#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/44/2214425.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_2214425
loop_
_publ_author_name
'Paolo Ballirano'
'Girolamo Belardi'
'Ferdinando Bosi'
_publ_section_title
;
 Redetermination of the Tutton's salt Cs₂[Cu(H₂O)₆](SO₄)₂
;
_journal_coeditor_code           WM2127
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i164
_journal_page_last               i165
_journal_paper_doi               10.1107/S1600536807029790
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'Cs2 [Cu (H2 O)6] (S O4)2'
_chemical_formula_structural     'Cs2 [Cu (H2 O)6] (S O4)2'
_chemical_formula_sum            'Cs2 Cu H12 O14 S2'
_chemical_formula_weight         629.61
_chemical_name_common            'Caesium hexaaquacopper sulfate'
_chemical_name_systematic
;
Dicaesium hexaaquacopper(II) bis[sulfate(VI)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 106.199(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4383(6)
_cell_length_b                   12.7605(12)
_cell_length_c                   6.3130(6)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      4.0
_cell_volume                     730.14(11)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'ATOMS (Dowty, 2003)'
_computing_publication_material
;
PARST (Nardelli, 1982) and publCIF (Westrip, 2007)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       ω
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3436
_diffrn_reflns_reduction_process 'LP correction applied'
_diffrn_reflns_theta_full        35.03
_diffrn_reflns_theta_max         35.03
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 47
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.757
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.226
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al.,  1968)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             613.8
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.530
_refine_diff_density_min         -2.571
_refine_ls_extinction_coef       0.080(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     109
_refine_ls_number_reflns         3208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0335
_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/[σ²(Fo²)+(0.0466P)²+0.5369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0847
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                2728
_reflns_number_total             3208
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2127.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2214425
_cod_database_fobs_code          2214425
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
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_refinement_flags
_atom_site_occupancy
Cu Cu 0.0000 0.0000 0.0000 0.01692(10) Uani d S 1
Cs Cs 0.11407(2) 0.354561(15) 0.35562(3) 0.02654(8) Uani d . 1
S S 0.37975(7) 0.14584(5) 0.73909(10) 0.01703(11) Uani d . 1
O O1 0.3992(3) 0.24027(18) 0.6156(4) 0.0273(4) Uani d . 1
O O2 0.5138(3) 0.0821(2) 0.7893(5) 0.0314(5) Uani d . 1
O O3 0.2560(2) 0.08353(19) 0.6000(3) 0.0250(4) Uani d . 1
O O4 0.3439(3) 0.1767(2) 0.9448(4) 0.0280(4) Uani d . 1
O OW1 0.1450(3) 0.1085(2) 0.1577(4) 0.0252(4) Uani d . 1
O OW2 -0.1908(3) 0.1109(2) 0.0139(4) 0.0297(5) Uani d . 1
O OW3 -0.0002(2) -0.06342(18) 0.2836(3) 0.0205(3) Uani d . 1
H H11 0.184(7) 0.093(5) 0.277(11) 0.050 Uiso d . 1
H H12 0.199(7) 0.122(5) 0.094(11) 0.050 Uiso d . 1
H H21 -0.281(7) 0.099(5) -0.063(10) 0.050 Uiso d . 1
H H22 -0.181(7) 0.166(5) -0.017(11) 0.050 Uiso d . 1
H H31 -0.071(7) -0.051(5) 0.310(11) 0.050 Uiso d . 1
H H32 0.034(7) -0.113(5) 0.308(10) 0.050 Uiso d . 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O1- 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu2+ 0.2630 1.2660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 0 1
0 4 0
0 0 3
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
_geom_angle_publ_flag
OW3 Cu OW3 . 3 180.00(17) ?
OW3 Cu OW1 . . 90.34(9) ?
OW3 Cu OW1 3 . 89.66(9) ?
OW3 Cu OW1 . 3 89.66(9) ?
OW3 Cu OW1 3 3 90.34(9) ?
OW1 Cu OW1 . 3 180.00(16) ?
OW3 Cu OW2 . 3 88.94(9) ?
OW3 Cu OW2 3 3 91.06(9) ?
OW1 Cu OW2 . 3 90.60(10) ?
OW1 Cu OW2 3 3 89.40(10) ?
OW3 Cu OW2 . . 91.06(9) ?
OW3 Cu OW2 3 . 88.94(9) ?
OW1 Cu OW2 . . 89.40(10) ?
OW1 Cu OW2 3 . 90.60(10) ?
OW2 Cu OW2 3 . 180.00(17) ?
O1 Cs O4 . 4_564 140.29(7) ?
O1 Cs O3 . 2_556 97.49(6) ?
O4 Cs O3 4_564 2_556 113.63(6) ?
O1 Cs O2 . 2_556 141.84(6) ?
O4 Cs O2 4_564 2_556 73.76(6) ?
O3 Cs O2 2_556 2_556 44.43(6) ?
O1 Cs O1 . 4_565 97.59(5) ?
O4 Cs O1 4_564 4_565 83.64(6) ?
O3 Cs O1 2_556 4_565 126.51(6) ?
O2 Cs O1 2_556 4_565 104.49(6) ?
O1 Cs OW2 . 4_665 81.11(6) ?
O4 Cs OW2 4_564 4_665 87.04(6) ?
O3 Cs OW2 2_556 4_665 69.69(6) ?
O2 Cs OW2 2_556 4_665 85.68(7) ?
O1 Cs OW2 4_565 4_665 163.61(6) ?
