Redox-active proligands from the direct connection of 1,3-dithiol-2-one to tetrathiafulvalene (TTF): syntheses, characterizations and metal complexation
Camerel, Franck; Jeannin, Olivier; Yzambart, Gilles; Fabre, Bruno; Lorcy, Dominique; Fourmigué, Marc; New Journal of Chemistry 37 (2013) 992–; doi:10.1039/c3nj41097h

data_7053038
_publ_section_title
;
 Redox-active proligands from the direct connection of 1,3-dithiol-2-one
 to tetrathiafulvalene (TTF): syntheses, characterizations and metal
 complexation
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              992
_journal_paper_doi               10.1039/c3nj41097h
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C30 H34 O2 S13'
_chemical_formula_sum            'C30 H34 O2 S13'
_chemical_formula_weight         843.35
_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                95.476(5)
_cell_angle_beta                 90.546(5)
_cell_angle_gamma                91.274(5)
_cell_formula_units_Z            2
_cell_length_a                   7.569(5)
_cell_length_b                   14.725(5)
_cell_length_c                   18.158(5)
_cell_measurement_reflns_used    4267
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.82
_cell_measurement_theta_min      2.69
_cell_volume                     2013.9(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_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  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1192
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29876
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sword
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         9193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1813
_refine_ls_R_factor_gt           0.0668
_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^)+(0.1269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.2442
_reflns_number_gt                3954
_reflns_number_total             9193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj41097h.txt
_cod_data_source_block           import3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7053038