# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jb164(2)_v2
_database_code_depnum_ccdc_archive 'CCDC 2366237'
loop_
_audit_author_name
_audit_author_address
'Markus Stroebele'
;University of Tuebingen
Germany
;
_audit_update_record             
;
2024-06-27 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_jb1642_v2           
;
PROBLEM: Check Calcd Resid. Dens.  0.66Ang From I15A           -3.13 eA-3  
RESPONSE: We have used three different refinement programs
(Jana2006, Shelxl and olex2.refine) to check this alert. All programs show much smaller residual density on the Iodine or Niobium atoms. Therefore, we assume that there is an error in the checkcif calculation.
;
# end Validation Reply Form
_audit_creation_date             2024-03-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '(I12 Nb4 O)'
_chemical_formula_sum            'I12 Nb4 O'
_chemical_formula_weight         1910.44
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Nb4 O I12'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           26
_space_group_name_H-M_alt        'P m c 21'
_space_group_name_Hall           'P 2c -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'

_cell_length_a                   37.9189(8)
_cell_length_b                   17.8026(4)
_cell_length_c                   7.3403(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4955.1(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    17063
_cell_measurement_temperature    269.99(10)
_cell_measurement_theta_max      31.9830
_cell_measurement_theta_min      2.2750
_shelx_estimated_absorpt_T_max   0.359
_shelx_estimated_absorpt_T_min   0.141
_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_absorpt_special_details   ?
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.122
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6464
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-32 11 7 0.0649
44 0 -6 0.0861
-48 -11 1 0.0158
9 24 -3 0.0646
53 -2 -1 0.0985
7 -24 3 0.0172
-30 21 -2 0.0429
7 -25 0 0.0139
5 -25 -1 0.0147
10 -22 -5 0.0287
17 -14 -8 0.0457
14 -6 -10 0.0589
29 -3 9 0.0867
11 -15 8 0.0479
52 2 2 0.1076
41 -13 4 0.0834
-44 0 6 0.0398
45 12 -3 0.0996
4 -4 10 0.0702

_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.077
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-31.5446 10.9194 7.0323 -0.8493 -0.2658 0.4561
44.3986 0.3427 -5.7672 0.5135 0.1590 -0.8433
-48.0032 -10.7030 1.1859 0.0787 -0.1451 0.9863
9.0173 23.6833 -2.9516 -0.2858 -0.6835 -0.6716
52.9676 -1.5314 -1.2843 0.2115 0.5163 -0.8299
7.1084 -24.0889 2.5537 0.3494 0.8387 0.4176
-29.7289 20.5225 -1.5235 -0.3830 -0.9232 0.0303
6.7219 -24.8731 0.4055 0.5372 0.7501 0.3856
5.1016 -24.7352 -1.4223 0.6771 0.6402 0.3630
10.4645 -22.0277 -4.5137 0.8693 0.4708 0.1503
17.4357 -13.5708 -8.0167 0.9672 0.1445 -0.2088
14.1733 -6.4913 -9.6081 0.9297 -0.1552 -0.3341
29.1582 -2.6468 8.6049 -0.5829 0.7897 -0.1913
11.3622 -15.2501 7.9201 -0.2700 0.9105 0.3133
51.7675 2.2648 2.4293 -0.1707 0.5855 -0.7925
41.2488 -13.1790 3.7170 0.0597 0.9527 -0.2978
-44.4310 -0.3967 5.7573 -0.5115 -0.1584 0.8446
44.5943 11.6880 -3.0794 0.0448 -0.0089 -0.9990
4.2793 -4.1025 10.1745 -0.7101 0.6526 0.2644

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00 -18.00   0.50   30.00    --  -31.76 105.00  18.00  160
  2  ω    -60.00  28.00   0.50   30.00    --   33.64 -44.00   6.00  176
  3  ω     42.00 116.00   0.50   30.00    --   33.64 178.00 -30.00  148
  4  ω    -67.00   5.00   0.50   30.00    --   33.64 -19.00 -90.00  144
  5  ω    -67.00   5.00   0.50   30.00    --   33.64 -19.00 -60.00  144
  6  ω    -41.00  22.00   0.50   30.00    --  -31.76 -83.00 168.00  126
  7  ω    -23.00  31.00   0.50   30.00    --  -31.76 -99.00 -90.00  108
  8  ω    -23.00  31.00   0.50   30.00    --  -31.76 -99.00   0.00  108
  9  ω    -23.00  31.00   0.50   30.00    --  -31.76 -99.00  60.00  108
 10  ω    -67.00   5.00   0.50   30.00    --   33.64 -19.00  30.00  144
 11  ω    -67.00   5.00   0.50   30.00    --   33.64 -19.00-150.00  144
 12  ω    -67.00   5.00   0.50   30.00    --   33.64 -19.00 150.00  144
 13  ω    -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       'ω 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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_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_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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_coef       .
_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_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0517
_refine_ls_restrained_S_all      1.084
_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/[σ²(Fo²)+(0.0778P)²+14.5761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1467
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_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)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.25058(4) 0.84709(9) 1.4195(3) 0.0405(8) Uani 1 1 d . . . . .
I2 I 0.25144(5) 0.93464(9) 0.9274(3) 0.0463(8) Uani 1 1 d . . . . .
I3 I 0.32617(5) 0.70088(10) 1.2787(3) 0.0482(8) Uani 1 1 d . . . . .
I4 I 0.32637(5) 0.79495(9) 0.7745(3) 0.0469(8) Uani 1 1 d . . . . .
I5 I 0.24892(5) 0.56475(10) 1.1264(3) 0.0503(8) Uani 1 1 d . . . . .
I6 I 0.24964(5) 0.65193(10) 0.6317(3) 0.0440(8) Uani 1 1 d . . . . .
I7 I 0.17368(5) 0.70501(10) 1.2790(3) 0.0466(8) Uani 1 1 d . . . . .
I8 I 0.17378(5) 0.79907(10) 0.7761(3) 0.0516(8) Uani 1 1 d . . . . .
I9 I 0.16383(6) 0.93011(12) 1.2174(3) 0.0621(9) Uani 1 1 d . . . . .
I10 I 0.33860(6) 0.92417(11) 1.2227(3) 0.0607(9) Uani 1 1 d . . . . .
I11 I 0.33715(6) 0.57159(11) 0.8286(4) 0.0620(9) Uani 1 1 d . . . . .
I12 I 0.16125(6) 0.57722(13) 0.8229(4) 0.0690(9) Uani 1 1 d . . . . .
Nb1 Nb 0.21026(6) 0.82296(13) 1.1026(3) 0.0391(8) Uani 1 1 d . . . . .
Nb2 Nb 0.29072(6) 0.82072(13) 1.1025(3) 0.0380(8) Uani 1 1 d . . . . .
Nb3 Nb 0.28973(6) 0.67672(13) 0.9487(4) 0.0419(9) Uani 1 1 d . . . . .
Nb4 Nb 0.20946(6) 0.67930(13) 0.9498(4) 0.0432(9) Uani 1 1 d . . . . .
O1 O 0.2501(6) 0.7533(12) 1.038(4) 0.045(3) Uani 1 1 d . . . . .
I14 I 0.42317(5) 0.79662(10) 0.3491(3) 0.0543(8) Uani 1 1 d . . . . .
I19 I 0.41189(6) 0.57482(12) 0.3967(4) 0.0667(9) Uani 1 1 d . . . . .
I20 I 0.41290(6) 0.92829(11) 0.7886(4) 0.0643(9) Uani 1 1 d . . . . .
Nb5 Nb 0.45979(7) 0.67804(13) 0.5209(4) 0.0443(9) Uani 1 1 d . . . . .
Nb6 Nb 0.45993(7) 0.82232(13) 0.6753(4) 0.0426(9) Uani 1 1 d . . . . .
O2 O 0.500000 0.7538(16) 0.611(5) 0.062(8) Uani 1 2 d S T P A .
I13 I 0.42402(6) 0.70309(11) 0.8517(3) 0.0458(9) Uani 0.947(4) 1 d . . P A 3
I15 I 0.500000 0.84739(12) 0.9920(4) 0.0397(9) Uani 0.947(4) 2 d S TU P A 3
I16 I 0.500000 0.93446(12) 0.4959(4) 0.0482(9) Uani 0.947(4) 2 d S T P A 3
I17 I 0.500000 0.56431(13) 0.6949(5) 0.0467(9) Uani 0.947(4) 2 d S T P A 3
I18 I 0.500000 0.65274(12) 0.2021(4) 0.0404(9) Uani 0.947(4) 2 d S T P A 3
I13B I 0.401(2) 0.706(3) 0.860(8) 0.0458(9) Uani 0.026(2) 1 d . . P A 4
I15A I 0.5082(13) 0.871(3) 0.908(8) 0.0395(12) Uani 0.026(2) 1 d . U P A 4
I16A I 0.500000 0.910(2) 0.371(7) 0.0482(9) Uani 0.053(4) 2 d S T P A 4
I13A I 0.438(2) 0.699(4) 0.829(12) 0.0458(9) Uani 0.026(2) 1 d . . P A 5
I21 I 0.07685(7) 0.70357(17) 0.6632(6) 0.0540(10) Uani 0.699(4) 1 d . . P B 1
I22 I 0.07588(7) 0.79688(16) 0.1603(6) 0.0505(10) Uani 0.699(4) 1 d . . P B 1
I23 I 0.000000 0.8469(2) 0.8024(5) 0.0466(10) Uani 0.699(4) 2 d S T P B 1
I24 I 0.000000 0.9347(2) 0.3092(8) 0.0528(12) Uani 0.699(4) 2 d S T P B 1
I25 I 0.000000 0.6512(2) 0.0133(5) 0.0489(10) Uani 0.699(4) 2 d S T P B 1
I26 I 0.08751(9) 0.5719(2) 0.2215(7) 0.0653(12) Uani 0.699(4) 1 d . . P B 1
I27 I 0.08750(9) 0.9265(2) 0.6121(7) 0.0692(12) Uani 0.699(4) 1 d . . P B 1
I28 I 0.000000 0.5651(2) 0.5114(6) 0.0514(11) Uani 0.699(4) 2 d S T P B 1
Nb7 Nb 0.03994(9) 0.6776(2) 0.3374(7) 0.0472(12) Uani 0.699(4) 1 d . . P B 1
Nb8 Nb 0.04018(9) 0.8222(2) 0.4898(7) 0.0450(11) Uani 0.699(4) 1 d . . P B 1
O3 O 0.000000 0.754(2) 0.429(5) 0.042(7) Uani 0.699(4) 2 d S TU P B 1
I21A I 0.0760(2) 0.7035(4) 0.7768(12) 0.0594(18) Uani 0.301(4) 1 d . . P B 2
I22A I 0.07571(19) 0.7971(4) 0.2710(12) 0.0570(18) Uani 0.301(4) 1 d . . P B 2
I23A I 0.000000 0.8489(5) 0.9075(15) 0.0466(10) Uani 0.301(4) 2 d S T P B 2
I24A I 0.000000 0.9363(7) 0.417(2) 0.063(3) Uani 0.301(4) 2 d S T P B 2
I25A I 0.000000 0.6529(5) 0.1244(15) 0.0489(10) Uani 0.301(4) 2 d S T P B 2
I26A I 0.0890(3) 0.5763(6) 0.3264(17) 0.078(3) Uani 0.301(4) 1 d . . P B 2
I27A I 0.0873(3) 0.9257(6) 0.7190(17) 0.074(2) Uani 0.301(4) 1 d . . P B 2
I28A I 0.000000 0.5629(6) 0.6150(17) 0.0514(11) Uani 0.301(4) 2 d S T P B 2
Nb7A Nb 0.0395(3) 0.6790(6) 0.4543(14) 0.057(2) Uani 0.301(4) 1 d . . P B 2
Nb8A Nb 0.0400(3) 0.8208(6) 0.6041(14) 0.055(2) Uani 0.301(4) 1 d . . P B 2
O3A O 0.000000 0.754(5) 0.540(12) 0.042(7) Uani 0.301(4) 2 d S TU P B 2
I17A I 0.5179(19) 0.562(3) 0.712(10) 0.0467(9) Uani 0.026(2) 1 d . . P A 4
I18A I 0.5183(17) 0.654(3) 0.185(8) 0.0404(9) Uani 0.026(2) 1 d . . P A 4


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Nb1 2.816(3) . ?
