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_7719753
_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, I5 Ta'
_chemical_formula_sum            'I16 O4 Ta6'
_chemical_formula_weight         3180.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-25
_audit_creation_method
;
Olex2 1.5-ac6-018
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6920)
;
_audit_update_record
;
2024-04-25 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            8
_cell_length_a                   17.7586(3)
_cell_length_b                   13.4107(4)
_cell_length_c                   30.4660(6)
_cell_measurement_reflns_used    11467
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      48.5230
_cell_measurement_theta_min      2.0170
_cell_volume                     7255.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.119a 64-bit (release 08-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(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 0.999
_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     68.00 115.00   0.50   90.00    --   59.49 133.00  47.00   94
  2  \w     67.00 120.00   0.50   90.00    --   59.49 135.00-133.00  106
  3  \w     59.00 130.00   0.50   90.00    --   59.49  40.00-178.00  142
  4  \w     -4.00  25.00   0.50   80.00    --    1.41 -99.00 -90.00   58
  5  \w    -38.00 -12.00   0.50   80.00    --    1.41   0.00 -60.00   52
  6  \w    -26.00   1.00   0.50   80.00    --    1.41 -19.00  30.00   54
  7  \w    -60.00   8.00   0.50   90.00    --  -56.68  77.00 -60.00  136
  8  \w    -99.00 -48.00   0.50   90.00    --  -56.68 125.00 -60.00  102
  9  \w     -4.00  21.00   0.50   90.00    --   59.49 -37.00 -30.00   50
 10  \w    -12.00  20.00   0.50   90.00    --   59.49 -37.00-150.00   64
;
_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      0.0049344000
_diffrn_orient_matrix_UB_12      -0.0101742000
_diffrn_orient_matrix_UB_13      -0.0226744000
_diffrn_orient_matrix_UB_21      -0.0194621000
_diffrn_orient_matrix_UB_22      0.0445880000
_diffrn_orient_matrix_UB_23      -0.0053166000
_diffrn_orient_matrix_UB_31      0.0345086000
_diffrn_orient_matrix_UB_32      0.0265719000
_diffrn_orient_matrix_UB_33      0.0002484000
_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  0.0507
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            53383
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.017
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    31.645
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.110
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.111a (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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    5.822
_exptl_crystal_description       plate
_exptl_crystal_F_000             10544
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.947
_refine_diff_density_min         -1.789
_refine_diff_density_rms         0.377
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         6642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+28.7457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5637
_reflns_number_total             6642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02097b2.cif
_cod_data_source_block           fg134_litaoicn_v3
_cod_depositor_comments
'Adding full bibliography for 7719753--7719758.cif.'
_cod_database_code               7719753
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Ta6 O4 I16'
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.095
_olex2_refinement_description
;
1. Others
 Sof(I16)=1-FVAR(1)
 Sof(I16A)=FVAR(1)
;
_shelx_res_checksum              73166
_shelx_hkl_checksum              90289
_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 1.792
_oxdiff_exptl_absorpt_empirical_full_min 0.631