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_4108012
_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_sum            'C47.5 H70 F6 Mo4 O6 S10'
_chemical_formula_weight         1555.40
_chemical_name_common            '[Cp*sMo(S2)SSMe][O3SCF3]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 132.887(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.703(5)
_cell_length_b                   20.664(3)
_cell_length_c                   23.485(4)
_cell_measurement_reflns_used    7971
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      2.12
_cell_volume                     11984(3)
_computing_cell_refinement       'Bruker, 2006; SAINT+  v. 7.23a'
_computing_data_collection       'Bruker, 2001; SMART v. 5.630'
_computing_data_reduction        'Bruker, 2006; SAINT+  v. 7.23a'
_computing_molecular_graphics    'Bruker, 2003; XP, SHELXTL  v. 6.14'
_computing_publication_material  'Bruker, 2003; 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0940
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            136982
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_correction_T_min  0.5565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Twinabs (Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       needle
_exptl_crystal_F_000             6280
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.950
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         26319
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0962P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1756
_reflns_number_gt                16703
_reflns_number_total             26319
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja078115r-file003.cif
_cod_data_source_block           S4Me+
_cod_original_formula_sum        'C47.50 H70 F6 Mo4 O6 S10'
_cod_database_code               4108012