#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/35/2213539.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_2213539
loop_
_publ_author_name
'Rothenberger, Alexander'
'Ponikiewski, Lukasz'
_publ_section_title
;
 Hexakis(trimethylsiloxymethyl)benzene methanol disolvate
;
_journal_coeditor_code           SG2156
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2634
_journal_page_last               o2635
_journal_paper_doi               10.1107/S1600536807017047
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C30 H66 O6 Si6, 2C1 H4 O'
_chemical_formula_moiety         'C30 H66 O6 Si6, 2C1 H4 O'
_chemical_formula_sum            'C32 H74 O8 Si6'
_chemical_formula_weight         755.45
_chemical_name_systematic
;
Hexakis(trimethylsiloxymethyl)benzene methanol disolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.34(3)
_cell_angle_beta                 97.61(4)
_cell_angle_gamma                96.04(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7075(19)
_cell_length_b                   10.153(2)
_cell_length_c                   12.227(2)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     1160.4(4)
_computing_cell_refinement
;
STADI4
;
_computing_data_collection
;
STADI4 (Stoe & Cie, 1995)
;
_computing_data_reduction
;
STADI4
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 1997b)
;
_computing_publication_material
;
SHELXTL
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 1997a)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 1997a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.639
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       rotation
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9084
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.92
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.771
_refine_diff_density_min         -1.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5117
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0569
_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)+(0.1223P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.2133
_reflns_number_gt                3168
_reflns_number_total             5117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sg2156.cif
_cod_data_source_block           I
_cod_database_code               2213539
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 Si1 0.90880(9) 0.31022(9) 0.29937(7) 0.0341(3) Uani d . 1 . .
Si Si2 0.33061(10) 0.27694(9) 0.06752(7) 0.0356(3) Uani d . 1 . .
Si Si3 0.26566(10) 0.86762(9) 0.31390(8) 0.0360(3) Uani d . 1 . .
C C1 0.5779(3) 0.4086(3) 0.4422(2) 0.0239(6) Uani d . 1 . .
C C2 0.4839(3) 0.4733(3) 0.3816(2) 0.0235(6) Uani d . 1 . .
C C3 0.4052(3) 0.5642(3) 0.4391(2) 0.0229(6) Uani d . 1 . .
C C5 0.4705(3) 0.4483(3) 0.2546(2) 0.0292(6) Uani d . 1 . .
H H5A 0.4472 0.5308 0.2285 0.035 Uiso calc R 1 A .
H H5B 0.5608 0.4270 0.2309 0.035 Uiso calc R 1 . .
C C6 0.2986(3) 0.6286(3) 0.3736(3) 0.0305(7) Uani d . 1 . .
H H6A 0.2648 0.5693 0.2982 0.037 Uiso calc R 1 . .
H H6B 0.2172 0.6399 0.4138 0.037 Uiso calc R 1 . .
C C7 0.9483(5) 0.4172(5) 0.1970(4) 0.0708(13) Uani d . 1 A .
H H7A 0.9566 0.5131 0.2339 0.106 Uiso calc R 1 . .
H H7B 0.8723 0.3966 0.1323 0.106 Uiso calc R 1 . .
H H7C 1.0367 0.3980 0.1707 0.106 Uiso calc R 1 . .
C C8 0.8447(4) 0.1313(4) 0.2281(4) 0.0588(11) Uani d . 1 A .
H H8A 0.8145 0.0811 0.2834 0.088 Uiso calc R 1 . .
H H8B 0.9204 0.0901 0.1945 0.088 Uiso calc R 1 . .
H H8C 0.7653 0.1283 0.1686 0.088 Uiso calc R 1 . .
C C9 1.0670(4) 0.3188(4) 0.4023(3) 0.0512(9) Uani d . 1 A .
H H9A 1.0507 0.2527 0.4494 0.077 Uiso calc R 1 . .
H H9B 1.0889 0.4102 0.4502 0.077 Uiso calc R 1 . .
H H9C 1.1457 0.2981 0.3623 0.077 Uiso calc R 1 . .
C C10 0.2869(6) 0.4140(5) -0.0054(3) 0.0690(13) Uani d . 1 . .
H H10A 0.3616 0.4912 0.0190 0.104 Uiso calc R 1 . .
H H10B 0.1981 0.4426 0.0134 0.104 Uiso calc R 1 . .
H H10C 0.2778 0.3806 -0.0872 0.104 Uiso calc R 1 . .
C C11 0.4854(5) 0.2047(4) 0.0192(3) 0.0610(11) Uani d . 1 . .
H H11A 0.5668 0.2754 0.0379 0.092 Uiso calc R 1 . .
H H11B 0.4659 0.1700 -0.0628 0.092 Uiso calc R 1 . .
