Reactions of Group 4 Metallocene Alkyne Complexes with Azobenzene: Formation of Diazametallacyclopropanes and N═N Bond Activation
Kaleta, Katharina; Arndt, Perdita; Beweries, Torsten; Spannenberg, Anke; Theilmann, Oliver; Rosenthal, Uwe; Organometallics 29 (2010) 2604–; doi:10.1021/om100306b

data_4066133
_publ_section_title
;
 Reactions of Group 4 Metallocene Alkyne Complexes with Azobenzene:
 Formation of Diazametallacyclopropanes and N&#x2550;N Bond Activation
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2604
_journal_paper_doi               10.1021/om100306b
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C51 H60 N4 Ti2'
_chemical_formula_weight         824.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 114.170(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8043(12)
_cell_length_b                   23.0575(11)
_cell_length_c                   9.4585(6)
_cell_measurement_reflns_used    3276
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.77
_cell_measurement_theta_min      2.03
_cell_volume                     4338.4(4)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       \w
_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  0.1111
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30700
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.9887
_exptl_absorpt_correction_T_min  0.6060
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4278
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                2661
_reflns_number_total             4278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100306b_si_004.cif
_cod_data_source_block           ks1098
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4066133