Formation of a Cationic Vinylimido Group upon C-H Activation of Nitriles by Trialkylamines in the Presence of TaCl5.
Rahman, Md Mamdudur; Smith, Mark D.; Peryshkov, Dmitry V.; Inorganic chemistry 55 (2016) 5101–5103; doi:10.1021/acs.inorgchem.6b00677

data_4347833
_publ_section_title
;
 Formation of a Cationic Vinylimido Group upon C-H Activation of Nitriles
 by Trialkylamines in the Presence of TaCl5.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5101
_journal_page_last               5103
_journal_paper_doi               10.1021/acs.inorgchem.6b00677
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C8 H17 Cl5 N2 Ta, C6 H16 N'
_chemical_formula_sum            'C14 H33 Cl5 N3 Ta'
_chemical_formula_weight         601.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.23 svn.r2946 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.834(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1004(12)
_cell_length_b                   10.5361(8)
_cell_length_c                   13.4658(10)
_cell_measurement_reflns_used    7825
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.276
_cell_measurement_theta_min      2.328
_cell_volume                     2227.2(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.631 (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33354
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.297
_diffrn_source_current           37.0
_diffrn_source_power             1.739
_diffrn_source_voltage           47.0
_exptl_absorpt_coefficient_mu    5.537
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.665400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0895 before and 0.0327 after correction.
The Ratio of minimum to maximum transmission is 0.6654.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.709
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+1.5658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                4243
_reflns_number_total             4910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00677_si_002.cif
_cod_data_source_block           p142
_cod_database_code               4347833
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.375
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C11(H11A,H11B), C13(H13A,H13B),
 C15(H15A,H15B)
2.b X=CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              90068
_shelx_hkl_checksum              26444
_olex2_submission_special_instructions 'No special instructions were received'