# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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. 
# 
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data_knb1
_database_code_depnum_ccdc_archive 'CCDC 1426204'
loop_
_audit_author_name
_audit_author_address
'Bipul Sarma'
;Tezpur University
India
;
_audit_update_record             
;
2023-06-15 deposited with the CCDC.	2023-06-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'K3 Nb O8'
_chemical_formula_weight         338.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.2009 0.2494 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_H-M_alt        'I -4 2 m'
_space_group_name_Hall           'I -4 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y, -z'
'-y, -x, z'
'-x, y, -z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   6.7850(2)
_cell_length_b                   6.7850(2)
_cell_length_c                   7.7718(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     357.78(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3301
_cell_measurement_theta_min      3.99
_cell_measurement_theta_max      28.39

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.139
_exptl_crystal_F_000             324
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.270
_exptl_absorpt_coefficient_mu    3.432
_shelx_estimated_absorpt_T_min   0.416
_shelx_estimated_absorpt_T_max   0.458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_T_max  0.395
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   SADABS
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2916
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.987
_diffrn_reflns_theta_max         28.459
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 0.895
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 0.923
_reflns_number_total             236
_reflns_number_gt                236
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.662
_reflns_Friedel_fraction_max     0.980
_reflns_Friedel_fraction_full    0.970

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0119P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.049(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.12(5)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         236
_refine_ls_number_parameters     21
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0071
_refine_ls_R_factor_gt           0.0071
_refine_ls_wR_factor_ref         0.0178
_refine_ls_wR_factor_gt          0.0178
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.133
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.5000 0.5000 0.5000 0.00545(11) Uani 1 8 d S T P . .
O1 O 0.36031(12) 0.36031(12) 0.30914(16) 0.0102(2) Uani 1 2 d S T P . .
O2 O 0.28652(10) 0.28652(10) 0.4808(3) 0.0119(3) Uani 1 2 d S T P . .
K1 K 0.0000 0.5000 0.2500 0.01392(13) Uani 1 4 d S T P . .
K3 K 0.0000 0.0000 0.5000 0.00844(14) Uani 1 8 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
Nb1 O1 1.9992(12) 4_656 ?
Nb1 O1 1.9992(12) 2_566 ?
Nb1 O1 1.9992(12) 3_665 ?
Nb1 O1 1.9992(12) . ?
Nb1 O2 2.0539(10) . ?
Nb1 O2 2.0539(10) 3_665 ?
Nb1 O2 2.0539(10) 4_656 ?
Nb1 O2 2.0539(10) 2_566 ?
Nb1 K3 3.88590(15) 9 ?
Nb1 K3 3.88590(15) 9_554 ?
Nb1 K1 3.90949(9) . ?
Nb1 K1 3.90949(9) 13 ?
O1 O2 1.510(2) . ?
O1 K1 2.6620(5) . ?
O1 K1 2.6620(5) 13 ?
O1 K3 2.7512(12) 9_554 ?
O2 K3 2.7533(10) . ?
O2 K1 3.0156(14) 13 ?
O2 K1 3.0156(14) . ?
O2 K1 3.2024(15) 9_545 ?
O2 K1 3.2024(15) 5_566 ?
K1 O1 2.6620(5) 10_455 ?
K1 O1 2.6620(5) 12 ?
K1 O1 2.6620(5) 3_565 ?
K1 O2 3.0156(14) 10_455 ?
K1 O2 3.0156(14) 12 ?
K1 O2 3.0156(14) 3_565 ?
K1 O2 3.2024(15) 2_566 ?
K1 O2 3.2024(15) 11_554 ?
K1 O2 3.2024(15) 4_556 ?
K1 O2 3.2024(15) 9_454 ?
K3 O1 2.7512(12) 11 ?
K3 O1 2.7512(12) 12_545 ?
K3 O1 2.7512(12) 10_455 ?
K3 O1 2.7512(12) 9_445 ?
K3 O2 2.7533(10) 3 ?
K3 O2 2.7533(10) 4_556 ?
K3 O2 2.7533(10) 2_556 ?
K3 Nb1 3.88590(15) 9_444 ?
