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_4323911
_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            'C24 H46 Li N3 S'
_chemical_formula_weight         415.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.805(7)
_cell_length_b                   9.206(4)
_cell_length_c                   18.923(7)
_cell_volume                     2714(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      228(2)
_diffrn_measurement_device       'Siemens P 2~1~'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube Cu K\a'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3092
_diffrn_reflns_theta_max         52.63
_diffrn_reflns_theta_min         2.84
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.132
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3088
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_obs          0.0850
_refine_ls_shift/esd_max         0.449
_refine_ls_shift/esd_mean        0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w^-1^=\s^2^(Fo^2^)+(0.1126P)^2^+3.1953P] 
where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2369
_refine_ls_wR_factor_obs         0.2017
_reflns_number_observed          2047
_reflns_number_total             3092
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960375e_2.cif
_cod_data_source_block           Li(PMDTA)STrip
_cod_original_cell_volume        2713.6(20)
_cod_database_code               4323911