#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:17:59 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178502 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/40/4064073.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_4064073
loop_
_publ_author_name
'Wallner, Andreas'
'Hlina, Johann'
'Wagner, Harald'
'Baumgartner, Judith'
'Marschner, Christoph'
_publ_section_title
;
 Conformational Control of Polysilanes: Use of CH(2) Spacers in the
 Silicon Backbone.
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3930
_journal_page_last               3938
_journal_paper_doi               10.1021/om1011159
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C22 H62 Si8'
_chemical_formula_weight         551.44
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.188(3)
_cell_length_b                   9.960(2)
_cell_length_c                   25.704(5)
_cell_measurement_reflns_used    5305
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.511
_cell_measurement_theta_min      4.909
_cell_volume                     3783.1(14)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       'ω scans'
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11475
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.9172
_exptl_absorpt_correction_T_min  0.8794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.353
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.353
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0930
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0599P)²+27.5688P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1980
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                2649
_reflns_number_total             2791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011159_si_001.cif
_cod_data_source_block           12_349j
_cod_original_cell_volume        3783.1(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4064073
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
Si1 Si 0.11867(10) 0.74857(15) 0.10174(6) 0.0160(4) Uani 1 1 d .
Si2 Si -0.01045(11) 0.87764(16) 0.10318(6) 0.0209(4) Uani 1 1 d .
Si3 Si 0.08075(10) 0.52138(15) 0.11143(6) 0.0180(4) Uani 1 1 d .
Si4 Si 0.23535(11) 0.81554(16) 0.17458(6) 0.0206(4) Uani 1 1 d .
C1 C 0.1519(4) 0.7910(5) 0.0360(2) 0.0181(12) Uani 1 1 d .
H1A H 0.1006 0.7661 0.0061 0.022 Uiso 1 1 calc R
H1B H 0.1593 0.8896 0.0345 0.022 Uiso 1 1 calc R
C2 C 0.2376(4) 0.7255(5) 0.0256(2) 0.0208(13) Uani 1 1 d .
H2A H 0.2887 0.7443 0.0564 0.025 Uiso 1 1 calc R
H2B H 0.2287 0.6270 0.0234 0.025 Uiso 1 1 calc R
C5 C 0.0211(5) 1.0612(6) 0.1113(3) 0.0373(17) Uani 1 1 d .
H5A H -0.0339 1.1155 0.1069 0.056 Uiso 1 1 calc R
H5B H 0.0540 1.0870 0.0842 0.056 Uiso 1 1 calc R
H5C H 0.0597 1.0763 0.1470 0.056 Uiso 1 1 calc R
C6 C -0.0975(5) 0.8579(7) 0.0381(2) 0.0360(17) Uani 1 1 d .
H6A H -0.1179 0.7643 0.0340 0.054 Uiso 1 1 calc R
H6B H -0.0705 0.8825 0.0083 0.054 Uiso 1 1 calc R
H6C H -0.1493 0.9166 0.0382 0.054 Uiso 1 1 calc R
C7 C -0.0627(4) 0.8263(6) 0.1597(2) 0.0300(15) Uani 1 1 d .
H7A H -0.0162 0.8260 0.1932 0.045 Uiso 1 1 calc R
H7B H -0.0886 0.7362 0.1528 0.045 Uiso 1 1 calc R
H7C H -0.1106 0.8901 0.1625 0.045 Uiso 1 1 calc R
C8 C -0.0355(4) 0.4787(7) 0.0700(3) 0.0314(15) Uani 1 1 d .
H8A H -0.0378 0.4965 0.0322 0.047 Uiso 1 1 calc R
H8B H -0.0809 0.5338 0.0816 0.047 Uiso 1 1 calc R
H8C H -0.0482 0.3835 0.0746 0.047 Uiso 1 1 calc R
C9 C 0.0767(4) 0.4908(6) 0.1831(2) 0.0298(15) Uani 1 1 d .
H9A H 0.0601 0.3970 0.1874 0.045 Uiso 1 1 calc R
H9B H 0.0315 0.5502 0.1928 0.045 Uiso 1 1 calc R
H9C H 0.1362 0.5091 0.2064 0.045 Uiso 1 1 calc R
C10 C 0.1656(4) 0.4038(6) 0.0935(3) 0.0302(15) Uani 1 1 d .
H10A H 0.1528 0.3119 0.1033 0.045 Uiso 1 1 calc R
H10B H 0.2266 0.4295 0.1129 0.045 Uiso 1 1 calc R
H10C H 0.1616 0.4084 0.0549 0.045 Uiso 1 1 calc R
C11 C 0.1905(4) 0.8294(7) 0.2369(2) 0.0330(16) Uani 1 1 d .
