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_4075182
_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
;
?
;
_chemical_formula_moiety         ' C33 H13 B1 Cl1 F20 N1 '
_chemical_formula_sum            'C33 H13 B Cl F20 N'
_chemical_formula_weight         849.70
_chemical_name_systematic
;                                      
 [PhNMe2(CH2Cl)][B(ArF)4]          
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.8835(2)
_cell_length_b                   18.8229(3)
_cell_length_c                   24.5280(5)
_cell_measurement_reflns_used    7675
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     6409.85(19)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 SIR97 (Altomare et al, 1999) 
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
; 
Enraf Nonius Kappa CCD 
;
_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  0.02
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14358
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             3363.970
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_refine_diff_density_max         0.75
_refine_diff_density_min         -0.60
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       196.2(263)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0698
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         3795
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000284
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Tukey and Prince 
 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 
 
 0.443 0.145 0.157
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0396
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                3795
_reflns_number_total             7304
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            om060096rsi20060131_031028.cif
_cod_data_source_block           compound_12-B(ArF)4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic ' changed to
'orthorhombic' 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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        6409.8(2)
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        ' C33 H13 B1 Cl1 F20 N1 '
_cod_database_code               4075182