 1 calc R . . H34B H 0.6849 0.2822 0.2043 0.070 Uiso 1 1 calc R . . H34C H 0.5980 0.2812 0.1395 0.070 Uiso 1 1 calc R . . C40 C 0.6359(3) 0.5685(3) -0.04692(17) 0.0311(8) Uani 1 1 d . . . H40A H 0.6439 0.5294 -0.0896 0.047 Uiso 1 1 calc R . . H40B H 0.5328 0.5903 -0.0315 0.047 Uiso 1 1 calc R . . H40C H 0.6844 0.5167 -0.0140 0.047 Uiso 1 1 calc R . . C41 C 0.7064(3) 0.6732(3) -0.05545(16) 0.0258(8) Uani 1 1 d . . . C42 C 0.7697(3) 0.7217(3) -0.11010(17) 0.0290(8) Uani 1 1 d . . . H42A H 0.7805 0.6935 -0.1542 0.035 Uiso 1 1 calc R . . C43 C 0.8163(3) 0.8217(3) -0.08905(17) 0.0272(8) Uani 1 1 d . . . C44 C 0.8935(4) 0.9046(3) -0.12999(18) 0.0373(9) Uani 1 1 d . . . H44A H 0.9274 0.9577 -0.1007 0.056 Uiso 1 1 calc R . . H44B H 0.8266 0.9480 -0.1597 0.056 Uiso 1 1 calc R . . H44C H 0.9772 0.8624 -0.1565 0.056 Uiso 1 1 calc R . . C50 C 0.3857(4) 0.9548(3) 0.5721(2) 0.0591(13) Uani 1 1 d . . . H50A H 0.2946 1.0079 0.5686 0.089 Uiso 1 1 calc R . . H50B H 0.4360 0.9409 0.5277 0.089 Uiso 1 1 calc R . . H50C H 0.4482 0.9884 0.6001 0.089 Uiso 1 1 calc R . . C51 C 0.3530(4) 0.8447(3) 0.60233(18) 0.0379(9) Uani 1 1 d . . . C52 C 0.2269(4) 0.8110(4) 0.62534(19) 0.0417(10) Uani 1 1 d . . . H52A H 0.1329 0.8562 0.6263 0.050 Uiso 1 1 calc R . . C53 C 0.2593(4) 0.6966(3) 0.64770(18) 0.0385(10) Uani 1 1 d . . . C54 C 0.1600(4) 0.6178(4) 0.6781(2) 0.0596(13) Uani 1 1 d . . . H54A H 0.2157 0.5570 0.7038 0.089 Uiso 1 1 calc R . . H54B H 0.1162 0.5832 0.6428 0.089 Uiso 1 1 calc R . . H54C H 0.0829 0.6613 0.7076 0.089 Uiso 1 1 calc R . . C60 C 0.9645(4) 0.6627(3) 0.51147(18) 0.0350(9) Uani 1 1 d . . . H60A H 0.9725 0.7284 0.5388 0.052 Uiso 1 1 calc R . . H60B H 1.0493 0.6490 0.4787 0.052 Uiso 1 1 calc R . . H60C H 0.9609 0.5943 0.5400 0.052 Uiso 1 1 calc R . . C61 C 0.8304(4) 0.6875(3) 0.47663(17) 0.0287(8) Uani 1 1 d . . . C62 C 0.8099(4) 0.6842(3) 0.41115(18) 0.0357(9) Uani 1 1 d . . . H62A H 0.8826 0.6638 0.3756 0.043 Uiso 1 1 calc R . . C63 C 0.6611(4) 0.7167(3) 0.40638(17) 0.0376(9) Uani 1 1 d . . . C64 C 0.5806(5) 0.7255(4) 0.34523(19) 0.0603(13) Uani 1 1 d . . . H64A H 0.4810 0.7652 0.3557 0.090 Uiso 1 1 calc R . . H64B H 0.5776 0.6482 0.3293 0.090 Uiso 1 1 calc R . . H64C H 0.6305 0.7689 0.3106 0.090 Uiso 1 1 calc R . . C70 C 0.5995(4) 0.8598(3) 0.73860(17) 0.0418(10) Uani 1 1 d . . . H70A H 0.5989 0.9084 0.7772 0.063 Uiso 1 1 calc R . . H70B H 0.6432 0.7809 0.7492 0.063 Uiso 1 1 calc R . . H70C H 0.4993 0.8605 0.7274 0.063 Uiso 1 1 calc R . . C71 C 0.6850(4) 0.9042(3) 0.68170(17) 0.0310(8) Uani 1 1 d . . . C72 C 0.7474(4) 1.0013(3) 0.67451(18) 0.0359(9) Uani 1 1 d . . . H72A H 0.7482 1.0567 0.7077 0.043 Uiso 1 1 calc R . . C73 C 0.8102(4) 1.0038(3) 0.60906(19) 0.0351(9) Uani 1 1 d . . . C74 C 0.8879(5) 1.0940(3) 0.5751(2) 0.0539(12) Uani 1 1 d . . . H74A H 0.9393 1.0641 0.5332 0.081 Uiso 1 1 calc R . . H74B H 0.9583 1.1151 0.6039 0.081 Uiso 1 1 calc R . . H74C H 0.8171 1.1620 0.5658 0.081 Uiso 1 1 calc R . . C80 C 0.6491(4) 0.4655(3) 0.55142(17) 0.0367(9) Uani 1 1 d . . . H80A H 0.6464 0.3827 0.5511 0.055 Uiso 1 1 calc R . . H80B H 0.7056 0.4878 0.5112 0.055 Uiso 1 1 calc R . . H80C H 0.5495 0.5076 0.5526 0.055 Uiso 1 1 calc R . . C81 C 0.7188(3) 0.4939(3) 0.61145(17) 0.0282(8) Uani 1 1 d . . . C82 C 0.7844(4) 0.4247(3) 0.65788(16) 0.0305(8) Uani 1 1 d . . . H82A H 0.8013 0.3430 0.6585 0.037 Uiso 1 1 calc R . . C83 C 0.8232(3) 0.4975(3) 0.70531(16) 0.0269(8) Uani 1 1 d . . . C84 C 0.8973(4) 0.4640(3) 0.76619(17) 0.0374(9) Uani 1 1 d . . . H84A H 0.9252 0.5321 0.7852 0.056 Uiso 1 1 calc R . . H84B H 0.9847 0.4078 0.7551 0.056 Uiso 1 1 calc R . . H84C H 0.8312 0.4300 0.7987 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 Si1 0.0198(5) 0.0217(5) 0.0265(5) 0.0019(4) -0.0045(4) -0.0038(4) N1 0.0191(14) 0.0251(16) 0.0262(15) 0.0010(12) -0.0052(12) -0.0038(12) Si2 0.0242(5) 0.0291(6) 0.0265(5) 0.0019(4) -0.0041(4) -0.0072(4) N2 0.0234(15) 0.0272(17) 0.0303(16) -0.0001(13) -0.0095(13) -0.0033(12) N3 0.0248(15) 0.0212(15) 0.0240(15) 0.0024(12) -0.0059(13) -0.0057(12) N4 0.0255(16) 0.0244(16) 0.0262(16) 0.0028(12) -0.0076(13) -0.0038(12) N5 0.0199(15) 0.0221(16) 0.0325(16) 0.0025(13) -0.0065(13) -0.0076(12) N6 0.0267(16) 0.0268(17) 0.0343(17) 0.0035(13) -0.0074(13) -0.0103(13) N7 0.0225(15) 0.0210(15) 0.0270(16) 0.0018(12) -0.0041(12) -0.0069(12) N8 0.0203(15) 0.0232(16) 0.0293(16) 0.0049(12) -0.0052(12) -0.0037(12) N9 0.0241(16) 0.0369(18) 0.0288(17) 0.0051(14) -0.0030(13) -0.0057(14) N10 0.0314(18) 0.0362(18) 0.0363(18) 0.0035(14) -0.0035(14) -0.0146(14) C10 0.031(2) 0.025(2) 0.043(2) 0.0016(17) -0.0077(17) -0.0023(16) N11 0.0245(16) 0.0290(17) 0.0285(16) 0.0029(13) -0.0084(13) -0.0076(13) C11 0.0227(18) 0.023(2) 0.032(2) 0.0005(15) -0.0002(15) -0.0015(15) N12 0.0314(17) 0.0377(19) 0.0293(17) 0.0047(14) -0.0090(14) -0.0094(14) C12 0.0283(19) 0.025(2) 0.033(2) -0.0074(16) -0.0037(16) -0.0041(15) N13 0.0249(15) 0.0273(16) 0.0242(16) 0.0033(13) -0.0022(13) -0.0072(12) C13 0.0234(19) 0.025(2) 0.035(2) 0.0004(16) -0.0086(16) -0.0047(15) C23 0.0266(19) 0.029(2) 0.030(2) -0.0038(16) -0.0044(16) -0.0057(16) N14 0.0311(16) 0.0279(17) 0.0337(17) 0.0000(14) 0.0016(14) -0.0075(13) C14 0.042(2) 0.041(2) 0.039(2) -0.0046(18) -0.0172(19) -0.0066(19) N15 0.0247(15) 0.0289(17) 0.0246(15) 0.0016(13) -0.0050(13) -0.0053(13) N16 0.0262(16) 0.0317(18) 0.0250(16) 0.0020(13) -0.0052(13) -0.0065(13) C20 0.040(2) 0.046(2) 0.025(2) -0.0012(17) 0.0026(17) -0.0002(18) C21 0.0249(19) 0.0239(19) 0.0272(19) -0.0008(15) 0.0044(16) -0.0054(15) C22 0.0187(18) 0.028(2) 0.039(2) -0.0007(16) 0.0004(16) -0.0030(15) C24 0.029(2) 0.053(3) 0.046(2) 0.007(2) -0.0146(18) -0.0041(18) C30 0.027(2) 0.034(2) 0.041(2) -0.0030(18) -0.0040(17) -0.0036(17) C31 0.0251(19) 0.0222(19) 0.0292(19) -0.0022(15) -0.0063(15) -0.0047(15) C32 0.033(2) 0.023(2) 0.039(2) 0.0005(16) -0.0142(17) 0.0019(16) C33 0.036(2) 0.025(2) 0.037(2) 0.0042(16) -0.0109(17) -0.0076(17) C34 0.056(3) 0.029(2) 0.058(3) 0.011(2) -0.010(2) -0.0110(19) C40 0.0268(19) 0.035(2) 0.033(2) -0.0052(17) -0.0014(16) -0.0085(16) C41 0.0215(18) 0.029(2) 0.027(2) -0.0014(16) -0.0044(15) -0.0022(15) C42 0.0258(19) 0.033(2) 0.027(2) -0.0024(16) -0.0040(16) -0.0012(16) C43 0.0214(18) 0.030(2) 0.029(2) 0.0058(16) -0.0023(15) 0.0007(15) C44 0.039(2) 0.037(2) 0.034(2) 0.0110(17) 0.0033(18) -0.0084(18) C50 0.042(3) 0.050(3) 0.080(3) 0.024(2) -0.002(2) -0.001(2) C51 0.028(2) 0.041(2) 0.043(2) 0.0101(19) -0.0047(18) -0.0023(18) C52 0.019(2) 0.056(3) 0.049(3) 0.003(2) -0.0027(18) -0.0042(18) C53 0.027(2) 0.052(3) 0.040(2) 0.003(2) -0.0023(17) -0.0177(19) C54 0.034(2) 0.076(3) 0.074(3) 0.010(3) 0.001(2) -0.031(2) C60 0.028(2) 0.038(2) 0.038(2) -0.0011(18) 0.0021(17) -0.0075(17) C61 0.027(2) 0.028(2) 0.031(2) 0.0004(16) 0.0009(16) -0.0073(16) C62 0.041(2) 0.042(2) 0.026(2) -0.0047(17) 0.0028(17) -0.0134(18) C63 0.043(2) 0.051(3) 0.024(2) 0.0056(18) -0.0094(18) -0.0211(19) C64 0.056(3) 0.096(4) 0.034(2) 0.012(2) -0.014(2) -0.026(3) C70 0.044(2) 0.051(3) 0.029(2) -0.0018(19) -0.0002(18) -0.004(2) C71 0.0266(19) 0.035(2) 0.030(2) -0.0032(17) -0.0043(16) -0.0002(16) C72 0.041(2) 0.033(2) 0.036(2) -0.0088(17) -0.0048(18) -0.0072(18) C73 0.035(2) 0.025(2) 0.045(2) -0.0057(17) 0.0007(18) -0.0059(17) C74 0.070(3) 0.036(2) 0.059(3) -0.007(2) 0.011(2) -0.026(2) C80 0.041(2) 0.036(2) 0.036(2) -0.0018(17) -0.0101(18) -0.0098(18) C81 0.0253(19) 0.029(2) 0.031(2) 0.0002(16) 0.0016(16) -0.0088(16) C82 0.036(2) 0.025(2) 0.031(2) 0.0011(16) -0.0030(17) -0.0082(16) C83 0.0286(19) 0.027(2) 0.0258(19) 0.0020(15) -0.0001(15) -0.0070(16) C84 0.050(2) 0.033(2) 0.030(2) 0.0027(17) -0.0084(18) -0.0055(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N7 1.714(3) . ? Si1 N5 1.716(3) . ? Si1 N3 1.722(3) . ? Si1 N1 1.724(3) . ? N1 C11 1.380(4) . ? N1 N2 1.392(3) . ? Si2 N9 1.712(3) . ? Si2 N11 1.715(3) . ? Si2 N13 1.724(3) . ? Si2 N15 1.725(3) . ? N2 C23 1.319(4) . ? N3 C21 1.377(4) . ? N3 N4 1.397(3) . ? N4 C13 1.324(4) . ? N5 C31 1.376(4) . ? N5 N6 1.391(3) . ? N6 C33 1.321(4) . ? N7 C41 1.378(4) . ? N7 N8 1.398(3) . ? N8 C43 1.317(4) . ? N9 C51 1.376(4) . ? N9 N10 1.403(4) . ? N10 C53 1.327(4) . ? C10 C11 1.481(4) . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? N11 C61 1.369(4) . ? N11 N12 1.386(3) . ? C11 C12 1.358(4) . ? N12 C63 1.317(4) . ? C12 C23 1.409(4) . ? C12 H12B 0.9500 . ? N13 C71 1.373(4) . ? N13 N14 1.400(4) . ? C13 C22 1.403(5) . ? C13 C24 1.484(4) . ? C23 C14 1.495(4) . ? N14 C73 1.323(4) . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? N15 C81 1.380(4) . ? N15 N16 1.395(3) . ? N16 C83 1.322(4) . ? C20 C21 1.470(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.355(4) . ? C22 H22A 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C30 C31 1.481(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.358(4) . ? C32 C33 1.391(5) . ? C32 H32A 0.9500 . ? C33 C34 1.496(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C40 C41 1.485(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.358(4) . ? C42 C43 1.407(4) . ? C42 H42A 0.9500 . ? C43 C44 1.490(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C50 C51 1.480(5) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.340(5) . ? C52 C53 1.405(5) . ? C52 H52A 0.9500 . ? C53 C54 1.494(5) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C60 C61 1.475(4) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.354(5) . ? C62 C63 1.392(5) . ? C62 H62A 0.9500 . ? C63 C64 1.493(5) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C70 C71 1.469(5) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.361(5) . ? C72 C73 1.397(5) . ? C72 H72A 0.9500 . ? C73 C74 1.495(5) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C80 C81 1.495(4) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.348(4) . ? C82 C83 1.411(4) . ? C82 H82A 0.9500 . ? C83 C84 1.476(4) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 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 N7 Si1 N5 107.74(13) . . ? N7 Si1 N3 109.03(13) . . ? N5 Si1 N3 109.96(13) . . ? N7 Si1 N1 111.64(13) . . ? N5 Si1 N1 109.82(13) . . ? N3 Si1 N1 108.64(13) . . ? C11 N1 N2 110.6(2) . . ? C11 N1 Si1 130.1(2) . . ? N2 N1 Si1 119.3(2) . . ? N9 Si2 N11 112.38(13) . . ? N9 Si2 N13 108.54(14) . . ? N11 Si2 N13 108.41(14) . . ? N9 Si2 N15 108.69(14) . . ? N11 Si2 N15 106.55(14) . . ? N13 Si2 N15 112.32(13) . . ? C23 N2 N1 104.6(2) . . ? C21 N3 N4 111.2(2) . . ? C21 N3 Si1 131.4(2) . . ? N4 N3 Si1 117.1(2) . . ? C13 N4 N3 104.2(3) . . ? C31 N5 N6 110.4(2) . . ? C31 N5 Si1 130.3(2) . . ? N6 N5 Si1 119.03(19) . . ? C33 N6 N5 105.0(3) . . ? C41 N7 N8 110.3(3) . . ? C41 N7 Si1 129.1(2) . . ? N8 N7 Si1 120.5(2) . . ? C43 N8 N7 105.3(3) . . ? C51 N9 N10 110.5(3) . . ? C51 N9 Si2 132.9(2) . . ? N10 N9 Si2 116.6(2) . . ? C53 N10 N9 104.1(3) . . ? C11 C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 C10 H10D 109.5 . . ? H10B C10 H10D 109.5 . . ? H10C C10 H10D 109.5 . . ? C61 N11 N12 110.7(3) . . ? C61 N11 Si2 129.8(2) . . ? N12 N11 Si2 119.4(2) . . ? C12 C11 N1 106.9(3) . . ? C12 C11 C10 131.3(3) . . ? N1 C11 C10 121.8(3) . . ? C63 N12 N11 104.4(3) . . ? C11 C12 C23 105.9(3) . . ? C11 C12 H12B 127.0 . . ? C23 C12 H12B 127.0 . . ? C71 N13 N14 110.4(3) . . ? C71 N13 Si2 130.8(2) . . ? N14 N13 Si2 118.1(2) . . ? N4 C13 C22 111.6(3) . . ? N4 C13 C24 119.7(3) . . ? C22 C13 C24 128.7(3) . . ? N2 C23 C12 112.0(3) . . ? N2 C23 C14 120.6(3) . . ? C12 C23 C14 127.3(3) . . ? C73 N14 N13 104.8(3) . . ? C23 C14 H14B 109.5 . . ? C23 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C23 C14 H14D 109.5 . . ? H14B C14 H14D 109.5 . . ? H14C C14 H14D 109.5 . . ? C81 N15 N16 110.2(3) . . ? C81 N15 Si2 129.7(2) . . ? N16 N15 Si2 119.9(2) . . ? C83 N16 N15 104.8(3) . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N3 106.0(3) . . ? C22 C21 C20 131.8(3) . . ? N3 C21 C20 122.1(3) . . ? C21 C22 C13 107.1(3) . . ? C21 C22 H22A 126.5 . . ? C13 C22 H22A 126.5 . . ? C13 C24 H24A 109.5 . . ? C13 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C13 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N5 106.2(3) . . ? C32 C31 C30 132.2(3) . . ? N5 C31 C30 121.5(3) . . ? C31 C32 C33 107.1(3) . . ? C31 C32 H32A 126.4 . . ? C33 C32 H32A 126.4 . . ? N6 C33 C32 111.3(3) . . ? N6 C33 C34 119.8(3) . . ? C32 C33 C34 128.9(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 N7 106.4(3) . . ? C42 C41 C40 131.6(3) . . ? N7 C41 C40 121.9(3) . . ? C41 C42 C43 107.0(3) . . ? C41 C42 H42A 126.5 . . ? C43 C42 H42A 126.5 . . ? N8 C43 C42 111.0(3) . . ? N8 C43 C44 121.0(3) . . ? C42 C43 C44 128.0(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 N9 106.8(3) . . ? C52 C51 C50 131.4(4) . . ? N9 C51 C50 121.8(3) . . ? C51 C52 C53 107.3(3) . . ? C51 C52 H52A 126.3 . . ? C53 C52 H52A 126.3 . . ? N10 C53 C52 111.3(3) . . ? N10 C53 C54 119.0(4) . . ? C52 C53 C54 129.8(3) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 N11 106.7(3) . . ? C62 C61 C60 130.8(3) . . ? N11 C61 C60 122.5(3) . . ? C61 C62 C63 106.2(3) . . ? C61 C62 H62A 126.9 . . ? C63 C62 H62A 126.9 . . ? N12 C63 C62 112.1(3) . . ? N12 C63 C64 120.0(3) . . ? C62 C63 C64 127.9(4) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C71 C70 H70A 109.5 . . ? C71 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C71 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 N13 106.5(3) . . ? C72 C71 C70 130.9(3) . . ? N13 C71 C70 122.6(3) . . ? C71 C72 C73 106.9(3) . . ? C71 C72 H72A 126.5 . . ? C73 C72 H72A 126.5 . . ? N14 C73 C72 111.4(3) . . ? N14 C73 C74 120.1(3) . . ? C72 C73 C74 128.5(3) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C81 C80 H80A 109.5 . . ? C81 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C81 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C82 C81 N15 107.1(3) . . ? C82 C81 C80 130.6(3) . . ? N15 C81 C80 122.3(3) . . ? C81 C82 C83 106.5(3) . . ? C81 C82 H82A 126.8 . . ? C83 C82 H82A 126.8 . . ? N16 C83 C82 111.4(3) . . ? N16 C83 C84 120.8(3) . . ? C82 C83 C84 127.8(3) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 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 N7 Si1 N1 C11 72.9(3) . . . . ? N5 Si1 N1 C11 -167.7(3) . . . . ? N3 Si1 N1 C11 -47.4(3) . . . . ? N7 Si1 N1 N2 -110.2(2) . . . . ? N5 Si1 N1 N2 9.2(3) . . . . ? N3 Si1 N1 N2 129.5(2) . . . . ? C11 N1 N2 C23 -0.5(3) . . . . ? Si1 N1 N2 C23 -177.9(2) . . . . ? N7 Si1 N3 C21 -174.0(3) . . . . ? N5 Si1 N3 C21 68.1(3) . . . . ? N1 Si1 N3 C21 -52.1(3) . . . . ? N7 Si1 N3 N4 -1.8(2) . . . . ? N5 Si1 N3 N4 -119.7(2) . . . . ? N1 Si1 N3 N4 120.1(2) . . . . ? C21 N3 N4 C13 -0.3(3) . . . . ? Si1 N3 N4 C13 -174.1(2) . . . . ? N7 Si1 N5 C31 47.2(3) . . . . ? N3 Si1 N5 C31 165.9(3) . . . . ? N1 Si1 N5 C31 -74.6(3) . . . . ? N7 Si1 N5 N6 -125.7(2) . . . . ? N3 Si1 N5 N6 -7.0(3) . . . . ? N1 Si1 N5 N6 112.5(2) . . . . ? C31 N5 N6 C33 0.2(3) . . . . ? Si1 N5 N6 C33 174.5(2) . . . . ? N5 Si1 N7 C41 52.8(3) . . . . ? N3 Si1 N7 C41 -66.5(3) . . . . ? N1 Si1 N7 C41 173.5(3) . . . . ? N5 Si1 N7 N8 -130.2(2) . . . . ? N3 Si1 N7 N8 110.5(2) . . . . ? N1 Si1 N7 N8 -9.5(3) . . . . ? C41 N7 N8 C43 -0.3(3) . . . . ? Si1 N7 N8 C43 -177.9(2) . . . . ? N11 Si2 N9 C51 -72.8(4) . . . . ? N13 Si2 N9 C51 47.0(4) . . . . ? N15 Si2 N9 C51 169.5(3) . . . . ? N11 