#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/94/2019423.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2019423
loop_
_publ_author_name
'Stöger, Berthold'
'Weil, Matthias'
_publ_section_title
;
 The isotypic hydrogen phosphate and arsenate dihydrates
 M₂HXO₄·2H₂O (M = Rb, Cs; X = P,
 As)
;
_journal_coeditor_code           FN3158
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              7
_journal_page_last               11
_journal_paper_doi               10.1107/S205322961303338X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'Cs2 H P O4, 2H2 O'
_chemical_formula_sum            'Cs2 H5 O6 P'
_chemical_formula_weight         397.8
_chemical_name_systematic
;
Dicaesium monohydrogen phosphate(V) dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     isomor
_cell_angle_alpha                90
_cell_angle_beta                 116.880(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4764(5)
_cell_length_b                   14.1898(10)
_cell_length_c                   7.9535(6)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.6
_cell_measurement_theta_min      2.9
_cell_volume                     752.61(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2013)'
_computing_molecular_graphics    'ATOMS (Dowty, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement
'JANA2006 (Petříček et al., 2006)'
_computing_structure_solution    'coordinates of Rb₂HAsO₄.2H₂O'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25736
_diffrn_reflns_theta_full        32.62
_diffrn_reflns_theta_max         32.62
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    9.869
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2013)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    3.5098
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.65
_refine_ls_extinction_coef       141E1(5)
_refine_ls_extinction_method
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_ref   1.61
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_constraints    2
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2756
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.0296
_refine_ls_shift/su_mean         0.0035
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0323
_refine_ls_wR_factor_ref         0.0332
_reflns_number_gt                2503
_reflns_number_total             2756
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            fn3158sup1.cif
_cod_data_source_block           Cs2HPO4.2H2O
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'Cs2 H5 O6 P1'
