[2 x 2] Molecular Grids of Ni(II) and Zn(II) with Redox-Active 1,4-Pyrazine-Bis(thiosemicarbazone) Ligands
Arefyeva, N.; Sandleben, A.; Krest, A.; Baumann, U.; Schafer, M.; Kempf, M.; Klein, A.; Inorganics 6 (2018) 51–; doi:10.3390/inorganics6020051

data_1556601
_publ_section_title
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 [2 x 2] Molecular Grids of Ni(II) and Zn(II) with Redox-Active
 1,4-Pyrazine-Bis(thiosemicarbazone) Ligands
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_journal_name_full               Inorganics
_journal_page_first              51
_journal_paper_doi               10.3390/inorganics6020051
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C56 H80 N32 S8 Zn4'
_chemical_formula_sum            'C56 H80 N32 S8 Zn4'
_chemical_formula_weight         1719.48
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.7800(10)
_cell_length_b                   19.7800(10)
_cell_length_c                   20.2910(10)
_cell_measurement_reflns_used    41764
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.873
_cell_measurement_theta_min      2.007
_cell_volume                     7938.8(7)
_computing_cell_refinement       'X-AREA (STOE & Cie 2001)'
_computing_data_collection       'X-AREA (STOE & Cie 2001)'
_computing_data_reduction        'X-RED (STOE & Cie 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS IIT'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1391
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41764
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.873
_diffrn_reflns_theta_min         2.007
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.9006
_exptl_absorpt_correction_T_min  0.6935
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correction (X-RED; Stoe & Cie, 2001) 
was performed after optimizing the crystal shape 
using X-SHAPE (Stoe & Cie, 1999).
;
_exptl_crystal_colour            rot
_exptl_crystal_density_diffrn    0.719
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.60(11)
_refine_ls_extinction_coef       0.0025(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         4242
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.2583
_refine_ls_R_factor_gt           0.1616
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3933
_refine_ls_wR_factor_ref         0.4359
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                1360
_reflns_number_total             4242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1435303__ZnL3_4.cif
_cod_data_source_block           '[Zn4(LiPr)4]'
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_cell_volume        7938.8(9)
_cod_database_code               1556601
_shelx_res_checksum              27486
_shelx_hkl_checksum              11906