Si2 N9 N10 106.5(2) . . . . ? N13 Si2 N9 N10 -133.6(2) . . . . ? N15 Si2 N9 N10 -11.2(3) . . . . ? C51 N9 N10 C53 -0.8(4) . . . . ? Si2 N9 N10 C53 179.7(2) . . . . ? N9 Si2 N11 C61 -168.6(3) . . . . ? N13 Si2 N11 C61 71.4(3) . . . . ? N15 Si2 N11 C61 -49.7(3) . . . . ? N9 Si2 N11 N12 6.5(3) . . . . ? N13 Si2 N11 N12 -113.5(2) . . . . ? N15 Si2 N11 N12 125.4(2) . . . . ? N2 N1 C11 C12 0.6(4) . . . . ? Si1 N1 C11 C12 177.7(2) . . . . ? N2 N1 C11 C10 -179.9(3) . . . . ? Si1 N1 C11 C10 -2.8(5) . . . . ? C61 N11 N12 C63 0.0(4) . . . . ? Si2 N11 N12 C63 -175.9(2) . . . . ? N1 C11 C12 C23 -0.5(4) . . . . ? C10 C11 C12 C23 -179.9(3) . . . . ? N9 Si2 N13 C71 47.4(3) . . . . ? N11 Si2 N13 C71 169.8(3) . . . . ? N15 Si2 N13 C71 -72.8(3) . . . . ? N9 Si2 N13 N14 -122.2(2) . . . . ? N11 Si2 N13 N14 0.1(2) . . . . ? N15 Si2 N13 N14 117.6(2) . . . . ? N3 N4 C13 C22 0.0(4) . . . . ? N3 N4 C13 C24 177.4(3) . . . . ? N1 N2 C23 C12 0.2(4) . . . . ? N1 N2 C23 C14 178.0(3) . . . . ? C11 C12 C23 N2 0.2(4) . . . . ? C11 C12 C23 C14 -177.4(3) . . . . ? C71 N13 N14 C73 0.5(3) . . . . ? Si2 N13 N14 C73 172.2(2) . . . . ? N9 Si2 N15 C81 74.3(3) . . . . ? N11 Si2 N15 C81 -47.0(3) . . . . ? N13 Si2 N15 C81 -165.6(3) . . . . ? N9 Si2 N15 N16 -101.2(2) . . . . ? N11 Si2 N15 N16 137.4(2) . . . . ? N13 Si2 N15 N16 18.9(3) . . . . ? C81 N15 N16 C83 0.5(3) . . . . ? Si2 N15 N16 C83 176.8(2) . . . . ? N4 N3 C21 C22 0.6(3) . . . . ? Si1 N3 C21 C22 173.1(2) . . . . ? N4 N3 C21 C20 -178.6(3) . . . . ? Si1 N3 C21 C20 -6.0(5) . . . . ? N3 C21 C22 C13 -0.6(4) . . . . ? C20 C21 C22 C13 178.5(4) . . . . ? N4 C13 C22 C21 0.4(4) . . . . ? C24 C13 C22 C21 -176.8(3) . . . . ? N6 N5 C31 C32 -0.4(3) . . . . ? Si1 N5 C31 C32 -173.8(2) . . . . ? N6 N5 C31 C30 -178.8(3) . . . . ? Si1 N5 C31 C30 7.7(5) . . . . ? N5 C31 C32 C33 0.4(4) . . . . ? C30 C31 C32 C33 178.6(3) . . . . ? N5 N6 C33 C32 0.0(4) . . . . ? N5 N6 C33 C34 -179.2(3) . . . . ? C31 C32 C33 N6 -0.3(4) . . . . ? C31 C32 C33 C34 178.9(3) . . . . ? N8 N7 C41 C42 0.3(3) . . . . ? Si1 N7 C41 C42 177.5(2) . . . . ? N8 N7 C41 C40 -178.9(3) . . . . ? Si1 N7 C41 C40 -1.6(4) . . . . ? N7 C41 C42 C43 -0.1(3) . . . . ? C40 C41 C42 C43 178.9(3) . . . . ? N7 N8 C43 C42 0.3(3) . . . . ? N7 N8 C43 C44 -179.1(3) . . . . ? C41 C42 C43 N8 -0.1(4) . . . . ? C41 C42 C43 C44 179.3(3) . . . . ? N10 N9 C51 C52 0.7(4) . . . . ? Si2 N9 C51 C52 -180.0(3) . . . . ? N10 N9 C51 C50 -178.7(3) . . . . ? Si2 N9 C51 C50 0.6(6) . . . . ? N9 C51 C52 C53 -0.3(4) . . . . ? C50 C51 C52 C53 179.1(4) . . . . ? N9 N10 C53 C52 0.6(4) . . . . ? N9 N10 C53 C54 -179.4(3) . . . . ? C51 C52 C53 N10 -0.2(5) . . . . ? C51 C52 C53 C54 179.8(4) . . . . ? N12 N11 C61 C62 -0.1(4) . . . . ? Si2 N11 C61 C62 175.3(3) . . . . ? N12 N11 C61 C60 179.5(3) . . . . ? Si2 N11 C61 C60 -5.0(5) . . . . ? N11 C61 C62 C63 0.1(4) . . . . ? C60 C61 C62 C63 -179.5(4) . . . . ? N11 N12 C63 C62 0.0(4) . . . . ? N11 N12 C63 C64 179.1(3) . . . . ? C61 C62 C63 N12 -0.1(4) . . . . ? C61 C62 C63 C64 -179.0(4) . . . . ? N14 N13 C71 C72 -0.8(4) . . . . ? Si2 N13 C71 C72 -171.0(2) . . . . ? N14 N13 C71 C70 177.5(3) . . . . ? Si2 N13 C71 C70 7.3(5) . . . . ? N13 C71 C72 C73 0.7(4) . . . . ? C70 C71 C72 C73 -177.4(3) . . . . ? N13 N14 C73 C72 -0.1(4) . . . . ? N13 N14 C73 C74 -178.5(3) . . . . ? C71 C72 C73 N14 -0.4(4) . . . . ? C71 C72 C73 C74 177.8(4) . . . . ? N16 N15 C81 C82 -0.9(4) . . . . ? Si2 N15 C81 C82 -176.8(2) . . . . ? N16 N15 C81 C80 177.1(3) . . . . ? Si2 N15 C81 C80 1.2(5) . . . . ? N15 C81 C82 C83 1.0(4) . . . . ? C80 C81 C82 C83 -176.8(3) . . . . ? N15 N16 C83 C82 0.2(4) . . . . ? N15 N16 C83 C84 179.8(3) . . . . ? C81 C82 C83 N16 -0.8(4) . . . . ? C81 C82 C83 C84 179.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.266 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.063 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_LiTpsd _database_code_depnum_ccdc_archive 'CCDC 725896' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H29 Li N6 O Si' _chemical_formula_sum 'C19 H29 Li N6 O Si' _chemical_formula_weight 392.51 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' Li Li -0.0003 0.0001 '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' N N 0.0061 0.0033 '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 '-P 2yn' 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 7.908(2) _cell_length_b 14.520(3) _cell_length_c 18.629(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.99(3) _cell_angle_gamma 90.00 _cell_volume 2127.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14395 _cell_measurement_theta_min 3.82 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.131 _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 150(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 'Stoe Stadi 4 with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14395 _diffrn_reflns_av_R_equivalents 0.1423 _diffrn_reflns_av_sigmaI/netI 0.1231 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3704 _reflns_number_gt 2767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0518P)^2^+1.6948P] 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 3704 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1748 _refine_ls_R_factor_gt 0.1338 _refine_ls_wR_factor_ref 0.2197 _refine_ls_wR_factor_gt 0.2015 _refine_ls_goodness_of_fit_ref 1.306 _refine_ls_restrained_S_all 1.306 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.0299(2) 0.78986(10) 0.03793(8) 0.0323(4) Uani 1 1 d . . . N5 N -0.0580(5) 0.8177(3) 0.1232(2) 0.0295(11) Uani 1 1 d . . . O1 O 0.0371(5) 0.5350(2) 0.23854(19) 0.0348(10) Uani 1 1 d . . . N6 N -0.0710(5) 0.7580(3) 0.1803(2) 0.0291(11) Uani 1 1 d . . . N2 N 0.2497(6) 0.6742(3) 0.1319(2) 0.0313(11) Uani 1 1 d . . . N3 N -0.0919(5) 0.6838(3) 0.0181(2) 0.0284(11) Uani 1 1 d . . . N1 N 0.2305(5) 0.7373(3) 0.0764(2) 0.0280(10) Uani 1 1 d . . . N4 N -0.0995(5) 0.6084(3) 0.0642(2) 0.0295(11) Uani 1 1 d . . . C23 C -0.1993(6) 0.5478(3) 0.0275(3) 0.0303(13) Uani 1 1 d . . . C21 C -0.1885(7) 0.6665(4) -0.0452(3) 0.0335(14) Uani 1 1 d . . . C33 C -0.1473(7) 0.8051(3) 0.2290(3) 0.0304(13) Uani 1 1 d . . . C11 C 0.3853(7) 0.7574(4) 0.0549(3) 0.0311(13) Uani 1 1 d . . . C100 C 0.0820(7) 0.4431(4) 0.2182(3) 0.0390(15) Uani 1 1 d . . . H10A H 0.1496 0.4451 0.1764 0.047 Uiso 1 1 calc R . . H10B H -0.0216 0.4061 0.2049 0.047 Uiso 1 1 calc R . . C31 C -0.1271(7) 0.9008(3) 0.1386(3) 0.0307(13) Uani 1 1 d . . . C13 C 0.4149(7) 0.6578(3) 0.1437(3) 0.0330(14) Uani 1 1 d . . . C32 C -0.1823(7) 0.8948(4) 0.2049(3) 0.0344(14) Uani 1 1 d . . . H32A H -0.2345 0.9422 0.2300 0.041 Uiso 1 1 calc R . . C30 C -0.1362(8) 0.9802(4) 0.0873(3) 0.0482(17) Uani 1 1 d . . . H30A H -0.1803 1.0344 0.1105 0.072 Uiso 1 1 calc R . . H30B H -0.2120 0.9646 0.0439 0.072 Uiso 1 1 calc R . . H30C H -0.0223 0.9936 0.0737 0.072 Uiso 1 1 calc R . . C12 C 0.5031(7) 0.7085(4) 0.0971(3) 0.0354(14) Uani 1 1 d . . . H12A H 0.6226 0.7090 0.0951 0.042 Uiso 1 1 calc R . . C24 C -0.2380(7) 0.4568(4) 0.0594(3) 0.0425(15) Uani 1 1 d . . . H24A H -0.2572 0.4651 0.1101 0.064 Uiso 1 1 calc R . . H24B H -0.1419 0.4149 0.0562 0.064 Uiso 1 1 calc R . . H24C H -0.3402 0.4307 0.0327 0.064 Uiso 1 1 calc R . . C22 C -0.2584(7) 0.5821(4) -0.0409(3) 0.0373(14) Uani 1 1 d . . . H22A H -0.3327 0.5520 -0.0768 0.045 Uiso 1 1 calc R . . C14 C 0.4844(7) 0.5926(4) 0.2010(3) 0.0464(16) Uani 1 1 d . . . H14A H 0.4499 0.6124 0.2477 0.070 Uiso 1 1 calc R . . H14B H 0.6088 0.5919 0.2034 0.070 Uiso 1 1 calc R . . H14C H 0.4403 0.5306 0.1898 0.070 Uiso 1 1 calc R . . C20 C -0.2043(7) 0.7332(4) -0.1063(3) 0.0452(16) Uani 1 1 d . . . H20A