I1 Nb2 2.820(3) . ?
I2 Nb1 2.837(3) . ?
I2 Nb2 2.825(3) . ?
I3 Nb2 2.834(3) . ?
I3 Nb3 2.822(3) . ?
I4 Nb2 2.799(3) . ?
I4 Nb3 2.828(3) . ?
I5 Nb3 2.841(3) . ?
I5 Nb4 2.842(3) . ?
I6 Nb3 2.814(3) . ?
I6 Nb4 2.830(3) . ?
I7 Nb1 2.830(3) . ?
I7 Nb4 2.809(3) . ?
I8 Nb1 2.800(3) . ?
I8 Nb4 2.829(3) . ?
I9 Nb1 2.729(3) . ?
I10 Nb2 2.733(3) . ?
I11 Nb3 2.741(3) . ?
I12 Nb4 2.741(3) . ?
Nb1 Nb2 3.051(3) . ?
Nb1 Nb4 2.793(3) . ?
Nb1 O1 2.01(2) . ?
Nb2 Nb3 2.801(3) . ?
Nb2 O1 2.01(2) . ?
Nb3 Nb4 3.044(4) . ?
Nb3 O1 2.13(2) . ?
Nb4 O1 2.13(2) . ?
I14 Nb5 2.824(3) . ?
I14 Nb6 2.808(3) . ?
I19 Nb5 2.740(3) . ?
I20 Nb6 2.726(3) . ?
Nb5 Nb5 3.049(5) 4_655 ?
Nb5 Nb6 2.807(3) . ?
Nb5 O2 2.139(19) . ?
Nb5 I13 2.817(4) . ?
Nb5 I17 2.838(3) . ?
Nb5 I18 2.829(4) . ?
Nb5 I13A 2.44(9) . ?
Nb5 I17A 2.64(6) 4_655 ?
Nb5 I18A 2.64(6) 4_655 ?
Nb6 Nb6 3.039(5) 4_655 ?
Nb6 O2 2.006(18) . ?
Nb6 I13 2.835(3) . ?
Nb6 I15 2.813(3) . ?
Nb6 I16 2.833(3) . ?
Nb6 I15A 2.65(5) . ?
Nb6 I15A 2.26(5) 4_655 ?
Nb6 I16A 3.12(4) . ?
Nb6 I13A 2.61(8) . ?
I15A I15A 0.63(10) 4_655 ?
I21 Nb7 2.809(6) . ?
I21 Nb8 2.831(5) . ?
I22 Nb7 2.838(5) . ?
I22 Nb8 2.808(6) . ?
I23 Nb8 2.789(5) . ?
I23 Nb8 2.789(5) 4 ?
I24 Nb8 2.844(6) . ?
I24 Nb8 2.844(6) 4 ?
I25 Nb7 2.859(6) . ?
I25 Nb7 2.859(6) 4 ?
I26 Nb7 2.742(5) . ?
I27 Nb8 2.734(5) . ?
I28 Nb7 2.818(5) 4 ?
I28 Nb7 2.818(5) . ?
Nb7 Nb7 3.029(7) 4 ?
Nb7 Nb8 2.806(5) . ?
Nb7 O3 2.14(3) . ?
Nb8 Nb8 3.047(6) 4 ?
Nb8 O3 2.00(3) . ?
I21A Nb7A 2.778(12) . ?
I21A Nb8A 2.799(13) . ?
I22A Nb7A 2.849(12) . ?
I22A Nb8A 2.827(12) . ?
I23A Nb8A 2.741(12) 4 ?
I23A Nb8A 2.741(12) . ?
I24A Nb8A 2.900(15) . ?
I24A Nb8A 2.900(15) 4 ?
I25A Nb7A 2.885(13) . ?
I25A Nb7A 2.885(13) 4 ?
I26A Nb7A 2.784(14) . ?
I27A Nb8A 2.723(12) . ?
I28A Nb7A 2.811(14) . ?
I28A Nb7A 2.811(14) 4 ?
Nb7A Nb7A 3.00(2) 4 ?
Nb7A Nb8A 2.754(13) . ?
Nb7A O3A 2.10(6) . ?
Nb8A Nb8A 3.034(19) 4 ?
Nb8A O3A 1.99(6) . ?
I17A I17A 1.36(14) 4_655 ?
I18A I18A 1.39(13) 4_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Nb1 I1 Nb2 65.54(8) . . ?
Nb2 I2 Nb1 65.21(8) . . ?
Nb3 I3 Nb2 59.38(7) . . ?
Nb2 I4 Nb3 59.72(8) . . ?
Nb3 I5 Nb4 64.77(8) . . ?
Nb3 I6 Nb4 65.27(9) . . ?
Nb4 I7 Nb1 59.37(7) . . ?
Nb1 I8 Nb4 59.49(8) . . ?
I1 Nb1 I2 88.22(9) . . ?
I1 Nb1 I7 90.08(9) . . ?
I1 Nb1 Nb2 57.29(7) . . ?
I2 Nb1 Nb2 57.22(7) . . ?
I7 Nb1 I2 175.81(10) . . ?
I7 Nb1 Nb2 118.73(9) . . ?
I8 Nb1 I1 176.72(11) . . ?
I8 Nb1 I2 89.44(9) . . ?
I8 Nb1 I7 92.11(9) . . ?
I8 Nb1 Nb2 119.45(9) . . ?
I9 Nb1 I1 89.34(9) . . ?
I9 Nb1 I2 90.30(9) . . ?
I9 Nb1 I7 93.50(10) . . ?
I9 Nb1 I8 92.96(9) . . ?
I9 Nb1 Nb2 130.87(10) . . ?
I9 Nb1 Nb4 139.20(11) . . ?
Nb4 Nb1 I1 118.51(9) . . ?
Nb4 Nb1 I2 117.75(9) . . ?
Nb4 Nb1 I7 59.93(8) . . ?
Nb4 Nb1 I8 60.77(7) . . ?
Nb4 Nb1 Nb2 89.93(9) . . ?
O1 Nb1 I1 83.2(7) . . ?
O1 Nb1 I2 84.9(7) . . ?
O1 Nb1 I7 91.1(7) . . ?
O1 Nb1 I8 94.3(7) . . ?
O1 Nb1 I9 171.3(7) . . ?
O1 Nb1 Nb2 40.6(7) . . ?
O1 Nb1 Nb4 49.4(7) . . ?
I1 Nb2 I2 88.36(9) . . ?
I1 Nb2 I3 90.27(9) . . ?
I1 Nb2 Nb1 57.17(7) . . ?
I2 Nb2 I3 176.37(10) . . ?
I2 Nb2 Nb1 57.57(7) . . ?
I3 Nb2 Nb1 118.95(9) . . ?
I4 Nb2 I1 176.18(11) . . ?
I4 Nb2 I2 88.91(9) . . ?
I4 Nb2 I3 92.30(9) . . ?
I4 Nb2 Nb1 119.04(8) . . ?
I4 Nb2 Nb3 60.65(7) . . ?
I10 Nb2 I1 88.85(9) . . ?
I10 Nb2 I2 90.77(9) . . ?
I10 Nb2 I3 92.56(9) . . ?
I10 Nb2 I4 93.86(9) . . ?
I10 Nb2 Nb1 130.95(10) . . ?
I10 Nb2 Nb3 139.10(12) . . ?
Nb3 Nb2 I1 118.53(9) . . ?
Nb3 Nb2 I2 117.81(9) . . ?
Nb3 Nb2 I3 60.09(8) . . ?
Nb3 Nb2 Nb1 89.93(9) . . ?
O1 Nb2 I1 83.2(7) . . ?
O1 Nb2 I2 85.3(7) . . ?
O1 Nb2 I3 91.2(7) . . ?
O1 Nb2 I4 93.9(7) . . ?
O1 Nb2 I10 171.2(7) . . ?
O1 Nb2 Nb1 40.7(6) . . ?
O1 Nb2 Nb3 49.3(6) . . ?
I3 Nb3 I4 91.95(9) . . ?
I3 Nb3 I5 88.82(9) . . ?
I3 Nb3 Nb4 119.02(9) . . ?
I4 Nb3 I5 176.07(10) . . ?
I4 Nb3 Nb4 118.77(9) . . ?
I5 Nb3 Nb4 57.64(7) . . ?
I6 Nb3 I3 176.58(11) . . ?
I6 Nb3 I4 90.48(9) . . ?
I6 Nb3 I5 88.59(9) . . ?
I6 Nb3 Nb4 57.62(7) . . ?
I11 Nb3 I3 93.36(10) . . ?
