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_7133346
_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         'C30 H31 N3 Ti'
_chemical_formula_sum            'C30 H31 N3 Ti'
_chemical_formula_weight         481.48
_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     dual
_audit_creation_date             2024-07-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-05 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.6090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5575(2)
_cell_length_b                   17.8865(3)
_cell_length_c                   11.9883(2)
_cell_measurement_reflns_used    12822
_cell_measurement_temperature    100.4(9)
_cell_measurement_theta_max      73.9700
_cell_measurement_theta_min      3.9180
_cell_volume                     2408.68(7)
_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      100.4(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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  77.00   0.50    0.50    --   59.77-125.00 150.00   94
  2  \w     20.00  51.00   0.50    0.50    --   59.77 -95.00-150.00   62
  3  \w    -71.00 -21.00   0.50    0.50    --  -61.73 125.00 120.00  100
  4  \w   -121.00 -88.00   0.50    2.00    --  -76.34 -15.00 120.00   66
  5  \w    -68.00 -34.00   0.50    2.00    --  -76.34 112.00-120.00   68
  6  \w   -112.00 -56.00   0.50    2.00    --  -76.34 -15.00-120.00  112
  7  \w   -114.00 -63.00   0.50    2.00    --  -76.34 -15.00 -30.00  102
  8  \w    -91.00 -65.00   0.50    2.00    --  -79.50 130.00 115.20   52
  9  \w    -98.00 -72.00   0.50    2.00    --  -79.50 120.00 158.45   52
 10  \w     49.00  75.00   0.50    2.00    --   80.34 -95.00 150.00   52
 11  \w     54.00  98.00   0.50    2.00    --   80.34  15.00 -90.00   88
 12  \w     88.00 125.00   0.50    2.00    --   80.34  15.00 -60.00   74
 13  \w     44.00  82.00   0.50    2.00    --   80.34 -95.00  90.00   76
 14  \w     40.00  65.00   0.50    2.00    --   80.34 -95.00-120.00   50
 15  \w     41.00  75.00   0.50    2.00    --   80.34-112.00  30.00   68
 16  \w     58.00  94.00   0.50    2.00    --   80.34  15.00  60.00   72
 17  \w     42.00  82.00   0.50    2.00    --   80.34 -95.00  60.00   80
 18  \w     37.00  62.00   0.50    2.00    --   80.34-112.00  90.00   50
 19  \w     86.00 127.00   0.50    2.00    --   80.34  15.00 150.00   82
 20  \w     41.00  66.00   0.50    2.00    --   80.34-112.00 -60.00   50
 21  \w     44.00  69.00   0.50    2.00    --   80.34 -95.00 -30.00   50
 22  \w     59.00  85.00   0.50    2.00    --   80.34  15.00 150.00   52
 23  \w     42.00  81.00   0.50    2.00    --   80.34 -95.00-180.00   78
 24  \w     39.00  91.00   0.50    2.00    --   80.34-112.00 -90.00  104
 25  \w     38.00  92.00   0.50    2.00    --   80.34-112.00 -30.00  108
 26  \w     44.00  69.00   0.50    2.00    --   80.34 -95.00   0.00   50
 27  \w     57.00  82.00   0.50    2.00    --   80.34 -95.00  30.00   50
 28  \w     41.00  66.00   0.50    2.00    --   80.34 -95.00 120.00   50
 29  \w     55.00  92.00   0.50    2.00    --   80.34-112.00-180.00   74
 30  \w     54.00  89.00   0.50    2.00    --   80.34-112.00-120.00   70
 31  \w     40.00  65.00   0.50    2.00    --   80.34 -95.00-150.00   50
 32  \w     99.00 127.00   0.50    2.00    --   80.34  15.00  60.00   56
 33  \w     37.00  62.00   0.50    2.00    --   80.34-112.00-150.00   50
 34  \w     37.00  62.00   0.50    2.00    --   80.34-112.00   0.00   50
 35  \w     81.00 110.00   0.50    2.00    --   80.34  15.00-150.00   58
 36  \w    101.00 126.00   0.50    2.00    --   80.34  15.00  90.00   50
 37  \w     46.00  75.00   0.50    2.00    --   83.50 -76.00  70.91   58
;
_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      0.0381940000
_diffrn_orient_matrix_UB_12      -0.0796342000
_diffrn_orient_matrix_UB_13      -0.0247496000
_diffrn_orient_matrix_UB_21      0.0990741000
_diffrn_orient_matrix_UB_22      0.0019494000
_diffrn_orient_matrix_UB_23      0.1112981000
_diffrn_orient_matrix_UB_31      -0.0867571000
_diffrn_orient_matrix_UB_32      -0.0327865000
_diffrn_orient_matrix_UB_33      0.0669804000
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25101
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.170
_diffrn_reflns_theta_min         3.935
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.178
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.721
_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    1.328
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0685P)^2^+0.7734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4230
_reflns_number_total             4851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02500h2.cif
_cod_data_source_block           gahi017_mp
_cod_depositor_comments
'Adding full bibliography for 7133345--7133348.cif.'
_cod_database_code               7133346
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H31N3Ti
_chemical_oxdiff_usercomment     'orange plates'
_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 Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C7(H7A,H7B), C24(H24A,H24B), C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C26(H26), C5(H5), C3(H3), C30(H30), C20(H20), C11(H11),
 C18(H18), C4(H4), C29(H29), C19(H19), C28(H28), C27(H27)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C)
;
_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 1.638
_oxdiff_exptl_absorpt_empirical_full_min 0.662