K3 Nb1 3.88590(15) 9_445 ?
K3 K1 3.90949(9) 13_455 ?
K3 K1 3.90949(10) 5_566 ?

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
O1 Nb1 O1 84.21(7) 4_656 2_566 ?
O1 Nb1 O1 123.40(4) 4_656 3_665 ?
O1 Nb1 O1 123.40(4) 2_566 3_665 ?
O1 Nb1 O1 123.40(4) 4_656 . ?
O1 Nb1 O1 123.40(4) 2_566 . ?
O1 Nb1 O1 84.21(7) 3_665 . ?
O1 Nb1 O2 93.10(5) 4_656 . ?
O1 Nb1 O2 93.10(5) 2_566 . ?
O1 Nb1 O2 127.93(8) 3_665 . ?
O1 Nb1 O2 43.72(6) . . ?
O1 Nb1 O2 93.09(5) 4_656 3_665 ?
O1 Nb1 O2 93.09(5) 2_566 3_665 ?
O1 Nb1 O2 43.72(6) 3_665 3_665 ?
O1 Nb1 O2 127.93(8) . 3_665 ?
O2 Nb1 O2 171.65(13) . 3_665 ?
O1 Nb1 O2 43.72(6) 4_656 4_656 ?
O1 Nb1 O2 127.93(8) 2_566 4_656 ?
O1 Nb1 O2 93.09(5) 3_665 4_656 ?
O1 Nb1 O2 93.09(5) . 4_656 ?
O2 Nb1 O2 90.303(9) . 4_656 ?
O2 Nb1 O2 90.303(10) 3_665 4_656 ?
O1 Nb1 O2 127.93(8) 4_656 2_566 ?
O1 Nb1 O2 43.72(6) 2_566 2_566 ?
O1 Nb1 O2 93.09(5) 3_665 2_566 ?
O1 Nb1 O2 93.09(5) . 2_566 ?
O2 Nb1 O2 90.303(9) . 2_566 ?
O2 Nb1 O2 90.303(9) 3_665 2_566 ?
O2 Nb1 O2 171.65(13) 4_656 2_566 ?
O1 Nb1 K3 42.10(3) 4_656 9 ?
O1 Nb1 K3 42.10(3) 2_566 9 ?
O1 Nb1 K3 137.90(3) 3_665 9 ?
O1 Nb1 K3 137.90(3) . 9 ?
O2 Nb1 K3 94.17(6) . 9 ?
O2 Nb1 K3 94.17(6) 3_665 9 ?
O2 Nb1 K3 85.83(6) 4_656 9 ?
O2 Nb1 K3 85.83(6) 2_566 9 ?
O1 Nb1 K3 137.90(3) 4_656 9_554 ?
O1 Nb1 K3 137.90(3) 2_566 9_554 ?
O1 Nb1 K3 42.10(3) 3_665 9_554 ?
O1 Nb1 K3 42.10(3) . 9_554 ?
O2 Nb1 K3 85.83(6) . 9_554 ?
O2 Nb1 K3 85.83(6) 3_665 9_554 ?
O2 Nb1 K3 94.17(6) 4_656 9_554 ?
O2 Nb1 K3 94.17(6) 2_566 9_554 ?
K3 Nb1 K3 180.0 9 9_554 ?
O1 Nb1 K1 141.272(7) 4_656 . ?
O1 Nb1 K1 87.55(3) 2_566 . ?
O1 Nb1 K1 92.45(3) 3_665 . ?
O1 Nb1 K1 38.728(7) . . ?
O2 Nb1 K1 49.60(4) . . ?
O2 Nb1 K1 125.16(4) 3_665 . ?
O2 Nb1 K1 130.40(4) 4_656 . ?
O2 Nb1 K1 54.84(4) 2_566 . ?
K3 Nb1 K1 119.801(1) 9 . ?
K3 Nb1 K1 60.199(1) 9_554 . ?
O1 Nb1 K1 87.55(3) 4_656 13 ?
O1 Nb1 K1 141.272(7) 2_566 13 ?
O1 Nb1 K1 92.45(3) 3_665 13 ?
O1 Nb1 K1 38.728(6) . 13 ?
