Unique Radical Dearomatization and Two-Electron Reduction of a Redox-Active Ligand
Daniel A. Evans; Alan H. Cowley; Journal of the American Chemical Society 134 (2012) 15672–15675; doi:10.1021/ja307050r

data_4118673
_publ_section_title
;
 Unique Radical Dearomatization and Two-Electron Reduction of a
 Redox-Active Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15672
_journal_page_last               15675
_journal_paper_doi               10.1021/ja307050r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C88 H116 Li4 N4, C6 H6'
_chemical_formula_sum            'C94 H122 Li4 N4'
_chemical_formula_weight         1335.72
_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                100.698(9)
_cell_angle_beta                 99.299(10)
_cell_angle_gamma                105.796(9)
_cell_formula_units_Z            2
_cell_length_a                   12.916(2)
_cell_length_b                   13.320(3)
_cell_length_c                   25.385(5)
_cell_measurement_reflns_used    14176
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1552
_cell_measurement_theta_min      1.6375
_cell_volume                     4024.0(14)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            85689
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi. (2001). Rigaku Corp. Tokyo, Japan
;
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         18485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0953
_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^)+(0.0993P)^2^+3.0319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2224
_refine_ls_wR_factor_ref         0.2397
_reflns_number_gt                15079
_reflns_number_total             18485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307050r_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4024.1(14)
_cod_database_code               4118673