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_7246334
_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         'C84 H126 N2 O36 Ti10'
_chemical_formula_sum            'C84 H126 N2 O36 Ti10'
_chemical_formula_weight         2218.86
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-08
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2022-12-09 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                119.360(4)
_cell_angle_beta                 99.503(4)
_cell_angle_gamma                106.205(4)
_cell_formula_units_Z            1
_cell_length_a                   15.2841(7)
_cell_length_b                   15.8379(5)
_cell_length_c                   16.1254(6)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7360
_cell_measurement_theta_min      3.1820
_cell_volume                     3046.9(3)
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12433
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.064
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.684
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         12433
_refine_ls_number_restraints     311
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0963P)^2^+0.9085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8412
_reflns_number_total             12433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01653b2.cif
_cod_data_source_block           Ti-MB
_cod_depositor_comments
'Adding full bibliography for 7246333--7246336.cif.'
_cod_original_cell_volume        3046.9(2)
_cod_database_code               7246334
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.875
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8894(13)
 0.1106(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C36-C34 = C47-C46 = C47-C35 = C45-C34
 1.52 with sigma of 0.02
 C39-C37 = C44-C37 = C48-C37A = C43-C37A
 1.52 with sigma of 0.02
 O17-C34 = O17-C47
 1.4 with sigma of 0.02
 C51-C32 = C53-C31 = C33-C31 = C52-C51
 1.52 with sigma of 0.02
 O17-C47 \\sim O17-C34
 with sigma of 0.02
 O14-C49 \\sim O14-C28
 with sigma of 0.02
 C29-C28 \\sim C49-C38 \\sim C50-C28 \\sim C49-C30
 with sigma of 0.02
 O15-C51 \\sim O15-C31
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C48 \\sim C37A \\sim O16 \\sim C43: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C47 \\sim C46 \\sim C35 \\sim O17: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C36 \\sim C34 \\sim C45 \\sim O17: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C44 \\sim C37 \\sim C39 \\sim O16: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C49 \\sim C38 \\sim C30: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C29 \\sim C28 \\sim C50 \\sim O14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C48) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(O16)
\\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C39) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(O16)
\\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C48, C37A, C43, O16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C47, C35, C46, O17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C34, C36, C45, O17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C39, C37, C44, O16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C38, C49, C30, O14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C28, C50, C29, O14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C32, C51, C52, O15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C53, C31, C33, O15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C34)=Sof(H34)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(H45C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(H43C)=Sof(C37A)=Sof(H37A)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=
 Sof(C49)=Sof(H49)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C51)=Sof(H51)=1-
 FVAR(1)
 Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C31)=Sof(H31)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C37)=Sof(H37)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C46)=Sof(H46A)=
 Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=
 FVAR(1)
7.a Riding coordinates:
 C48(H48A,H48B,H48C)
7.b Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C31(H31), C34(H34), C37(H37), C47(H47), C37A(H37A),
 C49(H49), C51(H51)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C11(H11), C12(H12), C15(H15), C16(H16),
 C19(H19), C20(H20), C23(H23), C24(H24), C40(H40)
7.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C45(H45A,H45B,
 H45C), C46(H46A,H46B,H46C), C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C38(H38A,
 H38B,H38C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              76938
_shelx_fab_checksum              9861
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'