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_4112906
_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_sum            'C66 H90 B N2 O2 V'
_chemical_formula_weight         1005.15
_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                95.661(19)
_cell_angle_beta                 101.827(16)
_cell_angle_gamma                101.927(19)
_cell_formula_units_Z            2
_cell_length_a                   12.054(8)
_cell_length_b                   14.486(10)
_cell_length_c                   18.387(13)
_cell_measurement_reflns_used    781
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.29
_cell_volume                     3041(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local program)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      118(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
'   0.30 degree frames measured for  30.17 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  0.1131
_diffrn_reflns_av_sigmaI/netI    0.1796
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27320
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     990
_refine_ls_number_reflns         13345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1509
_reflns_number_gt                5888
_reflns_number_total             13345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0472376si20040720_050329.cif
_cod_data_source_block           03260
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4112906