Substituted benzoate-anchored decanuclear titanium-oxo clusters featuring an unprecedented defective double-cubane geometry
Pei, Xin-Yue; He, Ying; Wang, Jia-Yin; Wang, Hong-Yan; Bo, Qi-Bing; CrystEngComm 25 (2023) 1617–1625; doi:10.1039/D2CE01653B

data_7246333
_publ_section_title
;
 Substituted benzoate-anchored decanuclear titanium-oxo clusters featuring
 an unprecedented defective double-cubane geometry
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1617
_journal_page_last               1625
_journal_paper_doi               10.1039/D2CE01653B
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C126 H210 N2 O36 Ti10'
_chemical_formula_sum            'C126 H210 N2 O36 Ti10'
_chemical_formula_weight         2807.95
_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     iterative
_audit_creation_date             2022-12-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-12-09 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                83.659(2)
_cell_angle_beta                 66.309(3)
_cell_angle_gamma                89.939(2)
_cell_formula_units_Z            1
_cell_length_a                   15.7345(4)
_cell_length_b                   16.7320(4)
_cell_length_c                   17.2068(6)
_cell_measurement_reflns_used    13157
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9010
_cell_measurement_theta_min      3.7500
_cell_volume                     4118.2(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  Xcaibur,Eos,Gemini
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54048
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.213
_diffrn_reflns_theta_min         3.031
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         19458
_refine_ls_number_restraints     759
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0654P)^2^+1.7221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12597
_reflns_number_total             19458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01653b2.cif
_cod_data_source_block           Ti-DTBB
_cod_depositor_comments
'Adding full bibliography for 7246333--7246336.cif.'
_cod_database_code               7246333
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.903
_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
 C59-C58
 1.5 with sigma of 0.02
 C40-C38 = C39A-C38 = C39-C38 = C41A-C38 = C41-C38 = C40A-C38
 1.52 with sigma of 0.02
 C26-C23 = C25A-C23 = C25-C23 = C24A-C23 = C24-C23 = C26A-C23
 1.52 with sigma of 0.02
 C11-C10 = C8-C11 = C9-C11
 1.52 with sigma of 0.02
 C11A-C10A = C9A-C11A = C8A-C11A
 1.52 with sigma of 0.02
 C14-C12 = C14A-C12 = C13-C12 = C13A-C12 = C15-C12 = C15A-C12
 1.52 with sigma of 0.02
 C29A-C27 = C30-C27 = C30A-C27 = C28-C27 = C28A-C27 = C29-C27
 1.52 with sigma of 0.02
 C57-C55 = C56A-C55A = C57A-C55A = C56-C55
 1.52 with sigma of 0.02
 C56-C55 = C55-C57
 1.52 with sigma of 0.02
 C59-C58 = C58-C60
 1.52 with sigma of 0.02
 C59A-C58A = C58A-C60A
 1.52 with sigma of 0.02
 C53-C64 = C64-C54
 1.52 with sigma of 0.02
 C54A-C64A = C64A-C53A
 1.52 with sigma of 0.02
 C56-C57
 2.633 with sigma of 0.04
 C59A-C60A
 2.633 with sigma of 0.04
 C59-C60
 2.633 with sigma of 0.04
 C53-C54
 2.633 with sigma of 0.04
 C54A-C53A
 2.633 with sigma of 0.04
 C38-C36 \\sim C38-C39 \\sim C38-C40 \\sim C38-C41 \\sim C38-C41A \\sim
C38-C40A \\sim C38-C39A
 with sigma of 0.02
 C39-C40 \\sim C39-C41 \\sim C40-C41 \\sim C41A-C40A \\sim C41A-C39A \\sim
C40A-C39A
 with sigma of 0.04
 C24-C26 \\sim C24A-C26A \\sim C25-C26 \\sim C25A-C26A
 with sigma of 0.04
 C23-C24 \\sim C23-C24A \\sim C23-C25 \\sim C23-C25A \\sim C23-C26 \\sim
C23-C26A \\sim C23-C19
 with sigma of 0.02
 C11A-C8A \\sim C11A-C10A \\sim C11A-C9A \\sim C11A-C4
 with sigma of 0.02
 C8-C9 \\sim C8-C10 \\sim C9-C10
 with sigma of 0.04
 C11-C4 \\sim C11-C8 \\sim C11-C9 \\sim C11-C10
 with sigma of 0.02
 C8A-C10A \\sim C8A-C9A \\sim C10A-C9A
 with sigma of 0.04
 C4-C11A \\sim C4-C11
 with sigma of 0.02
 C15-C14 \\sim C15A-C14A \\sim C13-C14 \\sim C13A-C14A
 with sigma of 0.04
 C12-C15 \\sim C12-C15A \\sim C12-C13 \\sim C12-C13A \\sim C12-C6 \\sim C12-C14
\\sim C12-C14A
 with sigma of 0.02
 C27-C21 \\sim C27-C28 \\sim C27-C29 \\sim C27-C30 \\sim C27-C29A \\sim
C27-C30A \\sim C27-C28A
