Reactions of Secondary Amines with Bis(η5:η1-pentafulvene)titanium Complexes: Formation of Titanium Amides and Titanaaziridines
Manßen, Manfred; Lauterbach, Nicolai; Woriescheck, Tim; Schmidtmann, Marc; Beckhaus, Rüdiger; Organometallics 36 (2017) 867–; doi:10.1021/acs.organomet.6b00915

data_4087093
_publ_section_title
;
 Reactions of Secondary Amines with Bis(\h5:\h1-pentafulvene)titanium
 Complexes: Formation of Titanium Amides and Titanaaziridines
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              867
_journal_paper_doi               10.1021/acs.organomet.6b00915
_journal_volume                  36
_journal_year                    2017
_chemical_formula_structural     Ti(C20H18)(C20H19)(C8H10N)
_chemical_formula_sum            'C48 H47 N Ti'
_chemical_formula_weight         685.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 91.599(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.960(3)
_cell_length_b                   17.433(4)
_cell_length_c                   16.575(4)
_cell_measurement_reflns_used    8802
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.46
_cell_volume                     3743.4(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.979
_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  0.0586
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            63403
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.572
_diffrn_reflns_theta_min         2.722
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_T_max  0.9051
_exptl_absorpt_correction_T_min  0.8919
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.380
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         9361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0447
_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^+0.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5439
_reflns_number_total             9361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00915_si_002.cif
_cod_data_source_block           2c
_cod_original_cell_volume        3743.3(15)
_cod_database_code               4087093
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.907
_shelx_res_checksum              36343
_shelx_hkl_checksum              6724