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_4110335
_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 H41 B Mo N6 O2 S'
_chemical_formula_weight         632.49
_chemical_name_systematic
;
(2-sec-butylphenolato)-
{hydrotris(3-isopropylpyrazol-1-yl)borato}-
oxothiomolybdenum(VI)
;
_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                76.061(4)
_cell_angle_beta                 77.347(3)
_cell_angle_gamma                75.608(3)
_cell_formula_units_Z            2
_cell_length_a                   8.628(2)
_cell_length_b                   12.607(3)
_cell_length_c                   15.573(4)
_cell_measurement_reflns_used    1217
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.70
_cell_measurement_theta_min      2.47
_cell_volume                     1569.5(7)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5301
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red/brown
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          2.597
_refine_ls_shift/su_mean         0.163
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                2638
_reflns_number_total             3978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056109usi20050913_093818.cif
_cod_data_source_block           TpiPrMoOS(OC6H4sBu-2)#(1)
_cod_original_cell_volume        1569.4(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4110335