The family of tetranuclear Nb<sub>4</sub>OI<sub>12-<i>x</i></sub> clusters (<i>x</i> = 0, 1, 2): from the molecular Nb<sub>4</sub>OI<sub>12</sub> cluster to extended chains and layers.
Beitlberger, Jan; Martin, Mario; Scheele, Marcus; Schmidt, Patrick; Ströbele, Markus; Meyer, H-Jürgen; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5486–5493; doi:10.1039/d5dt00174a

data_7718163
_publ_section_title
;
 The family of tetranuclear Nb<sub>4</sub>OI<sub>12-<i>x</i></sub>
 clusters (<i>x</i> = 0, 1, 2): from the molecular
 Nb<sub>4</sub>OI<sub>12</sub> cluster to extended chains and layers.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5486
_journal_page_last               5493
_journal_paper_doi               10.1039/d5dt00174a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'I22 Nb8 O2'
_chemical_formula_sum            'I22 Nb8 O2'
_chemical_formula_weight         3567.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-08
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2024-12-08 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                88.968(2)
_cell_angle_beta                 89.093(2)
_cell_angle_gamma                85.329(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1217(2)
_cell_length_b                   13.9844(3)
_cell_length_c                   16.3913(3)
_cell_measurement_reflns_used    13492
_cell_measurement_temperature    150.01(18)
_cell_measurement_theta_max      38.3710
_cell_measurement_theta_min      3.5930
_cell_volume                     2311.80(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.142a 64-bit (release 17-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.142a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_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    -44.00  21.00   0.50   20.00    --  -21.41  84.00 -91.00  130
  2  \w    -42.00  46.00   0.50   20.00    --   23.60 -84.00 147.00  176
  3  \w    -93.00  -2.00   0.50   20.00    --  -21.41 -77.00  90.00  182
  4  \w    -27.00  50.00   0.50   20.00    --  -21.41  37.00 -90.00  154
  5  \w    -93.00  -2.00   0.50   20.00    --  -21.41 -77.00 -90.00  182
  6  \w    -93.00 -10.00   0.50   20.00    --  -21.41 -57.00   0.00  166
  7  \w    -93.00 -10.00   0.50   20.00    --  -21.41 -57.00 150.00  166
  8  \w    -93.00  -2.00   0.50   20.00    --  -21.41 -77.00 -30.00  182
  9  \w    -48.00   5.00   0.50   20.00    --   23.60 -19.00-150.00  106
 10  \w    -48.00   5.00   0.50   20.00    --   23.60 -19.00  30.00  106
 11  \w     39.00  95.00   0.50   20.00    --   23.60-178.00  60.00  112
 12  \w      4.00  95.00   0.50   20.00    --   23.60  77.00-120.00  182
 13  \w    -93.00 -10.00   0.50   20.00    --  -21.41 -57.00 120.00  166
 14  \w    -48.00   5.00   0.50   20.00    --   23.60 -19.00 -60.00  106
 15  \w    -23.00  53.00   0.50   20.00    --   23.60 -99.00 120.00  152
 16  \w    -23.00  53.00   0.50   20.00    --   23.60 -99.00-120.00  152
 17  \w    -23.00  53.00   0.50   20.00    --   23.60 -99.00 -60.00  152
 18  \w    -23.00  53.00   0.50   20.00    --   23.60 -99.00  60.00  152
 19  \w    -23.00  53.00   0.50   20.00    --   23.60 -99.00  30.00  152
 20  \w    -23.00  53.00   0.50   20.00    --   23.60 -99.00-150.00  152
 21  \w    -23.00  25.00   0.50   20.00    --   23.60 -99.00 -30.00   96
 22  \w     39.00  95.00   0.50   20.00    --   23.60-178.00 -90.00  112
;
_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      0.0259904000
_diffrn_orient_matrix_UB_12      -0.0276487000
_diffrn_orient_matrix_UB_13      0.0336406000
_diffrn_orient_matrix_UB_21      0.0200786000
_diffrn_orient_matrix_UB_22      0.0421974000
_diffrn_orient_matrix_UB_23      0.0178841000
_diffrn_orient_matrix_UB_31      -0.0621766000
_diffrn_orient_matrix_UB_32      0.0067415000
_diffrn_orient_matrix_UB_33      0.0205429000
_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  0.020
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17704
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.019
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.607
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.142a (Rigaku Oxford Diffraction, 2024)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    5.124
_exptl_crystal_description       block
_exptl_crystal_F_000             3020
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         17704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0301P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16216
_reflns_number_total             17704
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9968\% 
around [0.00 0.00 1.00] (reciprocal) or [-0.02 -0.02 1.00] (direct)
;
_cod_data_source_file            d5dt00174a1.cif
_cod_data_source_block           nb4oi11v5_twin
_cod_depositor_comments
'Adding full bibliography for 7718162--7718164.cif.'
_cod_database_code               7718163
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'O2 Nb8 I22 '
_shelx_estimated_absorpt_t_max   0.491
_shelx_estimated_absorpt_t_min   0.389
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4924(4)
 0.5076(4)
;
_shelx_res_checksum              55547
_shelx_hkl_checksum              63182
_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 1.172
_oxdiff_exptl_absorpt_empirical_full_min 0.873
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2