H11A H 0.1650 0.7429 0.2441 0.049 Uiso 1 1 calc R
H11B H 0.1433 0.8984 0.2318 0.049 Uiso 1 1 calc R
H11C H 0.2399 0.8540 0.2672 0.049 Uiso 1 1 calc R
C12 C 0.3324(4) 0.6947(7) 0.1886(2) 0.0340(16) Uani 1 1 d .
H12A H 0.3821 0.7323 0.2160 0.051 Uiso 1 1 calc R
H12B H 0.3532 0.6788 0.1558 0.051 Uiso 1 1 calc R
H12C H 0.3128 0.6096 0.2014 0.051 Uiso 1 1 calc R
C13 C 0.2805(4) 0.9839(6) 0.1593(3) 0.0313(15) Uani 1 1 d .
H13A H 0.2341 1.0528 0.1583 0.047 Uiso 1 1 calc R
H13B H 0.2965 0.9800 0.1245 0.047 Uiso 1 1 calc R
H13C H 0.3344 1.0064 0.1871 0.047 Uiso 1 1 calc R
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'
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
C1 Si1 Si2 106.45(18) .
C1 Si1 Si4 109.57(18) .
Si2 Si1 Si4 108.02(8) .
C1 Si1 Si3 115.07(17) .
Si2 Si1 Si3 107.30(8) .
Si4 Si1 Si3 110.13(8) .
C7 Si2 C6 108.8(3) .
C7 Si2 C5 108.6(3) .
C6 Si2 C5 107.9(3) .
C7 Si2 Si1 111.5(2) .
C6 Si2 Si1 110.2(2) .
C5 Si2 Si1 109.8(2) .
C10 Si3 C9 108.6(3) .
C10 Si3 C8 109.0(3) .
C9 Si3 C8 106.1(3) .
C10 Si3 Si1 112.0(2) .
C9 Si3 Si1 108.8(2) .
C8 Si3 Si1 112.0(2) .
C12 Si4 C11 107.8(3) .
C12 Si4 C13 107.7(3) .
C11 Si4 C13 109.4(3) .
C12 Si4 Si1 112.7(2) .
C11 Si4 Si1 110.0(2) .
C13 Si4 Si1 109.2(2) .
C2 C1 Si1 117.7(4) .
C2 C2 C1 113.7(6) 7_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C1 1.920(5) .
Si1 Si2 2.352(2) .
Si1 Si4 2.357(2) .
Si1 Si3 2.362(2) .
Si2 C7 1.880(6) .
Si2 C6 1.888(7) .
Si2 C5 1.890(7) .
Si3 C10 1.876(6) .
Si3 C9 1.882(6) .
Si3 C8 1.888(6) .
Si4 C12 1.873(6) .
Si4 C11 1.885(6) .
Si4 C13 1.887(6) .
C1 C2 1.533(8) .
C2 C2 1.532(11) 7_565
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_4
C1 Si1 Si2 C7 170.6(3) .
Si4 Si1 Si2 C7 -71.8(2) .
Si3 Si1 Si2 C7 46.9(2) .
C1 Si1 Si2 C6 49.7(3) .
Si4 Si1 Si2 C6 167.3(2) .
Si3 Si1 Si2 C6 -74.0(2) .
C1 Si1 Si2 C5 -69.0(3) .
Si4 Si1 Si2 C5 48.6(3) .
Si3 Si1 Si2 C5 167.3(2) .
C1 Si1 Si3 C10 47.0(3) .
Si2 Si1 Si3 C10 165.3(2) .
Si4 Si1 Si3 C10 -77.4(2) .
C1 Si1 Si3 C9 167.1(3) .
Si2 Si1 Si3 C9 -74.7(2) .
Si4 Si1 Si3 C9 42.7(2) .
C1 Si1 Si3 C8 -75.9(3) .
Si2 Si1 Si3 C8 42.4(2) .
Si4 Si1 Si3 C8 159.7(2) .
C1 Si1 Si4 C12 -78.5(3) .
Si2 Si1 Si4 C12 165.9(2) .
Si3 Si1 Si4 C12 49.0(2) .
C1 Si1 Si4 C11 161.1(3) .
Si2 Si1 Si4 C11 45.6(3) .
Si3 Si1 Si4 C11 -71.3(3) .
C1 Si1 Si4 C13 41.1(3) .
Si2 Si1 Si4 C13 -74.5(2) .
Si3 Si1 Si4 C13 168.6(2) .
Si2 Si1 C1 C2 177.1(4) .
Si4 Si1 C1 C2 60.5(4) .
Si3 Si1 C1 C2 -64.2(4) .
Si1 C1 C2 C2 -175.3(5) 7_565
