C−N Coupling Reactions of Allenes and Methylacetylenes with an Imidotitanium Complex
Trösch, Dominique J. M.; Collier, Philip E.; Bashall, Alan; Gade, Lutz H.; McPartlin, Mary; Mountford, Philip; Radojevic, Sanja; Organometallics 20 (2001) 3308–; doi:10.1021/om010253g

data_4077332
_publ_section_title
;
 C&#x2212;N Coupling Reactions of Allenes and Methylacetylenes with an
 Imidotitanium Complex
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3308
_journal_paper_doi               10.1021/om010253g
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C23 H44 N4 Si2 Ti'
_chemical_formula_weight         480.70
_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                 100.50(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.721(7)
_cell_length_b                   10.450(2)
_cell_length_c                   18.866(4)
_cell_measurement_temperature    223(2)
_cell_volume                     5568(2)
_computing_cell_refinement       'Siemens XSCAN'
_computing_data_collection       'Siemens XSCAN'
_computing_data_reduction        'Siemens XSCAN'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       theta/2theta
_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  0.0893
_diffrn_reflns_av_sigmaI/netI    0.2039
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4176
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   semi-emprical
_exptl_absorpt_process_details   psi-scans
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3391
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      0.860
_refine_ls_R_factor_all          0.1821
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                1422
_reflns_number_total             3391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010253g.cif
_cod_data_source_block           sy333
_cod_original_cell_volume        5567(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4077332