Phase transition and structures of the twinned low-temperature phases of (Et~4~N)[ReS~4~]
Bernhardt, Eduard; Herbst-Irmer, Regine; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S205322961901725X

data_2021972
_publ_section_title
;
 Phase transition and structures of the twinned low-temperature phases of
 (Et~4~N)[ReS~4~]
;
_journal_coeditor_code           EF3002
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205322961901725X
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C8 H20 N) [Re S4]'
_chemical_formula_moiety         'C8 H20 N +, Re S4 -'
_chemical_formula_sum            'C8 H20 N Re S4'
_chemical_formula_weight         444.69
_chemical_name_systematic
;
Tetraethylammonium tetrathiorhenate
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_atom_sites_solution_hydrogens   geom
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_cell_length_a                   8.150(2)
_cell_length_b                   8.150(3)
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_cell_measurement_temperature    297(2)
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_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2016)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2016)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2016)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2001)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      297(2)
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_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 1.003
_diffrn_measurement_device_type
'Oxford Diffraction Gemini E Ultra diffractometer with an EOS CCD camera'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube Enhanced (Mo)'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0244
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_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1804
_diffrn_reflns_theta_full        26.400
_diffrn_reflns_theta_max         26.702
_diffrn_reflns_theta_min         2.886
_exptl_absorpt_coefficient_mu    8.592
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2013), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_description       prism
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_exptl_crystal_size_max          0.3177
_exptl_crystal_size_mid          0.0331
_exptl_crystal_size_min          0.0256
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_refine_diff_density_min         -0.424
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         513
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.071
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_refine_ls_R_factor_gt           0.0208
_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^)+(0.0180P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0475
_reflns_number_gt                392
_reflns_number_total             513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef3002sup1.cif
_cod_data_source_block           Ia
_cod_database_code               2021972
_shelx_hkl_checksum              26001
_shelx_res_checksum              88081
_shelxl_version_number           20.13
_cod_database_fobs_code 2021972