H -0.2462 0.7923 -0.0898 0.068 Uiso 1 1 calc R . . H20B H -0.2844 0.7091 -0.1456 0.068 Uiso 1 1 calc R . . H20C H -0.0928 0.7422 -0.1238 0.068 Uiso 1 1 calc R . . C34 C -0.1850(8) 0.7606(4) 0.2977(3) 0.0451(16) Uani 1 1 d . . . H34A H -0.1484 0.6961 0.2980 0.068 Uiso 1 1 calc R . . H34B H -0.3075 0.7635 0.3016 0.068 Uiso 1 1 calc R . . H34C H -0.1238 0.7930 0.3386 0.068 Uiso 1 1 calc R . . C10 C 0.4111(7) 0.8225(4) -0.0048(3) 0.0425(15) Uani 1 1 d . . . H10C H 0.3665 0.8833 0.0062 0.064 Uiso 1 1 calc R . . H10D H 0.3509 0.7996 -0.0500 0.064 Uiso 1 1 calc R . . H10E H 0.5328 0.8275 -0.0101 0.064 Uiso 1 1 calc R . . C103 C 0.0959(9) 0.5486(4) 0.3130(3) 0.0545(19) Uani 1 1 d . . . H10F H 0.0048 0.5761 0.3387 0.065 Uiso 1 1 calc R . . H10G H 0.1950 0.5907 0.3177 0.065 Uiso 1 1 calc R . . C101 C 0.1842(8) 0.4019(4) 0.2822(3) 0.0521(18) Uani 1 1 d . . . H10H H 0.1517 0.3368 0.2886 0.063 Uiso 1 1 calc R . . H10I H 0.3072 0.4047 0.2765 0.063 Uiso 1 1 calc R . . Li1 Li 0.0256(11) 0.6314(6) 0.1632(5) 0.032(2) Uani 1 1 d . . . C102 C 0.1447(10) 0.4575(5) 0.3439(4) 0.072(2) Uani 1 1 d . . . H10J H 0.2452 0.4627 0.3800 0.086 Uiso 1 1 calc R . . H10K H 0.0499 0.4299 0.3672 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0316(9) 0.0327(9) 0.0328(9) 0.0029(7) 0.0043(7) 0.0040(7) N5 0.029(3) 0.029(2) 0.030(3) 0.003(2) 0.003(2) 0.001(2) O1 0.044(2) 0.031(2) 0.028(2) 0.0024(16) -0.0001(18) 0.0033(18) N6 0.031(3) 0.029(2) 0.027(3) -0.003(2) -0.001(2) 0.002(2) N2 0.033(3) 0.024(2) 0.035(3) 0.006(2) -0.002(2) 0.005(2) N3 0.027(3) 0.031(2) 0.026(3) -0.001(2) 0.002(2) 0.001(2) N1 0.027(3) 0.029(2) 0.028(3) 0.000(2) 0.003(2) 0.004(2) N4 0.031(3) 0.029(2) 0.029(3) 0.004(2) 0.007(2) 0.004(2) C23 0.022(3) 0.034(3) 0.035(4) -0.007(3) 0.004(3) 0.000(3) C21 0.035(3) 0.042(4) 0.024(3) -0.004(3) 0.003(3) 0.007(3) C33 0.028(3) 0.031(3) 0.031(3) -0.007(3) -0.002(3) -0.001(2) C11 0.036(3) 0.031(3) 0.028(3) -0.005(2) 0.009(3) 0.001(3) C100 0.043(4) 0.034(3) 0.040(4) 0.000(3) 0.002(3) 0.004(3) C31 0.030(3) 0.023(3) 0.039(4) 0.001(2) 0.003(3) 0.005(2) C13 0.027(3) 0.028(3) 0.043(4) -0.003(3) 0.000(3) 0.005(3) C32 0.036(3) 0.031(3) 0.037(4) -0.003(3) 0.008(3) 0.003(3) C30 0.060(4) 0.034(3) 0.054(4) 0.003(3) 0.017(3) 0.007(3) C12 0.024(3) 0.040(3) 0.043(4) -0.003(3) 0.004(3) 0.002(3) C24 0.034(4) 0.049(4) 0.043(4) -0.005(3) -0.002(3) -0.011(3) C22 0.034(3) 0.053(4) 0.024(3) -0.012(3) -0.004(3) 0.004(3) C14 0.037(4) 0.047(4) 0.055(4) 0.006(3) 0.002(3) 0.006(3) C20 0.043(4) 0.062(4) 0.029(3) 0.001(3) -0.005(3) 0.008(3) C34 0.052(4) 0.047(4) 0.038(4) 0.003(3) 0.012(3) 0.010(3) C10 0.041(4) 0.052(4) 0.037(4) -0.003(3) 0.018(3) 0.000(3) C103 0.091(6) 0.042(4) 0.028(4) -0.002(3) -0.005(3) 0.006(4) C101 0.061(5) 0.045(4) 0.047(4) 0.003(3) -0.012(3) 0.005(3) Li1 0.028(5) 0.031(5) 0.035(6) -0.001(4) -0.003(4) 0.004(4) C102 0.093(6) 0.076(5) 0.043(5) 0.008(4) -0.004(4) 0.034(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N3 1.833(4) . ? Si1 N1 1.837(4) . ? Si1 N5 1.845(4) . ? N5 C31 1.368(6) . ? N5 N6 1.383(5) . ? O1 C103 1.430(6) . ? O1 C100 1.441(6) . ? O1 Li1 1.977(9) . ? N6 C33 1.330(6) . ? N6 Li1 2.030(9) . ? N2 C13 1.324(6) . ? N2 N1 1.379(5) . ? N2 Li1 2.020(10) . ? N3 C21 1.361(6) . ? N3 N4 1.396(5) . ? N1 C11 1.359(6) . ? N4 C23 1.323(6) . ? N4 Li1 2.028(10) . ? C23 C22 1.401(7) . ? C23 C24 1.494(7) . ? C21 C22 1.350(7) . ? C21 C20 1.490(7) . ? C33 C32 1.396(7) . ? C33 C34 1.491(7) . ? C11 C12 1.356(7) . ? C11 C10 1.491(7) . ? C100 C101 1.494(7) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C31 C32 1.355(7) . ? C31 C30 1.494(7) . ? C13 C12 1.381(7) . ? C13 C14 1.489(7) . ? C32 H32A 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C12 H12A 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C22 H22A 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C10 H10E 0.9800 . ? C103 C102 1.478(8) . ? C103 H10F 0.9900 . ? C103 H10G 0.9900 . ? C101 C102 1.464(9) . ? C101 H10H 0.9900 . ? C101 H10I 0.9900 . ? C102 H10J 0.9900 . ? C102 H10K 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 N3 Si1 N1 98.25(19) . . ? N3 Si1 N5 96.92(19) . . ? N1 Si1 N5 98.2(2) . . ? C31 N5 N6 109.2(4) . . ? C31 N5 Si1 124.6(4) . . ? N6 N5 Si1 126.1(3) . . ? C103 O1 C100 108.6(4) . . ? C103 O1 Li1 125.2(4) . . ? C100 O1 Li1 117.6(4) . . ? C33 N6 N5 106.2(4) . . ? C33 N6 Li1 141.0(5) . . ? N5 N6 Li1 112.8(4) . . ? C13 N2 N1 105.9(4) . . ? C13 N2 Li1 141.0(4) . . ? N1 N2 Li1 112.9(4) . . ? C21 N3 N4 109.4(4) . . ? C21 N3 Si1 124.4(4) . . ? N4 N3 Si1 126.2(3) . . ? C11 N1 N2 109.4(4) . . ? C11 N1 Si1 124.3(4) . . ? N2 N1 Si1 126.3(3) . . ? C23 N4 N3 105.4(4) . . ? C23 N4 Li1 141.9(4) . . ? N3 N4 Li1 112.4(4) . . ? N4 C23 C22 111.0(5) . . ? N4 C23 C24 121.3(5) . . ? C22 C23 C24 127.8(5) . . ? C22 C21 N3 108.2(5) . . ? C22 C21 C20 129.3(5) . . ? N3 C21 C20 122.5(5) . . ? N6 C33 C32 110.4(5) . . ? N6 C33 C34 120.6(5) . . ? C32 C33 C34 129.0(5) . . ? C12 C11 N1 107.6(5) . . ? C12 C11 C10 128.8(5) . . ? N1 C11 C10 123.6(5) . . ? O1 C100 C101 106.8(4) . . ? O1 C100 H10A 110.4 . . ? C101 C100 H10A 110.4 . . ? O1 C100 H10B 110.4 . . ? C101 C100 H10B 110.4 . . ? H10A C100 H10B 108.6 . . ? C32 C31 N5 107.9(4) . . ? C32 C31 C30 129.4(5) . . ? N5 C31 C30 122.7(5) . . ? N2 C13 C12 110.8(5) . . ? N2 C13 C14 121.1(5) . . ? C12 C13 C14 128.1(5) . . ? C31 C32 C33 106.4(5) . . ? C31 C32 H32A 126.8 . . ? C33 C32 H32A 126.8 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C11 C12 C13 106.4(5) . . ? C11 C12 H12A 126.8 . . ? C13 C12 H12A 126.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C22 C23 106.1(5) . . ? C21 C22 H22A 127.0 . . ? C23 C22 H22A 127.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C11 C10 H10C 109.5 . . ? C11 C10 H10D 109.5 . . ? H10C C10 H10D 109.5 . . ? C11 C10 H10E 109.5 . . ? H10C C10 H10E 109.5 . . ? H10D C10 H10E 109.5 . . ? O1 C103 C102 107.4(5) . . ? O1 C103 H10F 110.2 . . ? C102 C103 H10F 110.2 . . ? O1 C103 H10G 110.2 . . ? C102 C103 H10G 110.2 . . ? H10F C103 H10G 108.5 . . ? C102 C101 C100 105.2(5) . . ? C102 C101 H10H 110.7 . . ? C100 C101 H10H 110.7 . . ? C102 C101 H10I 110.7 . . ? C100 C101 H10I 110.7 . . ? H10H C101 H10I 108.8 . . ? O1 Li1 N2 116.5(4) . . ? O1 Li1 N4 120.7(4) . . ? N2 Li1 N4 98.5(4) . . ? O1 Li1 N6 121.3(5) . . ? N2 Li1 N6 97.0(4) . . ? N4 Li1 N6 97.8(4) . . ? C101 C102 C103 104.9(5) . . ? C101 C102 H10J 110.8 . . ? C103 C102 H10J 110.8 . . ? C101 C102 H10K 110.8 . . ? C103 C102 H10K 110.8 . . ? H10J C102 H10K 108.8 . . ? 