 with sigma of 0.02
 C28-C29 \\sim C28-C30 \\sim C29-C30 \\sim C29A-C30A \\sim C29A-C28A \\sim
C30A-C28A
 with sigma of 0.04
 O16-C55 \\sim O16-C55A
 with sigma of 0.02
 O17-C58 \\sim O17-C58A
 with sigma of 0.02
 O15-C64A \\sim O15-C64
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C14A \\sim C12 \\sim C15A \\sim C13A \\sim C6: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C29A \\sim C27 \\sim C28A \\sim C30A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C42 \\sim C43 \\sim C44 \\sim C45: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2A
Uanis(C8) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C59) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C26A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C4) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C10A)
\\sim Ueq, Uanis(C8A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 C39, C41, C40, C38, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C41A, C39A, C40A, C36, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C23, C24A, C25A, C26A, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C23, C24, C25, C26, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8A, C10A, C9A, C11A, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, C9, C10, C11, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C12, C13A, C14A, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C13, C14, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14A, C12, C15A, C13A, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C55, C57, C56, O16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C55A, C57A, C56A, O16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C60A, C58A, C59A, O17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C59, C58, C60, O17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C53, C64, C54, O15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C54A, C64A, C53A, O15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=
 Sof(H40F)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(1)
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(2)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(2)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(3)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(3)
 Sof(C11A)=1-FVAR(4)
 Sof(C11)=FVAR(4)
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(5)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(5)
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(6)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(6)
 Sof(C57A)=Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(C55A)=Sof(H55A)=Sof(C56A)=
 Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(7)
 Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C57)=Sof(H57A)=
 Sof(H57B)=Sof(H57C)=FVAR(7)
 Sof(C58A)=Sof(H58A)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C59A)=
 Sof(H59D)=Sof(H59E)=Sof(H59F)=1-FVAR(8)
 Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60)=Sof(H60A)=
 Sof(H60B)=Sof(H60C)=FVAR(8)
 Sof(C64A)=Sof(H64A)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=
 Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(9)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=
 Sof(C64)=Sof(H64)=FVAR(9)
6.a Ternary CH refined with riding coordinates:
 C46(H46), C49(H49), C55(H55), C58(H58), C55A(H55A), C58A(H58A), C64(H64),
 C64A(H64A)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C18(H18), C20(H20), C22(H22), C33(H33), C35(H35),
 C37(H37), C61(H61)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,
 H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C41A(H41D,H41E,H41F), C40A(H40D,H40E,H40F), C39A(H39D,H39E,H39F),
 C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C8A(H8AA,
 H8AB,H8AC), C10A(H10D,H10E,H10F), C9A(H9AA,H9AB,H9AC), C13A(H13D,H13E,H13F),
 C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F), C29A(H29D,H29E,H29F), C30A(H30D,
 H30E,H30F), C28A(H28D,H28E,H28F), C57A(H57D,H57E,H57F), C56A(H56D,H56E,H56F),
 C60A(H60D,H60E,H60F), C59A(H59D,H59E,H59F), C53A(H53D,H53E,H53F), C54A(H54D,
 H54E,H54F)
;
_shelx_res_checksum              5803
_shelx_fab_checksum              48199
_olex2_submission_special_instructions 'No special instructions were received'