Sequential N-O and N-N Bond Cleavage of N-Heterocyclic Carbene-Activated Nitrous Oxide with a Vanadium Complex
Alexander G. Tskhovrebov; Euro Solari; Matthew D. Wodrich; Rosario Scopelliti; Kay Severin; Journal of the American Chemical Society 134 (2012) 1471–1473; doi:10.1021/ja210976a

data_4117349
_publ_section_title
;
 Sequential N-O and N-N Bond Cleavage of N-Heterocyclic Carbene-Activated
 Nitrous Oxide with a Vanadium Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1471
_journal_page_last               1473
_journal_paper_doi               10.1021/ja210976a
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C48 H57 N4 O V'
_chemical_formula_sum            'C48 H57 N4 O V'
_chemical_formula_weight         756.92
_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                85.57(3)
_cell_angle_beta                 79.28(3)
_cell_angle_gamma                62.45(3)
_cell_formula_units_Z            2
_cell_length_a                   10.984(3)
_cell_length_b                   11.655(4)
_cell_length_c                   18.774(8)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     2093.6(14)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega 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  0.1322
_diffrn_reflns_av_sigmaI/netI    0.1157
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36660
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.277
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0018(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1421
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0171P)^2^+2.6201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                4548
_reflns_number_total             7293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210976a_si_002.cif
_cod_data_source_block           al268
_cod_original_cell_volume        2093.6(12)
_cod_database_code               4117349