#------------------------------------------------------------------------------
#$Date: 2015-09-08 09:24:02 +0300 (Tue, 08 Sep 2015) $
#$Revision: 155199 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/20/7222038.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_7222038
loop_
_publ_author_name
'Percino, M. Judith'
'Pacheco, José Alberto'
'Soriano, Guillermo'
'Ceron, Margarita'
'Castro, María Eugenia'
'Chapela, Víctor M.'
'bonilla-cruz, jose'
'Lara, Tania'
'Flores, Mildred'
'Saldivar, Enrique'
_publ_section_title
;
 Synthesis, characterization and theoretical calculations of model
 compounds of silanols catalyzed by TEMPO to elucidate the presence of
 Si-O-Si and Si-O-N bonds.
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA10056A
_journal_year                    2015
_chemical_formula_moiety         'C36 H30 O Si2'
_chemical_formula_sum            'C36 H30 O Si2'
_chemical_formula_weight         534.78
_chemical_melting_point          498
_chemical_name_common            'hexaphenyldisiloxane '
_chemical_name_systematic        di(triphenylsilane)ether
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2013
_audit_update_record
;
2015-05-09 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.951(4)
_cell_angle_beta                 111.779(4)
_cell_angle_gamma                113.352(4)
_cell_formula_units_Z            1
_cell_length_a                   8.5829(4)
_cell_length_b                   9.4856(4)
_cell_length_c                   10.9694(5)
_cell_measurement_reflns_used    7041
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.95
_cell_measurement_theta_min      4.51
_cell_volume                     727.71(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9218
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.896
_diffrn_reflns_theta_min         4.541
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             282
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0360P)²+0.3704P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2707
_reflns_number_total             2833
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ra10056a1.cif
_cod_data_source_block           '[di(triphenylsilane)ether]'
_cod_original_cell_volume        727.71(6)
_cod_database_code               7222038
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C -0.12889(18) -0.09447(14) 0.69656(13) 0.0198(3) Uani 1 1 d . . .
C2 C -0.3149(2) -0.19993(17) 0.59728(14) 0.0273(3) Uani 1 1 d . . .
H2 H -0.3571 -0.1903 0.5068 0.033 Uiso 1 1 calc R U .
C3 C -0.4394(2) -0.31904(18) 0.62915(16) 0.0323(3) Uani 1 1 d . . .
H3 H -0.5653 -0.3899 0.5605 0.039 Uiso 1 1 calc R U .
C4 C -0.3800(2) -0.33421(16) 0.76031(16) 0.0293(3) Uani 1 1 d . . .
H4 H -0.4649 -0.4155 0.7819 0.035 Uiso 1 1 calc R U .
C5 C -0.1967(2) -0.23093(16) 0.86022(15) 0.0265(3) Uani 1 1 d . . .
H5 H -0.1556 -0.2412 0.9505 0.032 Uiso 1 1 calc R U .
C6 C -0.07258(18) -0.11194(15) 0.82839(13) 0.0215(3) Uani 1 1 d . . .
H6 H 0.0529 -0.0412 0.8978 0.026 Uiso 1 1 calc R U .
C7 C 0.28916(18) 0.12124(15) 0.77453(13) 0.0209(3) Uani 1 1 d . . .
C8 C 0.3611(2) 0.01474(16) 0.75904(15) 0.0278(3) Uani 1 1 d . . .
H8 H 0.2830 -0.0824 0.6857 0.033 Uiso 1 1 calc R U .
C9 C 0.5444(2) 0.04859(18) 0.84905(17) 0.0337(3) Uani 1 1 d . . .
H9 H 0.5903 -0.0254 0.8375 0.040 Uiso 1 1 calc R U .
C10 C 0.6595(2) 0.19032(19) 0.95534(16) 0.0331(3) Uani 1 1 d . . .
H10 H 0.7847 0.2136 1.0170 0.040 Uiso 1 1 calc R U .
C11 C 0.5930(2) 0.29854(19) 0.97223(15) 0.0320(3) Uani 1 1 d . . .
H11 H 0.6729 0.3966 1.0446 0.038 Uiso 1 1 calc R U .
C12 C 0.40892(19) 0.26333(16) 0.88297(14) 0.0250(3) Uani 1 1 d . . .
H12 H 0.3637 0.3375 0.8960 0.030 Uiso 1 1 calc R U .
C13 C 0.00314(18) 0.24806(15) 0.67306(13) 0.0203(3) Uani 1 1 d . . .
C14 C 0.11180(19) 0.38318(16) 0.64541(14) 0.0253(3) Uani 1 1 d . . .
H14 H 0.2017 0.3809 0.6155 0.030 Uiso 1 1 calc R U .
