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_7718164
_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         'I11 Nb4 O'
_chemical_formula_sum            'I11 Nb4 O'
_chemical_formula_weight         1783.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-15 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.698(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4442(3)
_cell_length_b                   13.0449(2)
_cell_length_c                   11.9078(2)
_cell_measurement_reflns_used    18269
_cell_measurement_temperature    220.0(9)
_cell_measurement_theta_max      45.2750
_cell_measurement_theta_min      2.0500
_cell_volume                     2309.56(7)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.0(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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    -61.00 -27.00   0.50   65.00    --  -39.27 107.00 -57.00   68
  2  \w      4.00  35.00   0.50   65.00    --   40.83-107.00-155.00   62
  3  \w   -110.00 -34.00   0.50   65.00    --  -39.27 -37.00   0.00  152
  4  \w   -109.00 -77.00   0.50   65.00    --  -39.27 178.00 120.00   64
  5  \w   -107.00 -27.00   0.50   65.00    --  -39.27 -77.00-150.00  160
  6  \w    -88.00 -33.00   0.50   65.00    --  -39.27   0.00-150.00  110
  7  \w   -110.00 -84.00   0.50   65.00    --  -39.27 -57.00-120.00   52
  8  \w    -44.00  18.00   0.50   65.00    --  -39.27  19.00-150.00  124
  9  \w    -61.00 -29.00   0.50   65.00    --  -39.27 -57.00-120.00   64
 10  \w    -13.00  27.00   0.50   65.00    --  -39.27  57.00  30.00   80
 11  \w    -43.00   0.00   0.50   65.00    --  -39.27  57.00 -90.00   86
 12  \w   -110.00 -66.00   0.50   65.00    --  -39.27 178.00-150.00   88
 13  \w   -110.00 -22.00   0.50   65.00    --  -39.27 -77.00 120.00  176
 14  \w    -96.00 -20.00   0.50   65.00    --  -39.27 -77.00-120.00  152
 15  \w    -24.00   2.00   0.50   65.00    --   40.83 -19.00   0.00   52
 16  \w     43.00  69.00   0.50   65.00    --   40.83 -99.00 -60.00   52
 17  \w    -22.00  20.00   0.50   65.00    --   40.83 -99.00 -60.00   84
 18  \w     87.00 112.00   0.50   65.00    --   40.83-178.00 -60.00   50
 19  \w     46.00  71.00   0.50   65.00    --   40.83-178.00 -60.00   50
 20  \w    -26.00   4.00   0.50   65.00    --   40.83 -19.00 -30.00   60
 21  \w      4.00  30.00   0.50   65.00    --   40.83   0.00-120.00   52
 22  \w    -64.00 -21.00   0.50   65.00    --  -39.27 -74.00   0.70   86
 23  \w     -4.00  32.00   0.50   65.00    --  -39.27  37.00-150.00   72
 24  \w   -110.00 -29.00   0.50   65.00    --  -39.27 -52.00 140.34  162
 25  \w   -111.00 -66.00   0.50   65.00    --  -39.27 -25.00-167.43   90
 26  \w    -89.00 -40.00   0.50   65.00    --  -39.27 135.00  26.80   98
 27  \w    -91.00 -49.00   0.50   65.00    --  -39.27 139.00 -16.89   84
 28  \w    -38.00 -13.00   0.50   65.00    --  -39.27 -92.00  55.39   50
 29  \w    -98.00 -34.00   0.50   65.00    --  -39.27 -37.00 -90.00  128
 30  \w   -108.00 -81.00   0.50   65.00    --  -39.27 -74.00   0.70   54
 31  \w    -89.00 -46.00   0.50   65.00    --  -39.27 135.00  98.04   86
 32  \w    -89.00 -63.00   0.50   65.00    --  -39.27 -77.00 -60.00   52
 33  \w    -50.00 -20.00   0.50   65.00    --  -39.27 -77.00 -60.00   60
 34  \w    -90.00 -41.00   0.50   65.00    --  -39.27 137.00 143.68   98
 35  \w    -87.00 -34.00   0.50   65.00    --  -39.27   0.00  90.00  106
 36  \w   -107.00 -74.00   0.50   65.00    --  -39.27 -57.00  60.00   66
 37  \w    -70.00 -28.00   0.50   65.00    --  -39.27 -57.00  60.00   84
 38  \w   -103.00 -70.00   0.50   65.00    --  -39.27 -77.00-180.00   66
 39  \w    -47.00 -20.00   0.50   65.00    --  -39.27 -77.00-180.00   54
 40  \w    -41.00 -14.00   0.50   65.00    --  -39.27  37.00-150.00   54
 41  \w     27.00  59.00   0.50   65.00    --   40.83-153.00   4.37   64
 42  \w    -27.00   5.00   0.50   65.00    --   40.83 -19.00  60.00   64
 43  \w     78.00 103.00   0.50   65.00    --   40.83-153.00   4.37   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      0.0079757000
_diffrn_orient_matrix_UB_12      -0.0155283000
_diffrn_orient_matrix_UB_13      0.0589941000
_diffrn_orient_matrix_UB_21      -0.0136768000
_diffrn_orient_matrix_UB_22      -0.0505658000
_diffrn_orient_matrix_UB_23      -0.0185354000
_diffrn_orient_matrix_UB_31      0.0450105000
_diffrn_orient_matrix_UB_32      -0.0126087000
_diffrn_orient_matrix_UB_33      0.0016586000
_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  0.0189
_diffrn_reflns_av_unetI/netI     0.0067
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            44103
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.698
_diffrn_reflns_theta_min         2.077
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.624
_exptl_absorpt_correction_T_max  0.731
_exptl_absorpt_correction_T_min  0.566
_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    5.129
_exptl_crystal_description       block
_exptl_crystal_F_000             3020
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.000165(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.430
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         3115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.430
_refine_ls_R_factor_all          0.0151
_refine_ls_R_factor_gt           0.0150
_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^)+15.3976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0314
_refine_ls_wR_factor_ref         0.0315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3104
_reflns_number_total             3115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00174a1.cif
_cod_data_source_block           jb189(6)v3
_cod_depositor_comments
'Adding full bibliography for 7718162--7718164.cif.'
_cod_database_code               7718164
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Nb4 O I11'
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.462
_olex2_refinement_description
;
1. Others
 Fixed Sof: Nb2(0.5)
;
_shelx_res_checksum              14222
_shelx_hkl_checksum              91301
_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 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.850