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_4087097
_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     Ti2(C15H19)4(C16H10)
_chemical_formula_sum            'C76 H86 Ti2'
_chemical_formula_weight         1095.24
_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                 102.7831(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7939(7)
_cell_length_b                   16.5637(9)
_cell_length_c                   13.3367(7)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.46
_cell_volume                     2756.2(3)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            80722
_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         1.632
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Sheldrick)'
_exptl_crystal_colour            'dark green brown'
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         8048
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0378
_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^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6572
_reflns_number_total             8048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00915_si_002.cif
_cod_data_source_block           7
_cod_database_code               4087097
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              32457
_shelx_hkl_checksum              41426