Terminal Vanadium-Neopentylidyne Complexes and Intramolecular Cross-Metathesis Reactions to Generate Azametalacyclohexatrienes
Falguni Basuli; Brad C. Bailey; Douglas Brown; John Tomaszewski; John C. Huffman; Mu-Hyun Baik; Daniel J. Mindiola; Journal of the American Chemical Society 126 (2004) 10506–10507; doi:10.1021/ja0472376

data_4112905
_publ_contact_author             'J.C. Huffman'
_publ_section_title
;
 Terminal Vanadium-Neopentylidyne Complexes and Intramolecular
 Cross-Metathesis Reactions to Generate Azametalacyclohexatrienes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10506
_journal_page_last               10507
_journal_paper_doi               10.1021/ja0472376
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C35 H50 F3 N2 O3 S V'
_chemical_formula_structural     V(C22H33N)(NC6H3(iPr)2)(Otf)
_chemical_formula_sum            'C35 H50 F3 N2 O3 S V'
_chemical_formula_weight         686.77
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.789(2)
_cell_angle_beta                 91.184(3)
_cell_angle_gamma                99.567(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4958(9)
_cell_length_b                   10.8384(10)
_cell_length_c                   17.7702(17)
_cell_measurement_reflns_used    939
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.42
_cell_volume                     1789.3(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      112(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
'   0.30 degree frames measured for   3.17 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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29159
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       'cleaved fragment'
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         8239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                6257
_reflns_number_total             8239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0472376si20040720_050246.cif
_cod_data_source_block           03226
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4112905