Structural Distortions upon Oxidation in Heteroleptic [Cp2W(dmit)] Tungsten Dithiolene Complex: Combined Structural, Spectroscopic, and Magnetic Studies
Eric W. Reinheimer; Iwona Olejniczak; Andrzej Łapiński; Roman Świetlik; Olivier Jeannin; Marc Fourmigué; Inorganic Chemistry 49 (2010) 9777–9787; doi:10.1021/ic1006296

data_4316895
_publ_section_title
;
 Structural Distortions upon Oxidation in Heteroleptic [Cp2W(dmit)]
 Tungsten Dithiolene Complex: Combined Structural, Spectroscopic, and
 Magnetic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9777
_journal_page_last               9787
_journal_paper_doi               10.1021/ic1006296
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C13 H10 S5 W, P F6'
_chemical_formula_sum            'C13 H10 F6 P S5 W'
_chemical_formula_weight         655.33
_chemical_name_common            'Cp~2~W(dmit), PF~6~'
_chemical_name_systematic
; 
   [4,5-disulfanyl-1,3-dithiole-2-thionato]bis[h-cyclopentadienyl]
 tungsten[V] hexafluorophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.861(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6514(7)
_cell_length_b                   15.6801(13)
_cell_length_c                   17.442(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.5
_cell_volume                     1818.9(3)
_computing_cell_refinement       'SELECT (Stoe IPDS)'
_computing_data_collection       'EXPOSE (Stoe IPDS)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS)'
_computing_molecular_graphics    'DIAMOND 2.1a (Brandenburg, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Rotation, \D\Y = 1.2'
_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  0.1046
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17078
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    7.067
_exptl_absorpt_correction_T_max  0.7204
_exptl_absorpt_correction_T_min  0.1514
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.384
_exptl_crystal_size_min          0.173
_refine_diff_density_max         2.944
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                3113
_reflns_number_total             4347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1006296_si_001_2.cif
_cod_data_source_block           wdmpf6a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4316895