Highly Reactive Metal−Nitrogen Bond Induced C−H Bond Activation and Azametallacycle Formation
Panda, Tarun K.; Tsurugi, Hayato; Pal, Kuntal; Kaneko, Hiroshi; Mashima, Kazushi; Organometallics 29 (2010) 34–; doi:10.1021/om901027v

data_4067590
_publ_section_title
;
 Highly Reactive Metal&#x2212;Nitrogen Bond Induced C&#x2212;H Bond
 Activation and Azametallacycle Formation
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              34
_journal_paper_doi               10.1021/om901027v
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C21 H46 N6 Ti'
_chemical_formula_sum            'C21 H46 N6 Ti'
_chemical_formula_weight         430.51
_chemical_name_common            3a
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 105.929(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.776(5)
_cell_length_b                   11.125(5)
_cell_length_c                   18.248(5)
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      3.1
_cell_volume                     2494.1(16)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'teXan (Rigaku/MSC, 2004)'
_computing_molecular_graphics    Ortep-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR 97'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1957
_diffrn_reflns_av_sigmaI/netI    0.2055
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42843
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Higashi, H. (1995), ABSCOR: Program for Absorption
Correction, Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.063
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         7568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                4377
_reflns_number_total             7568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901027v_si_002.cif
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4067590