I11 Nb3 I4 92.32(9) . . ?
I11 Nb3 I5 91.48(9) . . ?
I11 Nb3 I6 88.94(10) . . ?
I11 Nb3 Nb2 138.21(12) . . ?
I11 Nb3 Nb4 131.85(10) . . ?
Nb2 Nb3 I3 60.53(7) . . ?
Nb2 Nb3 I4 59.63(8) . . ?
Nb2 Nb3 I5 117.67(10) . . ?
Nb2 Nb3 I6 118.95(9) . . ?
Nb2 Nb3 Nb4 89.92(9) . . ?
O1 Nb3 I3 89.1(7) . . ?
O1 Nb3 I4 90.5(6) . . ?
O1 Nb3 I5 85.7(6) . . ?
O1 Nb3 I6 88.5(7) . . ?
O1 Nb3 I11 176.2(6) . . ?
O1 Nb3 Nb2 45.6(6) . . ?
O1 Nb3 Nb4 44.3(6) . . ?
I5 Nb4 Nb3 57.59(7) . . ?
I6 Nb4 I5 88.24(9) . . ?
I6 Nb4 Nb3 57.10(7) . . ?
I7 Nb4 I5 88.79(9) . . ?
I7 Nb4 I6 176.20(11) . . ?
I7 Nb4 I8 91.94(9) . . ?
I7 Nb4 Nb3 119.20(9) . . ?
I8 Nb4 I5 176.53(11) . . ?
I8 Nb4 I6 90.88(9) . . ?
I8 Nb4 Nb3 119.23(9) . . ?
I12 Nb4 I5 91.75(10) . . ?
I12 Nb4 I6 87.97(10) . . ?
I12 Nb4 I7 94.49(10) . . ?
I12 Nb4 I8 91.58(10) . . ?
I12 Nb4 Nb1 138.67(12) . . ?
I12 Nb4 Nb3 131.00(10) . . ?
Nb1 Nb4 I5 117.91(9) . . ?
Nb1 Nb4 I6 118.89(10) . . ?
Nb1 Nb4 I7 60.69(7) . . ?
Nb1 Nb4 I8 59.74(8) . . ?
Nb1 Nb4 Nb3 90.23(9) . . ?
O1 Nb4 I5 85.7(6) . . ?
O1 Nb4 I6 88.1(7) . . ?
O1 Nb4 I7 89.3(7) . . ?
O1 Nb4 I8 90.9(6) . . ?
O1 Nb4 I12 175.4(6) . . ?
O1 Nb4 Nb1 45.8(6) . . ?
O1 Nb4 Nb3 44.4(6) . . ?
Nb1 O1 Nb3 175.0(14) . . ?
Nb1 O1 Nb4 84.8(8) . . ?
Nb2 O1 Nb1 98.7(10) . . ?
Nb2 O1 Nb3 85.1(8) . . ?
Nb2 O1 Nb4 175.3(14) . . ?
Nb4 O1 Nb3 91.2(9) . . ?
Nb6 I14 Nb5 59.80(8) . . ?
I14 Nb5 Nb5 119.46(7) . 4_655 ?
I14 Nb5 I17 176.74(11) . . ?
I14 Nb5 I18 90.85(10) . . ?
I19 Nb5 I14 91.54(10) . . ?
I19 Nb5 Nb5 131.53(7) . 4_655 ?
I19 Nb5 Nb6 138.52(13) . . ?
I19 Nb5 I13 94.22(11) . . ?
I19 Nb5 I17 91.56(9) . . ?
I19 Nb5 I18 88.59(10) . . ?
Nb6 Nb5 I14 59.82(8) . . ?
Nb6 Nb5 Nb5 89.89(8) . 4_655 ?
Nb6 Nb5 I13 60.54(8) . . ?
Nb6 Nb5 I17 118.03(11) . . ?
Nb6 Nb5 I18 118.59(10) . . ?
O2 Nb5 I14 91.0(8) . . ?
O2 Nb5 I19 176.1(5) . . ?
O2 Nb5 Nb5 44.5(5) . 4_655 ?
O2 Nb5 Nb6 45.4(5) . . ?
O2 Nb5 I13 88.7(8) . . ?
O2 Nb5 I17 85.9(7) . . ?
O2 Nb5 I18 88.3(8) . . ?
O2 Nb5 I13A 82(2) . . ?
O2 Nb5 I17A 95.8(16) . 4_655 ?
O2 Nb5 I18A 99.4(16) . 4_655 ?
I13 Nb5 I14 91.71(10) . . ?
I13 Nb5 I17 89.06(11) . . ?
I13 Nb5 I18 176.15(12) . . ?
I18 Nb5 I17 88.23(10) . . ?
I13A Nb5 I14 97.6(19) . . ?
I13A Nb5 I19 100.5(19) . . ?
I13A Nb5 Nb6 59.2(19) . . ?
I13A Nb5 I18A 178(2) . 4_655 ?
I17A Nb5 I14 168.8(15) 4_655 . ?
I17A Nb5 I19 82.2(14) 4_655 . ?
I17A Nb5 Nb6 120.1(14) 4_655 . ?
I18A Nb5 I14 81.8(13) 4_655 . ?
I18A Nb5 I19 77.9(13) 4_655 . ?
I18A Nb5 Nb6 121.5(11) 4_655 . ?
I14 Nb6 Nb6 119.77(7) . 4_655 ?
I14 Nb6 I13 91.67(9) . . ?
I14 Nb6 I15 177.08(12) . . ?
I14 Nb6 I16 89.13(10) . . ?
I14 Nb6 I16A 73.3(7) . . ?
I20 Nb6 I14 92.77(10) . . ?
I20 Nb6 Nb5 139.04(13) . . ?
I20 Nb6 Nb6 130.86(7) . 4_655 ?
I20 Nb6 I13 93.70(10) . . ?
I20 Nb6 I15 89.50(10) . . ?
I20 Nb6 I16 90.29(9) . . ?
I20 Nb6 I16A 101.1(6) . . ?
Nb5 Nb6 I14 60.38(7) . . ?
Nb5 Nb6 Nb6 90.11(8) . 4_655 ?
Nb5 Nb6 I13 59.90(9) . . ?
Nb5 Nb6 I15 118.68(10) . . ?
Nb5 Nb6 I16 117.27(11) . . ?
Nb5 Nb6 I16A 99.7(9) . . ?
Nb6 Nb6 I16A 60.8(4) 4_655 . ?
O2 Nb6 I14 94.3(9) . . ?
O2 Nb6 I20 171.4(6) . . ?
O2 Nb6 Nb5 49.4(6) . . ?
O2 Nb6 Nb6 40.8(6) . 4_655 ?
O2 Nb6 I13 90.9(8) . . ?
O2 Nb6 I15 83.3(8) . . ?
O2 Nb6 I16 85.0(8) . . ?
O2 Nb6 I15A 90.5(15) . 4_655 ?
O2 Nb6 I15A 80.2(12) . . ?
O2 Nb6 I16A 76.4(11) . . ?
O2 Nb6 I13A 81(2) . . ?
I15 Nb6 I13 90.03(10) . . ?
I15 Nb6 I16 89.00(10) . . ?
I16 Nb6 I13 175.89(11) . . ?
I15A Nb6 I14 165.8(15) 4_655 . ?
I15A Nb6 I14 160.9(14) . . ?
I15A Nb6 I20 81.4(13) 4_655 . ?
I15A Nb6 I20 91.6(10) . . ?
I15A Nb6 Nb5 131.2(14) 4_655 . ?
I15A Nb6 Nb5 124.3(9) . . ?
I15A Nb6 I15A 11.5(18) 4_655 . ?
I15A Nb6 I16A 87.6(16) . . ?
I15A Nb6 I16A 95.0(15) 4_655 . ?
I13A Nb6 I14 94.1(19) . . ?
I13A Nb6 I20 103.8(18) . . ?
I13A Nb6 Nb5 53.4(19) . . ?
Nb5 O2 Nb5 90.9(10) 4_655 . ?
Nb6 O2 Nb5 85.20(13) . . ?
Nb6 O2 Nb5 175.0(16) 4_655 . ?
Nb6 O2 Nb5 175.0(16) . 4_655 ?
Nb6 O2 Nb5 85.20(13) 4_655 4_655 ?
Nb6 O2 Nb6 98.5(12) 4_655 . ?
Nb5 I13 Nb6 59.56(8) . . ?
Nb6 I15 Nb6 65.38(12) . 4_655 ?
Nb6 I16 Nb6 64.86(11) 4_655 . ?
Nb5 I17 Nb5 64.98(12) 4_655 . ?
Nb5 I18 Nb5 65.22(12) 4_655 . ?
Nb6 I15A Nb6 75.9(15) 4_655 . ?
I15A I15A Nb6 46.3(12) 4_655 . ?
Nb6 I16A Nb6 58.4(8) 4_655 . ?
Nb5 I13A Nb6 67(2) . . ?
Nb7 I21 Nb8 59.69(13) . . ?
Nb8 I22 Nb7 59.61(13) . . ?
Nb8 I23 Nb8 66.22(17) 4 . ?
Nb8 I24 Nb8 64.78(16) 4 . ?
Nb7 I25 Nb7 63.96(17) 4 . ?
Nb7 I28 Nb7 65.03(17) 4 . ?
I21 Nb7 I22 91.59(15) . . ?
I21 Nb7 I25 177.89(16) . . ?
I21 Nb7 I28 89.94(17) . . ?
I21 Nb7 Nb7 119.88(9) . 4 ?
I22 Nb7 I25 89.79(17) . . ?
I22 Nb7 Nb7 118.70(9) . 4 ?
I25 Nb7 Nb7 58.02(8) . 4 ?
I26 Nb7 I21 92.82(16) . . ?
I26 Nb7 I22 93.18(15) . . ?
I26 Nb7 I25 88.70(18) . . ?
I26 Nb7 I28 90.34(15) . . ?
I26 Nb7 Nb7 131.13(12) . 4 ?
I26 Nb7 Nb8 138.68(17) . . ?
I28 Nb7 I22 176.08(15) . . ?
I28 Nb7 I25 88.58(15) . . ?
I28 Nb7 Nb7 57.49(9) . 4 ?
Nb8 Nb7 I21 60.54(13) . . ?
Nb8 Nb7 I22 59.66(13) . . ?
Nb8 Nb7 I25 118.98(17) . . ?
Nb8 Nb7 I28 118.25(18) . . ?
