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_4110340
_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            'C28 H34 B Cl0 Mo N6 O2 S'
_chemical_formula_weight         625.42
_chemical_name_systematic
;
{hydrotris(3-isopropylpyrazol-1-yl)borato}-
(2-mercaptonaphthalato)oxomolybdenum(V)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   16.101(5)
_cell_length_b                   17.766(5)
_cell_length_c                   20.420(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5841(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1061
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            67500
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.557
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prism
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.752
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.647
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.647
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+11.2455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1724
_reflns_number_gt                3441
_reflns_number_total             5139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056109usi20050913_095216.cif
_cod_data_source_block           TpiPrMoO(OSC10H6-2)#(11)
_cod_database_code               4110340