O2 Nb1 K1 49.60(4) . 13 ?
O2 Nb1 K1 125.16(4) 3_665 13 ?
O2 Nb1 K1 54.84(4) 4_656 13 ?
O2 Nb1 K1 130.40(4) 2_566 13 ?
K3 Nb1 K1 119.801(1) 9 13 ?
K3 Nb1 K1 60.199(1) 9_554 13 ?
K1 Nb1 K1 75.700(1) . 13 ?
O2 O1 Nb1 70.06(6) . . ?
O2 O1 K1 88.06(4) . . ?
Nb1 O1 K1 113.25(3) . . ?
O2 O1 K1 88.06(4) . 13 ?
Nb1 O1 K1 113.25(3) . 13 ?
K1 O1 K1 128.62(4) . 13 ?
O2 O1 K3 178.80(8) . 9_554 ?
Nb1 O1 K3 108.74(5) . 9_554 ?
K1 O1 K3 92.46(3) . 9_554 ?
K1 O1 K3 92.46(3) 13 9_554 ?
O1 O2 Nb1 66.21(6) . . ?
O1 O2 K3 121.07(10) . . ?
Nb1 O2 K3 172.71(11) . . ?
O1 O2 K1 61.91(5) . 13 ?
Nb1 O2 K1 99.16(4) . 13 ?
K3 O2 K1 85.20(3) . 13 ?
O1 O2 K1 61.91(5) . . ?
Nb1 O2 K1 99.16(4) . . ?
K3 O2 K1 85.20(3) . . ?
K1 O2 K1 105.40(7) 13 . ?
O1 O2 K1 128.93(3) . 9_545 ?
Nb1 O2 K1 93.53(5) . 9_545 ?
K3 O2 K1 81.68(3) . 9_545 ?
K1 O2 K1 77.291(6) 13 9_545 ?
K1 O2 K1 166.35(4) . 9_545 ?
O1 O2 K1 128.93(3) . 5_566 ?
Nb1 O2 K1 93.53(5) . 5_566 ?
K3 O2 K1 81.68(3) . 5_566 ?
K1 O2 K1 166.35(4) 13 5_566 ?
K1 O2 K1 77.291(6) . 5_566 ?
K1 O2 K1 97.02(6) 9_545 5_566 ?
O1 K1 O1 91.708(9) . 10_455 ?
O1 K1 O1 91.709(9) . 12 ?
O1 K1 O1 160.11(5) 10_455 12 ?
O1 K1 O1 160.11(5) . 3_565 ?
O1 K1 O1 91.709(9) 10_455 3_565 ?
O1 K1 O1 91.709(9) 12 3_565 ?
O1 K1 O2 30.03(3) . . ?
O1 K1 O2 83.75(3) 10_455 . ?
O1 K1 O2 108.32(3) 12 . ?
O1 K1 O2 131.33(5) 3_565 . ?
O1 K1 O2 108.32(3) . 10_455 ?
O1 K1 O2 30.03(3) 10_455 10_455 ?
O1 K1 O2 131.33(5) 12 10_455 ?
O1 K1 O2 83.75(3) 3_565 10_455 ?
O2 K1 O2 110.71(4) . 10_455 ?
O1 K1 O2 83.75(3) . 12 ?
O1 K1 O2 131.33(5) 10_455 12 ?
O1 K1 O2 30.03(3) 12 12 ?
O1 K1 O2 108.32(3) 3_565 12 ?
O2 K1 O2 110.71(4) . 12 ?
O2 K1 O2 107.01(7) 10_455 12 ?
O1 K1 O2 131.33(5) . 3_565 ?
O1 K1 O2 108.32(3) 10_455 3_565 ?
O1 K1 O2 83.75(3) 12 3_565 ?
O1 K1 O2 30.03(3) 3_565 3_565 ?
O2 K1 O2 107.01(7) . 3_565 ?
O2 K1 O2 110.71(4) 10_455 3_565 ?
O2 K1 O2 110.71(4) 12 3_565 ?
O1 K1 O2 59.39(3) . 2_566 ?
O1 K1 O2 138.10(4) 10_455 2_566 ?
