A family of oxime-based titanium-oxo clusters: synthesis, structures, and photoelectric responses
Wang, Chao; Chen, Ning; Kong, Fangong; Wang, Shoujuan; CrystEngComm  (2022) –; doi:10.1039/D2CE00195K

data_7244723
_publ_section_title
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 A family of oxime-based titanium-oxo clusters: synthesis, structures, and
 photoelectric responses
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00195K
_journal_year                    2022
_chemical_formula_moiety         'C41 H39 N3 O13 Ti3'
_chemical_formula_sum            'C41 H39 N3 O13 Ti3'
_chemical_formula_weight         925.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-12-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-06-22 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.6678(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8670(3)
_cell_length_b                   21.1077(5)
_cell_length_c                   18.0596(4)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.26
_cell_volume                     4333.59(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61884
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         2.035
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0681 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.4094.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         8876
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0510P)^2^+1.2663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7190
_reflns_number_total             8876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00195k2.cif
_cod_data_source_block           cluster-5
_cod_database_code               7244723
_shelx_shelxl_version_number     2018/3
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C39A)
\\sim Ueq, Uanis(C5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Rigid body (RIGU) restrains
 O8, C5, C5A, C19, C39, C39A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 Sof(C39A)=Sof(H39A)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C39)=
 Sof(H39)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C30(H30), C39(H39), C39A(H39A)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C17(H17), C20(H20), C22(H22), C23(H23), C26(H26), C27(H27),
  C28(H28), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
 C40(H40), C41(H41)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C19(H19A,H19B,H19C), C19(H19D,H19E,
 H19F), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              38067
_shelx_hkl_checksum              32003
_olex2_submission_special_instructions 'No special instructions were received'