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_7133347
_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         'C45 H55 N3 Ti'
_chemical_formula_sum            'C45 H55 N3 Ti'
_chemical_formula_weight         685.82
_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             2023-11-20
_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                71.4210(10)
_cell_angle_beta                 85.3130(10)
_cell_angle_gamma                66.8060(10)
_cell_formula_units_Z            2
_cell_length_a                   10.13950(10)
_cell_length_b                   12.81710(10)
_cell_length_c                   16.65920(10)
_cell_measurement_reflns_used    21159
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      73.8920
_cell_measurement_theta_min      2.7930
_cell_volume                     1883.94(3)
_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      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.957
_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     20.00  87.00   0.50    0.25    --   58.75-126.00-180.00  134
  2  \w     29.00  79.00   0.50    0.25    --   71.46 -95.00-120.00  100
  3  \w     16.00  66.00   0.50    0.25    --   58.75 -95.00  30.00  100
  4  \w     31.00  93.00   0.50    0.25    --   76.32-112.00 120.00  124
  5  \w     31.00  93.00   0.50    0.25    --   76.32-112.00  30.00  124
  6  \w     34.00  84.00   0.50    0.25    --   76.32 -95.00 -30.00  100
  7  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00 -60.00  100
  8  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00-120.00  100
  9  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00-180.00  100
 10  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00-150.00  100
 11  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00 -90.00  100
 12  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00   0.00  100
 13  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00  60.00  100
 14  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00  90.00  100
 15  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00 150.00  100
 16  \w     42.00  92.00   0.50    0.25    --   84.34 -95.00 120.00  100
 17  \w    -82.00 -35.00   0.50    0.25    --  -30.00 -26.00-134.07   94
 18  \w   -102.00 -51.00   0.50    0.25    --  -50.00 -24.00-172.79  102
 19  \w    -94.00 -47.00   0.50    0.25    --  -42.00 -26.00  36.67   94
 20  \w   -102.00 -54.00   0.50    0.25    --  -50.00 -25.00 122.78   96
 21  \w    -98.00 -50.00   0.50    0.25    --  -46.00 -25.00  72.69   96
 22  \w   -132.00 -85.00   0.50    0.25    --  -79.50 -26.00 -29.90   94
 23  \w   -106.00 -58.00   0.50    0.25    --  -54.00 -25.00 -40.42   96
 24  \w   -122.00 -68.00   0.50    0.25    --  -70.00 -23.00   5.07  108
 25  \w   -132.00 -85.00   0.50    0.25    --  -79.50 -26.00  83.06   94
 26  \w   -132.00 -85.00   0.50    0.25    --  -79.50 -26.00 116.38   94
 27  \w   -132.00 -85.00   0.50    0.25    --  -79.50 -26.00 173.88   94
 28  \w   -131.00 -73.00   0.50    0.25    --  -79.50 -22.00  36.59  116
 29  \w   -114.00 -50.00   0.50    0.25    --  -62.00 -21.00 -90.14  128
 30  \w   -122.00 -68.00   0.50    0.25    --  -70.00 -23.00-121.16  108
 31  \w   -131.00 -73.00   0.50    0.25    --  -79.50 -22.00-161.62  116
 32  \w   -131.00 -65.00   0.50    0.25    --  -79.50 -19.00-100.99  132
 33  \w   -113.00 -49.00   0.50    0.25    --  -62.00 -20.00 130.00  128
 34  \w   -102.00 -32.00   0.50    0.25    --  -79.50 129.00 127.55  140
 35  \w    -98.00 -22.00   0.50    0.25    --  -69.85 126.00 150.00  152
 36  \w    -98.00 -22.00   0.50    0.25    --  -69.85 126.00  30.00  152
 37  \w    -98.00 -22.00   0.50    0.25    --  -69.85 126.00 -90.00  152
 38  \w    -92.00 -31.00   0.50    0.25    --  -76.37 112.00-120.00  122
 39  \w    -98.00 -22.00   0.50    0.25    --  -69.85 126.00-150.00  152
 40  \w    -92.00 -31.00   0.50    0.25    --  -76.37 112.00   0.00  122
;
_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      0.0763333000
_diffrn_orient_matrix_UB_12      -0.1069360000
_diffrn_orient_matrix_UB_13      -0.0335981000
_diffrn_orient_matrix_UB_21      -0.0701906000
_diffrn_orient_matrix_UB_22      -0.0737321000
_diffrn_orient_matrix_UB_23      0.0670025000
_diffrn_orient_matrix_UB_31      -0.1289905000
_diffrn_orient_matrix_UB_32      0.0456124000
_diffrn_orient_matrix_UB_33      -0.0626398000
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34556
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.581
_diffrn_reflns_theta_min         2.802
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.176
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.740
_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_density_diffrn    1.209
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0472P)^2^+0.7273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7029
_reflns_number_total             7378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02500h2.cif
_cod_data_source_block           gahi001_ap
_cod_depositor_comments
'Adding full bibliography for 7133345--7133348.cif.'
_cod_database_code               7133347
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C45 H55 N3 Ti'
_chemical_oxdiff_usercomment     PF012
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.733
_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:
 C43(H43), C28(H28), C31(H31), C40(H40)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C1(H1A,H1B), C21(H21A,H21B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C25(H25), C24(H24), C38(H38), C26(H26), C4(H4), C36(H36),
 C18(H18), C10(H10), C8(H8), C14(H14), C37(H37), C11(H11), C13(H13), C5(H5),
 C7(H7), C12(H12), C6(H6)
2.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C32(H32A,H32B,H32C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C45(H45A,H45B,H45C), C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C41(H41A,
 H41B,H41C)
;
_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 1.811
_oxdiff_exptl_absorpt_empirical_full_min 0.776