Two polymorphs of tetraethylammonium [hydrogen tris(3,5-dimethylpyrazolyl)borato]di-μ~2~-sulfido-disulfido(η^2^-tetrasulfido)ditungsten(V) with <i>Z</i>' = 1 and 2
Beheshti, Azizolla; Clegg, William; Ebrahimi Filoori, Nahid; Russo, Luca; Acta Crystallographica Section C 67 (2011) m149–m153; doi:10.1107/S0108270111013035

data_2018049
_publ_section_title
;
 Two polymorphs of tetraethylammonium [hydrogen
 tris(3,5-dimethylpyrazolyl)borato]di-\m~2~-sulfido-disulfido(\h^2^-tetrasulfido)ditungsten(V)
 with <i>Z</i>' = 1 and 2
;
_journal_coeditor_code           BI3009
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m149
_journal_page_last               m153
_journal_paper_doi               10.1107/S0108270111013035
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C8 H20 N) [W2 S4 (S)4 (C15 H22 B N6)]'
_chemical_formula_moiety         'C8 H20 N +, C15 H22 B N6 S8 W2 -'
_chemical_formula_sum            'C23 H42 B N7 S8 W2'
_chemical_formula_weight         1051.63
_chemical_name_systematic
;
tetraethylammonium [hydrogen
tris(3,5-dimethylpyrazolyl)borato]di-\m~2~-sulfido-disulfido(\h^2^-
tetrasulfido)ditungsten(V)
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.343(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.8602(10)
_cell_length_b                   18.8742(10)
_cell_length_c                   20.6188(10)
_cell_measurement_reflns_used    6724
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.93
_cell_measurement_theta_min      2.96
_cell_volume                     6950.4(6)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.735
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_av_sigmaI/netI    0.1575
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23985
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         3.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.124
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlisPro; Oxford Diffraction, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.815
_refine_diff_density_min         -2.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         11129
_refine_ls_number_restraints     760
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1711
_reflns_number_gt                6168
_reflns_number_total             11129
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi3009.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2018049
_cod_database_fobs_code          2018049