Models for the Molybdenum Hydroxylases: Synthesis, Characterization and Reactivity of cis-Oxosulfido-Mo(VI) Complexes
Christian J. Doonan; David J. Nielsen; Paul D. Smith; Jonathan M. White; Graham N. George; Charles G. Young; Journal of the American Chemical Society 128 (2006) 305–316; doi:10.1021/ja056109u

data_4110338
_publ_section_title
;
 Models for the Molybdenum Hydroxylases: Synthesis, Characterization and
 Reactivity of cis-Oxosulfido-Mo(VI) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              305
_journal_page_last               316
_journal_paper_doi               10.1021/ja056109u
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C38 H49 B Mo N6 O2 S'
_chemical_formula_weight         760.64
_chemical_name_systematic
;
mu-disulfidobis[(3,5-di-tert-butylphenolato)-
{hydrotris(3-isopropylpyrazol-1-yl)borato}-
oxomolybdenum(V)]
;
_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                80.907(5)
_cell_angle_beta                 70.853(5)
_cell_angle_gamma                80.146(4)
_cell_formula_units_Z            2
_cell_length_a                   11.544(3)
_cell_length_b                   11.580(3)
_cell_length_c                   17.527(4)
_cell_measurement_reflns_used    3153
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.82
_cell_measurement_theta_min      2.35
_cell_volume                     2167.6(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11532
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       plate
_exptl_crystal_F_000             796
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0796P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                5506
_reflns_number_total             7547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056109usi20050913_095107.cif
_cod_data_source_block           '[TpiPrMoOS(OC6H3tBu2-3,5)]2(mu-S2)#(5)'
_cod_original_cell_volume        2167.5(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4110338