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#$Date: 2016-03-22 11:36:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178907 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/36/4113648.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_4113648
loop_
_publ_author_name
'Cosmina Dutan'
'Sylvie Choua'
'Théo Berclaz'
'Michel Geoffroy'
'Nicolas Mézailles'
'Audrey Moores'
'Louis Ricard'
'Pascal Le Floch'
_publ_contact_author             'Louis Ricard'
_publ_contact_author_address
;
                    Labo DCPH,
                    Ecole Polytechnique
                    Route de Saclay
                    91128 Palaiseau
                    France
;
_publ_contact_author_email       louis.ricard@polytechnique.fr
_publ_contact_author_fax         01-69-33-39-90
_publ_contact_author_phone       01-69-33-45-72
_publ_section_title
;
 Electron Transfer between Two Silyl-Substituted Phenylene Rings:
 EPR/ENDOR Spectra, DFT Calculations, and Crystal Structure of the
 One-Electron Reduction Compound of a Di(m-silylphenylenedisiloxane)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4487
_journal_page_last               4494
_journal_paper_doi               10.1021/ja0209060
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C20 H32 O2 Si4'
_chemical_formula_weight         416.82
_chemical_name_systematic
;
 ?
;
_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                100.590(5)
_cell_angle_beta                 106.340(5)
_cell_angle_gamma                106.110(5)
_cell_formula_units_Z            1
_cell_length_a                   7.617(5)
_cell_length_b                   8.567(5)
_cell_length_c                   10.404(5)
_cell_measurement_reflns_used    251
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.0
_cell_volume                     600.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0501
_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       -14
_diffrn_reflns_number            4853
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.9746
_exptl_absorpt_correction_T_min  0.9500
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       plate
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         3476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0368P)²+0.1553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                3021
_reflns_number_total             3476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0209060_1.cif
_cod_data_source_block           cyclosi;compound4
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4113648
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si 0.62111(4) 0.14210(4) 0.83745(3) 0.02152(10) Uani 1 1 d .
Si2 Si 0.59672(5) -0.22167(4) 0.71293(3) 0.02309(10) Uani 1 1 d .
O1 O 0.62726(14) -0.04952(11) 0.82911(9) 0.0299(2) Uani 1 1 d .
C1 C 0.55048(16) 0.20534(13) 0.56859(12) 0.0207(2) Uani 1 1 d .
H1 H 0.4178 0.1736 0.5621 0.025 Uiso 1 1 calc R
C2 C 0.68996(16) 0.21024(14) 0.69171(12) 0.0211(2) Uani 1 1 d .
C3 C 0.88441(17) 0.25861(16) 0.69892(14) 0.0291(3) Uani 1 1 d .
H3 H 0.9831 0.2644 0.7813 0.035 Uiso 1 1 calc R
C4 C 0.93588(18) 0.29825(18) 0.58790(15) 0.0337(3) Uani 1 1 d .
H4 H 1.0686 0.3297 0.5945 0.040 Uiso 1 1 calc R
C5 C 0.79414(18) 0.29199(16) 0.46759(14) 0.0288(3) Uani 1 1 d .
H5 H 0.8312 0.3201 0.3925 0.035 Uiso 1 1 calc R
C6 C 0.59674(17) 0.24491(14) 0.45451(12) 0.0215(2) Uani 1 1 d .
C7 C 0.8031(2) 0.28403(17) 1.00836(14) 0.0346(3) Uani 1 1 d .
H7A H 0.7706 0.2438 1.0840 0.052 Uiso 1 1 calc R
H7B H 0.8014 0.3995 1.0178 0.052 Uiso 1 1 calc R
H7C H 0.9335 0.2837 1.0136 0.052 Uiso 1 1 calc R
C8 C 0.37239(18) 0.13985(17) 0.82376(15) 0.0305(3) Uani 1 1 d .
H8A H 0.2780 0.0616 0.7342 0.046 Uiso 1 1 calc R
H8B H 0.3680 0.2541 0.8294 0.046 Uiso 1 1 calc R
H8C H 0.3397 0.1027 0.9004 0.046 Uiso 1 1 calc R
C9 C 0.8283(2) -0.2090(2) 0.68320(17) 0.0416(4) Uani 1 1 d .
