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_4066132
_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            'C32 H40 N2 Ti'
_chemical_formula_weight         500.56
_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                 102.43(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.737(3)
_cell_length_b                   11.119(2)
_cell_length_c                   16.958(3)
_cell_measurement_reflns_used    6103
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.43
_cell_volume                     2713.6(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1121
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20198
_diffrn_reflns_theta_full        26.76
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2894
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0870P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                2188
_reflns_number_total             2894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100306b_si_003.cif
_cod_data_source_block           ks1110m
_cod_original_cell_volume        2713.7(9)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4066132