Synthesis and Structures of Bis(dithiolene)tungsten(IV,VI) Thiolate and Selenolate Complexes: Approaches to the Active Sites of Molybdenum and Tungsten Formate Dehydrogenases
Stanislav Groysman; R. H. Holm; Inorganic Chemistry 46 (2007) 4090–4102; doi:10.1021/ic062441a

data_4307937
_publ_contact_author_address
;
Department of Chemistry and Chemical Biology
Harvard University
12 Oxford Street
Cambridge, MA 02138
USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_fax         '617 496-9289'
_publ_contact_author_name        'Richard H. Holm'
_publ_contact_author_phone       '617 495-0853'
_publ_section_title
;
Synthesis and Structures of Bis(dithiolene)tungsten(IV,VI) Thiolate and
Selenolate Complexes: Approaches to the Active Sites of Molybdenum and
Tungsten Formate Dehydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4090
_journal_page_last               4102
_journal_paper_doi               10.1021/ic062441a
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C20 H41 N O S4 Se W'
_chemical_formula_weight         702.59
_chemical_name_common            (Et4N)[12]
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.435(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5206(9)
_cell_length_b                   16.5220(17)
_cell_length_c                   17.5703(18)
_cell_measurement_temperature    193(2)
_cell_volume                     2688.2(5)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       \w
_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  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18636
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    5.974
_exptl_absorpt_correction_T_max  0.5865
_exptl_absorpt_correction_T_min  0.2673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.409
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                4111
_reflns_number_total             6406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062441asi20070323_105048_07.cif
_cod_data_source_block           stas19
_cod_database_code               4307937