Rubidium-Mediated Birch-Type Reduction of 1,2-Diphenylbenzene in Tetrahydrofuran
Sven Krieck; Robert Kretschmer; Helmar Görls; Matthias Westerhausen; Journal of the American Chemical Society 133 (2011) 6960–6963; doi:10.1021/ja2018527

data_4106125
_publ_contact_author
;
      Matthias Westerhausen
      Institut f\"ur anorganische und analytische Chemie
      Friedrich-Schiller-Universit\"at Jena
      August-Bebel-Str. 2
      07743 Jena
      Germany
;
_publ_contact_author_email       m.we@uni-jena.de
_publ_contact_author_fax         '03641 948 102'
_publ_contact_author_phone       '03641 948 110'
_publ_section_title
;
 Rubidium-Mediated Birch-Type Reduction of 1,2-Diphenylbenzene in
 Tetrahydrofuran
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6960
_journal_page_last               6963
_journal_paper_doi               10.1021/ja2018527
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C108 H90 Rb6'
_chemical_formula_sum            'C18 H15 Rb'
_chemical_formula_weight         316.77
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2010-12-06 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   21.1577(3)
_cell_length_b                   21.1577(3)
_cell_length_c                   17.4764(2)
_cell_measurement_reflns_used    12413
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      3.99
_cell_volume                     6775.16(16)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12413
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    3.272
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            opalizerend
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+43.8646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                2550
_reflns_number_total             3413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2018527_si_001.cif
_cod_data_source_block           FO4205
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4106125