Polynuclear tantalum(v) coordination complexes: from dinuclear {Ta2O} to octanuclear {Ta8O12} oxo species connected through aryl monotopic carboxylate linkers
Huerta, Alejandro Vieyra; Ahmed, Mahmud Beji; Essayem, Nadine; Djakovitch, Laurent; Mesbah, Adel; Loiseau, Thierry; Duval, Sylvain; CrystEngComm 27 (2025) 4734–4743; doi:10.1039/D5CE00444F

data_7250506
_publ_section_title
;
 Polynuclear tantalum(v) coordination complexes: from dinuclear {Ta2O} to
 octanuclear {Ta8O12} oxo species connected through aryl monotopic
 carboxylate linkers
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              4734
_journal_page_last               4743
_journal_paper_doi               10.1039/D5CE00444F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C52 H76 O20 Ta4'
_chemical_formula_sum            'C52 H76 O20 Ta4'
_chemical_formula_weight         1744.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-04-24 deposited with the CCDC.	2025-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.784(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9823(9)
_cell_length_b                   18.5216(15)
_cell_length_c                   14.4260(12)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.63
_cell_measurement_theta_min      2.40
_cell_volume                     3185.3(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            100994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.638
_diffrn_reflns_theta_min         2.065
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.702
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0666 before and 0.0524 after correction.
The Ratio of minimum to maximum transmission is 0.8721.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.735
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         9720
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0053P)^2^+7.9632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7888
_reflns_number_total             9720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00444f3.cif
_cod_data_source_block           rl29
_cod_depositor_comments
'Adding full bibliography for 7250504--7250508.cif.'
_cod_database_code               7250506
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.663
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C24B, C26A, C25A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24A, C26B, C25B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C26B) \\sim Ueq, Uanis(C24B) \\sim Ueq, Uanis(C25B) \\sim Ueq,
Uanis(C25A) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C26A) \\sim Ueq: with sigma
of 0.05 and sigma for terminal atoms of 0.05
4. Others
 Sof(C24B)=Sof(H24B)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C25A)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C25B)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=Sof(C24A)=Sof(H24A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C18(H18), C15(H15), C21(H21), C24B(H24B), C24A(H24A)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C10(H10), C7(H7), C5(H5),
 C11(H11), C6(H6)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C17(H17A,H17B,H17C), C26B(H26A,H26B,H26C),
 C25B(H25A,H25B,H25C), C26A(H26D,H26E,H26F), C25A(H25D,H25E,H25F)
;
_shelx_res_checksum              75108
_olex2_submission_special_instructions 'No special instructions were received'