Molybdenum Chalcogenobenzimidato Complexes: Radical Synthesis and Nitrile Extrusion via β-EPh (E = S, Se, and Te) Elimination
Arjun Mendiratta; Christopher C. Cummins; Olga P. Kryatova; Elena V. Rybak-Akimova; James E. McDonough; Carl D. Hoff; Inorganic Chemistry 42 (2003) 8621–8623; doi:10.1021/ic035077d

data_4312837
_publ_section_title
;
 Molybdenum Chalcogenobenzimidato Complexes: Radical Synthesis and Nitrile
 Extrusion via \b-EPh (E = S, Se, and Te) Elimination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8621
_journal_page_last               8623
_journal_paper_doi               10.1021/ic035077d
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C42 H59 Mo N3 Te'
_chemical_formula_weight         829.46
_chemical_name_common            3_Te
_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                91.445(2)
_cell_angle_beta                 90.692(2)
_cell_angle_gamma                90.663(2)
_cell_formula_units_Z            4
_cell_length_a                   11.1740(12)
_cell_length_b                   18.1215(19)
_cell_length_c                   20.134(2)
_cell_measurement_reflns_used    10405
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.25
_cell_volume                     4075.0(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15076
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.2689
_exptl_absorpt_correction_T_min  0.2184
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.452
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         10405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+35.3424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1533
_reflns_number_gt                9778
_reflns_number_total             10405
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ic035077dsi20030915_124914_2.cif
_cod_data_source_block           002247m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312837