Crystal structure of potassium triethylhydridoborate (`superhydride')
Fecker, Ann Christin; Freytag, Matthias; Walter, Marc D.; Jones, Peter G.; Acta Crystallographica Section E 77 (2021) 592–595; doi:10.1107/S2056989021004734

data_2243822
_publ_section_title
;
 Crystal structure of potassium triethylhydridoborate (`superhydride')
;
_journal_coeditor_code           YZ2007
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              592
_journal_page_last               595
_journal_paper_doi               10.1107/S2056989021004734
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'K +, C6 H16 B -'
_chemical_formula_moiety         'K +, C6 H16 B -'
_chemical_formula_sum            'C6 H16 B K'
_chemical_formula_weight         138.10
_chemical_name_common            Superhydride
_chemical_name_systematic
;
Potassium triethylhydridoborate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4758(3)
_cell_length_b                   7.6682(6)
_cell_length_c                   14.8010(12)
_cell_measurement_reflns_used    2443
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.1130
_cell_measurement_theta_min      2.7460
_cell_volume                     848.48(10)
_computing_cell_refinement
;
CrysAlisPro (Agilent, 2013)
;
_computing_data_collection
;
CrysAlisPro (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlisPro (Agilent, 2013)
;
_computing_molecular_graphics
;
XP (Siemens, 1994)
;
_computing_publication_material
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13206
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         2.752
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent, 2013)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.233
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 806 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons<i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         2441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0251P)^2^+0.0172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                2182
_reflns_number_total             2441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yz2007sup1.cif
_cod_data_source_block           I
_cod_database_code               2243822
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.924
_shelx_hkl_checksum              44557
_shelx_res_checksum              15826
_cod_database_fobs_code 2243822