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_2019158
_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          '[Zn (C24 H39 N4 S2) Cl]'
_chemical_formula_moiety         'C24 H39 Cl N4 S2 Zn'
_chemical_formula_sum            'C24 H39 Cl N4 S2 Zn'
_chemical_formula_weight         548.53
_chemical_name_systematic
;
[Bis(3,5-di-tert-butylpyrazol-1-yl)dithioacetato]chloridozinc(II)
;
_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           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.919(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2713(19)
_cell_length_b                   11.9298(17)
_cell_length_c                   16.8543(12)
_cell_measurement_reflns_used    238
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      6
_cell_volume                     2772.8(6)
_computing_cell_refinement       'EVALCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_data_collection       'COLLECT (Hooft, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method
;
\f- and \w-rotations with 2.00 \% and 120 sec per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68182
_diffrn_reflns_theta_full        28.52
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.7400882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.3233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                5579
_reflns_number_total             7007
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            yp3040.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2019158
_cod_database_fobs_code          2019158