#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:14:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179745 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/41/7004194.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_7004194
loop_
_publ_author_name
'Hameau, Aurélien'
'Guyon, Fabrice'
'Knorr, Michael'
'Däschlein, Christian'
'Strohmann, Carsten'
'Avarvari, Narcis'
_publ_section_title
;
 Synthesis and reactivity of silylated tetrathiafulvalenes
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              4866
_journal_page_last               4876
_journal_paper_doi               10.1039/b803947j
_journal_year                    2008
_chemical_formula_moiety         C54H44S4Si4
_chemical_formula_sum            'C54 H44 S4 Si4'
_chemical_formula_weight         933.49
_chemical_name_common            TTF(SiPh2H)4
_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                98.430(16)
_cell_angle_beta                 94.867(16)
_cell_angle_gamma                107.326(16)
_cell_formula_units_Z            1
_cell_length_a                   10.2738(14)
_cell_length_b                   10.9233(16)
_cell_length_c                   11.8812(15)
_cell_measurement_reflns_used    7933
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      2.0
_cell_volume                     1247.4(3)
_computing_cell_refinement       'SELECT, CELL [STOE-IPDS]'
_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.6
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Rotation, Phi. incr. = 2.0'
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12471
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.8414
_exptl_absorpt_correction_T_min  0.8236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
wingx software, R. H. Blessing, Acta Cryst. 1995, A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0374
_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)+(0.0556P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                3198
_reflns_number_total             4520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b803947j.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004194
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
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.11223(6) 0.06036(5) 0.35785(4) 0.05017(15) Uani 1 1 d . . .
Si1 Si 0.26651(6) -0.02881(6) 0.16501(4) 0.04471(15) Uani 1 1 d . . .
S2 S 0.01227(6) -0.19367(5) 0.42929(5) 0.05423(16) Uani 1 1 d . . .
Si2 Si 0.16633(7) -0.33313(6) 0.26757(5) 0.04972(17) Uani 1 1 d . . .
H1 H 0.208(2) -0.1177(18) 0.0668(15) 0.048(5) Uiso 1 1 d . . .
H2 H 0.212(2) -0.317(2) 0.1679(16) 0.057(6) Uiso 1 1 d . . .
C1 C 0.1579(2) -0.06876(19) 0.28236(15) 0.0428(5) Uani 1 1 d . . .
C2 C 0.1140(2) -0.1850(2) 0.31659(16) 0.0462(5) Uani 1 1 d . . .
C5 C 0.5129(3) -0.0892(2) 0.13113(18) 0.0582(6) Uani 1 1 d . . .
H5 H 0.4716 -0.1222 0.0556 0.070 Uiso 1 1 calc R . .
C16 C 0.3062(3) -0.3409(2) 0.3741(2) 0.0583(6) Uani 1 1 d . . .
C4 C 0.4427(2) -0.03433(19) 0.20857(16) 0.0459(5) Uani 1 1 d . . .
C22 C 0.0137(2) -0.4828(2) 0.24333(17) 0.0525(5) Uani 1 1 d . . .
C3 C 0.0262(2) -0.02725(19) 0.45690(16) 0.0438(5) Uani 1 1 d . . .
C27 C 0.0128(3) -0.5919(2) 0.2901(2) 0.0647(6) Uani 1 1 d . . .
H27 H 0.0884 -0.5889 0.3406 0.078 Uiso 1 1 calc R . .
C9 C 0.5089(2) 0.0155(2) 0.32097(18) 0.0558(6) Uani 1 1 d . . .
H9 H 0.4649 0.0532 0.3747 0.067 Uiso 1 1 calc R . .
C10 C 0.2689(2) 0.1356(2) 0.13598(16) 0.0494(5) Uani 1 1 d . . .
C11 C 0.3879(3) 0.2387(2) 0.1523(2) 0.0662(7) Uani 1 1 d . . .
H11 H 0.4701 0.2283 0.1816 0.079 Uiso 1 1 calc R . .
C25 C -0.2065(3) -0.7131(3) 0.1879(2) 0.0781(8) Uani 1 1 d . . .
H25 H -0.2793 -0.7905 0.1679 0.094 Uiso 1 1 calc R . .
C8 C 0.6384(3) 0.0093(2) 0.3531(2) 0.0687(7) Uani 1 1 d . . .
