#------------------------------------------------------------------------------
#$Date: 2016-12-02 04:09:34 +0200 (Fri, 02 Dec 2016) $
#$Revision: 188820 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/80/2108020.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2108020
loop_
_publ_author_name
'Binns, Jack'
'McIntyre, Garry J.'
'Parsons, Simon'
_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 hydrogensulfate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 118.054(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.3405(7)
_cell_length_b                   4.6150(2)
_cell_length_c                   14.3723(12)
_cell_measurement_reflns_used    2854
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     839.42(9)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_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 0.524
_diffrn_measured_fraction_theta_max 0.524
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4260
_diffrn_reflns_theta_full        25.031
_diffrn_reflns_theta_max         25.031
_diffrn_reflns_theta_min         3.219
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.163
_exptl_absorpt_correction_T_max  0.30
_exptl_absorpt_correction_T_min  0.09
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.889
_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          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.73
_refine_ls_extinction_coef       14(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9896
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         780
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.0001528
_refine_ls_shift/su_mean         0.0000084
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)²]²
 Ai are:
 9.71 14.5 6.69 1.68
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1569
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1569
_reflns_number_gt                673
_reflns_number_total             781
_reflns_threshold_expression     I>2.0σ(I)
_cod_data_source_file            fx5004sup1.cif
_cod_data_source_block           JB0008
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'H1 O4 Rb1 S1'
_cod_database_code               2108020
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
Rb Rb1 0.70777(9) 0.6398(2) 0.58454(14) 0.0326 Uani 1.0000
Rb Rb2 0.46120(10) 0.7021(3) 0.83642(15) 0.0357 Uani 1.0000
S S1 0.5491(3) 0.2144(6) 0.6739(4) 0.0295 Uani 1.0000
S S2 0.2063(2) 0.7605(6) 0.5788(3) 0.0265 Uani 1.0000
O O1 0.4584(7) 0.012(2) 0.6002(11) 0.0473 Uani 1.0000
O O2 0.5521(9) 0.202(3) 0.7746(15) 0.0609 Uani 1.0000
O O3 0.5153(9) 0.489(2) 0.6218(13) 0.0665 Uani 1.0000
O O4 0.6463(7) 0.117(2) 0.6768(11) 0.0413 Uani 1.0000
O O5 0.2579(7) 0.9962(18) 0.6677(9) 0.0358 Uani 1.0000
O O6 0.1979(7) 0.8856(19) 0.4832(11) 0.0364 Uani 1.0000
O O7 0.2813(7) 0.5250(17) 0.6193(10) 0.0386 Uani 1.0000
O O8 0.1062(7) 0.692(2) 0.5744(11) 0.0425 Uani 1.0000
H H1 0.4723 -0.1615 0.6089 0.0687 Uiso 1.0000
H H2 0.2615 1.1587 0.6461 0.0486 Uiso 1.0000
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Rb1 0.0343(8) 0.0301(9) 0.0325(16) 0.0006(5) 0.0150(9) 0.0010(5)
Rb2 0.0314(8) 0.0363(9) 0.0355(17) 0.0002(5) 0.0125(9) 0.0010(6)
S1 0.0362(18) 0.0221(17) 0.034(3) -0.0019(12) 0.019(2) -0.0033(12)
S2 0.0318(17) 0.0171(17) 0.028(4) -0.0021(10) 0.012(2) -0.0001(11)
O1 0.035(4) 0.040(5) 0.049(8) -0.002(3) 0.005(5) -0.010(4)
O2 0.057(6) 0.096(9) 0.038(6) -0.006(6) 0.029(7) -0.016(5)
O3 0.064(6) 0.031(4) 0.096(11) 0.007(4) 0.031(8) 0.020(4)
O4 0.034(4) 0.051(6) 0.041(10) -0.001(3) 0.019(5) -0.008(5)
O5 0.053(5) 0.025(4) 0.021(6) -0.004(3) 0.011(5) 0.000(3)
O6 0.040(5) 0.044(5) 0.021(6) 0.001(4) 0.011(5) 0.001(3)
O7 0.046(4) 0.022(4) 0.047(9) 0.007(3) 0.021(6) 0.009(3)
O8 0.033(4) 0.050(6) 0.042(11) -0.005(3) 0.015(5) 0.003(4)
loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O 3.0485 2.2868 1.5463 0.8670 13.2771 5.7011 0.3239 32.9089 0.2508 0.0106
0.0060 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.4930 0.3229 0.1402 0.0408 10.5109 26.1257 3.1424 57.7998 0.0030 0.0000
0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 6.9053 5.2034 1.4379 1.5863 1.4679 22.2151 0.2536 56.1720 0.8669 0.1246
0.1234 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Rb 17.1784 9.6435 5.1399 1.5292 1.7888 17.3151 0.2748 164.9340 3.4873 -0.9393
2.9676 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O1 S1 O2 106.5(8) yes
O1 S1 O3 102.0(7) yes
O2 S1 O3 113.8(9) yes
O1 S1 O4 108.8(6) yes
O2 S1 O4 112.9(8) yes
O3 S1 O4 112.0(7) yes
O5 S2 O6 107.1(6) yes
O5 S2 O7 102.5(6) yes
O6 S2 O7 113.5(7) yes
O5 S2 O8 105.5(7) yes
O6 S2 O8 114.2(7) yes
O7 S2 O8 112.9(6) yes
S1 O1 H1 114.8 no
S2 O5 H2 114.4 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S1 O1 1.547(10) yes
S1 O2 1.429(19) yes
S1 O3 1.435(10) yes
S1 O4 1.445(10) yes
S2 O5 1.573(10) yes
S2 O6 1.443(14) yes
S2 O7 1.445(9) yes
S2 O8 1.441(10) yes
O1 H1 0.820 no
O5 H2 0.822 no

_cod_database_fobs_code 2108020