O1 K1 O2 58.75(3) 12 2_566 ?
O1 K1 O2 106.48(3) 3_565 2_566 ?
O2 K1 O2 55.76(3) . 2_566 ?
O2 K1 O2 166.35(4) 10_455 2_566 ?
O2 K1 O2 78.780(7) 12 2_566 ?
O2 K1 O2 77.61(3) 3_565 2_566 ?
O1 K1 O2 58.75(3) . 11_554 ?
O1 K1 O2 59.38(3) 10_455 11_554 ?
O1 K1 O2 106.48(3) 12 11_554 ?
O1 K1 O2 138.10(4) 3_565 11_554 ?
O2 K1 O2 78.780(7) . 11_554 ?
O2 K1 O2 55.76(3) 10_455 11_554 ?
O2 K1 O2 77.61(3) 12 11_554 ?
O2 K1 O2 166.35(4) 3_565 11_554 ?
O2 K1 O2 115.27(3) 2_566 11_554 ?
O1 K1 O2 106.48(3) . 4_556 ?
O1 K1 O2 58.75(3) 10_455 4_556 ?
O1 K1 O2 138.10(4) 12 4_556 ?
O1 K1 O2 59.38(3) 3_565 4_556 ?
O2 K1 O2 77.61(3) . 4_556 ?
O2 K1 O2 78.780(7) 10_455 4_556 ?
O2 K1 O2 166.35(4) 12 4_556 ?
O2 K1 O2 55.76(3) 3_565 4_556 ?
O2 K1 O2 98.41(6) 2_566 4_556 ?
O2 K1 O2 115.27(3) 11_554 4_556 ?
O1 K1 O2 138.10(4) . 9_454 ?
O1 K1 O2 106.48(3) 10_455 9_454 ?
O1 K1 O2 59.38(3) 12 9_454 ?
O1 K1 O2 58.75(3) 3_565 9_454 ?
O2 K1 O2 166.35(4) . 9_454 ?
O2 K1 O2 77.61(3) 10_455 9_454 ?
O2 K1 O2 55.76(3) 12 9_454 ?
O2 K1 O2 78.780(7) 3_565 9_454 ?
O2 K1 O2 115.27(3) 2_566 9_454 ?
O2 K1 O2 98.41(6) 11_554 9_454 ?
O2 K1 O2 115.27(3) 4_556 9_454 ?
O1 K3 O1 139.70(3) 11 12_545 ?
O1 K3 O1 139.70(3) 11 10_455 ?
O1 K3 O1 58.31(5) 12_545 10_455 ?
O1 K3 O1 58.31(5) 11 9_445 ?
O1 K3 O1 139.70(3) 12_545 9_445 ?
O1 K3 O1 139.70(3) 10_455 9_445 ?
O1 K3 O2 122.27(6) 11 3 ?
O1 K3 O2 87.28(4) 12_545 3 ?
O1 K3 O2 87.28(4) 10_455 3 ?
O1 K3 O2 63.95(5) 9_445 3 ?
O1 K3 O2 87.28(4) 11 4_556 ?
O1 K3 O2 122.27(6) 12_545 4_556 ?
O1 K3 O2 63.95(5) 10_455 4_556 ?
O1 K3 O2 87.28(4) 9_445 4_556 ?
O2 K3 O2 90.169(5) 3 4_556 ?
O1 K3 O2 87.28(4) 11 2_556 ?
O1 K3 O2 63.95(5) 12_545 2_556 ?
O1 K3 O2 122.27(6) 10_455 2_556 ?
O1 K3 O2 87.28(4) 9_445 2_556 ?
O2 K3 O2 90.169(5) 3 2_556 ?
O2 K3 O2 173.78(9) 4_556 2_556 ?
O1 K3 O2 63.95(5) 11 . ?
O1 K3 O2 87.28(4) 12_545 . ?
O1 K3 O2 87.28(4) 10_455 . ?
O1 K3 O2 122.27(6) 9_445 . ?
O2 K3 O2 173.78(9) 3 . ?
O2 K3 O2 90.169(5) 4_556 . ?
O2 K3 O2 90.169(5) 2_556 . ?
O1 K3 Nb1 150.84(2) 11 9_444 ?
