#------------------------------------------------------------------------------
#$Date: 2017-11-15 14:59:14 +0200 (Wed, 15 Nov 2017) $
#$Revision: 203217 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/31/2103123.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_2103123
loop_
_publ_author_name
'Herbst-Irmer, Regine'
'Sheldrick, George M.'
_publ_section_title
;
 Refinement of obverse/reverse twins
;
_journal_coden_ASTM              ASBSDK
_journal_issue                   3
_journal_name_full
;
 Acta Crystallographica, Section B: Structural Science
;
_journal_page_first              477
_journal_page_last               481
_journal_paper_doi               10.1107/S0108768102001039
_journal_volume                  58
_journal_year                    2002
_chemical_formula_sum            'C24 H54 O3 Si3'
_chemical_formula_weight         474.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   10.0793(7)
_cell_length_b                   10.0793(7)
_cell_length_c                   48.409(4)
_cell_measurement_reflns_used    849
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     4259.1(6)
_computing_cell_refinement       'Siemens SAINT (V. 4.050, Siemens 1996)'
_computing_data_collection       'Siemens SMART (V. 4.202, Siemens 1996)'
_computing_data_reduction        'Siemens SAINT (V. 4.050, Siemens 1996)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'Stoe-Siemens-Huber four circle diffractometer'
_diffrn_measurement_method       'phi 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  0.037
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            47973
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0349
_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)+(0.0527P)²+2.7315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                751
_reflns_number_total             849
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jz0014.cif
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               2103123
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
loop_
_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_type_symbol
Si 0.84589(6) 0.3333 0.0833 0.0157(2) Uani d S 1 Si
O 0.6667 0.17946(18) 0.0833 0.0259(5) Uani d S 1 O
C3 1.0225(2) 0.2288(2) 0.05245(4) 0.0285(5) Uani d . 1 C
H3A 1.0699 0.2298 0.0347 0.043 Uiso calc R 1 H
H3B 0.9403 0.1244 0.0565 0.043 Uiso calc R 1 H
H3C 1.0999 0.2637 0.0671 0.043 Uiso calc R 1 H
C2 1.0871(2) 0.5007(2) 0.04538(4) 0.0275(5) Uani d . 1 C
H2A 1.1412 0.5020 0.0285 0.041 Uiso calc R 1 H
H2B 1.1588 0.5352 0.0610 0.041 Uiso calc R 1 H
H2C 1.0452 0.5693 0.0432 0.041 Uiso calc R 1 H
C 0.9555(2) 0.3364(2) 0.05089(3) 0.0201(4) Uani d . 1 C
C1 0.8500(2) 0.2840(2) 0.02550(4) 0.0275(5) Uani d . 1 C
H1A 0.8036 0.3488 0.0234 0.041 Uiso calc R 1 H
H1B 0.7691 0.1771 0.0280 0.041 Uiso calc R 1 H
H1C 0.9098 0.2925 0.0090 0.041 Uiso calc R 1 H
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
Si 0.0160(3) 0.0144(4) 0.0161(3) 0.00718(18) 0.00040(13) 0.0008(3)
O 0.0222(10) 0.0277(8) 0.0261(9) 0.0111(5) 0.0001(7) 0.0001(4)
C3 0.0323(11) 0.0282(11) 0.0305(10) 0.0195(10) 0.0067(8) 0.0026(8)
C2 0.0257(11) 0.0258(11) 0.0289(9) 0.0114(9) 0.0084(8) 0.0080(8)
C 0.0203(10) 0.0184(9) 0.0220(8) 0.0100(8) 0.0039(7) 0.0015(7)
C1 0.0295(11) 0.0328(11) 0.0205(9) 0.0157(9) 0.0028(8) -0.0013(8)
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'
O O 0.0106 0.0060 '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
O Si O . 2_655 104.98(12)
O Si C . 17_554 109.63(6)
O Si C 2_655 17_554 110.99(6)
O Si C . . 110.99(6)
O Si C 2_655 . 109.63(6)
C Si C 17_554 . 110.49(11)
Si O Si . 3_665 135.02(12)
C1 C C3 . . 105.60(14)
C1 C C2 . . 107.87(14)
C3 C C2 . . 108.69(15)
C1 C Si . . 110.88(12)
C3 C Si . . 113.70(12)
C2 C Si . . 109.86(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Si O . 1.6932(8)
Si O 2_655 1.6932(8)
Si C 17_554 1.9115(16)
Si C . 1.9116(16)
O Si 3_665 1.6932(8)
C3 C . 1.539(2)
C2 C . 1.542(2)
C C1 . 1.536(2)
