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_4084761
_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            'C21 H19 N'
_chemical_formula_weight         285.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 100.419(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.0410(5)
_cell_length_b                   16.7131(8)
_cell_length_c                   17.6947(7)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.52
_cell_measurement_theta_min      2.64
_cell_volume                     3211.4(2)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48346
_diffrn_reflns_theta_full        32.61
_diffrn_reflns_theta_max         32.61
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9849
_exptl_absorpt_correction_T_min  0.9730
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         11616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.6258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                8335
_reflns_number_total             11616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500750y_si_001.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4084761--4084765.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4084761