K2Na(I3O8)3: a promising mid-infrared birefringent material with two different structures of octaoxotriiodate(v) polyanions
Lin, Min-Quan; Duan, Meng-Fan; Mao, Jiang-Gao; Yang, Bing-Ping; New Journal of Chemistry 49 (2025) 6103–6108; doi:10.1039/D5NJ00763A

data_7063692
_publ_section_title
;
 K2Na(I3O8)3: a promising mid-infrared birefringent material with two
 different structures of octaoxotriiodate(v) polyanions
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6103
_journal_page_last               6108
_journal_paper_doi               10.1039/D5NJ00763A
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'I9 K2 Na O24'
_chemical_formula_sum            'I9 K2 Na O24'
_chemical_formula_weight         1627.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-12-23
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;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-01-22 deposited with the CCDC.	2025-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
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_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.3(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  31.00   1.00    6.96    --    9.10 -61.00-126.00   51
  2  \w    -19.00  35.00   1.00    6.96    --    9.10-100.00 141.00   54
  3  \w    -12.00  46.00   1.00    6.96    --    9.10 -99.00  30.00   58
  4  \w     -8.00  19.00   1.00    6.96    --   -9.33 -99.00 -30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0563099000
_diffrn_orient_matrix_UB_12      -0.0112942000
_diffrn_orient_matrix_UB_13      0.0019991000
_diffrn_orient_matrix_UB_21      -0.0143471000
_diffrn_orient_matrix_UB_22      0.0175441000
_diffrn_orient_matrix_UB_23      0.0640086000
_diffrn_orient_matrix_UB_31      -0.0189494000
_diffrn_orient_matrix_UB_32      0.0203284000
_diffrn_orient_matrix_UB_33      -0.0541391000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12880
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.798
_diffrn_reflns_theta_min         2.551
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.524
_exptl_crystal_description       block
_exptl_crystal_F_000             2872
_refine_diff_density_max         1.657
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.347
_refine_ls_extinction_coef       0.00034(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0349
_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/[\s^2^(Fo^2^)+(0.0354P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2420
_reflns_number_total             3013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00763a2.cif
_cod_data_source_block           K2Na(I3O8)3
_cod_depositor_comments          'Adding full bibliography for 7063692.cif.'
_cod_original_cell_volume        2389.2(4)
_cod_database_code               7063692
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              3462
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.143
_oxdiff_exptl_absorpt_empirical_full_min 0.489