Synthesis and Structural Characterization of Lithium Thiolates: Dependence of Association and Aggregation on Donor Hapticity and Ligand Size and Synthesis of the First Trimeric Lithium Thiolate [Li(THF)SR]3 and the Solvent-Separated Ion Pair [Li(12-crown-4)2][SR] (R = 2,4,6-tBu3C6H2)1
Karin Ruhlandt-Senge; Ulrich Englich; Mathias O. Senge; Scott Chadwick; Inorganic Chemistry 35 (1996) 5820–5827; doi:10.1021/ic960375e

data_4323913
_publ_section_title
;
 Synthesis and Structural Characterization of Lithium Thiolates:
 Dependence of Association and Aggregation on Donor Hapticity and Ligand
 Size and Synthesis of the First Trimeric Lithium Thiolate [Li(THF)SR]3
 and the Solvent-Separated Ion Pair [Li(12-crown-4)2][SR] (R =
 2,4,6-tBu3C6H2)1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5820
_journal_page_last               5827
_journal_paper_doi               10.1021/ic960375e
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C42 H78 Li2 N4 S2'
_chemical_formula_weight         717.08
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.906(4)
_cell_length_b                   9.516(2)
_cell_length_c                   25.617(5)
_cell_volume                     4603.4(16)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130
_diffrn_measurement_device       'SIEMENS P4RA'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Ni-Filter
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            3257
_diffrn_reflns_theta_max         56.07
_diffrn_reflns_theta_min         3.45
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.257
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.00034(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3015
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_obs          0.0668
_refine_ls_shift/esd_max         -0.051
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0929P)^2^+15.6230P]
where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1891
_refine_ls_wR_factor_obs         0.1714
_reflns_number_observed          2390
_reflns_number_total             3015
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960375e_4.cif
_cod_data_source_block           '[Li(TMEDA)STrip]&v2&0'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4323913