The Crystal Structures of the Chiral Alkyllithium Bases [n-BuLi.(-)-Sparteine]2 and [Et2O.(i-PrLi)2.(-)-Sparteine]
Carsten Strohmann; Katja Strohfeldt; Daniel Schildbach; Journal of the American Chemical Society 125 (2003) 13672–13673; doi:10.1021/ja0374372

data_4114341
_publ_contact_author_address
;
Institut f\"ur Anorganische Chemie
Universit\"at W\"urzburg
Am Hubland
97074 W\"urzburg
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
;
 The Crystal Structures of the Chiral Alkyllithium Bases
 [n-BuLi.(-)-Sparteine]2 and [Et2O.(i-PrLi)2.(-)-Sparteine]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13672
_journal_page_last               13673
_journal_paper_doi               10.1021/ja0374372
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C38 H70 Li2 N4'
_chemical_formula_weight         596.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-08-03T13:40:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(4)
_cell_angle_beta                 122.694(3)
_cell_angle_gamma                90.000(4)
_cell_formula_units_Z            4
_cell_length_a                   24.519(6)
_cell_length_b                   9.344(2)
_cell_length_c                   19.291(5)
_cell_measurement_temperature    193(2)
_cell_volume                     3719.5(16)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.029
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36022
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                5394
_reflns_number_total             6546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0374372si20030721_123657.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        3719.3(16)
_cod_original_formula_sum        C38H70Li2N4
_cod_database_code               4114341