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_7707202
_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
'C6 H24 Cu3 K5 N6 Na1.5 Nb9 O50 Te V3, Na O6, 4.5(O)'
_chemical_formula_sum            'C6 H24 Cu3 K5 N6 Na2.5 Nb9 O60.5 Te V3'
_chemical_formula_weight         2708.52
_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             2020-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-01 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                79.580(16)
_cell_angle_beta                 82.368(16)
_cell_angle_gamma                60.151(9)
_cell_formula_units_Z            2
_cell_length_a                   12.824(4)
_cell_length_b                   12.873(5)
_cell_length_c                   27.492(14)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.299
_cell_measurement_theta_min      2.181
_cell_volume                     3867(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      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            48854
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.262
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    3.185
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1053 before and 0.0628 after correction. The Ratio of minimum to maximum transmission is 0.8550. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.326
_exptl_crystal_description       block
_exptl_crystal_F_000             2571
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.363
_refine_diff_density_min         -2.126
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         13753
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0368P)^2^+52.4680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11722
_reflns_number_total             13753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00223f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7707201--7707203.cif.'
_cod_original_formula_sum        'C6 H24 Cu3 K5 N6 Na2.50 Nb9 O60.50 Te V3'
_cod_database_code               7707202
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.598
_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
 O23W-O23W_$1
 2.65 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O16W) \\sim Ueq, Uanis(O16B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O16W(0.5) O20W(0.5) O21W(0.5) O22W(0.5) O23W(0.5) O16B(0.5)
 O24W(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 N1(H1C,H1D), N2(H2C,H2D), N3(H3C,H3D), N4(H4C,H4D), N5(H5C,H5D), N6(H6C,H6D)
;
_shelx_res_checksum              27785
_shelx_fab_checksum              32427
_olex2_submission_special_instructions 'No special instructions were received'