Nb8 Nb7 Nb7 90.19(9) . 4 ?
O3 Nb7 I21 88.9(9) . . ?
O3 Nb7 I22 90.6(9) . . ?
O3 Nb7 I25 89.5(9) . . ?
O3 Nb7 I26 175.8(8) . . ?
O3 Nb7 I28 85.8(9) . . ?
O3 Nb7 Nb7 45.0(7) . 4 ?
O3 Nb7 Nb8 45.3(7) . . ?
I21 Nb8 I24 176.36(16) . . ?
I21 Nb8 Nb8 119.41(9) . 4 ?
I22 Nb8 I21 91.76(14) . . ?
I22 Nb8 I24 88.27(18) . . ?
I22 Nb8 Nb8 118.82(10) . 4 ?
I23 Nb8 I21 90.92(17) . . ?
I23 Nb8 I22 175.70(17) . . ?
I23 Nb8 I24 88.84(16) . . ?
I23 Nb8 Nb7 118.08(16) . . ?
I23 Nb8 Nb8 56.89(9) . 4 ?
I24 Nb8 Nb8 57.61(8) . 4 ?
I27 Nb8 I21 92.11(16) . . ?
I27 Nb8 I22 94.33(15) . . ?
I27 Nb8 I23 88.93(17) . . ?
I27 Nb8 I24 91.51(16) . . ?
I27 Nb8 Nb7 139.11(17) . . ?
I27 Nb8 Nb8 131.02(11) . 4 ?
Nb7 Nb8 I21 59.77(14) . . ?
Nb7 Nb8 I22 60.73(12) . . ?
Nb7 Nb8 I24 117.27(18) . . ?
Nb7 Nb8 Nb8 89.81(9) . 4 ?
O3 Nb8 I21 91.1(10) . . ?
O3 Nb8 I22 94.5(10) . . ?
O3 Nb8 I23 82.1(10) . . ?
O3 Nb8 I24 85.3(10) . . ?
O3 Nb8 I27 170.5(9) . . ?
O3 Nb8 Nb7 49.5(9) . . ?
O3 Nb8 Nb8 40.4(9) . 4 ?
Nb7 O3 Nb7 90.1(15) . 4 ?
Nb8 O3 Nb7 173.7(18) . 4 ?
Nb8 O3 Nb7 85.2(2) 4 4 ?
Nb8 O3 Nb7 173.7(18) 4 . ?
Nb8 O3 Nb7 85.2(2) . . ?
Nb8 O3 Nb8 99.2(17) 4 . ?
Nb7A I21A Nb8A 59.2(3) . . ?
Nb8A I22A Nb7A 58.0(3) . . ?
Nb8A I23A Nb8A 67.2(4) 4 . ?
Nb8A I24A Nb8A 63.1(5) 4 . ?
Nb7A I25A Nb7A 62.6(4) 4 . ?
Nb7A I28A Nb7A 64.4(5) 4 . ?
I21A Nb7A I22A 92.6(4) . . ?
I21A Nb7A I25A 178.6(5) . . ?
I21A Nb7A I26A 93.1(4) . . ?
I21A Nb7A I28A 91.4(4) . . ?
I22A Nb7A I25A 88.4(3) . . ?
I26A Nb7A I22A 90.0(4) . . ?
I26A Nb7A I25A 87.8(4) . . ?
I26A Nb7A I28A 91.0(4) . . ?
I28A Nb7A I22A 175.8(4) . . ?
I28A Nb7A I25A 87.5(4) . . ?
Nb8A Nb7A I21A 60.8(3) . . ?
Nb8A Nb7A I22A 60.6(3) . . ?
Nb8A Nb7A I25A 119.1(4) . . ?
Nb8A Nb7A I26A 137.1(5) . . ?
Nb8A Nb7A I28A 120.7(4) . . ?
O3A Nb7A I21A 90(2) . . ?
O3A Nb7A I22A 91(2) . . ?
O3A Nb7A I25A 89(2) . . ?
O3A Nb7A I26A 176.6(19) . . ?
O3A Nb7A I28A 88(2) . . ?
O3A Nb7A Nb8A 45.9(17) . . ?
I21A Nb8A I22A 92.7(4) . . ?
I21A Nb8A I24A 176.8(4) . . ?
I22A Nb8A I24A 86.9(4) . . ?
I23A Nb8A I21A 92.2(4) . . ?
I23A Nb8A I22A 174.4(5) . . ?
I23A Nb8A I24A 88.0(4) . . ?
I23A Nb8A Nb7A 119.2(4) . . ?
I27A Nb8A I21A 92.8(4) . . ?
I27A Nb8A I22A 93.1(4) . . ?
I27A Nb8A I23A 89.3(4) . . ?
I27A Nb8A I24A 90.3(4) . . ?
I27A Nb8A Nb7A 139.2(5) . . ?
Nb7A Nb8A I21A 60.0(3) . . ?
Nb7A Nb8A I22A 61.4(3) . . ?
Nb7A Nb8A I24A 117.2(4) . . ?
O3A Nb8A I21A 92(2) . . ?
O3A Nb8A I22A 94(2) . . ?
O3A Nb8A I23A 83(2) . . ?
O3A Nb8A I24A 85(2) . . ?
O3A Nb8A I27A 171(2) . . ?
O3A Nb8A Nb7A 49.4(19) . . ?
Nb7A O3A Nb7A 91(3) 4 . ?
Nb8A O3A Nb7A 84.7(5) . . ?
Nb8A O3A Nb7A 175(4) 4 . ?
Nb8A O3A Nb8A 100(4) 4 . ?

_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
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.49(9)
2 0.51(9)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nb4oi11v5_twin
_database_code_depnum_ccdc_archive 'CCDC 2408695'
loop_
_audit_author_name
_audit_author_address
'Patrick Schmidt'
;University of Tuebingen
Germany
;
_audit_update_record             
;
2024-12-08 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_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)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I22 Nb8 O2'
_chemical_formula_sum            'I22 Nb8 O2'
_chemical_formula_weight         3567.08
_chemical_melting_point          ?
_chemical_oxdiff_formula         'O2 Nb8 I22 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1217(2)
_cell_length_b                   13.9844(3)
_cell_length_c                   16.3913(3)
_cell_angle_alpha                88.968(2)
_cell_angle_beta                 89.093(2)
_cell_angle_gamma                85.329(2)
_cell_volume                     2311.80(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13492
_cell_measurement_temperature    150.01(18)
_cell_measurement_theta_max      38.3710
_cell_measurement_theta_min      3.5930
_shelx_estimated_absorpt_T_max   0.491
_shelx_estimated_absorpt_T_min   0.389
_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_absorpt_special_details   ?
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.124
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3020
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 -1 0.0219
0 -2 -1 0.0166
-1 1 -2 0.0243
0 2 -1 0.0203
0 -1 -1 0.0192
1 2 2 0.0208
0 -2 1 0.0208
0 -1 -2 0.0255
-2 0 1 0.0339
2 0 -1 0.0370
1 0 2 0.0300
-1 -2 0 0.0167
0 1 1 0.0271
-1 -2 -2 0.0229

_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.041
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.0003 -0.0004 -1.0905 -0.0887 -0.0597 0.1020
-0.0003 -2.0003 -1.0770 0.0191 -0.1037 -0.0356
-1.0005 0.9993 -2.0062 -0.1211 -0.0138 0.0277
-0.0002 1.9996 -0.9225 -0.0863 0.0679 -0.0055
-0.0003 -1.0003 -1.0383 -0.0073 -0.0608 -0.0281
1.0005 2.0006 2.1221 0.0421 0.1425 -0.0051
0.0002 -1.9996 0.9225 0.0863 -0.0679 0.0055
-0.0005 -1.0006 -2.0381 -0.0409 -0.0787 -0.0486
-1.9998 0.0002 0.9090 -0.0214 -0.0239 0.1430
1.9998 -0.0002 -0.9090 0.0214 0.0239 -0.1430
1.0005 0.0007 2.0448 0.0948 0.0567 -0.0202
-1.0000 -2.0000 -0.1226 0.0252 -0.1067 0.0462
0.0003 1.0003 1.0383 0.0073 0.0608 0.0281
-1.0004 -1.7693 -1.5909 -0.0306 -0.1232 0.0176

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  21.00   0.50   20.00    --  -21.41  84.00 -91.00  130
  2  ω    -42.00  46.00   0.50   20.00    --   23.60 -84.00 147.00  176
  3  ω    -93.00  -2.00   0.50   20.00    --  -21.41 -77.00  90.00  182
  4  ω    -27.00  50.00   0.50   20.00    --  -21.41  37.00 -90.00  154
  5  ω    -93.00  -2.00   0.50   20.00    --  -21.41 -77.00 -90.00  182
  6  ω    -93.00 -10.00   0.50   20.00    --  -21.41 -57.00   0.00  166
  7  ω    -93.00 -10.00   0.50   20.00    --  -21.41 -57.00 150.00  166
  8  ω    -93.00  -2.00   0.50   20.00    --  -21.41 -77.00 -30.00  182
  9  ω    -48.00   5.00   0.50   20.00    --   23.60 -19.00-150.00  106
 10  ω    -48.00   5.00   0.50   20.00    --   23.60 -19.00  30.00  106
 11  ω     39.00  95.00   0.50   20.00    --   23.60-178.00  60.00  112
 12  ω      4.00  95.00   0.50   20.00    --   23.60  77.00-120.00  182
 13  ω    -93.00 -10.00   0.50   20.00    --  -21.41 -57.00 120.00  166
 14  ω    -48.00   5.00   0.50   20.00    --   23.60 -19.00 -60.00  106
 15  ω    -23.00  53.00   0.50   20.00    --   23.60 -99.00 120.00  152
 16  ω    -23.00  53.00   0.50   20.00    --   23.60 -99.00-120.00  152
 17  ω    -23.00  53.00   0.50   20.00    --   23.60 -99.00 -60.00  152
 18  ω    -23.00  53.00   0.50   20.00    --   23.60 -99.00  60.00  152
 19  ω    -23.00  53.00   0.50   20.00    --   23.60 -99.00  30.00  152
 20  ω    -23.00  53.00   0.50   20.00    --   23.60 -99.00-150.00  152
 21  ω    -23.00  25.00   0.50   20.00    --   23.60 -99.00 -30.00   96
 22  ω     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       'ω 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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16216
_reflns_number_total             17704
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0185
_refine_ls_restrained_S_all      1.037
_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/[σ²(Fo²)+(0.0301P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0590
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.4924(4)
 0.5076(4)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.46307(4) 0.90743(3) 0.87750(3) 0.01526(9) Uani 1 1 d . . . . .