C15 C 0.0912(2) 0.52089(16) 0.66072(15) 0.0302(3) Uani 1 1 d . . .
H15 H 0.1682 0.6122 0.6429 0.036 Uiso 1 1 calc R U .
C16 C -0.0411(2) 0.52537(17) 0.70181(15) 0.0320(3) Uani 1 1 d . . .
H16 H -0.0558 0.6194 0.7115 0.038 Uiso 1 1 calc R U .
C17 C -0.1516(2) 0.3933(2) 0.72865(18) 0.0392(4) Uani 1 1 d . . .
H17 H -0.2430 0.3960 0.7565 0.047 Uiso 1 1 calc R U .
C18 C -0.1291(2) 0.25591(18) 0.71486(17) 0.0336(3) Uani 1 1 d . . .
H18 H -0.2052 0.1657 0.7343 0.040 Uiso 1 1 calc R U .
O1 O 0.0000 0.0000 0.5000 0.0255(3) Uani 1 2 d S . P
Si1 Si 0.03907(5) 0.06718(4) 0.65595(3) 0.01775(11) Uani 1 1 d . . .
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
C6 C1 C2 117.84(12) .
C6 C1 Si1 120.71(10) .
C2 C1 Si1 121.44(10) .
C3 C2 C1 120.90(13) .
C3 C2 H2 119.5 .
C1 C2 H2 119.5 .
C4 C3 C2 120.13(13) .
C4 C3 H3 119.9 .
C2 C3 H3 119.9 .
C3 C4 C5 119.93(13) .
C3 C4 H4 120.0 .
C5 C4 H4 120.0 .
C4 C5 C6 119.91(13) .
C4 C5 H5 120.0 .
C6 C5 H5 120.0 .
C5 C6 C1 121.27(12) .
C5 C6 H6 119.4 .
C1 C6 H6 119.4 .
C12 C7 C8 117.58(12) .
C12 C7 Si1 122.53(10) .
C8 C7 Si1 119.86(10) .
C9 C8 C7 121.27(13) .
C9 C8 H8 119.4 .
C7 C8 H8 119.4 .
C10 C9 C8 119.76(13) .
C10 C9 H9 120.1 .
C8 C9 H9 120.1 .
C9 C10 C11 120.23(13) .
C9 C10 H10 119.9 .
C11 C10 H10 119.9 .
C10 C11 C12 119.80(14) .
C10 C11 H11 120.1 .
C12 C11 H11 120.1 .
C11 C12 C7 121.35(13) .
C11 C12 H12 119.3 .
C7 C12 H12 119.3 .
C14 C13 C18 117.44(12) .
C14 C13 Si1 120.17(10) .
C18 C13 Si1 122.39(10) .
C15 C14 C13 121.29(13) .
C15 C14 H14 119.4 .
C13 C14 H14 119.4 .
C16 C15 C14 120.11(13) .
C16 C15 H15 119.9 .
C14 C15 H15 119.9 .
C17 C16 C15 119.89(13) .
C17 C16 H16 120.1 .
C15 C16 H16 120.1 .
C16 C17 C18 119.93(14) .
C16 C17 H17 120.0 .
C18 C17 H17 120.0 .
C17 C18 C13 121.32(14) .
C17 C18 H18 119.3 .
C13 C18 H18 119.3 .
Si1 O1 Si1 180.0 2_556
O1 Si1 C13 109.69(4) .
O1 Si1 C7 108.53(4) .
C13 Si1 C7 109.80(6) .
O1 Si1 C1 108.72(4) .
C13 Si1 C1 110.30(6) .
C7 Si1 C1 109.77(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.3953(18) .
C1 C2 1.3978(19) .
C1 Si1 1.8692(13) .
C2 C3 1.394(2) .
C2 H2 0.9500 .
C3 C4 1.381(2) .
C3 H3 0.9500 .
C4 C5 1.383(2) .
C4 H4 0.9500 .
C5 C6 1.3910(18) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C12 1.3964(19) .
C7 C8 1.4023(18) .
C7 Si1 1.8654(13) .
C8 C9 1.391(2) .
C8 H8 0.9500 .
C9 C10 1.382(2) .
C9 H9 0.9500 .
C10 C11 1.385(2) .
C10 H10 0.9500 .
C11 C12 1.390(2) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.3955(18) .
C13 C18 1.3962(19) .
C13 Si1 1.8627(13) .
C14 C15 1.3877(19) .
C14 H14 0.9500 .
C15 C16 1.381(2) .
C15 H15 0.9500 .
C16 C17 1.377(2) .
C16 H16 0.9500 .
C17 C18 1.393(2) .
C17 H17 0.9500 .
C18 H18 0.9500 .
O1 Si1 1.6198(3) .
O1 Si1 1.6199(3) 2_556
