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_7246336
_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 H112 N14 O60 Ti10'
_chemical_formula_sum            'C84 H112 N14 O60 Ti10'
_chemical_formula_weight         2756.87
_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                107.392(6)
_cell_angle_beta                 107.891(6)
_cell_angle_gamma                95.423(6)
_cell_formula_units_Z            1
_cell_length_a                   13.1367(10)
_cell_length_b                   16.9074(11)
_cell_length_c                   17.9372(12)
_cell_measurement_reflns_used    7556
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7150
_cell_measurement_theta_min      3.3020
_cell_volume                     3541.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -51.00  43.00   1.00   63.26    --   16.17 -77.00 150.00   94
  2  \w    -11.00  84.00   1.00   63.26    --   16.17  77.00 -90.00   95
  3  \w    -51.00  33.00   1.00   63.26    --   16.17 -57.00  30.00   84
  4  \w    -25.00  22.00   1.00   63.26    --  -16.64 -99.00  30.00   47
  5  \w    -25.00  22.00   1.00   63.26    --  -16.64 -99.00 -60.00   47
  6  \w     -3.00  85.00   1.00   63.26    --   16.17  37.00-180.00   88
  7  \w     -3.00  85.00   1.00   63.26    --   16.17  37.00  90.00   88
  8  \w     35.00  88.00   1.00   63.26    --   16.17 178.00   0.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1202
_diffrn_reflns_av_unetI/netI     0.1710
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35948
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.117
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       block
_exptl_crystal_F_000             1414
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         12493
_refine_ls_number_restraints     1490
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1707
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1167P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2158
_refine_ls_wR_factor_ref         0.2680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5294
_reflns_number_total             12493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01653b2.cif
_cod_data_source_block           Ti-MDNB
_cod_depositor_comments
'Adding full bibliography for 7246333--7246336.cif.'
_cod_database_code               7246336
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.790
_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
 C61-C28 = C45-C29 = C32-C29 = C30-C28
 1.52 with sigma of 0.02
 C43-C31A = C44-C31 = C44-C33A = C43-C33
 1.52 with sigma of 0.02
 C36-C35 = C35-C34
 1.52 with sigma of 0.02
 C45-C29 = C29-C32
 1.52 with sigma of 0.02
 O14-C28 = O14-C29
 1.45 with sigma of 0.02
 C47-C46 = C46-C48
 1.52 with sigma of 0.02
 O16-C35 = O16-C46
 1.45 with sigma of 0.02
 O32-N8 = N8-O2
 1.25 with sigma of 0.02
 O20-N8 = N8-O19
 1.25 with sigma of 0.02
 O35-N6 = N6-O36
 1.25 with sigma of 0.02
 O27-N6 = N6-O28
 1.25 with sigma of 0.02
 O37-N7 = N7-O38
 1.25 with sigma of 0.02
 O29-N7 = N7-O30
 1.25 with sigma of 0.02
 O33-N3 = N3-O34
 1.25 with sigma of 0.02
 O21-N3 = N3-O22
 1.25 with sigma of 0.02
 C26-C25 = C25-C27A
 1.52 with sigma of 0.02
 C49-C26A = C26A-C27
 1.52 with sigma of 0.02
 C36-C34
 2.475 with sigma of 0.04
 C45-C32
 2.475 with sigma of 0.04
 C47-C48
 2.475 with sigma of 0.04
 O20-O19
 2.165 with sigma of 0.04
 O32-O2
 2.165 with sigma of 0.04
 O27-O28
 2.165 with sigma of 0.04
 O35-O36
 2.165 with sigma of 0.04
 O37-O38
 2.165 with sigma of 0.04
 O29-O30
 2.165 with sigma of 0.04
 O33-O34
 2.165 with sigma of 0.04
 O21-O22
 2.165 with sigma of 0.04
 C26-C27A
 2.475 with sigma of 0.04
 C49-C27
 2.475 with sigma of 0.04
 O13-C26A \\sim O13-C25
 with sigma of 0.02
 O15-C43 \\sim O15-C44
 with sigma of 0.02
 O14-C28 \\sim O14-C29
 with sigma of 0.02
 N3-C6 \\sim N3-O33 \\sim N3-O34 \\sim N3-O21 \\sim N3-O22
 with sigma of 0.02
 O33-O34 \\sim O21-O22
 with sigma of 0.04
3. Restrained planarity
 O32, N8, C4, O2
 with sigma of 0.1
 O20, N8, O19, C4
 with sigma of 0.1
 O33, N3, O34, C6
 with sigma of 0.1
 O21, N3, C6, O22
 with sigma of 0.1
 O35, N6, O36, C23
 with sigma of 0.1
 O27, N6, O28, C23
 with sigma of 0.1
 O30, N7, O29, C20
 with sigma of 0.1
 O37, N7, O38, C20
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C49, C25, C27A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C38, C37, C39, O17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C25, C26, C27A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C45 \\sim C28 \\sim C61 \\sim O14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C36 \\sim C35 \\sim C34 \\sim O16: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C26A \\sim C49 \\sim C27 \\sim O13: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C30 \\sim C29 \\sim C32 \\sim O14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C33 \\sim C43 \\sim C31A \\sim O15: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C33A \\sim C44 \\sim C31 \\sim O15: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C48 \\sim C46 \\sim C47 \\sim O16: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C12 \\sim N4 \\sim O23 \\sim O24: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O25 \\sim O26 \\sim N5 \\sim C14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N4 \\sim O23 \\sim O24 \\sim C12: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C26 \\sim C25 \\sim C27A \\sim O13: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C42 \\sim C41 \\sim N1 \\sim C40 \\sim O18: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(C33) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O37) \\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C20)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O33) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(C6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O21) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(C6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(O13)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 C31A, C43, O15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33A, C44, C31, O15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N8, O19, O20, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O32, N8, O2, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O33, N3, O34, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O22, O21, N3, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O37, O38, N7, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O30, N7, O29, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O36, N6, O35, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Sof(O19)=Sof(O20)=Sof(O21)=Sof(O22)=Sof(O27)=Sof(O28)=Sof(C25)=Sof(H25)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C44)=Sof(H44)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C28)=Sof(H28)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=
 Sof(C46)=Sof(H46)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C47)=Sof(H47A)=
 Sof(H47B)=Sof(H47C)=Sof(O37)=Sof(O38)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=
 1-FVAR(1)
 Sof(O29)=Sof(O30)=Sof(O2)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C33)=
 Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=
 Sof(H35)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C43)=Sof(H43)=Sof(C31A)=
 Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C29)=
 Sof(H29)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(O32)=Sof(O33)=Sof(O34)=
 Sof(O36)=Sof(O35)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C26A)=Sof(H26D)=
 FVAR(1)
8.a Riding coordinates:
 C34(H34A,H34B,H34C), C45(H45A,H45B,H45C), C61(H61A,H61B,H61C)
8.b Ternary CH refined with riding coordinates:
 C25(H25), C35(H35), C43(H43), C44(H44), C28(H28), C29(H29), C46(H46),
 C26A(H26D)
8.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C11(H11), C15(H15), C19(H19), C24(H24), C40(H40)
8.d Fitted hexagon refined as free rotating group:
 C21(C20,C19,C18,C24,C23)
8.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C33A(H33D,H33E,H33F), C31A(H31D,H31E,H31F), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C49(H49A,
 H49B,H49C), C27A(H27D,H27E,H27F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29809
_shelx_fab_checksum              95681
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;