Variable Magnetic Interactions between S = 1/2 Cation Radical Salts of Functionalizable Electron-Rich Dithiolene and Diselenolene Cp2Mo Complexes
Talia Bsaibess; Michel Guerro; Yann Le Gal; Daad Sarraf; Nathalie Bellec; Marc Fourmigué; Frédéric Barrière; Vincent Dorcet; Thierry Guizouarn; Thierry Roisnel; Dominique Lorcy; Inorganic Chemistry 52 (2013) 2162–2173; doi:10.1021/ic3025606

data_4333920
_publ_section_title
;
 Variable Magnetic Interactions between S = 1/2 Cation Radical Salts of
 Functionalizable Electron-Rich Dithiolene and Diselenolene Cp2Mo
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2162
_journal_page_last               2173
_journal_paper_doi               10.1021/ic3025606
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C15 H15 Mo N S4, C12 H4 N4'
_chemical_formula_sum            'C27 H19 Mo N5 S4'
_chemical_formula_weight         637.65
_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      2.3
_audit_creation_date             2011-05-26T17:43:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.393(5)
_cell_angle_beta                 88.209(5)
_cell_angle_gamma                73.987(5)
_cell_formula_units_Z            2
_cell_length_a                   7.8560(8)
_cell_length_b                   10.9798(13)
_cell_length_c                   15.4149(18)
_cell_measurement_reflns_used    7240
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.38
_cell_measurement_wavelength     0.71073
_cell_volume                     1276.5(3)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 1999),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999))'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19085
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+1.1384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                4997
_reflns_number_total             5703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3025606_si_001_08.cif
_cod_data_source_block           3bTCNQ
_cod_original_cell_volume        1276.5(2)
_cod_database_code               4333920