A Structurally Characterized Nitrous Oxide Complex of Vanadium
Nicholas A. Piro; Michael F. Lichterman; W. Hill Harman; Christopher J. Chang; Journal of the American Chemical Society 133 (2011) 2108–2111; doi:10.1021/ja110798w

data_4105665
_publ_contact_author_address
;Department of Chemistry
University of California
Berkeley, CA  94720
;
_publ_contact_author_email       chrischang@berkeley.edu
_publ_contact_author_name        'Christopher J. Chang'
_publ_section_title
;
 A Structurally Characterized Nitrous Oxide Complex of Vanadium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2108
_journal_page_last               2111
_journal_paper_doi               10.1021/ja110798w
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C46 H53 N4 O V'
_chemical_formula_weight         728.86
_chemical_name_common            (THF)V(tpaMes)
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 93.368(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.910(7)
_cell_length_b                   11.252(7)
_cell_length_c                   16.024(10)
_cell_measurement_reflns_used    4428
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      2.60
_cell_volume                     1964(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0544
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11544
_diffrn_reflns_theta_full        25.84
_diffrn_reflns_theta_max         25.84
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.9798
_exptl_absorpt_correction_T_min  0.9173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       blade
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0382P)^2^+0.0705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                5971
_reflns_number_total             7101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja110798w_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4105665