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 N3 Si1 N5 C31 -127.9(4) . . . . ? N1 Si1 N5 C31 132.7(4) . . . . ? N3 Si1 N5 N6 49.3(4) . . . . ? N1 Si1 N5 N6 -50.1(4) . . . . ? C31 N5 N6 C33 0.1(5) . . . . ? Si1 N5 N6 C33 -177.5(4) . . . . ? C31 N5 N6 Li1 179.4(4) . . . . ? Si1 N5 N6 Li1 1.8(5) . . . . ? N1 Si1 N3 C21 -133.7(4) . . . . ? N5 Si1 N3 C21 126.9(4) . . . . ? N1 Si1 N3 N4 45.6(4) . . . . ? N5 Si1 N3 N4 -53.8(4) . . . . ? C13 N2 N1 C11 0.6(5) . . . . ? Li1 N2 N1 C11 -175.5(4) . . . . ? C13 N2 N1 Si1 -177.8(3) . . . . ? Li1 N2 N1 Si1 6.1(5) . . . . ? N3 Si1 N1 C11 128.7(4) . . . . ? N5 Si1 N1 C11 -133.1(4) . . . . ? N3 Si1 N1 N2 -53.2(4) . . . . ? N5 Si1 N1 N2 45.1(4) . . . . ? C21 N3 N4 C23 0.3(5) . . . . ? Si1 N3 N4 C23 -179.1(3) . . . . ? C21 N3 N4 Li1 -175.5(4) . . . . ? Si1 N3 N4 Li1 5.1(5) . . . . ? N3 N4 C23 C22 -0.7(6) . . . . ? Li1 N4 C23 C22 173.0(6) . . . . ? N3 N4 C23 C24 179.8(5) . . . . ? Li1 N4 C23 C24 -6.5(10) . . . . ? N4 N3 C21 C22 0.3(6) . . . . ? Si1 N3 C21 C22 179.6(4) . . . . ? N4 N3 C21 C20 -178.9(5) . . . . ? Si1 N3 C21 C20 0.4(7) . . . . ? N5 N6 C33 C32 -0.7(6) . . . . ? Li1 N6 C33 C32 -179.7(6) . . . . ? N5 N6 C33 C34 178.9(5) . . . . ? Li1 N6 C33 C34 -0.1(9) . . . . ? N2 N1 C11 C12 -0.9(6) . . . . ? Si1 N1 C11 C12 177.6(3) . . . . ? N2 N1 C11 C10 179.2(5) . . . . ? Si1 N1 C11 C10 -2.4(7) . . . . ? C103 O1 C100 C101 -4.3(6) . . . . ? Li1 O1 C100 C101 145.3(5) . . . . ? N6 N5 C31 C32 0.6(6) . . . . ? Si1 N5 C31 C32 178.2(4) . . . . ? N6 N5 C31 C30 -178.8(5) . . . . ? Si1 N5 C31 C30 -1.2(7) . . . . ? N1 N2 C13 C12 -0.1(6) . . . . ? Li1 N2 C13 C12 174.2(6) . . . . ? N1 N2 C13 C14 179.5(5) . . . . ? Li1 N2 C13 C14 -6.2(10) . . . . ? N5 C31 C32 C33 -1.0(6) . . . . ? C30 C31 C32 C33 178.4(6) . . . . ? N6 C33 C32 C31 1.1(6) . . . . ? C34 C33 C32 C31 -178.5(5) . . . . ? N1 C11 C12 C13 0.8(6) . . . . ? C10 C11 C12 C13 -179.3(5) . . . . ? N2 C13 C12 C11 -0.4(6) . . . . ? C14 C13 C12 C11 180.0(5) . . . . ? N3 C21 C22 C23 -0.7(6) . . . . ? C20 C21 C22 C23 178.5(5) . . . . ? N4 C23 C22 C21 0.9(6) . . . . ? C24 C23 C22 C21 -179.7(5) . . . . ? C100 O1 C103 C102 -12.4(7) . . . . ? Li1 O1 C103 C102 -159.1(5) . . . . ? O1 C100 C101 C102 19.4(7) . . . . ? C103 O1 Li1 N2 72.0(7) . . . . ? C100 O1 Li1 N2 -72.0(6) . . . . ? C103 O1 Li1 N4 -168.8(5) . . . . ? C100 O1 Li1 N4 47.2(7) . . . . ? C103 O1 Li1 N6 -45.6(8) . . . . ? C100 O1 Li1 N6 170.4(4) . . . . ? C13 N2 Li1 O1 2.4(9) . . . . ? N1 N2 Li1 O1 176.4(4) . . . . ? C13 N2 Li1 N4 -128.3(6) . . . . ? N1 N2 Li1 N4 45.7(5) . . . . ? C13 N2 Li1 N6 132.7(6) . . . . ? N1 N2 Li1 N6 -53.3(5) . . . . ? C23 N4 Li1 O1 7.4(10) . . . . ? N3 N4 Li1 O1 -179.2(4) . . . . ? C23 N4 Li1 N2 135.2(6) . . . . ? N3 N4 Li1 N2 -51.4(5) . . . . ? C23 N4 Li1 N6 -126.4(6) . . . . ? N3 N4 Li1 N6 47.0(5) . . . . ? C33 N6 Li1 O1 -5.1(9) . . . . ? N5 N6 Li1 O1 176.0(4) . . . . ? C33 N6 Li1 N2 -132.0(6) . . . . ? N5 N6 Li1 N2 49.0(5) . . . . ? C33 N6 Li1 N4 128.4(6) . . . . ? N5 N6 Li1 N4 -50.6(5) . . . . ? C100 C101 C102 C103 -26.5(8) . . . . ? O1 C103 C102 C101 24.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.315 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.062 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_Me3SiSipz3 _database_code_depnum_ccdc_archive 'CCDC 725897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 N6 Si2' _chemical_formula_sum 'C18 H30 N6 Si2' _chemical_formula_weight 386.66 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' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I23 _symmetry_space_group_name_Hall I223 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' _cell_length_a 16.497(2) _cell_length_b 16.497(2) _cell_length_c 16.497(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4489.7(9) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 17063 _cell_measurement_theta_min 3.91 _cell_measurement_theta_max 26.93 _exptl_crystal_description cube _exptl_crystal_colour 'colourless crystal' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.172 _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 200(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 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17063 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 26.93 _reflns_number_total 1622 _reflns_number_gt 1613 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0370P)^2^+1.9727P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.11(18) _refine_ls_number_reflns 1622 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.78662(3) 0.78662(3) 0.78662(3) 0.0306(2) Uani 1 3 d S . . Si2 Si 0.86770(3) 0.86770(3) 0.86770(3) 0.0354(2) Uani 1 3 d S A . N1 N 0.8146(3) 0.7916(3) 0.6855(4) 0.0330(10) Uani 0.50 1 d P A 1 N1' N 0.7911(3) 0.8140(4) 0.6840(4) 0.0336(10) Uani 0.50 1 d P A 2 N2 N 0.8272(2) 0.8714(2) 0.66178(19) 0.0399(7) Uani 0.50 1 d P A 1 N2' N 0.8712(2) 0.8271(2) 0.66162(18) 0.0393(7) Uani 0.50 1 d P A 2 C10 C 0.8100(5) 0.6516(4) 0.6261(5) 0.0536(18) Uani 0.50 1 d P A 1 H10A H 0.8292 0.6258 0.5762 0.080 Uiso 0.50 1 calc PR A 1 H10B H 0.7525 0.6390 0.6340 0.080 Uiso 0.50 1 calc PR A 1 H10C H 0.8412 0.6311 0.6723 0.080 Uiso 0.50 1 calc PR A 1 C10' C 0.6516(4) 0.8102(5) 0.6267(5) 0.0521(17) Uani 0.50 1 d P A 2 H10D H 0.6312 0.8422 0.6724 0.078 Uiso 0.50 1 calc PR A 2 H10E H 0.6392 0.7528 0.6356 0.078 Uiso 0.50 1 calc PR A 2 H10F H 0.6256 0.8285 0.5766 0.078 Uiso 0.50 1 calc PR A 2 C11 C 0.8206(2) 0.7410(2) 0.6198(2) 0.0401(8) Uani 0.50 1 d P A 1 C11' C 0.7409(2) 0.8209(2) 0.6199(3) 0.0399(8) Uani 0.50 1 d P A 2 C12 C 0.8371(3) 0.7877(3) 0.5548(2) 0.0481(10) Uani 0.50 1 d P A 1 H12 H 0.8447 0.7699 0.5006 0.058 Uiso 0.50 1 calc PR A 1 C12' C 0.7876(3) 0.8375(3) 0.5549(2) 0.0468(10) Uani 0.50 1 d P A 2 H12' H 0.7694 0.8456 0.5009 0.056 Uiso 0.50 1 calc PR A 2 C14 C 0.8584(3) 0.9437(3) 0.5372(3) 0.0604(12) Uani 0.50 1 d P A 1 H14A H 0.9163 0.9460 0.5243 0.091 Uiso 0.50 1 calc PR A 1 H14B H 0.8436 0.9907 0.5705 0.091 Uiso 0.50 1 calc PR A 1 H14C H 0.8268 0.9444 0.4869 0.091 Uiso 0.50 1 calc PR A 1 C14' C 0.9436(3) 0.8582(3) 0.5369(3) 0.0601(12) Uani 0.50 1 d P A 2 H14D H 0.9455 0.8255 0.4874 0.090 Uiso 0.50 1 calc PR A 2 H14E H 0.9902 0.8449 0.5712 0.090 Uiso 0.50 1 calc PR A 2 H14F H 0.9453 0.9159 0.5226 0.090 Uiso 0.50 1 calc PR A 2 C13 C 0.8406(4) 0.8673(4) 0.5831(3) 0.0418(13) Uani 0.50 1 d P A 1 C13' C 0.8672(4) 0.8406(4) 0.5817(4) 0.0427(13) Uani 0.50 1 d P A 2 C1 C 0.9695(3) 0.8737(4) 0.8206(3) 0.0604(12) Uani 0.50 1 d P A 1 H1A H 0.9651 0.8994 0.7672 0.091 Uiso 0.50 1 calc PR A 1 H1B H 0.9918 0.8190 0.8145 0.091 Uiso 0.50 1 calc PR A 1 H1C H 1.0054 0.9060 0.8551 0.091 Uiso 0.50 1 calc PR A 1 C1' C 0.9698(3) 0.8208(3) 0.8738(4) 0.0601(12) Uani 0.50 1 d P A 2 H1'1 H 0.9929 0.8166 0.8193 0.090 Uiso 0.50 1 calc PR A 2 H1'2 H 0.9652 0.7665 0.8976 0.090 Uiso 0.50 1 calc PR A 2 H1'3 H 1.0050 0.8544 0.9078 0.090 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0306(2) 0.0306(2) 0.0306(2) 0.00014(18) 0.00014(18) 0.00014(18) Si2 0.0354(2) 0.0354(2) 0.0354(2) -0.0019(2) -0.0019(2) -0.0019(2) N1 0.034(3) 0.033(3) 0.0311(17) 0.0006(19) 0.001(2) 0.0012(17) N1' 0.029(3) 0.038(3) 0.0338(17) 0.0088(19) -0.0044(19) 0.0016(17) N2 0.0456(18) 0.0350(17) 0.0390(16) 0.0008(13) 0.0044(13) -0.0018(16) N2' 0.0343(16) 0.0456(18) 0.0380(16) 0.0034(13) 0.0032(13) -0.0023(16) C10 0.070(4) 0.041(4) 0.050(4) -0.014(3) 0.010(3) -0.004(3) C10' 0.038(4) 0.068(4) 0.050(4) 0.011(3) -0.013(3) -0.006(3) C11 0.0410(18) 0.0398(19) 0.0396(19) -0.0077(15) 0.0058(16) -0.0043(15) C11' 0.0405(19) 0.0386(18) 0.0405(19) 0.0039(16) -0.0081(15) -0.0037(14) C12 0.058(2) 0.056(3) 0.0305(18) -0.0055(18) 0.0071(16) -0.010(2) C12' 0.054(3) 0.056(2) 0.0302(18) 0.0070(16) -0.0073(18) -0.009(2) C14 0.074(3) 0.057(3) 0.051(2) 0.016(2) 0.015(2) -0.002(2) C14' 0.056(3) 0.078(3) 0.046(2) 0.014(2) 0.014(2) -0.005(2) C13 0.047(3) 0.042(3) 0.036(2) 0.002(2) 0.012(2) -0.001(2) C13' 0.044(3) 0.046(3) 0.039(2) 0.006(2) 0.009(2) 0.002(2) C1 0.043(2) 0.069(3) 0.070(3) -0.013(3) 0.002(2) -0.008(2) C1' 0.037(2) 0.071(3) 0.073(3) -0.011(3) -0.010(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.732(6) 9 ? Si1 N1 1.732(6) . ? Si1 N1 1.732(6) 5 ? Si1 N1' 1.753(6) 9 ? Si1 N1' 1.753(6) . ? Si1 N1' 1.753(6) 5 ? Si1 Si2 2.3169(11) . ? Si2 C1 1.853(4) 9 ? Si2 C1 1.853(4) . ? Si2 C1 1.853(4) 5 ? Si2 C1' 1.856(4) 5 ? Si2 C1' 1.856(4) . ? Si2 C1' 1.856(4) 9 ? N1 C11 1.372(7) . ? N1 N2 1.390(7) . ? N1' C11' 1.348(7) . ? N1' N2' 1.388(7) . ? N2 C13 1.318(6) . ? N2' C13' 1.338(6) . ? C10 C11 1.489(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10' C11' 1.488(7) . