Carbon Monoxide, Isocyanide, and Nitrile Complexes of Cationic, d0 Vanadium Bisimides: π-Back Bonding Derived from the π Symmetry, Bonding Metal Bisimido Ligand Orbitals
Henry S. La Pierre; John Arnold; Robert G. Bergman; F. Dean Toste; Inorganic Chemistry 51 (2012) 13334–13344; doi:10.1021/ic302044q

data_4331336
_publ_section_title
;
 Carbon Monoxide, Isocyanide, and Nitrile Complexes of Cationic, d0
 Vanadium Bisimides: \p-Back Bonding Derived from the \p Symmetry, Bonding
 Metal Bisimido Ligand Orbitals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13334
_journal_page_last               13344
_journal_paper_doi               10.1021/ic302044q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C39 H45 Al F36 N3 O4 P2 V'
_chemical_formula_sum            'C39 H45 Al F36 N3 O4 P2 V'
_chemical_formula_weight         1443.64
_chemical_name_common
'[v(pme3)2(ntbu)2(2,6-xylylisocyanide)][al(pftb)]'
_chemical_name_systematic
;
 [v(pme3)2(ntbu)2(2,6-xylylisocyanide)][al(pftb)4]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_beta                 91.2611(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0395(8)
_cell_length_b                   17.3604(14)
_cell_length_c                   33.167(3)
_cell_measurement_reflns_used    9691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.39
_cell_volume                     5779.3(8)
_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, 1997)'
_computing_structure_solution    sir-2004
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            156432
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  0.8896
_exptl_absorpt_correction_T_min  0.8663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       blade
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.012
_refine_diff_density_min         -2.237
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         10613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.411
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(fo^2^)+(0.0346p)^2^+24.2433p] where p=(fo^2^+2fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                8595
_reflns_number_total             10613
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ic302044q_si_002_1.cif
_cod_data_source_block           hsl51_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_structure_factor_coef' value 'fsqd' changed to 'Fsqd'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_atom_site_adp_type'
value 'uani' changed to 'Uani' according to the built-in table from
CIF Core dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29 (86 times).

'_atom_site_adp_type' value 'uiso' changed to
'Uiso' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (45
times).

'_atom_site_refinement_flags' value 'r' changed to 'R'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (45 times).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               4331336