A Model for the Active-Site Formation Process in DMSO Reductase Family Molybdenum Enzymes Involving Oxido-Alcoholato and Oxido-Thiolato Molybdenum(VI) Core Structures.
Sugimoto, Hideki; Sato, Masanori; Asano, Kaori; Suzuki, Takeyuki; Mieda, Kaoru; Ogura, Takashi; Matsumoto, Takashi; Giles, Logan J.; Pokhrel, Amrit; Kirk, Martin L.; Itoh, Shinobu; Inorganic chemistry 55 (2016) 1542–1550; doi:10.1021/acs.inorgchem.5b02395

data_4346943
_publ_section_title
;
 A Model for the Active-Site Formation Process in DMSO Reductase Family
 Molybdenum Enzymes Involving Oxido-Alcoholato and Oxido-Thiolato
 Molybdenum(VI) Core Structures.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1542
_journal_page_last               1550
_journal_paper_doi               10.1021/acs.inorgchem.5b02395
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C41 H43 Mo O11 P S4'
_chemical_formula_sum            'C41 H43 Mo O11 P S4'
_chemical_formula_weight         966.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-27
_audit_creation_method           'by CrystalStructure 4.2'
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.879(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   11.0598(7)
_cell_length_b                   16.9292(11)
_cell_length_c                   11.8567(8)
_cell_measurement_reflns_used    17036
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.60
_cell_volume                     2180.1(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b32'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b32'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12615
_diffrn_reflns_point_group_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.010
_diffrn_reflns_theta_min         3.796
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.079
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             996.00
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.84
_refine_ls_abs_structure_details
;
 Flack x determined using 1658 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     558
_refine_ls_number_reflns         7074
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0653P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.795
_reflns_Friedel_fraction_max     0.791
_reflns_number_gt                5057
_reflns_number_total             7074
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic5b02395_si_002.cif
_cod_data_source_block           global
_cod_database_code               4346943
_shelx_res_checksum              56855
_shelx_hkl_checksum              58036