# 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 'Norbert Mitzel' _publ_contact_author_email MITZEL@UNI-BIELEFELD.DE _publ_section_title ; Syntheses and structures of (N',N'-dimethylhydrazido)silanes ; loop_ _publ_author_name 'Norbert Mitzel' 'Ingo Gronde' 'Tania Pape' 'Alexander Willner' # Attachment 'compound_1.CIF' data_comp_1 _database_code_depnum_ccdc_archive 'CCDC 715611' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H24 N4 Si' _chemical_formula_sum 'C16 H24 N4 Si' _chemical_formula_weight 300.48 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8297(17) _cell_length_b 9.9066(18) _cell_length_c 10.182(2) _cell_angle_alpha 93.77(2) _cell_angle_beta 91.31(2) _cell_angle_gamma 98.49(2) _cell_volume 878.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 106 _cell_measurement_theta_min 4.58 _cell_measurement_theta_max 27.06 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 324 _exptl_absorpt_coefficient_mu 0.134 _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 163(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 IPDS-1' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13667 _diffrn_reflns_av_R_equivalents 0.1390 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.58 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3509 _reflns_number_gt 2633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1' _computing_cell_refinement 'STOE IPDS-1 software package' _computing_data_reduction 'STOE IPDS-1 software package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.1192P)^2^+0.3996P] 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 3509 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.2056 _refine_ls_wR_factor_gt 0.1820 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.10714(8) 0.25811(8) 0.82861(7) 0.0154(2) Uani 1 1 d . . . N1 N 0.2013(3) 0.4018(3) 0.7675(2) 0.0203(6) Uani 1 1 d . . . H1 H 0.2810 0.4489 0.8116 0.024 Uiso 1 1 d R . . N2 N 0.1521(3) 0.4468(3) 0.6456(2) 0.0226(6) Uani 1 1 d . . . N3 N 0.1174(3) 0.1146(3) 0.7293(2) 0.0218(6) Uani 1 1 d . . . H3 H 0.0331 0.0561 0.7120 0.026 Uiso 1 1 d R . . N4 N 0.2553(3) 0.0854(3) 0.6730(2) 0.0239(6) Uani 1 1 d . . . C1 C 0.2810(4) 0.4679(5) 0.5602(3) 0.0455(10) Uani 1 1 d . . . H1A H 0.3600 0.5388 0.6015 0.068 Uiso 1 1 calc R . . H1B H 0.2470 0.4968 0.4756 0.068 Uiso 1 1 calc R . . H1C H 0.3233 0.3823 0.5457 0.068 Uiso 1 1 calc R . . C2 C 0.0870(5) 0.5722(4) 0.6704(4) 0.0410(9) Uani 1 1 d . . . H2A H 0.0030 0.5563 0.7314 0.062 Uiso 1 1 calc R . . H2B H 0.0480 0.6005 0.5873 0.062 Uiso 1 1 calc R . . H2C H 0.1664 0.6443 0.7093 0.062 Uiso 1 1 calc R . . C3 C 0.2326(5) 0.0646(5) 0.5315(4) 0.0520(11) Uani 1 1 d . . . H3A H 0.1554 -0.0160 0.5098 0.078 Uiso 1 1 calc R . . H3B H 0.3295 0.0505 0.4916 0.078 Uiso 1 1 calc R . . H3C H 0.1975 0.1453 0.4973 0.078 Uiso 1 1 calc R . . C4 C 0.3042(5) -0.0327(4) 0.7267(4) 0.0489(10) Uani 1 1 d . . . H4A H 0.3214 -0.0156 0.8221 0.073 Uiso 1 1 calc R . . H4B H 0.3997 -0.0505 0.6863 0.073 Uiso 1 1 calc R . . H4C H 0.2249 -0.1124 0.7081 0.073 Uiso 1 1 calc R . . C5 C -0.1040(3) 0.2557(3) 0.8383(3) 0.0182(6) Uani 1 1 d . . . C6 C -0.1936(3) 0.2558(3) 0.7240(3) 0.0249(7) Uani 1 1 d . . . H6 H -0.1458 0.2592 0.6413 0.030 Uiso 1 1 calc R . . C7 C -0.3517(4) 0.2510(4) 0.7283(4) 0.0337(8) Uani 1 1 d . . . H7 H -0.4108 0.2509 0.6491 0.040 Uiso 1 1 calc R . . C8 C -0.4223(4) 0.2464(4) 0.8477(4) 0.0390(9) Uani 1 1 d . . . H8 H -0.5302 0.2436 0.8509 0.047 Uiso 1 1 calc R . . C9 C -0.3365(4) 0.2457(4) 0.9620(4) 0.0345(8) Uani 1 1 d . . . H9 H -0.3854 0.2418 1.0441 0.041 Uiso 1 1 calc R . . C10 C -0.1781(3) 0.2507(3) 0.9582(3) 0.0237(7) Uani 1 1 d . . . H10 H -0.1199 0.2506 1.0378 0.028 Uiso 1 1 calc R . . C11 C 0.1992(3) 0.2553(3) 0.9958(3) 0.0174(6) Uani 1 1 d . . . C12 C 0.2085(3) 0.1314(3) 1.0505(3) 0.0251(7) Uani 1 1 d . . . H12 H 0.1635 0.0488 1.0032 0.030 Uiso 1 1 calc R . . C13 C 0.2810(4) 0.1245(3) 1.1710(3) 0.0281(7) Uani 1 1 d . . . H13 H 0.2852 0.0386 1.2059 0.034 Uiso 1 1 calc R . . C14 C 0.3474(4) 0.2444(4) 1.2402(3) 0.0285(7) Uani 1 1 d . . . H14 H 0.3991 0.2407 1.3224 0.034 Uiso 1 1 calc R . . C15 C 0.3388(4) 0.3684(3) 1.1902(3) 0.0292(7) Uani 1 1 d . . . H15 H 0.3837 0.4504 1.2384 0.035 Uiso 1 1 calc R . . C16 C 0.2648(4) 0.3747(3) 1.0697(3) 0.0238(7) Uani 1 1 d . . . H16 H 0.2584 0.4613 1.0367 0.029 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 0.0116(4) 0.0179(5) 0.0163(4) 0.0034(3) 0.0003(3) 0.0003(3) N1 0.0192(12) 0.0205(14) 0.0202(12) 0.0075(10) -0.0048(9) -0.0027(10) N2 0.0271(13) 0.0232(15) 0.0168(12) 0.0078(10) 0.0002(9) -0.0012(10) N3 0.0128(11) 0.0252(15) 0.0254(13) -0.0030(10) 0.0014(9) -0.0020(10) N4 0.0168(12) 0.0282(16) 0.0279(13) 0.0006(10) 0.0046(10) 0.0071(10) C1 0.040(2) 0.065(3) 0.0291(18) 0.0125(17) 0.0123(15) -0.0055(19) C2 0.055(2) 0.030(2) 0.040(2) 0.0090(15) -0.0087(17) 0.0106(17) C3 0.050(2) 0.079(3) 0.0298(19) -0.0049(19) 0.0131(17) 0.020(2) C4 0.047(2) 0.034(3) 0.070(3) 0.0103(19) 0.007(2) 0.0191(18) C5 0.0151(13) 0.0155(15) 0.0237(14) 0.0028(11) 0.0011(10) 0.0013(10) C6 0.0182(14) 0.0248(18) 0.0320(16) 0.0052(12) -0.0014(12) 0.0033(11) C7 0.0181(15) 0.032(2) 0.050(2) 0.0049(15) -0.0077(14) 0.0020(13) C8 0.0151(15) 0.031(2) 0.071(3) 0.0024(17) 0.0034(15) 0.0045(13) C9 0.0241(16) 0.030(2) 0.050(2) 0.0023(15) 0.0182(15) 0.0024(13) C10 0.0200(14) 0.0224(17) 0.0292(16) 0.0039(12) 0.0056(11) 0.0029(12) C11 0.0134(12) 0.0218(16) 0.0170(13) 0.0028(10) 0.0019(10) 0.0021(10) C12 0.0280(16) 0.0230(18) 0.0222(14) 0.0053(12) -0.0024(12) -0.0045(12) C13 0.0380(18) 0.0234(19) 0.0236(15) 0.0088(12) -0.0027(13) 0.0038(13) C14 0.0330(17) 0.037(2) 0.0161(14) 0.0036(12) -0.0026(12) 0.0073(14) C15 0.0372(18) 0.0261(19) 0.0224(15) -0.0048(12) -0.0061(13) 0.0021(14) C16 0.0306(16) 0.0187(17) 0.0221(14) 0.0002(11) -0.0019(12) 0.0051(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.702(2) . ? Si1 N3 1.704(3) . ? Si1 C5 1.866(3) . ? Si1 C11 1.874(3) . ? N1 N2 1.426(3) . ? N1 H1 0.8800 . ? N2 C1 1.447(4) . ? N2 C2 1.454(5) . ? N3 N4 1.418(3) . ? N3 H3 0.8795 . ? N4 C4 1.442(5) . ? N4 C3 1.447(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.393(4) . ? C5 C10 1.398(4) . ? C6 C7 1.391(4) . ? C6 H6 0.9500 . ? C7 C8 1.379(5) . ? C7 H7 0.9500 . ? C8 C9 1.376(5) . ? C8 H8 0.9500 . ? C9 C10 1.393(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.393(4) . ? C11 C16 1.400(4) . ? C12 C13 1.381(4) . ? C12 H12 0.9500 . ? C13 C14 1.384(5) . ? C13 H13 0.9500 . ? C14 C15 1.372(5) . ? C14 H14 0.9500 . