Tetraethylammonium (1-Pyrrolidinecarbodithioato-<i>S</i>,<i>S</i>')(tetrathiotungstenio-<i>S</i>,<i>S</i>')nickelate(1 ‒)
De-Liang Long; Qing-Hua Wang; Jin-Shun Huang; Acta Crystallographica Section C 54 (1998) 1251–1253; doi:10.1107/S0108270198004296

data_2007580
_publ_section_title
;Tetraethylammonium
 (1-Pyrrolidinecarbodithioato-<i>S</i>,<i>S</i>')(tetrathiotungstenio-<i>S</i>,<i>S</i>')nickelate(1
 --)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1251
_journal_page_last               1253
_journal_paper_doi               10.1107/S0108270198004296
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '(C8 H20 N)[NiWS4 (C5 H8 NS2)]'
_chemical_formula_moiety         'C8 H20 N 1+ , C5 H8 N Ni S6 W 1-'
_chemical_formula_sum            'C13 H28 N2 Ni S6 W'
_chemical_formula_weight         647.3
_chemical_name_systematic
;
Tetraethylammonium
(1-Pyrrolidinecarbodithioate-S,S')(tetrathiotungstenio-S,S')-nickelate(1-)
;
_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_type_scat_source
'International Tables for X-ray Crystallography (Vol. IV)'
_cell_angle_alpha                90
_cell_angle_beta                 93.74(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.610(4)
_cell_length_b                   8.2860(10)
_cell_length_c                   19.848(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      13
_cell_measurement_theta_min      11
_cell_volume                     2233.5(8)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.013
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4395
_diffrn_reflns_theta_max         25.0
_diffrn_standards_decay_%        0.6(variation)
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.55
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_correction_T_min  0.271
_exptl_absorpt_correction_type   'Empirical \y scan (North et al., 1968)'
_exptl_crystal_colour            'brownish green'
_exptl_crystal_density_diffrn    1.92
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Lath
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.00_(1.05\%A_from_W)
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.69
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3170
_refine_ls_R_factor_obs          .037
_refine_ls_shift/esd_max         0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F)+(0.020F)^2^+1.0] - F'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .047
_reflns_number_observed          3170
_reflns_number_total             4230
_reflns_observed_criterion       I_>_3.0_\s(I)
_cod_data_source_file            bm1219.cif
_cod_data_source_block           bm1219
_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.

'_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 (11
times).

'_geom_bond_publ_flag' value 'No' changed to 'no' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (39 times).

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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F)+(0.020F)^2^+1.0]
- F' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w =
1/[\s^2^(F)+(0.020F)^2^+1.0] - F'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C13 H28 N2 Ni1 S6 W1'
_cod_database_code               2007580