Synthesis and reactivity of silylated tetrathiafulvalenes
Hameau, Aurélien; Guyon, Fabrice; Knorr, Michael; Däschlein, Christian; Strohmann, Carsten; Avarvari, Narcis; Dalton Transactions  (2008) 4866–4876; doi:10.1039/b803947j

data_7004194
_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
_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/[\s^2^(Fo^2^)+(0.0556P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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