On the (non-)existence of Tutton salts with formula types [<i>M</i>(H~2~O)~6~](ClO~4~)~2~(H~2~O)~2~ and Na~2~<i>M</i>(SO~4~)~2~(H~2~O)~6~ (<i>M</i> is a first-row transition metal)
Weil, Matthias; Acta Crystallographica Section C 69 (2013) 990–994; doi:10.1107/S0108270113020027

data_2019136
_publ_section_title
;
 On the (non-)existence of Tutton salts with formula types
 [<i>M</i>(H~2~O)~6~](ClO~4~)~2~(H~2~O)~2~ and
 Na~2~<i>M</i>(SO~4~)~2~(H~2~O)~6~ (<i>M</i> 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0379P)^2^+0.6100P] where P=(Fo^2^+2Fc^2^)/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