Heteroscorpionate complexes based on bis(3,5-di-<i>tert</i>-butylpyrazol-1-yl)dithioacetate
Tampier, Stefan; Burzlaff, Nicolai; Acta Crystallographica Section C 69 (2013) 981–985; doi:10.1107/S0108270113021148

data_2019159
_publ_section_title
;
 Heteroscorpionate complexes based on
 bis(3,5-di-<i>tert</i>-butylpyrazol-1-yl)dithioacetate
;
_journal_coeditor_code           YP3040
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              981
_journal_page_last               985
_journal_paper_doi               10.1107/S0108270113021148
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Li (C24 H39 N4 S2) (C4 H8 O1)], C4 H8 O'
_chemical_formula_moiety         'C28 H47 Li N4 O S2, C4 H8 O'
_chemical_formula_sum            'C32 H55 Li N4 O2 S2'
_chemical_formula_weight         598.86
_chemical_name_systematic
'[Bis(3,5-di-<i>tert</i>-butylpyrazol-1-yl)dithioacetato](tetrahydrofuran)lithium(I) tetrahydrofuran monosolvate'
_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
_cell_angle_alpha                90
_cell_angle_beta                 105.013(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4026(3)
_cell_length_b                   16.3932(4)
_cell_length_c                   17.8867(4)
_cell_measurement_reflns_used    4077
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      23.81
_cell_measurement_theta_min      2.45
_cell_volume                     3512.56(15)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25289
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7066
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+0.7204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                4549
_reflns_number_total             7066
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            yp3040.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        3512.56(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019159
_cod_database_fobs_code          2019159