Harnessing Redox-Active Ligands for Low-Barrier Radical Addition at Oxorhenium Complexes
Cameron A. Lippert; Kenneth I. Hardcastle; Jake D. Soper; Inorganic Chemistry 50 (2011) 9864–9878; doi:10.1021/ic200923q

data_4326469
_publ_contact_author_address
;School of Chemistry and Biochemistry
Georgia Institute of Technology
901 Atlantic Drive NW
Atlanta, GA  30332-0400
;
_publ_contact_author_email       jake.soper@chemistry.gatech.edu
_publ_contact_author_name        'Jake D. Soper'
_publ_contact_author_phone       404-894-4022
_publ_section_title
;
 Harnessing Redox-Active Ligands for Low-Barrier Radical Addition at
 Oxorhenium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9864
_journal_page_last               9878
_journal_paper_doi               10.1021/ic200923q
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C80 H100 N4 O6 Re2'
_chemical_formula_sum            'C80 H100 N4 O6 Re2'
_chemical_formula_weight         1586.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 102.387(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   25.507(8)
_cell_length_b                   14.111(4)
_cell_length_c                   10.667(3)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.43
_cell_volume                     3750.0(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37675
_diffrn_reflns_theta_full        30.41
_diffrn_reflns_theta_max         30.41
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    3.278
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.108
_refine_diff_density_max         3.229
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.204
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.503(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         11306
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0570P)^2^+26.3075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                9763
_reflns_number_total             11306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200923q_si_002_4.cif
_cod_data_source_block           '[Re2(O)2(ap)2(isq)2]'
_cod_original_cell_volume        3749.7(19)
_cod_database_code               4326469