H9A H 0.8639 -0.1175 0.6407 0.062 Uiso 1 1 calc R
H9B H 0.8115 -0.3168 0.6205 0.062 Uiso 1 1 calc R
H9C H 0.9319 -0.1861 0.7726 0.062 Uiso 1 1 calc R
C10 C 0.5202(2) -0.40209(16) 0.78388(15) 0.0350(3) Uani 1 1 d .
H10A H 0.6177 -0.3825 0.8754 0.053 Uiso 1 1 calc R
H10B H 0.5087 -0.5068 0.7199 0.053 Uiso 1 1 calc R
H10C H 0.3936 -0.4123 0.7939 0.053 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.02560(17) 0.02133(16) 0.01731(17) 0.00662(12) 0.00622(12) 0.00832(12)
Si2 0.03101(18) 0.02562(17) 0.02125(17) 0.01171(13) 0.01281(13) 0.01579(13)
O1 0.0455(5) 0.0257(4) 0.0217(4) 0.0102(3) 0.0106(4) 0.0163(4)
C1 0.0235(5) 0.0202(5) 0.0216(5) 0.0070(4) 0.0102(4) 0.0093(4)
C2 0.0242(5) 0.0190(5) 0.0205(5) 0.0060(4) 0.0079(4) 0.0078(4)
C3 0.0231(5) 0.0335(6) 0.0269(6) 0.0096(5) 0.0057(5) 0.0069(5)
C4 0.0227(5) 0.0421(7) 0.0353(7) 0.0125(6) 0.0126(5) 0.0063(5)
C5 0.0297(6) 0.0320(6) 0.0286(6) 0.0122(5) 0.0154(5) 0.0091(5)
C6 0.0275(5) 0.0191(5) 0.0224(5) 0.0078(4) 0.0120(4) 0.0104(4)
C7 0.0381(7) 0.0350(7) 0.0216(6) 0.0045(5) 0.0045(5) 0.0072(6)
C8 0.0309(6) 0.0354(7) 0.0319(7) 0.0158(5) 0.0161(5) 0.0125(5)
C9 0.0354(7) 0.0673(10) 0.0386(8) 0.0266(8) 0.0177(6) 0.0303(7)
C10 0.0590(9) 0.0276(6) 0.0321(7) 0.0164(5) 0.0230(7) 0.0233(6)
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_3
O1 Si1 C8 109.08(6) .
O1 Si1 C7 107.24(6) .
C8 Si1 C7 110.68(7) .
O1 Si1 C2 108.67(5) .
C8 Si1 C2 111.18(6) .
C7 Si1 C2 109.88(7) .
O1 Si2 C9 110.28(7) .
O1 Si2 C10 107.06(7) .
C9 Si2 C10 109.92(7) .
O1 Si2 C6 108.90(6) 2_656
C9 Si2 C6 109.88(7) 2_656
C10 Si2 C6 110.76(7) 2_656
Si2 O1 Si1 139.61(6) .
C2 C1 C6 123.34(11) .
C2 C1 C1 92.51(8) 2_656
C6 C1 C1 91.81(8) 2_656
C3 C2 C1 117.13(11) .
C3 C2 Si1 120.53(9) .
C1 C2 Si1 122.22(9) .
C3 C2 C6 116.09(8) 2_656
C1 C2 C6 77.82(7) 2_656
Si1 C2 C6 74.66(5) 2_656
C4 C3 C2 121.21(12) .
C5 C4 C3 120.15(12) .
C4 C5 C6 121.21(12) .
C1 C6 C5 116.97(11) .
C1 C6 Si2 121.82(9) 2_656
C5 C6 Si2 121.08(9) 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O1 1.6423(13) .
Si1 C8 1.8538(18) .
Si1 C7 1.8560(15) .
Si1 C2 1.8756(14) .
Si2 O1 1.6390(12) .
Si2 C9 1.8524(18) .
Si2 C10 1.8535(15) .
Si2 C6 1.8738(14) 2_656
C1 C2 1.4004(16) .
C1 C6 1.4017(16) .
C1 C1 3.323(3) 2_656
C2 C3 1.3988(18) .
C2 C6 3.676(2) 2_656
C3 C4 1.3886(19) .
C4 C5 1.385(2) .
C5 C6 1.4036(19) .
C6 Si2 1.8738(14) 2_656
