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_4334141
_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         'C16 H36 N, C22 H13 Mo N4 O S3'
_chemical_formula_sum            'C38 H49 Mo N5 O S3'
_chemical_formula_weight         783.94
_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                84.521(5)
_cell_angle_beta                 84.034(5)
_cell_angle_gamma                79.187(5)
_cell_formula_units_Z            2
_cell_length_a                   8.981(5)
_cell_length_b                   12.170(5)
_cell_length_c                   19.631(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2089.8(15)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.960
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11403
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.25
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.579
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                6641
_reflns_number_total             8440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302485c_si_002_03.cif
_cod_data_source_block           2b
_cod_database_code               4334141