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_7244720
_publ_section_title
;
 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         'C42 H30 N6 O12 Ti3, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H34 Cl4 N6 O12 Ti3'
_chemical_formula_weight         1124.27
_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             2021-02-09
_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                79.464(5)
_cell_angle_beta                 74.926(4)
_cell_angle_gamma                64.319(6)
_cell_formula_units_Z            1
_cell_length_a                   9.2333(5)
_cell_length_b                   10.1635(8)
_cell_length_c                   14.3186(5)
_cell_measurement_reflns_used    4108
_cell_measurement_temperature    297
_cell_measurement_theta_max      71.0090
_cell_measurement_theta_min      5.4550
_cell_volume                     1165.49(13)
_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      297
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.960
_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     -4.00  21.00   1.00    5.00    --    0.00 -99.00-150.00   25
  2  \w     -4.00  22.00   1.00    5.00    --    0.00 -99.00 -60.00   26
  3  \w     32.00  64.00   1.00    5.00    --    0.00  77.00-120.00   32
  4  \w    -30.00  -3.00   1.00    5.00    --    0.00  77.00-120.00   27
  5  \w    -69.00 -34.00   1.00    5.00    --    0.00 178.00 -30.00   35
  6  \w     -9.00  76.00   1.00   19.00    --   54.63 -77.00  90.00   85
  7  \w     46.00 117.00   1.00   19.00    --   54.63  57.00 -60.00   71
  8  \w     24.00 113.00   1.00   19.00    --   54.63  19.00 -90.00   89
  9  \w     24.00  94.00   1.00   19.00    --   54.63 -99.00-120.00   70
 10  \w     44.00  94.00   1.00   19.00    --   54.63  57.00-180.00   50
 11  \w     -4.00  74.00   1.00   19.00    --   54.63 -57.00 -30.00   78
 12  \w     42.00 100.00   1.00   19.00    --  109.26-111.00-120.00   58
 13  \w     38.00  64.00   1.00   19.00    --  109.26-111.00 -90.00   26
 14  \w     43.00 116.00   1.00   19.00    --  109.26 -63.00  30.00   73
 15  \w     36.00 137.00   1.00   19.00    --  109.26 -25.00 150.00  101
 16  \w     40.00 130.00   1.00   19.00    --  109.26 -50.00-120.00   90
 17  \w     70.00 115.00   1.00   19.00    --  109.26 -37.00  60.00   45
 18  \w     42.00 144.00   1.00   19.00    --  109.26 -91.00 -90.00  102
 19  \w     66.00  92.00   1.00   19.00    --  109.26 178.00-180.00   26
 20  \w     49.00 141.00   1.00   19.00    --  109.26 -25.00 -60.00   92
 21  \w     58.00 113.00   1.00   19.00    --  109.26-111.00  60.00   55
 22  \w     89.00 167.00   1.00   19.00    --  109.26  63.00 -30.00   78
 23  \w     88.00 148.00   1.00   19.00    --  109.26  50.00 120.00   60
 24  \w     96.00 149.00   1.00   19.00    --  109.26 178.00 -90.00   53
 25  \w    104.00 129.00   1.00   19.00    --  109.26  63.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1056399000
_diffrn_orient_matrix_UB_12      -0.0894768000
_diffrn_orient_matrix_UB_13      0.0258518000
_diffrn_orient_matrix_UB_21      0.1329272000
_diffrn_orient_matrix_UB_22      -0.1243181000
_diffrn_orient_matrix_UB_23      0.0489383000
_diffrn_orient_matrix_UB_31      -0.0832824000
_diffrn_orient_matrix_UB_32      0.0707967000
_diffrn_orient_matrix_UB_33      0.0971270000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7342
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.178
_diffrn_reflns_theta_min         5.430
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.978
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64375
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.961
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4349
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1619P)^2^+1.6622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3945
_reflns_number_total             4349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00195k2.cif
_cod_data_source_block           cluster-2
_cod_database_code               7244720
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 Cl1, Cl2, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22)
;
_shelx_res_checksum              35228
_shelx_hkl_checksum              23215
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.636
_oxdiff_exptl_absorpt_empirical_full_min 0.696