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_7131363
_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
'C4 H16 Co2 N4 O38 Ta12, 4(C6 H24 Co N6), C2 O4, 14(O), 52[H2O]'
_chemical_formula_sum            'C30 H218 Co6 N28 O111 Ta12'
_chemical_formula_weight         5273.29
_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             2023-03-02
_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                 118.206(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.181(13)
_cell_length_b                   18.194(6)
_cell_length_c                   24.574(9)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    175
_cell_measurement_theta_max      25.71
_cell_measurement_theta_min      2.49
_cell_volume                     14650(9)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_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_temperature      175
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31830
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.882
_diffrn_reflns_theta_min         1.881
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    9.696
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1001 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.6315.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.391
_exptl_crystal_description       block
_exptl_crystal_F_000             10080
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
TITL 2A in C2/c
CELL   37.1810   18.1940   24.5740     90.00    118.21     90.00
SPGR C2/c
C101 1.000 0.203 0.749 !       6.12 eA-3
Q102 0.218 0.420 0.268 !       5.87 eA-3
C103 0.280 0.040 0.438 !       5.48 eA-3
C104 0.094 0.328 0.074 !       4.59 eA-3
C105 0.869 0.266 0.307 !       4.49 eA-3
C106 0.646 0.045 0.070 !       4.19 eA-3
C107 0.401 0.218 0.416 !       4.12 eA-3
Q108 0.834 0.175 0.139 !       3.84 eA-3
C109 0.691 0.264 0.016 !       3.82 eA-3
C110 0.741 0.332 0.947 !       3.82 eA-3
C111 0.615 0.083 0.501 !       3.76 eA-3
Q112 0.173 0.065 0.252 !       3.65 eA-3
Q113 1.000 0.172 0.252 !       3.38 eA-3
C114 0.788 0.504 0.034 !       3.37 eA-3
C115 0.418 0.161 0.275 !       3.28 eA-3
C116 0.196 0.389 0.252 !       3.27 eA-3
C117 0.952 0.472 0.367 !       3.23 eA-3
C118 0.447 0.200 0.285 !       3.16 eA-3
C119 0.584 0.077 0.322 !       3.15 eA-3
C120 0.033 0.341 0.301 !       3.10 eA-3
Q121 0.661 0.485 0.111 !       2.99 eA-3
C122 0.641 0.109 0.070 !       2.82 eA-3
Q123 0.190 0.190 0.492 !       2.79 eA-3
C124 0.865 0.233 0.231 !       2.78 eA-3
Q125 0.619 0.342 0.615 !       2.69 eA-3
C126 0.188 0.571 0.484 !       2.66 eA-3
C127 0.688 0.071 0.484 !       2.66 eA-3
C128 0.975 0.420 0.110 !       2.63 eA-3
Q129 0.617 0.186-0.003 !       2.62 eA-3
C130 0.855 0.247 0.244 !       2.60 eA-3
C131 0.946 0.392 0.909 !       2.60 eA-3
C132 0.508 0.140 0.391 !       2.60 eA-3
C133 0.087 0.373 0.388 !       2.58 eA-3
C134 0.123 0.312 0.297 !       2.57 eA-3
C135 0.967 0.314 0.231 !       2.57 eA-3
C136 0.489 0.032 0.041 !       2.55 eA-3
Q137 0.893 0.346 0.780 !       2.53 eA-3
C138 0.960 0.456 0.412 !       2.49 eA-3
C139 0.423 0.048 0.212 !       2.47 eA-3
C140 0.594 0.065 0.486 !       2.47 eA-3
C141 0.907 0.437 0.457 !       2.42 eA-3
C142 0.087 0.465 0.428 !       2.36 eA-3
C143 0.439 0.077 0.139 !       2.35 eA-3
Q144 0.578 0.500 0.199 !       2.34 eA-3
C145 0.591 0.150 0.012 !       2.33 eA-3
C146 0.880 0.345 0.295 !       2.32 eA-3
Q147 0.174 0.314 0.376 !       2.30 eA-3
C148 0.812 0.456 0.012 !       2.29 eA-3
C149 0.551 0.189 0.810 !       2.27 eA-3
Q150 0.804 0.467 0.393 !       2.26 eA-3
C151 0.951 0.425 0.376 !       2.25 eA-3
