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_7244722
_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         'C32 H32 N2 O13 Ti3'
_chemical_formula_sum            'C32 H32 N2 O13 Ti3'
_chemical_formula_weight         796.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 110.549(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5281(11)
_cell_length_b                   30.0488(17)
_cell_length_c                   10.1629(9)
_cell_measurement_reflns_used    1787
_cell_measurement_temperature    297
_cell_measurement_theta_max      68.4560
_cell_measurement_theta_min      3.7640
_cell_volume                     3582.4(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.974
_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     30.00  66.00   1.00    6.00    --    0.00  57.00 -60.00   36
  2  \w      9.00  64.00   1.00    6.00    --    0.00  57.00  30.00   55
  3  \w     16.00  41.00   1.00    6.00    --    0.00 -99.00  60.00   25
  4  \w      6.00  33.00   1.00   27.50    --   54.63 -57.00 -90.00   27
  5  \w     29.00 120.00   1.00   27.50    --   54.63  37.00-180.00   91
  6  \w     -9.00  80.00   1.00   27.50    --   54.63 -37.00   0.00   89
  7  \w     36.00 101.00   1.00   27.50    --   54.63-125.00  30.00   65
  8  \w     49.00  76.00   1.00   27.50    --   54.63  57.00-120.00   27
  9  \w     37.00 112.00   1.00   27.50    --  109.26-111.00  60.00   75
 10  \w     40.00 113.00   1.00   27.50    --  109.26-111.00-150.00   73
 11  \w     39.00 142.00   1.00   27.50    --  109.26 -25.00   0.00  103
 12  \w    113.00 143.00   1.00   27.50    --  109.26 178.00  60.00   30
 13  \w    117.00 164.00   1.00   27.50    --  109.26  63.00 -30.00   47
 14  \w     43.00 132.00   1.00   27.50    --  109.26 -63.00  30.00   89
 15  \w     87.00 176.00   1.00   27.50    --  109.26  50.00-180.00   89
;
_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      -0.0641645000
_diffrn_orient_matrix_UB_12      -0.0013882000
_diffrn_orient_matrix_UB_13      0.1045483000
_diffrn_orient_matrix_UB_21      0.1144455000
_diffrn_orient_matrix_UB_22      -0.0037774000
_diffrn_orient_matrix_UB_23      0.1231023000
_diffrn_orient_matrix_UB_31      0.0065383000
_diffrn_orient_matrix_UB_32      0.0510682000
_diffrn_orient_matrix_UB_33      0.0118466000
_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  0.0838
_diffrn_reflns_av_unetI/netI     0.1180
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13917
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.681
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58401
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0676P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.2034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3514
_reflns_number_total             6819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00195k2.cif
_cod_data_source_block           cluster-4
_cod_original_cell_volume        3582.4(5)
_cod_database_code               7244722
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C41(H41), C42(H42), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C43(H43A,H43B,
 H43C)
;
_shelx_res_checksum              38717
_shelx_hkl_checksum              40371
_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 1.493
_oxdiff_exptl_absorpt_empirical_full_min 0.737