Oxalate-assisted assembly of two polyoxotantalate supramolecular frameworks with proton conduction properties.
Yu, Yong; Lai, Rong-Da; Sun, Cai; Sun, Yan-Qiong; Zeng, Qing-Xin; Li, Xin-Xiong; Zheng, Shou-Tian; Chemical communications (Cambridge, England) 59 (2023) 3735–3738; doi:10.1039/d2cc07027h

data_7131364
_publ_section_title
;
 Oxalate-assisted assembly of two polyoxotantalate supramolecular
 frameworks with proton conduction properties.
;
_journal_issue                   25
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3735
_journal_page_last               3738
_journal_paper_doi               10.1039/d2cc07027h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety
'C8 H28 Co4 N4 O52 Ta12, 3(C6 H24 Co N6), C2 O4, C4 H15 Co N5 O, 9(O), 32[H2O]'
_chemical_formula_sum            'C32 H177 Co8 N26 O98 Ta12'
_chemical_formula_weight         5137.83
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-03-02 deposited with the CCDC.	2023-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.348(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.6228(8)
_cell_length_b                   31.5888(7)
_cell_length_c                   15.5673(3)
_cell_measurement_reflns_used    17031
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.4260
_cell_measurement_theta_min      2.0330
_cell_volume                     15344.1(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      175
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.797
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -68.00   7.00   0.12   15.00    --   -5.30 -57.00  30.00  625
  2  \w    -76.00  -4.00   0.12   15.00    --   -5.30 -77.00 -60.00  600
  3  \w    -17.00  16.00   0.12   15.00    --   -5.30  57.00  60.00  275
  4  \w    -18.00  14.28   0.12   15.00    --    6.55 -99.00 -60.00  269
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0040629000
_diffrn_orient_matrix_UB_12      -0.0142134000
_diffrn_orient_matrix_UB_13      0.0329808000
_diffrn_orient_matrix_UB_21      -0.0001768000
_diffrn_orient_matrix_UB_22      0.0172217000
_diffrn_orient_matrix_UB_23      0.0291962000
_diffrn_orient_matrix_UB_31      -0.0223585000
_diffrn_orient_matrix_UB_32      0.0024448000
_diffrn_orient_matrix_UB_33      -0.0138613000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.797
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55766
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.754
_diffrn_reflns_theta_min         2.041
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.224
_exptl_crystal_description       block
_exptl_crystal_F_000             9708
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL 1A  in C2/c
CELL   31.6228   31.5888   15.5673     90.00     99.35     90.00
SPGR C2/c
Q101 0.233 0.468 0.132 !       4.77 eA-3
Q102 0.969 0.220 0.452 !       4.67 eA-3
Q103 0.469 0.720 0.452 !       4.67 eA-3
C104 0.923 0.172 0.098 !       4.47 eA-3
C105 0.954 0.190 0.065 !       4.45 eA-3
Q106 0.663 0.072 0.160 !       4.36 eA-3
C107 0.700 0.063 0.470 !       4.29 eA-3
C108 0.227 0.452 0.089 !       3.93 eA-3
C109 0.336 0.929 0.572 !       3.66 eA-3
C110 0.836 0.429 0.572 !       3.66 eA-3
C111 0.664 0.930 0.916 !       3.66 eA-3
Q112 0.687 0.199 0.099 !       3.41 eA-3
C113 0.921 0.455 0.486 !       3.27 eA-3
C114 0.126 0.501 0.374 !       3.05 eA-3
Q115 0.798 0.345 0.050 !       3.02 eA-3
C116 0.097 0.298 0.337 !       3.00 eA-3
C117 0.499 0.273 0.315 !       2.98 eA-3
Q118 0.857 0.190 0.566 !       2.94 eA-3
C119 0.936 0.216 0.214 !       2.89 eA-3
C120 0.923 0.365 0.248 !       2.88 eA-3
C121 0.468 0.226 0.201 !       2.84 eA-3
Q122 0.219 0.247 0.389 !       2.82 eA-3
C123 0.964 0.407 0.065 !       2.76 eA-3
Q124 0.700 0.267 0.260 !       2.73 eA-3
Q125 0.142 0.497 0.127 !       2.73 eA-3
Q126 0.280 0.272 0.464 !       2.72 eA-3
C127 0.990 0.452 0.171 !       2.71 eA-3
C128 0.023 0.311 0.104 !       2.71 eA-3
C129 0.010 0.454 0.327 !       2.71 eA-3
Q130 0.655 0.311 0.387 !       2.71 eA-3
Q131 0.851 0.177 0.755 !       2.67 eA-3
C132 0.008 0.280 0.115 !       2.66 eA-3
C133 0.446 0.232 0.455 !       2.66 eA-3
C134 0.021 0.410 0.912 !       2.65 eA-3
Q135 0.861 0.336-0.002 !       2.64 eA-3
Q136 0.425 0.238 0.369 !       2.63 eA-3
C137 0.071 0.307 0.294 !       2.63 eA-3
C138 0.039 0.359 0.803 !       2.63 eA-3
Q139 0.888 0.743 0.260 !       2.61 eA-3
Q140 0.388 0.243 0.260 !       2.61 eA-3
Q141 0.360 0.422 0.222 !       2.61 eA-3
C142 0.566 0.023 0.558 !       2.61 eA-3
Q143 0.733 0.266 0.373 !       2.59 eA-3
C144 1.001 0.317 0.434 !       2.57 eA-3
Q145 0.900 0.307 0.293 !       2.57 eA-3
C146 0.446 0.272 0.866 !       2.57 eA-3
