Complexing Ability of the Versatile, Redox-Active, 3-[3-(Diphenylphosphino)propylthio]- -3',4,4'-trimethyl-tetrathiafulvalene Ligand
Pascal Pellon; Grégory Gachot; Jérome Le Bris; Stéphane Marchin; Roger Carlier; Dominique Lorcy; Inorganic Chemistry 42 (2003) 2056–2060; doi:10.1021/ic026186f

data_4313407
_publ_section_title
;
 Complexing Ability of the Versatile, Redox-Active,
 3-[3-(Diphenylphosphino)propylthio]-
 -3',4,4'-trimethyl-tetrathiafulvalene Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2056
_journal_page_last               2060
_journal_paper_doi               10.1021/ic026186f
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H25 O4 P S5 W'
_chemical_formula_sum            'C28 H25 O4 P S5 W'
_chemical_formula_weight         800.6
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2001-12-12T15:56:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 99.656(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   54.705(5)
_cell_length_b                   8.049(5)
_cell_length_c                   14.243(5)
_cell_measurement_reflns_used    112665
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     6183(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.115708E-1
_diffrn_orient_matrix_UB_12      -0.82027E-2
_diffrn_orient_matrix_UB_13      0.621219E-1
_diffrn_orient_matrix_UB_21      0.137232E-1
_diffrn_orient_matrix_UB_22      0.459215E-1
_diffrn_orient_matrix_UB_23      -0.306046E-1
_diffrn_orient_matrix_UB_31      -0.46486E-2
_diffrn_orient_matrix_UB_32      0.115149
_diffrn_orient_matrix_UB_33      0.166304E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52347
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.51
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.158
_exptl_absorpt_correction_T_max  0.9136
_exptl_absorpt_correction_T_min  0.5323
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        a grid of  8 x 20 x 12 =  1920 sampling points was used
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.72
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.37
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.00018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                4797
_reflns_number_total             7121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026186fsi20030113_040054_2.cif
_cod_data_source_block           complex6
_cod_depositor_comments
;

2020-11-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C56 H50 O8 P2 S10 W2'
_cod_original_formula_weight         1601.2
_cod_original_formula_moiety         'C44 H50 O4 P2 S10 W1'
_cod_original_formula_units_Z            4
_cod_database_code               4313407
_exptl_absorpt_correction_t_ave  0.8215