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_7719755
_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      orthorhombic
_space_group_IT_number           26
_space_group_name_Hall           'P 2c -2'
_space_group_name_H-M_alt        'P m c 21'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-28
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-28 deposited with the CCDC.	2025-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.81980(10)
_cell_length_b                   17.85390(10)
_cell_length_c                   15.36720(10)
_cell_measurement_reflns_used    71453
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      44.9120
_cell_measurement_theta_min      2.2720
_cell_volume                     2694.20(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.121a 64-bit (release 24-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      199.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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     -8.00  22.00   0.50   44.00    --  -38.33  54.00 147.00   60
  2  \w     79.00 105.00   0.50   44.00    --   40.83  66.00 -28.00   52
  3  \w     84.00 113.00   0.50   44.00    --   40.83 145.00  16.00   58
  4  \w    -26.00   4.00   0.50   44.00    --   40.83 -19.00  30.00   60
  5  \w     40.00 104.00   0.50   44.00    --   40.83-178.00  60.00  128
  6  \w      1.00  45.00   0.50   44.00    --   40.83   0.00-120.00   88
  7  \w     55.00 112.00   0.50   44.00    --   40.83 178.00-180.00  114
  8  \w     37.00 112.00   0.50   44.00    --   40.83  37.00 -30.00  150
  9  \w      4.00  38.00   0.50   44.00    --   40.83   0.00-180.00   68
 10  \w    -12.00  18.00   0.50   44.00    --   40.83 -77.00 150.00   60
 11  \w    -27.00   5.00   0.50   44.00    --   40.83 -19.00 -60.00   64
 12  \w     -6.00  20.00   0.50   44.00    --   40.83 -37.00-120.00   52
 13  \w    -30.00  -4.00   0.50   44.00    --   40.83 -37.00 -90.00   52
 14  \w     60.00 105.00   0.50   44.00    --   40.83-178.00 -60.00   90
 15  \w     52.00  77.00   0.50   44.00    --   40.83-178.00 120.00   50
 16  \w     -7.00  44.00   0.50   44.00    --   40.83 -57.00-120.00  102
 17  \w    -31.00   2.00   0.50   44.00    --   40.83 -19.00  60.00   66
 18  \w    -74.00 -27.00   0.50   44.00    --  -38.33 -57.00-120.00   94
 19  \w    -53.00 -27.00   0.50   44.00    --  -38.33 -57.00  90.00   52
 20  \w     69.00  95.00   0.50   44.00    --   40.83-141.00 -43.51   52
 21  \w     68.00  95.00   0.50   44.00    --   40.83-141.00 155.77   54
 22  \w     22.00  81.00   0.50   44.00    --   40.83  77.00 -30.00  118
 23  \w     22.00  96.00   0.50   44.00    --   40.83  77.00  30.00  148
 24  \w     22.00  67.00   0.50   44.00    --   40.83  77.00 -90.00   90
 25  \w     22.00 103.00   0.50   44.00    --   40.83  77.00  60.00  162
 26  \w     82.00 109.00   0.50   44.00    --   40.83  77.00 -90.00   54
 27  \w    -14.00  24.00   0.50   44.00    --   40.83 -99.00  60.00   76
 28  \w     30.00  70.00   0.50   44.00    --   40.83 -99.00  60.00   80
 29  \w    -17.00  27.00   0.50   44.00    --   40.83 -99.00-120.00   88
 30  \w     45.00  70.00   0.50   44.00    --   40.83 -99.00-120.00   50
 31  \w     22.00  53.00   0.50   44.00    --   40.83  77.00 120.00   62
 32  \w     85.00 111.00   0.50   44.00    --   40.83  77.00 120.00   52
 33  \w     22.00  87.00   0.50   44.00    --   40.83  77.00-180.00  130
 34  \w     37.00 113.00   0.50   44.00    --   40.83  37.00-150.00  152
 35  \w    -21.00  70.00   0.50   44.00    --   40.83 -99.00-180.00  182
 36  \w     22.00  48.00   0.50   44.00    --   40.83-141.00 155.77   52
 37  \w     54.00  92.00   0.50   44.00    --   40.83-137.00  -2.33   76
 38  \w      8.00  60.00   0.50   44.00    --   40.83 -77.00   0.00  104
 39  \w     22.00  99.00   0.50   44.00    --   40.83  77.00-150.00  154
 40  \w    -22.00  70.00   0.50   44.00    --   40.83 -99.00-150.00  184
 41  \w     37.00 103.00   0.50   44.00    --   40.83  37.00 150.00  132
 42  \w     21.00  48.00   0.50   44.00    --   40.83-137.00  -2.33   54
;
_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      -0.0056686000
_diffrn_orient_matrix_UB_12      -0.0390919000
_diffrn_orient_matrix_UB_13      0.0074191000
_diffrn_orient_matrix_UB_21      -0.0548356000
_diffrn_orient_matrix_UB_22      0.0065083000
_diffrn_orient_matrix_UB_23      0.0290619000
_diffrn_orient_matrix_UB_31      -0.0466776000
_diffrn_orient_matrix_UB_32      -0.0028785000
_diffrn_orient_matrix_UB_33      -0.0350701000
_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  0.0403
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            128478
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.074
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    32.835
_exptl_absorpt_correction_T_max  0.459
_exptl_absorpt_correction_T_min  0.017
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.121a (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            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.830
_exptl_crystal_description       needle
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.509
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.191
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.003(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         8650
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0376P)^2^+11.8426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8578
_reflns_number_total             8650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02097b2.cif
_cod_data_source_block           fgjb144_v3
_cod_depositor_comments
'Adding full bibliography for 7719753--7719758.cif.'
_cod_database_code               7719755
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Ta5 O4 I11'
_shelx_estimated_absorpt_t_max   0.346
_shelx_estimated_absorpt_t_min   0.030
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.997(5)
 0.003(5)
;
_shelx_res_checksum              54796
_shelx_hkl_checksum              384
_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 4.644
_oxdiff_exptl_absorpt_empirical_full_min 0.517