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_4118457
_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         'C46 H70 N2 O1 V1'
_chemical_formula_sum            'C46 H70 N2 O V'
_chemical_formula_weight         718.02
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-02-28
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.767(2)
_cell_length_b                   19.760(2)
_cell_length_c                   10.9044(13)
_cell_measurement_reflns_used    6135
_cell_measurement_temperature    150
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     4474.7(8)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.073
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            56723
_diffrn_reflns_theta_full        25.074
_diffrn_reflns_theta_max         25.074
_diffrn_reflns_theta_min         1.961
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_description       prism
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.88
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0237
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         4059
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.0294607
_refine_ls_shift/su_mean         0.0001783
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 4.37P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1340
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1340
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2963
_reflns_number_total             4081
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      190.21
_oxford_refine_ls_r_factor_ref   0.0720
_oxford_refine_ls_scale          0.08242(3)
_oxford_reflns_number_all        4059
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_12020_0ma in Pnma'
_cod_data_source_file            ja303360v_si_003.cif
_cod_data_source_block           12020
_cod_original_cell_volume        4474.7(9)
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C46 H70 N2 O1 V1'
_cod_database_code               4118457
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT V    (    1 ,X'S,U'S)  UNTIL C    (   22 ) 
CONT C    (   23 ,X'S,U[ISO])  UNTIL C    (   27 ) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,X'S) 
RIDE C   (  23,X'S) H   ( 232,X'S) H   ( 233,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.540000 , 0.007000 = C(24) TO C(25) 
END                                                                             
;