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_7250508
_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         'C112 H110 O36 Ta8, C112 H112 O36 Ta8'
_chemical_formula_sum            'C224 H222 O72 Ta16'
_chemical_formula_weight         6961.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                87.046(5)
_cell_angle_beta                 78.852(5)
_cell_angle_gamma                80.786(5)
_cell_formula_units_Z            1
_cell_length_a                   11.3938(14)
_cell_length_b                   23.187(4)
_cell_length_c                   24.311(4)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.61
_cell_measurement_theta_min      2.68
_cell_volume                     6218.8(17)
_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 0.995
_diffrn_measured_fraction_theta_max 0.978
_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  0.0725
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            339380
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.702
_diffrn_reflns_theta_min         0.674
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.791
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.4661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1033 before and 0.0761 after correction.
The Ratio of minimum to maximum transmission is 0.6261.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_description       block
_exptl_crystal_F_000             3310
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         7.116
_refine_diff_density_min         -3.448
_refine_diff_density_rms         0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1343
_refine_ls_number_reflns         25543
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0766
_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^)+373.8911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17567
_reflns_number_total             25543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00444f3.cif
_cod_data_source_block           avh61
_cod_depositor_comments
'Adding full bibliography for 7250504--7250508.cif.'
_cod_original_cell_volume        6218.7(16)
_cod_database_code               7250508
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.659
_shelx_estimated_absorpt_t_min   0.428
_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. Restrained distances
 C101-C103
 1.5 with sigma of 0.02
 C101-C102
 1.5 with sigma of 0.02
 C101-O33
 1.4 with sigma of 0.02
 C103-C101
 1.5 with sigma of 0.02
 C95-C97
 1.5 with sigma of 0.02
 C95-C96
 1.5 with sigma of 0.02
 C107-C109
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C97) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.1
Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.1
Uanis(C109) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.1
Uanis(C112) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.1
Uanis(C102) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C103) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.1
Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C79) = Uanis(C88) = Uanis(C80) = Uanis(C81) = Uanis(C87) = Uanis(C86) =
Uanis(C82) = Uanis(C84) = Uanis(C83) = Uanis(C85)
4.a Ternary CH refined with riding coordinates:
 C89(H89), C104(H104), C92(H92), C107(H107), C98(H98), C110(H110), C95(H95),
 C101(H101)
4.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C25(H25), C26(H26), C55(H55), C14(H14), C11(H11), C77(H77),
 C80(H80), C88(H88), C87(H87), C82(H82), C83(H83), C84(H84), C85(H85), C44(H44),
  C69(H69), C3(H3), C58(H58), C66(H66), C65(H65), C47(H47), C43(H43), C4(H4),
 C54(H54), C75(H75), C36(H36), C31(H31), C16(H16), C28(H28), C70(H70), C9(H9),
 C60(H60), C21(H21), C72(H72), C52(H52), C41(H41), C17(H17), C63(H63), C18(H18),
  C6(H6), C7(H7), C74(H74), C19(H19), C62(H62), C30(H30), C61(H61), C8(H8),
 C73(H73), C40(H40), C51(H51), C29(H29), C38(H38), C39(H39), C49(H49), C50(H50)
4.c Naphthalene refined as free rotating group:
 C80(C79,C88,C87,C86,C81,C82,C83,C84,C85)
4.d Idealised Me refined as rotating group:
 C91(H91A,H91B,H91C), C106(H10A,H10B,H10C), C111(H11A,H11B,H11C), C112(H11D,
 H11E,H11F), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C100(H10S,H10T,H10U),
 C99(H99A,H99B,H99C), C90(H90A,H90B,H90C), C105(H10D,H10E,H10F), C108(H10G,H10H,
 H10I), C109(H10J,H10K,H10L), C97(H97A,H97B,H97C), C96(H96A,H96B,H96C),
 C102(H10M,H10N,H10O), C103(H10P,H10Q,H10R)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30410
_shelx_fab_checksum              38343
_olex2_submission_special_instructions 'No special instructions were received'