H H11C 0.5053 0.1305 0.0569 0.092 Uiso calc R 1 . .
C C12 0.1787(5) 0.1428(4) 0.0464(3) 0.0616(11) Uani d . 1 . .
H H12A 0.0982 0.1832 0.0723 0.092 Uiso calc R 1 . .
H H12B 0.2028 0.0747 0.0897 0.092 Uiso calc R 1 . .
H H12C 0.1548 0.0998 -0.0340 0.092 Uiso calc R 1 . .
C C13 0.1785(5) 0.7904(4) 0.1665(3) 0.0676(13) Uani d . 1 . .
H H13A 0.2496 0.7628 0.1199 0.101 Uiso calc R 1 . .
H H13B 0.1282 0.8569 0.1354 0.101 Uiso calc R 1 . .
H H13C 0.1121 0.7108 0.1667 0.101 Uiso calc R 1 . .
C C14 0.1326(5) 0.9085(5) 0.4081(4) 0.0730(14) Uani d . 1 . .
H H14A 0.1799 0.9406 0.4863 0.109 Uiso calc R 1 . .
H H14B 0.0662 0.8269 0.4028 0.109 Uiso calc R 1 . .
H H14C 0.0819 0.9794 0.3847 0.109 Uiso calc R 1 . .
C C15 0.3936(4) 1.0176(4) 0.3196(4) 0.0581(11) Uani d . 1 . .
H H15A 0.4401 1.0530 0.3977 0.087 Uiso calc R 1 . .
H H15B 0.3449 1.0877 0.2926 0.087 Uiso calc R 1 . .
H H15C 0.4638 0.9919 0.2716 0.087 Uiso calc R 1 . .
O O1 0.7812(12) 0.3839(10) 0.3462(7) 0.0328(18) Uani d P 0.50 A 1
C C4 0.6588(3) 0.3062(3) 0.3804(3) 0.0301(6) Uani d P 0.50 A 1
H H4A 0.6927 0.2466 0.4303 0.036 Uiso calc PR 0.50 A 1
H H4B 0.5979 0.2491 0.3128 0.036 Uiso calc PR 0.50 A 1
O O1' 0.7948(12) 0.3646(11) 0.3863(7) 0.042(2) Uani d P 0.50 A 2
C C4' 0.6588(3) 0.3062(3) 0.3804(3) 0.0301(6) Uani d P 0.50 A 2
H H4'1 0.6580 0.2259 0.4151 0.036 Uiso calc PR 0.50 A 2
H H4'2 0.6142 0.2760 0.3004 0.036 Uiso calc PR 0.50 A 2
O O2 0.3628(2) 0.3377(2) 0.20517(15) 0.0328(5) Uani d . 1 A .
O O3 0.3611(2) 0.7584(2) 0.36112(18) 0.0351(5) Uani d . 1 . .
O O4 0.6205(5) 0.7826(5) 0.2746(4) 0.0869(14) Uiso d PD 0.75 B 1
H H4 0.5935 0.8544 0.3062 0.130 Uiso calc PR 0.75 B 1
C C16 0.7329(9) 0.7585(8) 0.3389(7) 0.064(2) Uiso d PD 0.75 B 1
H H16A 0.8180 0.7947 0.3137 0.096 Uiso calc PR 0.75 B 1
H H16B 0.7305 0.6606 0.3326 0.096 Uiso calc PR 0.75 B 1
H H16C 0.7329 0.8026 0.4178 0.096 Uiso calc PR 0.75 B 1
O O4' 0.7951(13) 0.6648(13) 0.3058(10) 0.064(3) Uiso d PD 0.25 C 2
H H4' 0.8378 0.6206 0.3475 0.096 Uiso calc PR 0.25 C 2
C C16' 0.720(3) 0.752(2) 0.3694(19) 0.064(6) Uiso d PD 0.25 C 2
H H16D 0.7309 0.7384 0.4471 0.097 Uiso calc PR 0.25 C 2
H H16E 0.6205 0.7331 0.3363 0.097 Uiso calc PR 0.25 C 2
H H16F 0.7556 0.8461 0.3696 0.097 Uiso calc PR 0.25 C 2
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
_geom_angle_publ_flag
O1 Si1 O1' . . 19.6(4) ?
O1 Si1 C9 . . 116.5(3) y
O1' Si1 C9 . . 100.7(4) ?
O1 Si1 C8 . . 110.1(4) y
O1' Si1 C8 . . 108.2(4) ?
C9 Si1 C8 . . 110.0(2) y
O1 Si1 C7 . . 98.4(3) y
O1' Si1 C7 . . 116.0(3) ?