H8 H 0.6812 0.0429 0.4281 0.082 Uiso 1 1 calc R . .
C15 C 0.1488(3) 0.1566(3) 0.0919(2) 0.0677(7) Uani 1 1 d . . .
H15 H 0.0662 0.0886 0.0802 0.081 Uiso 1 1 calc R . .
C6 C 0.6424(3) -0.0959(3) 0.1640(2) 0.0738(7) Uani 1 1 d . . .
H6 H 0.6875 -0.1337 0.1112 0.089 Uiso 1 1 calc R . .
C17 C 0.2849(3) -0.3646(3) 0.4848(2) 0.0762(8) Uani 1 1 d . . .
H17 H 0.1973 -0.3785 0.5061 0.091 Uiso 1 1 calc R . .
C26 C -0.0976(3) -0.7049(2) 0.2634(2) 0.0738(7) Uani 1 1 d . . .
H26 H -0.0968 -0.7760 0.2977 0.089 Uiso 1 1 calc R . .
C21 C 0.4384(3) -0.3186(2) 0.3475(3) 0.0765(8) Uani 1 1 d . . .
H21 H 0.4566 -0.3021 0.2749 0.092 Uiso 1 1 calc R . .
C23 C -0.0998(3) -0.4930(3) 0.1696(3) 0.0912(10) Uani 1 1 d . . .
H23 H -0.1036 -0.4211 0.1377 0.109 Uiso 1 1 calc R . .
C13 C 0.2681(4) 0.3749(3) 0.0820(2) 0.0869(9) Uani 1 1 d . . .
H13 H 0.2683 0.4549 0.0639 0.104 Uiso 1 1 calc R . .
C7 C 0.7042(3) -0.0461(3) 0.2751(3) 0.0734(7) Uani 1 1 d . . .
H7 H 0.7916 -0.0500 0.2975 0.088 Uiso 1 1 calc R . .
C14 C 0.1491(4) 0.2746(3) 0.0652(2) 0.0835(9) Uani 1 1 d . . .
H14 H 0.0675 0.2857 0.0355 0.100 Uiso 1 1 calc R . .
C19 C 0.5194(4) -0.3444(3) 0.5335(3) 0.0961(11) Uani 1 1 d . . .
H19 H 0.5905 -0.3451 0.5871 0.115 Uiso 1 1 calc R . .
C12 C 0.3882(4) 0.3586(3) 0.1257(3) 0.0887(9) Uani 1 1 d . . .
H12 H 0.4699 0.4277 0.1376 0.106 Uiso 1 1 calc R . .
C20 C 0.5466(3) -0.3203(3) 0.4279(4) 0.0936(10) Uani 1 1 d . . .
H20 H 0.6353 -0.3052 0.4087 0.112 Uiso 1 1 calc R . .
C18 C 0.3900(4) -0.3677(3) 0.5628(3) 0.0906(10) Uani 1 1 d . . .
H18 H 0.3729 -0.3856 0.6353 0.109 Uiso 1 1 calc R . .
C24 C -0.2095(3) -0.6073(3) 0.1410(3) 0.1025(12) Uani 1 1 d . . .
H24 H -0.2851 -0.6118 0.0897 0.123 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'
S S 0.1246 0.1234 '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
C3 S1 C1 96.57(9) . . ?
C4 Si1 C10 111.88(10) . . ?
C4 Si1 C1 109.66(9) . . ?
C10 Si1 C1 108.51(9) . . ?
C4 Si1 H1 109.6(8) . . ?
C10 Si1 H1 107.9(8) . . ?
C1 Si1 H1 109.3(8) . . ?
C3 S2 C2 96.45(10) . . ?
C16 Si2 C22 112.27(10) . . ?
C16 Si2 C2 109.75(9) . . ?
C22 Si2 C2 110.08(10) . . ?
C16 Si2 H2 110.4(9) . . ?
C22 Si2 H2 108.8(9) . . ?
C2 Si2 H2 105.3(9) . . ?
C2 C1 S1 116.71(16) . . ?
C2 C1 Si1 126.82(16) . . ?
S1 C1 Si1 116.44(11) . . ?
C1 C2 S2 116.68(16) . . ?
C1 C2 Si2 126.45(16) . . ?
S2 C2 Si2 116.51(11) . . ?
