#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/91/2019136.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_2019136
loop_
_publ_author_name
'Weil, Matthias'
_publ_section_title
;
 On the (non-)existence of Tutton salts with formula types
 [M(H₂O)₆](ClO₄)₂(H₂O)₂ and
 Na₂M(SO₄)₂(H₂O)₆ (M is a first-row transition
 metal)
;
_journal_coeditor_code           FN3144
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              990
_journal_page_last               994
_journal_paper_doi               10.1107/S0108270113020027
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[(N H4)1.176 K0.824] Cu (S O4)2 (H2 O)6'
_chemical_formula_moiety
'1.176(N H4 +), 0.824(K +), Cu H12 O6 2+, 2(O4 S 2-)'
_chemical_formula_sum            'Cu H16.704 K0.824 N1.176 O14 S2'
_chemical_formula_weight         417.195
_chemical_name_common            'Tutton salt ammonium/potassium copper'
_chemical_name_systematic
;
Di(ammonium/potassium) hexaaquacopper(II) disulfate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.2345(12)
_cell_length_b                   12.333(3)
_cell_length_c                   9.1822(18)
_cell_measurement_reflns_used    289
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2
_cell_volume                     680.1(3)
_computing_cell_refinement       'PROCESS (Rigaku, 1996)'
_computing_data_collection       'PROCESS (Rigaku, 1996)'
_computing_data_reduction        'PROCESS (Rigaku, 1996)'
_computing_molecular_graphics    'ATOMS for Windows (Dowty, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'coordinates taken from the previous model'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku R-AXIS IV image-plate'
_diffrn_measurement_method       'Oscillation frames'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1322
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.234
_exptl_absorpt_correction_T_max  0.7093
_exptl_absorpt_correction_T_min  0.6072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             427
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.403
_refine_ls_extinction_coef       0.054(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0379P)²+0.6100P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                1257
_reflns_number_total             1322
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fn3144.cif
_cod_data_source_block           FI2054_redetermined
_cod_original_cell_volume        680.1(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019136
_cod_database_fobs_code          2019136
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
K K1 0.8481(2) 0.35099(10) 0.62651(14) 0.0387(5) Uani d P 0.412(5) 1
N N1 0.8481(2) 0.35099(10) 0.62651(14) 0.0387(5) Uani d P 0.588(5) 1
Cu Cu1 0.5000 0.5000 1.0000 0.01986(18) Uani d S 1 2
O O1 0.5347(3) 0.38741(16) 0.8251(2) 0.0344(5) Uani d . 1 1
H H1E 0.5031 0.3269 0.8462 0.052 Uiso d R 1 1
H H1F 0.4391 0.4009 0.7342 0.052 Uiso d R 1 1
O O2 0.3314(3) 0.61377(17) 0.8339(2) 0.0362(5) Uani d . 1 1
H H2E 0.4091 0.6201 0.7650 0.054 Uiso d R 1 1
H H2F 0.1921 0.5941 0.7860 0.054 Uiso d R 1 1
O O3 0.7862(3) 0.56493(14) 0.9975(2) 0.0257(4) Uani d . 1 1
H H3E 0.8249 0.5629 0.9109 0.038 Uiso d R 1 1
H H3F 0.8009 0.6269 1.0249 0.038 Uiso d R 1 1
