Syntheses, structures and ligand binding modes of titanium-oxide complexes of 2-picolinate
Gao, Chang; Liu, Caiyun; Said, Amir; Niu, Huihui; Wang, Dexin; Wang, Guo; Tung, Chen-Ho; Wang, Yifeng; Dalton Transactions  (2022) –; doi:10.1039/D1DT04170C

data_7709487
_publ_section_title
;
 Syntheses, structures and ligand binding modes of titanium-oxide
 complexes of 2-picolinate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04170C
_journal_year                    2022
_chemical_formula_moiety
'C72 H108 N6 O44 Ti14, 2(C3 H8 O), 2(C2 H3 N), 2(C4 H11 N)'
_chemical_formula_sum            'C90 H152 N10 O46 Ti14'
_chemical_formula_weight         2780.81
_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   mixed
_audit_creation_date             2021-12-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-06 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.688(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.4181(2)
_cell_length_b                   16.6427(2)
_cell_length_c                   20.1511(4)
_cell_measurement_reflns_used    15892
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.4030
_cell_measurement_theta_min      2.7250
_cell_volume                     6204.36(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.943
_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     93.00 177.00   1.00    0.98    --  106.49  57.00 150.00   84
  2  \w     71.00  96.00   1.00    0.17    --   48.45 166.00 153.00   25
  3  \w    101.00 178.00   1.00    0.98    --  106.49 115.00   7.00   77
  4  \w     94.00 178.00   1.00    0.98    --  106.49  38.00-180.00   84
  5  \w    -27.00  27.00   1.00    0.17    --  -48.45  19.00 120.00   54
  6  \w    -27.00  27.00   1.00    0.17    --  -48.45  19.00   0.00   54
  7  \w    -42.00 -14.00   1.00    0.98    --  -86.25  38.00 -60.00   28
  8  \w    -42.00 -13.00   1.00    0.98    --  -86.25  38.00   0.00   29
  9  \w    -72.00 -47.00   1.00    0.98    --  -86.25 115.00   7.00   25
 10  \w    -69.00 -44.00   1.00    0.17    --  -48.45 115.00   7.00   25
 11  \w   -112.00 -86.00   1.00    0.17    --  -48.45 166.00 153.00   26
 12  \w    -98.00 -73.00   1.00    0.98    --  -86.25 166.00 153.00   25
 13  \w     37.00 105.00   1.00    0.98    --  106.49 -99.00 -60.00   68
 14  \w     83.00 108.00   1.00    0.98    --  106.49-115.00 -81.00   25
 15  \w     39.00  66.00   1.00    0.98    --  106.49-115.00 -81.00   27
 16  \w     65.00  91.00   1.00    0.17    --   48.45-115.00 -81.00   26
 17  \w     80.00 105.00   1.00    0.17    --   48.45-166.00 132.00   25
 18  \w     58.00 140.00   1.00    0.98    --  106.49-166.00 132.00   82
 19  \w     34.00  64.00   1.00    0.98    --  106.49 -57.00 120.00   30
 20  \w     35.00  66.00   1.00    0.98    --  106.49 -57.00 -30.00   31
 21  \w     34.00 104.00   1.00    0.98    --  106.49 -77.00 -60.00   70
 22  \w     34.00  66.00   1.00    0.98    --  106.49 -57.00-120.00   32
 23  \w   -115.00 -47.00   1.00    0.17    --  -48.45-166.00 132.00   68
 24  \w   -110.00 -84.00   1.00    0.98    --  -86.25-166.00 132.00   26
 25  \w   -120.00 -73.00   1.00    0.17    --  -48.45-125.00 -60.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0097305000
_diffrn_orient_matrix_UB_12      0.0730388000
_diffrn_orient_matrix_UB_13      0.0432550000
_diffrn_orient_matrix_UB_21      -0.0335539000
_diffrn_orient_matrix_UB_22      -0.0548646000
_diffrn_orient_matrix_UB_23      0.0435397000
_diffrn_orient_matrix_UB_31      0.0755602000
_diffrn_orient_matrix_UB_32      -0.0149246000
_diffrn_orient_matrix_UB_33      0.0517200000
_diffrn_radiation_monochromator  mirror
_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     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44175
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.709
_diffrn_reflns_theta_min         2.768
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.946
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       plate
_exptl_crystal_F_000             2876
_exptl_crystal_size_max          0.012
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         12329
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0706
_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^)+(0.0626P)^2^+34.7525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.1953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9698
_reflns_number_total             12329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04170c2.cif
_cod_data_source_block           ti14pa6
_cod_database_code               7709487
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'Ti C O N'
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.911
_reflns_odcompleteness_completeness 99.16
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C44-C45 = C44-C43 = O23-C44
 1.45 with sigma of 0.01
 N5-H5
 0.998 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O23 \\sim C43 \\sim C44 \\sim C45: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C26(H26), C29(H29), C32(H32), C35(H35), C44(H44)
4.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B)
4.c Me refined with riding coordinates:
 C33(H33A,H33B,H33C)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16)
4.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C)
4.f Idealised tetrahedral OH refined as rotating group:
 O23(H23A)
;
_shelx_res_checksum              98338
_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 2.020
_oxdiff_exptl_absorpt_empirical_full_min 0.588