O1 K3 Nb1 29.16(2) 12_545 9_444 ?
O1 K3 Nb1 29.16(2) 10_455 9_444 ?
O1 K3 Nb1 150.84(2) 9_445 9_444 ?
O2 K3 Nb1 86.89(5) 3 9_444 ?
O2 K3 Nb1 93.11(5) 4_556 9_444 ?
O2 K3 Nb1 93.11(5) 2_556 9_444 ?
O2 K3 Nb1 86.89(5) . 9_444 ?
O1 K3 Nb1 29.16(2) 11 9_445 ?
O1 K3 Nb1 150.84(2) 12_545 9_445 ?
O1 K3 Nb1 150.84(2) 10_455 9_445 ?
O1 K3 Nb1 29.16(2) 9_445 9_445 ?
O2 K3 Nb1 93.11(5) 3 9_445 ?
O2 K3 Nb1 86.89(5) 4_556 9_445 ?
O2 K3 Nb1 86.89(5) 2_556 9_445 ?
O2 K3 Nb1 93.11(5) . 9_445 ?
Nb1 K3 Nb1 180.0 9_444 9_445 ?
O1 K3 K1 137.135(10) 11 13_455 ?
O1 K3 K1 82.238(19) 12_545 13_455 ?
O1 K3 K1 42.865(10) 10_455 13_455 ?
O1 K3 K1 97.762(19) 9_445 13_455 ?
O2 K3 K1 50.23(3) 3 13_455 ?
O2 K3 K1 54.15(3) 4_556 13_455 ?
O2 K3 K1 129.77(3) 2_556 13_455 ?
O2 K3 K1 125.85(3) . 13_455 ?
Nb1 K3 K1 60.199(1) 9_444 13_455 ?
Nb1 K3 K1 119.801(1) 9_445 13_455 ?
O1 K3 K1 42.865(10) 11 5_566 ?
O1 K3 K1 137.135(10) 12_545 5_566 ?
O1 K3 K1 97.762(19) 10_455 5_566 ?
O1 K3 K1 82.238(19) 9_445 5_566 ?
O2 K3 K1 129.77(3) 3 5_566 ?
O2 K3 K1 50.23(3) 4_556 5_566 ?
O2 K3 K1 125.85(3) 2_556 5_566 ?
O2 K3 K1 54.15(3) . 5_566 ?
Nb1 K3 K1 119.801(1) 9_444 5_566 ?
Nb1 K3 K1 60.199(1) 9_445 5_566 ?
K1 K3 K1 104.300(1) 13_455 5_566 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 O1 O2 Nb1 -115.62(2) . . . . ?
K1 O1 O2 Nb1 115.62(2) 13 . . . ?
Nb1 O1 O2 K3 180.0 . . . . ?
K1 O1 O2 K3 64.38(2) . . . . ?
K1 O1 O2 K3 -64.38(2) 13 . . . ?
Nb1 O1 O2 K1 -115.62(2) . . . 13 ?
K1 O1 O2 K1 128.76(4) . . . 13 ?
Nb1 O1 O2 K1 115.62(2) . . . . ?
K1 O1 O2 K1 -128.76(4) 13 . . . ?
Nb1 O1 O2 K1 -74.36(8) . . . 9_545 ?
K1 O1 O2 K1 170.02(8) . . . 9_545 ?
K1 O1 O2 K1 41.26(9) 13 . . 9_545 ?
Nb1 O1 O2 K1 74.36(8) . . . 5_566 ?
K1 O1 O2 K1 -41.26(9) . . . 5_566 ?
K1 O1 O2 K1 -170.02(8) 13 . . 5_566 ?

_refine_diff_density_max         0.162
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.040

####################################################################### 
# 
# 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_BS_NSI01
_database_code_depnum_ccdc_archive 'CCDC 2149737'
loop_
_audit_author_name
_audit_author_address
'Bipul Sarma'
;Tezpur University
India
;
_audit_update_record             
;
2023-06-15 deposited with the CCDC.	2023-06-26 downloaded from the CCDC.
