Imido-Alkyne Coupling in Titanium Complexes: New Insights into the Alkyne Hydroamination Reaction
Vujkovic, Nadia; Ward, Benjamin D.; Maisse-François, Aline; Wadepohl, Hubert; Mountford, Philip; Gade, Lutz H.; Organometallics 26 (2007) 5522–; doi:10.1021/om700758v

data_4073952
_publ_section_title
;
 Imido-Alkyne Coupling in Titanium Complexes:&#x00A0; New Insights into
 the Alkyne Hydroamination Reaction
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5522
_journal_paper_doi               10.1021/om700758v
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C34 H45 N5 Ti'
_chemical_formula_sum            'C34 H45 N5 Ti'
_chemical_formula_weight         571.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_block_code                st1464new
_cell_angle_alpha                90
_cell_angle_beta                 98.831(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7877(2)
_cell_length_b                   11.6261(3)
_cell_length_c                   25.8717(7)
_cell_measurement_temperature    173
_cell_volume                     3206.33(14)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
   7708 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  36. mm.
 Scan angle =  1.6 deg 1 scans of   60 sec per frame.
 Data collection was divided into  2 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    8.80 Omega =    0.00 Kappa =    0.00  202 frames
 Set 2 Theta =   -8.20 Kappa = -168.00 Phi   =    0.00   46 frames
 Friedel pairs were not averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            7708
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.18
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.876
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.238
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3591
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.110
_refine_ls_R_factor_gt           0.087
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.014
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.209
_refine_ls_wR_factor_ref         0.101
_reflns_number_gt                3591
_reflns_number_total             7708
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            om700758v-file001.cif
_cod_data_source_block           2a
_cod_original_cell_volume        3206.3(1)
_cod_database_code               4073952