S S1 0.76452(11) 0.63851(5) 0.59658(7) 0.0252(2) Uani d . 1 1
O O4 0.8778(3) 0.56887(15) 0.7248(2) 0.0293(4) Uani d . 1 1
O O5 0.7358(4) 0.5769(2) 0.4569(2) 0.0491(6) Uani d . 1 1
O O6 0.9066(4) 0.73372(17) 0.5944(3) 0.0417(5) Uani d . 1 1
O O7 0.5467(3) 0.67430(16) 0.6151(2) 0.0359(5) Uani d . 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O4 K1 O7 . 3_666 108.73(7)
O4 K1 O6 . 2_746 102.26(6)
O7 K1 O6 3_666 2_746 138.70(7)
O4 K1 O5 . 3_766 79.30(7)
O7 K1 O5 3_666 3_766 117.01(7)
O6 K1 O5 2_746 3_766 94.77(7)
O4 K1 O6 . 3_766 122.65(7)
O7 K1 O6 3_666 3_766 85.81(7)
O6 K1 O6 2_746 3_766 99.98(6)
O5 K1 O6 3_766 3_766 46.59(6)
O4 K1 O1 . . 70.47(6)
O7 K1 O1 3_666 . 85.60(7)
O6 K1 O1 2_746 . 79.65(6)
O5 K1 O1 3_766 . 147.09(7)
O6 K1 O1 3_766 . 166.23(7)
O4 K1 O5 . . 46.32(6)
O7 K1 O5 3_666 . 71.58(7)
O6 K1 O5 2_746 . 147.28(7)
O5 K1 O5 3_766 . 73.12(8)
O6 K1 O5 3_766 . 93.36(6)
O1 K1 O5 . . 94.12(7)
O4 K1 O2 . 2_646 146.26(7)
O7 K1 O2 3_666 2_646 74.47(6)
O6 K1 O2 2_746 2_646 64.65(6)
O5 K1 O2 3_766 2_646 130.48(7)
O6 K1 O2 3_766 2_646 90.89(6)
O1 K1 O2 . 2_646 76.44(6)
O5 K1 O2 . 2_646 145.35(7)
O3 Cu1 O3 3_667 . 180.0000(10)
O3 Cu1 O2 3_667 3_667 89.90(8)
O3 Cu1 O2 . 3_667 90.10(8)
O3 Cu1 O2 3_667 . 90.10(8)
O3 Cu1 O2 . . 89.90(8)
O2 Cu1 O2 3_667 . 180.0000(10)
O3 Cu1 O1 3_667 3_667 88.90(8)
O3 Cu1 O1 . 3_667 91.10(8)
O2 Cu1 O1 3_667 3_667 91.12(8)
O2 Cu1 O1 . 3_667 88.88(8)
O3 Cu1 O1 3_667 . 91.10(8)
O3 Cu1 O1 . . 88.90(8)
O2 Cu1 O1 3_667 . 88.88(8)
O2 Cu1 O1 . . 91.12(8)
O1 Cu1 O1 3_667 . 180.0
K1 O3 K1 3_767 . 136.21(5)
Cu1 O3 K1 . 2_756 147.73(7)
K1 O3 K1 3_767 2_756 77.98(4)
K1 O3 K1 . 2_756 96.79(4)
O5 S1 O6 . . 109.58(15)
O5 S1 O4 . . 108.51(13)
O6 S1 O4 . . 108.30(12)
O5 S1 O7 . . 110.85(14)
O6 S1 O7 . . 109.70(12)
O4 S1 O7 . . 109.84(11)
S1 O4 K1 . . 108.83(10)
S1 O4 K1 . 2_756 80.40(8)
K1 O4 K1 . 2_756 158.82(6)
S1 O4 K1 . 3_766 56.66(7)
K1 O4 K1 . 3_766 89.06(5)
K1 O4 K1 2_756 3_766 80.16(4)
S1 O5 K1 . 3_766 99.07(13)
S1 O5 K1 . . 93.83(11)
K1 O5 K1 3_766 . 106.88(8)
S1 O5 K1 . 3_666 86.41(11)
K1 O5 K1 3_766 3_666 138.98(9)
K1 O5 K1 . 3_666 113.31(8)
S1 O6 K1 . 2_756 123.09(12)
S1 O6 K1 . 3_766 98.47(11)
K1 O6 K1 2_756 3_766 120.48(8)
S1 O7 K1 . 3_666 120.30(12)
S1 O7 K1 . . 48.17(7)
K1 O7 K1 3_666 . 101.15(6)
S1 O7 K1 . 2_656 150.23(11)
K1 O7 K1 3_666 2_656 89.01(6)
K1 O7 K1 . 2_656 136.85(5)
S1 O7 K1 . 2_756 62.27(8)
K1 O7 K1 3_666 2_756 153.99(7)
K1 O7 K1 . 2_756 97.79(4)
K1 O7 K1 2_656 2_756 89.26(5)
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
K1 O4 . 2.825(2) y
K1 O7 3_666 2.855(3) y
K1 O6 2_746 2.982(3) y
K1 O5 3_766 3.029(3) y
K1 O6 3_766 3.034(3) y
K1 O1 . 3.042(2) y
K1 O5 . 3.177(3) y
K1 O2 2_646 3.188(2) y
Cu1 O3 3_667 1.9616(18) ?
Cu1 O3 . 1.9616(18) ?
Cu1 O2 3_667 2.130(2) ?
Cu1 O2 . 2.130(2) ?
Cu1 O1 3_667 2.178(2) ?
Cu1 O1 . 2.178(2) ?
O2 H2E . 0.8974 ?
O2 H2F . 0.8954 ?
O3 H3E . 0.8911 ?
O3 H3F . 0.8025 ?
S1 O5 . 1.460(2) y
S1 O6 . 1.474(2) y
S1 O4 . 1.4750(18) y
S1 O7 . 1.480(2) y
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
O1 H1E O7 2_646 0.81 1.96 2.760(3) 173.0
O1 H1F O5 3_666 0.90 1.82 2.720(3) 175.0
O2 H2E O7 . 0.90 1.93 2.801(3) 164.1
O2 H2F O4 1_455 0.90 1.91 2.791(3) 166.0
O3 H3E O4 . 0.89 1.83 2.714(2) 173.6
O3 H3F O6 4_576 0.80 1.89 2.676(3) 166.6
