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_4112269
_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            'C49 H75 N2 P V'
_chemical_formula_weight         774.02
_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                 113.933(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.442(5)
_cell_length_b                   23.415(5)
_cell_length_c                   20.355(5)
_cell_measurement_reflns_used    928
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      20.13
_cell_measurement_theta_min      2.36
_cell_volume                     9341(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      113(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
'   0.30 degree frames measured for  30.15 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  0.2090
_diffrn_reflns_av_sigmaI/netI    0.2327
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            207958
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       plate
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1547
_refine_ls_number_reflns         21585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.860
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1658
_reflns_number_gt                8612
_reflns_number_total             21585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0392216si20031211_011312.cif
_cod_data_source_block           03185
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4112269