_cod_database_code               2019423
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-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_calc_flag
_atom_site_occupancy
Cs Cs1 0.742006(15) 0.731846(10) 0.746496(12) 0.00725(6) Uani d 1
Cs Cs2 0.251965(13) 0.918915(9) 0.745719(13) 0.00898(7) Uani d 1
P P 0.25330(5) 0.85516(4) 0.25943(5) 0.00527(16) Uani d 1
O O1 0.1409(2) 0.79501(10) 0.06896(18) 0.0112(4) Uani d 1
O O2 0.4132(2) 0.91487(9) 0.2418(2) 0.0093(5) Uani d 1
O O3 0.3467(2) 0.78525(9) 0.42224(18) 0.0114(5) Uani d 1
O O4 0.0879(2) 0.91339(9) 0.2696(2) 0.0096(5) Uani d 1
O Ow1 0.7811(3) 0.91652(10) 0.5516(2) 0.0118(5) Uani d 1
O Ow2 0.7218(3) 0.58033(9) 0.4544(2) 0.0114(5) Uani d 1
H Hw22 0.688(4) 0.5330(12) 0.381(3) 0.023(6) Uiso d 1
H Hw12 0.816(4) 0.9668(11) 0.617(3) 0.027(6) Uiso d 1
H Hw21 0.8430(16) 0.5766(17) 0.538(3) 0.023(6) Uiso d 1
H Hw11 0.665(2) 0.9235(17) 0.460(3) 0.027(6) Uiso d 1
H H1 0.218(3) 0.7729(17) 0.027(3) 0.053(10) Uiso d 1
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs -0.3680 2.1192 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Cs1 O2 1_656 4_565 130.63(4)
O1 Cs1 O3 1_656 . 148.38(4)
O1 Cs1 O4 1_656 4_665 71.87(4)
O1 Cs1 Ow1 1_656 . 84.02(4)
O1 Cs1 Ow1 1_656 4_565 80.39(4)
O1 Cs1 Ow2 1_656 . 121.80(4)
O1 Cs1 Ow2 1_656 4_565 64.88(4)
O2 Cs1 O3 4_565 . 72.74(4)
O2 Cs1 O4 4_565 4_665 100.09(4)
O2 Cs1 Ow1 4_565 . 141.38(4)
O2 Cs1 Ow1 4_565 4_565 51.25(4)
O2 Cs1 Ow2 4_565 . 76.42(5)
O2 Cs1 Ow2 4_565 4_565 109.51(5)
O3 Cs1 O4 . 4_665 131.03(4)
O3 Cs1 Ow1 . . 68.88(4)
O3 Cs1 Ow1 . 4_565 123.06(4)
O3 Cs1 Ow2 . . 80.63(4)
O3 Cs1 Ow2 . 4_565 88.59(4)
O4 Cs1 Ow1 4_665 . 108.04(5)
O4 Cs1 Ow1 4_665 4_565 74.69(5)
O4 Cs1 Ow2 4_665 . 51.21(4)
O4 Cs1 Ow2 4_665 4_565 136.68(4)
Ow1 Cs1 Ow1 . 4_565 162.42(4)
Ow1 Cs1 Ow2 . . 101.10(5)
Ow1 Cs1 Ow2 . 4_565 65.90(5)
Ow1 Cs1 Ow2 4_565 . 94.02(4)
Ow1 Cs1 Ow2 4_565 4_565 99.84(5)
Ow2 Cs1 Ow2 . 4_565 165.64(4)
O1 Cs2 O1 1_556 4_565 75.72(4)
O1 Cs2 O2 1_556 1_556 41.86(3)
O1 Cs2 O2 1_556 3_676 137.66(3)
O1 Cs2 O3 1_556 . 117.28(3)
O1 Cs2 O3 1_556 4_565 45.12(4)
O1 Cs2 O4 1_556 . 135.71(3)
O1 Cs2 O4 1_556 3_576 87.53(4)
O1 Cs2 Ow1 1_556 1_455 76.76(4)
O1 Cs2 Ow1 1_556 3_676 157.95(4)
O1 Cs2 Ow2 1_556 2_656 76.77(4)
O1 Cs2 Ow2 1_556 4_565 101.15(4)
O1 Cs2 O2 4_565 1_556 110.59(3)
O1 Cs2 O2 4_565 3_676 133.71(4)
O1 Cs2 O3 4_565 . 44.37(4)
O1 Cs2 O3 4_565 4_565 46.04(3)
O1 Cs2 O4 4_565 . 67.05(3)
O1 Cs2 O4 4_565 3_576 125.66(3)
O1 Cs2 Ow1 4_565 1_455 76.69(4)