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11 C12 1.347(6) . ? C11' C12' 1.349(6) . ? C12 C13 1.396(7) . ? C12 H12 0.9500 . ? C12' C13' 1.387(7) . ? C12' H12' 0.9500 . ? C14 C13 1.499(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14' C13' 1.490(7) . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1' H1'1 0.9800 . ? C1' H1'2 0.9800 . ? C1' H1'3 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 N1 Si1 N1 106.8(2) 9 . ? N1 Si1 N1 106.8(2) 9 5 ? N1 Si1 N1 106.8(2) . 5 ? N1 Si1 N1' 91.03(14) . 9 ? N1 Si1 N1' 120.22(14) 5 9 ? N1 Si1 N1' 120.22(14) 9 . ? N1 Si1 N1' 91.03(14) 5 . ? N1' Si1 N1' 106.2(2) 9 . ? N1 Si1 N1' 91.03(14) 9 5 ? N1 Si1 N1' 120.22(14) . 5 ? N1' Si1 N1' 106.2(2) 9 5 ? N1' Si1 N1' 106.2(2) . 5 ? N1 Si1 Si2 112.0(2) 9 . ? N1 Si1 Si2 112.0(2) . . ? N1 Si1 Si2 112.0(2) 5 . ? N1' Si1 Si2 112.6(2) 9 . ? N1' Si1 Si2 112.6(2) . . ? N1' Si1 Si2 112.6(2) 5 . ? C1 Si2 C1 110.73(16) 9 . ? C1 Si2 C1 110.73(16) 9 5 ? C1 Si2 C1 110.73(16) . 5 ? C1 Si2 C1' 139.1(2) 9 5 ? C1 Si2 C1' 74.2(2) . 5 ? C1 Si2 C1' 74.2(2) 9 . ? C1 Si2 C1' 139.1(2) 5 . ? C1' Si2 C1' 110.59(16) 5 . ? C1 Si2 C1' 139.1(2) . 9 ? C1 Si2 C1' 74.2(2) 5 9 ? C1' Si2 C1' 110.59(16) 5 9 ? C1' Si2 C1' 110.59(16) . 9 ? C1 Si2 Si1 108.18(16) 9 . ? C1 Si2 Si1 108.18(16) . . ? C1 Si2 Si1 108.18(16) 5 . ? C1' Si2 Si1 108.33(17) 5 . ? C1' Si2 Si1 108.33(17) . . ? C1' Si2 Si1 108.33(17) 9 . ? C11 N1 N2 110.0(5) . . ? C11 N1 Si1 138.7(5) . . ? N2 N1 Si1 110.9(4) . . ? C11' N1' N2' 111.3(5) . . ? C11' N1' Si1 138.8(5) . . ? N2' N1' Si1 109.7(4) . . ? C13 N2 N1 104.7(4) . . ? C13' N2' N1' 104.0(4) . . ? C11' C10' H10D 109.5 . . ? C11' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C11' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C12 C11 N1 107.2(4) . . ? C12 C11 C10 130.2(5) . . ? N1 C11 C10 122.6(5) . . ? N1' C11' C12' 106.8(4) . . ? N1' C11' C10' 122.7(5) . . ? C12' C11' C10' 130.5(5) . . ? C11 C12 C13 106.3(4) . . ? C11 C12 H12 126.8 . . ? C13 C12 H12 126.8 . . ? C11' C12' C13' 107.1(4) . . ? C11' C12' H12' 126.4 . . ? C13' C12' H12' 126.4 . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? N2 C13 C12 111.7(5) . . ? N2 C13 C14 119.1(5) . . ? C12 C13 C14 129.1(5) . . ? N2' C13' C12' 110.8(5) . . ? N2' C13' C14' 118.7(5) . . ? C12' C13' C14' 130.5(5) . . ? Si2 C1 H1A 109.5 . . ? Si2 C1 H1B 109.5 . . ? Si2 C1 H1C 109.5 . . ? Si2 C1' H1'1 109.5 . . ? Si2 C1' H1'2 109.5 . . ? H1'1 C1' H1'2 109.5 . . ? Si2 C1' H1'3 109.5 . . ? H1'1 C1' H1'3 109.5 . . ? H1'2 C1' H1'3 109.5 . . ? 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 N1 Si1 Si2 C1 -29.8(2) 9 . . 9 ? N1 Si1 Si2 C1 -149.8(2) . . . 9 ? N1 Si1 Si2 C1 90.2(2) 5 . . 9 ? N1' Si1 Si2 C1 -48.9(2) 9 . . 9 ? N1' Si1 Si2 C1 -168.9(2) . . . 9 ? N1' Si1 Si2 C1 71.1(2) 5 . . 9 ? N1 Si1 Si2 C1 90.2(2) 9 . . . ? N1 Si1 Si2 C1 -29.8(2) . . . . ? N1 Si1 Si2 C1 -149.8(2) 5 . . . ? N1' Si1 Si2 C1 71.1(2) 9 . . . ? N1' Si1 Si2 C1 -48.9(2) . . . . ? N1' Si1 Si2 C1 -168.9(2) 5 . . . ? N1 Si1 Si2 C1 -149.8(2) 9 . . 5 ? N1 Si1 Si2 C1 90.2(2) . . . 5 ? N1 Si1 Si2 C1 -29.8(2) 5 . . 5 ? N1' Si1 Si2 C1 -168.9(2) 9 . . 5 ? N1' Si1 Si2 C1 71.1(2) . . . 5 ? N1' Si1 Si2 C1 -48.9(2) 5 . . 5 ? N1 Si1 Si2 C1' 169.1(2) 9 . . 5 ? N1 Si1 Si2 C1' 49.1(2) . . . 5 ? N1 Si1 Si2 C1' -70.9(2) 5 . . 5 ? N1' Si1 Si2 C1' 150.0(2) 9 . . 5 ? N1' Si1 Si2 C1' 30.0(2) . . . 5 ? N1' Si1 Si2 C1' -90.0(2) 5 . . 5 ? N1 Si1 Si2 C1' 49.1(2) 9 . . . ? N1 Si1 Si2 C1' -70.9(2) . . . . ? N1 Si1 Si2 C1' 169.1(2) 5 . . . ? N1' Si1 Si2 C1' 30.0(2) 9 . . . ? N1' Si1 Si2 C1' -90.0(2) . . . . ? N1' Si1 Si2 C1' 150.0(2) 5 . . . ? N1 Si1 Si2 C1' -70.9(2) 9 . . 9 ? N1 Si1 Si2 C1' 169.1(2) . . . 9 ? N1 Si1 Si2 C1' 49.1(2) 5 . . 9 ? N1' Si1 Si2 C1' -90.0(2) 9 . . 9 ? N1' Si1 Si2 C1' 150.0(2) . . . 9 ? N1' Si1 Si2 C1' 30.0(2) 5 . . 9 ? N1 Si1 N1 C11 19.3(7) 9 . . . ? N1 Si1 N1 C11 -94.7(4) 5 . . . ? N1' Si1 N1 C11 27.4(5) 9 . . . ? N1' Si1 N1 C11 -122.3(18) . . . . ? N1' Si1 N1 C11 -82.1(6) 5 . . . ? Si2 Si1 N1 C11 142.3(5) . . . . ? N1 Si1 N1 N2 -168.7(3) 9 . . . ? N1 Si1 N1 N2 77.2(6) 5 . . . ? N1' Si1 N1 N2 -160.7(5) 9 . . . ? N1' Si1 N1 N2 49.7(12) . . . . ? N1' Si1 N1 N2 89.9(4) 5 . . . ? Si2 Si1 N1 N2 -45.8(4) . . . . ? N1 Si1 N1' C11' 84.0(7) 9 . . . ? N1 Si1 N1' C11' 127.5(19) . . . . ? N1 Si1 N1' C11' -26.2(5) 5 . . . ? N1' Si1 N1' C11' 95.8(4) 9 . . . ? N1' Si1 N1' C11' -17.0(8) 5 . . . ? Si2 Si1 N1' C11' -140.6(6) . . . . ? N1 Si1 N1' N2' -90.4(3) 9 . . . ? N1 Si1 N1' N2' -46.9(11) . . . . ? N1 Si1 N1' N2' 159.4(5) 5 . . . ? N1' Si1 N1' N2' -78.7(6) 9 . . . ? N1' Si1 N1' N2' 168.6(3) 5 . . . ? Si2 Si1 N1' N2' 45.0(4) . . . . ? C11 N1 N2 C13 -0.1(6) . . . . ? Si1 N1 N2 C13 -174.5(4) . . . . ? C11' N1' N2' C13' -1.1(6) . . . . ? Si1 N1' N2' C13' 174.9(4) . . . . ? N2 N1 C11 C12 0.1(5) . . . . ? Si1 N1 C11 C12 172.1(5) . . . . ? N2 N1 C11 C10 -180.0(5) . . . . ? Si1 N1 C11 C10 -8.0(9) . . . . ? N2' N1' C11' C12' 0.8(6) . . . . ? Si1 N1' C11' C12' -173.6(5) . . . . ? N2' N1' C11' C10' -179.8(5) . . . . ? Si1 N1' C11' C10' 5.9(9) . . . . ? N1 C11 C12 C13 -0.1(6) . . . . ? C10 C11 C12 C13 -180.0(6) . . . . ? N1' C11' C12' C13' -0.2(6) . . . . ? C10' C11' C12' C13' -179.5(6) . . . . ? N1 N2 C13 C12 0.1(6) . . . . ? N1 N2 C13 C14 -178.9(5) . . . . ? C11 C12 C13 N2 0.0(7) . . . . ? C11 C12 C13 C14 178.8(5) . . . . ? N1' N2' C13' C12' 1.0(6) . . . . ? N1' N2' C13' C14' 179.3(5) . . . . ? C11' C12' C13' N2' -0.6(6) . . . . ? C11' C12' C13' C14' -178.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.93 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.188 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.033 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_Ph3SnSipz3 _database_code_depnum_ccdc_archive 'CCDC 725898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H36 N6 Si Sn' _chemical_formula_sum 'C33 H36 N6 Si Sn' _chemical_formula_weight 663.48 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.455(2) _cell_length_b 17.266(4) _cell_length_c 17.588(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3174.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 17360 _cell_measurement_theta_min 4.04 _cell_measurement_theta_max 26.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.874 _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 200(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 'Stoe Stadi 4 with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17360 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6134 _reflns_number_gt 5220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0409P)^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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(2) _refine_ls_number_reflns 6134 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.016 _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 Sn1 Sn 0.27535(3) 0.124247(17) 0.228483(16) 0.02832(9) Uani 1 1 d . . . Si1 Si 0.50298(12) 0.07801(7) 0.24252(7) 0.0296(3) Uani 1 1 d . . . C32 C 0.7757(4) 0.2322(2) 0.2297(3) 0.0377(10) Uani 1 1 d . . . H32A H 0.8543 0.2566 0.2170 0.045 Uiso 1 1 calc R . . C200 C 0.2454(4) 0.2085(2) 0.1419(3) 0.0308(11) Uani 1 1 d . . . C10 C 0.6542(5) -0.1010(3) 0.2211(3) 0.0442(12) Uani 1 1 d . . . H10A H 0.6914 -0.1490 0.2011 0.066 Uiso 1 1 calc R . . H10B H 0.5884 -0.1136 0.2588 0.066 Uiso 1 1 calc R . . H10C H 0.7214 -0.0699 0.2451 0.066 Uiso 1 1 calc R . . N4 N 0.4234(4) -0.0236(2) 0.3375(2) 0.0427(11) Uani 1 1 d . . . N3 N 0.5213(4) 0.0300(2) 0.3282(2) 0.0346(9) Uani 1 1 d . . . C12 C 0.5828(5) -0.0723(3) 0.0832(3) 0.0390(12) Uani 1 1 d . . . H12A H 0.6163 -0.1162 0.0575 0.047 Uiso 1 1 calc R . . N1 N 0.5332(4) 0.0127(2) 0.1697(2) 0.0327(9) Uani 1 1 d . . . N2 N 0.4804(4) 0.0403(2) 