Synthesis and Structural Characterization of the First Thermally Stable, Neutral, and Electrophilic Phosphinidene Complexes of Vanadium
Graham, Todd W.; Udachin, Konstantin A.; Zgierski, Marek Z.; Carty, Arthur J.; Organometallics 30 (2011) 1382–; doi:10.1021/om100915v

data_4063756
_publ_section_title
;
 Synthesis and Structural Characterization of the First Thermally Stable,
 Neutral, and Electrophilic Phosphinidene Complexes of Vanadium
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1382
_journal_paper_doi               10.1021/om100915v
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C14 H19 N O3 P V'
_chemical_formula_sum            'C14 H19 N O3 P V'
_chemical_formula_weight         331.21
_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                 96.581(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0972(6)
_cell_length_b                   8.7514(4)
_cell_length_c                   13.8930(7)
_cell_measurement_temperature    125(2)
_cell_volume                     1581.91(13)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'ATOMS V.5.0'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            117992
_diffrn_reflns_theta_full        43.67
_diffrn_reflns_theta_max         43.67
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.9303
_exptl_absorpt_correction_T_min  0.7106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         11450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.1787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                9246
_reflns_number_total             11450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100915v_si_002.cif
_cod_data_source_block           tg71_compound_3a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4063756