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_7715243
_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         'C2 H4 K6 N2 Na4 Ni2 O49 Ta10, 2(O)'
_chemical_formula_sum            'C2 H4 K6 N2 Na4 Ni2 O51 Ta10'
_chemical_formula_weight         3125.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-03
_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                 113.4290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.8013(13)
_cell_length_b                   14.1230(3)
_cell_length_c                   20.2049(5)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    149.9
_cell_measurement_theta_max      28.319
_cell_measurement_theta_min      2.632
_cell_volume                     11468.4(5)
_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      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40822
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.197
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    20.203
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1343 before and 0.0790 after correction. The Ratio of minimum to maximum transmission is 0.4849. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             11056
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.506
_refine_diff_density_min         -2.347
_refine_diff_density_rms         0.345
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         10200
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+482.8080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7398
_reflns_number_total             10200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00048j2.cif
_cod_data_source_block           m6817_0m
_cod_depositor_comments
'Adding full bibliography for 7715243--7715244.cif.'
_cod_database_code               7715243
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.688
_shelx_estimated_absorpt_t_min   0.499
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O30)
\\sim Ueq, Uanis(O12W) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O18W) \\sim Ueq, Uanis(O13W) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(Na3)
\\sim Ueq, Uanis(K7) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
3. Others
 Fixed Sof: Na5(0.5) O13W(0.5) O18W(0.5) O19W(0.5) O20W(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
;
_shelx_res_checksum              2345
_shelx_fab_checksum              92303
_olex2_submission_special_instructions 'No special instructions were received'