#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/80/2228011.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_2228011
loop_
_publ_author_name
'Burnham, Lauren E.'
'Kachlan, Rulla M.'
'Thomas, Andy A.'
'Ogle, Craig A.'
'Jones, Daniel S.'
_publ_section_title
;
 Tetrakis(4-tert-butylbenzyl)silane
;
_journal_coeditor_code           SU2206
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2442
_journal_paper_doi               10.1107/S1600536810034173
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C44 H60 Si1'
_chemical_formula_moiety         'C44 H60 Si1'
_chemical_formula_sum            'C44 H60 Si'
_chemical_formula_weight         617.01
_chemical_name_systematic
;
Tetrakis(4-tert-butylbenzyl)silane
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.394(2)
_cell_length_b                   17.394(2)
_cell_length_c                   6.3613(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      35.28
_cell_measurement_theta_min      7.81
_cell_volume                     1924.6(4)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;ORTEP-3 for Windows (Farrugia, 1997) and
Mercury (Macrae et al., 2006)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5204
_diffrn_reflns_theta_full        67.4
_diffrn_reflns_theta_max         67.4
_diffrn_reflns_theta_min         3.59
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 113
_diffrn_standards_interval_time  57
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.125
_refine_diff_density_min         -0.114
_refine_ls_extinction_coef       0.0033(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0761P)²+0.1124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                1056
_reflns_number_total             1738
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su2206.cif
_cod_data_source_block           I
_cod_original_cell_volume        1924.7(4)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               2228011
_cod_database_fobs_code          2228011
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si Si 0.25 0.25 0.25 0.0599(4) Uani d S 1 . .
C C4 0.50538(12) 0.30509(12) 0.4293(4) 0.0780(7) Uani d . 1 . .
H H4 0.5263 0.2856 0.5529 0.094 Uiso calc R 1 . .
C C1 0.33661(10) 0.25820(11) 0.0742(4) 0.0674(7) Uani d . 1 . .
H H1A 0.3507 0.2069 0.0288 0.081 Uiso calc R 1 . .
H H1B 0.3217 0.2868 -0.0502 0.081 Uiso calc R 1 . .
C C5 0.54015(10) 0.36783(10) 0.3360(3) 0.0535(5) Uani d . 1 . .
C C7 0.44050(11) 0.35854(12) 0.0714(4) 0.0668(6) Uani d . 1 . .
H H7 0.4193 0.3779 -0.0519 0.08 Uiso calc R 1 . .
C C8 0.61357(11) 0.40291(11) 0.4257(4) 0.0624(6) Uani d . 1 . .
C C2 0.40700(10) 0.29575(10) 0.1652(4) 0.0580(5) Uani d . 1 . .
C C6 0.50509(12) 0.39375(12) 0.1556(4) 0.0674(6) Uani d . 1 . .
H H6 0.5255 0.4365 0.0876 0.081 Uiso calc R 1 . .
C C3 0.44105(12) 0.27021(12) 0.3468(4) 0.0837(8) Uani d . 1 . .
H H3 0.42 0.2281 0.4163 0.1 Uiso calc R 1 . .
C C9 0.62982(15) 0.48273(14) 0.3328(5) 0.0951(9) Uani d . 1 . .
H H9A 0.634 0.4789 0.1827 0.143 Uiso calc R 1 . .
H H9B 0.6771 0.5023 0.3896 0.143 Uiso calc R 1 . .
H H9C 0.5885 0.517 0.3682 0.143 Uiso calc R 1 . .
C C10 0.68066(12) 0.35026(15) 0.3687(5) 0.0992(9) Uani d . 1 . .
H H10A 0.672 0.3001 0.4269 0.149 Uiso calc R 1 . .
H H10B 0.7275 0.3711 0.4249 0.149 Uiso calc R 1 . .
H H10C 0.6848 0.3465 0.2186 0.149 Uiso calc R 1 . .
C C11 0.60896(17) 0.41111(18) 0.6619(5) 0.1047(9) Uani d . 1 . .
H H11A 0.5674 0.445 0.6977 0.157 Uiso calc R 1 . .
H H11B 0.6564 0.432 0.714 0.157 Uiso calc R 1 . .
H H11C 0.6002 0.3616 0.7241 0.157 Uiso calc R 1 . .
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 0 '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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 2 -1
-1 -1 -1
1 -2 -2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Si C1 8_656 2 110.68(7) ?
C1 Si C1 8_656 7_566 107.08(14) ?
C1 Si C1 2 7_566 110.68(7) ?
C1 Si C1 8_656 . 110.68(7) ?
C1 Si C1 2 . 107.08(14) ?
C1 Si C1 7_566 . 110.68(7) ?
C3 C4 C5 . . 122.7(2) ?
C3 C4 H4 . . 118.7 ?
C5 C4 H4 . . 118.7 ?
C2 C1 Si . . 117.14(16) ?
C2 C1 H1A . . 108 ?
Si C1 H1A . . 108 ?
C2 C1 H1B . . 108 ?
Si C1 H1B . . 108 ?
H1A C1 H1B . . 107.3 ?
C6 C5 C4 . . 115.05(19) ?
C6 C5 C8 . . 123.50(17) ?
C4 C5 C8 . . 121.4(2) ?
C2 C7 C6 . . 121.8(2) ?
C2 C7 H7 . . 119.1 ?
C6 C7 H7 . . 119.1 ?
C11 C8 C5 . . 111.41(19) ?
C11 C8 C10 . . 109.4(2) ?
C5 C8 C10 . . 108.13(17) ?
C11 C8 C9 . . 107.9(2) ?
C5 C8 C9 . . 111.83(18) ?
C10 C8 C9 . . 108.09(19) ?
C3 C2 C7 . . 116.09(19) ?
C3 C2 C1 . . 122.34(18) ?
C7 C2 C1 . . 121.6(2) ?
C5 C6 C7 . . 122.44(19) ?
C5 C6 H6 . . 118.8 ?
C7 C6 H6 . . 118.8 ?
C2 C3 C4 . . 121.94(19) ?
C2 C3 H3 . . 119 ?
C4 C3 H3 . . 119 ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C8 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C8 C10 H10A . . 109.5 ?
C8 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C8 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C8 C11 H11A . . 109.5 ?
C8 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C8 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Si C1 8_656 1.882(2) ?
Si C1 2 1.882(2) ?
Si C1 7_566 1.882(2) ?
Si C1 . 1.882(2) ?
C4 C3 . 1.377(3) ?
C4 C5 . 1.382(3) ?
C4 H4 . 0.93 ?
C1 C2 . 1.504(3) ?
C1 H1A . 0.97 ?
C1 H1B . 0.97 ?
C5 C6 . 1.375(3) ?
C5 C8 . 1.526(3) ?
C7 C2 . 1.374(3) ?
C7 C6 . 1.387(3) ?
C7 H7 . 0.93 ?
C8 C11 . 1.512(3) ?
C8 C10 . 1.527(3) ?
C8 C9 . 1.535(3) ?
C2 C3 . 1.372(3) ?
C6 H6 . 0.93 ?
C3 H3 . 0.93 ?
C9 H9A . 0.96 ?
C9 H9B . 0.96 ?
C9 H9C . 0.96 ?
C10 H10A . 0.96 ?
C10 H10B . 0.96 ?
C10 H10C . 0.96 ?
C11 H11A . 0.96 ?
C11 H11B . 0.96 ?
C11 H11C . 0.96 ?
