Crystal Structures of n-BuLi Adducts with (R,R)-TMCDA and the Consequences for the Deprotonation of Benzene
Carsten Strohmann; Viktoria H. Gessner; Journal of the American Chemical Society 130 (2008) 11719–11725; doi:10.1021/ja8017187

data_4108257
_publ_contact_author_address
;
Institut fuer Anorganische Chemie
Universitaet Wuerzburg
Am Hubland
97074 Wuerzburg
Germany
;
_publ_contact_author_email       mail@carsten-strohmann.de
_publ_contact_author_fax         '0049 931 888 4605'
_publ_contact_author_name        'Carsten Strohmann'
_publ_contact_author_phone       '0049 931 888 4613'
_publ_section_title
;
 Crystal Structures of n-BuLi Adducts with (R,R)-TMCDA and the
 Consequences for the Deprotonation of Benzene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11719
_journal_page_last               11725
_journal_paper_doi               10.1021/ja8017187
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C36 H80 Li4 N4'
_chemical_formula_weight         596.8
_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_date             2007-08-16T21:01:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.217(9)
_cell_angle_beta                 95.838(10)
_cell_angle_gamma                105.366(11)
_cell_formula_units_Z            4
_cell_length_a                   13.427(5)
_cell_length_b                   13.440(5)
_cell_length_c                   24.950(9)
_cell_measurement_temperature    173(2)
_cell_volume                     4202(3)
_computing_cell_refinement       'SAINTPLUS 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART 5.622 (Bruker AXS, 2001)'
_computing_data_reduction        'SAINTPLUS 6.02 (Bruker AXS, 1999)'
_computing_molecular_graphics    'Ortep-3 V1.073 (Farrugia, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker APEX-CCD'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.06
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32682
_diffrn_reflns_theta_full        24
_diffrn_reflns_theta_max         24
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.052
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     948
_refine_ls_number_reflns         13210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1133P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2097
_refine_ls_wR_factor_ref         0.2336
_reflns_number_gt                6671
_reflns_number_total             13210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8017187-file001.cif
_cod_data_source_block           vi180407
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