Salt-Free Reducing Reagent of Bis(trimethylsilyl)cyclohexadiene Mediates Multielectron Reduction of Chloride Complexes of W(VI) and W(IV)
Hayato Tsurugi; Hiromasa Tanahashi; Haruka Nishiyama; Waldemar Fegler; Teruhiko Saito; Andreas Sauer; Jun Okuda; Kazushi Mashima; Journal of the American Chemical Society 135 (2013) 5986–5989; doi:10.1021/ja401589a

data_4119641
_publ_section_title
;
 Salt-Free Reducing Reagent of Bis(trimethylsilyl)cyclohexadiene Mediates
 Multielectron Reduction of Chloride Complexes of W(VI) and W(IV)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5986
_journal_page_last               5989
_journal_paper_doi               10.1021/ja401589a
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
'C52 H72 Cl5 N4 W2, 0.5 (C26 H36 N2), 0.5 (C6 H6)'
_chemical_formula_sum            'C68 H93 Cl5 N5 W2'
_chemical_formula_weight         1525.48
_chemical_name_common            7
_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_creation_method           SHELXL-97
_cell_angle_alpha                80.947(10)
_cell_angle_beta                 83.188(9)
_cell_angle_gamma                74.034(6)
_cell_formula_units_Z            2
_cell_length_a                   11.850(4)
_cell_length_b                   12.830(4)
_cell_length_c                   25.097(8)
_cell_measurement_reflns_used    8386
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.16
_cell_volume                     3611(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0660
_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       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34683
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    3.410
_exptl_absorpt_correction_T_max  0.6468
_exptl_absorpt_correction_T_min  0.3902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.041
_refine_diff_density_min         -2.267
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         16098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0482P)^2^+14.8393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                13103
_reflns_number_total             16098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja401589a_si_001_6.cif
_cod_data_source_block           7
_cod_original_cell_volume        3611.3(19)
_cod_database_code               4119641