Crystal structure of the η<sup>4</sup>-ketimine titanium complex (di-phenyl-amido-κ<i>N</i>){3-methyl-6-[(4-methyl-phen-yl)(phenyl-aza-nid-yl)methyl-idene]cyclo-hexa-2,4-dien-1-yl-κ<sup>2</sup><i>N</i>,<i>C</i><sup>1</sup>}(η<sup>5</sup>-penta-methyl-cyclo-penta-dien-yl)titanium(IV).
Fischer, Malte; Schmidtmann, Marc; Beckhaus, Rüdiger; Acta crystallographica. Section E, Crystallographic communications 74 (2018) 34–37; doi:10.1107/S2056989017017455

data_2311557
_publ_section_title
;
 Crystal structure of the \h<sup>4</sup>-ketimine titanium complex
 (di-phenyl-amido-\k<i>N</i>){3-methyl-6-[(4-methyl-phen-yl)(phenyl-aza-nid-yl)methyl-idene]cyclo-hexa-2,4-dien-1-yl-\k<sup>2</sup><i>N</i>,<i>C</i><sup>1</sup>}(\h<sup>5</sup>-penta-methyl-cyclo-penta-dien-yl)titanium(IV).
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_journal_coeditor_code           WM5424
_journal_issue                   'Pt 1'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              34
_journal_page_last               37
_journal_paper_doi               10.1107/S2056989017017455
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Ti (C10 H15) (C21 H19 N) (C12 H10 N)]'
_chemical_formula_moiety         'C43 H44 N2 Ti'
_chemical_formula_sum            'C43 H44 N2 Ti'
_chemical_formula_weight         636.70
_chemical_name_systematic
(Diphenylamido-\k<i>N</i>){3-methyl-6-[(4-methylphenyl)(phenylazanidyl)methylidene]cyclohexa-2,4-dien-1-yl-\k^2^<i>N</i>,<i>C</i>^1^}(\h^5^-pentamethylcyclopentadienyl)titanium(IV)
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0633(4)
_cell_length_b                   20.0633(4)
_cell_length_c                   16.8156(4)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.27
_cell_volume                     6768.9(2)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            152032
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         1.435
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       'tetragonal prism'
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.529
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3640 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         9906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0600P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                8703
_reflns_number_total             9906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5424sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        6768.9(3)
_cod_database_code               2311557
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.961
_shelx_hkl_checksum              34372
_shelx_res_checksum              10741