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_4066134
_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            'C38 H45 N3 Ti2'
_chemical_formula_weight         639.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_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            16
_cell_length_a                   23.7318(4)
_cell_length_b                   23.7318(4)
_cell_length_c                   23.7318(4)
_cell_measurement_reflns_used    10385
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.04
_cell_volume                     13365.7(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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0668
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            106041
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.8977
_exptl_absorpt_correction_T_min  0.8248
_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    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5408
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2687
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+16.1106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                2352
_reflns_number_total             2687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100306b_si_005.cif
_cod_data_source_block           ks1069
_cod_database_code               4066134