The crystal structure of BaH6As4O14 redetermined, revealing the localization of the hydrogen atoms
Weil, Matthias; IUCrData 4 (2019) x190075–; doi:10.1107/S2414314619000750

data_1550494
_publ_section_title
;
 The crystal structure of BaH6As4O14 redetermined, revealing the
 localization of the hydrogen atoms
;
_journal_coeditor_code           BT4081
_journal_issue                   1
_journal_name_full               IUCrData
_journal_page_first              x190075
_journal_paper_doi               10.1107/S2414314619000750
_journal_volume                  4
_journal_year                    2019
_chemical_formula_iupac          'Ba H6 As4 O14'
_chemical_formula_moiety         'As4 H6 Ba O14'
_chemical_formula_sum            'As4 Ba H6 O14'
_chemical_formula_weight         667.07
_chemical_name_systematic
;
Barium hexahydrogen <i>cyclo</i>-tetradecaoxidotetraarsenate(V)
;
_space_group_IT_number           53
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2'
_symmetry_space_group_name_H-M   'P m a n'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4638(5)
_cell_length_b                   11.1799(7)
_cell_length_c                   5.8353(4)
_cell_measurement_reflns_used    8994
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.987
_cell_measurement_theta_min      3.018
_cell_volume                     552.16(6)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
ATOMS (Dowty, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution    'coordinates taken from previous refinement'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            18011
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.014
_diffrn_reflns_theta_min         3.019
_exptl_absorpt_coefficient_mu    15.571
_exptl_absorpt_correction_T_max  0.7489
_exptl_absorpt_correction_T_min  0.5506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.012
_exptl_crystal_description       fragment
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.980
_refine_ls_extinction_coef       0.0072(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2017 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         2384
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0149
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+0.1747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0314
_refine_ls_wR_factor_ref         0.0323
_reflns_number_gt                2146
_reflns_number_total             2384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4081sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'As4 H6 Ba O14'
_cod_database_code               1550494
_cod_database_fobs_code          1550494
_shelx_hkl_checksum              22470
_shelx_res_checksum              74849