Formation and Reactivity of a Persistent Radical in a Dinuclear Molybdenum Complex
Aaron M. Appel; Suh-Jane Lee; James A. Franz; Daniel L. DuBois; M. Rakowski DuBois; Jerome C. Birnbaum; Brendan Twamley; Journal of the American Chemical Society 130 (2008) 8940–8951; doi:10.1021/ja078115r

data_4108013
_publ_section_title
;
 Formation and Reactivity of a Persistent Radical in a Dinuclear
 Molybdenum Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8940
_journal_page_last               8951
_journal_paper_doi               10.1021/ja078115r
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C28 H40 Mo2 S4, C6 H6'
_chemical_formula_sum            'C34 H46 Mo2 S4'
_chemical_formula_weight         774.83
_chemical_name_common            '[Cp*2Mo2S2S(Bz)S(Me)] + C6H6'
_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                87.631(2)
_cell_angle_beta                 84.018(2)
_cell_angle_gamma                78.866(1)
_cell_formula_units_Z            4
_cell_length_a                   10.5202(4)
_cell_length_b                   12.5398(5)
_cell_length_c                   26.2385(10)
_cell_measurement_reflns_used    9408
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.20
_cell_volume                     3377.0(2)
_computing_cell_refinement       'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_data_collection       'SMART v. 5.632 (Bruker, 2006)'
_computing_data_reduction        'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_molecular_graphics    'XP, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)'
_computing_structure_refinement  'XL, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_structure_solution    'XS, SHELXTL  v. 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            48347
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.9417
_exptl_absorpt_correction_T_min  0.7647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2004/1 (Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         12243
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0385P)^2^+1.9286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                9539
_reflns_number_total             12243
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja078115r-file004.cif
_cod_data_source_block           S4MeBz
_cod_database_code               4108013