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 N3 112.46(12) . . ? N1 Si1 C5 113.94(13) . . ? N3 Si1 C5 102.01(12) . . ? N1 Si1 C11 104.02(12) . . ? N3 Si1 C11 113.31(13) . . ? C5 Si1 C11 111.44(12) . . ? N2 N1 Si1 120.56(17) . . ? N2 N1 H1 119.7 . . ? Si1 N1 H1 119.7 . . ? N1 N2 C1 109.3(3) . . ? N1 N2 C2 109.4(2) . . ? C1 N2 C2 111.0(3) . . ? N4 N3 Si1 123.01(19) . . ? N4 N3 H3 118.5 . . ? Si1 N3 H3 118.5 . . ? N3 N4 C4 111.1(3) . . ? N3 N4 C3 109.1(3) . . ? C4 N4 C3 110.8(3) . . ? N2 C1 H1A 109.5 . . ? N2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N4 C3 H3A 109.5 . . ? N4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C10 117.8(3) . . ? C6 C5 Si1 120.2(2) . . ? C10 C5 Si1 122.0(2) . . ? C7 C6 C5 121.3(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C8 C7 C6 119.9(3) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 119.9(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.4(3) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C5 120.6(3) . . ? C9 C10 H10 119.7 . . ? C5 C10 H10 119.7 . . ? C12 C11 C16 117.1(3) . . ? C12 C11 Si1 120.4(2) . . ? C16 C11 Si1 122.5(2) . . ? C13 C12 C11 122.2(3) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 119.3(3) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 120.9(3) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.608 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.091 _vrf_PLAT029_comp_1 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.92 RESPONSE: 1-circle goniometer of STOE diffractometer and space group (rotation around the spindle axis only) ; # Attachment 'compound_2.cif' data_comp_2 _database_code_depnum_ccdc_archive 'CCDC 715612' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H20 N4 Si' _chemical_formula_sum 'C6 H20 N4 Si' _chemical_formula_weight 176.35 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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.239(8) _cell_length_b 8.702(9) _cell_length_c 8.730(9) _cell_angle_alpha 117.443(15) _cell_angle_beta 97.648(17) _cell_angle_gamma 92.130(18) _cell_volume 547.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 196 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9206 _exptl_absorpt_correction_T_max 0.9830 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.426167 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2368 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 24.00 _reflns_number_total 1600 _reflns_number_gt 1192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Hydrogens bonded to nitrogen were refined isotropically. 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^)+(0.0923P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1600 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1551 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.40519(12) 0.80892(12) 0.63588(12) 0.0231(3) Uani 1 1 d . . . N1 N 0.6095(4) 0.7858(4) 0.6667(4) 0.0304(8) Uani 1 1 d . . . H1N H 0.640(4) 0.699(4) 0.677(4) 0.018(9) Uiso 1 1 d . . . N2 N 0.7317(3) 0.9068(4) 0.6678(4) 0.0283(7) Uani 1 1 d . . . N3 N 0.3133(4) 0.7572(4) 0.4288(4) 0.0295(8) Uani 1 1 d . . . H3N H 0.298(4) 0.822(4) 0.395(4) 0.007(9) Uiso 1 1 d . . . N4 N 0.2816(3) 0.5804(4) 0.2971(4) 0.0260(7) Uani 1 1 d . . . C1 C 0.3735(5) 1.0400(5) 0.7700(5) 0.0345(9) Uani 1 1 d . . . H1A H 0.4215 1.1109 0.7233 0.052 Uiso 1 1 calc R . . H1B H 0.4270 1.0808 0.8914 0.052 Uiso 1 1 calc R . . H1C H 0.2552 1.0505 0.7662 0.052 Uiso 1 1 calc R . . C2 C 0.3069(5) 0.6614(5) 0.7030(5) 0.0324(9) Uani 1 1 d . . . H2A H 0.1880 0.6696 0.6929 0.049 Uiso 1 1 calc R . . H2B H 0.3536 0.6948 0.8248 0.049 Uiso 1 1 calc R . . H2C H 0.3269 0.5414 0.6271 0.049 Uiso 1 1 calc R . . C3 C 0.8324(5) 0.9971(5) 0.8404(5) 0.0440(11) Uani 1 1 d . . . H3A H 0.7628 1.0603 0.9272 0.066 Uiso 1 1 calc R . . H3B H 0.9172 1.0798 0.8416 0.066 Uiso 1 1 calc R . . H3C H 0.8851 0.9123 0.8690 0.066 Uiso 1 1 calc R . . C4 C 0.8343(5) 0.8159(5) 0.5383(5) 0.0361(10) Uani 1 1 d . . . H4A H 0.8893 0.7316 0.5659 0.054 Uiso 1 1 calc R . . H4B H 0.9173 0.9001 0.5393 0.054 Uiso 1 1 calc R . . H4C H 0.7656 0.7546 0.4220 0.054 Uiso 1 1 calc R . . C5 C 0.3653(5) 0.5508(5) 0.1515(5) 0.0362(10) Uani 1 1 d . . . H5A H 0.3228 0.6208 0.0969 0.054 Uiso 1 1 calc R . . H5B H 0.3458 0.4270 0.0650 0.054 Uiso 1 1 calc R . . H5C H 0.4839 0.5844 0.1941 0.054 Uiso 1 1 calc R . . C6 C 0.1061(4) 0.5348(5) 0.2381(5) 0.0412(10) Uani 1 1 d . . . H6A H 0.0522 0.5484 0.3364 0.062 Uiso 1 1 calc R . . H6B H 0.0841 0.4136 0.1455 0.062 Uiso 1 1 calc R . . H6C H 0.0628 0.6116 0.1922 0.062 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 0.0252(6) 0.0254(6) 0.0216(5) 0.0136(4) 0.0052(4) -0.0025(4) N1 0.0314(19) 0.0258(19) 0.043(2) 0.0247(16) 0.0066(14) -0.0027(14) N2 0.0251(17) 0.0301(17) 0.0301(17) 0.0158(14) 0.0016(13) -0.0045(12) N3 0.041(2) 0.029(2) 0.0258(18) 0.0208(16) 0.0007(13) 0.0005(14) N4 0.0262(17) 0.0284(18) 0.0231(16) 0.0123(13) 0.0050(12) -0.0045(12) C1 0.039(2) 0.031(2) 0.036(2) 0.0171(18) 0.0082(17) 0.0005(16) C2 0.035(2) 0.037(2) 0.031(2) 0.0208(18) 0.0081(16) -0.0042(16) C3 0.042(3) 0.043(3) 0.040(2) 0.017(2) -0.0028(19) -0.0069(19) C4 0.034(2) 0.038(2) 0.042(2) 0.0231(19) 0.0110(18) -0.0016(17) C5 0.042(2) 0.041(2) 0.031(2) 0.0195(19) 0.0155(18) 0.0027(17) C6 0.033(2) 0.044(3) 0.040(2) 0.015(2) 0.0047(18) -0.0068(17) _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 1.703(4) . ? Si1 N3 1.704(4) . ? Si1 C2 1.841(4) . ? Si1 C1 1.853(4) . ? N1 N2 1.425(4) . ? N1 H1N 0.84(4) . ? N2 C4 1.448(5) . ? N2 C3 1.450(5) . ? N2 H3N 2.67(3) 2_676 ? N3 N4 1.420(4) . ? N3 H3N 0.75(3) . ? N4 C6 1.444(5) . ? N4 C5 1.450(4) . ? N4 H1N 2.64(4) 2_666 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 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 N3 117.21(16) . . ? N1 Si1 C2 104.07(18) . . ? N3 Si1 C2 108.62(17) . . ? N1 Si1 C1 109.44(17) . . ? N3 Si1 C1 104.65(18) . . ? C2 Si1 C1 113.12(18) . . ? N2 N1 Si1 121.3(3) . . ? N2 N1 H1N 118(2) . . ? Si1 N1 H1N 120(2) . . ? N1 N2 C4 110.0(3) . . ? N1 N2 C3 109.1(3) . . ? C4 N2 C3 109.8(3) . . ? N1 N2 H3N 130.7(7) . 2_676 ? C4 N2 H3N 97.1(7) . 2_676 ? C3 N2 H3N 98.5(7) . 2_676 ? N4 N3 Si1 120.3(3) . . ? N4 N3 H3N 114(2) . . ? Si1 N3 H3N 125(2) . . ? N3 N4 C6 109.3(3) . . ? N3 N4 C5 111.0(3) . . ? C6 N4 C5 110.5(3) . . ? N3 N4 H1N 127.9(7) . 2_666 ? C6 N4 H1N 99.9(7) . 2_666 ? C5 N4 H1N 96.9(7) . 2_666 ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N N4 0.84(4) 2.64(4) 3.483(6) 176.65 2_666 N3 H3N N2 0.76(3) 2.67(3) 3.416(6) 169.94 2_676 _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.566 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.065 _vrf_PLAT222_comp_2 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 9.43 Ratio RESPONSE: Hydrogens bonded to nitrogen were refined isotropically with a small Ueq, hydrogens bonded to carbons were included at calculated positions with Ueq = 1.5 times of the corresponding carbon. ; _vrf_PLAT352_comp_2 ; PROBLEM: Short N-H Bond (0.87A) N3 - H3N ... 