Synthesis, Structure, and Dynamic Behavior of Cyclopentadienyl-Lithium, -Sodium, and -Potassium Annelated with Bicyclo[2.2.2]octene Units: A Systematic Study on Site Exchange of Alkali Metals on a Cyclopentadienyl Ring in Tetrahydrofuran
Tohru Nishinaga; Daisuke Yamazaki; Helmut Stahr; Atsushi Wakamiya; Koichi Komatsu; Journal of the American Chemical Society 125 (2003) 7324–7335; doi:10.1021/ja0346431

data_4113824
_publ_contact_author_address
;
    Institute for Chemical Research, Kyoto University, Gokasho, Uji, 
    Kyoto 611-0011, Japan. 
;
_publ_contact_author_email       ' komatsu@scl.kyoto-u.ac.jp'
_publ_contact_author_fax         ' +81-774-38-3178 '
_publ_contact_author_name        ' Koichi Komatsu '
_publ_contact_author_phone       ' +81-774-38-3172 '
_publ_section_title
;
 Synthesis, Structure, and Dynamic Behavior of Cyclopentadienyl-Lithium,
 -Sodium, and -Potassium Annelated with Bicyclo[2.2.2]octene Units: A
 Systematic Study on Site Exchange of Alkali Metals on a Cyclopentadienyl
 Ring in Tetrahydrofuran
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7324
_journal_page_last               7335
_journal_paper_doi               10.1021/ja0346431
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C23 H25 Li'
_chemical_formula_sum            'C35 H49 Li O3'
_chemical_formula_weight         524.68
_chemical_name_common
5-phenyl-1,2:3,4-bis(bicyclo[2.2.2]octeno)cyclopentadienyllithium-(THF)3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             ' Wed Oct 11 2001 '
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.4024(12)
_cell_length_b                   17.796(2)
_cell_length_c                   31.256(4)
_cell_measurement_temperature    123(2)
_cell_volume                     5786.1(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      123(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27771
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       prism
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1143P)^2^+9.8876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2161
_reflns_number_gt                3876
_reflns_number_total             5038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0346431si20030213_020714.cif
_cod_data_source_block           1Li(THF)3
_cod_original_cell_volume        5786.2(11)
_cod_database_code               4113824