Bis(η5:η1-pentafulvene)titanium Complexes: Catalysts for Intramolecular Alkene Hydroamination and Reagents for Selective Reactions with N−H Acidic Substrates†
Janssen, Thomas; Severin, René; Diekmann, Mira; Friedemann, Marion; Haase, Detlev; Saak, Wolfgang; Doye, Sven; Beckhaus, Rüdiger; Organometallics 29 (2010) 1806–; doi:10.1021/om100056q

data_4065665
_publ_section_title
;
 Bis(\h5:\h1-pentafulvene)titanium Complexes: Catalysts for Intramolecular
 Alkene Hydroamination and Reagents for Selective Reactions with
 N&#x2212;H Acidic Substrates&#x2020;
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1806
_journal_paper_doi               10.1021/om100056q
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C50 H54 N2 Ti'
_chemical_formula_weight         730.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            4
_cell_length_a                   27.621(4)
_cell_length_b                   8.5889(10)
_cell_length_c                   16.100(2)
_cell_measurement_reflns_used    7891
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.45
_cell_volume                     3819.5(9)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'XRED (Stoe, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.1581
_diffrn_reflns_av_sigmaI/netI    0.1191
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31194
_diffrn_reflns_theta_full        26.08
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_T_max  0.9767
_exptl_absorpt_correction_T_min  0.9137
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.770
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.770
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0905
_reflns_number_gt                1997
_reflns_number_total             3740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100056q_si_002.cif
_cod_data_source_block           5d
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4065665