AlMe3 and ZnMe2 Adducts of a Titanium Imido Methyl Cation: A Combined Crystallographic, Spectroscopic, and DFT Study
Paul D. Bolton; Eric Clot; Andrew R. Cowley; Philip Mountford; Journal of the American Chemical Society 128 (2006) 15005–15018; doi:10.1021/ja065638a

data_4111110
_publ_contact_author
;
 Professor P. Mountford           
 Chemistry Research Laboratory
 University of Oxford
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 285141'
_publ_contact_author_phone       '+44 1865 285140'
_publ_section_title
;
 AlMe3 and ZnMe2 Adducts of a Titanium Imido Methyl Cation: A Combined
 Crystallographic, Spectroscopic, and DFT Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15005
_journal_page_last               15018
_journal_paper_doi               10.1021/ja065638a
_journal_volume                  128
_journal_year                    2006
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C17 H42 Al N4 Ti, C24 B F20, C H2 Cl2 '
_chemical_formula_sum            'C42 H44 Al B Cl2 F20 N4 Ti'
_chemical_formula_weight         1141.40
_chemical_name_systematic
; 
[Ti(NtBu)(Me3[9]aneN3)(u-Me)2AlMe2][B(C6F5)4]
;
_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_creation_date             23-07-06
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 109.7558(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7837(2)
_cell_length_b                   19.5766(3)
_cell_length_c                   18.6673(2)
_cell_measurement_reflns_used    47232
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     4740.67(11)
_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_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.047
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47232
_diffrn_reflns_theta_full        27.482
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         5.110
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' orange-yellow '
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_thermal_history
; 
The material was crystallised at ambient temperature. A suitable crystal 
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. 
;
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         7266
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.045157
_refine_ls_structure_factor_coef F
_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: 
 1.85 -0.349 1.07 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0533
_refine_ls_wR_factor_gt          0.0371
_refine_ls_wR_factor_ref         0.0371
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7266
_reflns_number_total             10760
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ja065638asi20060803_061850.cif
_cod_data_source_block           Compound_7
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C42 H44 Al B Cl2 F20 N4 Ti '
_cod_database_code               4111110