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_4323912
_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            'C54 H62 Li2 O4 S2'
_chemical_formula_weight         853.04
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.141(3)
_cell_length_b                   12.381(2)
_cell_length_c                   14.664(3)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      0
_cell_volume                     2377.3(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       '2\q - \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4726
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.156
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.006
_refine_ls_goodness_of_fit_obs   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_obs          0.0524
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
  w^-1^=\s^2^(Fo^2^)+(0.0389P)^2^+1.7765P] '
where P=(Fo^2^+2Fc^2^0)/3' 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1405
_refine_ls_wR_factor_obs         0.1145
_reflns_number_observed          2622
_reflns_number_total             4192
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960375e_3.cif
_cod_data_source_block           '[Li(THF)&v2&0STrityl]&v2&0'
_cod_original_formula_sum        'Li2 S2 C54 H62 O4'
_cod_database_code               4323912