Reactions of Titanocene Bis(trimethylsilyl)acetylene Complexes with Carbodiimides: An Experimental and Theoretical Study of Complexation versus C-N Bond Activation
Martin Haehnel; Martin Ruhmann; Oliver Theilmann; Subhendu Roy; Torsten Beweries; Perdita Arndt; Anke Spannenberg; Alexander Villinger; Eluvathingal D. Jemmis; Axel Schulz; Uwe Rosenthal; Journal of the American Chemical Society 134 (2012) 15979–15991; doi:10.1021/ja3070649

data_4118676
_publ_section_title
;
 Reactions of Titanocene Bis(trimethylsilyl)acetylene Complexes with
 Carbodiimides: An Experimental and Theoretical Study of Complexation
 versus C-N Bond Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15979
_journal_page_last               15991
_journal_paper_doi               10.1021/ja3070649
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C34 H48 N4 Ti2'
_chemical_formula_sum            'C34 H48 N4 Ti2'
_chemical_formula_weight         608.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           121
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      121
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9445(3)
_cell_length_b                   8.9445(3)
_cell_length_c                   20.4004(14)
_cell_measurement_reflns_used    1417
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      49.900
_cell_measurement_theta_min      4.973
_cell_volume                     1632.12(14)
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_collection       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and psi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            4043
_diffrn_reflns_theta_full        29.03
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.9598
_exptl_absorpt_correction_T_min  0.8083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0622P)^2^+1.0914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                1036
_reflns_number_total             1191
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja3070649_si_001.cif
_cod_data_source_block           is_mr017
_cod_original_cell_volume        1632.11(14)
_cod_database_code               4118676