I2 I 0.67731(4) 0.63744(3) 0.87175(3) 0.01391(8) Uani 1 1 d . . . . .
I3 I 0.47664(4) 0.91177(3) 0.63459(3) 0.01421(9) Uani 1 1 d . . . . .
I4 I 0.67372(4) 0.65854(3) 0.62756(3) 0.01426(9) Uani 1 1 d . . . . .
I5 I 0.13519(4) 0.79761(3) 0.62647(3) 0.01485(9) Uani 1 1 d . . . . .
I6 I 0.34035(4) 0.52733(3) 0.61638(3) 0.01854(9) Uani 1 1 d . . . . .
I7 I 0.13696(4) 0.77318(3) 0.87034(3) 0.01445(9) Uani 1 1 d . . . . .
I8 I 0.33009(4) 0.52249(3) 0.86448(3) 0.01668(9) Uani 1 1 d . . . . .
I9 I 0.81443(4) 0.86639(3) 0.76206(3) 0.01890(10) Uani 1 1 d . . . . .
I10 I 0.43361(4) 0.72740(3) 0.45056(3) 0.01619(9) Uani 1 1 d . . . . .
I11 I -0.00392(4) 0.56786(3) 0.73489(3) 0.02046(10) Uani 1 1 d . . . . .
I12 I 0.43026(4) 0.69689(3) 1.04648(3) 0.01646(9) Uani 1 1 d . . . . .
I13 I 0.39547(4) 0.86278(3) 0.24110(3) 0.01421(9) Uani 1 1 d . . . . .
I14 I 0.32274(4) 0.59310(3) 0.25703(3) 0.01383(8) Uani 1 1 d . . . . .
I15 I 0.13307(4) 0.91830(3) 0.07156(3) 0.01572(9) Uani 1 1 d . . . . .
I16 I 0.05047(4) 0.62680(3) 0.08369(3) 0.01699(9) Uani 1 1 d . . . . .
I17 I -0.14677(4) 0.96613(3) 0.24189(3) 0.01608(9) Uani 1 1 d . . . . .
I18 I -0.22376(4) 0.70304(3) 0.25562(3) 0.01607(9) Uani 1 1 d . . . . .
I19 I 0.12862(4) 0.93343(3) 0.41247(3) 0.01528(9) Uani 1 1 d . . . . .
I20 I 0.05045(4) 0.64287(3) 0.42895(3) 0.01683(9) Uani 1 1 d . . . . .
I21 I -0.23256(5) 0.84102(3) 0.03437(3) 0.02329(10) Uani 1 1 d . . . . .
I22 I -0.23502(4) 0.86004(3) 0.46207(3) 0.02135(10) Uani 1 1 d . . . . .
Nb1 Nb 0.41095(5) 0.71329(4) 0.87066(3) 0.01105(11) Uani 1 1 d . . . . .
Nb2 Nb 0.58359(5) 0.78205(4) 0.75808(4) 0.01138(11) Uani 1 1 d . . . . .
Nb3 Nb 0.39834(5) 0.72066(4) 0.62599(3) 0.01135(11) Uani 1 1 d . . . . .
Nb4 Nb 0.22749(5) 0.65220(4) 0.73944(3) 0.01160(11) Uani 1 1 d . . . . .
Nb5 Nb 0.21651(5) 0.75941(4) 0.33774(3) 0.01044(11) Uani 1 1 d . . . . .
Nb6 Nb 0.21732(5) 0.75033(4) 0.16009(3) 0.01030(11) Uani 1 1 d . . . . .
Nb7 Nb -0.04793(5) 0.80271(4) 0.15143(3) 0.01160(11) Uani 1 1 d . . . . .
Nb8 Nb -0.04904(5) 0.81147(4) 0.34609(3) 0.01179(11) Uani 1 1 d . . . . .
O1 O 0.4058(5) 0.7142(3) 0.7481(4) 0.0289(12) Uani 1 1 d . . . . .
O2 O 0.0789(4) 0.7822(3) 0.2476(3) 0.0250(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Nb1 2.8121(7) . ?
I1 Nb2 2.8449(7) . ?
I2 Nb1 2.8159(7) . ?
I2 Nb2 2.8406(7) . ?
I3 Nb2 2.8596(7) . ?
I3 Nb3 2.8554(7) . ?
I4 Nb2 2.8648(7) . ?
I4 Nb3 2.8515(7) . ?
I5 Nb3 2.7903(7) . ?
I5 Nb4 2.8366(7) . ?
I6 Nb3 2.8205(7) . ?
I6 Nb4 2.8552(7) . ?
I7 Nb1 2.8309(7) . ?
I7 Nb4 2.8499(7) . ?
I8 Nb1 2.8579(7) . ?
I8 Nb4 2.8630(7) . ?
I9 Nb2 2.7039(6) . ?
I10 Nb3 2.8928(7) . ?
I10 Nb5 2.8961(7) . ?
I11 Nb4 2.7096(6) . ?
I12 Nb1 2.8954(7) . ?
I12 Nb6 2.8865(7) 1_556 ?
I13 Nb5 2.8519(6) . ?
I13 Nb6 2.8461(6) . ?
I14 Nb5 2.8238(7) . ?
I14 Nb6 2.8360(7) . ?
I15 Nb6 2.8180(7) . ?
I15 Nb7 2.8308(7) . ?
I16 Nb6 2.8327(7) . ?
I16 Nb7 2.8178(7) . ?
I17 Nb7 2.8505(7) . ?
I17 Nb8 2.8540(7) . ?
I18 Nb7 2.8721(7) . ?
I18 Nb8 2.8681(7) . ?
I19 Nb5 2.8169(7) . ?
I19 Nb8 2.8206(7) . ?
I20 Nb5 2.8275(6) . ?
I20 Nb8 2.8212(7) . ?
I21 Nb7 2.7156(7) . ?
I22 Nb8 2.7101(7) . ?
Nb1 Nb2 2.7369(8) . ?
Nb1 Nb4 3.0423(8) . ?
Nb1 O1 2.010(6) . ?
Nb2 Nb3 3.0656(8) . ?
Nb2 O1 2.111(5) . ?
Nb3 Nb4 2.7329(8) . ?
Nb3 O1 2.004(6) . ?
Nb4 O1 2.073(5) . ?
Nb5 Nb6 2.9168(7) . ?
Nb5 Nb8 2.7288(8) . ?
Nb5 O2 2.050(5) . ?
Nb6 Nb7 2.7299(8) . ?
Nb6 O2 2.018(5) . ?
Nb7 Nb8 3.1950(8) . ?
Nb7 O2 2.050(5) . ?
Nb8 O2 2.080(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Nb1 I1 Nb2 57.866(17) . . ?
Nb1 I2 Nb2 57.874(17) . . ?
Nb3 I3 Nb2 64.880(17) . . ?
Nb3 I4 Nb2 64.863(17) . . ?
Nb3 I5 Nb4 58.107(18) . . ?
Nb3 I6 Nb4 57.564(18) . . ?
Nb1 I7 Nb4 64.759(18) . . ?
Nb1 I8 Nb4 64.252(18) . . ?
Nb3 I10 Nb5 123.59(2) . . ?
Nb6 I12 Nb1 124.76(2) 1_556 . ?
Nb6 I13 Nb5 61.581(17) . . ?
Nb5 I14 Nb6 62.042(17) . . ?
Nb6 I15 Nb7 57.799(17) . . ?
Nb7 I16 Nb6 57.779(17) . . ?
Nb7 I17 Nb8 68.125(18) . . ?
Nb8 I18 Nb7 67.643(17) . . ?
Nb5 I19 Nb8 57.900(17) . . ?
Nb8 I20 Nb5 57.774(17) . . ?
I1 Nb1 I2 96.54(2) . . ?
I1 Nb1 I7 88.35(2) . . ?
I1 Nb1 I8 174.19(3) . . ?
I1 Nb1 I12 89.99(2) . . ?
I1 Nb1 Nb4 118.75(2) . . ?
I2 Nb1 I7 175.09(2) . . ?
I2 Nb1 I8 89.26(2) . . ?
I2 Nb1 I12 84.211(19) . . ?
I2 Nb1 Nb4 119.49(2) . . ?
I7 Nb1 I8 85.850(19) . . ?
I7 Nb1 I12 95.37(2) . . ?
I7 Nb1 Nb4 57.923(17) . . ?
I8 Nb1 I12 90.30(2) . . ?
I8 Nb1 Nb4 57.954(17) . . ?
I12 Nb1 Nb4 137.28(2) . . ?
Nb2 Nb1 I1 61.669(18) . . ?
Nb2 Nb1 I2 61.516(18) . . ?
Nb2 Nb1 I7 121.74(2) . . ?
Nb2 Nb1 I8 122.00(3) . . ?
Nb2 Nb1 I12 129.90(2) . . ?
Nb2 Nb1 Nb4 92.60(2) . . ?
O1 Nb1 I1 93.48(14) . . ?
O1 Nb1 I2 92.33(14) . . ?
O1 Nb1 I7 87.82(14) . . ?
O1 Nb1 I8 86.57(14) . . ?
O1 Nb1 I12 175.36(14) . . ?
O1 Nb1 Nb2 49.99(13) . . ?
O1 Nb1 Nb4 42.63(13) . . ?
I1 Nb2 I3 88.521(19) . . ?
I1 Nb2 I4 172.81(2) . . ?
I1 Nb2 Nb3 115.49(2) . . ?
I2 Nb2 I1 95.24(2) . . ?
I2 Nb2 I3 173.86(2) . . ?
I2 Nb2 I4 89.273(19) . . ?
I2 Nb2 Nb3 116.40(2) . . ?
I3 Nb2 I4 86.52(2) . . ?
I3 Nb2 Nb3 57.492(17) . . ?
I4 Nb2 Nb3 57.360(17) . . ?
I9 Nb2 I1 92.41(2) . . ?
I9 Nb2 I2 91.74(2) . . ?
I9 Nb2 I3 92.94(2) . . ?
I9 Nb2 I4 93.05(2) . . ?
I9 Nb2 Nb1 136.22(3) . . ?
I9 Nb2 Nb3 136.44(3) . . ?
Nb1 Nb2 I1 60.465(18) . . ?
Nb1 Nb2 I2 60.610(18) . . ?
Nb1 Nb2 I3 117.73(2) . . ?
