Synthesis and Structures of Bis(dithiolene)-Tungsten(IV) Complexes Related to the Active Sites of Tungstoenzymes
Kie-Moon Sung; R. H. Holm; Inorganic Chemistry 39 (2000) 1275–1281; doi:10.1021/ic991153u

data_4300206
_publ_section_title
;
Synthesis and Structures of Bis(dithiolene)-Tungsten(IV) Complexes
Related to the Active Sites of Tungstoenzymes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1275
_journal_page_last               1281
_journal_paper_doi               10.1021/ic991153u
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C23 H37 N O S5 W'
_chemical_formula_weight         687.69
_space_group_IT_number           2
_symmetry_cell_setting           Triclinic
_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                88.9150(10)
_cell_angle_beta                 82.50
_cell_angle_gamma                84.2420(10)
_cell_formula_units_Z            6
_cell_length_a                   10.1257(2)
_cell_length_b                   16.17560(10)
_cell_length_c                   25.8216(5)
_cell_measurement_temperature    213(2)
_cell_volume                     4171.89(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0877
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18067
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         0.80
_exptl_absorpt_coefficient_mu    4.545
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.884
_refine_diff_density_min         -1.757
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         10874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                7904
_reflns_number_total             10874
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        4171.87(12)
_cod_database_code               4300206