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_7133345
_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         'C37 H39 N3 Ti'
_chemical_formula_sum            'C37 H39 N3 Ti'
_chemical_formula_weight         573.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-14
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6089(2)
_cell_length_b                   14.6227(2)
_cell_length_c                   24.9167(3)
_cell_measurement_reflns_used    14222
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.7980
_cell_measurement_theta_min      3.5540
_cell_volume                     6051.44(13)
_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(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 0.999
_diffrn_measured_fraction_theta_max 0.948
_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  66.00   0.50    2.00    --   60.24 -97.00 161.00   92
  2  \w    -68.00 -21.00   0.50    2.00    --  -61.82  97.00 -90.00   94
  3  \w    -78.00 -38.00   0.50    2.00    --  -72.04  97.00 -90.00   80
  4  \w     33.00  58.00   0.50    6.00    --   73.62 -97.00 161.00   50
  5  \w     40.00  66.00   0.50    6.00    --   75.00 -97.00 161.00   52
  6  \w    -82.00 -57.00   0.50    6.00    --  -75.84  97.00 -90.00   50
  7  \w     44.00  88.00   0.50    6.00    --   83.27 -97.00 161.00   88
  8  \w     32.00  57.00   0.50    2.00    --   60.24 -95.00-120.00   50
  9  \w    -69.00 -33.00   0.50    2.00    --  -72.04 125.00   0.00   72
 10  \w     89.00 116.00   0.50    6.00    --   73.62  15.00  90.00   54
 11  \w     53.00  78.00   0.50    6.00    --   73.62 -95.00 120.00   50
 12  \w     33.00  58.00   0.50    6.00    --   73.62 -95.00 -90.00   50
 13  \w     59.00 120.00   0.50    6.00    --   73.62  15.00-150.00  122
 14  \w     59.00  84.00   0.50    6.00    --   73.62  15.00  90.00   50
 15  \w    -89.00 -57.00   0.50    6.00    --  -75.84 -15.00-120.00   64
 16  \w   -123.00 -95.00   0.50    6.00    --  -75.84 -15.00-120.00   56
 17  \w     45.00  87.00   0.50    6.00    --   83.27 -95.00  90.00   84
 18  \w     59.00 131.00   0.50    6.00    --   83.27  15.00 -90.00  144
;
_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      -0.0370011000
_diffrn_orient_matrix_UB_12      0.0801193000
_diffrn_orient_matrix_UB_13      0.0316969000
_diffrn_orient_matrix_UB_21      0.0755945000
_diffrn_orient_matrix_UB_22      0.0579447000
_diffrn_orient_matrix_UB_23      -0.0110911000
_diffrn_orient_matrix_UB_31      -0.0388253000
_diffrn_orient_matrix_UB_32      0.0365024000
_diffrn_orient_matrix_UB_33      -0.0519354000
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            30986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.077
_diffrn_reflns_theta_min         3.548
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.614
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.646
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       plate
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0635P)^2^+1.6948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5071
_reflns_number_total             5919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02500h2.cif
_cod_data_source_block           gahi006_op
_cod_depositor_comments
'Adding full bibliography for 7133345--7133348.cif.'
_cod_database_code               7133345
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H50 Ti N3'
_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:
 C1(H1A,H1B), C21(H21A,H21B), C15(H15A,H15B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C19(H19), C24(H24), C17(H17), C34(H34), C26(H26), C18(H18), C14(H14),
 C32(H32), C25(H25), C8(H8), C10(H10), C5(H5), C33(H33), C7(H7), C6(H6),
 C13(H13), C12(H12), C11(H11)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C28(H28A,H28B,H28C), C37(H37A,H37B,
 H37C)
;
_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 1.510
_oxdiff_exptl_absorpt_empirical_full_min 0.765