Low-Coordinate and Neutral Nitrido Complexes of Vanadium
Ba L. Tran; Maren Pink; Xinfeng Gao; Hyunsoo Park; Daniel J. Mindiola; Journal of the American Chemical Society 132 (2010) 1458–1459; doi:10.1021/ja908303k

data_4101847
_publ_section_title
;
 Low-Coordinate and Neutral Nitrido Complexes of Vanadium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1458
_journal_page_last               1459
_journal_paper_doi               10.1021/ja908303k
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C44 H55 N4 O1 V1'
_chemical_formula_sum            'C44 H55 N4 O V'
_chemical_formula_weight         707.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 103.704(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.480(2)
_cell_length_b                   18.768(4)
_cell_length_c                   20.844(4)
_cell_measurement_reflns_used    1564
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      1.48
_cell_volume                     3983.1(14)
_computing_cell_refinement       'APEX II v.2.2 (Bruker, 2009)'
_computing_data_collection       'APEX II v.2.2 (Bruker, 2009)'
_computing_data_reduction        'APEX II v.2.2 (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  kappa
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61687
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX II'
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.9430
_exptl_absorpt_correction_T_min  0.8672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.695
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         12090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+2.1987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                9705
_reflns_number_total             12090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja908303k_si_002.cif
_cod_data_source_block           09017
_cod_original_cell_volume        3983.2(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C44 H55 N4 O1 V1'
_cod_database_code               4101847