0.76 Ang. RESPONSE: within 3 esds the bond is in the expected value ; _vrf_PLAT771_comp_2 ; PROBLEM: Suspect N-H Bond in CIF: N2 -- H3N .. 2.67 Ang. RESPONSE: discussed N...H contact ; # Attachment 'compound_5.cif' data_comp_5 _database_code_depnum_ccdc_archive 'CCDC 715613' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Chloro-(bis-dimethylhydrazino)-phenylsilane _chemical_melting_point ? _chemical_formula_moiety 'C10 H19 Cl N4 Si' _chemical_formula_sum 'C10 H19 Cl N4 Si' _chemical_formula_weight 258.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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 8.9720(8) _cell_length_b 12.1156(10) _cell_length_c 12.9035(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1402.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 5.01 _cell_measurement_theta_max 72.39 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 3.084 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.3492 _exptl_absorpt_correction_T_max 0.9342 _exptl_absorpt_process_details 'SADABS - Bruker Nonius - V2.10' _exptl_special_details ; sadabs reports ratio of Tmin/Tmax = 0.373787 ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54186 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w and \phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8190 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 5.01 _diffrn_reflns_theta_max 72.39 _reflns_number_total 2651 _reflns_number_gt 2338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0816P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 2651 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.79252(8) 0.51056(6) 0.71003(6) 0.0214(2) Uani 1 1 d . . . Cl1 Cl 0.88422(8) 0.35552(6) 0.74458(6) 0.0329(2) Uani 1 1 d . . . N1 N 0.8346(3) 0.5557(2) 0.58952(19) 0.0273(6) Uani 1 1 d . . . N2 N 0.9803(3) 0.5964(2) 0.5688(2) 0.0313(6) Uani 1 1 d . . . N3 N 0.8633(3) 0.6057(2) 0.79305(19) 0.0258(6) Uani 1 1 d . . . N4 N 0.8646(3) 0.5855(2) 0.90256(17) 0.0268(6) Uani 1 1 d . . . C1 C 1.0600(4) 0.5191(4) 0.5021(3) 0.0453(10) Uani 1 1 d . . . H1B H 1.0693 0.4478 0.5373 0.068 Uiso 1 1 calc R . . H1C H 1.1595 0.5483 0.4868 0.068 Uiso 1 1 calc R . . H1D H 1.0047 0.5093 0.4372 0.068 Uiso 1 1 calc R . . C2 C 0.9672(5) 0.7044(3) 0.5201(3) 0.0468(10) Uani 1 1 d . . . H2A H 0.9105 0.6976 0.4555 0.070 Uiso 1 1 calc R . . H2B H 1.0669 0.7332 0.5048 0.070 Uiso 1 1 calc R . . H2C H 0.9155 0.7551 0.5671 0.070 Uiso 1 1 calc R . . C3 C 0.8063(5) 0.6839(3) 0.9541(2) 0.0396(8) Uani 1 1 d . . . H3B H 0.8667 0.7481 0.9348 0.059 Uiso 1 1 calc R . . H3C H 0.8102 0.6736 1.0294 0.059 Uiso 1 1 calc R . . H3D H 0.7028 0.6960 0.9326 0.059 Uiso 1 1 calc R . . C4 C 1.0165(4) 0.5624(3) 0.9363(3) 0.0384(8) Uani 1 1 d . . . H4A H 1.0546 0.4978 0.8990 0.058 Uiso 1 1 calc R . . H4B H 1.0170 0.5476 1.0109 0.058 Uiso 1 1 calc R . . H4C H 1.0799 0.6264 0.9215 0.058 Uiso 1 1 calc R . . C5 C 0.5880(3) 0.4921(2) 0.71787(19) 0.0215(6) Uani 1 1 d . . . C6 C 0.5159(3) 0.3910(3) 0.7308(2) 0.0252(7) Uani 1 1 d . . . H6A H 0.5735 0.3257 0.7382 0.030 Uiso 1 1 calc R . . C7 C 0.3613(3) 0.3842(3) 0.7330(2) 0.0283(7) Uani 1 1 d . . . H7A H 0.3140 0.3148 0.7426 0.034 Uiso 1 1 calc R . . C8 C 0.2767(4) 0.4785(3) 0.7213(2) 0.0330(7) Uani 1 1 d . . . H8A H 0.1710 0.4740 0.7228 0.040 Uiso 1 1 calc R . . C9 C 0.3454(4) 0.5795(3) 0.7074(3) 0.0379(8) Uani 1 1 d . . . H9A H 0.2871 0.6443 0.6988 0.046 Uiso 1 1 calc R . . C10 C 0.4996(3) 0.5861(3) 0.7060(3) 0.0316(7) Uani 1 1 d . . . H10A H 0.5460 0.6558 0.6969 0.038 Uiso 1 1 calc R . . H1A H 0.784(4) 0.538(2) 0.539(2) 0.016(8) Uiso 1 1 d . . . H3A H 0.920(4) 0.644(3) 0.782(2) 0.017(9) Uiso 1 1 d . . . 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 0.0190(4) 0.0235(4) 0.0217(3) 0.0013(3) -0.0005(3) -0.0013(3) Cl1 0.0258(4) 0.0270(4) 0.0459(4) 0.0040(3) -0.0024(3) 0.0034(3) N1 0.0237(14) 0.0365(16) 0.0216(12) -0.0023(11) -0.0031(10) -0.0060(11) N2 0.0241(15) 0.0451(17) 0.0246(13) 0.0043(11) 0.0008(10) -0.0082(13) N3 0.0272(14) 0.0284(14) 0.0218(11) 0.0057(11) -0.0005(11) -0.0105(12) N4 0.0301(15) 0.0302(14) 0.0200(11) 0.0006(10) 0.0003(10) -0.0046(11) C1 0.037(2) 0.070(3) 0.0296(16) 0.0049(18) 0.0056(13) 0.0114(18) C2 0.058(3) 0.047(2) 0.0360(19) 0.0081(16) 0.0036(17) -0.015(2) C3 0.057(2) 0.0334(19) 0.0279(16) -0.0026(13) 0.0050(15) -0.0005(17) C4 0.038(2) 0.051(2) 0.0261(16) 0.0003(15) -0.0049(13) -0.0002(17) C5 0.0207(14) 0.0255(15) 0.0184(12) -0.0004(12) -0.0004(9) -0.0017(11) C6 0.0254(16) 0.0258(15) 0.0243(16) 0.0039(11) -0.0036(11) -0.0021(11) C7 0.0272(16) 0.0334(17) 0.0243(15) -0.0007(11) 0.0005(12) -0.0093(12) C8 0.0197(15) 0.046(2) 0.0334(16) -0.0037(14) -0.0006(12) -0.0031(13) C9 0.0243(18) 0.0347(19) 0.0548(19) -0.0063(17) -0.0030(15) 0.0080(13) C10 0.0236(17) 0.0274(17) 0.0438(17) -0.0006(14) 0.0010(14) -0.0012(13) _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 1.691(3) . ? Si1 N3 1.697(3) . ? Si1 C5 1.851(3) . ? Si1 Cl1 2.0985(11) . ? Cl1 H3A 3.12(3) 3_746 ? N1 N2 1.422(4) . ? N1 H1A 0.82(3) . ? N2 C2 1.457(5) . ? N2 C1 1.459(5) . ? N3 N4 1.434(3) . ? N3 H3A 0.71(3) . ? N4 C4 1.457(4) . ? N4 C3 1.462(4) . ? N4 H1A 2.67(3) 2_665 ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.396(4) . ? C5 C6 1.394(4) . ? C6 C7 1.390(4) . ? C6 H6A 0.9500 . ? C7 C8 1.380(4) . ? C7 H7A 0.9500 . ? C8 C9 1.382(5) . ? C8 H8A 0.9500 . ? C9 C10 1.385(5) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 N3 106.08(14) . . ? N1 Si1 C5 108.11(12) . . ? N3 Si1 C5 114.74(14) . . ? N1 Si1 Cl1 113.42(10) . . ? N3 Si1 Cl1 109.09(10) . . ? C5 Si1 Cl1 105.60(10) . . ? Si1 Cl1 H3A 158.7(6) . 3_746 ? N2 N1 Si1 119.36(19) . . ? N2 N1 H1A 117(2) . . ? Si1 N1 H1A 121(2) . . ? N1 N2 C2 108.5(3) . . ? N1 N2 C1 109.8(3) . . ? C2 N2 C1 111.2(3) . . ? N4 N3 Si1 120.6(2) . . ? N4 N3 H3A 108(3) . . ? Si1 N3 H3A 126(3) . . ? N3 N4 C4 109.6(2) . . ? N3 N4 C3 107.8(2) . . ? C4 N4 C3 110.8(3) . . ? N3 N4 H1A 137.9(7) . 2_665 ? C4 N4 H1A 99.3(7) . 2_665 ? C3 N4 H1A 88.8(7) . 2_665 ? N2 C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N4 C3 H3B 109.5 . . ? N4 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 117.8(3) . . ? C10 C5 Si1 117.3(2) . . ? C6 C5 Si1 124.9(2) . . ? C7 C6 C5 121.2(3) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C8 C7 C6 119.9(3) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 119.9(3) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C9 C10 C5 121.3(3) . . ? C9 C10 H10A 119.4 . . ? C5 C10 H10A 119.4 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 72.39 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.527 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.067 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A N4 0.81(4) 2.68(4) 3.457(3) 160(2) 2_664 N3 H3a CL1 0.72(3) 3.11(3) 3.812(3) 166(3) 3_756 _vrf_PLAT771_comp_5 ; PROBLEM: Suspect N-H Bond in CIF: N4 -- H1A .. 