;
_vrf_PLAT430_BS_NSI01            
;
PROBLEM: Short Inter D...A Contact  O13 ..O14   .    2.07 Ang.  
                               x,-1+y,1+z  =      1_546 Check
RESPONSE: O13 and O14 are residual solvent molecules in the lattice
with high degree of thermal disorder.  
;
_vrf_PLAT306_BS_NSI01            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O11 Check
RESPONSE: O11, O12,O13 and O15 are disordered lattice water molecules.
Appropriate assignement of hydrogen atoms on these water oxygens from 
fourier map is not possible, particularly when heavy metal atoms are present.
And fixing such OH and NH hydrogens are not recommended.
Thus these H atoms are not fixed using AFIX command.  
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H30 Nb2 O29'
_chemical_formula_weight         1112.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   22.3770(14)
_cell_length_b                   13.3328(8)
_cell_length_c                   15.5757(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4647.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2699
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      18.65

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_F_000             2240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.588
_shelx_estimated_absorpt_T_min   0.853
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   SADABS
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46157
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_av_R_equivalents  0.1114
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.820
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4522
_reflns_number_gt                2714
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0811P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4522
_refine_ls_number_parameters     310
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1481
_refine_ls_wR_factor_gt          0.1237
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.69790(2) 0.09550(3) 0.15534(2) 0.03442(17) Uani 1 1 d . . . . .
O5 O 0.77498(15) 0.1028(2) 0.08131(19) 0.0454(8) Uani 1 1 d . . . . .
O1 O 0.69163(13) 0.2654(2) 0.15611(17) 0.0387(7) Uani 1 1 d . . . . .
O4 O 0.77210(15) 0.1105(2) 0.23451(19) 0.0427(8) Uani 1 1 d . . . . .
O3 O 0.66500(14) 0.1116(2) 0.2893(2) 0.0411(8) Uani 1 1 d . . . . .
O6 O 0.67089(15) 0.1112(2) 0.0187(2) 0.0443(8) Uani 1 1 d . . . . .
O2 O 0.60724(14) 0.1293(2) 0.15020(19) 0.0429(8) Uani 1 1 d . . . . .
C1 C 0.7711(2) 0.1106(3) -0.0047(3) 0.0397(12) Uani 1 1 d . . . . .
C3 C 0.7050(3) 0.1226(3) -0.1274(3) 0.0463(13) Uani 1 1 d . . . . .
H3 H 0.6665 0.1248 -0.1528 0.056 Uiso 1 1 calc R U . . .
C2 C 0.7120(2) 0.1149(3) -0.0373(3) 0.0395(11) Uani 1 1 d . . . . .
C4 C 0.7547(3) 0.1269(4) -0.1761(3) 0.0522(14) Uani 1 1 d . . . . .
H4 H 0.7499 0.1330 -0.2365 0.063 Uiso 1 1 calc R U . . .
C7 C 0.7045(2) 0.1203(3) 0.3476(3) 0.0368(11) Uani 1 1 d . . . . .
C6 C 0.6942(3) 0.1296(4) 0.4372(3) 0.0465(13) Uani 1 1 d . . . . .
H6 H 0.6547 0.1298 0.4595 0.056 Uiso 1 1 calc R U . . .
C8 C 0.7654(2) 0.1199(3) 0.3196(3) 0.0378(11) Uani 1 1 d . . . . .
C10 C 0.8751(3) 0.1346(5) 0.3546(4) 0.0658(16) Uani 1 1 d . . . . .
H10A H 0.8974 0.1627 0.4030 0.099 Uiso 1 1 calc R U . . .
H10B H 0.8803 0.1776 0.3041 0.099 Uiso 1 1 calc R U . . .
H10C H 0.8901 0.0672 0.3417 0.099 Uiso 1 1 calc R U . . .
C9 C 0.8113(2) 0.1290(4) 0.3768(3) 0.0439(12) Uani 1 1 d . . . . .
C5 C 0.7420(3) 0.1382(4) 0.4901(3) 0.0510(14) Uani 1 1 d . . . . .
H5 H 0.7351 0.1438 0.5501 0.061 Uiso 1 1 calc R U . . .
C12 C 0.5910(2) 0.2251(4) 0.1500(3) 0.0395(11) Uani 1 1 d . . . . .
