Two resistance-switchable hybrid polyoxotantalates based on {Co2Ta12} clusters
Cao, Yun-Fei; Lin, Yu-Jin; Li, Xin-Xiong; Sun, Yan-Qiong; Zheng, Shou-Tian; CrystEngComm 26 (2024) 3527–3534; doi:10.1039/D4CE00319E

data_7248703
_publ_section_title
;
 Two resistance-switchable hybrid polyoxotantalates based on {Co2Ta12}
 clusters
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3527
_journal_page_last               3534
_journal_paper_doi               10.1039/D4CE00319E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'C4 H4 Co2 N4 O38 Ta12, 2(C6 H6 Co N6), Na2 O10, 9(O)'
_chemical_formula_sum            'C16 H90 Co4 N16 Na2 O58 Ta12'
_chemical_formula_weight         3888.13
_chemical_name_systematic        1
_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             2024-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-03-25 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 132.465(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.025(5)
_cell_length_b                   30.658(6)
_cell_length_c                   18.995(4)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    170
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.37
_cell_volume                     11610(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      170
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29258
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.218
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    11.890
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1044 before and 0.0411 after correction.
The Ratio of minimum to maximum transmission is 0.6017.
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    2.224
_exptl_crystal_description       block
_exptl_crystal_F_000             7072
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.786
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         10260
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0521P)^2^+165.4357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8322
_reflns_number_total             10260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00319e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7248703--7248704.cif.'
_cod_database_code               7248703
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.383
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2. Restrained distances
 N4-C6 = N3-C5
 1.45 with sigma of 0.05
 C39-N7
 1.4 with sigma of 0.02
 N8-C19
 1.4 with sigma of 0.02
 C6-C5
 1.45 with sigma of 0.05
 C19-C39
 1.4 with sigma of 0.02
 N6-C7
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3 \\sim C6 \\sim C5 \\sim C39 \\sim C19: within 2A with sigma of 0.2 and sigma
for terminal atoms of 0.4 within 2A
N4 \\sim N1 \\sim N2 \\sim N3 \\sim N5 \\sim N6 \\sim N7 \\sim N8: within 2A
with sigma of 0.2 and sigma for terminal atoms of 0.4 within 2A
C6 \\sim C2 \\sim C1 \\sim C3 \\sim C5 \\sim C39 \\sim C19: within 2A with
sigma of 0.2 and sigma for terminal atoms of 0.4 within 2A
C7 \\sim C2 \\sim C1 \\sim C3 \\sim C5 \\sim C6 \\sim C39 \\sim C19: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C39 \\sim C2 \\sim C1 \\sim C3 \\sim C5 \\sim C6 \\sim C19 \\sim C7: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N6 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N7 \\sim N8: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N5 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N6 \\sim N7 \\sim N8: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(N4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim
Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(N8)
\\sim Ueq: with sigma of 0.2 and sigma for terminal atoms of 0.4
Uanis(C39) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma
of 0.2 and sigma for terminal atoms of 0.4
Uanis(Co2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C6) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N7) \\sim
Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.001
Uanis(O28) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O27)
\\sim Ueq, Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.001
4. Others
 Fixed X: C3(0.70381) N7(0.834709) N8(0.8575) C39(0.89717) C19(0.90831)
 Fixed Y: C3(0.59337) N7(0.51873) N8(0.518221) C39(0.52416) C19(0.50325)
 Fixed Z: C3(0.427629) N7(0.38777) N8(0.553061) C39(0.482559) C19(0.55909)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'