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_7718162
_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         '(I12 Nb4 O)'
_chemical_formula_sum            'I12 Nb4 O'
_chemical_formula_weight         1910.44
_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             2024-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.9189(8)
_cell_length_b                   17.8026(4)
_cell_length_c                   7.3403(2)
_cell_measurement_reflns_used    17063
_cell_measurement_temperature    269.99(10)
_cell_measurement_theta_max      31.9830
_cell_measurement_theta_min      2.2750
_cell_volume                     4955.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.109a 64-bit (release 21-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.111a (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      269.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    -98.00 -18.00   0.50   30.00    --  -31.76 105.00  18.00  160
  2  \w    -60.00  28.00   0.50   30.00    --   33.64 -44.00   6.00  176
  3  \w     42.00 116.00   0.50   30.00    --   33.64 178.00 -30.00  148
  4  \w    -67.00   5.00   0.50   30.00    --   33.64 -19.00 -90.00  144
  5  \w    -67.00   5.00   0.50   30.00    --   33.64 -19.00 -60.00  144
  6  \w    -41.00  22.00   0.50   30.00    --  -31.76 -83.00 168.00  126
  7  \w    -23.00  31.00   0.50   30.00    --  -31.76 -99.00 -90.00  108
  8  \w    -23.00  31.00   0.50   30.00    --  -31.76 -99.00   0.00  108
  9  \w    -23.00  31.00   0.50   30.00    --  -31.76 -99.00  60.00  108
 10  \w    -67.00   5.00   0.50   30.00    --   33.64 -19.00  30.00  144
 11  \w    -67.00   5.00   0.50   30.00    --   33.64 -19.00-150.00  144
 12  \w    -67.00   5.00   0.50   30.00    --   33.64 -19.00 150.00  144
 13  \w    -67.00   5.00   0.50   30.00    --   33.64 -19.00  90.00  144
;
_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      0.0014163472
_diffrn_orient_matrix_UB_12      -0.0225105823
_diffrn_orient_matrix_UB_13      -0.0794629966
_diffrn_orient_matrix_UB_21      0.0101684569
_diffrn_orient_matrix_UB_22      -0.0266095817
_diffrn_orient_matrix_UB_23      0.0491322159
_diffrn_orient_matrix_UB_31      -0.0156261032
_diffrn_orient_matrix_UB_32      -0.0193225324
_diffrn_orient_matrix_UB_33      0.0247717346
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            53804
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.744
_exptl_absorpt_correction_T_max  0.517
_exptl_absorpt_correction_T_min  0.160
_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            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.122
_exptl_crystal_description       block
_exptl_crystal_F_000             6464
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.873
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         9037
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0778P)^2^+14.5761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                8035
_reflns_number_total             9037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00174a1.cif
_cod_data_source_block           jb164(2)_v2
_cod_depositor_comments
'Adding full bibliography for 7718162--7718164.cif.'
_cod_database_code               7718162
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Nb4 O I12'
_shelx_estimated_absorpt_t_max   0.359
_shelx_estimated_absorpt_t_min   0.141
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(9)
 0.51(9)
2. Uiso/Uaniso restraints and constraints
I15 \\sim I15A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.005 within 2A
Uanis(O3) \\sim Ueq, Uanis(O3A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(I16) = Uanis(I16A)
Uanis(O3A) = Uanis(O3)
Uanis(I23) = Uanis(I23A)
Uanis(I18) = Uanis(I18A)
Uanis(I13) = Uanis(I13B) = Uanis(I13A)
Uanis(I25) = Uanis(I25A)
Uanis(I17) = Uanis(I17A)
Uanis(I28) = Uanis(I28A)
3. Others
 Sof(I21A)=Sof(I22A)=Sof(I26A)=Sof(I27A)=Sof(Nb7A)=Sof(Nb8A)=1-FVAR(1)
 Sof(I23A)=Sof(I24A)=Sof(I25A)=Sof(I28A)=Sof(O3A)=0.5*(1-FVAR(2))
 Sof(I23)=Sof(I24)=Sof(I25)=Sof(I28)=Sof(O3)=0.5*FVAR(2)
 Sof(I21)=Sof(I22)=Sof(I26)=Sof(I27)=Sof(Nb7)=Sof(Nb8)=FVAR(1)
 Sof(I13B)=Sof(I15A)=Sof(I16A)=Sof(I13A)=Sof(I17A)=Sof(I18A)=0.5*(1-FVAR(3))
 Sof(I15)=Sof(I16)=Sof(I17)=Sof(I18)=0.5*FVAR(3)
 Sof(I13)=FVAR(2)
;
_shelx_res_checksum              47547
_shelx_hkl_checksum              96264
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.753
_oxdiff_exptl_absorpt_empirical_full_min 0.490