C9 Si1 C7 . . 109.3(2) y
C8 Si1 C7 . . 112.0(2) y
O2 Si2 C10 . . 109.40(16) y
O2 Si2 C12 . . 104.65(15) y
C10 Si2 C12 . . 111.2(2) y
O2 Si2 C11 . . 110.01(17) y
C10 Si2 C11 . . 110.6(2) y
C12 Si2 C11 . . 110.8(2) y
O3 Si3 C15 . . 104.43(16) y
O3 Si3 C13 . . 108.77(17) y
C15 Si3 C13 . . 111.79(19) y
O3 Si3 C14 . . 109.25(17) y
C15 Si3 C14 . . 111.6(2) y
C13 Si3 C14 . . 110.7(2) y
C2 C1 C3 . 2_666 120.0(2) ?
C2 C1 C4 . . 120.2(2) ?
C3 C1 C4 2_666 . 119.8(3) ?
C1 C2 C3 . . 119.9(2) ?
C1 C2 C5 . . 119.9(3) ?
C3 C2 C5 . . 120.1(2) ?
C2 C3 C1 . 2_666 120.0(2) ?
C2 C3 C6 . . 119.9(2) ?
C1 C3 C6 2_666 . 120.0(3) ?
O2 C5 C2 . . 109.4(2) ?
O2 C5 H5A . . 109.8 ?
C2 C5 H5A . . 109.8 ?
O2 C5 H5B . . 109.8 ?
C2 C5 H5B . . 109.8 ?
H5A C5 H5B . . 108.2 ?
O3 C6 C3 . . 109.7(2) ?
O3 C6 H6A . . 109.7 ?
C3 C6 H6A . . 109.7 ?
O3 C6 H6B . . 109.7 ?
C3 C6 H6B . . 109.7 ?
H6A C6 H6B . . 108.2 ?
Si1 C7 H7A . . 109.5 ?
Si1 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
Si1 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
Si1 C8 H8A . . 109.5 ?
Si1 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
Si1 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
Si1 C9 H9A . . 109.5 ?
Si1 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
Si1 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
Si2 C10 H10A . . 109.5 ?
Si2 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
Si2 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
Si2 C11 H11A . . 109.5 ?
Si2 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
Si2 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
Si2 C12 H12A . . 109.5 ?
Si2 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
Si2 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
Si3 C13 H13A . . 109.5 ?
Si3 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
Si3 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
Si3 C14 H14A . . 109.5 ?
Si3 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
Si3 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
Si3 C15 H15A . . 109.5 ?
Si3 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
Si3 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C4 O1 Si1 . . 122.0(6) ?
O1 C4 C1 . . 107.6(5) ?
O1 C4 H4A . . 110.2 ?
C1 C4 H4A . . 110.2 ?
O1 C4 H4B . . 110.2 ?
C1 C4 H4B . . 110.2 ?
H4A C4 H4B . . 108.5 ?
C5 O2 Si2 . . 121.41(17) ?
C6 O3 Si3 . . 121.81(19) ?
C16' O4' H4' . . 109.5 ?
O4' C16' H16D . . 109.5 ?
O4' C16' H16E . . 109.5 ?
H16D C16' H16E . . 109.5 ?
O4' C16' H16F . . 109.5 ?
H16D C16' H16F . . 109.5 ?
H16E C16' H16F . . 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
Si1 O1 . 1.624(11) y
Si1 O1' . 1.694(11) ?
Si1 C9 . 1.835(4) y
Si1 C8 . 1.855(4) y
Si1 C7 . 1.862(4) y
Si2 O2 . 1.650(2) y
Si2 C10 . 1.850(4) y
Si2 C12 . 1.853(4) y
Si2 C11 . 1.855(4) y
Si3 O3 . 1.658(2) y
Si3 C15 . 1.845(4) y
Si3 C13 . 1.865(4) y
Si3 C14 . 1.867(4) y
C1 C2 . 1.397(4) ?
C1 C3 2_666 1.406(4) ?
C1 C4 . 1.513(4) ?
C2 C3 . 1.402(4) ?
C2 C5 . 1.510(4) ?
C3 C1 2_666 1.406(4) ?
C3 C6 . 1.507(4) ?
C5 O2 . 1.428(3) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 O3 . 1.436(3) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C13 H13C . 0.9800 ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
C15 H15A . 0.9800 ?
C15 H15B . 0.9800 ?
C15 H15C . 0.9800 ?
O1 C4 . 1.507(10) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
O4 C16 . 1.332(9) ?
O4 H4 . 0.8400 ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
O4' C16' . 1.391(18) ?
O4' H4' . 0.8400 ?
C16' H16D . 0.9800 ?
C16' H16E . 0.9800 ?
C16' H16F . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O4' H4' O1 0.84 2.41 2.981(15) 126.4
O4' H4' O1' 0.84 2.73 3.382(15) 135.3
O4 H4 O3 0.84 2.59 2.863(6) 100.6