0.1027(2) 0.0360(10) Uani 1 1 d . . . C33 C 0.6793(4) 0.2631(2) 0.2763(3) 0.0380(11) Uani 1 1 d . . . N6 N 0.5831(3) 0.2141(2) 0.2816(2) 0.0366(10) Uani 1 1 d . . . C31 C 0.7363(4) 0.1614(3) 0.2064(2) 0.0339(11) Uani 1 1 d . . . C103 C -0.0137(5) -0.0906(3) 0.1632(4) 0.0525(15) Uani 1 1 d . . . H10D H -0.0706 -0.1315 0.1507 0.063 Uiso 1 1 calc R . . N5 N 0.6172(3) 0.1502(2) 0.2380(2) 0.0341(9) Uani 1 1 d . . . C204 C 0.0982(6) 0.2992(3) 0.0843(3) 0.0517(15) Uani 1 1 d . . . H20A H 0.0177 0.3247 0.0855 0.062 Uiso 1 1 calc R . . C22 C 0.5662(7) -0.0353(3) 0.4310(3) 0.0590(17) Uani 1 1 d . . . H22A H 0.6058 -0.0535 0.4762 0.071 Uiso 1 1 calc R . . C100 C 0.1525(4) 0.0302(2) 0.2002(3) 0.0312(11) Uani 1 1 d . . . C202 C 0.2952(6) 0.2741(3) 0.0250(3) 0.0578(16) Uani 1 1 d . . . H20B H 0.3533 0.2829 -0.0155 0.069 Uiso 1 1 calc R . . C203 C 0.1805(6) 0.3130(3) 0.0265(3) 0.0532(15) Uani 1 1 d . . . H20C H 0.1594 0.3489 -0.0124 0.064 Uiso 1 1 calc R . . C101 C 0.1287(5) 0.0093(3) 0.1252(3) 0.0398(12) Uani 1 1 d . . . H10E H 0.1703 0.0369 0.0855 0.048 Uiso 1 1 calc R . . C205 C 0.1305(6) 0.2484(3) 0.1413(4) 0.0501(15) Uani 1 1 d . . . H20D H 0.0719 0.2404 0.1818 0.060 Uiso 1 1 calc R . . C13 C 0.5107(5) -0.0123(3) 0.0507(3) 0.0390(12) Uani 1 1 d . . . C14 C 0.4609(7) -0.0026(3) -0.0285(3) 0.0573(17) Uani 1 1 d . . . H14A H 0.4047 0.0427 -0.0306 0.086 Uiso 1 1 calc R . . H14B H 0.4127 -0.0489 -0.0432 0.086 Uiso 1 1 calc R . . H14C H 0.5328 0.0047 -0.0636 0.086 Uiso 1 1 calc R . . C20 C 0.7231(7) 0.0735(4) 0.3916(4) 0.0717(18) Uani 1 1 d . . . H20E H 0.6977 0.1277 0.3853 0.108 Uiso 1 1 calc R . . H20F H 0.7843 0.0593 0.3517 0.108 Uiso 1 1 calc R . . H20G H 0.7632 0.0666 0.4415 0.108 Uiso 1 1 calc R . . C105 C 0.0923(5) -0.0123(3) 0.2563(3) 0.0394(12) Uani 1 1 d . . . H10F H 0.1084 -0.0007 0.3082 0.047 Uiso 1 1 calc R . . C102 C 0.0472(6) -0.0497(3) 0.1067(4) 0.0516(15) Uani 1 1 d . . . H10G H 0.0326 -0.0624 0.0549 0.062 Uiso 1 1 calc R . . C34 C 0.6770(5) 0.3389(3) 0.3169(3) 0.0508(14) Uani 1 1 d . . . H34A H 0.6070 0.3390 0.3539 0.076 Uiso 1 1 calc R . . H34B H 0.6640 0.3807 0.2800 0.076 Uiso 1 1 calc R . . H34C H 0.7585 0.3466 0.3433 0.076 Uiso 1 1 calc R . . C201 C 0.3265(6) 0.2226(3) 0.0817(3) 0.0471(14) Uani 1 1 d . . . H20H H 0.4061 0.1962 0.0793 0.056 Uiso 1 1 calc R . . C23 C 0.4543(6) -0.0635(3) 0.3986(3) 0.0508(15) Uani 1 1 d . . . C24 C 0.3710(7) -0.1287(4) 0.4247(3) 0.0754(19) Uani 1 1 d . . . H24A H 0.2999 -0.1354 0.3890 0.113 Uiso 1 1 calc R . . H24B H 0.3372 -0.1169 0.4753 0.113 Uiso 1 1 calc R . . H24C H 0.4214 -0.1765 0.4268 0.113 Uiso 1 1 calc R . . C104 C 0.0088(5) -0.0717(3) 0.2377(3) 0.0488(13) Uani 1 1 d . . . H10H H -0.0333 -0.0996 0.2770 0.059 Uiso 1 1 calc R . . C11 C 0.5953(4) -0.0559(3) 0.1572(3) 0.0331(11) Uani 1 1 d . . . C21 C 0.6082(6) 0.0229(3) 0.3860(3) 0.0475(14) Uani 1 1 d . . . C300 C 0.2010(5) 0.1692(3) 0.3330(3) 0.0340(11) Uani 1 1 d . . . C30 C 0.8018(5) 0.1008(3) 0.1591(3) 0.0425(14) Uani 1 1 d . . . H30A H 0.8802 0.1225 0.1372 0.064 Uiso 1 1 calc R . . H30B H 0.7446 0.0841 0.1182 0.064 Uiso 1 1 calc R . . H30C H 0.8235 0.0563 0.1912 0.064 Uiso 1 1 calc R . . C305 C 0.2777(7) 0.1913(3) 0.3927(3) 0.0584(15) Uani 1 1 d . . . H30D H 0.3680 0.1866 0.3885 0.070 Uiso 1 1 calc R . . C301 C 0.0710(5) 0.1784(3) 0.3421(3) 0.0411(12) Uani 1 1 d . . . H30E H 0.0154 0.1634 0.3019 0.049 Uiso 1 1 calc R . . C302 C 0.0194(6) 0.2086(3) 0.4075(3) 0.0483(14) Uani 1 1 d . . . H30F H -0.0705 0.2151 0.4117 0.058 Uiso 1 1 calc R . . C303 C 0.0969(7) 0.2295(4) 0.4665(4) 0.0609(18) Uani 1 1 d . . . H30G H 0.0615 0.2499 0.5121 0.073 Uiso 1 1 calc R . . C304 C 0.2245(8) 0.2206(4) 0.4592(3) 0.077(2) Uani 1 1 d . . . H30H H 0.2790 0.2345 0.5002 0.093 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 Sn1 0.02450(15) 0.02930(14) 0.03115(15) -0.00002(14) 0.00001(13) 0.00139(13) Si1 0.0243(6) 0.0305(6) 0.0339(7) -0.0008(5) -0.0008(6) 0.0016(5) C32 0.021(2) 0.033(2) 0.058(3) 0.008(2) 0.004(3) -0.0018(19) C200 0.027(3) 0.029(2) 0.036(2) 0.0015(18) 0.001(2) -0.0030(19) C10 0.044(3) 0.035(3) 0.054(3) 0.003(2) 0.000(3) 0.010(2) N4 0.048(3) 0.035(2) 0.045(3) 0.004(2) 0.001(2) -0.007(2) N3 0.035(2) 0.033(2) 0.035(2) -0.0005(17) -0.0081(19) 0.0010(18) C12 0.038(3) 0.031(3) 0.048(3) -0.002(2) 0.015(2) 0.002(2) N1 0.028(2) 0.035(2) 0.036(2) 0.0028(17) 0.0000(17) 0.0046(17) N2 0.044(3) 0.034(2) 0.030(2) 0.0032(17) -0.002(2) 0.0022(19) C33 0.026(2) 0.034(2) 0.054(3) -0.001(2) -0.003(3) 0.0017(19) N6 0.026(2) 0.0294(19) 0.054(3) -0.006(2) 0.007(2) -0.0033(15) C31 0.022(2) 0.042(2) 0.038(3) 0.0097(19) 0.003(2) 0.004(2) C103 0.034(3) 0.035(3) 0.089(5) -0.018(3) -0.010(3) 0.001(2) N5 0.027(2) 0.0319(19) 0.043(2) -0.0030(17) 0.0023(18) 0.0029(14) C204 0.046(4) 0.050(3) 0.059(4) 0.017(3) -0.005(3) 0.015(3) C22 0.091(5) 0.052(4) 0.033(3) 0.009(3) -0.017(3) 0.017(3) C100 0.026(2) 0.026(2) 0.041(3) -0.0005(19) -0.005(2) 0.0027(19) C202 0.065(4) 0.050(3) 0.058(4) 0.025(3) 0.021(3) 0.003(3) C203 0.071(4) 0.037(3) 0.052(4) 0.012(3) -0.002(3) 0.006(3) C101 0.038(3) 0.039(3) 0.042(3) 0.002(2) -0.001(2) -0.002(2) C205 0.039(3) 0.054(3) 0.057(4) 0.017(3) 0.009(3) 0.012(3) C13 0.048(3) 0.035(3) 0.034(3) -0.001(2) 0.006(3) -0.003(2) C14 0.082(5) 0.053(4) 0.037(3) -0.002(3) -0.004(3) 0.011(3) C20 0.059(4) 0.087(4) 0.069(4) -0.001(4) -0.032(4) -0.003(4) C105 0.039(3) 0.035(2) 0.044(3) 0.001(2) 0.006(2) -0.002(2) C102 0.049(4) 0.047(3) 0.059(4) -0.011(3) -0.018(3) 0.001(3) C34 0.049(3) 0.031(3) 0.072(4) -0.011(3) 0.001(3) -0.002(2) C201 0.045(3) 0.041(3) 0.055(4) 0.010(3) 0.013(3) 0.012(3) C23 0.072(4) 0.044(3) 0.037(3) 0.005(3) 0.007(3) 0.007(3) C24 0.110(6) 0.055(4) 0.061(4) 0.016(4) 0.016(4) -0.008(4) C104 0.035(3) 0.040(3) 0.072(4) 0.005(3) 0.008(3) -0.008(2) C11 0.024(2) 0.028(3) 0.047(3) -0.003(2) 0.004(2) 0.0004(19) C21 0.048(4) 0.050(3) 0.045(3) -0.004(3) -0.018(3) 0.015(3) C300 0.031(3) 0.036(3) 0.035(3) -0.002(2) 0.003(2) 0.004(2) C30 0.043(3) 0.042(3) 0.042(3) -0.011(2) 0.004(2) 0.008(2) C305 0.044(3) 0.088(4) 0.043(3) -0.018(3) 0.001(3) -0.013(4) C301 0.044(3) 0.044(3) 0.036(3) 0.002(2) 0.002(2) 0.008(2) C302 0.041(3) 0.047(3) 0.056(3) 0.004(3) 0.012(3) 0.013(3) C303 0.070(5) 0.059(4) 0.054(4) -0.019(3) 0.022(3) -0.018(3) C304 0.067(5) 0.113(5) 0.051(4) -0.035(4) 0.000(4) -0.030(5) _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 Sn1 C200 2.129(4) . ? Sn1 C100 2.130(4) . ? Sn1 C300 2.142(5) . ? Sn1 Si1 2.5224(13) . ? Si1 N5 1.728(4) . ? Si1 N3 1.730(4) . ? Si1 N1 1.735(4) . ? C32 C31 1.355(6) . ? C32 C33 1.403(6) . ? C32 H32A 0.9500 . ? C200 C201 1.377(7) . ? C200 C205 1.385(7) . ? C10 C11 1.499(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N4 C23 1.316(6) . ? N4 N3 1.390(6) . ? N3 C21 1.369(6) . ? C12 C11 1.339(7) . ? C12 C13 1.403(7) . ? C12 H12A 0.9500 . ? N1 C11 1.369(6) . ? N1 N2 1.386(5) . ? N2 C13 1.327(6) . ? C33 N6 1.318(5) . ? C33 C34 1.491(6) . ? N6 N5 1.390(5) . ? C31 N5 1.377(6) . ? C31 C30 1.501(6) . ? C103 C104 1.371(8) . ? C103 C102 1.375(8) . ? C103 H10D 0.9500 . ? C204 C203 1.353(8) . ? C204 C205 1.374(7) . ? C204 H20A 0.9500 . ? C22 C21 1.353(8) . ? C22 C23 1.390(9) . ? C22 H22A 0.9500 . ? C100 C105 1.381(6) . ? C100 C101 1.391(7) . ? C202 C203 1.374(8) . ? C202 C201 1.375(7) . ? C202 H20B 0.9500 . ? C203 H20C 0.9500 . ? C101 C102 1.367(7) . ? C101 H10E 0.9500 . ? C205 H20D 0.9500 . ? C13 C14 1.496(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C20 C21 1.489(9) . ? C20 H20E 0.9800 . ? C20 H20F 0.9800 . ? C20 H20G 0.9800 . ? C105 C104 1.386(7) . ? C105 H10F 0.9500 . ? C102 H10G 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C201 