#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006506.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006506
loop_
_publ_author_name
'Nagel, N.'
'Ansari, M.'
'Bock, H.'
_publ_section_title
;
 1,2,4,5-Tetrakis(trimethylsilylmethyl)benzene at 150K
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1329
_journal_page_last               1331
_journal_volume                  53
_journal_year                    1997
_chemical_formula_analytical     'C22 H46 Si4'
_chemical_formula_sum            'C22 H46 Si4'
_chemical_formula_weight         422.95
_chemical_melting_point          401.0(10)
_chemical_name_systematic
;
1,2,4,5-Tetrakis(trimethylsilylmethyl)benzene
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.2226(13)
_cell_length_b                   17.8756(15)
_cell_length_c                   19.0452(18)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      10
_cell_volume                     5522.9(8)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL/PC XP (Sheldrick, 1990b)'
_computing_publication_material  'SHELXL93 CIFTAB'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Siemens P4 four-circle diffractometer'
_diffrn_measurement_method       '\w scan'
_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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1664
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.089
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_obs          0.0356
_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^)+(0.0389P)^2^+7.9743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0927
_refine_ls_wR_factor_obs         0.0862
_reflns_number_observed          1298
_reflns_number_total             1572
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    jz1201.cif
_[local]_cod_data_source_block   bock239
_[local]_cod_cif_authors_sg_H-M  'F d d d'
_cod_database_code               2006506
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Si1 0.0265(2) 0.0212(2) 0.0239(2) 0.0010(2) 0.0001(2) 0.0015(2)
C1 0.0250(10) 0.0241(10) 0.0202(9) 0.0008(8) 0.000 0.000
C2 0.0212(6) 0.0201(7) 0.0245(7) 0.0000(5) 0.0003(6) 0.0015(5)
C10 0.0266(7) 0.0212(7) 0.0257(7) -0.0006(6) 0.0016(6) 0.0029(6)
C11 0.0314(9) 0.0454(10) 0.0335(9) 0.0023(7) 0.0060(7) 0.0002(8)
C12 0.0380(10) 0.0413(10) 0.0366(10) -0.0036(7) -0.0033(8) -0.0090(8)
C13 0.0454(10) 0.0304(9) 0.0487(11) 0.0041(7) -0.0049(9) 0.0115(8)
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Si1 0.01246(3) 0.79043(2) 0.51812(2) 0.02389(14) Uani d . 1 Si
C1 0.1250 0.6250 0.55369(11) 0.0231(4) Uani d S 1 C
H1 0.1250 0.6250 0.50381(11) 0.024(6) Uiso calc SR 1 H
C2 0.12493(9) 0.69390(7) 0.58800(7) 0.0219(3) Uani d . 1 C
C10 0.12071(10) 0.76484(8) 0.54522(8) 0.0245(3) Uani d . 1 C
H10A 0.15494(10) 0.75872(8) 0.50258(8) 0.033(3) Uiso calc R 1 H
H10B 0.14432(10) 0.80643(8) 0.57304(8) 0.033(3) Uiso calc R 1 H
C11 -0.05838(11) 0.78298(10) 0.59470(9) 0.0368(4) Uani d . 1 C
H11A -0.0538(7) 0.7330(3) 0.6154(5) 0.068(4) Uiso calc R 1 H
H11B -0.11522(14) 0.7914(8) 0.5792(2) 0.068(4) Uiso calc R 1 H
H11C -0.0435(6) 0.8207(6) 0.6298(4) 0.068(4) Uiso calc R 1 H
C12 -0.02428(11) 0.72535(10) 0.44835(10) 0.0387(4) Uani d . 1 C
H12A -0.0231(9) 0.67391(13) 0.4661(3) 0.064(4) Uiso calc R 1 H
H12B 0.0117(5) 0.7294(6) 0.4072(3) 0.064(4) Uiso calc R 1 H
H12C -0.0808(3) 0.7386(5) 0.4350(5) 0.064(4) Uiso calc R 1 H
C13 0.01272(12) 0.88791(10) 0.48283(10) 0.0415(4) Uani d . 1 C
H13A 0.0535(6) 0.8919(2) 0.4451(5) 0.065(4) Uiso calc R 1 H
H13B 0.0268(9) 0.92296(12) 0.5205(2) 0.065(4) Uiso calc R 1 H
H13C -0.0421(3) 0.9000(3) 0.4644(7) 0.065(4) Uiso calc R 1 H
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C11 Si1 C12 . . 108.45(9) yes
C11 Si1 C13 . . 110.49(9) yes
C12 Si1 C13 . . 109.06(9) yes
C11 Si1 C10 . . 110.06(7) yes
C12 Si1 C10 . . 109.96(8) yes
C13 Si1 C10 . . 108.82(8) yes
C2 C1 C2 . 14_455 124.1(2) yes
C1 C2 C2 . 11_455 117.95(9) yes
C1 C2 C10 . . 119.30(13) yes
C2 C2 C10 11_455 . 122.69(8) yes
C2 C10 Si1 . . 113.19(10) yes
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
Si1 C11 . 1.862(2) yes
Si1 C12 . 1.864(2) yes
Si1 C13 . 1.868(2) yes
Si1 C10 . 1.887(2) yes
C1 C2 . 1.394(2) yes
C1 C2 14_455 1.394(2) yes
C2 C2 11_455 1.409(3) yes
C2 C10 . 1.509(2) yes
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 C1 C2 C2 14_455 11_455 0.10(14) no
C2 C1 C2 C10 14_455 . -177.06(15) no
C1 C2 C10 Si1 . . 82.40(14) yes
C2 C2 C10 Si1 11_455 . -94.6(2) no
C11 Si1 C10 C2 . . 46.89(13) yes
C12 Si1 C10 C2 . . -72.52(13) yes
C13 Si1 C10 C2 . . 168.09(11) yes