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_4313406
_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         'C52 H50 Mo O4 P2 S10, C1 H2 Cl2'
_chemical_formula_structural     'C53 H52 MO1 P2 O4 S10 Cl2'
_chemical_formula_sum            'C53 H52 Cl2 Mo O4 P2 S10'
_chemical_formula_weight         1302.33
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_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             2001-07-18T11:29:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                85.5664(8)
_cell_angle_beta                 73.1536(8)
_cell_angle_gamma                77.2220(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5784(2)
_cell_length_b                   13.5208(3)
_cell_length_c                   18.6103(5)
_cell_measurement_reflns_used    68049
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     2953.91(11)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.466661E-1
_diffrn_orient_matrix_UB_12      -0.709153E-1
_diffrn_orient_matrix_UB_13      0.24989E-2
_diffrn_orient_matrix_UB_21      0.32436E-2
_diffrn_orient_matrix_UB_22      0.193678E-1
_diffrn_orient_matrix_UB_23      0.732594E-1
_diffrn_orient_matrix_UB_31      -0.357643E-1
_diffrn_orient_matrix_UB_32      0.420289E-1
_diffrn_orient_matrix_UB_33      -0.103498E-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  0.0749
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56183
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         1.91
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  1.0144
_exptl_absorpt_correction_T_min  0.9344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.728
_refine_diff_density_min         -1.08
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0040(6)
_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   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         11699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+2.2364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                8621
_reflns_number_total             11699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026186fsi20030113_040054_1.cif
_cod_data_source_block           complex4
_cod_database_code               4313406