Niobium oxyiodide cluster compounds Li<sub>3</sub>Nb<sub>7</sub>O<sub>5</sub>I<sub>15</sub> and Nb<sub>8</sub>O<sub>5</sub>I<sub>17</sub>(NbI<sub>5</sub>) with expanding cluster architectures and multicentre Nb-Nb bonding.
Beitlberger, Jan; Ströbele, Markus; Schmidt, Patrick; Romao, Carl P.; Meyer, H-Jürgen; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14376–14383; doi:10.1039/d5dt01819f

data_7719442
_publ_section_title
;
 Niobium oxyiodide cluster compounds
 Li<sub>3</sub>Nb<sub>7</sub>O<sub>5</sub>I<sub>15</sub> and
 Nb<sub>8</sub>O<sub>5</sub>I<sub>17</sub>(NbI<sub>5</sub>) with expanding
 cluster architectures and multicentre Nb-Nb bonding.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14376
_journal_page_last               14383
_journal_paper_doi               10.1039/d5dt01819f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'I17 Nb8 O5, I4.788 Nb, I0.583'
_chemical_formula_sum            'I22.37 Nb9 O5'
_chemical_formula_weight         3755.26
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-04 deposited with the CCDC.	2025-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4282(4)
_cell_length_b                   13.4336(6)
_cell_length_c                   31.5794(12)
_cell_measurement_reflns_used    4242
_cell_measurement_temperature    200.0(3)
_cell_measurement_theta_max      77.5800
_cell_measurement_theta_min      3.5390
_cell_volume                     4848.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.142a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -13.00  15.00   0.50   15.00    --  -49.67  23.00 -28.00   56
  2  \w     47.00 117.00   0.50   15.00    --   49.67  23.00 -28.00  140
  3  \w   -151.00-124.00   0.50   30.00    --  -90.00 -23.00 165.00   54
  4  \w    -63.00 -28.00   0.50   30.00    --  -90.00 118.00  47.00   70
  5  \w     67.00 110.00   0.50   30.00    --  111.50-118.00 -38.00   86
  6  \w    113.00 177.00   0.50   30.00    --  111.50  23.00 -28.00  128
  7  \w    109.00 136.00   0.50   30.00    --  111.50 104.00 147.00   54
  8  \w    118.00 155.00   0.50   30.00    --  111.50 118.00  47.00   74
  9  \w    -61.00  22.00   0.50   15.00    --  -49.67  57.00   0.00  166
 10  \w    -26.00  22.00   0.50   15.00    --  -49.67  19.00  60.00   96
 11  \w   -117.00 -90.00   0.50   15.00    --  -49.67-125.00 -90.00   54
 12  \w   -118.00 -87.00   0.50   15.00    --  -49.67-125.00 -60.00   62
 13  \w     47.00  75.00   0.50   30.00    --  111.50-125.00  90.00   56
 14  \w     78.00 111.00   0.50   30.00    --  111.50-125.00  90.00   66
 15  \w     56.00  99.00   0.50   30.00    --  111.50 -94.00   0.00   86
 16  \w     43.00  68.00   0.50   30.00    --  111.50 -61.00 120.00   50
 17  \w     54.00 110.00   0.50   30.00    --  111.50-125.00  60.00  112
 18  \w     42.00  67.00   0.50   30.00    --  111.50 -61.00  60.00   50
 19  \w     41.00  70.00   0.50   30.00    --  111.50 -61.00 -30.00   58
 20  \w     72.00 105.00   0.50   30.00    --  111.50 -94.00 -30.00   66
 21  \w     42.00  70.00   0.50   30.00    --  111.50 -61.00 -90.00   56
 22  \w     41.00 100.00   0.50   30.00    --  111.50 -76.00  26.12  118
 23  \w    110.00 166.00   0.50   30.00    --  111.50  30.00  90.00  112
 24  \w    115.00 171.00   0.50   30.00    --  111.50  30.00-120.00  112
 25  \w    112.00 162.00   0.50   30.00    --  111.50  30.00  30.00  100
 26  \w    137.00 178.00   0.50   30.00    --  111.50  30.00   0.00   82
 27  \w     43.00  86.00   0.50   30.00    --  111.50 -94.00-150.00   86
