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_7707201
_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
'C40 H32 Cu4 K N8 Nb9 O39 Te V2, 3(O), 2(C H6 N3)'
_chemical_formula_sum            'C42 H44 Cu4 K N14 Nb9 O42 Te V2'
_chemical_formula_weight         2775.84
_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   mixed
_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                63.501(2)
_cell_angle_beta                 71.908(3)
_cell_angle_gamma                84.150(3)
_cell_formula_units_Z            2
_cell_length_a                   15.4162(15)
_cell_length_b                   18.9380(17)
_cell_length_c                   21.0858(19)
_cell_measurement_reflns_used    7359
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.976
_cell_measurement_theta_min      2.405
_cell_volume                     5232.1(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1295
_diffrn_reflns_av_unetI/netI     0.1399
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62433
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         2.163
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    2.295
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1213 before and 0.0817 after correction. The Ratio of minimum to maximum transmission is 0.7464. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.461
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         18559
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0902P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.2055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9272
_reflns_number_total             18559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00223f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7707201--7707203.cif.'
_cod_database_code               7707201
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.670
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 C42-N14
 1.38 with sigma of 0.02
 C22-C23
 1.39 with sigma of 0.02
 C21-C22
 1.39 with sigma of 0.02
 C23-C24
 1.39 with sigma of 0.02
3. Rigid bond restraints
 C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(C42)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Rotating group:
 N10(H10A,H10B), N11(H11A,H11B), N12(H12A,H12B), N13(H13A,H13B), N14(H14A,H14B)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C24(H24), C1(H1), C2(H2), C3(H3), C4(H4),
 C8(H8), C7(H7), C10(H10), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C20(H20), C27(H27), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40)
5.c Fitted hexagon refined as free rotating group:
 N5(C21,C22,C23,C24,C25), C8(C7,C6,N2,C10,C9)
5.d X=CH2 refined with riding coordinates:
 N9(H9A,H9B)
;
_shelx_res_checksum              95682
_shelx_fab_checksum              30020
_olex2_submission_special_instructions 'No special instructions were received'