Oxo-Mo(IV)(dithiolene)thiolato Complexes: Analogue of Reduced Sulfite Oxidase
Joyee Mitra; Sabyasachi Sarkar; Inorganic Chemistry 52 (2013) 3032–3042; doi:10.1021/ic302485c

data_4334148
_publ_contact_author_name        'Sabyasachi Sarkar'
_publ_section_title
;
 Oxo-Mo(IV)(dithiolene)thiolato Complexes: Analogue of Reduced Sulfite
 Oxidase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3032
_journal_page_last               3042
_journal_paper_doi               10.1021/ic302485c
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C22 H12 Mo N5 O3 S3, C24 H20 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H36 Cl4 Mo N5 O3 P S3'
_chemical_formula_weight         1095.74
_chemical_name_systematic
;
 ?
;
_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                87.666(5)
_cell_angle_beta                 89.071(5)
_cell_angle_gamma                78.301(5)
_cell_formula_units_Z            2
_cell_length_a                   10.981(5)
_cell_length_b                   12.218(5)
_cell_length_c                   18.179(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2386.3(16)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 ( Bruker, 2003)'
_computing_molecular_graphics    'Diamond 3.1e, Ortep'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13248
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.201
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1938
_reflns_number_gt                7757
_reflns_number_total             9113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302485c_si_002_10.cif
_cod_data_source_block           6b
_cod_database_code               4334148