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_4065666
_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            'C47 H55 N Ti'
_chemical_formula_weight         681.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.898(3)
_cell_angle_beta                 82.947(3)
_cell_angle_gamma                66.625(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3527(5)
_cell_length_b                   12.7086(6)
_cell_length_c                   15.6582(7)
_cell_measurement_reflns_used    8300
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.11
_cell_measurement_theta_min      2.84
_cell_volume                     1816.67(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40975
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.9116
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         10585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0740P)^2^+0.7731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                7340
_reflns_number_total             10585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100056q_si_002.cif
_cod_data_source_block           6
_cod_original_cell_volume        1816.67(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065666