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_4117317
_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         'C13 H26 Li N3 S'
_chemical_formula_sum            'C13 H26 Li N3 S'
_chemical_formula_weight         263.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.466(2)
_cell_length_b                   15.573(3)
_cell_length_c                   12.226(2)
_cell_measurement_reflns_used    5037
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.74
_cell_volume                     1609.1(6)
_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_publication_material  '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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart ApexII Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17890
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            'light red'
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3055
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0438P)^2^+0.2014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                2449
_reflns_number_total             3055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210382c_si_004.cif
_cod_data_source_block           5
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4117317