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_4084762
_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_sum            'C24 H23 N Ti'
_chemical_formula_weight         373.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.9609(2)
_cell_length_b                   16.6816(3)
_cell_length_c                   20.7506(4)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.90
_cell_measurement_theta_min      2.43
_cell_volume                     3794.15(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond (Crystal Impact, 2010)'
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63098
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.9304
_exptl_absorpt_correction_T_min  0.8697
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+2.1109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                3529
_reflns_number_total             5035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500750y_si_001.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4084761--4084765.cif.'
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4084762