 28  \w     85.00 114.00   0.50   30.00    --  111.50   0.00 120.00   58
 29  \w     45.00  71.00   0.50   30.00    --  111.50 -94.00  90.00   52
 30  \w     64.00  90.00   0.50   30.00    --  111.50   0.00  30.00   52
 31  \w     44.00  70.00   0.50   30.00    --  111.50 -61.00  90.00   52
 32  \w     77.00 103.00   0.50   30.00    --  111.50-104.00  45.00   52
 33  \w     51.00 105.00   0.50   30.00    --  111.50 -77.00-150.00  108
 34  \w     76.00 111.00   0.50   30.00    --  111.50-125.00   0.00   70
 35  \w     41.00  70.00   0.50   30.00    --  111.50 -61.00 -60.00   58
 36  \w    -46.00 -21.00   0.50   30.00    --  -90.00 123.00 -46.00   50
 37  \w   -118.00 -93.00   0.50   15.00    --  -49.67-125.00-180.00   50
 38  \w     51.00 100.00   0.50   30.00    --  111.50-125.00-150.00   98
 39  \w     46.00  73.00   0.50   30.00    --  111.50 -77.00  90.00   54
 40  \w     81.00 106.00   0.50   30.00    --  111.50 -77.00  90.00   50
 41  \w     98.00 155.00   0.50   30.00    --  111.50  61.00-120.00  114
 42  \w    152.00 178.00   0.50   30.00    --  111.50  15.00 150.00   52
 43  \w     80.00 106.00   0.50   30.00    --  111.50 -94.00 -60.00   52
 44  \w     71.00  97.00   0.50   30.00    --  111.50 -94.00  90.00   52
 45  \w     80.00 106.00   0.50   30.00    --  111.50 -94.00 -30.00   52
 46  \w     85.00 111.00   0.50   30.00    --  111.50-125.00  60.00   52
 47  \w    112.00 138.00   0.50   30.00    --  111.50  15.00 150.00   52
;
_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      -0.0142247000
_diffrn_orient_matrix_UB_12      0.1133429000
_diffrn_orient_matrix_UB_13      -0.0052691000
_diffrn_orient_matrix_UB_21      0.1295043000
_diffrn_orient_matrix_UB_22      0.0083927000
_diffrn_orient_matrix_UB_23      -0.0130719000
_diffrn_orient_matrix_UB_31      -0.0346652000
_diffrn_orient_matrix_UB_32      -0.0151631000
_diffrn_orient_matrix_UB_33      -0.0466854000
_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  0.0589
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47074
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.653
_diffrn_reflns_theta_max         66.653
_diffrn_reflns_theta_min         2.799
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    128.729
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.176
_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    5.145
_exptl_crystal_description       plate
_exptl_crystal_F_000             6379
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.011
_exptl_crystal_size_min          0.009
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0259P)^2^+2.6937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3739
_reflns_number_total             4437
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9979\% 
around [-0.24 0.00 0.97] (reciprocal) or [-0.89 -0.00 0.46] (direct)
;
_cod_data_source_file            d5dt01819f3.cif
_cod_data_source_block           Nb9O5I22
_cod_depositor_comments
'Adding full bibliography for 7719441--7719442.cif.'
_cod_database_code               7719442
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'O2.50 Nb4.50 I11 '
_olex2_refinement_description
;
1. Others
 Sof(Nb6B)=0.5*(1-FVAR(2))
 Sof(Nb6A)=0.5*FVAR(2)
 Sof(I11A)=0.5*(1-FVAR(3))
 Sof(I11B)=0.5*FVAR(3)
;
_shelx_res_checksum              63426
_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 2.378
_oxdiff_exptl_absorpt_empirical_full_min 0.615
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2