C11 C 0.6383(2) 0.2977(4) 0.1538(3) 0.0428(12) Uani 1 1 d . . . . .
O7 O 0.51965(18) 0.3555(3) 0.1463(3) 0.0705(12) Uani 1 1 d . . . . .
C15 C 0.6211(3) 0.4015(4) 0.1554(3) 0.0560(15) Uani 1 1 d . . . . .
H15 H 0.6504 0.4530 0.1589 0.067 Uiso 1 1 calc R U . . .
C13 C 0.5331(2) 0.2546(4) 0.1444(3) 0.0531(14) Uani 1 1 d . . . . .
C16 C 0.5626(3) 0.4238(5) 0.1520(4) 0.075(2) Uani 1 1 d . . . . .
H16 H 0.5513 0.4925 0.1536 0.090 Uiso 1 1 calc R U . . .
C17 C 0.4802(3) 0.1885(5) 0.1361(4) 0.0742(18) Uani 1 1 d . . . . .
H17A H 0.4663 0.1888 0.0764 0.111 Uiso 1 1 calc R U . . .
H17B H 0.4482 0.2129 0.1736 0.111 Uiso 1 1 calc R U . . .
H17C H 0.4910 0.1199 0.1527 0.111 Uiso 1 1 calc R U . . .
C18 C 0.8198(3) 0.1132(4) -0.0578(3) 0.0494(13) Uani 1 1 d . . . . .
O9 O 0.8098(2) 0.1232(3) -0.1448(2) 0.0564(11) Uani 1 1 d . . . . .
O8 O 0.79794(17) 0.1392(3) 0.4621(2) 0.0503(9) Uani 1 1 d . . . . .
C20 C 0.8833(2) 0.1114(4) -0.0327(4) 0.0670(17) Uani 1 1 d . . . . .
H20A H 0.8932 0.1736 -0.0024 0.100 Uiso 1 1 calc R U . . .
H20B H 0.9082 0.1054 -0.0841 0.100 Uiso 1 1 calc R U . . .
H20C H 0.8906 0.0540 0.0052 0.100 Uiso 1 1 calc R U . . .
O10 O 0.68508(15) -0.0320(2) 0.15760(19) 0.0464(9) Uani 1 1 d . . . . .
O15 O 0.8614(2) 0.2629(3) 0.1535(3) 0.1002(17) Uani 1 1 d . . . . .
O11 O 0.5230(3) 0.6808(6) 0.1604(5) 0.197(4) Uani 1 1 d . U . . .
O12 O 0.5603(3) 0.0534(5) 0.7739(6) 0.193(3) Uani 1 1 d . U . . .
O13 O 0.5469(5) 0.1048(9) 0.9378(8) 0.283(6) Uani 1 1 d . U . . .
O14 O 0.5600(5) 0.9803(12) 0.0153(10) 0.177(6) Uani 0.5 1 d . U 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
Nb1 O10 1.724(3) . ?
Nb1 O2 2.079(3) . ?
Nb1 O4 2.078(3) . ?
Nb1 O5 2.077(3) . ?
Nb1 O3 2.223(3) . ?
Nb1 O6 2.223(3) . ?
Nb1 O1 2.270(3) . ?
O5 C1 1.347(5) . ?
O1 C11 1.270(5) . ?
O4 C8 1.340(5) . ?
O3 C7 1.273(5) . ?
O6 C2 1.268(6) . ?
O2 C12 1.328(5) . ?
C1 C18 1.369(7) . ?
C1 C2 1.417(7) . ?
C3 C4 1.346(8) . ?
C3 C2 1.416(6) . ?
C3 H3 0.9500 . ?
C4 O9 1.327(7) . ?
C4 H4 0.9500 . ?
C7 C8 1.429(7) . ?
C7 C6 1.420(6) . ?
C6 C5 1.357(7) . ?
C6 H6 0.9500 . ?
C8 C9 1.364(7) . ?
C10 C9 1.472(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C9 O8 1.369(6) . ?
C5 O8 1.325(6) . ?
C5 H5 0.9500 . ?
C12 C13 1.358(7) . ?
