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_4073954
_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         'C34 H43 N5 Ti1'
_chemical_formula_sum            'C34 H43 N5 Ti'
_chemical_formula_weight         569.65
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_code                ga_nv5
_cell_angle_alpha                90
_cell_angle_beta                 93.924(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.650(6)
_cell_length_b                   20.362(13)
_cell_length_c                   17.777(11)
_cell_measurement_reflns_used    6839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.732
_cell_measurement_theta_min      1.523
_cell_volume                     3124(4)
_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    'SIR92 (Altomare et al., 1994)'
_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       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            77092
_diffrn_reflns_theta_full        26.732
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.523
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004-2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8625
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6606
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.006382
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 29.0 44.6 23.7 9.04 1.98 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1553
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1553
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                4508
_reflns_number_total             6633
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            om700758v-file001.cif
_cod_data_source_block           3c
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3124(3)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C34 H43 N5 Ti1'
_cod_database_code               4073954