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_7250504
_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         'C48 H60 O11 Ta2'
_chemical_formula_sum            'C48 H60 O11 Ta2'
_chemical_formula_weight         1174.86
_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             2024-04-16
_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                 95.399(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0631(12)
_cell_length_b                   10.1086(4)
_cell_length_c                   21.7781(11)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.22
_cell_measurement_theta_min      2.86
_cell_volume                     4835.6(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  0.0777
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70322
_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         20.551
_diffrn_reflns_theta_min         2.711
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.455
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.6537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0976 before and 0.0666 after correction.
The Ratio of minimum to maximum transmission is 0.8780.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       plate
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.377
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0138P)^2^+23.4797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3930
_reflns_number_total             4952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00444f3.cif
_cod_data_source_block           rl18
_cod_depositor_comments
'Adding full bibliography for 7250504--7250508.cif.'
_cod_database_code               7250504
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.710
_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
 C19-C20
 1.5 with sigma of 0.02
 C16-C17
 1.5 with sigma of 0.02
 C19-C21
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.05
4.a Ternary CH refined with riding coordinates:
 C22(H22), C16(H16), C19(H19)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C4(H4), C7(H7), C11(H11), C13(H13), C14(H14), C6(H6), C5(H5), C12(H12)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C17(H17A,H17B,H17C), C21(H21A,H21B,
 H21C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              10231
_olex2_submission_special_instructions 'No special instructions were received'