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_4073955
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C45 H50 N4 Ti1'
_chemical_formula_sum            'C45 H50 N4 Ti'
_chemical_formula_weight         694.82
_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_block_code                ga_nv10
_audit_creation_date             07-06-13
_audit_creation_method           CRYSTALS_ver_12.50
_cell_angle_alpha                90
_cell_angle_beta                 102.73(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.081(6)
_cell_length_b                   13.029(3)
_cell_length_c                   21.530(4)
_cell_measurement_reflns_used    203516
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.574
_cell_measurement_theta_min      1.710
_cell_volume                     8231(3)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            203516
_diffrn_reflns_theta_full        29.574
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_min         1.710
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       regular
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
;
_refine_diff_density_max         0.79
_refine_diff_density_min         -1.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0351
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         11514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.0995
_refine_ls_shift/su_max          0.000293
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 p=(max(Fo^2^,0) + 2Fc^2^)/3 
 Method = SHELXL 97 (Sheldrick, 1997) 
 w=1/[sigma^2^(F^2^) + 0.00 +*****p] 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2367
_refine_ls_wR_factor_gt          0.2296
_refine_ls_wR_factor_ref         0.2367
_reflns_limit_h_max              40
_reflns_limit_h_min              -41
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                7970
_reflns_number_total             11545
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            om700758v-file001.cif
_cod_data_source_block           5b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C45 H50 N4 Ti1'
_cod_database_code               4073955