2.68 Ang. RESPONSE: discussed N...H contact ; _vrf_PLAT352_comp_5 ; PROBLEM: Short N-H Bond (0.87A) N3 - H3A ... 0.72 Ang. RESPONSE: within 3 esds the bond is in the expected value ; _vrf_PLAT222_comp_5 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.19 Ratio RESPONSE: Hydrogens bonded to nitrogen were refined isotropically with a small Ueq, hydrogens bonded to carbons were included at calculated positions with Ueq = 1.5 times of the corresponding carbon. ; # Attachment 'compound_9.CIF' data_comp_9 _database_code_depnum_ccdc_archive 'CCDC 715614' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H18 N4 Si' _chemical_formula_sum 'C5 H18 N4 Si' _chemical_formula_weight 162.32 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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.326(5) _cell_length_b 8.332(5) _cell_length_c 9.182(5) _cell_angle_alpha 68.915(10) _cell_angle_beta 89.161(10) _cell_angle_gamma 60.685(9) _cell_volume 507.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 180 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9186 _exptl_absorpt_correction_T_max 0.9857 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4763 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0880 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2313 _reflns_number_gt 1528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _refine_special_details ; The carbon atom C1 and the SiH hydrogen atom are disordered to either side of the silicon atom with a 52:48 distribution. 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^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2313 _refine_ls_number_parameters 117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.84551(8) 0.29061(9) 0.07318(7) 0.0482(3) Uani 1 1 d . . . H11 H 0.800(7) 0.429(9) 0.186(7) 0.050 Uiso 0.482(4) 1 d P A 1 H11A H 0.735(7) 0.189(8) 0.041(6) 0.050 Uiso 0.518(4) 1 d P A 2 C1 C 0.6928(6) 0.2087(7) 0.0892(5) 0.0400(12) Uani 0.518(4) 1 d P A 1 H1A H 0.5691 0.3206 0.0248 0.060 Uiso 0.518(4) 1 calc PR A 1 H1B H 0.6825 0.1573 0.2009 0.060 Uiso 0.518(4) 1 calc PR A 1 H1C H 0.7386 0.1009 0.0512 0.060 Uiso 0.518(4) 1 calc PR A 1 C1A C 0.7227(7) 0.4443(8) 0.1616(6) 0.0456(14) Uani 0.482(4) 1 d P A 2 H1A1 H 0.5897 0.5249 0.1097 0.068 Uiso 0.482(4) 1 calc PR A 2 H1A2 H 0.7700 0.5337 0.1528 0.068 Uiso 0.482(4) 1 calc PR A 2 H1A3 H 0.7361 0.3644 0.2743 0.068 Uiso 0.482(4) 1 calc PR A 2 C2 C 0.7076(4) 0.4931(4) -0.3694(3) 0.0786(10) Uani 1 1 d . A . H2A H 0.5910 0.5116 -0.3328 0.118 Uiso 1 1 calc R . . H2B H 0.7276 0.4336 -0.4476 0.118 Uiso 1 1 calc R . . H2C H 0.6983 0.6238 -0.4188 0.118 Uiso 1 1 calc R . . C3 C 1.0379(3) 0.3331(3) -0.2851(3) 0.0522(6) Uani 1 1 d . A . H3A H 1.0289 0.4638 -0.3320 0.078 Uiso 1 1 calc R . . H3B H 1.0595 0.2755 -0.3647 0.078 Uiso 1 1 calc R . . H3C H 1.1427 0.2421 -0.1933 0.078 Uiso 1 1 calc R . . C4 C 1.3679(3) 0.0217(4) 0.1882(3) 0.0547(6) Uani 1 1 d . A . H4A H 1.4192 -0.1234 0.2265 0.082 Uiso 1 1 calc R . . H4B H 1.4588 0.0451 0.2294 0.082 Uiso 1 1 calc R . . H4C H 1.3430 0.0816 0.0715 0.082 Uiso 1 1 calc R . . C5 C 1.2280(4) 0.0230(4) 0.4171(3) 0.0615(7) Uani 1 1 d . A . H5A H 1.1096 0.0867 0.4523 0.092 Uiso 1 1 calc R . . H5B H 1.3196 0.0437 0.4609 0.092 Uiso 1 1 calc R . . H5C H 1.2770 -0.1216 0.4547 0.092 Uiso 1 1 calc R . . N1 N 0.8325(3) 0.4391(3) -0.1164(2) 0.0472(5) Uani 1 1 d . A . H1N H 0.836(3) 0.537(4) -0.138(3) 0.043(7) Uiso 1 1 d . . . N2 N 0.8652(3) 0.3595(3) -0.2340(2) 0.0440(5) Uani 1 1 d . . . N3 N 1.0587(3) 0.0879(3) 0.1799(2) 0.0443(5) Uani 1 1 d . A . H3N H 1.093(3) -0.025(3) 0.193(3) 0.037(6) Uiso 1 1 d . . . N4 N 1.1950(2) 0.1127(2) 0.2430(2) 0.0399(4) Uani 1 1 d . . . 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 0.0320(3) 0.0383(4) 0.0425(4) 0.0018(3) 0.0094(3) -0.0088(3) C1 0.039(3) 0.041(2) 0.043(3) -0.016(2) 0.0078(18) -0.024(2) C1A 0.043(3) 0.046(3) 0.038(3) -0.016(2) 0.002(2) -0.016(3) C2 0.086(2) 0.0630(17) 0.0636(17) 0.0124(14) -0.0316(15) -0.0471(17) C3 0.0674(16) 0.0476(14) 0.0422(13) -0.0153(11) 0.0158(11) -0.0323(13) C4 0.0455(14) 0.0512(14) 0.0647(16) -0.0227(13) 0.0062(12) -0.0236(12) C5 0.0783(18) 0.0502(14) 0.0417(13) -0.0150(11) 0.0006(12) -0.0256(14) N1 0.0519(12) 0.0304(10) 0.0426(11) -0.0030(8) 0.0109(9) -0.0179(9) N2 0.0551(12) 0.0357(10) 0.0352(9) -0.0016(8) -0.0045(8) -0.0279(9) N3 0.0403(11) 0.0278(10) 0.0489(11) -0.0053(8) -0.0019(8) -0.0133(9) N4 0.0409(10) 0.0302(9) 0.0389(9) -0.0117(8) -0.0001(8) -0.0131(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1A 1.669(6) . ? Si1 N3 1.699(2) . ? Si1 N1 1.702(2) . ? Si1 C1 1.696(5) . ? Si1 H11 1.72(6) . ? Si1 H11A 1.61(6) . ? C1 H11A 0.58(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1A H11 0.62(5) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2 N2 1.459(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 N2 1.443(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N4 1.443(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N4 1.464(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N1 N2 1.418(3) . ? N1 H1N 0.78(2) . ? N2 H3N 2.51(2) 2_755 ? N3 N4 1.416(3) . ? N3 H3N 0.80(2) . ? N4 H1N 2.60(2) 2_765 ? 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 C1A Si1 N3 116.36(18) . . ? C1A Si1 N1 106.8(2) . . ? N3 Si1 N1 118.42(10) . . ? C1A Si1 C1 91.2(2) . . ? N3 Si1 C1 107.06(19) . . ? N1 Si1 C1 113.94(19) . . ? C1A Si1 H11 20.9(17) . . ? N3 Si1 H11 99.8(18) . . ? N1 Si1 H11 107.4(18) . . ? C1 Si1 H11 109.1(18) . . ? C1A Si1 H11A 110.1(17) . . ? N3 Si1 H11A 102.9(19) . . ? N1 Si1 H11A 100.9(19) . . ? C1 Si1 H11A 20.0(17) . . ? H11 Si1 H11A 129(2) . . ? Si1 C1 H11A 72(6) . . ? Si1 C1 H1A 109.5 . . ? H11A C1 H1A 102.0 . . ? Si1 C1 H1B 109.5 . . ? H11A C1 H1B 145.4 . . ? Si1 C1 H1C 109.5 . . ? H11A C1 H1C 44.0 . . ? Si1 C1A H11 85(6) . . ? Si1 C1A H1A1 109.5 . . ? Si1 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? Si1 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 N1 Si1 118.72(16) . . ? N2 N1 H1N 116.1(17) . . ? Si1 N1 H1N 123.2(18) . . ? N1 N2 C3 110.62(18) . . ? N1 N2 C2 109.8(2) . . ? C3 N2 C2 110.3(2) . . ? N1 N2 H3N 124.8(5) . 2_755 ? C3 N2 H3N 99.8(5) . 2_755 ? C2 N2 H3N 100.5(5) . 2_755 ? N4 N3 Si1 120.64(15) . . ? N4 N3 H3N 115.3(16) . . ? Si1 N3 H3N 123.9(16) . . ? N3 N4 C4 110.58(19) . . ? N3 N4 C5 109.37(18) . . ? C4 N4 C5 110.50(18) . . ? N3 N4 H1N 120.5(5) . 2_765 ? C4 N4 H1N 93.6(5) . 2_765 ? C5 N4 H1N 111.2(5) . 2_765 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.321 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.043 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N N4 0.78(2) 2.60(3) 3.376(4) 172(3) 2_765 N3 H3N N2 0.80(2) 2.51(3) 3.303(4) 169(3) 2_755 _vrf_PLAT771_comp_9 ; PROBLEM: Suspect N-H Bond in CIF: N2 -- H3N .. 