Sulfur K-edge Spectroscopic Investigation of Second Coordination Sphere Effects in Oxomolybdenum-Thiolates: Relationship to Molybdenum-Cysteine Covalency and Electron Transfer in Sulfite Oxidase
Katrina Peariso; Matthew E. Helton; Eileen N. Duesler; Susan E. Shadle; Martin L. Kirk; Inorganic Chemistry 46 (2007) 1259–1267; doi:10.1021/ic061150z

data_4306903
_publ_section_title
;
Sulfur K-edge Spectroscopic Investigation of Second Coordination Sphere
Effects in Oxomolybdenum-Thiolates: Relationship to Molybdenum-Cysteine
Covalency and Electron Transfer in Sulfite Oxidase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1259
_journal_page_last               1267
_journal_paper_doi               10.1021/ic061150z
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C22 H28 B Mo N6 O2 S'
_chemical_formula_weight         547.31
_chemical_name_systematic
; 
 ? 
;
_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                 109.964(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.734(2)
_cell_length_b                   29.802(3)
_cell_length_c                   8.411(2)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.22
_cell_measurement_theta_min      2.79
_cell_volume                     2528.9(8)
_computing_cell_refinement       'Siemens, XSCANS, 1991'
_computing_data_collection       'Siemens, XSCANS, 1991'
_computing_data_reduction        'Siemens, XSCANS, 1991'
_computing_molecular_graphics    'Bruker SHELXTL-NT V5.1, 1998'
_computing_publication_material  'Bruker SHELXTL-NT V5.1, 1998'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10054
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'emerald green'
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+1.8400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                3611
_reflns_number_total             4703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061150z_si.cif
_cod_data_source_block           mk993a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2528.8(8)
_cod_database_code               4306903