H20H 0.9500 . ? C23 C24 1.494(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C104 H10H 0.9500 . ? C300 C305 1.375(7) . ? C300 C301 1.378(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C305 C304 1.390(8) . ? C305 H30D 0.9500 . ? C301 C302 1.375(7) . ? C301 H30E 0.9500 . ? C302 C303 1.364(8) . ? C302 H30F 0.9500 . ? C303 C304 1.349(10) . ? C303 H30G 0.9500 . ? C304 H30H 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 C200 Sn1 C100 105.37(17) . . ? C200 Sn1 C300 108.27(17) . . ? C100 Sn1 C300 104.96(18) . . ? C200 Sn1 Si1 115.13(13) . . ? C100 Sn1 Si1 110.53(12) . . ? C300 Sn1 Si1 111.90(13) . . ? N5 Si1 N3 108.01(19) . . ? N5 Si1 N1 108.00(19) . . ? N3 Si1 N1 108.13(19) . . ? N5 Si1 Sn1 114.77(13) . . ? N3 Si1 Sn1 109.95(15) . . ? N1 Si1 Sn1 107.77(14) . . ? C31 C32 C33 107.5(4) . . ? C31 C32 H32A 126.2 . . ? C33 C32 H32A 126.2 . . ? C201 C200 C205 116.1(4) . . ? C201 C200 Sn1 125.5(4) . . ? C205 C200 Sn1 118.2(4) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C23 N4 N3 105.4(4) . . ? C21 N3 N4 110.0(4) . . ? C21 N3 Si1 139.8(4) . . ? N4 N3 Si1 109.9(3) . . ? C11 C12 C13 107.0(4) . . ? C11 C12 H12A 126.5 . . ? C13 C12 H12A 126.5 . . ? C11 N1 N2 110.5(4) . . ? C11 N1 Si1 140.1(3) . . ? N2 N1 Si1 109.4(3) . . ? C13 N2 N1 104.9(4) . . ? N6 C33 C32 110.3(4) . . ? N6 C33 C34 121.1(4) . . ? C32 C33 C34 128.6(4) . . ? C33 N6 N5 105.9(4) . . ? C32 C31 N5 106.2(4) . . ? C32 C31 C30 131.2(4) . . ? N5 C31 C30 122.6(4) . . ? C104 C103 C102 119.3(5) . . ? C104 C103 H10D 120.4 . . ? C102 C103 H10D 120.4 . . ? C31 N5 N6 110.1(3) . . ? C31 N5 Si1 138.1(3) . . ? N6 N5 Si1 111.7(3) . . ? C203 C204 C205 120.3(6) . . ? C203 C204 H20A 119.9 . . ? C205 C204 H20A 119.9 . . ? C21 C22 C23 107.1(5) . . ? C21 C22 H22A 126.5 . . ? C23 C22 H22A 126.5 . . ? C105 C100 C101 117.3(4) . . ? C105 C100 Sn1 120.9(3) . . ? C101 C100 Sn1 121.8(4) . . ? C203 C202 C201 120.6(5) . . ? C203 C202 H20B 119.7 . . ? C201 C202 H20B 119.7 . . ? C204 C203 C202 118.9(5) . . ? C204 C203 H20C 120.5 . . ? C202 C203 H20C 120.5 . . ? C102 C101 C100 122.0(5) . . ? C102 C101 H10E 119.0 . . ? C100 C101 H10E 119.0 . . ? C204 C205 C200 122.4(5) . . ? C204 C205 H20D 118.8 . . ? C200 C205 H20D 118.8 . . ? N2 C13 C12 110.6(4) . . ? N2 C13 C14 118.9(5) . . ? C12 C13 C14 130.4(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 C20 H20E 109.5 . . ? C21 C20 H20F 109.5 . . ? H20E C20 H20F 109.5 . . ? C21 C20 H20G 109.5 . . ? H20E C20 H20G 109.5 . . ? H20F C20 H20G 109.5 . . ? C100 C105 C104 120.8(5) . . ? C100 C105 H10F 119.6 . . ? C104 C105 H10F 119.6 . . ? C101 C102 C103 120.0(5) . . ? C101 C102 H10G 120.0 . . ? C103 C102 H10G 120.0 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C202 C201 C200 121.7(5) . . ? C202 C201 H20H 119.2 . . ? C200 C201 H20H 119.2 . . ? N4 C23 C22 110.9(5) . . ? N4 C23 C24 120.2(6) . . ? C22 C23 C24 128.9(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C103 C104 C105 120.6(5) . . ? C103 C104 H10H 119.7 . . ? C105 C104 H10H 119.7 . . ? C12 C11 N1 107.0(4) . . ? C12 C11 C10 131.2(4) . . ? N1 C11 C10 121.6(4) . . ? C22 C21 N3 106.6(5) . . ? C22 C21 C20 131.2(5) . . ? N3 C21 C20 122.2(5) . . ? C305 C300 C301 117.1(5) . . ? C305 C300 Sn1 123.0(4) . . ? C301 C300 Sn1 119.9(4) . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C300 C305 C304 120.7(6) . . ? C300 C305 H30D 119.7 . . ? C304 C305 H30D 119.7 . . ? C302 C301 C300 121.8(5) . . ? C302 C301 H30E 119.1 . . ? C300 C301 H30E 119.1 . . ? C303 C302 C301 120.3(6) . . ? C303 C302 H30F 119.9 . . ? C301 C302 H30F 119.9 . . ? C304 C303 C302 118.9(6) . . ? C304 C303 H30G 120.5 . . ? C302 C303 H30G 120.5 . . ? C303 C304 C305 121.2(6) . . ? C303 C304 H30H 119.4 . . ? C305 C304 H30H 119.4 . . ? 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 C200 Sn1 Si1 N5 42.9(2) . . . . ? C100 Sn1 Si1 N5 162.1(2) . . . . ? C300 Sn1 Si1 N5 -81.3(2) . . . . ? C200 Sn1 Si1 N3 164.88(19) . . . . ? C100 Sn1 Si1 N3 -75.9(2) . . . . ? C300 Sn1 Si1 N3 40.7(2) . . . . ? C200 Sn1 Si1 N1 -77.5(2) . . . . ? C100 Sn1 Si1 N1 41.8(2) . . . . ? C300 Sn1 Si1 N1 158.36(19) . . . . ? C100 Sn1 C200 C201 -102.8(5) . . . . ? C300 Sn1 C200 C201 145.4(4) . . . . ? Si1 Sn1 C200 C201 19.3(5) . . . . ? C100 Sn1 C200 C205 71.4(4) . . . . ? C300 Sn1 C200 C205 -40.4(4) . . . . ? Si1 Sn1 C200 C205 -166.5(4) . . . . ? C23 N4 N3 C21 -2.0(6) . . . . ? C23 N4 N3 Si1 172.2(4) . . . . ? N5 Si1 N3 C21 -14.2(6) . . . . ? N1 Si1 N3 C21 102.4(6) . . . . ? Sn1 Si1 N3 C21 -140.2(5) . . . . ? N5 Si1 N3 N4 174.2(3) . . . . ? N1 Si1 N3 N4 -69.2(3) . . . . ? Sn1 Si1 N3 N4 48.3(3) . . . . ? N5 Si1 N1 C11 94.9(5) . . . . ? N3 Si1 N1 C11 -21.7(6) . . . . ? Sn1 Si1 N1 C11 -140.6(5) . . . . ? N5 Si1 N1 N2 -82.7(3) . . . . ? N3 Si1 N1 N2 160.7(3) . . . . ? Sn1 Si1 N1 N2 41.9(3) . . . . ? C11 N1 N2 C13 0.3(5) . . . . ? Si1 N1 N2 C13 178.7(3) . . . . ? C31 C32 C33 N6 -0.4(6) . . . . ? C31 C32 C33 C34 179.0(5) . . . . ? C32 C33 N6 N5 0.0(6) . . . . ? C34 C33 N6 N5 -179.4(4) . . . . ? C33 C32 C31 N5 0.5(5) . . . . ? C33 C32 C31 C30 -176.8(5) . . . . ? C32 C31 N5 N6 -0.5(5) . . . . ? C30 C31 N5 N6 177.1(4) . . . . ? C32 C31 N5 Si1 -176.3(4) . . . . ? C30 C31 N5 Si1 1.3(8) . . . . ? C33 N6 N5 C31 0.3(5) . . . . ? C33 N6 N5 Si1 177.3(3) . . . . ? N3 Si1 N5 C31 98.0(5) . . . . ? N1 Si1 N5 C31 -18.7(5) . . . . ? Sn1 Si1 N5 C31 -139.0(4) . . . . ? N3 Si1 N5 N6 -77.8(3) . . . . ? N1 Si1 N5 N6 165.5(3) . . . . ? Sn1 Si1 N5 N6 45.2(3) . . . . ? C200 Sn1 C100 C105 -144.2(4) . . . . ? C300 Sn1 C100 C105 -30.0(4) . . . . ? Si1 Sn1 C100 C105 90.8(4) . . . . ? C200 Sn1 C100 C101 35.4(4) . . . . ? C300 Sn1 C100 C101 149.6(4) . . . . ? Si1 Sn1 C100 C101 -89.6(4) . . . . ? C205 C204 C203 C202 1.4(9) . . . . ? C201 C202 C203 C204 -0.7(9) . . . . ? C105 C100 C101 C102 1.4(7) . . . . ? Sn1 C100 C101 C102 -178.2(4) . . . . ? C203 C204 C205 C200 -1.2(10) . . . . ? C201 C200 C205 C204 0.1(8) . . . . ? Sn1 C200 C205 C204 -174.6(5) . . . . ? N1 N2 C13 C12 -0.6(6) . . . . ? N1 N2 C13 C14 176.3(5) . . . . ? C11 C12 C13 N2 0.6(6) . . . . ? C11 C12 C13 C14 -175.8(6) . . . . ? C101 C100 C105 C104 -1.9(7) . . . . ? Sn1 C100 C105 C104 177.7(4) . . . . ? C100 C101 C102 C103 -0.3(8) . . . . ? C104 C103 C102 C101 -0.2(8) . . . . ? C203 C202 C201 C200 -0.4(9) . . . . ? C205 C200 C201 C202 0.7(8) . . . . ? Sn1 C200 C201 C202 175.0(4) . . . . ? N3 N4 C23 C22 2.6(6) . . . . ? N3 N4 C23 C24 -178.3(5) . . . . ? C21 C22 C23 N4 -2.2(7) . . . . ? C21 C22 C23 C24 178.7(6) . . . . ? C102 C103 C104 C105 -0.3(8) . . . . ? C100 C105 C104 C103 1.5(8) . . . . ? C13 C12 C11 N1 -0.4(5) . . . . ? C13 C12 C11 C10 175.3(5) . . . . ? N2 N1 C11 C12 0.0(5) . . . . ? Si1 N1 C11 C12 -177.5(4) . . . . ? N2 N1 C11 C10 -176.1(4) . . . . ? Si1 N1 C11 C10 6.3(8) . . . . ? C23 C22 C21 N3 0.9(6) . . . . ? C23 C22 C21 C20 -179.1(6) . . . . ? N4 N3 C21 C22 0.7(6) . . . . ? Si1 N3 C21 C22 -170.9(4) . . . . ? N4 N3 C21 C20 -179.4(5) . . . . ? Si1 N3 C21 C20 9.1(9) . . . . ? C200 Sn1 C300 C305 -109.9(4) . . . . ? C100 Sn1 C300 C305 137.9(4) . . . . ? Si1 Sn1 C300 C305 18.0(5) . . . . ? C200 Sn1 C300 C301 68.9(4) . . . . ? C100 Sn1 C300 C301 -43.3(4) . . . . ? Si1 Sn1 C300 C301 -163.2(4) . . . . ? C301 C300 C305 C304 0.8(8) . . . . ? Sn1 C300 C305 C304 179.7(5) . . . . ? C305 C300 C301 C302 0.4(8) . . . . ? Sn1 C300 C301 C302 -178.5(4) . . . . ? C300 C301 C302 C303 -1.1(9) . . . . ? C301 C302 C303 C304 0.7(10) . . . . ? C302 C303 C304 C305 0.5(11) . . . . ? C300 C305 C304 C303 -1.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.026 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.081