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_7131857
_publ_section_title
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 A mononuclear, terminal titanium(III) imido.
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_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc01758c
_journal_year                    2023
_chemical_formula_moiety         'C27 H49 B F N7 Si Ti'
_chemical_formula_sum            'C27 H49 B F N7 Si Ti'
_chemical_formula_weight         577.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2023-03-15 deposited with the CCDC.	2023-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   60.7204(15)
_cell_length_b                   21.7118(6)
_cell_length_c                   10.0607(2)
_cell_measurement_reflns_used    19270
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.5360
_cell_measurement_theta_min      2.2940
_cell_volume                     13263.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_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 10.0
_diffrn_detector_type            'Dectris Pilatus3 R 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_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    -25.00  30.00   0.50   90.00    --    6.66 -77.00 -30.00  110
  2  \w     -9.00  59.00   0.50   90.00    --    6.66  57.00-180.00  136
  3  \w    -17.00  25.00   0.50   90.00    --    6.66  77.00-120.00   84
  4  \w    -73.00   5.00   0.50   90.00    --    6.66 -19.00-120.00  156
  5  \w    -73.00 -35.00   0.50   90.00    --    6.66 -19.00-180.00   76
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0105530000
_diffrn_orient_matrix_UB_12      0.0137235000
_diffrn_orient_matrix_UB_13      -0.0059696000
_diffrn_orient_matrix_UB_21      0.0047336000
_diffrn_orient_matrix_UB_22      -0.0253308000
_diffrn_orient_matrix_UB_23      0.0341395000
_diffrn_orient_matrix_UB_31      0.0016080000
_diffrn_orient_matrix_UB_32      -0.0154122000
_diffrn_orient_matrix_UB_33      -0.0614058000
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       76
_diffrn_reflns_limit_h_min       -79
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31428
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         1.992
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       plank
_exptl_crystal_F_000             4960
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 3330 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7966
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+6.8356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                7612
_reflns_number_total             7966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01758c2.cif
_cod_data_source_block           90004_4
_cod_database_code               7131857
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C27H49BFN7SiTi
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.854
_shelx_res_checksum              20430
_shelx_hkl_checksum              90978
_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 1.577
_oxdiff_exptl_absorpt_empirical_full_min 0.504