A Planar Three-Coordinate Vanadium(II) Complex and the Study of Terminal Vanadium Nitrides from N2: A Kinetic or Thermodynamic Impediment to N-N Bond Cleavage?
Ba L. Tran; Balazs Pinter; Adam J. Nichols; Felicia T. Konopka; Rick Thompson; Chun-Hsing Chen; J. Krzystek; Andrew Ozarowski; Joshua Telser; Mu-Hyun Baik; Karsten Meyer; Daniel J. Mindiola; Journal of the American Chemical Society 134 (2012) 13035–13045; doi:10.1021/ja303360v

data_4118455
_publ_section_title
;
 A Planar Three-Coordinate Vanadium(II) Complex and the Study of Terminal
 Vanadium Nitrides from N2: A Kinetic or Thermodynamic Impediment to N-N
 Bond Cleavage?
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13035
_journal_page_last               13045
_journal_paper_doi               10.1021/ja303360v
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C41 H58 N3 O V, 0.5 C4 H10 O'
_chemical_formula_sum            'C43 H63 N3 O1.5 V'
_chemical_formula_weight         696.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.000(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.521(6)
_cell_length_b                   15.079(7)
_cell_length_c                   22.635(10)
_cell_measurement_reflns_used    1059
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.56
_cell_measurement_theta_min      2.59
_cell_volume                     4180(3)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2010)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2010)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2010)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2010)'
_computing_publication_material  'SHELXTL (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2010)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
'0.50 degree frames measured for 60 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi 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  0.1733
_diffrn_reflns_av_sigmaI/netI    0.2087
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28294
_diffrn_reflns_theta_full        25.22
_diffrn_reflns_theta_max         25.22
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.9707
_exptl_absorpt_correction_T_min  0.9476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         7401
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.2091
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                3036
_reflns_number_total             7401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303360v_si_001.cif
_cod_data_source_block           10057
_cod_original_formula_sum        'C43 H63 N3 O1.50 V'
_cod_database_code               4118455