Two binuclear Ni-inserted polyoxotantalates based on {NiTa10O32} units with catalytic activity
Zhao, Hui; Chen, Hanhan; yang Zhang, Ming; Yang, Yuanyuan; Yang, Zongfei; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton Transactions 53 (2024) 5562–5566; doi:10.1039/D4DT00048J

data_7715244
_publ_section_title
;
 Two binuclear Ni-inserted polyoxotantalates based on {NiTa10O32} units
 with catalytic activity
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              5562
_journal_page_last               5566
_journal_paper_doi               10.1039/D4DT00048J
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '0.5(K22 Na8 Ni8 O196 Ta40), 19(O)'
_chemical_formula_sum            'K11 Na4 Ni4 O117 Ta20'
_chemical_formula_weight         6247.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-18 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.159(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.2839(12)
_cell_length_b                   14.1700(8)
_cell_length_c                   27.1565(17)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.270
_cell_measurement_theta_min      2.529
_cell_volume                     6944.8(7)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0574
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            23237
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         2.257
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    16.648
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1414 before and 0.0945 after correction. The Ratio of minimum to maximum transmission is 0.4736. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.988
_exptl_crystal_description       block
_exptl_crystal_F_000             5522
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.735
_refine_diff_density_min         -4.479
_refine_diff_density_rms         0.616
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6411
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1419P)^2^+994.3566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2332
_refine_ls_wR_factor_ref         0.2417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5427
_reflns_number_total             6411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00048j2.cif
_cod_data_source_block           m7462_0m
_cod_depositor_comments
'Adding full bibliography for 7715243--7715244.cif.'
_cod_database_code               7715244
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.490
_shelx_estimated_absorpt_t_min   0.121
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O18) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O19)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(O8) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O9) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O21)
\\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
2. Others
 Fixed Sof: O14W(0.25) O15W(0.5) O16W(0.5)
;
_shelx_res_checksum              37776
_olex2_submission_special_instructions 'No special instructions were received'