A new series of bis(ene-1,2-dithiolato)tungsten(iv), -(v), -(vi) complexes as reaction centre models of tungsten enzymes: Preparation, crystal structures and spectroscopic properties.
Sugimoto, Hideki; Hatakeda, Kohei; Toyota, Kazuo; Tatemoto, Susumu; Kubo, Minoru; Ogura, Takashi; Itoh, Shinobu; Dalton transactions (Cambridge, England : 2003) 42 (2013) 3059–3070; doi:10.1039/c2dt32179c

data_7020855
_publ_section_title
;
 A new series of bis(ene-1,2-dithiolato)tungsten(iv), -(v), -(vi)
 complexes as reaction centre models of tungsten enzymes: Preparation,
 crystal structures and spectroscopic properties.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3059
_journal_page_last               3070
_journal_paper_doi               10.1039/c2dt32179c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C28 H52 N2 O9 S4 W'
_chemical_formula_sum            'C28 H52 N2 O9 S4 W'
_chemical_formula_weight         872.82
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.0939(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   20.0069(8)
_cell_length_b                   9.2346(4)
_cell_length_c                   20.0827(7)
_cell_measurement_reflns_used    32703
_cell_measurement_temperature    103
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.00
_cell_volume                     3700.9(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla, et al., 2003)'
_diffrn_ambient_temperature      103
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34711
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.399
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.210
_refine_diff_density_min         -0.750
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8424
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0254P)^2^+6.0554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                7872
_reflns_number_total             8424
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2dt32179c.txt
_cod_data_source_block           WOL
_cod_database_code               7020855