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_4108014
_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         'C21 H33 Mo2 S4'
_chemical_formula_sum            'C42 H66 Mo4 S8'
_chemical_formula_weight         1211.19
_chemical_name_common            '[Cp*2Mo2S3SMe]2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6316(4)
_cell_length_b                   11.6316(4)
_cell_length_c                   35.549(2)
_cell_measurement_reflns_used    8817
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.29
_cell_volume                     4809.6(4)
_computing_cell_refinement       'Bruker, 2006; SAINT+  v. 7.23a'
_computing_data_collection       'Bruker, 2006; SMART v. 5.632'
_computing_data_reduction        'Bruker, 2006; SAINT+  v. 7.23a'
_computing_molecular_graphics    'Bruker, 2003; XP, SHELXTL  v. 6.14'
_computing_publication_material  'Bruker, 2001; XCIF, SHELXTL, v. 6.14'
_computing_structure_refinement  'Bruker, 2003; XL,SHELXTL  v. 6.14''
_computing_structure_solution    'Bruker, 2003; XS, SHELXTL  v. 6.14'
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            68317
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_T_max  0.8616
_exptl_absorpt_correction_T_min  0.6559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2004/1 ; Bruker, 2004'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       plate
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4348
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0272P)^2^+7.0221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                4228
_reflns_number_total             4348
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja078115r-file005.cif
_cod_data_source_block           (S4Me)2
_cod_database_code               4108014