Template Effects of Lithium Salts on the Crystallization of Diazasulfates: X-ray Structures of {THF.Li2[O2S(NtBu)2]}8.2LiOH.2LiCl and {(THF.Li)2[O2S(NtBu)2].(THF)LiCl}2
Justin K. Brask; Tristram Chivers; Glenn P. A. Yap; Inorganic Chemistry 38 (1999) 5588–5592; doi:10.1021/ic990632q

data_4322434
_publ_section_title
;
 Template Effects of Lithium Salts on the Crystallization of
 Diazasulfates: X-ray Structures of {THF.Li2[O2S(NtBu)2]}8.2LiOH.2LiCl and
 {(THF.Li)2[O2S(NtBu)2].(THF)LiCl}2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5588
_journal_page_last               5592
_journal_paper_doi               10.1021/ic990632q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C110 H240 Cl2 Li20 N16 O28 S8'
_chemical_formula_weight         2701.36
_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                 107.3810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.5570(12)
_cell_length_b                   15.7307(10)
_cell_length_c                   28.0629(18)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     7817.9(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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    0.0417
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8396
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.988674
_exptl_absorpt_correction_T_min  0.665348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.00031(17)
_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_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         8396
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.179
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1140P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                5913
_reflns_number_total             8396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990632q_1.cif
_cod_data_source_block           tc011
_cod_database_code               4322434