#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:09:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179679 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/01/7000187.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_7000187
loop_
_publ_author_name
'Spirk, Stefan'
'Nieger, Martin'
'Belaj, Ferdinand'
'Pietschnig, Rudolf'
_publ_section_title
;
 Formation and hydrogen bonding of a novel POSS-trisilanol
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              163
_journal_page_last               167
_journal_paper_doi               10.1039/b812974f
_journal_year                    2009
_chemical_formula_moiety         'C28 H66 O12 Si7'
_chemical_formula_sum            'C28 H66 O12 Si7'
_chemical_formula_weight         791.44
_chemical_name_common
;Hepta-tert.butyl-tricyclo(7.3.3.1(5,11))heptasiloxane-ende-
endo-3,7,14-triol
;
_chemical_name_systematic
;
Hepta-tert.butyl-tricyclo[7.3.3.1(5,11)]heptasiloxane-ende-endo-3,7,14-triol
;
_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            12
_cell_length_a                   13.2424(15)
_cell_length_b                   13.2424(15)
_cell_length_c                   90.514(5)
_cell_measurement_reflns_used    303
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     13746(2)
_computing_cell_refinement       DIRAX
_computing_data_collection       Collect
_computing_data_reduction        EVALCCD
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 1 deg.'
_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  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       107
_diffrn_reflns_limit_l_min       -107
_diffrn_reflns_number            25425
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2697
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0604
_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)+(0.0237P)²+129.5700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                1812
_reflns_number_total             2697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812974f.txt
_cod_data_source_block           rp001_hy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7000187
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_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
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 1.0000 1.0000 0.06246(2) 0.0230(5) Uani 1 3 d S . .
Si2 Si 0.84674(10) 0.78225(10) 0.042632(12) 0.0219(3) Uani 1 1 d . . .
Si3 Si 0.76161(9) 0.92836(10) 0.024338(11) 0.0203(3) Uani 1 1 d . . .
O1 O 0.9048(2) 0.8716(2) 0.05637(3) 0.0293(7) Uani 1 1 d . . .
O2 O 0.9504(2) 0.7812(2) 0.03321(3) 0.0273(7) Uani 1 1 d . . .
O3 O 0.7767(2) 0.8268(2) 0.03222(3) 0.0257(7) Uani 1 1 d . . .
O4 O 0.8159(3) 0.9498(3) 0.00777(3) 0.0349(8) Uani 1 1 d D . .
H4 H 0.824(5) 0.895(3) 0.0046(5) 0.052 Uiso 1 1 d D . .
C11 C 1.0000 1.0000 0.08295(8) 0.051(3) Uani 1 3 d S . .
C12 C 0.8807(6) 0.9757(7) 0.08856(5) 0.091(3) Uani 1 1 d . . .
H12A H 0.8203 0.8986 0.0851 0.136 Uiso 1 1 calc R . .
H12B H 0.8644 1.0353 0.0847 0.136 Uiso 1 1 calc R . .
H12C H 0.8812 0.9775 0.0994 0.136 Uiso 1 1 calc R . .
C21 C 0.7447(4) 0.6322(4) 0.04965(5) 0.0337(11) Uani 1 1 d . . .
C22 C 0.6912(5) 0.5488(4) 0.03655(6) 0.0515(14) Uani 1 1 d . . .
H22A H 0.7534 0.5485 0.0307 0.077 Uiso 1 1 calc R . .
H22B H 0.6478 0.5746 0.0303 0.077 Uiso 1 1 calc R . .
H22C H 0.6382 0.4699 0.0402 0.077 Uiso 1 1 calc R . .
C23 C 0.8114(5) 0.5900(4) 0.05942(6) 0.0561(15) Uani 1 1 d . . .
H23A H 0.8730 0.5885 0.0536 0.084 Uiso 1 1 calc R . .
H23B H 0.7574 0.5114 0.0631 0.084 Uiso 1 1 calc R . .
H23C H 0.8463 0.6432 0.0678 0.084 Uiso 1 1 calc R . .
