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_7719757
_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 Nb5 O4'
_chemical_formula_sum            'I11 Nb5 O4'
_chemical_formula_weight         1924.45
_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     direct
_audit_creation_date             2025-01-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-07 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                   9.7963(2)
_cell_length_b                   17.8082(3)
_cell_length_c                   15.2052(2)
_cell_measurement_reflns_used    3874
_cell_measurement_temperature    150.01(17)
_cell_measurement_theta_max      78.8210
_cell_measurement_theta_min      3.8020
_cell_volume                     2652.62(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.142a 64-bit (release 17-10-2024))'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(17)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -26.00  21.00   0.50   20.00    --  -49.68   8.00 177.00   94
  2  \w    -86.00 -22.00   0.50   20.00    --  -49.68 134.00-144.00  128
  3  \w    -43.00 -18.00   0.50   60.00    --  -90.00 135.00  34.00   50
  4  \w   -153.00-127.00   0.50   60.00    --  -90.00  -8.00   2.00   52
  5  \w     45.00 103.00   0.50   60.00    --  111.50-121.00-129.00  116
  6  \w    -98.00 -64.00   0.50   20.00    --  -49.68   0.00 120.00   68
  7  \w    -18.00  19.00   0.50   20.00    --  -49.68  19.00-120.00   74
  8  \w    -48.00 -23.00   0.50   60.00    --  -90.00  45.00 -30.00   50
  9  \w     55.00 102.00   0.50   60.00    --  111.50-125.00 150.00   94
 10  \w     44.00  86.00   0.50   60.00    --  111.50-125.00-180.00   84
 11  \w    109.00 165.00   0.50   60.00    --  111.50  30.00-180.00  112
 12  \w     46.00  71.00   0.50   60.00    --  111.50 -61.00 -60.00   50
 13  \w     50.00  76.00   0.50   60.00    --  111.50-135.00 -31.00   52
 14  \w     94.00 119.00   0.50   60.00    --  111.50-135.00 -31.00   50
 15  \w     73.00 107.00   0.50   60.00    --  111.50   0.00 -30.00   68
 16  \w     63.00 108.00   0.50   60.00    --  111.50   0.00 120.00   90
 17  \w     76.00 106.00   0.50   60.00    --  111.50 -94.00-150.00   60
 18  \w     41.00  66.00   0.50   60.00    --  111.50 -61.00 120.00   50
;
_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      0.0001350000
_diffrn_orient_matrix_UB_12      0.0025652000
_diffrn_orient_matrix_UB_13      0.1012730000
_diffrn_orient_matrix_UB_21      -0.0169292000
_diffrn_orient_matrix_UB_22      -0.0859871000
_diffrn_orient_matrix_UB_23      0.0029507000
_diffrn_orient_matrix_UB_31      0.1562976000
_diffrn_orient_matrix_UB_32      -0.0093963000
_diffrn_orient_matrix_UB_33      0.0002437000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10180
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.216
_diffrn_reflns_theta_min         3.823
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    117.683
_exptl_absorpt_correction_T_max  0.718
_exptl_absorpt_correction_T_min  0.082
_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            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    4.819
_exptl_crystal_description       plate
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.205
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.170(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0485
_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^)+(0.1041P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_full    0.701
_reflns_Friedel_fraction_max     0.697
_reflns_number_gt                4114
_reflns_number_total             4407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02097b2.cif
_cod_data_source_block           jb102_52_v1
_cod_depositor_comments
'Adding full bibliography for 7719753--7719758.cif.'
_cod_original_cell_volume        2652.61(8)
_cod_database_code               7719757
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Nb5 O4 I11'
_shelx_estimated_absorpt_t_max   0.417
_shelx_estimated_absorpt_t_min   0.034
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.830(14)
 0.170(14)
;
_shelx_res_checksum              74015
_shelx_hkl_checksum              92766
_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 1.972
_oxdiff_exptl_absorpt_empirical_full_min 0.585