#------------------------------------------------------------------------------ #$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $ #$Revision: 201982 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/32/35/4323595.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4323595 loop_ _publ_author_name 'Norbert W. Mitzel' 'Hubert Schmidbaur' 'David W. H. Rankin' 'Bruce A. Smart' 'Matthias Hofmann' 'Paul von Ragu\'e Schleyer' _publ_section_title ; Synthesis of Volatile Cyclic Silylamines and the Molecular Structures of Two 1-Aza-2,5-disilacyclopentane Derivatives ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 4360 _journal_page_last 4368 _journal_paper_doi 10.1021/ic9703179 _journal_volume 36 _journal_year 1997 _chemical_formula_sum 'C4 H14 N2 Si2' _chemical_formula_weight 146.35 _chemical_melting_point 160 _chemical_name_systematic ; N-(Dimethylamino)-2,5-disilapyrrolidine ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 95.20(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.050(3) _cell_length_b 8.547(4) _cell_length_c 9.878(3) _cell_measurement_reflns_used 44 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 16 _cell_measurement_theta_min 14 _cell_volume 845.0(5) _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 113(2) _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 2693 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_min 3.13 _diffrn_standards_decay_% None _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.338 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_type Psi-scans _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.150 _exptl_crystal_description Cylinder _exptl_crystal_F_000 320 _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _refine_diff_density_max 0.447 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.071 _refine_ls_extinction_coef 0.1401(75) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.029 _refine_ls_goodness_of_fit_obs 1.075 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 130 _refine_ls_number_reflns 2466 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_restrained_S_obs 1.075 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_obs 0.0390 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0987 _refine_ls_wR_factor_obs 0.0890 _reflns_number_observed 1888 _reflns_number_total 2467 _reflns_observed_criterion >2sigma(I) _cod_data_source_file ic9703179.cif _cod_data_source_block si2hyd _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 4323595 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 0.0159(2) 0.0168(2) 0.0173(2) -0.0020(2) -0.0009(2) 0.0013(2) Si2 0.0165(2) 0.0202(2) 0.0227(3) -0.0021(2) -0.0026(2) 0.0010(2) N1 0.0179(6) 0.0129(6) 0.0196(7) -0.0005(5) -0.0003(5) 0.0010(5) N2 0.0210(7) 0.0137(6) 0.0181(7) 0.0003(5) 0.0023(5) -0.0007(5) C2 0.0206(8) 0.0196(8) 0.0249(9) -0.0016(6) 0.0002(7) 0.0054(6) C1 0.0214(8) 0.0176(8) 0.0253(9) -0.0016(6) -0.0005(7) -0.0012(6) C3 0.0308(10) 0.0221(9) 0.0233(9) 0.0030(7) 0.0087(8) -0.0008(7) C4 0.0331(10) 0.0194(8) 0.0200(9) -0.0032(6) 0.0048(7) 0.0020(7) 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Si1 Si 0.60060(4) 0.21491(5) 0.29248(5) 0.01680(14) Uani 1 d . . Si2 Si 0.87316(5) 0.24778(6) 0.42352(5) 0.02009(14) Uani 1 d . . N1 N 0.72985(13) 0.3382(2) 0.35051(14) 0.0169(3) Uani 1 d . . N2 N 0.70073(14) 0.5041(2) 