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_7250507
_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         'C68 H84 O20 Ta4'
_chemical_formula_sum            'C68 H84 O20 Ta4'
_chemical_formula_weight         1945.15
_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     iterative
_audit_creation_date             2023-04-11
_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                 102.8516(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4485(8)
_cell_length_b                   12.6909(7)
_cell_length_c                   20.2649(10)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.89
_cell_measurement_theta_min      2.49
_cell_volume                     3622.8(3)
_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      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            116530
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         21.982
_diffrn_reflns_theta_min         2.526
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.261
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1164 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.7427.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.568
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         8972
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0116P)^2^+8.3979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7208
_reflns_number_total             8972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00444f3.cif
_cod_data_source_block           rl23
_cod_depositor_comments
'Adding full bibliography for 7250504--7250508.cif.'
_cod_database_code               7250507
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.553
_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. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C11(H11), C28(H28)
3.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C35(H35), C7(H7),
 C14(H14), C15(H15), C16(H16), C10(H10), C8(H8), C12(H12)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C3(H3A,H3B,
 H3C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C33(H33A,H33B,H33C), C31(H31A,
 H31B,H31C)
;
_shelx_res_checksum              16433
_olex2_submission_special_instructions 'No special instructions were received'