Order-disorder (OD) polytypism of K<sub>3</sub>FeTe<sub>2</sub>O<sub>8</sub>(OH)<sub>2</sub>(H<sub>2</sub>O)<sub>1+x</sub>.
Wolflehner, Tobias; Stöger, Berthold; Acta crystallographica Section B, Structural science, crystal engineering and materials 79 (2023) 510–518; doi:10.1107/S2052520623009162

data_2312336
_publ_section_title
;
 Order-disorder (OD) polytypism of
 K<sub>3</sub>FeTe<sub>2</sub>O<sub>8</sub>(OH)<sub>2</sub>(H<sub>2</sub>O)<sub>1+x</sub>.
;
_journal_issue                   6
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              510
_journal_page_last               518
_journal_paper_doi               10.1107/S2052520623009162
_journal_volume                  79
_journal_year                    2023
_chemical_formula_sum            'Fe H4.86 K3 O11.43 Te2'
_chemical_formula_weight         616.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2023-05-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c185 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.047(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7660(6)
_cell_length_b                   14.9470(6)
_cell_length_c                   5.9706(2)
_cell_measurement_reflns_used    14095
_cell_measurement_temperature    432
_cell_measurement_theta_max      36.20
_cell_measurement_theta_min      2.72
_cell_volume                     1139.27(8)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      432
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
 2678 frames, detector distance = 100 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10382
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        36.030
_diffrn_reflns_theta_max         36.030
_diffrn_reflns_theta_min         2.725
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    7.491
_exptl_absorpt_correction_T_max  0.1043
_exptl_absorpt_correction_T_min  0.0617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1133
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.100
_refine_diff_density_max         3.771
_refine_diff_density_min         -1.670
_refine_diff_density_rms         0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2711
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2207
_reflns_number_total             2711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yv5013sup1.cif
_cod_data_source_block           436K
_cod_depositor_comments
'Adding full bibliography for 2312335--2312336.cif.'
_cod_database_code               2312336
_cod_database_fobs_code          2312336
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.346
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.530(3)
 0.470(3)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
3. Shared sites
{Te1, Fe1'}
{Fe1, Te1'}
4. Restrained distances
 O5-H5 = O6-H6
 0.87 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(Te1) = Uanis(Fe1')
Uanis(Fe1) = Uanis(Te1')
6. Others
 Sof(Te1')=Sof(Fe1')=0.5*(1-FVAR(2))
 Sof(Te1)=Sof(Fe1)=0.5*FVAR(2)
;
_shelx_res_checksum              43818
_shelx_hkl_checksum              8420
_olex2_submission_special_instructions 'No special instructions were received'