Hexameric Polyoxotantalate with Proton Conduction Property
Chen, Hanhan; Zhang, Mingyang; Li, Yuyan; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Chemical Communications  (2023) –; doi:10.1039/D3CC03645F

data_7132009
_publ_section_title
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 Hexameric Polyoxotantalate with Proton Conduction Property
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03645F
_journal_year                    2023
_chemical_formula_moiety
'Fe10.7 H183.8 K12 Na14 O214.2 Ta37.3, 11(H2 O), 0.8(O), 20.5[H2O]'
_chemical_formula_sum            'Fe10.7 H248.4 K12 Na14 O246.5 Ta37.3'
_chemical_formula_weight         12332.47
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-25 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                113.52(2)
_cell_angle_beta                 94.90(2)
_cell_angle_gamma                113.32(3)
_cell_formula_units_Z            1
_cell_length_a                   18.011(18)
_cell_length_b                   19.645(19)
_cell_length_c                   20.630(17)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.287
_cell_measurement_theta_min      2.349
_cell_volume                     5884(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 v2019.11-0 (Bruker-AXS, 2019)'
_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 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  0.0504
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            127309
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.978
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    18.260
_exptl_absorpt_correction_T_max  0.0479
_exptl_absorpt_correction_T_min  0.0230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0757 before and 0.0626 after correction. The Ratio of minimum to maximum transmission is 0.4802. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.481
_exptl_crystal_description       block
_exptl_crystal_F_000             5604
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.524
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1435
_refine_ls_number_reflns         21832
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0206P)^2^+58.2951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18765
_reflns_number_total             21832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03645f2.cif
_cod_data_source_block           2245515
_cod_original_cell_volume        5883(9)
_cod_original_formula_sum        'Fe10.70 H248.40 K12 Na14 O246.50 Ta37.30'
_cod_database_code               7132009
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.361
_shelx_estimated_absorpt_t_min   0.262
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H,H) groups
2. Shared sites
{Ta19, Fe6}
3. Restrained distances
 H35B-H42B_$2 = H36B-H42A_$2
 2.2 with sigma of 0.01
 H12A-H34A_$1
 2.2 with sigma of 0.01
 O43W-H43A = O43W-H43B = O7W-H7WA = O7W-H7WB
 0.82 with sigma of 0.01
 H5WB-H38A = H5WB-H38B = H8WB-H20A = H8WB-H20B
 2.2 with sigma of 0.02
 H8WA-H40A
 2.25 with sigma of 0.02
4. Rigid bond restraints
 O43W, Na5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O43W \\sim Na5: within 2.5A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O30) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O20W) \\sim Ueq, Uanis(O30W)
\\sim Ueq, Uanis(O39W) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O34W)
\\sim Ueq, Uanis(O38W) \\sim Ueq, Uanis(O37W) \\sim Ueq, Uanis(O43W) \\sim Ueq,
Uanis(O36W) \\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O7W) \\sim Ueq, Uanis(O11W)
\\sim Ueq, Uanis(O35W) \\sim Ueq, Uanis(O40W) \\sim Ueq, Uanis(O41W) \\sim Ueq,
Uanis(K5) \\sim Ueq, Uanis(Na6) \\sim Ueq, Uanis(K5B) \\sim Ueq, Uanis(O45W)
\\sim Ueq, Uanis(O46W) \\sim Ueq, Uanis(O47W) \\sim Ueq, Uanis(O48W) \\sim Ueq,
Uanis(O2BW) \\sim Ueq, Uanis(O50W) \\sim Ueq, Uanis(O52W) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(Ta19) = Uanis(Fe6)
6. Others
 Fixed Sof: Ta19(0.65) Fe6(0.35) K5(0.7) K5B(0.3) O22W(0.6) O30W(0.6)
 H30A(0.6) H30B(0.6) H45A(0.7) H45B(0.7) H45C(0.3) H45D(0.3) O46W(0.5)
 H46A(0.5) H46B(0.5) O47W(0.6) O52W(0.4) O48W(0.5) H48A(0.5) H48B(0.5)
 O2BW(0.4) O50W(0.5) H50A(0.5) H50B(0.5) O3BW(0.4) H3BA(0.4) H3BB(0.4) O39W(0.5)
7.a Riding coordinates:
 O45W(H45A,H45B), O45W(H45C,H45D)
7.b Rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O7W(H7WA,
 H7WB), O8W(H8WA,H8WB), O10W(H10A,H10B), O13W(H13A,H13B), O20W(H20A,H20B),
 O21W(H21A,H21B), O23W(H23A,H23B), O30W(H30A,H30B), O46W(H46A,H46B), O32W(H32A,
 H32B), O33W(H33A,H33B), O34W(H34A,H34B), O35W(H35A,H35B), O36W(H36A,H36B),
 O43W(H43A,H43B), O42W(H42A,H42B), O40W(H40A,H40B), O48W(H48A,H48B), O12W(H12A,
 H12B), O41W(H41A,H41B), O31W(H31A,H31B), O37W(H37A,H37B), O49W(H49A,H49B),
 O38W(H38A,H38B), O50W(H50A,H50B), O3BW(H3BA,H3BB)
;
_smtbx_masks_special_details
;
 Highly disordered solvent was located in the structures.
 Reflection contributions from this solvent were removed
 using program OLEX2, function MSAKS, which determined
 there to be 205.6 electrons in 550.4 \%A^3^ removed per unit cell. 
 This is consistent with the presence of 20.5[H2O] per formula unit
 which account for 205 electrons.
 Therefore, there are about 20.5[H2O] molecules
 were added to the chemical formulas.
 Thus all reported items that derive from the molecular formula
 (<i>e.g.</i>, <i>F</i>(000), density, molecular weight,
 <i>etc</i>.) are inconsistent with the calculated values.
;
_shelx_res_checksum              78357
_shelx_hkl_checksum              54015
_shelx_fab_checksum              57306
_olex2_submission_special_instructions 'No special instructions were received'