#------------------------------------------------------------------------------ #$Date: 2014-07-12 00:06:05 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120077 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/45/4114563.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_4114563 loop_ _publ_author_name 'Yuxia Liu' 'Thomas C. Stringfellow' 'David Ballweg' 'Ilia A. Guzei' 'Robert West' _publ_contact_author ; Prof. Robert West Department of Chemistry University of Wisconsin 1101 University Ave. Madison, WI 53706-1396 USA ; _publ_contact_author_email west@chem.wisc.edu _publ_contact_author_fax 1(608)2620381 _publ_contact_author_phone 1(608)2621873 _publ_section_title ; Structure and Chemistry of 1-Silafluorenyl Dianion, Its Derivatives, and an Organosilicon Diradical Dianion ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 49 _journal_page_last 57 _journal_volume 124 _journal_year 2002 _chemical_formula_moiety 'C12 H8 Cl2 Si' _chemical_formula_sum 'C12 H8 Cl2 Si' _chemical_formula_weight 251.17 _chemical_name_systematic ; ? ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.4375(6) _cell_length_b 12.1540(10) _cell_length_c 12.7246(11) _cell_measurement_reflns_used 4183 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 25.0 _cell_measurement_theta_min 3.0 _cell_volume 1150.24(17) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 133(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'Bruker SMART/Platform' _diffrn_measurement_method '\w scan frames' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 6939 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 27.22 _diffrn_reflns_theta_min 2.32 _diffrn_standards_decay_% 0.20 _diffrn_standards_number 134 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_type empirical _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.450 _exptl_crystal_description prism _exptl_crystal_F_000 512 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.342 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 1342 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0292 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.0650P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.0777 _reflns_number_gt 1121 _reflns_number_total 1342 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ja011821m_2.cif _[local]_cod_data_source_block n98064 _cod_original_cell_volume 1150.25(17) _cod_database_code 4114563 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' 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 Si1 Si 0.15157(8) 0.7500 0.50528(5) 0.02618(17) Uani 1 2 d S Cl1 Cl 0.16233(9) 0.7500 0.66592(4) 0.04216(19) Uani 1 2 d S Cl2 Cl -0.11585(7) 0.7500 0.46546(6) 0.04038(19) Uani 1 2 d S C1 C 0.27862(19) 0.63858(13) 0.44129(11) 0.0266(3) Uani 1 1 d . C2 C 0.2641(2) 0.52476(14) 0.44536(12) 0.0309(4) Uani 1 1 d . H2A H 0.1781 0.4914 0.4904 0.037 Uiso 1 1 calc R C3 C 0.3755(2) 0.45959(16) 0.38346(14) 0.0362(4) Uani 1 1 d . H3A H 0.3653 0.3817 0.3860 0.043 Uiso 1 1 calc R C4 C 0.5011(2) 0.50852(15) 0.31819(13) 0.0388(4) Uani 1 1 d . H4A H 0.5768 0.4637 0.2760 0.047 Uiso 1 1 calc R C5 C 0.5182(2) 0.62196(15) 0.31356(12) 0.0348(4) Uani 1 1 d . H5A H 0.6058 0.6542 0.2688 0.042 Uiso 1 1 calc R C6 C 0.40697(18) 0.68878(14) 0.37443(11) 0.0274(3) 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 0.0257(3) 0.0258(3) 0.0270(3) 0.000 0.0051(2) 0.000 Cl1 0.0682(4) 0.0334(3) 0.0249(3) 0.000 0.0119(3) 0.000 Cl2 0.0228(3) 0.0349(3) 0.0634(4) 0.000 0.0050(3) 0.000 C1 0.0220(7) 0.0337(9) 0.0242(7) -0.0036(6) -0.0014(6) 0.0007(6) C2 0.0269(8) 0.0342(9) 0.0315(8) -0.0061(7) -0.0019(6) -0.0008(7) C3 0.0335(9) 0.0365(9) 0.0386(9) -0.0116(7) -0.0035(7) 0.0028(7) C4 0.0322(9) 0.0486(12) 0.0354(9) -0.0152(8) -0.0007(7) 0.0088(7) C5 0.0272(8) 0.0502(11) 0.0270(8) -0.0053(7) 0.0025(6) 0.0017(7) C6 0.0211(7) 0.0402(9) 0.0209(7) -0.0020(7) -0.0030(6) 0.0011(6) 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 Si1 C1 94.70(10) 7_575 . C1 Si1 Cl1 114.95(5) 7_575 . C1 Si1 Cl1 114.95(5) . . C1 Si1 Cl2 112.84(5) 7_575 . C1 Si1 Cl2 112.84(5) . . Cl1 Si1 Cl2 106.53(4) . . C2 C1 C6 120.25(14) . . C2 C1 Si1 132.56(12) . . C6 C1 Si1 107.14(11) . . C1 C2 C3 120.01(15) . . C4 C3 C2 119.81(17) . . C3 C4 C5 120.97(15) . . C4 C5 C6 120.10(15) . . C5 C6 C1 118.85(15) . . C5 C6 C6 125.63(10) . 7_575 C1 C6 C6 115.51(9) . 7_575 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si1 C1 1.8411(16) 7_575 Si1 C1 1.8411(15) . Si1 Cl1 2.0456(9) . Si1 Cl2 2.0524(8) . C1 C2 1.389(2) . C1 C6 1.417(2) . C2 C3 1.391(2) . C3 C4 1.385(2) . C4 C5 1.386(2) . C5 C6 1.394(2) . C6 C6 1.488(3) 7_575 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_4 C1 Si1 C1 C2 -178.25(11) 7_575 . Cl1 Si1 C1 C2 61.41(16) . . Cl2 Si1 C1 C2 -61.04(16) . . C1 Si1 C1 C6 -0.90(13) 7_575 . Cl1 Si1 C1 C6 -121.24(9) . . Cl2 Si1 C1 C6 116.31(9) . . C6 C1 C2 C3 -0.2(2) . . Si1 C1 C2 C3 176.90(12) . . C1 C2 C3 C4 0.3(2) . . C2 C3 C4 C5 0.1(2) . . C3 C4 C5 C6 -0.6(2) . . C4 C5 C6 C1 0.6(2) . . C4 C5 C6 C6 -177.91(10) . 7_575 C2 C1 C6 C5 -0.3(2) . . Si1 C1 C6 C5 -178.02(11) . . C2 C1 C6 C6 178.41(10) . 7_575 Si1 C1 C6 C6 0.68(10) . 7_575 _journal_paper_doi 10.1021/ja011821m