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_2021974
_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      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 119.04(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.900(2)
_cell_length_b                   12.842(3)
_cell_length_c                   8.118(2)
_cell_measurement_reflns_used    3279
_cell_measurement_temperature    149.9(3)
_cell_measurement_theta_max      29.5080
_cell_measurement_theta_min      2.9080
_cell_volume                     720.0(3)
_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      149.9(3)
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.935
_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
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4476
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.279
_diffrn_reflns_theta_min         3.280
_exptl_absorpt_coefficient_mu    8.986
_exptl_absorpt_correction_T_max  0.336
_exptl_absorpt_correction_T_min  0.241
_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    2.051
_exptl_crystal_description       prism
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.2391
_exptl_crystal_size_mid          0.2035
_exptl_crystal_size_min          0.1704
_refine_diff_density_max         2.005
_refine_diff_density_min         -4.804
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1080 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.105(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         2814
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+29.5424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                2808
_reflns_number_total             2814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef3002sup1.cif
_cod_data_source_block           Ic
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2021974
_cod_database_fobs_code          2021974
_shelx_hkl_checksum              45234
_shelx_res_checksum              68323