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_4316896
_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, Br'
_chemical_formula_sum            'C13 H10 Br S5 W'
_chemical_formula_weight         590.27
_chemical_name_common            'Cp2W(dmit), Br'
_chemical_name_systematic
;
Bis(cyclopentadienyl)(&,3-dithiole-2-thione)-4,5-dithiolate)tunsten(V),
bromide
;
_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_date             2009-09-22T15:46:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.26(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.705(3)
_cell_length_b                   7.2790(15)
_cell_length_c                   12.856(3)
_cell_measurement_reflns_used    5774
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.51
_cell_volume                     1553.9(6)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21364
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    10.662
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.482550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0178
_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^)+(0.0106P)^2^+1.8527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0337
_refine_ls_wR_factor_ref         0.0355
_reflns_number_gt                3135
_reflns_number_total             3562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1006296_si_001_3.cif
_cod_data_source_block           WBr
_cod_original_cell_volume        1553.8(5)
_cod_database_code               4316896