Ti(NMe2)4and [HNMe2Ph][B(C6F5)4]: A Convenient Blend for Effective Catalytic Carboamination of Alkynes
Aneetha, Halikhedkar; Basuli, Falguni; Bollinger, John; Huffman, John C.; Mindiola, Daniel J.; Organometallics 25 (2006) 2402–; doi:10.1021/om0602207

data_4075329
_publ_section_title
;
 Ti(NMe2)4and [HNMe2Ph][B(C6F5)4]:&#x00A0; A Convenient Blend for
 Effective Catalytic Carboamination of Alkynes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2402
_journal_paper_doi               10.1021/om0602207
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C8 H25 N4 Ti +, C24 B F20 -'
_chemical_formula_structural     '(Ti (N H (C H3)2) (N (C H3)2)3) (B (C6 F5)4)'
_chemical_formula_sum            'C32 H25 B F20 N4 Ti'
_chemical_formula_weight         904.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.676(3)
_cell_angle_beta                 108.043(3)
_cell_angle_gamma                106.675(3)
_cell_formula_units_Z            4
_cell_length_a                   14.4540(17)
_cell_length_b                   17.392(2)
_cell_length_c                   17.702(2)
_cell_measurement_reflns_used    1020
_cell_measurement_temperature    127(2)
_cell_measurement_theta_max      32.34
_cell_measurement_theta_min      2.74
_cell_volume                     3583.6(7)
_computing_cell_refinement       'SAINT 6.45A (Bruker, 2004)'
_computing_data_collection       'SMART 5.630 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      127(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'   0.30 degree frames measured for  30.15 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            117040
_diffrn_reflns_theta_full        32.52
_diffrn_reflns_theta_max         32.52
_diffrn_reflns_theta_min         2.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Semi-empirical absorption correction via SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1245
_refine_ls_number_reflns         25940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
   [\s^2^(Fo^2^)+1.25Fo^2^+(0.05Fo^2^)^2^]^-1^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                19516
_reflns_number_total             25940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om0602207si20060308_123353.cif
_cod_data_source_block           05323
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'multiscan'
changed to 'multi-scan' 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        3583.7(7)
_cod_database_code               4075329