Neutron and high-pressure X-ray diffraction study of hydrogen-bonded ferroelectric rubidium hydrogen sulfate
Binns, Jack; McIntyre, Garry J.; Parsons, Simon; Acta Crystallographica Section B 72 (2016) 855–863; doi:10.1107/S2052520616013494

data_2108018
_publ_section_title
;
 Neutron and high-pressure X-ray diffraction study of hydrogen-bonded
 ferroelectric rubidium hydrogen sulfate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              855
_journal_page_last               863
_journal_paper_doi               10.1107/S2052520616013494
_journal_volume                  72
_journal_year                    2016
_chemical_formula_moiety         'H1 O4 S1, Rb1'
_chemical_formula_sum            'H O4 Rb S'
_chemical_formula_weight         182.54
_chemical_name_systematic        'rubidium hydrogen sulfate'
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 117.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.166(5)
_cell_length_b                   4.5982(9)
_cell_length_c                   14.326(4)
_cell_measurement_reflns_used    3627
_cell_measurement_temperature    293
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     826.4(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.417
_diffrn_measured_fraction_theta_max 0.409
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4613
_diffrn_reflns_theta_full        25.094
_diffrn_reflns_theta_max         26.140
_diffrn_reflns_theta_min         3.343
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.355
_exptl_absorpt_correction_T_max  0.29
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.84
_refine_diff_density_min         -1.01
_refine_ls_abs_structure_details 'Flack (1983), 562 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.236(18)
_refine_ls_extinction_coef       42(7)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.8328
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1149
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.0000811
_refine_ls_shift/su_mean         0.0000244
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 22.4 35.5 18.6 5.57
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1823
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                1149
_reflns_number_total             1240
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            fx5004sup1.cif
_cod_data_source_block           JB0005
_cod_original_sg_symbol_H-M      'P 1 n 1 '
_cod_original_formula_sum        'H1 O4 Rb1 S1'
_cod_database_code               2108018
_cod_database_fobs_code 2108018