C12 C11 1.434(7) . ?
C11 C15 1.437(6) . ?
O7 C16 1.327(8) . ?
O7 C13 1.378(6) . ?
C15 C16 1.344(9) . ?
C15 H15 0.9500 . ?
C13 C17 1.483(7) . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O9 1.380(6) . ?
C18 C20 1.473(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

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
O10 Nb1 O2 92.98(15) . . ?
O10 Nb1 O4 102.46(14) . . ?
O2 Nb1 O4 141.40(12) . . ?
O10 Nb1 O5 101.28(14) . . ?
O2 Nb1 O5 141.14(12) . . ?
O4 Nb1 O5 70.20(13) . . ?
O10 Nb1 O3 91.19(12) . . ?
O2 Nb1 O3 72.08(12) . . ?
O4 Nb1 O3 72.44(12) . . ?
O5 Nb1 O3 142.33(12) . . ?
O10 Nb1 O6 93.86(12) . . ?
O2 Nb1 O6 71.19(12) . . ?
O4 Nb1 O6 140.94(12) . . ?
O5 Nb1 O6 71.92(12) . . ?
O3 Nb1 O6 143.12(13) . . ?
O10 Nb1 O1 166.80(14) . . ?
O2 Nb1 O1 73.98(12) . . ?
O4 Nb1 O1 87.14(11) . . ?
O5 Nb1 O1 90.43(11) . . ?
O3 Nb1 O1 83.02(10) . . ?
O6 Nb1 O1 83.92(10) . . ?
C1 O5 Nb1 120.1(3) . . ?
C11 O1 Nb1 113.3(3) . . ?
C8 O4 Nb1 120.4(3) . . ?
C7 O3 Nb1 116.6(3) . . ?
C2 O6 Nb1 117.6(3) . . ?
C12 O2 Nb1 118.3(3) . . ?
O5 C1 C18 123.5(5) . . ?
O5 C1 C2 114.8(4) . . ?
C18 C1 C2 121.7(4) . . ?
C4 C3 C2 118.1(5) . . ?
C4 C3 H3 121.0 . . ?
C2 C3 H3 121.0 . . ?
O6 C2 C3 127.1(5) . . ?
O6 C2 C1 115.5(4) . . ?
C3 C2 C1 117.4(5) . . ?
O9 C4 C3 123.9(5) . . ?
O9 C4 H4 118.0 . . ?
C3 C4 H4 118.0 . . ?
O3 C7 C8 116.4(4) . . ?
O3 C7 C6 126.5(5) . . ?
C8 C7 C6 117.1(5) . . ?
C5 C6 C7 118.4(5) . . ?
C5 C6 H6 120.8 . . ?
C7 C6 H6 120.8 . . ?
O4 C8 C9 124.7(5) . . ?
O4 C8 C7 114.1(4) . . ?
C9 C8 C7 121.2(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O8 C9 C8 118.6(5) . . ?
O8 C9 C10 115.8(4) . . ?
C8 C9 C10 125.6(5) . . ?
O8 C5 C6 123.1(4) . . ?
O8 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
O2 C12 C13 122.7(5) . . ?
O2 C12 C11 116.6(4) . . ?
C13 C12 C11 120.7(5) . . ?
O1 C11 C15 125.2(5) . . ?
O1 C11 C12 117.7(4) . . ?
C15 C11 C12 117.0(5) . . ?
C16 O7 C13 120.9(5) . . ?
C16 C15 C11 118.2(5) . . ?
C16 C15 H15 120.9 . . ?
C11 C15 H15 120.9 . . ?
C12 C13 O7 119.3(5) . . ?
C12 C13 C17 126.6(5) . . ?
O7 C13 C17 114.1(5) . . ?
O7 C16 C15 123.8(5) . . ?
O7 C16 H16 118.1 . . ?
C15 C16 H16 118.1 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 C18 O9 117.8(5) . . ?
C1 C18 C20 127.3(5) . . ?
O9 C18 C20 114.8(4) . . ?
C4 O9 C18 121.0(4) . . ?
C5 O8 C9 121.6(4) . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_refine_diff_density_max         1.045
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.088

