Aromatic Imines in the Titanocene Coordination Sphere—Titanaaziridine vs 1-Aza-2-titanacyclopent-4-ene Structures
Loose, Florian; Plettenberg, Inka; Haase, Detlev; Saak, Wolfgang; Schmidtmann, Marc; Schäfer, André; Müller, Thomas; Beckhaus, Rüdiger; Organometallics 33 (2014) 6785–; doi:10.1021/om500750y

data_4084764
_publ_section_title
;
 Aromatic Imines in the Titanocene Coordination Sphere---Titanaaziridine
 vs 1-Aza-2-titanacyclopent-4-ene Structures
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6785
_journal_paper_doi               10.1021/om500750y
_journal_volume                  33
_journal_year                    2014
_chemical_formula_structural     TiCl(C10H15)(C21H19N)
_chemical_formula_sum            'C31 H34 Cl N Ti'
_chemical_formula_weight         503.94
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 100.2620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.4824(4)
_cell_length_b                   8.1061(2)
_cell_length_c                   39.8669(11)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.51
_cell_volume                     5241.3(2)
_computing_cell_refinement       'Bruker SAINT V8.27B'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.27B'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            74562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         2.077
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.9892
_exptl_absorpt_correction_T_min  0.8955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Sheldrick)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         7666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+5.0000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5782
_reflns_number_total             7666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500750y_si_001.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 4084761--4084765.cif.'
_cod_database_code               4084764
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.987