2.51 Ang. RESPONSE: discussed N...H contact ; # Attachment 'compound_11.cif' data_comp_11 _database_code_depnum_ccdc_archive 'CCDC 715615' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H36 N10 Si2' _chemical_formula_sum 'C10 H36 N10 Si2' _chemical_formula_weight 352.67 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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.121(5) _cell_length_b 11.644(6) _cell_length_c 16.611(8) _cell_angle_alpha 80.456(9) _cell_angle_beta 89.014(9) _cell_angle_gamma 84.806(9) _cell_volume 2112.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9313 _exptl_absorpt_correction_T_max 0.9928 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16414 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7431 _reflns_number_gt 5367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7431 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.70728(5) 0.61240(5) 0.25284(4) 0.02221(16) Uani 1 1 d . . . H1 H 0.6894(17) 0.7078(16) 0.2878(11) 0.016(5) Uiso 1 1 d . . . Si2 Si 0.82158(6) 0.57511(5) 0.08425(4) 0.02525(17) Uani 1 1 d . . . H2 H 0.8050(18) 0.6274(18) 0.0063(12) 0.027(6) Uiso 1 1 d . . . N1 N 0.74285(15) 0.65476(15) 0.15102(10) 0.0237(4) Uani 1 1 d . . . N2 N 0.67783(17) 0.76796(16) 0.12023(11) 0.0287(4) Uani 1 1 d . . . N3 N 0.82885(18) 0.52008(18) 0.28632(12) 0.0282(5) Uani 1 1 d . . . H3N H 0.883(2) 0.524(2) 0.2618(14) 0.029(8) Uiso 1 1 d . . . N4 N 0.83231(16) 0.43268(16) 0.35720(11) 0.0285(4) Uani 1 1 d . . . N5 N 0.57664(18) 0.54979(18) 0.27394(12) 0.0281(5) Uani 1 1 d . . . H5N H 0.528(2) 0.583(2) 0.2906(14) 0.028(8) Uiso 1 1 d . . . N6 N 0.55769(16) 0.44025(16) 0.25110(11) 0.0293(4) Uani 1 1 d . . . N7 N 0.76494(19) 0.44365(18) 0.10362(13) 0.0332(5) Uani 1 1 d . . . H7N H 0.718(2) 0.425(2) 0.1389(13) 0.023(7) Uiso 1 1 d . . . N8 N 0.79636(17) 0.35830(16) 0.05303(12) 0.0314(5) Uani 1 1 d . . . N9 N 0.97458(18) 0.57047(19) 0.08966(12) 0.0322(5) Uani 1 1 d . . . H9N H 1.018(2) 0.594(2) 0.0503(14) 0.027(7) Uiso 1 1 d . . . N10 N 1.03423(16) 0.54261(17) 0.16652(11) 0.0295(4) Uani 1 1 d . . . C1 C 0.7621(3) 0.8528(2) 0.08944(17) 0.0493(7) Uani 1 1 d . . . H1A H 0.8166 0.8613 0.1334 0.074 Uiso 1 1 calc R . . H1B H 0.7174 0.9284 0.0696 0.074 Uiso 1 1 calc R . . H1C H 0.8091 0.8262 0.0445 0.074 Uiso 1 1 calc R . . C2 C 0.5861(2) 0.7583(2) 0.06074(15) 0.0451(7) Uani 1 1 d . . . H2A H 0.6251 0.7344 0.0121 0.068 Uiso 1 1 calc R . . H2B H 0.5395 0.8342 0.0455 0.068 Uiso 1 1 calc R . . H2C H 0.5319 0.6998 0.0846 0.068 Uiso 1 1 calc R . . C3 C 0.9256(2) 0.4546(2) 0.41154(14) 0.0431(7) Uani 1 1 d . . . H3A H 1.0033 0.4559 0.3827 0.065 Uiso 1 1 calc R . . H3B H 0.9315 0.3926 0.4594 0.065 Uiso 1 1 calc R . . H3C H 0.9050 0.5303 0.4292 0.065 Uiso 1 1 calc R . . C4 C 0.8583(2) 0.3188(2) 0.33312(15) 0.0417(7) Uani 1 1 d . . . H4A H 0.7963 0.3065 0.2950 0.063 Uiso 1 1 calc R . . H4B H 0.8585 0.2580 0.3816 0.063 Uiso 1 1 calc R . . H4C H 0.9376 0.3151 0.3066 0.063 Uiso 1 1 calc R . . C5 C 0.5351(2) 0.3573(2) 0.32392(16) 0.0451(7) Uani 1 1 d . . . H5A H 0.6033 0.3504 0.3615 0.068 Uiso 1 1 calc R . . H5B H 0.5254 0.2808 0.3088 0.068 Uiso 1 1 calc R . . H5C H 0.4612 0.3846 0.3506 0.068 Uiso 1 1 calc R . . C6 C 0.4560(2) 0.4555(2) 0.19534(18) 0.0495(7) Uani 1 1 d . . . H6A H 0.3840 0.4878 0.2216 0.074 Uiso 1 1 calc R . . H6B H 0.4410 0.3796 0.1811 0.074 Uiso 1 1 calc R . . H6C H 0.4744 0.5092 0.1457 0.074 Uiso 1 1 calc R . . C7 C 0.8473(3) 0.2511(2) 0.10208(18) 0.0553(8) Uani 1 1 d . . . H7A H 0.9196 0.2664 0.1300 0.083 Uiso 1 1 calc R . . H7B H 0.8689 0.1927 0.0668 0.083 Uiso 1 1 calc R . . H7C H 0.7877 0.2215 0.1426 0.083 Uiso 1 1 calc R . . C8 C 0.6892(2) 0.3369(3) 0.01124(15) 0.0458(7) Uani 1 1 d . . . H8A H 0.6292 0.3077 0.0515 0.069 Uiso 1 1 calc R . . H8B H 0.7106 0.2787 -0.0242 0.069 Uiso 1 1 calc R . . H8C H 0.6556 0.4099 -0.0219 0.069 Uiso 1 1 calc R . . C9 C 1.1205(2) 0.4412(2) 0.16807(16) 0.0410(6) Uani 1 1 d . . . H9A H 1.0788 0.3750 0.1566 0.061 Uiso 1 1 calc R . . H9B H 1.1582 0.4212 0.2221 0.061 Uiso 1 1 calc R . . H9C H 1.1828 0.4588 0.1266 0.061 Uiso 1 1 calc R . . C10 C 1.0927(2) 0.6425(2) 0.18346(16) 0.0467(7) Uani 1 1 d . . . H10A H 1.1535 0.6628 0.1413 0.070 Uiso 1 1 calc R . . H10B H 1.1319 0.6229 0.2370 0.070 Uiso 1 1 calc R . . H10C H 1.0323 0.7091 0.1835 0.070 Uiso 1 1 calc R . . Si3 Si 0.33043(5) 0.83111(5) 0.24721(3) 0.02246(16) Uani 1 1 d . . . H3 H 0.3514(18) 0.7329(17) 0.2154(11) 0.020(5) Uiso 1 1 d . . . Si4 Si 0.23654(6) 0.87514(5) 0.41890(4) 0.02709(17) Uani 1 1 d . . . H4 H 0.2665(19) 0.8340(18) 0.4969(12) 0.029(6) Uiso 1 1 d . . . N11 N 0.30705(16) 0.79243(15) 0.35124(10) 0.0250(4) Uani 1 1 d . . . N12 N 0.37304(16) 0.67883(15) 0.37984(11) 0.0270(4) Uani 1 1 d . . . N13 N 0.45772(19) 0.89623(17) 0.21728(12) 0.0275(5) Uani 1 1 d . . . H13N H 0.505(2) 0.860(2) 0.2009(15) 0.039(9) Uiso 1 1 d . . . N14 N 0.47898(17) 1.00799(16) 0.23542(11) 0.0301(5) Uani 1 1 d . . . N15 N 0.20355(18) 0.91864(17) 0.21771(12) 0.0270(5) Uani 1 1 d . . . H15N H 0.149(2) 0.912(2) 0.2456(13) 0.023(7) Uiso 1 1 d . . . N16 N 0.19228(16) 1.00133(16) 0.14455(10) 0.0269(4) Uani 1 1 d . . . N17 N 0.08473(19) 0.86695(19) 0.42691(13) 0.0338(5) Uani 1 1 d . . . H17N H 0.051(2) 0.857(2) 0.4681(15) 0.036(8) Uiso 1 1 d . . . N18 N 0.00950(17) 0.89445(17) 0.35702(12) 0.0338(5) Uani 1 1 d . . . N19 N 0.27827(19) 1.01101(18) 0.38664(12) 0.0324(5) Uani 1 1 d . . . H19N H 0.330(2) 1.0280(19) 0.3527(13) 0.024(7) Uiso 1 1 d . . . N20 N 0.24465(17) 1.10053(17) 0.43376(12) 0.0332(5) Uani 1 1 d . . . C11 C 0.2925(2) 0.5964(2) 0.42156(16) 0.0424(7) Uani 1 1 d . . . H11A H 0.3366 0.5190 0.4351 0.064 Uiso 1 1 calc R . . H11B H 0.2244 0.5920 0.3859 0.064 Uiso 1 1 calc R . . H11C H 0.2623 0.6228 0.4718 0.064 Uiso 1 1 calc R . . C12 C 0.4747(2) 0.6901(2) 0.43148(14) 0.0387(6) Uani 1 1 d . . . H12A H 0.4445 0.7177 0.4813 0.058 Uiso 1 1 calc R . . H12B H 0.5270 0.7463 0.4019 0.058 Uiso 1 1 calc R . . H12C H 0.5208 0.6138 0.4459 0.058 Uiso 1 1 calc R . . C13 C 0.5875(2) 0.9970(2) 0.28439(17) 0.0467(7) Uani 1 1 d . . . H13A H 0.5770 0.9431 0.3354 0.070 Uiso 1 1 calc R . . H13B H 0.6026 1.0739 0.2968 0.070 Uiso 1 1 calc R . . H13C H 0.6563 0.9667 0.2540 0.070 Uiso 1 1 calc R . . C14 C 0.4918(2) 1.0880(2) 0.15930(16) 0.0464(7) Uani 1 1 d . . . H14A H 0.5632 1.0612 0.1298 0.070 Uiso 1 1 calc R . . H14B H 0.5009 1.1665 0.1711 0.070 Uiso 1 1 calc R . . H14C H 0.4198 1.0903 0.1256 0.070 Uiso 1 1 calc R . . C15 C 0.1667(2) 1.1174(2) 0.16487(15) 0.0388(6) Uani 1 1 d . . . H15A H 0.0920 1.1204 0.1969 0.058 Uiso 1 1 calc R . . H15B H 0.1573 1.1747 0.1146 0.058 Uiso 1 1 calc R . . H15C H 