Structural modifications of <i>M</i><sub>5</sub>O<sub>4</sub>I<sub>11</sub> (<i>M</i> = Nb, Ta) cluster networks from heterogeneous solid-state reactions.
Grahlow, Fabian; Beitlberger, Jan; Martin, Mario; Juriatti, Eric; Peisert, Heiko; Scheele, Marcus; Ströbele, Markus; Romao, Carl P.; Meyer, Hans-Jürgen; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16593–16604; doi:10.1039/d5dt02097b

data_7719758
_publ_section_title
;
 Structural modifications of
 <i>M</i><sub>5</sub>O<sub>4</sub>I<sub>11</sub> (<i>M</i> = Nb, Ta)
 cluster networks from heterogeneous solid-state reactions.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16593
_journal_page_last               16604
_journal_paper_doi               10.1039/d5dt02097b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'I11 O4 Ta5'
_chemical_formula_sum            'I11 O4 Ta5'
_chemical_formula_weight         2364.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-18
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-02-18 deposited with the CCDC.	2025-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.500(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.95940(10)
_cell_length_b                   13.60770(10)
_cell_length_c                   11.6208(2)
_cell_measurement_reflns_used    34540
_cell_measurement_temperature    150.00(18)
_cell_measurement_theta_max      45.2280
_cell_measurement_theta_min      2.3500
_cell_volume                     1351.20(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -54.00 -27.00   0.50    5.00    --  -39.26  79.00 -11.00   54
  2  \w    -24.00   1.00   0.50    5.00    --   40.82 -79.00-135.00   50
  3  \w   -104.00 -36.00   0.50    5.00    --  -39.26 -37.00  90.00  136
  4  \w   -110.00 -61.00   0.50    5.00    --  -39.26 178.00 -90.00   98
  5  \w     -8.00  21.00   0.50    5.00    --  -39.26  79.00 -11.00   58
  6  \w    -58.00  12.00   0.50    5.00    --  -39.26  77.00-150.00  140
  7  \w    -95.00 -35.00   0.50    5.00    --  -39.26 -37.00-120.00  120
  8  \w   -105.00 -67.00   0.50    5.00    --  -39.26 178.00-150.00   76
  9  \w   -102.00 -76.00   0.50    5.00    --  -39.26 -57.00  60.00   52
 10  \w    -67.00 -41.00   0.50    5.00    --  -39.26 -57.00  60.00   52
 11  \w   -108.00 -63.00   0.50    5.00    --  -39.26 178.00  90.00   90
 12  \w   -106.00 -63.00   0.50    5.00    --  -39.26-178.00-180.00   86
 13  \w    -30.00  -1.00   0.50    5.00    --   40.82 -19.00 -90.00   58
 14  \w    -31.00   4.00   0.50    5.00    --   40.82 -19.00 150.00   70
 15  \w    -30.00  -5.00   0.50    5.00    --   40.82 -19.00 120.00   50
 16  \w    -28.00  -2.00   0.50    5.00    --   40.82 -19.00  60.00   52
 17  \w    -90.00 -65.00   0.50    5.00    --  -39.26 136.00-125.23   50
 18  \w    -74.00 -31.00   0.50    5.00    --  -39.26 -46.00 -31.35   86
 19  \w   -104.00 -32.00   0.50    5.00    --  -39.26 -43.00 158.76  144
 20  \w   -110.00 -20.00   0.50    5.00    --  -39.26 -77.00-120.00  180
 21  \w    -39.00 -13.00   0.50    5.00    --  -39.26 -92.00 168.45   52
 22  \w    -86.00 -33.00   0.50    5.00    --  -39.26   0.00   0.00  106
 23  \w   -110.00 -49.00   0.50    5.00    --  -39.26 -77.00  90.00  122
 24  \w   -110.00 -83.00   0.50    5.00    --  -39.26 -46.00 -31.35   54
 25  \w   -110.00 -81.00   0.50    5.00    --  -39.26 -77.00 -60.00   58
 26  \w    -46.00  31.00   0.50    5.00    --  -39.26  57.00  90.00  154
 27  \w   -110.00 -79.00   0.50    5.00    --  -39.26 -77.00-150.00   62
 28  \w    -67.00 -20.00   0.50    5.00    --  -39.26 -77.00-150.00   94
 29  \w    -80.00 -20.00   0.50    5.00    --  -39.26 -77.00  30.00  120
 30  \w    -79.00 -28.00   0.50    5.00    --  -39.26 -57.00 120.00  102
 31  \w   -110.00 -40.00   0.50    5.00    --  -39.26 -11.00  83.89  140
 32  \w    -93.00 -43.00   0.50    5.00    --  -39.26 141.00 103.84  100
 33  \w    -46.00 -20.00   0.50    5.00    --  -39.26 -77.00  90.00   52
 34  \w    -93.00 -43.00   0.50    5.00    --  -39.26 141.00   1.08  100
 35  \w   -110.00 -20.00   0.50    5.00    --  -39.26 -77.00 -30.00  180
 36  \w    -65.00 -20.00   0.50    5.00    --  -39.26 -77.00 -60.00   90
 37  \w     41.00  70.00   0.50    5.00    --   40.82 -99.00-120.00   58
 38  \w    -20.00  26.00   0.50    5.00    --   40.82 -99.00-120.00   92
 39  \w     32.00 101.00   0.50    5.00    --   40.82-150.00  55.09  138
 40  \w     25.00  70.00   0.50    5.00    --   40.82 -99.00 120.00   90
 41  \w    -19.00  15.00   0.50    5.00    --   40.82 -99.00 120.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0708642000
_diffrn_orient_matrix_UB_12      0.0128028000
_diffrn_orient_matrix_UB_13      0.0116121000
_diffrn_orient_matrix_UB_21      -0.0362615000
_diffrn_orient_matrix_UB_22      -0.0426602000
_diffrn_orient_matrix_UB_23      -0.0312007000
_diffrn_orient_matrix_UB_31      0.0235785000
_diffrn_orient_matrix_UB_32      -0.0270847000
_diffrn_orient_matrix_UB_33      0.0546411000
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            39410
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         2.370
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    32.735
_exptl_absorpt_correction_T_max  0.717
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.812
_exptl_crystal_description       plate
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       0.000284(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.479
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.479
_refine_ls_R_factor_all          0.0154
_refine_ls_R_factor_gt           0.0154
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+8.8720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0342
_refine_ls_wR_factor_ref         0.0343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2582
_reflns_number_total             2583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02097b2.cif
_cod_data_source_block           fg143_2_v2
_cod_depositor_comments
'Adding full bibliography for 7719753--7719758.cif.'
_cod_database_code               7719758
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Ta5 O4 I11'
_shelx_estimated_absorpt_t_max   0.495
_shelx_estimated_absorpt_t_min   0.067
_olex2_refinement_description
;
;
_shelx_res_checksum              21353
_shelx_hkl_checksum              29900
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.541
_oxdiff_exptl_absorpt_empirical_full_min 0.590