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_7250505
_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         'C46 H64 O11 Ta2'
_chemical_formula_sum            'C46 H64 O11 Ta2'
_chemical_formula_weight         1154.87
_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     iterative
_audit_creation_date             2023-03-30
_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                 94.4971(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6357(5)
_cell_length_b                   9.2183(2)
_cell_length_c                   21.2142(5)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.36
_cell_volume                     4802.90(18)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.1
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61939
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.382
_diffrn_reflns_theta_min         1.926
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.608
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0952 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.8577.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.340
_refine_diff_density_min         -2.288
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4922
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0036P)^2^+45.6493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3869
_reflns_number_total             4922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00444f3.cif
_cod_data_source_block           rl32
_cod_depositor_comments
'Adding full bibliography for 7250504--7250508.cif.'
_cod_database_code               7250505
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.421
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-C23B
 1.5 with sigma of 0.02
 C21-C23A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0
Uanis(C23B) \\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0 and sigma for
terminal atoms of 0.03
4. Others
 Sof(H21A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(H21)=Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C10B)=Sof(H10B)=
 Sof(C11B)=Sof(H11B)=Sof(C9B)=Sof(H9B)=Sof(C12B)=Sof(H12B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C21(H21A), C15(H15), C18(H18)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C4(H4), C5(H5), C10B(H10B), C11B(H11B), C9B(H9B), C9A(H9A),
 C12B(H12B), C10A(H10A), C11A(H11A), C12A(H12A)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C16(H16A,H16B,H16C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C23B(H23A,H23B,H23C), C14(H14A,H14B,H14C),
 C23A(H23D,H23E,H23F)
;
_shelx_res_checksum              46460
_olex2_submission_special_instructions 'No special instructions were received'