Coordination-induced reductive elimination from a titanium(IV) complex.
Fritsche, Paul; Geyer, Lucia; Czernetzki, Corinna; Hierlmeier, Gabriele; Chemical communications (Cambridge, England) 60 (2024) 9030–9033; doi:10.1039/d4cc02500h

data_7133348
_publ_section_title
;
 Coordination-induced reductive elimination from a titanium(IV) complex.
;
_journal_issue                   68
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9030
_journal_page_last               9033
_journal_paper_doi               10.1039/d4cc02500h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C39 H53 N3 Ti'
_chemical_formula_sum            'C39 H53 N3 Ti'
_chemical_formula_weight         611.74
_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     dual
_audit_creation_date             2024-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-20 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                77.339(2)
_cell_angle_beta                 77.207(2)
_cell_angle_gamma                70.6190(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0602(2)
_cell_length_b                   12.0620(2)
_cell_length_c                   14.3315(3)
_cell_measurement_reflns_used    29914
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      73.0610
_cell_measurement_theta_min      3.1920
_cell_volume                     1736.62(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.959
_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    -36.00 -10.00   0.50    0.10    --  -14.00 121.00-178.49   52
  2  \w    -97.00 -36.00   0.50    0.40    --  -79.50 115.00 -83.14  122
  3  \w    -85.00 -17.00   0.50    0.10    --  -61.62 125.00 -60.00  136
  4  \w   -106.00 -35.00   0.50    0.40    --  -79.50 136.00 -31.64  142
  5  \w    -97.00 -36.00   0.50    0.40    --  -79.50 114.00   7.80  122
  6  \w    -97.00 -36.00   0.50    0.40    --  -79.50 114.00  56.29  122
  7  \w    -97.00 -36.00   0.50    0.40    --  -79.50 115.00 118.64  122
  8  \w    -97.00 -36.00   0.50    0.40    --  -79.50 114.00 171.89  122
  9  \w    -97.00 -36.00   0.50    0.40    --  -79.50 114.00  89.83  122
 10  \w    -97.00 -36.00   0.50    0.40    --  -79.50 114.00  56.29  122
 11  \w    -97.00 -36.00   0.50    0.40    --  -79.50 114.00  27.35  122
 12  \w    -97.00 -36.00   0.50    0.40    --  -79.50 114.00  27.35  122
 13  \w    -97.00 -36.00   0.50    0.40    --  -79.50 114.00 -61.46  122
 14  \w    -92.00 -33.00   0.50    0.40    --  -76.29 112.00-120.00  118
 15  \w    -97.00 -36.00   0.50    0.40    --  -79.50 114.00-158.58  122
 16  \w    -92.00 -33.00   0.50    0.40    --  -76.29 112.00-180.00  118
 17  \w    -92.00 -33.00   0.50    0.40    --  -76.29 112.00   0.00  118
 18  \w    -92.00 -33.00   0.50    0.40    --  -76.29 112.00 150.00  118
 19  \w     54.00  85.00   0.50    0.10    --   38.00  49.00 178.09   62
 20  \w     54.00  84.00   0.50    0.10    --   38.00  52.00 136.46   60
 21  \w     28.00  54.00   0.50    0.10    --   14.00  61.00  20.21   52
 22  \w     32.00  60.00   0.50    0.10    --   18.00  58.00-105.76   56
 23  \w     54.00 128.00   0.50    0.40    --   80.32  15.00 -60.00  148
 24  \w     54.00 128.00   0.50    0.40    --   80.32  15.00-120.00  148
 25  \w     54.00 128.00   0.50    0.40    --   80.32  15.00  30.00  148
 26  \w     41.00  92.00   0.50    0.40    --   83.50-103.00  11.76  102
 27  \w     43.00  90.00   0.50    0.40    --   83.50 -98.00 -41.64   94
 28  \w     40.00  86.00   0.50    0.40    --   80.32 -95.00-180.00   92
 29  \w     33.00  79.00   0.50    0.10    --   73.43 -95.00-180.00   92
 30  \w     40.00  86.00   0.50    0.40    --   80.32 -95.00 -90.00   92
 31  \w     43.00  89.00   0.50    0.40    --   83.50 -95.00  82.59   92
 32  \w    -54.00 -28.00   0.50    0.10    --  -14.00 -58.00 102.55   52
 33  \w    -54.00 -28.00   0.50    0.10    --  -14.00 -57.00  65.40   52
 34  \w    -98.00 -65.00   0.50    0.10    --  -50.00 -42.00 -48.98   66