C24 C 0.6474(5) 0.6331(5) 0.05882(6) 0.0560(16) Uani 1 1 d . . .
H24A H 0.6818 0.6860 0.0672 0.084 Uiso 1 1 calc R . .
H24B H 0.5939 0.5542 0.0624 0.084 Uiso 1 1 calc R . .
H24C H 0.6045 0.6596 0.0526 0.084 Uiso 1 1 calc R . .
C31 C 0.6040(4) 0.8822(4) 0.02301(5) 0.0280(10) Uani 1 1 d . . .
C32 C 0.5469(4) 0.8599(5) 0.03825(5) 0.0475(13) Uani 1 1 d . . .
H32A H 0.5871 0.9310 0.0442 0.071 Uiso 1 1 calc R . .
H32B H 0.5523 0.7968 0.0432 0.071 Uiso 1 1 calc R . .
H32C H 0.4647 0.8377 0.0371 0.071 Uiso 1 1 calc R . .
C33 C 0.5420(4) 0.7703(4) 0.01360(5) 0.0487(13) Uani 1 1 d . . .
H33A H 0.5493 0.7080 0.0184 0.073 Uiso 1 1 calc R . .
H33B H 0.5781 0.7854 0.0038 0.073 Uiso 1 1 calc R . .
H33C H 0.4594 0.7464 0.0126 0.073 Uiso 1 1 calc R . .
C34 C 0.5906(4) 0.9778(4) 0.01516(6) 0.0448(13) Uani 1 1 d . . .
H34A H 0.6304 1.0501 0.0209 0.067 Uiso 1 1 calc R . .
H34B H 0.5077 0.9531 0.0143 0.067 Uiso 1 1 calc R . .
H34C H 0.6253 0.9911 0.0053 0.067 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Si1 O1 109.11(11) 2_765 . ?
O1 Si1 O1 109.11(11) 2_765 3_675 ?
O1 Si1 O1 109.11(11) . 3_675 ?
O1 Si1 C11 109.83(11) 2_765 . ?
O1 Si1 C11 109.83(11) . . ?
O1 Si1 C11 109.83(11) 3_675 . ?
O1 Si2 O2 108.38(16) . . ?
O1 Si2 O3 109.12(15) . . ?
O2 Si2 O3 109.73(14) . . ?
O1 Si2 C21 110.01(18) . . ?
O2 Si2 C21 109.52(18) . . ?
O3 Si2 C21 110.05(18) . . ?
O2 Si3 O3 111.31(15) 3_675 . ?
O2 Si3 O4 107.74(16) 3_675 . ?
O3 Si3 O4 108.93(16) . . ?
O2 Si3 C31 110.16(17) 3_675 . ?
O3 Si3 C31 109.80(17) . . ?
O4 Si3 C31 108.84(18) . . ?
Si2 O1 Si1 149.39(19) . . ?
Si3 O2 Si2 157.8(2) 2_765 . ?
Si3 O3 Si2 152.34(19) . . ?
Si3 O4 H4 113(3) . . ?
C12 C11 C12 109.6(3) 3_675 2_765 ?
C12 C11 C12 109.6(3) 3_675 . ?
C12 C11 C12 109.6(3) 2_765 . ?
C12 C11 Si1 109.3(3) 3_675 . ?
C12 C11 Si1 109.3(3) 2_765 . ?
C12 C11 Si1 109.3(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C22 C21 C23 109.0(4) . . ?
C22 C21 C24 109.6(4) . . ?
C23 C21 C24 109.2(4) . . ?
C22 C21 Si2 109.3(3) . . ?
C23 C21 Si2 109.9(3) . . ?
C24 C21 Si2 109.8(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C32 C31 C34 109.1(4) . . ?
C32 C31 C33 109.8(4) . . ?
C34 C31 C33 108.1(4) . . ?
C32 C31 Si3 111.7(3) . . ?
C34 C31 Si3 109.3(3) . . ?
C33 C31 Si3 108.7(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 O1 1.625(3) 2_765 ?
Si1 O1 1.625(3) . ?
