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_4118675
_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         'C43.50 H54 N2 O'
_chemical_formula_sum            'C43.5 H54 N2 O'
_chemical_formula_weight         620.89
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.876(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.840(3)
_cell_length_b                   15.555(4)
_cell_length_c                   23.010(6)
_cell_measurement_reflns_used    7788
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.8787
_cell_measurement_theta_min      1.5805
_cell_volume                     3877.8(18)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku SCX-Mini Mercury 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     0.71075
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40438
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.9944
_exptl_absorpt_correction_T_min  0.9797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi. (2001). Rigaku Corp. Tokyo, Japan
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       prism
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8888
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0827P)^2^+1.1585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1785
_reflns_number_gt                6576
_reflns_number_total             8888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307050r_si_003.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C43.50 H54 N2 O'
_cod_database_code               4118675