Q152 0.899 0.468 0.791 !       2.24 eA-3
C153 0.172 0.455 0.554 !       2.24 eA-3
C154 0.633 0.093 0.428 !       2.23 eA-3
Q155 0.525 0.218 0.077 !       2.21 eA-3
C156 0.622 0.028 0.407 !       2.18 eA-3
Q157 0.298 0.017 0.402 !       2.17 eA-3
C158 0.032 0.420 0.515 !       2.16 eA-3
Q159 0.967 0.343 0.942 !       2.16 eA-3
C160 1.000 0.344 0.251 !       2.16 eA-3
C161 0.055 0.452 0.871 !       2.15 eA-3
C162 0.539 0.157 0.099 !       2.15 eA-3
Q163 0.537 0.188 0.125 !       2.13 eA-3
Q164 0.888 0.044 0.274 !       2.12 eA-3
C165 0.365 0.109 0.040 !       2.12 eA-3
C166 0.539 0.032 0.974 !       2.09 eA-3
Q167 0.451 0.140 0.813 !       2.08 eA-3
C168 0.094 0.486 0.198 !       2.08 eA-3
C169 0.885 0.435 0.637 !       2.08 eA-3
C170 0.048 0.408 0.206 !       2.07 eA-3
C171 0.116 0.466 0.828 !       2.07 eA-3
C172 0.415 0.095 0.228 !       2.06 eA-3
C173 0.494 0.141 0.189 !       2.05 eA-3
Q174 0.789 0.142 0.752 !       2.05 eA-3
C175 0.412 0.170 0.753 !       2.04 eA-3
Q176 0.851 0.046 0.386 !       2.04 eA-3
C177 0.345 0.169 0.664 !       2.04 eA-3
Q178 0.982 0.111 0.841 !       2.04 eA-3
C179 0.633 0.017 0.374 !       2.04 eA-3
Q180 0.610 0.172 0.184 !       2.03 eA-3
Q181 0.885 0.345 0.469 !       2.03 eA-3
Q182 0.396 0.390 0.525 !       2.03 eA-3
C183 0.397 0.016 0.246 !       2.01 eA-3
Q184 0.905 0.468 0.828 !       2.01 eA-3
Q185 0.637 0.294 0.821 !       2.01 eA-3
C186 0.976 0.469 0.826 !       2.01 eA-3
C187 0.070 0.471 0.884 !       2.01 eA-3
C188 0.392 0.061 0.223 !       2.00 eA-3
C189 0.882 0.247 0.277 !       2.00 eA-3
Q190 0.820 0.404 0.176 !       2.00 eA-3
C191 0.989 0.498 0.228 !       2.00 eA-3
Q192 0.070 0.031 0.153 !       1.99 eA-3
C193 0.920 0.344 0.225 !       1.99 eA-3
Q194 0.469 0.329 0.705 !       1.98 eA-3
Q195 0.648 0.219 0.078 !       1.97 eA-3
Q196 0.340 0.377 0.422 !       1.97 eA-3
C197 0.009 0.312 0.279 !       1.95 eA-3
C198 0.907 0.442 0.293 !       1.95 eA-3
Q199 0.253 0.326 0.438 !       1.94 eA-3
;
_refine_diff_density_max         3.544
_refine_diff_density_min         -2.450
_refine_diff_density_rms         0.308
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         13203
_refine_ls_number_restraints     306
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0723P)^2^+653.8829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9663
_reflns_number_total             13203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc07027h2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7131363--7131364.cif.'
_cod_original_cell_volume        14649(9)
_cod_database_code               7131363
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.324
_shelx_estimated_absorpt_t_min   0.037
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. 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 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 N14: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 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(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(N14) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N11) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O5W(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1C,H1D), N2(H2A,H2B), N3(H3C,H3D), N4(H4A,H4B), N5(H5C,H5D), N6(H6A,H6B),
 N7(H7C,H7D), N8(H8A,H8B), N9(H9A,H9B), N10(H10A,H10B), N11(H11A,H11B),
 N12(H12A,H12B), N13(H13A,H13B), N14(H14A,H14B), C1(H1A,H1B), C2(H2C,H2D),
 C3(H3A,H3B), C4(H4C,H4D), C5(H5A,H5B), C6(H6C,H6D), C7(H7A,H7B), C8(H8C,H8D),
 C9(H9C,H9D), C11(H11C,H11D), C12(H12C,H12D), C13(H13C,H13D), C14(H14C,H14D),
 C15(H15A,H15B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              91165