0.2335 1.1356 0.1969 0.058 Uiso 1 1 calc R . . C16 C 0.0950(2) 0.9736(2) 0.09604(14) 0.0413(6) Uani 1 1 d . . . H16A H 0.1140 0.8956 0.0818 0.062 Uiso 1 1 calc R . . H16B H 0.0855 1.0315 0.0460 0.062 Uiso 1 1 calc R . . H16C H 0.0197 0.9749 0.1276 0.062 Uiso 1 1 calc R . . C17 C -0.0642(3) 0.7987(3) 0.35264(18) 0.0534(8) Uani 1 1 d . . . H17A H -0.0118 0.7265 0.3520 0.080 Uiso 1 1 calc R . . H17B H -0.1127 0.8164 0.3027 0.080 Uiso 1 1 calc R . . H17C H -0.1178 0.7886 0.4003 0.080 Uiso 1 1 calc R . . C18 C -0.0662(2) 1.0025(2) 0.35948(18) 0.0492(7) Uani 1 1 d . . . H18A H -0.1179 0.9929 0.4081 0.074 Uiso 1 1 calc R . . H18B H -0.1167 1.0211 0.3105 0.074 Uiso 1 1 calc R . . H18C H -0.0151 1.0662 0.3616 0.074 Uiso 1 1 calc R . . C19 C 0.3472(2) 1.1195(3) 0.48126(16) 0.0497(7) Uani 1 1 d . . . H19A H 0.3743 1.0466 0.5173 0.075 Uiso 1 1 calc R . . H19B H 0.3235 1.1803 0.5142 0.075 Uiso 1 1 calc R . . H19C H 0.4132 1.1442 0.4444 0.075 Uiso 1 1 calc R . . C20 C 0.2044(3) 1.2075(2) 0.38034(18) 0.0523(8) Uani 1 1 d . . . H20A H 0.2710 1.2336 0.3445 0.078 Uiso 1 1 calc R . . H20B H 0.1780 1.2679 0.4131 0.078 Uiso 1 1 calc R . . H20C H 0.1368 1.1936 0.3472 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0164(3) 0.0223(3) 0.0273(3) -0.0027(3) -0.0016(2) -0.0004(2) Si2 0.0222(3) 0.0251(3) 0.0281(3) -0.0046(3) -0.0004(3) -0.0002(3) N1 0.0206(10) 0.0205(10) 0.0284(10) -0.0016(8) -0.0036(8) 0.0032(8) N2 0.0268(11) 0.0236(10) 0.0324(10) 0.0017(8) 0.0003(8) 0.0039(8) N3 0.0164(11) 0.0352(12) 0.0284(11) 0.0061(9) 0.0045(9) 0.0007(9) N4 0.0203(10) 0.0337(11) 0.0277(10) 0.0049(8) -0.0019(8) 0.0005(8) N5 0.0179(11) 0.0266(11) 0.0405(12) -0.0093(9) 0.0029(9) 0.0009(9) N6 0.0239(10) 0.0230(10) 0.0409(11) -0.0046(8) -0.0020(9) -0.0023(8) N7 0.0304(12) 0.0310(12) 0.0413(12) -0.0141(10) 0.0112(10) -0.0069(9) N8 0.0258(11) 0.0303(11) 0.0414(12) -0.0142(9) -0.0022(9) -0.0039(9) N9 0.0215(11) 0.0465(13) 0.0294(11) -0.0068(10) 0.0056(9) -0.0074(9) N10 0.0212(10) 0.0353(11) 0.0341(11) -0.0096(9) 0.0014(8) -0.0061(9) C1 0.0559(19) 0.0273(14) 0.0609(18) 0.0003(13) 0.0209(15) -0.0009(13) C2 0.0448(16) 0.0502(17) 0.0358(14) -0.0047(12) -0.0134(12) 0.0177(13) C3 0.0299(14) 0.0574(18) 0.0377(14) 0.0052(12) -0.0083(11) -0.0034(13) C4 0.0378(15) 0.0322(14) 0.0491(15) 0.0041(12) 0.0039(12) 0.0081(12) C5 0.0434(16) 0.0303(14) 0.0582(17) 0.0009(12) 0.0160(13) -0.0029(12) C6 0.0321(15) 0.0436(17) 0.077(2) -0.0203(15) -0.0153(14) -0.0053(13) C7 0.0493(18) 0.0384(17) 0.078(2) -0.0140(15) -0.0178(16) 0.0091(14) C8 0.0363(15) 0.0607(19) 0.0437(15) -0.0112(13) -0.0066(12) -0.0156(13) C9 0.0286(14) 0.0445(16) 0.0495(16) -0.0089(13) -0.0005(12) 0.0007(12) C10 0.0441(17) 0.0520(18) 0.0519(17) -0.0239(14) 0.0074(13) -0.0198(14) Si3 0.0192(3) 0.0218(3) 0.0255(3) -0.0026(2) -0.0021(2) 0.0013(3) Si4 0.0248(4) 0.0278(4) 0.0282(3) -0.0043(3) 0.0005(3) -0.0008(3) N11 0.0222(10) 0.0217(10) 0.0288(10) 0.0000(8) -0.0021(8) 0.0025(8) N12 0.0257(10) 0.0227(10) 0.0297(10) 0.0018(8) -0.0029(8) 0.0027(8) N13 0.0235(11) 0.0227(11) 0.0367(12) -0.0080(9) 0.0028(9) 0.0013(9) N14 0.0251(11) 0.0245(10) 0.0402(11) -0.0040(9) 0.0010(9) -0.0020(8) N15 0.0186(11) 0.0313(12) 0.0274(11) 0.0040(9) 0.0014(9) 0.0018(9) N16 0.0245(10) 0.0266(10) 0.0273(10) 0.0013(8) -0.0052(8) 0.0005(8) N17 0.0281(12) 0.0417(13) 0.0320(12) -0.0068(10) 0.0069(10) -0.0056(10) N18 0.0233(11) 0.0375(12) 0.0424(12) -0.0113(9) 0.0023(9) -0.0042(9) N19 0.0324(12) 0.0330(12) 0.0340(11) -0.0109(9) 0.0092(10) -0.0070(9) N20 0.0281(11) 0.0307(11) 0.0437(12) -0.0138(9) -0.0030(9) -0.0032(9) C11 0.0427(16) 0.0288(14) 0.0514(16) 0.0052(12) 0.0058(13) -0.0032(12) C12 0.0298(14) 0.0485(16) 0.0345(13) -0.0029(12) -0.0091(11) 0.0083(12) C13 0.0364(15) 0.0420(16) 0.0652(18) -0.0157(14) -0.0110(14) -0.0076(13) C14 0.0473(17) 0.0295(14) 0.0580(17) 0.0038(13) 0.0121(14) -0.0021(12) C15 0.0397(15) 0.0287(14) 0.0450(15) -0.0007(11) -0.0051(12) 0.0036(11) C16 0.0370(15) 0.0479(16) 0.0372(14) 0.0025(12) -0.0147(12) -0.0095(12) C17 0.0426(17) 0.0573(19) 0.070(2) -0.0309(16) 0.0130(15) -0.0229(15) C18 0.0343(16) 0.0457(17) 0.0665(19) -0.0098(14) -0.0005(14) 0.0036(13) C19 0.0466(17) 0.0592(19) 0.0489(16) -0.0220(14) -0.0095(14) -0.0088(15) C20 0.0426(17) 0.0341(16) 0.081(2) -0.0120(14) -0.0153(15) 0.0013(13) _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 N5 1.690(2) . ? Si1 N3 1.690(2) . ? Si1 N1 1.7309(19) . ? Si1 H1 1.334(19) . ? Si2 N7 1.687(2) . ? Si2 N9 1.701(2) . ? Si2 N1 1.7372(19) . ? Si2 H2 1.344(19) . ? N1 N2 1.462(2) . ? N2 C1 1.449(3) . ? N2 C2 1.457(3) . ? N3 N4 1.421(3) . ? N3 H3N 0.72(2) . ? N4 C4 1.450(3) . ? N4 C3 1.454(3) . ? N5 N6 1.424(3) . ? N5 H5N 0.72(2) . ? N6 C5 1.451(3) . ? N6 C6 1.454(3) . ? N7 N8 1.421(3) . ? N7 H7N 0.80(2) . ? N8 C7 1.447(3) . ? N8 C8 1.450(3) . ? N9 N10 1.424(3) . ? N9 H9N 0.83(2) . ? N10 C9 1.449(3) . ? N10 C10 1.451(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? Si3 N15 1.693(2) . ? Si3 N13 1.694(2) . ? Si3 N11 1.733(2) . ? Si3 H3 1.34(2) . ? Si4 N19 1.688(2) . ? Si4 N17 1.701(2) . ? Si4 N11 1.7313(19) . ? Si4 H4 1.342(19) . ? N11 N12 1.464(2) . ? N12 C11 1.455(3) . ? N12 C12 1.459(3) . ? N13 N14 1.424(3) . ? N13 H13N 0.72(3) . ? N14 C13 1.451(3) . ? N14 C14 1.454(3) . ? N15 N16 1.420(2) . ? N15 H15N 0.76(2) . ? N16 C15 1.449(3) . ? N16 C16 1.450(3) . ? N17 N18 1.418(3) . ? N17 H17N 0.77(2) . ? N18 C17 1.454(3) . ? N18 C18 1.455(3) . ? N19 N20 1.425(3) . ? N19 H19N 0.81(2) . ? N20 C20 1.444(3) . ? N20 C19 1.451(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 N5 Si1 N3 111.98(11) . . ? N5 Si1 N1 117.28(9) . . ? N3 Si1 N1 101.89(10) . . ? N5 Si1 H1 102.1(8) . . ? N3 Si1 H1 115.6(8) . . ? N1 Si1 H1 108.6(8) . . ? N7 Si2 N9 114.93(11) . . ? N7 Si2 N1 103.65(10) . . ? N9 Si2 N1 115.20(10) . . ? N7 Si2 H2 112.5(8) . . ? N9 Si2 H2 99.7(9) . . ? N1 Si2 H2 111.2(9) . . ? N2 N1 Si1 109.63(13) . . ? N2 N1 Si2 120.27(13) . . ? Si1 N1 Si2 129.36(10) . . ? C1 N2 C2 112.9(2) . . ? C1 N2 N1 110.34(18) . . ? C2 N2 N1 111.92(18) . . ? N4 N3 Si1 125.54(16) . . ? N4 N3 H3N 117(2) . . ? Si1 N3 H3N 117(2) . . ? N3 N4 C4 109.04(18) . . ? N3 N4 C3 108.83(18) . . ? C4 N4 C3 110.44(19) . . ? N6 N5 Si1 121.72(16) . . ? N6 N5 H5N 120(2) . . ? Si1 N5 H5N 118(2) . . ? N5 N6 C5 109.11(19) . . ? N5 N6 C6 109.37(18) . . ? C5 N6 C6 110.7(2) . . ? N8 N7 Si2 120.31(17) . . ? N8 N7 H7N 114.7(17) . . ? Si2 N7 H7N 125.0(17) . . ? N7 N8 C7 109.9(2) . . ? N7 N8 C8 109.16(19) . . ? C7 N8 C8 110.1(2) . . ? N10 N9 Si2 120.52(15) . . ? N10 N9 H9N 115.5(16) . . ? Si2 N9 H9N 123.2(16) . . ? N9 N10 C9 110.51(18) . . ? N9 N10 C10 110.17(19) . . ? C9 N10 C10 111.1(2) . . ? N2 C1 H1A 109.5 . . ? N2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N4 C3 H3A 109.5 . . ? N4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N6 C5 H5A 109.5 . . ? N6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N6 C6 H6A 109.5 . . ? N6 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N6 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N8 C7 H7A 109.5 . . ? N8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N8 C8 H8A 109.5 . . ? N8 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N8 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N10 C9 H9A 109.5 . . ? N10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N10 C10 H10A 109.5 . . ? N10 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N10 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N15 Si3 N13 112.39(11) . . ? N15 Si3 N11 102.12(10) . . ? N13 Si3 N11 117.27(10) . . ? N15 Si3 H3 117.7(8) . . ? N13 Si3 H3 100.0(8) . . ? N11 Si3 H3 108.1(8) . . ? N19 Si4 N17 114.52(11) . . ? N19 Si4 N11 104.08(10) . . ? N17 Si4 N11 114.26(10) . . ? N19 Si4 H4 112.9(9) . . ? N17 Si4 H4 98.6(9) . . ? N11 Si4 H4 112.9(9) . . ? N12 N11 Si4 121.41(13) . . ? N12 N11 Si3 109.15(13) . . ? Si4 N11 Si3 128.92(11) . . ? C11 N12 C12 111.37(19) . . ? C11 N12 N11 110.87(18) . . ? C12 N12 N11 111.40(18) . . ? N14 N13 Si3 122.33(16) . . ? N14 N13 H13N 121(2) . . ? Si3 N13 H13N 115(2) . . ? N13 N14 C13 109.28(18) . . ? N13 N14 C14 108.92(19) . . ? C13 N14 C14 110.7(2) . . ? N16 N15 Si3 124.63(16) . . ? N16 N15 H15N 118.2(17) . . ? Si3 N15 H15N 117.1(17) . . ? N15 N16 C15 109.11(17) . . ? N15 N16 C16 109.11(18) . . ? C15 N16 C16 110.20(19) . . ? N18 N17 Si4 121.01(16) . . ? N18 N17 H17N 115.3(19) . . ? Si4 N17 H17N 123.1(19) . . ? N17 N18 C17 109.9(2) . . ? N17 N18 C18 110.32(19) . . ? C17 N18 C18 110.6(2) . . ? N20 N19 Si4 119.08(16) . . ? N20 N19 H19N 113.5(16) . . ? Si4 N19 H19N 125.6(16) . . ? N19 N20 C20 109.73(19) . . ? N19 N20 C19 109.68(19) . . ? C20 N20 C19 109.8(2) . . ? N12 C11 H11A 109.5 . . ? N12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N12 C12 H12A 109.5 . . ? N12 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N12 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N14 C13 H13A 109.5 . . ? N14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N14 C14 H14A 109.5 . . ? N14 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N14 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N16 C15 H15A 109.5 . . ? N16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N16 C16 H16A 109.5 . . ? N16 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N16 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N18 C17 H17A 109.5 . . ? N18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N18 C18 H18A 109.5 . . ? N18 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N18 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N20 C19 H19A 109.5 . . ? N20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N20 C20 H20A 109.5 . . ? N20 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N20 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 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 N5 Si1 N1 N2 81.33(16) . . . . ? N3 Si1 N1 N2 -156.06(14) . . . . ? N5 Si1 N1 Si2 -88.70(16) . . . . ? N3 Si1 N1 Si2 33.91(16) . . . . ? N7 Si2 N1 N2 -125.64(16) . . . . ? N9 Si2 N1 N2 107.95(16) . . . . ? N7 Si2 N1 Si1 43.47(16) . . . . ? N9 Si2 N1 Si1 -82.94(16) . . . . ? Si1 N1 N2 C1 121.51(17) . . . . ? Si2 N1 N2 C1 -67.4(2) . . . . ? Si1 N1 N2 C2 -111.85(18) . . . . ? Si2 N1 N2 C2 59.2(2) . . . . ? N5 Si1 N3 N4 -32.9(2) . . . . ? N1 Si1 N3 N4 -159.05(19) . . . . ? Si1 N3 N4 C4 117.8(2) . . . . ? Si1 N3 N4 C3 -121.6(2) . . . . ? N3 Si1 N5 N6 -52.6(2) . . . . ? N1 Si1 N5 N6 64.64(19) . . . . ? Si1 N5 N6 C5 119.88(19) . . . . ? Si1 N5 N6 C6 -118.9(2) . . . . ? N9 Si2 N7 N8 -61.6(2) . . . . ? N1 Si2 N7 N8 171.83(16) . . . . ? Si2 N7 N8 C7 124.1(2) . . . . ? Si2 N7 N8 C8 -115.1(2) . . . . ? N7 Si2 N9 N10 -72.0(2) . . . . ? N1 Si2 N9 N10 48.4(2) . . . . ? Si2 N9 N10 C9 122.11(19) . . . . ? Si2 N9 N10 C10 -114.8(2) . . . . ? N19 Si4 N11 N12 133.40(16) . . . . ? N17 Si4 N11 N12 -100.99(17) . . . . ? N19 Si4 N11 Si3 -37.43(16) . . . . ? N17 Si4 N11 Si3 88.18(16) . . . . ? N15 Si3 N11 N12 152.97(14) . . . . ? N13 Si3 N11 N12 -83.74(16) . . . . ? N15 Si3 N11 Si4 -35.31(16) . . . . ? N13 Si3 N11 Si4 87.98(16) . . . . ? Si4 N11 N12 C11 62.7(2) . . . . ? Si3 N11 N12 C11 -124.81(17) . . . . ? Si4 N11 N12 C12 -61.9(2) . . . . ? Si3 N11 N12 C12 110.55(17) . . . . ? N15 Si3 N13 N14 53.2(2) . . . . ? N11 Si3 N13 N14 -64.65(19) . . . . ? Si3 N13 N14 C13 119.4(2) . . . . ? Si3 N13 N14 C14 -119.55(19) . . . . ? N13 Si3 N15 N16 33.2(2) . . . . ? N11 Si3 N15 N16 159.72(17) . . . . ? Si3 N15 N16 C15 -118.1(2) . . . . ? Si3 N15 N16 C16 121.4(2) . . . . ? N19 Si4 N17 N18 64.2(2) . . . . ? N11 Si4 N17 N18 -55.7(2) . . . . ? Si4 N17 N18 C17 127.03(19) . . . . ? Si4 N17 N18 C18 -110.7(2) . . . . ? N17 Si4 N19 N20 60.3(2) . . . . ? N11 Si4 N19 N20 -174.29(16) . . . . ? Si4 N19 N20 C20 -137.57(19) . . . . ? Si4 N19 N20 C19 101.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.514 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.050 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3N N10 0.72(2) 2.29(2) 3.004(3) 171(2) 1_555 N5 H5N N12 0.72(2) 2.55(2) 3.256(3) 168(2) 1_555 N7 H7N N6 0.80(2) 2.57(2) 3.332(3) 161(2) 1_555 N13 H13N N2 0.72(2) 2.58(2) 3.290(3) 168(2) 1_555 N15 H15N N18 0.76(2) 2.39(2) 3.133(3) 166(2) 1_555 N19 H19N N14 0.81(2) 2.56(2) 3.334(3) 159(2) 1_555 _vrf_PLAT222_comp_11 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.19 Ratio RESPONSE: Hydrogens bonded to nitrogen were refined isotropically with a small Ueq, hydrogens bonded to carbons were included at calculated positions with Ueq = 1.5 times of the corresponding carbon. ; _vrf_PLAT374_comp_11 ; PROBLEM: Long N - N Bond N1 - N2 ... 1.46 Ang. RESPONSE: discussed in the paper (The doubly silicon-bonded atom N(1)...) ; # Attachment 'compound_12.cif' data_comp_12 _database_code_depnum_ccdc_archive 'CCDC 715616' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H28 N8 Si' _chemical_formula_sum 'C8 H28 N8 Si' _chemical_formula_weight 264.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M P2/c _symmetry_space_group_name_Hall '-P 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.998(5) _cell_length_b 5.0153(13) _cell_length_c 18.163(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.464(5) _cell_angle_gamma 90.00 _cell_volume 1545.