C147 0.446 0.077 0.474 !       2.55 eA-3
Q148 0.580 0.173 0.088 !       2.55 eA-3
Q149 0.763 0.237 0.688 !       2.54 eA-3
Q150 0.181 0.413 0.941 !       2.54 eA-3
C151 0.508 0.150 0.127 !       2.53 eA-3
Q152 0.986 0.180 0.139 !       2.51 eA-3
Q153 0.888 0.192 0.683 !       2.49 eA-3
C154 0.986 0.447 0.265 !       2.45 eA-3
C155 0.455 0.127 0.579 !       2.44 eA-3
Q156 0.053 0.341 0.839 !       2.43 eA-3
Q157 0.369 0.406 0.244 !       2.42 eA-3
C158 0.065 0.359 0.465 !       2.42 eA-3
Q159 0.932 0.389 0.232 !       2.42 eA-3
C160 0.403 0.236 0.812 !       2.41 eA-3
Q161 0.735 0.483 0.126 !       2.40 eA-3
Q162 0.879 0.462 0.856 !       2.40 eA-3
Q163 0.624 0.305 0.472 !       2.39 eA-3
Q164 0.805 0.228 0.044 !       2.39 eA-3
Q165 0.747 0.148 0.496 !       2.39 eA-3
Q166 0.488 0.249 0.168 !       2.39 eA-3
Q167 0.700 0.370 0.421 !       2.38 eA-3
C168 0.009 0.306 0.237 !       2.38 eA-3
C169 0.491 0.194 0.763 !       2.38 eA-3
C170 0.962 0.416 0.377 !       2.37 eA-3
C171 0.065 0.387 0.357 !       2.37 eA-3
C172 0.446 0.056 0.951 !       2.37 eA-3
C173 0.376 0.049 0.047 !       2.36 eA-3
Q174 0.560 0.311 0.688 !       2.36 eA-3
Q175 0.420 0.314 0.684 !       2.36 eA-3
C176 0.600 0.093 0.091 !       2.35 eA-3
C177 0.606 0.041 0.497 !       2.34 eA-3
Q178 0.092 0.243 0.079 !       2.34 eA-3
C179 0.023 0.463 0.089 !       2.34 eA-3
C180 0.477 0.037 0.911 !       2.34 eA-3
C181 0.974 0.398 0.434 !       2.34 eA-3
C182 0.477 0.262 0.296 !       2.34 eA-3
Q183 0.944 0.252 0.908 !       2.33 eA-3
C184 0.460 0.204 0.139 !       2.33 eA-3
Q185 0.905 0.390 0.251 !       2.32 eA-3
Q186 0.337 0.303 0.293 !       2.32 eA-3
Q187 0.868 0.288 0.308 !       2.31 eA-3
Q188 0.283 0.357 0.251 !       2.31 eA-3
C189 0.540 0.017 0.266 !       2.31 eA-3
C190 0.454 0.180 0.702 !       2.30 eA-3
Q191 0.361 0.287 0.340 !       2.28 eA-3
Q192 0.124 0.322 0.369 !       2.28 eA-3
Q193 0.865 0.482 0.153 !       2.28 eA-3
Q194 0.069 0.303 0.895 !       2.27 eA-3
C195 0.538 0.052 0.034 !       2.27 eA-3
Q196 0.336 0.103 0.017 !       2.27 eA-3
C197 0.397 0.062 0.110 !       2.26 eA-3
Q198 0.273 0.379 0.283 !       2.26 eA-3
Q199 0.766 0.361 0.279 !       2.26 eA-3
;
_refine_diff_density_max         3.204
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.306
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         19080
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0753P)^2^+297.9199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14090
_reflns_number_total             19080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc07027h2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7131363--7131364.cif.'
_cod_database_code               7131364
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ta O Co C N'
_shelx_estimated_absorpt_t_max   0.452
_shelx_estimated_absorpt_t_min   0.313
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C16-C17 = C18-C15
 1.53 with sigma of 0.01
 C17-N15 = C16-N12 = C15-N13
 1.48 with sigma of 0.02
 C10-C10_$4 = C9-C14_$3
 1.53 with sigma of 0.01
 O11-Co5 = O11-Co5_$1
 2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C16 \\sim C17 \\sim C18
\\sim C15 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim
N8 \\sim N9 \\sim N10 \\sim N11 \\sim N12 \\sim N13 \\sim N15 \\sim N14 \\sim
O11 \\sim O2W \\sim O1W: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(N8)
\\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(N11) \\sim Ueq,
Uanis(N12) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(N14)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O1W) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Co5(0.5) N12(0.5) N13(0.5) H13C(0.5) H13D(0.5) N15(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 C15(0.5) H15A(0.5) H15B(0.5) O11(0.5) H11(0.5) O4W(0.75) O6W(0.5) O7W(0.5)
 O8W(0.75)
 Fixed X: H2C(0.13602) H2D(0.11693) H1WA(0.155201) H1WB(0.18993)
 Fixed Y: H2C(0.09372) H2D(0.06545) H1WA(0.174439) H1WB(0.15267)
 Fixed Z: H2C(0.09849) H2D(0.015221) H1WA(0.15966) H1WB(0.10498)
5.a Riding coordinates:
 O11(H11)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 N7(H7A,H7B), N8(H8C,H8D), N9(H9A,H9B), N10(H10A,H10B), N11(H11A,H11B), C3(H3C,
 H3D), C4(H4C,H4D), C6(H6C,H6D), C7(H7C,H7D), C8(H8A,H8B), C9(H9C,H9D),
 C11(H11C,H11D), C12(H12A,H12B), C13(H13A,H13B), C14(H14C,H14D), N13(H13C,H13D),
  C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C15(H15A,H15B), N14(H14A,H14B)
5.c X=CH2 refined with riding coordinates:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.921
_oxdiff_exptl_absorpt_empirical_full_min 0.697
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              82625