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_7244724
_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         'C27 H29 N3 O8 Ti2'
_chemical_formula_sum            'C27 H29 N3 O8 Ti2'
_chemical_formula_weight         619.33
_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             2020-12-23
_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                 101.132(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6916(7)
_cell_length_b                   14.6046(9)
_cell_length_c                   14.2100(8)
_cell_measurement_reflns_used    3163
_cell_measurement_temperature    137(1)
_cell_measurement_theta_max      69.0880
_cell_measurement_theta_min      4.3720
_cell_volume                     2788.0(3)
_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_environment      N~2~
_diffrn_ambient_temperature      137(1)
_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 0.972
_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    -17.00   9.00   1.00    2.00    --    0.00  57.00 -30.00   26
  2  \w     12.00  42.00   1.00    2.00    --    0.00 -99.00  30.00   30
  3  \w    -70.00 -40.00   1.00    2.00    --    0.00 178.00-120.00   30
  4  \w     23.00  68.00   1.00    2.00    --    0.00  57.00 -30.00   45
  5  \w     87.00 118.00   1.00   10.00    --   54.63  77.00  60.00   31
  6  \w     28.00  66.00   1.00   10.00    --   54.63  77.00  60.00   38
  7  \w     75.00 115.00   1.00   10.00    --   54.63 157.00  12.00   40
  8  \w     39.00 121.00   1.00   10.00    --   54.63  57.00  30.00   82
  9  \w     18.00 105.00   1.00   10.00    --   54.63-125.00   0.00   87
 10  \w     34.00  59.00   1.00   10.00    --   54.63  57.00 120.00   25
 11  \w    122.00 176.00   1.00   10.00    --  109.26  50.00  30.00   54
 12  \w     83.00 109.00   1.00   10.00    --  109.26-111.00-180.00   26
 13  \w     88.00 171.00   1.00   10.00    --  109.26  63.00 120.00   83
 14  \w    100.00 164.00   1.00   10.00    --  109.26 111.00-150.00   64
 15  \w    108.00 174.00   1.00   10.00    --  109.26 111.00 -60.00   66
 16  \w     38.00 108.00   1.00   10.00    --  109.26-111.00 -60.00   70
 17  \w     38.00  63.00   1.00   10.00    --  109.26-111.00   0.00   25
 18  \w     60.00 110.00   1.00   10.00    --  109.26 -37.00 120.00   50
 19  \w    114.00 150.00   1.00   10.00    --  109.26 178.00-180.00   36
 20  \w     64.00  94.00   1.00   10.00    --  109.26 -63.00 -30.00   30
;
_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      -0.0193092000
_diffrn_orient_matrix_UB_12      -0.1039475000
_diffrn_orient_matrix_UB_13      -0.0065221000
_diffrn_orient_matrix_UB_21      -0.0448197000
_diffrn_orient_matrix_UB_22      0.0098056000
_diffrn_orient_matrix_UB_23      -0.1076400000
_diffrn_orient_matrix_UB_31      0.1036681000
_diffrn_orient_matrix_UB_32      -0.0148139000
_diffrn_orient_matrix_UB_33      -0.0244248000
_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  0.0551
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10646
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.581
_diffrn_reflns_theta_min         4.105
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52569
_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    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0828P)^2^+2.0292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3814
_reflns_number_total             5288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00195k2.cif
_cod_data_source_block           cluster-3
_cod_database_code               7244724
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.75
_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 Ternary CH refined with riding coordinates:
 C3(H3), C5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C24(H24), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C)
;
_shelx_res_checksum              74167
_shelx_hkl_checksum              34890
_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 1.780
_oxdiff_exptl_absorpt_empirical_full_min 0.479