A mononuclear, terminal titanium(III) imido.
Mohar, Jacob S.; Reinholdt, Anders; Keller, Taylor M.; Carroll, Patrick J.; Telser, Joshua; Mindiola, Daniel J.; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc01758c

data_7131859
_publ_section_title
;
 A mononuclear, terminal titanium(III) imido.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc01758c
_journal_year                    2023
_chemical_formula_moiety         'C31 H57 B N7 O Si Ti, 0.5(C5 H12)'
_chemical_formula_sum            'C33.5 H63 B N7 O Si Ti'
_chemical_formula_weight         666.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-24
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-15 deposited with the CCDC.	2023-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.9280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9991(2)
_cell_length_b                   26.3427(3)
_cell_length_c                   12.1440(2)
_cell_measurement_reflns_used    67969
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.0490
_cell_measurement_theta_min      2.2650
_cell_volume                     3818.05(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix 3000HE'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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     17.00  55.00   0.50   27.00    --  -14.00  52.00  21.00   76
  2  \w    -47.00 -22.00   0.50   27.00    --   14.62 -52.00-123.00   50
  3  \w     36.00  83.00   0.50   27.00    --   14.62  52.00  21.00   94
  4  \w     -2.00  31.00   0.50   27.00    --   14.62  52.00  21.00   66
  5  \w    -81.00 -20.00   0.50   27.00    --  -14.00 -37.00  90.00  122
  6  \w    -15.00  13.00   0.50   27.00    --  -14.00 -79.00 149.75   56
  7  \w    -18.00  13.00   0.50   27.00    --  -14.00 -80.00 -60.65   62
  8  \w    -36.00  12.00   0.50   27.00    --  -14.00  57.00-150.00   96
  9  \w    -25.00   0.00   0.50   27.00    --  -14.00 -77.00  90.00   50
 10  \w    -14.00  14.00   0.50   27.00    --  -14.00 -80.00  80.29   56
 11  \w    -37.00  59.00   0.50   27.00    --  -14.00  19.00   0.00  192
 12  \w    -14.00  11.00   0.50   27.00    --  -14.00 -77.00  30.00   50
 13  \w    -18.00   8.00   0.50   27.00    --  -14.00 -80.00 -19.48   52
 14  \w     25.00  54.00   0.50   27.00    --  -14.00  57.00-150.00   58
 15  \w    -22.00   9.00   0.50   27.00    --  -14.00 -80.00 -94.51   62
 16  \w    -24.00   2.00   0.50   27.00    --  -14.00 -77.00   0.00   52
 17  \w    -13.00  15.00   0.50   27.00    --  -14.00 -80.00-156.12   56
 18  \w     15.00  54.00   0.50   27.00    --  -14.00  57.00  30.00   78
 19  \w    -80.00 -16.00   0.50   27.00    --  -14.00 -52.00-123.00  128
 20  \w    -21.00  12.00   0.50   27.00    --  -14.00 -80.00  70.43   66
 21  \w    -25.00   0.00   0.50   27.00    --  -14.00 -77.00 120.00   50
 22  \w    -20.00   5.00   0.50   27.00    --  -14.00 -80.00 145.63   50
 23  \w    -36.00  10.00   0.50   27.00    --  -14.00  57.00  30.00   92
 24  \w     14.00  46.00   0.50   27.00    --   14.62  37.00 150.00   64
 25  \w    -17.00  38.00   0.50   27.00    --   14.62 -80.00-100.08  110
 26  \w     13.00  81.00   0.50   27.00    --   14.62  37.00-150.00  136
 27  \w    -22.00  29.00   0.50   27.00    --   14.62 -80.00 -35.08  102
 28  \w     15.00  57.00   0.50   27.00    --   14.62  57.00  90.00   84
 29  \w    -24.00  23.00   0.50   27.00    --   14.62 -78.00-123.58   94
 30  \w    -58.00   4.00   0.50   27.00    --   14.62 -19.00 -60.00  124
 31  \w    -59.00  -2.00   0.50   27.00    --   14.62 -19.00 150.00  114
 32  \w    -32.00  -6.00   0.50   27.00    --   14.62 -19.00-120.00   52
 33  \w      7.00  32.00   0.50   27.00    --   14.62  57.00  60.00   50
 34  \w     54.00  83.00   0.50   27.00    --   14.62  37.00 150.00   58
 35  \w    -22.00  39.00   0.50   27.00    --   14.62 -76.00-153.29  122
 36  \w     -3.00  28.00   0.50   27.00    --   14.62 -79.00  84.49   62
 37  \w     -8.00  51.00   0.50   27.00    --   14.62  57.00-180.00  118
 38  \w    -49.00 -23.00   0.50   27.00    --   14.62 -37.00-120.00   52
 39  \w    -12.00  18.00   0.50   27.00    --   14.62  80.00 -46.52   60
 40  \w    -58.00   4.00   0.50   27.00    --   14.62 -19.00  30.00  124
 41  \w     -6.00  22.00   0.50   27.00    --   14.62  80.00  88.62   56
 42  \w     13.00  44.00   0.50   27.00    --   14.62 -80.00-164.36   62
 43  \w    -52.00  15.00   0.50   27.00    --   14.62 -57.00  90.00  134
 44  \w    -13.00  39.00   0.50   27.00    --   14.62 -77.00 -90.00  104
 45  \w    -20.00   8.00   0.50   27.00    --   14.62 -80.00-164.36   56
 46  \w    -23.00  43.00   0.50   27.00    --   14.62 -79.00  48.38  132
 47  \w    -13.00  22.00   0.50   27.00    --   14.62  80.00  11.18   70
 48  \w    -58.00   3.00   0.50   27.00    --   14.62 -19.00  90.00  122
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-i'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0530732000
_diffrn_orient_matrix_UB_12      -0.0107430000
_diffrn_orient_matrix_UB_13      -0.0176070000
_diffrn_orient_matrix_UB_21      -0.0237651000
_diffrn_orient_matrix_UB_22      0.0131340000
_diffrn_orient_matrix_UB_23      0.0428305000
_diffrn_orient_matrix_UB_31      -0.0122794000
_diffrn_orient_matrix_UB_32      0.0209104000
_diffrn_orient_matrix_UB_33      -0.0360932000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            123109
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.153
_diffrn_reflns_theta_min         1.855
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            'yellowish red'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.663
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         17709
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0701
_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^)+(0.1076P)^2^+3.5719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1901
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.919
_reflns_number_gt                14536
_reflns_number_total             17709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01758c2.cif
_cod_data_source_block           jm_processed_2
_cod_original_formula_sum        'C33.50 H63 B N7 O Si Ti'
_cod_database_code               7131859
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C31H57BN7OSiTi
_chemical_oxdiff_usercomment     'Orange Blocks- grown from Pentane v Toluene'
_shelx_res_checksum              64498
_shelx_hkl_checksum              65764
_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 1.346
_oxdiff_exptl_absorpt_empirical_full_min 0.607