Experimental and DFT Studies of Cationic Imido Titanium Alkyls: Agostic Interactions and C−H Bond and Solvent Activation Reactions of Isolobal Analogues of Group 4 Metallocenium Cations
Bolton, Paul D.; Clot, Eric; Adams, Nico; Dubberley, Stuart R.; Cowley, Andrew R.; Mountford, Philip; Organometallics 25 (2006) 2806–; doi:10.1021/om060096r

data_4075181
_publ_section_title
;
 Experimental and DFT Studies of Cationic Imido Titanium Alkyls:&#x00A0;
 Agostic Interactions and C&#x2212;H Bond and Solvent Activation Reactions
 of Isolobal Analogues of Group 4 Metallocenium Cations
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2806
_journal_paper_doi               10.1021/om060096r
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C42 H35 B1 Cl1 F20 N5 Ti1 '
_chemical_formula_sum            'C42 H35 B Cl F20 N5 Ti'
_chemical_formula_weight         1083.90
_chemical_name_systematic
;                                                             
[Ti(tBu)(Me3[9]aneN3)Cl(py)][B(ArF)4]
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.9546(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1935(2)
_cell_length_b                   21.1046(3)
_cell_length_c                   15.6878(3)
_cell_measurement_reflns_used    46808
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     4367.56(12)
_computing_cell_refinement
;                                                             
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)          
;
_computing_data_collection
;                                                             
KappaCCD software 'Collect' (Nonius, 2000)                    
;
_computing_data_reduction
;                                                             
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)          
;
_computing_publication_material
;                                                             
CRYSTALS (Watkin et al, 2001)                                 
;
_computing_structure_refinement
;                                                             
CRYSTALS (Watkin et al, 2001)                                 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;                                                             
Nonius KappaCCD                                               
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46808
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         5.11
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' pale orange '
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             2186.739
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.81
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0386
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         5541
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.023421
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979)
0.931    0.531    0.506    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0680
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5541
_reflns_number_total             9953
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            om060096rsi20060131_031028.cif
_cod_data_source_block           compound_9-B(ArF)4
_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_cell_volume        4367.6(1)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C42 H35 B1 Cl1 F20 N5 Ti1 '
_cod_database_code               4075181