A 3D heteropolyoxoniobate framework based on heart-shaped {Te<sub>2</sub>Nb<sub>19</sub>O<sub>60</sub>} clusters with proton conductivity property.
Wu, Ping-Xin; Han, Yue; Lin, Yu-Jin; Sun, Yan-Qiong; Zheng, Shou-Tian; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7424–7429; doi:10.1039/d4dt00386a

data_7715568
_publ_section_title
;
 A 3D heteropolyoxoniobate framework based on heart-shaped
 {Te<sub>2</sub>Nb<sub>19</sub>O<sub>60</sub>} clusters with proton
 conductivity property.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7424
_journal_page_last               7429
_journal_paper_doi               10.1039/d4dt00386a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C8 H48 Cu2 K1.6 N8 Na0.4 Nb19 O68 Te2, C1.46 H10.91 Cu N1.46 O2.54, H12 K1.4 Na0.6 O6, 4(H2 O), 0.5(H2 O2)'
_chemical_formula_sum            'C9.45 H79.91 Cu3 K3 N9.45 Na Nb19 O81.54 Te2'
_chemical_formula_weight         3982.69
_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
_audit_creation_date             2024-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.516(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.108(9)
_cell_length_b                   15.854(5)
_cell_length_c                   25.997(8)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    175.00(10)
_cell_measurement_theta_max      25.014
_cell_measurement_theta_min      2.537
_cell_volume                     11215(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXTL (Bruker, 2013)'
_diffrn_ambient_temperature      175.00(10)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28294
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.021
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_min         1.487
_exptl_absorpt_coefficient_mu    3.138
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0546 before and 0.0423 after correction.
The Ratio of minimum to maximum transmission is 0.8988.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.359
_exptl_crystal_description       block
_exptl_crystal_F_000             7573
_exptl_crystal_recrystallization_method
'The crystals were growth by means of evaporation of a mixture of n-hexane and toluene at RT.'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.219
_refine_diff_density_min         -4.462
_refine_diff_density_rms         0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         9807
_refine_ls_number_restraints     775
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0883P)^2^+563.2802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8393
_reflns_number_total             9807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00386a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7715568.cif.'
_cod_database_code               7715568
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.573
_shelx_estimated_absorpt_t_min   0.508
_exptl_crystal_mounting_method
'Crystals were removed from the crystallisation vial and immediately coated with polybutenes oil (CAS: 9003-29-6) on a glass slide. A suitable single crystal coated with polybutenes oil as less as possible was sealed in capillary tube filled with argon. The capillary tube with single crystal was mounted on copper pin with solid paraffin.'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H,H) groups
2. Shared sites
{K1, Na1}
{K2, Na2}
3. Restrained distances
 H8WB-O4W
 1.8 with sigma of 0.1
 C5-N5
 1.45 with sigma of 0.1
 C15-N8
 1.45 with sigma of 0.1
 H8WB-H4WB
 2.1 with sigma of 0.1
 H1W_$1-H1W
 1.45 with sigma of 0.1
 H2WA-O9W
 1.8 with sigma of 0.1
 H10A-N2
 2.1 with sigma of 0.1
 H4WB-H8WB
 2.2 with sigma of 0.02
 H10B-O5W
 1.9 with sigma of 0.02
 H7WA-O23
 1.8 with sigma of 0.1
 H1W-O18
 1.8 with sigma of 0.1
 H3WB-H8WA
 2.12 with sigma of 0.02
 K3-H3WB \\sim K3-H3WA
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O7W: within 0.8A with sigma of 0.04 and sigma for terminal atoms of 0.08
O1 \\sim O2 \\sim O2W \\sim O3 \\sim O3W \\sim O4 \\sim O4W \\sim O5 \\sim O5W
\\sim O6 \\sim O6W \\sim O7 \\sim O7W \\sim O8 \\sim O9 \\sim O9W \\sim O10
\\sim O10W \\sim O11 \\sim O11W \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim
O16 \\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim
O24 \\sim O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O8W \\sim
O1W \\sim O32: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02
N5 \\sim O33 \\sim O34 \\sim N8 \\sim C5 \\sim C15 \\sim Cu2: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
O1 \\sim O2 \\sim O2W \\sim O3 \\sim O3W \\sim O4 \\sim O4W \\sim O5 \\sim O5W
\\sim O6 \\sim O6W \\sim O7 \\sim O7W \\sim O8 \\sim O9 \\sim O9W \\sim O10
\\sim O10W \\sim O11 \\sim O11W \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim
O16 \\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim
O24 \\sim O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O8W \\sim
O1W \\sim O32 \\sim O33 \\sim O34: within 3.8A with sigma of 0.001 and sigma
for terminal atoms of 0.002
O31: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O9W) \\sim Ueq, Uanis(O10W) \\sim Ueq, Uanis(O11W) \\sim Ueq, Uanis(O5W)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.0025
Uanis(O4W) \\sim Ueq, Uanis(O6W) \\sim Ueq, Uanis(O19) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.005
Uanis(O31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K1) = Uanis(Na1)
Uanis(K2) = Uanis(Na2)
5. Rigid body (RIGU) restrains
 O9W, O31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(O33)=Sof(H33A)=Sof(H33B)=Sof(O34)=Sof(H34A)=Sof(H34B)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(N5)=Sof(H5C)=Sof(H5D)=Sof(N8)=Sof(H8A)=Sof(H8B)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=FVAR(1)
 Fixed Sof: O5W(0.5) H5WA(0.4) H5WB(0.4) H5WC(0.1) H5WD(0.1) O9W(0.65)
 H9WA(0.65) H9WB(0.65) O10W(0.5) H10A(0.5) H10B(0.5) O11W(0.5) H11A(0.4)
 H11B(0.4) H11C(0.1) H11D(0.1) K1(0.3) K2(0.7) K3(0.5) Na1(0.2) H1W(0.5)
 O32(0.5) H32A(0.5) H32B(0.5) Na2(0.3) O31(0.35) H31A(0.35) H31B(0.35)
 Fixed X: O5W(-0.30941) O10W(-0.32013) C15(-0.406899) O1W(-0.5) O32(-0.632299)
 Fixed Y: O5W(-0.15277) O10W(-0.033791) C15(0.5563) O1W(-0.10224) O32(0.1564)
 Fixed Z: O5W(0.10648) O10W(0.121011) C15(0.0348) O1W(0.25) O32(-0.019401)
7.a Riding coordinates:
 O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB,H5WC,H5WD), O6W(H6WA,H6WB),
 O7W(H7WA,H7WB), O9W(H9WA,H9WB), O10W(H10A,H10B), O11W(H11A,H11B,H11C,H11D),
 O8W(H8WA,H8WB), O32(H32A,H32B), O34(H34A,H34B), O31(H31A,H31B)
7.b Free rotating group:
 O1W(H1W)
7.c Rotating group:
 O2W(H2WA,H2WB), O33(H33A,H33B)
7.d Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), N1(H1C,H1D),
 N2(H2C,H2D), N3(H3C,H3D), N4(H4C,H4D), N5(H5C,H5D), N8(H8A,H8B), C15(H15A,H15B)
;
_shelx_res_checksum              63748
_olex2_submission_special_instructions 'No special instructions were received'