Aggregation of Donor Base Stabilized 2-Thienyllithium in a Single Crystal and in Solution: Distances from X-ray Diffraction and the Nuclear Overhauser Effect
Markus Granitzka; Ann-Christin Pöppler; Eike K. Schwarze; Daniel Stern; Thomas Schulz; Michael John; Regine Herbst-Irmer; Sushil K. Pandey; Dietmar Stalke; Journal of the American Chemical Society 134 (2012) 1344–1351; doi:10.1021/ja210382c

data_4117315
_publ_section_title
;
 Aggregation of Donor Base Stabilized 2-Thienyllithium in a Single Crystal
 and in Solution: Distances from X-ray Diffraction and the Nuclear
 Overhauser Effect
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1344
_journal_page_last               1351
_journal_paper_doi               10.1021/ja210382c
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C24 H38 Li2 O4 S2'
_chemical_formula_sum            'C24 H38 Li2 O4 S2'
_chemical_formula_weight         468.54
_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_method           SHELXL-97
_cell_angle_alpha                97.29(2)
_cell_angle_beta                 97.15(2)
_cell_angle_gamma                98.03(2)
_cell_formula_units_Z            2
_cell_length_a                   9.303(2)
_cell_length_b                   9.531(3)
_cell_length_c                   14.945(2)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.408
_cell_volume                     1287.8(5)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'BRUKER SMART APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Turbo Xray-source rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25595
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  0.9505
_exptl_absorpt_correction_T_min  0.8089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         5251
_refine_ls_number_restraints     1498
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.5012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                4626
_reflns_number_total             5251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210382c_si_002.cif
_cod_data_source_block           2
_cod_database_code               4117315