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_7244721
_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         'C64 H100 N4 O28 Ti8'
_chemical_formula_sum            'C64 H100 N4 O28 Ti8'
_chemical_formula_weight         1756.67
_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             2020-12-26
_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                93.9774(15)
_cell_angle_beta                 95.1157(14)
_cell_angle_gamma                100.3300(15)
_cell_formula_units_Z            2
_cell_length_a                   13.5956(5)
_cell_length_b                   14.9312(5)
_cell_length_c                   20.3151(7)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.35
_cell_volume                     4025.6(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            75194
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.392
_diffrn_reflns_theta_min         2.105
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0661 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.3949.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         16460
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0704P)^2^+3.2384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12281
_reflns_number_total             16460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00195k2.cif
_cod_data_source_block           cluster-6
_cod_database_code               7244721
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C61-O22
 1.4 with sigma of 0.02
 C19-C61 = C61-C31
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C59A) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C7, C7A, C48, C59, C59A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C31, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C39, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C55, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5)
 H7AC(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) H48(0.5) H48A(0.5) C59(0.5)
 H59A(0.5) H59B(0.5) H59C(0.5) C59A(0.5) H59D(0.5) H59E(0.5) H59F(0.5)
 H61A(0.5) H61(0.5) C31A(0.5) H31D(0.5) H31E(0.5) H31F(0.5)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C14(H14), C17(H17), C23(H23), C37(H37), C39(H39), C44(H44),
 C48(H48), C48(H48A), C53(H53), C54(H54), C55(H55), C61(H61A), C61(H61)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C10(H10), C11(H11), C16(H16), C18(H18), C22(H22), C26(H26),
 C28(H28), C33(H33), C34(H34), C40(H40), C45(H45), C47(H47), C50(H50), C64(H64)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C7A(H7AA,
 H7AB,H7AC), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C),
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C46(H46A,
 H46B,H46C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C56(H56A,H56B,H56C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C59A(H59D,H59E,
 H59F), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C),
 C31A(H31D,H31E,H31F)
;
_shelx_res_checksum              31175
_shelx_hkl_checksum              85866
_olex2_submission_special_instructions 'No special instructions were received'