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_4118456
_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         'C52 H78 N4 O2.00 V1'
_chemical_formula_sum            'C52 H78 N4 O2 V'
_chemical_formula_weight         842.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-06-21
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 96.580(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.409(5)
_cell_length_b                   19.013(7)
_cell_length_c                   19.713(7)
_cell_measurement_reflns_used    5025
_cell_measurement_temperature    150
_cell_measurement_theta_max      24
_cell_measurement_theta_min      3
_cell_volume                     4993(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31646
_diffrn_reflns_theta_full        25.088
_diffrn_reflns_theta_max         25.088
_diffrn_reflns_theta_min         1.493
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'USER DEFINED ABSORPTION METHOD'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       prism
_exptl_crystal_F_000             1828.000
_exptl_crystal_size_max          0.597
_exptl_crystal_size_mid          0.288
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.84
_refine_diff_density_min         -1.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0071
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         8568
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.0232493
_refine_ls_shift/su_mean         0.0005965
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 3.73P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1419
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1419
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                4910
_reflns_number_total             8568
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.21
_oxford_diffrn_Wilson_scale      140.60
_oxford_refine_ls_r_factor_ref   0.1067
_oxford_refine_ls_scale          0.08530(2)
_oxford_reflns_number_all        8568
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mo_10060_0m in P2(1)/n'
_cod_data_source_file            ja303360v_si_002.cif
_cod_data_source_block           10060
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C52 H78 N4 O2.00 V1'
_cod_database_code               4118456