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_4110339
_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            'C36 H56 B2 Mo2 N12 O3 S2'
_chemical_formula_weight         982.55
_chemical_name_systematic
;
mu-disulfido-mu-oxobis-
[{hydrotris(3-isopropylpyrazol-1-yl)borato}-
oxomolybdenum(V)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.1940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.9498(9)
_cell_length_b                   19.1027(10)
_cell_length_c                   31.9945(17)
_cell_measurement_reflns_used    5183
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.05
_cell_measurement_theta_min      2.20
_cell_volume                     10723.1(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1210
_diffrn_reflns_av_sigmaI/netI    0.1424
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            56380
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       rod
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         18862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0896P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.2060
_reflns_number_gt                9858
_reflns_number_total             18862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056109usi20050913_095129.cif
_cod_data_source_block           '[TpiPrMoO]2(mu-S2)(mu-O)#(8)'
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4110339