O1 Cs O2 . 4_565 94.88(6) ?
O4 Cs O2 4_564 4_565 111.81(6) ?
O3 Cs O2 2_556 4_565 83.77(6) ?
O2 Cs O2 2_556 4_565 80.69(8) ?
O1 Cs O2 4_565 4_565 43.99(6) ?
OW2 Cs O2 4_665 4_565 152.24(6) ?
O1 Cs OW1 . . 67.15(6) ?
O4 Cs OW1 4_564 . 73.24(6) ?
O3 Cs OW1 2_556 . 144.36(5) ?
O2 Cs OW1 2_556 . 142.85(6) ?
O1 Cs OW1 4_565 . 88.33(6) ?
OW2 Cs OW1 4_665 . 76.06(6) ?
O2 Cs OW1 4_565 . 127.78(6) ?
O1 Cs O2 . 4_564 126.34(6) ?
O4 Cs O2 4_564 4_564 42.23(6) ?
O3 Cs O2 2_556 4_564 82.25(6) ?
O2 Cs O2 2_556 4_564 61.70(8) ?
O1 Cs O2 4_565 4_564 125.49(6) ?
OW2 Cs O2 4_665 4_564 48.26(6) ?
O2 Cs O2 4_565 4_564 137.77(8) ?
OW1 Cs O2 . 4_564 82.32(6) ?
O2 S O1 . . 109.96(15) y
O2 S O3 . . 108.73(15) y
O1 S O3 . . 108.61(14) y
O2 S O4 . . 110.66(16) y
O1 S O4 . . 109.77(14) y
O3 S O4 . . 109.07(13) y
S O1 Cs . . 116.54(12) ?
S O1 Cs . 4_665 98.82(11) ?
Cs O1 Cs . 4_665 119.34(7) ?
S O2 Cs . 2_546 102.10(12) ?
S O2 Cs . 4_665 96.71(12) ?
Cs O2 Cs 2_546 4_665 99.31(8) ?
S O2 Cs . 4_666 93.62(13) ?
Cs O2 Cs 2_546 4_666 118.30(8) ?
Cs O2 Cs 4_665 4_666 137.77(8) ?
S O3 Cs . 2_546 102.83(11) ?
S O4 Cs . 4_666 111.17(13) ?
Cu OW1 Cs . . 134.36(11) ?
Cu OW1 H11 . . 113(5) ?
Cs OW1 H11 . . 87(5) ?
Cu OW1 H12 . . 112(5) ?
Cs OW1 H12 . . 97(5) ?
H11 OW1 H12 . . 112(6) ?
Cu OW2 Cs . 4_565 134.73(10) ?
Cu OW2 H21 . . 122(4) ?
Cs OW2 H21 4_565 . 75(4) ?
Cu OW2 H22 . . 114(5) ?
Cs OW2 H22 4_565 . 101(5) ?
H21 OW2 H22 . . 101(6) ?
Cu OW3 H31 . . 110(5) ?
Cu OW3 H32 . . 117(5) ?
H31 OW3 H32 . . 122(7) ?
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
Cu OW3 . 1.965(2) y
Cu OW3 3 1.965(2) ?
Cu OW1 . 2.005(2) y
Cu OW1 3 2.005(2) ?
Cu OW2 3 2.311(2) ?
Cu OW2 . 2.311(2) y
Cs O1 . 3.098(2) y
Cs O4 4_564 3.114(2) y
Cs O3 2_556 3.151(3) y
Cs O2 2_556 3.179(3) y
Cs O1 4_565 3.182(2) y
Cs OW2 4_665 3.233(3) y
Cs O2 4_565 3.239(3) y
Cs OW1 . 3.422(3) y
Cs O2 4_564 3.528(3) y
Cs S 4_565 3.7066(7) ?
Cs S 2_556 3.7677(7) ?
Cs S 4_564 3.9035(8) ?
Cs H11 . 3.47(6) ?
S O2 . 1.463(2) y
S O1 . 1.474(2) y
S O3 . 1.482(2) y
S O4 . 1.484(2) y
S Cs 4_665 3.7066(7) ?
S Cs 2_546 3.7677(7) ?
S Cs 4_666 3.9035(8) ?
O1 Cs 4_665 3.182(2) ?
O2 Cs 2_546 3.179(3) ?
O2 Cs 4_665 3.239(3) ?
O2 Cs 4_666 3.528(3) ?
O3 Cs 2_546 3.151(3) ?
O4 Cs 4_666 3.114(2) ?
OW1 H11 . 0.77(7) ?
OW1 H12 . 0.76(7) ?
OW2 Cs 4_565 3.233(3) ?
OW2 H21 . 0.87(7) ?
OW2 H22 . 0.74(6) ?
OW3 H31 . 0.75(7) ?
OW3 H32 . 0.70(7) ?
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
OW1 H11 O3 1_555 0.77(7) 1.97(7) 2.714(2) 166(7) y
OW1 H12 O4 1_554 0.75(7) 1.99(7) 2.738(4) 173(7) y
OW2 H21 O2 1_454 0.87(6) 1.91(7) 2.777(3) 174(7) y
OW2 H22 O4 4_564 0.74(6) 2.04(6) 2.779(4) 171(6) y
OW3 H31 O3 3_556 0.74(7) 2.02(7) 2.725(3) 155(7) y
OW3 H32 O1 2_546 0.71(7) 1.99(6) 2.693(3) 171(6) y
