Vanadium Bisimide Bonding Investigated by X-ray Crystallography, 51V and 13C Nuclear Magnetic Resonance Spectroscopy, and V L3,2-Edge X-ray Absorption Near-Edge Structure Spectroscopy
Henry S. La Pierre; Stefan G. Minasian; Mark Abubekerov; Stosh A. Kozimor; David K. Shuh; Tolek Tyliszczak; John Arnold; Robert G. Bergman; F. Dean Toste; Inorganic Chemistry 52 (2013) 11650–11660; doi:10.1021/ic4020543

data_4336378
_publ_section_title
;
 Vanadium Bisimide Bonding Investigated by X-ray Crystallography, 51V and
 13C Nuclear Magnetic Resonance Spectroscopy, and V L3,2-Edge X-ray
 Absorption Near-Edge Structure Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11650
_journal_page_last               11660
_journal_paper_doi               10.1021/ic4020543
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         VI(PMe3)2(NtBu)2
_chemical_formula_sum            'C14 H36 I N2 P2 V'
_chemical_formula_weight         472.23
_chemical_name_common            VI(PMe3)2(NtBu)2
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.5148(13)
_cell_length_b                   28.109(3)
_cell_length_c                   14.1707(16)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.29
_cell_volume                     4586.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SUPERFLIP
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46440
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       rod
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0116P)^2^+11.4662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                3202
_reflns_number_total             4422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4020543_si_003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4586.7(9)
_cod_database_code               4336378