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_4087098
_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_absolute_configuration ad
_chemical_formula_structural     Ti(C15H19)(C17H24ONSi(CH3)3)(C25H37O)
_chemical_formula_sum            'C66 H103 N O2 Si Ti'
_chemical_formula_weight         1018.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 101.0497(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8512(10)
_cell_length_b                   20.3693(18)
_cell_length_c                   12.3394(11)
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.95
_cell_measurement_theta_min      2.40
_cell_volume                     2923.5(4)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(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  0.0335
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            135945
_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         34.971
_diffrn_reflns_theta_min         1.681
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Sheldrick)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 10755 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         25685
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0500P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                23804
_reflns_number_total             25685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00915_si_002.cif
_cod_data_source_block           8
_cod_database_code               4087098
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              30180
_shelx_hkl_checksum              64473