 35  \w    -95.00 -60.00   0.50    0.10    --  -46.00 -38.00 -93.79   70
 36  \w   -124.00 -56.00   0.50    0.40    --  -76.29 -15.00 -30.00  136
 37  \w   -123.00 -93.00   0.50    0.40    --  -79.50 -61.00-170.45   60
 38  \w   -123.00 -93.00   0.50    0.40    --  -79.50 -63.00 -39.81   60
 39  \w   -119.00 -89.00   0.50    0.10    --  -74.00 -56.00-149.20   60
 40  \w   -119.00 -88.00   0.50    0.10    --  -74.00 -58.00 -27.25   62
 41  \w   -119.00 -89.00   0.50    0.10    --  -74.00 -56.00  17.37   60
 42  \w   -125.00 -94.00   0.50    0.40    --  -79.50 -56.00   6.13   62
 43  \w   -118.00 -88.00   0.50    0.10    --  -74.00 -59.00  63.14   60
 44  \w   -118.00 -88.00   0.50    0.10    --  -74.00 -60.00 167.97   60
 45  \w   -114.00 -85.00   0.50    0.10    --  -70.00 -59.00 109.30   58
 46  \w   -119.00 -89.00   0.50    0.10    --  -74.00 -55.00  33.39   60
 47  \w   -104.00 -74.00   0.50    0.10    --  -58.00 -51.00  59.19   60
 48  \w   -125.00 -94.00   0.50    0.40    --  -79.50 -53.00 123.34   62
 49  \w   -114.00 -82.00   0.50    0.10    --  -66.00 -46.00 121.45   64
 50  \w   -116.00 -85.00   0.50    0.10    --  -70.00 -54.00 -85.93   62
 51  \w   -122.00 -89.00   0.50    0.10    --  -74.00 -44.00-123.14   66
 52  \w   -126.00 -95.00   0.50    0.40    --  -79.50 -51.00-101.75   62
 53  \w   -125.00 -95.00   0.50    0.40    --  -79.50 -54.00-127.61   60
 54  \w   -119.00 -89.00   0.50    0.10    --  -74.00 -55.00-164.13   60
 55  \w   -110.00 -77.00   0.50    0.10    --  -62.00 -44.00-151.40   66
 56  \w   -124.00 -56.00   0.50    0.40    --  -76.29 -15.00   0.00  136
 57  \w   -102.00 -69.00   0.50    0.10    --  -54.00 -43.00  21.13   66
 58  \w   -123.00 -88.00   0.50    0.10    --  -74.00 -40.00  76.55   70
 59  \w   -128.00 -94.00   0.50    0.40    --  -79.50 -43.00 137.44   68
 60  \w   -125.00 -90.00   0.50    0.40    --  -79.50-126.00   2.82   70
 61  \w   -124.00 -91.00   0.50    0.40    --  -79.50-124.00 -17.22   66
 62  \w   -125.00 -90.00   0.50    0.40    --  -79.50-126.00 147.81   70
 63  \w   -125.00 -90.00   0.50    0.40    --  -79.50-126.00 165.41   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0355439000
_diffrn_orient_matrix_UB_12      -0.0201125000
_diffrn_orient_matrix_UB_13      -0.0917228000
_diffrn_orient_matrix_UB_21      -0.1422586000
_diffrn_orient_matrix_UB_22      0.0720206000
_diffrn_orient_matrix_UB_23      0.0301601000
_diffrn_orient_matrix_UB_31      0.0297657000
_diffrn_orient_matrix_UB_32      0.1149410000
_diffrn_orient_matrix_UB_33      -0.0560431000
_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  0.0252
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41332
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.971
_diffrn_reflns_theta_min         3.203
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.299
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         6859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0398P)^2^+0.6290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6764
_reflns_number_total             6859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02500h2.cif
_cod_data_source_block           gahi007_ap
_cod_depositor_comments
'Adding full bibliography for 7133345--7133348.cif.'
_cod_database_code               7133348
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C39H53N3Ti
_chemical_oxdiff_usercomment     n-hexane
_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.a Ternary CH refined with riding coordinates:
 C34(H34), C37(H37), C25(H25), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C31(H31), C30(H30), C11(H11), C12(H12), C13(H13), C18(H18),
 C20(H20), C19(H19)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C27(H27A,H27B,H27C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C6(H6A,H6B,
 H6C)
;
_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 1.910
_oxdiff_exptl_absorpt_empirical_full_min 0.791