Nb1 Nb2 I4 117.67(2) . . ?
Nb1 Nb2 Nb3 87.34(2) . . ?
O1 Nb2 I1 90.40(15) . . ?
O1 Nb2 I2 89.54(14) . . ?
O1 Nb2 I3 85.58(14) . . ?
O1 Nb2 I4 84.03(15) . . ?
O1 Nb2 I9 176.79(16) . . ?
O1 Nb2 Nb1 46.82(16) . . ?
O1 Nb2 Nb3 40.54(16) . . ?
I3 Nb3 I10 89.722(19) . . ?
I3 Nb3 Nb2 57.627(16) . . ?
I4 Nb3 I3 86.852(18) . . ?
I4 Nb3 I10 84.761(19) . . ?
I4 Nb3 Nb2 57.777(17) . . ?
I5 Nb3 I3 88.18(2) . . ?
I5 Nb3 I4 175.01(2) . . ?
I5 Nb3 I6 95.90(2) . . ?
I5 Nb3 I10 95.66(2) . . ?
I5 Nb3 Nb2 118.82(2) . . ?
I6 Nb3 I3 175.90(3) . . ?
I6 Nb3 I4 89.07(2) . . ?
I6 Nb3 I10 89.50(2) . . ?
I6 Nb3 Nb2 120.20(2) . . ?
I10 Nb3 Nb2 128.74(2) . . ?
Nb4 Nb3 I3 120.83(2) . . ?
Nb4 Nb3 I4 120.74(2) . . ?
Nb4 Nb3 I5 61.796(19) . . ?
Nb4 Nb3 I6 61.854(19) . . ?
Nb4 Nb3 I10 138.86(2) . . ?
Nb4 Nb3 Nb2 92.17(2) . . ?
O1 Nb3 I3 87.66(14) . . ?
O1 Nb3 I4 86.27(14) . . ?
O1 Nb3 I5 93.09(14) . . ?
O1 Nb3 I6 92.48(14) . . ?
O1 Nb3 I10 170.78(14) . . ?
O1 Nb3 Nb2 43.20(13) . . ?
O1 Nb3 Nb4 48.99(13) . . ?
I5 Nb4 I6 94.11(2) . . ?
I5 Nb4 I7 89.58(2) . . ?
I5 Nb4 I8 173.53(2) . . ?
I5 Nb4 Nb1 115.93(2) . . ?
I6 Nb4 I8 90.64(2) . . ?
I6 Nb4 Nb1 117.52(2) . . ?
I7 Nb4 I6 174.71(2) . . ?
I7 Nb4 I8 85.40(2) . . ?
I7 Nb4 Nb1 57.318(17) . . ?
I8 Nb4 Nb1 57.794(17) . . ?
I11 Nb4 I5 91.97(2) . . ?
I11 Nb4 I6 90.92(2) . . ?
I11 Nb4 I7 92.75(2) . . ?
I11 Nb4 I8 92.35(2) . . ?
I11 Nb4 Nb1 136.58(3) . . ?
I11 Nb4 Nb3 135.53(3) . . ?
Nb3 Nb4 I5 60.097(18) . . ?
Nb3 Nb4 I6 60.581(18) . . ?
Nb3 Nb4 I7 118.55(2) . . ?
Nb3 Nb4 I8 119.10(2) . . ?
Nb3 Nb4 Nb1 87.88(2) . . ?
O1 Nb4 I5 90.30(14) . . ?
O1 Nb4 I6 90.06(15) . . ?
O1 Nb4 I7 86.12(16) . . ?
O1 Nb4 I8 85.29(15) . . ?
O1 Nb4 I11 177.46(16) . . ?
O1 Nb4 Nb1 41.05(16) . . ?
O1 Nb4 Nb3 46.85(16) . . ?
I10 Nb5 Nb6 129.87(2) . . ?
I13 Nb5 I10 85.446(18) . . ?
I13 Nb5 Nb6 59.112(17) . . ?
I14 Nb5 I10 87.05(2) . . ?
I14 Nb5 I13 86.925(19) . . ?
I14 Nb5 I20 88.440(19) . . ?
I14 Nb5 Nb6 59.185(18) . . ?
I19 Nb5 I10 91.57(2) . . ?
I19 Nb5 I13 88.284(19) . . ?
I19 Nb5 I14 175.11(2) . . ?
I19 Nb5 I20 96.33(2) . . ?
I19 Nb5 Nb6 118.83(2) . . ?
I20 Nb5 I10 93.45(2) . . ?
I20 Nb5 I13 175.28(3) . . ?
I20 Nb5 Nb6 118.89(2) . . ?
Nb8 Nb5 I10 137.24(3) . . ?
Nb8 Nb5 I13 122.56(2) . . ?
Nb8 Nb5 I14 122.64(2) . . ?
Nb8 Nb5 I19 61.118(18) . . ?
Nb8 Nb5 I20 60.997(18) . . ?
Nb8 Nb5 Nb6 92.87(2) . . ?
O2 Nb5 I10 173.48(14) . . ?
O2 Nb5 I13 88.94(13) . . ?
O2 Nb5 I14 89.34(14) . . ?
O2 Nb5 I19 91.57(14) . . ?
O2 Nb5 I20 91.88(13) . . ?
O2 Nb5 Nb6 43.77(14) . . ?
O2 Nb5 Nb8 49.11(14) . . ?
I12 Nb6 Nb5 130.40(2) 1_554 . ?
I13 Nb6 I12 87.723(19) . 1_554 ?
I13 Nb6 Nb5 59.307(17) . . ?
I14 Nb6 I12 85.741(19) . 1_554 ?
I14 Nb6 I13 86.803(19) . . ?
I14 Nb6 Nb5 58.773(18) . . ?
I15 Nb6 I12 93.60(2) . 1_554 ?
I15 Nb6 I13 86.990(18) . . ?
I15 Nb6 I14 173.78(2) . . ?
I15 Nb6 I16 96.88(2) . . ?
I15 Nb6 Nb5 117.93(2) . . ?
I16 Nb6 I12 90.95(2) . 1_554 ?
I16 Nb6 I13 175.99(3) . . ?
I16 Nb6 I14 89.322(19) . . ?
I16 Nb6 Nb5 119.27(2) . . ?
Nb7 Nb6 I12 136.60(3) . 1_554 ?
Nb7 Nb6 I13 122.38(2) . . ?
Nb7 Nb6 I14 122.85(2) . . ?
Nb7 Nb6 I15 61.336(18) . . ?
Nb7 Nb6 I16 60.837(18) . . ?
Nb7 Nb6 Nb5 92.97(2) . . ?
O2 Nb6 I12 174.83(15) . 1_554 ?
O2 Nb6 I13 89.72(14) . . ?
O2 Nb6 I14 89.63(14) . . ?
O2 Nb6 I15 90.76(14) . . ?
O2 Nb6 I16 91.30(14) . . ?
O2 Nb6 Nb5 44.63(15) . . ?
O2 Nb6 Nb7 48.34(15) . . ?
I15 Nb7 I17 88.703(19) . . ?
I15 Nb7 I18 170.66(3) . . ?
I15 Nb7 Nb8 114.84(2) . . ?
I16 Nb7 I15 96.92(2) . . ?
I16 Nb7 I17 171.76(3) . . ?
I16 Nb7 I18 89.90(2) . . ?
I16 Nb7 Nb8 115.93(2) . . ?
I17 Nb7 I18 83.87(2) . . ?
I17 Nb7 Nb8 55.989(17) . . ?
I18 Nb7 Nb8 56.118(16) . . ?
I21 Nb7 I15 92.22(2) . . ?
I21 Nb7 I16 94.15(2) . . ?
I21 Nb7 I17 91.63(2) . . ?
I21 Nb7 I18 93.64(2) . . ?
I21 Nb7 Nb6 138.04(3) . . ?
I21 Nb7 Nb8 134.88(3) . . ?
Nb6 Nb7 I15 60.866(18) . . ?
Nb6 Nb7 I16 61.384(19) . . ?
Nb6 Nb7 I17 117.08(2) . . ?
Nb6 Nb7 I18 117.92(2) . . ?
Nb6 Nb7 Nb8 87.01(2) . . ?
O2 Nb7 I15 89.76(13) . . ?
O2 Nb7 I16 91.08(14) . . ?
O2 Nb7 I17 82.90(14) . . ?
O2 Nb7 I18 83.73(13) . . ?
O2 Nb7 I21 174.15(14) . . ?
O2 Nb7 Nb6 47.37(14) . . ?
O2 Nb7 Nb8 39.65(14) . . ?
I17 Nb8 I18 83.879(19) . . ?
I17 Nb8 Nb7 55.886(17) . . ?
I18 Nb8 Nb7 56.238(16) . . ?
I19 Nb8 I17 88.893(19) . . ?
I19 Nb8 I18 171.26(3) . . ?
I19 Nb8 I20 96.39(2) . . ?
I19 Nb8 Nb7 115.42(2) . . ?
I20 Nb8 I17 171.89(3) . . ?
I20 Nb8 I18 90.289(19) . . ?
I20 Nb8 Nb7 116.09(2) . . ?
I22 Nb8 I17 91.69(2) . . ?
I22 Nb8 I18 93.43(2) . . ?
I22 Nb8 I19 91.70(2) . . ?
I22 Nb8 I20 94.29(2) . . ?
I22 Nb8 Nb5 138.00(3) . . ?
I22 Nb8 Nb7 134.78(3) . . ?
Nb5 Nb8 I17 116.88(2) . . ?
Nb5 Nb8 I18 118.30(2) . . ?
Nb5 Nb8 I19 60.983(18) . . ?
Nb5 Nb8 I20 61.230(18) . . ?
Nb5 Nb8 Nb7 87.14(2) . . ?
O2 Nb8 I17 82.32(14) . . ?
O2 Nb8 I18 83.33(13) . . ?
O2 Nb8 I19 90.85(13) . . ?
O2 Nb8 I20 91.43(14) . . ?
O2 Nb8 I22 173.44(14) . . ?
O2 Nb8 Nb5 48.17(14) . . ?
O2 Nb8 Nb7 38.97(14) . . ?
Nb1 O1 Nb2 83.2(2) . . ?
Nb1 O1 Nb4 96.3(2) . . ?
Nb3 O1 Nb1 177.8(3) . . ?
Nb3 O1 Nb2 96.3(2) . . ?
Nb3 O1 Nb4 84.2(2) . . ?
Nb4 O1 Nb2 178.0(3) . . ?
