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_7719441
_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         'I15 Li3 Nb7 O5'
_chemical_formula_sum            'I15 Li3 Nb7 O5'
_chemical_formula_weight         2654.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-01 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                   14.5783(3)
_cell_length_b                   17.6445(3)
_cell_length_c                   13.5823(2)
_cell_measurement_reflns_used    4174
_cell_measurement_temperature    230.00(11)
_cell_measurement_theta_max      77.8980
_cell_measurement_theta_min      3.8960
_cell_volume                     3493.73(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      230.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -63.00 -18.00   0.50   60.00    --  -90.00  55.00 117.00   90
  2  \w   -159.00 -82.00   0.50   60.00    --  -90.00-110.00-105.00  154
  3  \w   -161.00 -74.00   0.50   60.00    --  -90.00 -68.00 135.00  174
  4  \w    -83.00 -18.00   0.50   60.00    --  -90.00  68.00 -91.00  130
  5  \w     39.00  83.00   0.50   60.00    --  109.74 -68.00 135.00   88
  6  \w    -61.00  22.00   0.50   30.00    --  -49.70  57.00  30.00  166
  7  \w   -118.00 -73.00   0.50   30.00    --  -49.70-125.00 -60.00   90
  8  \w    -26.00  22.00   0.50   30.00    --  -49.70  19.00 120.00   96
  9  \w   -118.00 -73.00   0.50   30.00    --  -49.70-125.00  60.00   90
 10  \w   -160.00 -86.00   0.50   60.00    --  -90.00 -99.00 120.00  148
 11  \w    -85.00 -21.00   0.50   60.00    --  -90.00 125.00 150.00  128
 12  \w   -138.00 -83.00   0.50   60.00    --  -90.00   0.00 -30.00  110
 13  \w    -85.00 -21.00   0.50   60.00    --  -90.00 125.00  30.00  128
 14  \w     61.00 116.00   0.50   60.00    --  109.74   0.00 -90.00  110
 15  \w     39.00  66.00   0.50   60.00    --  109.74 -57.00   0.00   54
 16  \w     39.00  66.00   0.50   60.00    --  109.74 -57.00 -90.00   54
 17  \w     39.00  66.00   0.50   60.00    --  109.74 -57.00 -30.00   54
 18  \w     61.00 116.00   0.50   60.00    --  109.74   0.00 120.00  110
 19  \w     61.00 116.00   0.50   60.00    --  109.74   0.00-120.00  110
 20  \w   -120.00 -38.00   0.50   30.00    --  -49.70 -57.00  60.00  164
 21  \w   -120.00 -30.00   0.50   30.00    --  -49.70 -77.00 -30.00  180
 22  \w   -120.00 -38.00   0.50   30.00    --  -49.70 -57.00-120.00  164
 23  \w   -120.00 -30.00   0.50   30.00    --  -49.70 -77.00-180.00  180
 24  \w   -138.00 -83.00   0.50   60.00    --  -90.00   0.00 -90.00  110
 25  \w     40.00  93.00   0.50   60.00    --  109.74 -99.00 -30.00  106
;
_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      0.0485248000
_diffrn_orient_matrix_UB_12      -0.0628827000
_diffrn_orient_matrix_UB_13      -0.0588978000
_diffrn_orient_matrix_UB_21      0.0502092000
_diffrn_orient_matrix_UB_22      -0.0256647000
_diffrn_orient_matrix_UB_23      0.0940259000
_diffrn_orient_matrix_UB_31      -0.0793118000
_diffrn_orient_matrix_UB_32      -0.0548752000
_diffrn_orient_matrix_UB_33      0.0235238000
_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  0.0316
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17730
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.227
_diffrn_reflns_theta_min         3.933
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    122.292
_exptl_absorpt_correction_T_max  0.358
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    5.047
_exptl_crystal_description       needle
_exptl_crystal_F_000             4524
_exptl_crystal_size_max          0.036
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0329P)^2^+3.4693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1590
_reflns_number_total             1742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01819f2.cif
_cod_data_source_block           jb102_17
_cod_depositor_comments
'Adding full bibliography for 7719441--7719442.cif.'
_cod_database_code               7719441
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Nb7 O5 I15 Li3'
_shelx_estimated_absorpt_t_max   0.245
_shelx_estimated_absorpt_t_min   0.096
_olex2_refinement_description
;
;
_shelx_res_checksum              14092
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.011
_oxdiff_exptl_absorpt_empirical_full_min 0.596