#------------------------------------------------------------------------------
#$Date: 2016-02-20 01:53:41 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/55/2105559.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_2105559
loop_
_publ_author_name
'Chisholm, Calum R. I.'
'Haile, Sossina M.'
_publ_section_title
;
 Structure and thermal behavior of the new superprotonic conductor
 Cs₂(HSO₄)(H₂PO₄)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              937
_journal_page_last               946
_journal_paper_doi               10.1107/S0108768199009921
_journal_volume                  55
_journal_year                    1999
_chemical_formula_structural     Cs2(HSO4)(H2PO4)
_chemical_formula_sum            'Cs2 H3 O8 P S'
_chemical_formula_weight         458.85
_chemical_name_systematic        ' ?'
_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_type_scat_source           'Cromer & Waber (1974)'
_cell_angle_alpha                90
_cell_angle_beta                 99.92(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.856(8)
_cell_length_b                   7.732(7)
_cell_length_c                   7.827(7)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.3
_cell_measurement_theta_min      4
_cell_volume                     468.3(8)
_computing_molecular_graphics    'ATOMS (Dowty, 1999)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_measurement_device_type  'Syntex four-circle'
_diffrn_measurement_method       θ-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71070
_diffrn_reflns_av_R_equivalents  .0470
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2629
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         3.39
_diffrn_standards_decay_%        .7
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.692
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  .36
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ψ scan'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.261
_exptl_crystal_F_000             416
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .05
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.324
_refine_ls_extinction_coef       .0116(12)
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1361
_refine_ls_R_factor_all          .0399
_refine_ls_R_factor_gt           .0348
_refine_ls_shift/su_max          .516
_refine_ls_shift/su_mean         .031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;w = [σ²(Fₒ²)+(0.0502P)²+0.23049P]⁻¹
where  P = 1/3[max(Fₒ², 0)+2Fc²]
;
_refine_ls_wR_factor_all         .0890
_refine_ls_wR_factor_ref         .0855
_reflns_number_gt                1210
_reflns_number_total             1364
_reflns_threshold_expression     I>=2σ(I)
_cod_data_source_file            bs0007.cif
_cod_data_source_block           bs0007
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2105559
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
1/2+x,1/2-y,1/2+z
1/2-x,1/2+y,1/2-z
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
Cs .0320(10) .0280(10) .0310(10) .0000(10) .0000(10) -.0040(10)
S .0200(10) .0190(10) .0260(10) -.0010(10) .0040(10) -.0030(10)
P .0200(10) .0190(10) .0260(10) -.0010(10) .0040(10) -.0030(10)
O(1) .030(2) .029(2) .039(2) -.0130(10) .0080(10) -.0060(10)
O(2) .033(2) .031(2) .037(2) .0040(10) .0100(10) -.0060(10)
O(3) .032(2) .031(2) .039(2) -.0060(10) .0120(10) -.0030(10)
O(4) .032(2) .030(2) .050(2) .0070(10) -.0080(10) -.0020(10)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Cs(1) .72800(10) .15880(10) .11800(10) .0310(10) 1
S .75650(10) .16210(10) -.38870(10) .0220(10) .5
P .75650(10) .16210(10) -.38870(10) .0220(10) .5
O(1) .6584(4) .0269(3) .4937(4) .0320(10) 1
O(2) .8377(2) .2882(2) -.4882(3) .0340(10) 1
O(3) .6287(2) .2447(2) -.2880(2) .0330(10) 1
O(4) .8930(2) .0690(3) -.2607(2) .0390(10) 1
H(1) .5387(4) .0329(6) .5012(6) .0800(10) .5
H(2) .8558(2) -.0469(3) -.2449(2) .0800(10) 1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cs(1) O(2) 4_644 3.055(4) y
Cs(1) O(2) 3_455 3.063(4) y
Cs(1) O(1) 4_655 3.151(3) y
Cs(1) O(3) 3 3.196(4) y
Cs(1) O(3) . 3.208(3) y
Cs(1) O(2) 1_556 3.214(4) y
Cs(1) O(1) . 3.247(4) y
Cs(1) O(4) 2_755 3.475(4) y
Cs(1) O(4) . 3.502(3) y
Cs(1) O(4) 3_455 3.622(4) y
