Dinitrogen Partial Reduction by Formally Zero- and Divalent Vanadium Complexes Supported by the Bis-iminopyridine System
Indu Vidyaratne; Sandro Gambarotta; Ilia Korobkov; Peter H. M. Budzelaar; Inorganic Chemistry 44 (2005) 1187–1189; doi:10.1021/ic048358+

data_4327313
_publ_section_title
;
 Dinitrogen Partial Reduction by Formally Zero- and Divalent Vanadium
 Complexes Supported by the Bis-iminopyridine System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1187
_journal_page_last               1189
_journal_paper_doi               10.1021/ic048358+
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H58 N4 O V'
_chemical_formula_weight         661.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 113.643(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.401(2)
_cell_length_b                   11.6983(11)
_cell_length_c                   30.425(3)
_cell_measurement_reflns_used    990
_cell_measurement_temperature    206(2)
_cell_measurement_theta_max      20.39
_cell_measurement_theta_min      2.22
_cell_volume                     8281.9(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      206(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            18239
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         5943
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+11.5585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                3848
_reflns_number_total             5943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0483582Bsi20041121_045711_1.cif
_cod_data_source_block           sg421_complex1
_cod_database_code               4327313