Rapid, Covalent Addition of Phosphine to Dithiolene in a Molybdenum Tris(dithiolene). A New Structural Model for Dimethyl Sulfoxide Reductase
Neilson Nguyen; Alan J. Lough; Ulrich Fekl; Inorganic Chemistry 51 (2012) 6446–6448; doi:10.1021/ic301031b

data_4329566
_publ_section_title
;
 Rapid, Covalent Addition of Phosphine to Dithiolene in a Molybdenum
 Tris(dithiolene). A New Structural Model for Dimethyl Sulfoxide Reductase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6446
_journal_page_last               6448
_journal_paper_doi               10.1021/ic301031b
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C50 H34 F12 Mo P2 S6, 0.5(C6 H6)'
_chemical_formula_sum            'C53 H37 F12 Mo P2 S6'
_chemical_formula_weight         1252.07
_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                73.317(7)
_cell_angle_beta                 88.340(7)
_cell_angle_gamma                76.867(5)
_cell_formula_units_Z            2
_cell_length_a                   11.8783(12)
_cell_length_b                   13.9884(17)
_cell_length_c                   17.2680(15)
_cell_measurement_reflns_used    21197
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.6
_cell_volume                     2674.5(5)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.1311
_diffrn_reflns_av_sigmaI/netI    0.1841
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21197
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  1.076
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       needle
_exptl_crystal_F_000             1262
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         8593
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1848
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1949
_reflns_number_gt                4165
_reflns_number_total             8593
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic301031b_si_002_1.cif
_cod_data_source_block           k10102
_cod_database_code               4329566