Nb5 O2 Nb8 82.7(2) . . ?
Nb6 O2 Nb5 91.60(19) . . ?
Nb6 O2 Nb7 84.3(2) . . ?
Nb6 O2 Nb8 174.3(3) . . ?
Nb7 O2 Nb5 175.9(3) . . ?
Nb7 O2 Nb8 101.4(2) . . ?

_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
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4924(4) 38203 28541 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.5076(4) 38381 28541 nmt -1.0001 -0.0001 0.0002 0.0001 -1.0000 0.0003
-0.0454 -0.0386 0.9999

_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)
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jb189(6)v3
_database_code_depnum_ccdc_archive 'CCDC 2391069'
loop_
_audit_author_name
_audit_author_address
'Markus Stroebele'
;University of Tuebingen
Germany
;
_audit_update_record             
;
2024-10-15 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_audit_creation_date             2024-10-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I11 Nb4 O'
_chemical_formula_sum            'I11 Nb4 O'
_chemical_formula_weight         1783.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Nb4 O I11'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   15.4442(3)
_cell_length_b                   13.0449(2)
_cell_length_c                   11.9078(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.698(2)
_cell_angle_gamma                90
_cell_volume                     2309.56(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18269
_cell_measurement_temperature    220.0(9)
_cell_measurement_theta_max      45.2750
_cell_measurement_theta_min      2.0500
_shelx_estimated_absorpt_T_max   0.602
_shelx_estimated_absorpt_T_min   0.462
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3020
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
21 -4 -4 0.0238
5 13 -12 0.0256
-8 14 -8 0.0205
-13 8 14 0.0207
13 3 10 0.0276
-9 -5 -12 0.0119
14 -8 -13 0.0232
18 10 -8 0.0246
-9 16 -3 0.0228
-3 -10 14 0.0110
13 -10 7 0.0181
-4 11 -12 0.0185
-7 2 -14 0.0136
2 15 9 0.0275
20 8 -3 0.0247

_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.034
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
21.2912 -3.8342 -4.2867 -0.0235 -0.0179 0.9996
5.1218 13.2029 -11.6602 -0.8521 -0.5215 0.0447
-7.5932 13.6249 -7.6948 -0.7261 -0.4425 -0.5263
-13.1364 7.9029 13.6006 0.5749 -0.4720 -0.6684
12.8953 3.3456 9.9964 0.6406 -0.5308 0.5548
-9.2428 -4.7449 -12.0999 -0.7139 0.5906 -0.3763
14.1509 -7.7983 -13.1476 -0.5417 0.4445 0.7135
17.6837 9.5478 -7.9865 -0.4784 -0.5766 0.6623
-8.9615 15.7372 -3.1981 -0.5045 -0.6139 -0.6071
-3.1675 -10.1798 13.9175 0.9539 0.3001 0.0089
12.7417 -10.1803 6.9191 0.6679 0.2123 0.7133
-4.3522 11.0101 -11.6308 -0.8918 -0.2816 -0.3540
-6.6010 1.9391 -13.9325 -0.9047 0.2505 -0.3447
2.4719 14.5960 9.1436 0.3325 -0.9413 -0.0576
19.6905 7.7782 -3.2236 -0.1539 -0.6029 0.7829

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -61.00 -27.00   0.50   65.00    --  -39.27 107.00 -57.00   68
  2  ω      4.00  35.00   0.50   65.00    --   40.83-107.00-155.00   62
  3  ω   -110.00 -34.00   0.50   65.00    --  -39.27 -37.00   0.00  152
  4  ω   -109.00 -77.00   0.50   65.00    --  -39.27 178.00 120.00   64
  5  ω   -107.00 -27.00   0.50   65.00    --  -39.27 -77.00-150.00  160
  6  ω    -88.00 -33.00   0.50   65.00    --  -39.27   0.00-150.00  110
  7  ω   -110.00 -84.00   0.50   65.00    --  -39.27 -57.00-120.00   52
  8  ω    -44.00  18.00   0.50   65.00    --  -39.27  19.00-150.00  124
  9  ω    -61.00 -29.00   0.50   65.00    --  -39.27 -57.00-120.00   64
 10  ω    -13.00  27.00   0.50   65.00    --  -39.27  57.00  30.00   80
 11  ω    -43.00   0.00   0.50   65.00    --  -39.27  57.00 -90.00   86
 12  ω   -110.00 -66.00   0.50   65.00    --  -39.27 178.00-150.00   88
 13  ω   -110.00 -22.00   0.50   65.00    --  -39.27 -77.00 120.00  176
 14  ω    -96.00 -20.00   0.50   65.00    --  -39.27 -77.00-120.00  152
 15  ω    -24.00   2.00   0.50   65.00    --   40.83 -19.00   0.00   52
 16  ω     43.00  69.00   0.50   65.00    --   40.83 -99.00 -60.00   52
 17  ω    -22.00  20.00   0.50   65.00    --   40.83 -99.00 -60.00   84
 18  ω     87.00 112.00   0.50   65.00    --   40.83-178.00 -60.00   50
 19  ω     46.00  71.00   0.50   65.00    --   40.83-178.00 -60.00   50
 20  ω    -26.00   4.00   0.50   65.00    --   40.83 -19.00 -30.00   60
 21  ω      4.00  30.00   0.50   65.00    --   40.83   0.00-120.00   52
 22  ω    -64.00 -21.00   0.50   65.00    --  -39.27 -74.00   0.70   86
 23  ω     -4.00  32.00   0.50   65.00    --  -39.27  37.00-150.00   72
 24  ω   -110.00 -29.00   0.50   65.00    --  -39.27 -52.00 140.34  162
 25  ω   -111.00 -66.00   0.50   65.00    --  -39.27 -25.00-167.43   90
 26  ω    -89.00 -40.00   0.50   65.00    --  -39.27 135.00  26.80   98
 27  ω    -91.00 -49.00   0.50   65.00    --  -39.27 139.00 -16.89   84
 28  ω    -38.00 -13.00   0.50   65.00    --  -39.27 -92.00  55.39   50
 29  ω    -98.00 -34.00   0.50   65.00    --  -39.27 -37.00 -90.00  128
 30  ω   -108.00 -81.00   0.50   65.00    --  -39.27 -74.00   0.70   54
 31  ω    -89.00 -46.00   0.50   65.00    --  -39.27 135.00  98.04   86
 32  ω    -89.00 -63.00   0.50   65.00    --  -39.27 -77.00 -60.00   52
 33  ω    -50.00 -20.00   0.50   65.00    --  -39.27 -77.00 -60.00   60
 34  ω    -90.00 -41.00   0.50   65.00    --  -39.27 137.00 143.68   98
 35  ω    -87.00 -34.00   0.50   65.00    --  -39.27   0.00  90.00  106
 36  ω   -107.00 -74.00   0.50   65.00    --  -39.27 -57.00  60.00   66
 37  ω    -70.00 -28.00   0.50   65.00    --  -39.27 -57.00  60.00   84
 38  ω   -103.00 -70.00   0.50   65.00    --  -39.27 -77.00-180.00   66
 39  ω    -47.00 -20.00   0.50   65.00    --  -39.27 -77.00-180.00   54
 40  ω    -41.00 -14.00   0.50   65.00    --  -39.27  37.00-150.00   54
 41  ω     27.00  59.00   0.50   65.00    --   40.83-153.00   4.37   64
 42  ω    -27.00   5.00   0.50   65.00    --   40.83 -19.00  60.00   64
 43  ω     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       'ω 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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3104
_reflns_number_total             3115
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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+0.001xFc²λ³/sin(2θ)]^-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_R_factor_all          0.0151
_refine_ls_R_factor_gt           0.0150
_refine_ls_restrained_S_all      1.430
_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/[σ²(Fo²)+15.3976P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0314
_refine_ls_wR_factor_ref         0.0315
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: Nb2(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.60649(2) 0.71807(2) 0.12624(2) 0.02241(5) Uani 1 1 d . . . . .
I2 I 0.51871(2) 0.500000 0.29781(3) 0.02205(7) Uani 1 2 d S T P . .
I3 I 0.27706(2) 0.500000 0.01732(3) 0.02030(7) Uani 1 2 d S T P . .
I4 I 0.36213(2) 0.74644(2) 0.20202(2) 0.02622(6) Uani 1 1 d . . . . .
I5 I 0.50822(2) 1.000000 0.20286(3) 0.02314(7) Uani 1 2 d S T P . .
I6 I 0.61198(2) 0.78171(2) 0.45196(2) 0.02274(5) Uani 1 1 d . . . . .
I7 I 0.77129(2) 1.000000 0.37317(4) 0.03423(9) Uani 1 2 d S T P . .
I8 I 0.71191(2) 1.000000 0.67664(3) 0.01837(6) Uani 1 2 d S T P . .
Nb1 Nb 0.44318(2) 0.60490(2) 0.08630(3) 0.01717(6) Uani 1 1 d . . . . .
Nb2 Nb 0.45479(4) 0.89265(4) 0.37754(5) 0.01424(10) Uani 0.5 1 d . . P . .
Nb3 Nb 0.61459(3) 1.000000 0.43768(4) 0.01691(8) Uani 1 2 d S T P . .
O1 O 0.500000 0.500000 0.000000 0.0260(11) Uani 1 4 d S T P . .
O2 O 0.500000 1.000000 0.500000 0.0264(11) Uani 1 4 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Nb1 2.8491(4) . ?
I1 Nb1 2.8499(4) 2_655 ?
I2 Nb1 2.8262(4) . ?
I2 Nb1 2.8262(4) 6_565 ?
I3 Nb1 2.8265(4) 6_565 ?
I3 Nb1 2.8265(4) . ?
I4 Nb1 2.7943(4) . ?
I4 Nb2 2.9044(6) . ?
I5 Nb2 2.8103(6) 6_575 ?
I5 Nb2 2.8103(6) . ?
I5 Nb3 2.8340(5) . ?
I6 Nb2 2.7585(6) . ?
I6 Nb2 2.9003(6) 2_656 ?
I6 Nb3 2.8536(2) . ?
I7 Nb3 2.7300(5) . ?
I8 Nb2 2.8472(6) 5_676 ?
I8 Nb2 2.8472(6) 2_656 ?
I8 Nb3 2.8358(5) . ?
Nb1 Nb1 3.0423(6) 2_655 ?
Nb1 Nb1 2.7368(6) 6_565 ?
Nb1 O1 2.0461(3) . ?
