Synthesis, structures and stability of three V-substituted polyoxoniobate clusters based on [TeNb<sub>9</sub>O<sub>33</sub>]<sup>17-</sup> units.
Yang, Zongfei; Shang, Jingjing; Yang, Yuanyuan; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7610–7620; doi:10.1039/d1dt00223f

data_7707203
_publ_section_title
;
 Synthesis, structures and stability of three V-substituted polyoxoniobate
 clusters based on [TeNb<sub>9</sub>O<sub>33</sub>]<sup>17-</sup> units.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7610
_journal_page_last               7620
_journal_paper_doi               10.1039/d1dt00223f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C9 H30 Cu3 K3 N6 Na4 Nb9 O54 Te V3, Na O6, 2(O)'
_chemical_formula_sum            'C9 H30 Cu3 K3 N6 Na5 Nb9 O62 Te V3'
_chemical_formula_weight         2753.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-25 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                92.939(2)
_cell_angle_beta                 90.728(2)
_cell_angle_gamma                119.9480(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7909(6)
_cell_length_b                   12.8502(5)
_cell_length_c                   24.5446(11)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.267
_cell_measurement_theta_min      2.425
_cell_volume                     3487.6(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            54932
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         2.392
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    3.432
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1372 before and 0.0837 after correction. The Ratio of minimum to maximum transmission is 0.7435. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.622
_exptl_crystal_description       block
_exptl_crystal_F_000             2622
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.555
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         12407
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+23.1348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9784
_reflns_number_total             12407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00223f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7707201--7707203.cif.'
_cod_database_code               7707203
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.627
_shelx_estimated_absorpt_t_min   0.547
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C9-C8 = C8-C7
 1.5 with sigma of 0.01
 C7-N5
 1.47 with sigma of 0.02
 N6-C9
 1.47 with sigma of 0.02
 C7-C8 = C8-C9
 1.5 with sigma of 0.02
 N5-C7
 1.47 with sigma of 0.02
 H7A-H8B_$1
 2.5 with sigma of 0.04
 H7A-H7A_$1
 2.5 with sigma of 0.04
3. Rigid bond restraints
 C9, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C9 \\sim N6 \\sim C8: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C7 \\sim N5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), N5(H5A,H5B), N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B),
 C1(H1C,H1D), C2(H2C,H2D), C3(H3C,H3D), C4(H4C,H4D), C5(H5C,H5D), C6(H6C,H6D),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
;
_shelx_res_checksum              84374
_olex2_submission_special_instructions 'No special instructions were received'