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_4077333
_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            'C28 H46 N4 Si2 Ti'
_chemical_formula_weight         542.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           Pna2(1)
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            8
_cell_length_a                   21.060(5)
_cell_length_b                   10.250(4)
_cell_length_c                   30.243(12)
_cell_measurement_temperature    293(2)
_cell_volume                     6528(4)
_computing_cell_refinement       'SIEMENS XSCANS'
_computing_data_collection       'SIEMENS XSCANS'
_computing_data_reduction        'SIEMENS XSCANS'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1010
_diffrn_reflns_av_sigmaI/netI    0.2133
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4584
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        21
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.6558
_exptl_absorpt_correction_T_min  0.5604
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         3769
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.2633
_refine_ls_R_factor_gt           0.0980
_refine_ls_shift/su_max          0.557
_refine_ls_shift/su_mean         0.096
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2162
_refine_ls_wR_factor_ref         0.2802
_reflns_number_gt                1314
_reflns_number_total             3769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010253g.cif
_cod_data_source_block           mx389
_cod_original_cell_volume        6529(4)
_cod_original_sg_symbol_H-M      orthorhombic
_cod_database_code               4077333