A 2:1 Mixture of Tetrabutylammonium Bis(4,5-dimercapto-1,3-dithiole-2-thionato)nickelate(II) and its 2-Selenone Analogue
Fun, H.-K.; Sivakumar, K.; Zuo, J.-L.; Yao, T.-M.; You, X.-Z.; Acta Crystallographica Section C 52 (1996) 312–315; doi:10.1107/S0108270195010754

data_2004522
_publ_section_title
;
 A 2:1 Mixture of Tetrabutylammonium
 Bis(4,5-dimercapto-1,3-dithiole-2-thionato)nickelate(II) and its
 2-Selenone Analogue
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              312
_journal_page_last               315
_journal_paper_doi               10.1107/S0108270195010754
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         '(C3 S4.67 Se0.33)2 Ni 2-, (N(C4 H9)+)2'
_chemical_formula_sum            'C38 H72 N2 Ni S9.34 Se0.66'
_chemical_formula_weight         967.264
_chemical_name_systematic
;
Tetrabutylammonium Bis(1,3-dithiol-2-thione/selone-4,5-dithioate)
Nickel (II)
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.420(2)
_cell_length_b                   14.796(2)
_cell_length_c                   19.50400(10)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      10
_cell_volume                     2415.5(7)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL-PC (Sheldrick, 1990)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \q/2\q
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7096
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.331
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   '\y scans (Siemens, 1994)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1027.8
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.27
_refine_ls_extinction_coef       0.0107(8)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.070
_refine_ls_goodness_of_fit_obs   1.150
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5499
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.159
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_obs          0.0335
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0523P)^2^ + 0.1746P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0969
_refine_ls_wR_factor_obs         0.0921
_reflns_number_observed          4366
_reflns_number_total             5500
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1199.cif
_cod_data_source_block           asse02n
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (27
times).

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (33
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2004522