Nb2 Nb2 2.8726(11) 2_656 ?
Nb2 Nb2 2.8008(11) 6_575 ?
Nb2 Nb3 2.7584(7) . ?
Nb2 Nb3 3.0375(6) 5_676 ?
Nb2 O2 2.0060(5) . ?
Nb3 O2 2.0961(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Nb1 I1 Nb1 64.529(12) . 2_655 ?
Nb1 I2 Nb1 57.918(13) 6_565 . ?
Nb1 I3 Nb1 57.910(13) 6_565 . ?
Nb1 I4 Nb2 126.127(15) . . ?
Nb2 I5 Nb2 59.78(2) . 6_575 ?
Nb2 I5 Nb3 58.511(14) 6_575 . ?
Nb2 I5 Nb3 58.510(14) . . ?
Nb2 I6 Nb2 60.95(2) . 2_656 ?
Nb2 I6 Nb3 58.852(15) . . ?
Nb3 I6 Nb2 63.721(14) . 2_656 ?
Nb2 I8 Nb2 58.93(2) 2_656 5_676 ?
Nb3 I8 Nb2 64.618(14) . 2_656 ?
Nb3 I8 Nb2 64.618(14) . 5_676 ?
I1 Nb1 I1 83.874(12) . 2_655 ?
I1 Nb1 Nb1 57.726(9) 2_655 2_655 ?
I1 Nb1 Nb1 57.748(9) . 2_655 ?
I2 Nb1 I1 88.213(11) . . ?
I2 Nb1 I1 171.587(14) . 2_655 ?
I2 Nb1 I3 98.505(12) . . ?
I2 Nb1 Nb1 115.313(14) . 2_655 ?
I3 Nb1 I1 172.874(14) . . ?
I3 Nb1 I1 89.293(11) . 2_655 ?
I3 Nb1 Nb1 116.608(14) . 2_655 ?
I4 Nb1 I1 94.000(11) . . ?
I4 Nb1 I1 92.681(11) . 2_655 ?
I4 Nb1 I2 90.710(11) . . ?
I4 Nb1 I3 88.320(11) . . ?
I4 Nb1 Nb1 138.626(8) . 2_655 ?
Nb1 Nb1 I1 121.198(8) 6_565 2_655 ?
Nb1 Nb1 I1 121.208(8) 6_565 . ?
Nb1 Nb1 I2 61.041(7) 6_565 . ?
Nb1 Nb1 I3 61.044(7) 6_565 . ?
Nb1 Nb1 I4 131.357(8) 6_565 . ?
Nb1 Nb1 Nb1 90.0 6_565 2_655 ?
O1 Nb1 I1 87.102(11) . 2_655 ?
O1 Nb1 I1 87.122(11) . . ?
O1 Nb1 I2 89.660(11) . . ?
O1 Nb1 I3 90.527(11) . . ?
O1 Nb1 I4 178.829(15) . . ?
O1 Nb1 Nb1 41.973(8) . 2_655 ?
O1 Nb1 Nb1 48.027(8) . 6_565 ?
I4 Nb2 Nb3 128.49(2) . 5_676 ?
I5 Nb2 I4 88.897(17) . . ?
I5 Nb2 I6 176.33(2) . 2_656 ?
I5 Nb2 I8 90.902(18) . 5_676 ?
I5 Nb2 Nb2 126.30(3) . 2_656 ?
I5 Nb2 Nb3 122.56(2) . 5_676 ?
I6 Nb2 I4 96.090(18) . . ?
I6 Nb2 I4 88.673(17) 2_656 . ?
I6 Nb2 I5 95.166(18) . . ?
I6 Nb2 I6 87.823(18) . 2_656 ?
I6 Nb2 I8 173.76(2) . 5_676 ?
I6 Nb2 Nb2 61.964(17) . 2_656 ?
I6 Nb2 Nb2 121.644(13) . 6_575 ?
I6 Nb2 Nb3 117.48(2) . 5_676 ?
I6 Nb2 Nb3 57.390(12) 2_656 5_676 ?
I8 Nb2 I4 85.450(16) 5_676 . ?
I8 Nb2 I6 86.168(16) 5_676 2_656 ?
I8 Nb2 Nb2 113.05(2) 5_676 2_656 ?
I8 Nb2 Nb3 57.510(14) 5_676 5_676 ?
Nb2 Nb2 I4 131.047(12) 6_575 . ?
Nb2 Nb2 I4 137.743(14) 2_656 . ?
Nb2 Nb2 I5 60.112(12) 6_575 . ?
Nb2 Nb2 I6 119.931(12) 6_575 2_656 ?
Nb2 Nb2 I6 57.084(17) 2_656 2_656 ?
Nb2 Nb2 I8 60.537(12) 6_575 5_676 ?
Nb2 Nb2 Nb2 90.0 6_575 2_656 ?
Nb2 Nb2 Nb3 62.545(11) 6_575 5_676 ?
Nb2 Nb2 Nb3 55.562(18) 2_656 5_676 ?
Nb3 Nb2 I4 138.78(2) . . ?
Nb3 Nb2 I5 61.174(16) . . ?
Nb3 Nb2 I6 122.29(2) . 2_656 ?
Nb3 Nb2 I6 62.295(13) . . ?
Nb3 Nb2 I8 119.99(2) . 5_676 ?
Nb3 Nb2 Nb2 65.253(19) . 2_656 ?
Nb3 Nb2 Nb2 59.491(13) . 6_575 ?
Nb3 Nb2 Nb3 92.529(19) . 5_676 ?
O2 Nb2 I4 171.26(3) . . ?
O2 Nb2 I5 94.36(2) . . ?
O2 Nb2 I6 91.70(2) . . ?
O2 Nb2 I6 87.665(19) . 2_656 ?
O2 Nb2 I8 86.385(19) . 5_676 ?
O2 Nb2 Nb2 44.276(16) . 2_656 ?
O2 Nb2 Nb2 45.725(16) . 6_575 ?
O2 Nb2 Nb3 49.145(14) . . ?
O2 Nb2 Nb3 43.384(12) . 5_676 ?
I5 Nb3 I6 92.581(10) . 6_575 ?
I5 Nb3 I6 92.581(10) . . ?
I5 Nb3 I8 176.758(18) . . ?
I5 Nb3 Nb2 119.392(17) . 5_676 ?
I5 Nb3 Nb2 119.392(17) . 2_656 ?
I6 Nb3 I6 172.560(19) . 6_575 ?
I6 Nb3 Nb2 58.888(13) . 2_656 ?
I6 Nb3 Nb2 58.888(13) 6_575 5_676 ?
I6 Nb3 Nb2 113.794(17) 6_575 2_656 ?
I6 Nb3 Nb2 113.794(17) . 5_676 ?
I7 Nb3 I5 92.508(16) . . ?
I7 Nb3 I6 92.562(9) . 6_575 ?
I7 Nb3 I6 92.561(9) . . ?
I7 Nb3 I8 90.735(16) . . ?
I7 Nb3 Nb2 136.551(17) . . ?
I7 Nb3 Nb2 135.817(17) . 5_676 ?
I7 Nb3 Nb2 136.551(17) . 6_575 ?
I7 Nb3 Nb2 135.817(17) . 2_656 ?
I8 Nb3 I6 87.272(10) . 6_575 ?
I8 Nb3 I6 87.271(10) . . ?
I8 Nb3 Nb2 57.872(14) . 2_656 ?
I8 Nb3 Nb2 57.872(14) . 5_676 ?
Nb2 Nb3 I5 60.316(15) . . ?
Nb2 Nb3 I5 60.316(15) 6_575 . ?
Nb2 Nb3 I6 58.852(13) 6_575 6_575 ?
Nb2 Nb3 I6 119.736(18) 6_575 . ?
Nb2 Nb3 I6 119.734(18) . 6_575 ?
Nb2 Nb3 I6 58.853(13) . . ?
Nb2 Nb3 I8 117.036(17) . . ?
Nb2 Nb3 I8 117.036(17) 6_575 . ?
Nb2 Nb3 Nb2 87.473(19) . 5_676 ?
Nb2 Nb3 Nb2 59.19(2) 6_575 5_676 ?
Nb2 Nb3 Nb2 61.02(3) . 6_575 ?
Nb2 Nb3 Nb2 54.91(2) 5_676 2_656 ?
Nb2 Nb3 Nb2 59.19(2) . 2_656 ?
Nb2 Nb3 Nb2 87.473(19) 6_575 2_656 ?
O2 Nb3 I5 91.705(16) . . ?
O2 Nb3 I6 87.247(9) . 6_575 ?
O2 Nb3 I6 87.248(9) . . ?
O2 Nb3 I7 175.79(2) . . ?
O2 Nb3 I8 85.053(15) . . ?
O2 Nb3 Nb2 46.374(13) . . ?
O2 Nb3 Nb2 41.099(12) . 2_656 ?
O2 Nb3 Nb2 41.099(12) . 5_676 ?
O2 Nb3 Nb2 46.374(13) . 6_575 ?
Nb1 O1 Nb1 96.053(17) 2_655 . ?
Nb1 O1 Nb1 96.055(17) 5_665 6_565 ?
Nb1 O1 Nb1 83.947(17) 6_565 . ?
Nb1 O1 Nb1 180.000(13) 6_565 2_655 ?
Nb1 O1 Nb1 180.0 5_665 . ?
Nb1 O1 Nb1 83.945(17) 5_665 2_655 ?
Nb2 O2 Nb2 180.0 . 5_676 ?
Nb2 O2 Nb2 88.55(3) 5_676 2_656 ?
Nb2 O2 Nb2 91.45(3) . 2_656 ?
Nb2 O2 Nb2 88.55(3) . 6_575 ?
Nb2 O2 Nb2 91.45(3) 5_676 6_575 ?
Nb2 O2 Nb2 180.0 6_575 2_656 ?
Nb2 O2 Nb3 84.483(18) 2_656 5_676 ?
Nb2 O2 Nb3 84.483(18) 5_676 5_676 ?
Nb2 O2 Nb3 95.518(18) . 5_676 ?
Nb2 O2 Nb3 84.482(18) 6_575 . ?
Nb2 O2 Nb3 95.517(18) 6_575 5_676 ?
Nb2 O2 Nb3 95.518(18) 2_656 . ?
Nb2 O2 Nb3 84.481(18) . . ?
Nb2 O2 Nb3 95.518(18) 5_676 . ?
Nb3 O2 Nb3 180.0 . 5_676 ?

_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
