A Biomimetic Approach to Oxidized Sites in the Xanthine Oxidoreductase Family: Synthesis and Stereochemistry of Tungsten(VI) Analogue Complexes
Stanislav Groysman; Jun-Jieh Wang; Ranitendranath Tagore; Sonny C. Lee; Richard H. Holm; Journal of the American Chemical Society 130 (2008) 12794–12807; doi:10.1021/ja804000k

data_4108372
_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
;
 A Biomimetic Approach to Oxidized Sites in the Xanthine Oxidoreductase
 Family: Synthesis and Stereochemistry of Tungsten(VI) Analogue Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12794
_journal_page_last               12807
_journal_paper_doi               10.1021/ja804000k
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         '(C8 H20 N 1+), (C24 H19 O S4 Si W 1-)'
_chemical_formula_sum            'C32 H39 N O S4 Si W'
_chemical_formula_weight         793.82
_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                79.190(2)
_cell_angle_beta                 88.356(2)
_cell_angle_gamma                64.1320(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2753(9)
_cell_length_b                   9.9505(10)
_cell_length_c                   20.736(2)
_cell_measurement_temperature    193(2)
_cell_volume                     1688.4(3)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\w scans, 0.3\% rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12775
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.729
_exptl_absorpt_correction_T_max  0.6047
_exptl_absorpt_correction_T_min  0.4008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.711
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         8550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                7339
_reflns_number_total             8550
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja804000k_si_001_8.cif
_cod_data_source_block           17
_cod_database_code               4108372