C6 C5 C4 121.4(2) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C21 C16 C17 116.8(2) . . ?
C21 C16 Si2 120.5(2) . . ?
C17 C16 Si2 122.6(2) . . ?
C5 C4 C9 117.5(2) . . ?
C5 C4 Si1 121.38(15) . . ?
C9 C4 Si1 121.11(17) . . ?
C23 C22 C27 116.6(2) . . ?
C23 C22 Si2 120.34(17) . . ?
C27 C22 Si2 122.80(18) . . ?
C3 C3 S1 123.1(2) 2_556 . ?
C3 C3 S2 123.7(2) 2_556 . ?
S1 C3 S2 113.23(11) . . ?
C26 C27 C22 121.5(2) . . ?
C26 C27 H27 119.3 . . ?
C22 C27 H27 119.3 . . ?
C8 C9 C4 120.8(2) . . ?
C8 C9 H9 119.6 . . ?
C4 C9 H9 119.6 . . ?
C11 C10 C15 117.1(2) . . ?
C11 C10 Si1 122.14(18) . . ?
C15 C10 Si1 120.75(18) . . ?
C10 C11 C12 121.2(2) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C26 C25 C24 119.6(3) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C7 C8 C9 120.2(2) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C14 C15 C10 121.8(3) . . ?
C14 C15 H15 119.1 . . ?
C10 C15 H15 119.1 . . ?
C7 C6 C5 119.4(2) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C18 C17 C16 121.7(3) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C25 C26 C27 120.4(2) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C16 C21 C20 121.5(3) . . ?
C16 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C22 C23 C24 121.9(2) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 H23 119.1 . . ?
C14 C13 C12 120.0(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C8 C7 C6 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C13 C14 C15 120.0(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C20 C19 C18 121.4(3) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C13 C12 C11 119.9(3) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C19 C20 C21 118.9(3) . . ?
C19 C20 H20 120.6 . . ?
C21 C20 H20 120.6 . . ?
C19 C18 C17 119.7(3) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C25 C24 C23 119.9(3) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
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
S1 C3 1.756(2) . ?
S1 C1 1.763(2) . ?
Si1 C4 1.861(2) . ?
Si1 C10 1.872(2) . ?
Si1 C1 1.880(2) . ?
Si1 H1 1.366(18) . ?
S2 C3 1.759(2) . ?
S2 C2 1.764(2) . ?
Si2 C16 1.863(2) . ?
Si2 C22 1.864(2) . ?
Si2 C2 1.881(2) . ?
Si2 H2 1.33(2) . ?
C1 C2 1.350(3) . ?
C5 C6 1.381(3) . ?
C5 C4 1.391(3) . ?
C5 H5 0.9300 . ?
C16 C21 1.380(4) . ?
C16 C17 1.399(3) . ?
C4 C9 1.398(3) . ?
C22 C23 1.364(3) . ?
C22 C27 1.385(3) . ?
C3 C3 1.342(4) 2_556 ?
C27 C26 1.379(3) . ?
C27 H27 0.9300 . ?
C9 C8 1.376(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.370(3) . ?
C10 C15 1.394(3) . ?
C11 C12 1.391(3) . ?
C11 H11 0.9300 . ?
C25 C26 1.346(4) . ?
C25 C24 1.362(4) . ?
C25 H25 0.9300 . ?
C8 C7 1.366(4) . ?
C8 H8 0.9300 . ?
C15 C14 1.371(4) . ?
C15 H15 0.9300 . ?
C6 C7 1.373(4) . ?
C6 H6 0.9300 . ?
C17 C18 1.374(4) . ?
C17 H17 0.9300 . ?
C26 H26 0.9300 . ?
C21 C20 1.409(4) . ?
C21 H21 0.9300 . ?
C23 C24 1.384(4) . ?
C23 H23 0.9300 . ?
C13 C14 1.354(4) . ?
C13 C12 1.368(4) . ?
C13 H13 0.9300 . ?
C7 H7 0.9300 . ?
C14 H14 0.9300 . ?
C19 C20 1.354(5) . ?
C19 C18 1.363(5) . ?
C19 H19 0.9300 . ?
C12 H12 0.9300 . ?
C20 H20 0.9300 . ?
C18 H18 0.9300 . ?
C24 H24 0.9300 . ?