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9552 _exptl_absorpt_correction_T_max 0.9941 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.752910 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11890 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2863 _reflns_number_gt 1974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2863 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.5000 0.56959(19) 0.7500 0.0175(2) Uani 1 2 d S . . N1 N 0.57072(12) 0.7894(4) 0.80090(12) 0.0208(5) Uani 1 1 d . . . H1N H 0.5592(14) 0.917(5) 0.8239(15) 0.016(7) Uiso 1 1 d . . . N2 N 0.64927(11) 0.7007(4) 0.84200(12) 0.0239(5) Uani 1 1 d . . . N3 N 0.52912(13) 0.3519(5) 0.69319(13) 0.0212(5) Uani 1 1 d . . . H3N H 0.5517(14) 0.240(5) 0.7128(14) 0.006(7) Uiso 1 1 d . . . N4 N 0.54403(12) 0.4373(4) 0.62469(12) 0.0228(5) Uani 1 1 d . . . C1 C 0.65888(17) 0.6486(6) 0.92290(16) 0.0393(8) Uani 1 1 d . . . H1A H 0.6510 0.8105 0.9475 0.059 Uiso 1 1 calc R . . H1B H 0.7111 0.5825 0.9492 0.059 Uiso 1 1 calc R . . H1C H 0.6210 0.5179 0.9258 0.059 Uiso 1 1 calc R . . C2 C 0.70303(15) 0.9089(6) 0.83656(18) 0.0339(7) Uani 1 1 d . . . H2A H 0.6979 0.9367 0.7828 0.051 Uiso 1 1 calc R . . H2B H 0.7561 0.8568 0.8653 0.051 Uiso 1 1 calc R . . H2C H 0.6907 1.0712 0.8580 0.051 Uiso 1 1 calc R . . C3 C 0.62726(16) 0.4973(6) 0.64224(17) 0.0363(7) Uani 1 1 d . . . H3A H 0.6425 0.6363 0.6807 0.054 Uiso 1 1 calc R . . H3B H 0.6363 0.5549 0.5955 0.054 Uiso 1 1 calc R . . H3C H 0.6579 0.3403 0.6621 0.054 Uiso 1 1 calc R . . C4 C 0.52085(17) 0.2261(6) 0.56728(15) 0.0311(7) Uani 1 1 d . . . H4A H 0.5501 0.0674 0.5882 0.047 Uiso 1 1 calc R . . H4B H 0.5315 0.2793 0.5210 0.047 Uiso 1 1 calc R . . H4C H 0.4655 0.1914 0.5545 0.047 Uiso 1 1 calc R . . Si2 Si 1.0000 0.6784(2) 0.7500 0.0186(3) Uani 1 2 d S . . N5 N 1.04712(12) 0.4566(4) 0.70958(13) 0.0209(5) Uani 1 1 d . . . H5N H 1.0222(15) 0.325(5) 0.6875(15) 0.019(7) Uiso 1 1 d . . . N6 N 1.10598(12) 0.5411(4) 0.67782(13) 0.0246(5) Uani 1 1 d . . . N7 N 0.93920(12) 0.8974(5) 0.68582(13) 0.0222(5) Uani 1 1 d . . . H7N H 0.9262(16) 1.027(5) 0.7038(16) 0.023(8) Uiso 1 1 d . . . N8 N 0.88359(12) 0.8025(5) 0.61469(12) 0.0279(5) Uani 1 1 d . . . C5 C 1.16591(16) 0.3352(6) 0.69393(17) 0.0351(7) Uani 1 1 d . . . H5A H 1.1888 0.3105 0.7493 0.053 Uiso 1 1 calc R . . H5B H 1.2062 0.3877 0.6730 0.053 Uiso 1 1 calc R . . H5C H 1.1424 0.1711 0.6701 0.053 Uiso 1 1 calc R . . C6 C 1.07149(17) 0.5792(7) 0.59457(16) 0.0395(8) Uani 1 1 d . . . H6A H 1.0466 0.4168 0.5707 0.059 Uiso 1 1 calc R . . H6B H 1.1120 0.6268 0.5734 0.059 Uiso 1 1 calc R . . H6C H 1.0330 0.7192 0.5842 0.059 Uiso 1 1 calc R . . C7 C 0.80653(16) 0.7699(7) 0.62383(19) 0.0456(8) Uani 1 1 d . . . H7A H 0.8111 0.6511 0.6665 0.068 Uiso 1 1 calc R . . H7B H 0.7701 0.6971 0.5767 0.068 Uiso 1 1 calc R . . H7C H 0.7877 0.9401 0.6342 0.068 Uiso 1 1 calc R . . C8 C 0.87853(19) 0.9917(7) 0.55349(17) 0.0433(8) Uani 1 1 d . . . H8A H 0.8621 1.1616 0.5670 0.065 Uiso 1 1 calc R . . H8B H 0.8409 0.9301 0.5055 0.065 Uiso 1 1 calc R . . H8C H 0.9292 1.0093 0.5472 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0135(5) 0.0198(5) 0.0184(5) 0.000 0.0042(4) 0.000 N1 0.0140(11) 0.0224(12) 0.0238(12) -0.0037(10) 0.0033(9) 0.0026(9) N2 0.0118(10) 0.0251(12) 0.0301(12) 0.0019(10) 0.0006(9) -0.0003(9) N3 0.0203(12) 0.0199(13) 0.0217(12) 0.0048(10) 0.0047(9) 0.0056(10) N4 0.0203(11) 0.0282(12) 0.0214(11) -0.0016(10) 0.0092(9) -0.0024(9) C1 0.0280(16) 0.048(2) 0.0321(16) 0.0073(14) -0.0029(13) -0.0033(14) C2 0.0170(14) 0.0331(16) 0.0461(18) 0.0000(14) 0.0035(12) -0.0057(12) C3 0.0246(15) 0.0500(19) 0.0377(17) -0.0017(15) 0.0151(13) -0.0060(14) C4 0.0356(17) 0.0350(17) 0.0242(14) -0.0011(13) 0.0120(12) 0.0005(13) Si2 0.0133(5) 0.0200(5) 0.0213(5) 0.000 0.0042(4) 0.000 N5 0.0163(11) 0.0208(12) 0.0268(12) -0.0033(10) 0.0087(9) -0.0046(9) N6 0.0182(11) 0.0296(13) 0.0292(12) 0.0024(10) 0.0120(9) 0.0013(9) N7 0.0185(12) 0.0209(13) 0.0227(12) -0.0022(10) 0.0008(9) 0.0009(9) N8 0.0204(12) 0.0330(13) 0.0239(12) -0.0009(10) -0.0010(9) -0.0010(10) C5 0.0251(15) 0.0388(18) 0.0458(18) -0.0004(15) 0.0176(13) 0.0051(13) C6 0.0356(17) 0.054(2) 0.0322(16) 0.0049(15) 0.0157(14) 0.0016(15) C7 0.0185(15) 0.066(2) 0.0439(18) -0.0005(17) -0.0009(13) -0.0097(15) C8 0.0377(18) 0.058(2) 0.0294(16) 0.0102(15) 0.0048(13) 0.0099(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 Si1 N3 1.700(2) . ? Si1 N3 1.700(2) 2_656 ? Si1 N1 1.705(2) . ? Si1 N1 1.705(2) 2_656 ? N1 N2 1.432(3) . ? N1 H1N 0.83(3) . ? N2 C1 1.445(4) . ? N2 C2 1.449(3) . ? N3 N4 1.423(3) . ? N3 H3N 0.72(2) . ? N4 C4 1.447(3) . ? N4 C3 1.455(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? Si2 N5 1.706(2) . ? Si2 N5 1.706(2) 2_756 ? Si2 N7 1.707(2) 2_756 ? Si2 N7 1.707(2) . ? N5 N6 1.429(3) . ? N5 H5N 0.82(3) . ? N6 C6 1.443(4) . ? N6 C5 1.451(3) . ? N7 N8 1.427(3) . ? N7 H7N 0.80(3) . ? N8 C8 1.441(3) . ? N8 C7 1.460(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Si1 N3 100.12(16) . 2_656 ? N3 Si1 N1 114.76(11) . . ? N3 Si1 N1 114.30(11) 2_656 . ? N3 Si1 N1 114.30(11) . 2_656 ? N3 Si1 N1 114.76(11) 2_656 2_656 ? N1 Si1 N1 99.41(15) . 2_656 ? N2 N1 Si1 120.73(17) . . ? N2 N1 H1N 110.3(18) . . ? Si1 N1 H1N 120.4(18) . . ? N1 N2 C1 110.4(2) . . ? N1 N2 C2 107.8(2) . . ? C1 N2 C2 110.1(2) . . ? N4 N3 Si1 121.56(18) . . ? N4 N3 H3N 115(2) . . ? Si1 N3 H3N 116(2) . . ? N3 N4 C4 108.5(2) . . ? N3 N4 C3 110.5(2) . . ? C4 N4 C3 109.8(2) . . ? N2 C1 H1A 109.5 . . ? N2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N4 C3 H3A 109.5 . . ? N4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N5 Si2 N5 98.62(16) . 2_756 ? N5 Si2 N7 114.59(11) . 2_756 ? N5 Si2 N7 115.04(11) 2_756 2_756 ? N5 Si2 N7 115.04(11) . . ? N5 Si2 N7 114.59(11) 2_756 . ? N7 Si2 N7 99.87(16) 2_756 . ? N6 N5 Si2 121.48(17) . . ? N6 N5 H5N 113.4(18) . . ? Si2 N5 H5N 117.7(18) . . ? N5 N6 C6 110.1(2) . . ? N5 N6 C5 108.0(2) . . ? C6 N6 C5 109.7(2) . . ? N8 N7 Si2 120.03(18) . . ? N8 N7 H7N 115(2) . . ? Si2 N7 H7N 117(2) . . ? N7 N8 C8 108.9(2) . . ? N7 N8 C7 109.9(2) . . ? C8 N8 C7 110.1(2) . . ? N6 C5 H5A 109.5 . . ? N6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N6 C6 H6A 109.5 . . ? N6 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N6 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N8 C7 H7A 109.5 . . ? N8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N8 C8 H8A 109.5 . . ? N8 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N8 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.472 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.056 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N N3 0.83(2) 2.66(3) 3.366(3) 145(2) 2_666 N5 H5N N7 0.82(2) 2.61(3) 3.356(3) 152(2) 1_545 N7 H7N N5 0.80(3) 2.62(3) 3.350(3) 154(3) 2_766 _vrf_PLAT222_comp_12 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.19 Ratio RESPONSE: Hydrogens bonded to nitrogen were refined isotropically with a small Ueq, hydrogens bonded to carbons were included at calculated positions with Ueq = 1.5 times of the corresponding carbon. ;