0.33556(14) 0.0176(3) Uani 1 d . . C2 C 0.8301(2) 0.0421(2) 0.3696(2) 0.0218(3) Uani 1 d . . C1 C 0.6758(2) 0.0255(2) 0.3563(2) 0.0216(3) Uani 1 d . . C3 C 0.7980(2) 0.5784(2) 0.2559(2) 0.0251(4) Uani 1 d . . C4 C 0.7027(2) 0.5759(2) 0.4693(2) 0.0240(4) Uani 1 d . . H11 H 0.4838(21) 0.2526(23) 0.3498(22) 0.023(5) Uiso 1 d . . H12 H 0.5790(22) 0.2255(23) 0.1494(23) 0.024(5) Uiso 1 d . . H21 H 0.9882(19) 0.2998(23) 0.3707(20) 0.017(5) Uiso 1 d . . H22 H 0.8946(23) 0.2661(25) 0.5684(24) 0.032(6) Uiso 1 d . . H11C H 0.6458(23) 0.0025(27) 0.4378(24) 0.031(6) Uiso 1 d . . H12C H 0.6498(22) -0.0614(26) 0.3066(22) 0.027(6) Uiso 1 d . . H21C H 0.8648(24) 0.0257(28) 0.2829(25) 0.038(6) Uiso 1 d . . H22C H 0.8771(24) -0.0385(28) 0.4269(24) 0.038(7) Uiso 1 d . . H31C H 0.8885(23) 0.5693(25) 0.3014(22) 0.027(6) Uiso 1 d . . H32C H 0.7723(20) 0.6894(25) 0.2432(22) 0.021(5) Uiso 1 d . . H33C H 0.8032(27) 0.5281(30) 0.1741(27) 0.046(7) Uiso 1 d . . H41C H 0.7906(23) 0.5677(26) 0.5198(23) 0.031(6) Uiso 1 d . . H42C H 0.6354(22) 0.5261(25) 0.5182(23) 0.026(5) Uiso 1 d . . H43C H 0.6809(23) 0.6881(28) 0.4560(24) 0.033(6) Uiso 1 d . . 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' 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 C1 98.49(8) . . ? N1 Si1 H11 111.2(8) . . ? C1 Si1 H11 113.2(8) . . ? N1 Si1 H12 109.6(9) . . ? C1 Si1 H12 114.4(8) . . ? H11 Si1 H12 109.5(12) . . ? N1 Si2 C2 97.94(8) . . ? N1 Si2 H21 113.0(8) . . ? C2 Si2 H21 111.9(8) . . ? N1 Si2 H22 114.2(9) . . ? C2 Si2 H22 113.3(8) . . ? H21 Si2 H22 106.6(12) . . ? N2 N1 Si1 115.01(10) . . ? N2 N1 Si2 129.05(11) . . ? Si1 N1 Si2 115.90(8) . . ? N1 N2 C3 110.01(13) . . ? N1 N2 C4 109.46(13) . . ? C3 N2 C4 110.61(15) . . ? C1 C2 Si2 108.25(11) . . ? C1 C2 H21C 110.6(15) . . ? Si2 C2 H21C 107.2(14) . . ? C1 C2 H22C 114.1(14) . . ? Si2 C2 H22C 114.0(14) . . ? H21C C2 H22C 102.5(19) . . ? C2 C1 Si1 108.61(12) . . ? C2 C1 H11C 110.8(15) . . ? Si1 C1 H11C 109.3(15) . . ? C2 C1 H12C 110.7(14) . . ? Si1 C1 H12C 115.7(14) . . ? H11C C1 H12C 101.5(19) . . ? N2 C3 H31C 111.0(13) . . ? N2 C3 H32C 108.0(12) . . ? H31C C3 H32C 110.8(17) . . ? N2 C3 H33C 111.4(16) . . ? H31C C3 H33C 104.0(21) . . ? H32C C3 H33C 111.8(20) . . ? N2 C4 H41C 111.8(13) . . ? N2 C4 H42C 108.4(13) . . ? H41C C4 H42C 110.8(19) . . ? N2 C4 H43C 107.7(14) . . ? H41C C4 H43C 108.4(18) . . ? H42C C4 H43C 109.7(18) . . ? 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 1.7298(15) . ? Si1 C1 1.872(2) . ? Si1 H11 1.39(2) . ? Si1 H12 1.41(2) . ? Si2 N1 1.7332(15) . ? Si2 C2 1.876(2) . ? Si2 H21 1.38(2) . ? Si2 H22 1.44(2) . ? N1 N2 1.452(2) . ? N2 C3 1.455(2) . ? N2 C4 1.455(2) . ? C2 C1 1.551(3) . ? C2 H21C 0.96(2) . ? C2 H22C 0.98(2) . ? C1 H11C 0.91(2) . ? C1 H12C 0.91(2) . ? C3 H31C 0.98(2) . ? C3 H32C 0.99(2) . ? C3 H33C 0.92(3) . ? C4 H41C 0.98(2) . ? C4 H42C 0.97(2) . ? C4 H43C 0.99(2) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Si1 N1 N2 -172.06(11) . . . . ? C1 Si1 N1 Si2 5.73(10) . . . . ? C2 Si2 N1 N2 -170.89(14) . . . . ? C2 Si2 N1 Si1 11.68(10) . . . . ? Si1 N1 N2 C3 -122.96(13) . . . . ? Si2 N1 N2 C3 59.6(2) . . . . ? Si1 N1 N2 C4 115.30(14) . . . . ? Si2 N1 N2 C4 -62.1(2) . . . . ? N1 Si2 C2 C1 -28.78(14) . . . . ? Si2 C2 C1 Si1 34.8(2) . . . . ? N1 Si1 C1 C2 -25.50(14) . . . . ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 25935227