Si1 O1 1.625(3) 3_675 ?
Si1 C11 1.855(8) . ?
Si2 O1 1.621(3) . ?
Si2 O2 1.623(3) . ?
Si2 O3 1.627(3) . ?
Si2 C21 1.869(4) . ?
Si3 O2 1.609(3) 3_675 ?
Si3 O3 1.620(3) . ?
Si3 O4 1.626(3) . ?
Si3 C31 1.863(4) . ?
O2 Si3 1.609(3) 2_765 ?
O4 H4 0.833(19) . ?
C11 C12 1.532(7) 3_675 ?
C11 C12 1.532(7) 2_765 ?
C11 C12 1.532(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 C22 1.532(6) . ?
C21 C23 1.538(6) . ?
C21 C24 1.538(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C32 1.529(6) . ?
C31 C34 1.537(6) . ?
C31 C33 1.542(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 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
_geom_hbond_site_symmetry_A
O4 H4 O4 0.833(19) 1.80(2) 2.596(4) 158(5) 21_655
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Si2 O1 Si1 51.4(4) . . . . ?
O3 Si2 O1 Si1 -68.0(4) . . . . ?
C21 Si2 O1 Si1 171.2(4) . . . . ?
O1 Si1 O1 Si2 -52.2(4) 2_765 . . . ?
O1 Si1 O1 Si2 66.9(4) 3_675 . . . ?
C11 Si1 O1 Si2 -172.7(3) . . . . ?
O1 Si2 O2 Si3 -50.3(5) . . . 2_765 ?
O3 Si2 O2 Si3 68.7(5) . . . 2_765 ?
C21 Si2 O2 Si3 -170.4(5) . . . 2_765 ?
O2 Si3 O3 Si2 -25.0(4) 3_675 . . . ?
O4 Si3 O3 Si2 93.7(4) . . . . ?
C31 Si3 O3 Si2 -147.2(4) . . . . ?
O1 Si2 O3 Si3 37.5(4) . . . . ?
O2 Si2 O3 Si3 -81.1(4) . . . . ?
C21 Si2 O3 Si3 158.3(4) . . . . ?
O1 Si1 C11 C12 56.7(3) 2_765 . . 3_675 ?
O1 Si1 C11 C12 176.7(3) . . . 3_675 ?
O1 Si1 C11 C12 -63.3(3) 3_675 . . 3_675 ?
O1 Si1 C11 C12 -63.3(3) 2_765 . . 2_765 ?
O1 Si1 C11 C12 56.7(3) . . . 2_765 ?
O1 Si1 C11 C12 176.7(3) 3_675 . . 2_765 ?
O1 Si1 C11 C12 176.7(3) 2_765 . . . ?
O1 Si1 C11 C12 -63.3(3) . . . . ?
O1 Si1 C11 C12 56.7(3) 3_675 . . . ?
O1 Si2 C21 C22 -179.7(3) . . . . ?
O2 Si2 C21 C22 -60.7(4) . . . . ?
O3 Si2 C21 C22 60.0(4) . . . . ?
O1 Si2 C21 C23 -60.0(4) . . . . ?
O2 Si2 C21 C23 59.0(4) . . . . ?
O3 Si2 C21 C23 179.7(3) . . . . ?
O1 Si2 C21 C24 60.0(4) . . . . ?
O2 Si2 C21 C24 179.0(3) . . . . ?
O3 Si2 C21 C24 -60.3(4) . . . . ?
O2 Si3 C31 C32 -62.3(4) 3_675 . . . ?
O3 Si3 C31 C32 60.6(4) . . . . ?
O4 Si3 C31 C32 179.8(3) . . . . ?
O2 Si3 C31 C34 58.5(3) 3_675 . . . ?
O3 Si3 C31 C34 -178.6(3) . . . . ?
O4 Si3 C31 C34 -59.4(3) . . . . ?
O2 Si3 C31 C33 176.4(3) 3_675 . . . ?
O3 Si3 C31 C33 -60.7(3) . . . . ?
O4 Si3 C31 C33 58.4(3) . . . . ?
