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_7246335
_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 O42 Ti10'
_chemical_formula_sum            'C84 H126 N2 O42 Ti10'
_chemical_formula_weight         2314.86
_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     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                64.800(4)
_cell_angle_beta                 66.955(5)
_cell_angle_gamma                75.967(4)
_cell_formula_units_Z            1
_cell_length_a                   15.0565(8)
_cell_length_b                   15.5845(7)
_cell_length_c                   16.1779(7)
_cell_measurement_reflns_used    11817
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0330
_cell_measurement_theta_min      3.2690
_cell_volume                     3147.6(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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Xcaibur,Eos,Gemini
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_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            38329
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.133
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.776
_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    1.221
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         12836
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0553P)^2^+2.0909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9056
_reflns_number_total             12836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01653b2.cif
_cod_data_source_block           Ti-MOB
_cod_depositor_comments
'Adding full bibliography for 7246333--7246336.cif.'
_cod_database_code               7246335
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.776
_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
 C38-C37 = C45-C43
 1.52 with sigma of 0.02
 C13-C12 = C50-C49 = C33-C31
 1.52 with sigma of 0.02
 C49-C32 = C83-C31
 1.52 with sigma of 0.02
 C47-C46 = C36-C34
 1.52 with sigma of 0.02
 C48-C46 = C35-C34
 1.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C49 \\sim C32 \\sim C50 \\sim O17: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C38 \\sim C37 \\sim C39 \\sim O16: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C45 \\sim C43 \\sim C44 \\sim O16: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C48 \\sim C46 \\sim C47 \\sim O15: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C34 \\sim C36 \\sim C35: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C83 \\sim C31 \\sim C33 \\sim O17: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O17, C49, C50, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O16, C37, C38, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O15, C46, C48, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O16, C43, C44, C45
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O17, C31, C33, C83
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O15, C34, C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C31)=Sof(H31)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C43)=Sof(H43)=
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C46)=Sof(H46)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C47)=Sof(H47A)=
 Sof(H47B)=Sof(H47C)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=1-FVAR(1)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C49)=Sof(H49)=FVAR(1)
6.a Riding coordinates:
 C49(H49)
6.b Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C31(H31), C34(H34), C37(H37), C43(H43), C46(H46)
6.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)
6.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),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C47(H47A,
 H47B,H47C), C50(H50A,H50B,H50C), C83(H83A,H83B,H83C)
;
_shelx_res_checksum              47254
_shelx_fab_checksum              3749
_olex2_submission_special_instructions 'No special instructions were received'