#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:00:39 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178881 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/10/4111091.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_4111091
loop_
_publ_author_name
'Eric Block'
'Evgeny V. Dikarev'
'Richard S. Glass'
'Jin Jin'
'Bo Li'
'Xiaojie Li'
'Shao-Zhong Zhang'
_publ_section_title
;
 Synthesis, Structure, and Chemistry of New, Mixed Group 14 and 16
 Heterocycles: Nucleophile-Induced Ring Contraction of Mesocyclic
 Dications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14949
_journal_page_last               14961
_journal_paper_doi               10.1021/ja065037j
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'Si (C H2 Br)2 (Si (C H3)3)2'
_chemical_formula_sum            'C8 H22 Br2 Si3'
_chemical_formula_weight         362.35
_chemical_name_systematic
; 
 Bis(bromomethyl)bis(trimethylsilyl)silane 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.5570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4033(14)
_cell_length_b                   7.8526(7)
_cell_length_c                   12.3918(10)
_cell_measurement_reflns_used    3916
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.47
_cell_volume                     1605.4(2)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide ω exposures'
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6775
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    5.241
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6223
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0481P)²+1.0034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                1614
_reflns_number_total             1897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065037jsi20060721_015934.cif
_cod_data_source_block           C8H22Br2Si3_23b
_cod_database_code               4111091
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Br1 Br 1.112276(18) 1.00988(4) 0.91449(3) 0.05621(13) Uani 1 1 d .
Si1 Si 1.0000 0.73278(10) 0.7500 0.02501(18) Uani 1 2 d S
Si2 Si 0.88434(3) 0.56633(8) 0.73414(5) 0.02780(15) Uani 1 1 d .
C2 C 0.91875(15) 0.3841(3) 0.8357(2) 0.0370(5) Uani 1 1 d .
C1 C 1.01269(14) 0.8758(3) 0.8767(2) 0.0336(5) Uani 1 1 d .
C3 C 0.80697(17) 0.6929(4) 0.7753(3) 0.0455(6) Uani 1 1 d .
C4 C 0.83905(18) 0.4854(4) 0.5858(2) 0.0419(6) Uani 1 1 d .
H1 H 0.9705(19) 0.958(4) 0.863(3) 0.049(8) Uiso 1 1 d .
H2 H 1.0147(17) 0.821(4) 0.940(3) 0.049(8) Uiso 1 1 d .
H3 H 0.8767(17) 0.317(4) 0.837(2) 0.053(8) Uiso 1 1 d .
H4 H 0.945(2) 0.429(5) 0.912(3) 0.070(10) Uiso 1 1 d .
H5 H 0.9561(18) 0.311(4) 0.820(2) 0.048(8) Uiso 1 1 d .
H6 H 0.7889(19) 0.778(4) 0.726(3) 0.060(9) Uiso 1 1 d .
H7 H 0.828(2) 0.739(5) 0.847(3) 0.074(11) Uiso 1 1 d .
H8 H 0.761(2) 0.624(4) 0.773(3) 0.062(9) Uiso 1 1 d .
H9 H 0.8221(17) 0.581(4) 0.536(2) 0.048(8) Uiso 1 1 d .
H10 H 0.796(2) 0.425(5) 0.582(3) 0.074(11) Uiso 1 1 d .
H11 H 0.873(2) 0.418(5) 0.563(3) 0.059(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
Br1 0.04880(19) 0.0524(2) 0.0672(2) -0.02777(14) 0.01821(15) -0.01905(12)
Si1 0.0231(4) 0.0217(4) 0.0297(4) 0.000 0.0077(3) 0.000
Si2 0.0229(3) 0.0273(3) 0.0330(3) 0.0015(2) 0.0086(2) -0.0002(2)
C2 0.0323(12) 0.0352(13) 0.0434(14) 0.0085(10) 0.0121(10) -0.0010(10)
C1 0.0351(12) 0.0312(12) 0.0346(12) -0.0034(9) 0.0111(10) -0.0026(9)
C3 0.0357(13) 0.0434(15) 0.0636(18) 0.0036(14) 0.0243(13) 0.0067(11)
C4 0.0378(14) 0.0428(15) 0.0389(14) -0.0001(11) 0.0035(11) -0.0060(11)
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'
Br Br -0.2901 2.4595 '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 106.89(16) . 2_756
C1 Si1 Si2 105.69(7) . .
C1 Si1 Si2 112.99(8) 2_756 .
C1 Si1 Si2 112.99(8) . 2_756
C1 Si1 Si2 105.69(7) 2_756 2_756
Si2 Si1 Si2 112.58(4) . 2_756
C4 Si2 C3 109.55(15) . .
C4 Si2 C2 110.27(13) . .
C3 Si2 C2 109.05(13) . .
C4 Si2 Si1 110.67(10) . .
C3 Si2 Si1 110.64(10) . .
C2 Si2 Si1 106.61(8) . .
Si2 C2 H3 111.9(18) . .
Si2 C2 H4 109(2) . .
H3 C2 H4 109(3) . .
Si2 C2 H5 115.2(17) . .
H3 C2 H5 105(3) . .
H4 C2 H5 106(3) . .
Si1 C1 Br1 112.35(12) . .
Si1 C1 H1 111.9(18) . .
Br1 C1 H1 104.6(18) . .
Si1 C1 H2 114.1(19) . .
Br1 C1 H2 105.5(19) . .
H1 C1 H2 108(3) . .
Si2 C3 H6 110(2) . .
Si2 C3 H7 112(2) . .
H6 C3 H7 108(3) . .
Si2 C3 H8 111(2) . .
H6 C3 H8 107(3) . .
H7 C3 H8 109(3) . .
Si2 C4 H9 108.3(18) . .
Si2 C4 H10 109(2) . .
H9 C4 H10 108(3) . .
Si2 C4 H11 113(2) . .
H9 C4 H11 111(3) . .
H10 C4 H11 107(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C1 1.953(2) .
Si1 C1 1.886(2) .
Si1 C1 1.886(2) 2_756
Si1 Si2 2.3551(7) .
Si1 Si2 2.3551(7) 2_756
Si2 C4 1.866(3) .
Si2 C3 1.871(3) .
Si2 C2 1.873(2) .
C2 H3 0.91(3) .
C2 H4 0.98(4) .
C2 H5 0.93(3) .
C1 H1 0.95(3) .
C1 H2 0.89(3) .
C3 H6 0.89(3) .
C3 H7 0.92(4) .
C3 H8 0.96(3) .
C4 H9 0.96(3) .
C4 H10 0.88(4) .
C4 H11 0.91(3) .
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
C1 Si1 Si2 C4 156.90(13) .
C1 Si1 Si2 C4 40.35(13) 2_756
Si2 Si1 Si2 C4 -79.30(10) 2_756
C1 Si1 Si2 C3 35.28(14) .
C1 Si1 Si2 C3 -81.28(14) 2_756
Si2 Si1 Si2 C3 159.08(12) 2_756
C1 Si1 Si2 C2 -83.16(13) .
C1 Si1 Si2 C2 160.28(12) 2_756
Si2 Si1 Si2 C2 40.63(9) 2_756
C1 Si1 C1 Br1 -65.12(10) 2_756
Si2 Si1 C1 Br1 174.26(10) .
Si2 Si1 C1 Br1 50.72(14) 2_756
