Terminal and Four-Coordinate Vanadium(IV) Phosphinidene Complexes. A Pseudo Jahn-Teller Effect of Second Order Stabilizing the V-P Multiple Bond
Falguni Basuli; Brad C. Bailey; John C. Huffman; Mu-Hyun Baik; Daniel J. Mindiola; Journal of the American Chemical Society 126 (2004) 1924–1925; doi:10.1021/ja0392216

data_4112267
_publ_section_title
;
 Terminal and Four-Coordinate Vanadium(IV) Phosphinidene Complexes. A
 Pseudo Jahn-Teller Effect of Second Order Stabilizing the V-P Multiple
 Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1924
_journal_page_last               1925
_journal_paper_doi               10.1021/ja0392216
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C59 H89 N2 P2 V'
_chemical_formula_weight         938.70
_chemical_name_systematic
; 
 ? 
;
_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                90.00
_cell_angle_beta                 92.674(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.245(4)
_cell_length_b                   20.453(4)
_cell_length_c                   24.056(5)
_cell_measurement_reflns_used    1002
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      24.31
_cell_measurement_theta_min      2.90
_cell_volume                     11424(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'   0.30 degree frames measured for  10.17 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\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  0.1891
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            254459
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             4076
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1217
_refine_ls_number_reflns         26158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0991
_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^)+(0.0455P)^2^+69.2895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2409
_refine_ls_wR_factor_ref         0.2560
_reflns_number_gt                17845
_reflns_number_total             26158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0392216rom20031211_011154.cif
_cod_data_source_block           03140
_cod_original_cell_volume        11425(4)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4112267