O1 Cs2 Ow1 4_565 3_676 115.48(4)
O1 Cs2 Ow2 4_565 2_656 152.15(5)
O1 Cs2 Ow2 4_565 4_565 103.61(4)
O2 Cs2 O2 1_556 3_676 95.88(4)
O2 Cs2 O3 1_556 . 136.18(3)
O2 Cs2 O3 1_556 4_565 66.28(3)
O2 Cs2 O4 1_556 . 177.48(3)
O2 Cs2 O4 1_556 3_576 85.70(4)
O2 Cs2 Ow1 1_556 1_455 106.66(5)
O2 Cs2 Ow1 1_556 3_676 133.82(3)
O2 Cs2 Ow2 1_556 2_656 47.24(3)
O2 Cs2 Ow2 1_556 4_565 71.15(5)
O2 Cs2 O3 3_676 . 90.36(4)
O2 Cs2 O3 3_676 4_565 127.44(3)
O2 Cs2 O4 3_676 . 86.50(4)
O2 Cs2 O4 3_676 3_576 92.49(4)
O2 Cs2 Ow1 3_676 1_455 131.85(4)
O2 Cs2 Ow1 3_676 3_676 48.52(3)
O2 Cs2 Ow2 3_676 2_656 72.00(5)
O2 Cs2 Ow2 3_676 4_565 49.42(3)
O3 Cs2 O3 . 4_565 75.61(4)
O3 Cs2 O4 . . 42.79(3)
O3 Cs2 O4 . 3_576 137.43(3)
O3 Cs2 Ow1 . 1_455 100.74(4)
O3 Cs2 Ow1 . 3_676 80.18(4)
O3 Cs2 Ow2 . 2_656 162.23(4)
O3 Cs2 Ow2 . 4_565 80.85(4)
O3 Cs2 O4 4_565 . 111.60(3)
O3 Cs2 O4 4_565 3_576 131.57(4)
O3 Cs2 Ow1 4_565 1_455 100.66(4)
O3 Cs2 Ow1 4_565 3_676 155.54(5)
O3 Cs2 Ow2 4_565 2_656 113.18(4)
O3 Cs2 Ow2 4_565 4_565 78.18(4)
O4 Cs2 O4 . 3_576 95.01(4)
O4 Cs2 Ow1 . 1_455 72.16(5)
O4 Cs2 Ow1 . 3_676 48.61(4)
O4 Cs2 Ow2 . 2_656 134.67(3)
O4 Cs2 Ow2 . 4_565 110.01(5)
O4 Cs2 Ow1 3_576 1_455 49.06(4)
O4 Cs2 Ow1 3_576 3_676 70.48(5)
O4 Cs2 Ow2 3_576 2_656 48.49(3)
O4 Cs2 Ow2 3_576 4_565 130.46(3)
Ow1 Cs2 Ow1 1_455 3_676 87.17(4)
Ow1 Cs2 Ow2 1_455 2_656 92.91(5)
Ow1 Cs2 Ow2 1_455 4_565 177.78(5)
Ow1 Cs2 Ow2 3_676 2_656 89.26(4)
Ow1 Cs2 Ow2 3_676 4_565 94.65(4)
Ow2 Cs2 Ow2 2_656 4_565 85.85(4)
O1 P O2 . . 107.85(9)
O1 P O3 . . 107.37(8)
O1 P O4 . . 104.36(7)
O2 P O3 . . 111.25(8)
O3 P O4 . . 112.31(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cs1 O1 1_656 3.0595(13)
Cs1 O2 4_565 3.2088(17)
Cs1 O3 . 3.0112(13)
Cs1 O4 4_665 3.2464(17)
Cs1 Ow1 . 3.1249(17)
Cs1 Ow1 4_565 3.1249(18)
Cs1 Ow2 . 3.1186(18)
Cs1 Ow2 4_565 3.1759(16)
Cs2 O1 1_556 3.5098(17)
Cs2 O1 4_565 3.2901(15)
Cs2 O2 1_556 3.5671(17)
Cs2 O2 3_676 3.4081(16)
Cs2 O3 . 3.5166(17)
Cs2 O3 4_565 3.1570(14)
Cs2 O4 . 3.4135(16)
Cs2 O4 3_576 3.4429(16)
Cs2 Ow1 1_455 3.1408(18)
Cs2 Ow1 3_676 3.2522(17)
Cs2 Ow2 2_656 3.2482(17)
Cs2 Ow2 4_565 3.1339(18)
P O1 . 1.6057(14)
P O2 . 1.5226(18)
P O3 . 1.5267(14)
P O4 . 1.5195(18)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 O3 4_564 0.85(3) 1.74(3) 2.579(2) 171(2) yes
Ow1 Hw11 O2 . 0.850(15) 1.902(15) 2.7400(19) 169(2) yes
Ow1 Hw12 O4 3_676 0.850(18) 1.908(17) 2.747(2) 169(3) yes
Ow2 Hw21 O4 4_665 0.850(12) 1.927(16) 2.753(2) 164(3) yes
Ow2 Hw22 O2 2_645 0.850(19) 1.915(18) 2.7461(19) 165(3) yes
