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_4323910
_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            'C28 H38 Li N3 S'
_chemical_formula_weight         455.61
_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                 106.90(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.152(3)
_cell_length_b                   15.260(3)
_cell_length_c                   14.764(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2619.6(12)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measurement_device       'Siemens P2~1~'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0848
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3884
_diffrn_reflns_theta_max         57.02
_diffrn_reflns_theta_min         3.80
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.227
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_obs          0.0644
_refine_ls_shift/esd_max         0.032
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w^-1^=[\s^2^(Fo^2^)+(0.0697P)^2^+2.0424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1624
_refine_ls_wR_factor_obs         0.1426
_reflns_number_observed          2526
_reflns_number_total             3531
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960375e_1.cif
_cod_data_source_block           Li(PMDTA)STrityl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value
'w^-1^=[\s^2^(Fo^2^)+(0.0697P)^2^+2.0424P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w^-1^=[\s^2^(Fo^2^)+(0.0697P)^2^+2.0424P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323910