#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:44:54 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178532 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/37/4063759.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4063759
loop_
_publ_author_name
'Graham, Todd W.'
'Udachin, Konstantin A.'
'Zgierski, Marek Z.'
'Carty, Arthur J.'
_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_sum            'C20 H24 N2 O3 P V'
_chemical_formula_weight         422.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   12.202(2)
_cell_length_b                   10.882(2)
_cell_length_c                   29.912(6)
_cell_measurement_temperature    100(2)
_cell_volume                     3971.8(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      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            27273
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.9150
_exptl_absorpt_correction_T_min  0.7526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0492
_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/[σ²(Fo²)+(0.0000P)²+17.0722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                2907
_reflns_number_total             3055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100915v_si_002.cif
_cod_data_source_block           tgg77_compound_14
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4063759
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
V1 V 0.04329(5) 0.21016(6) 0.062432(19) 0.01501(17) Uani 1 1 d .
P1 P 0.02163(7) 0.23734(8) 0.14028(3) 0.0134(2) Uani 1 1 d .
O1 O -0.0775(2) -0.0312(3) 0.08497(9) 0.0265(6) Uani 1 1 d .
O2 O 0.1918(2) 0.0095(3) 0.02385(9) 0.0300(7) Uani 1 1 d .
O3 O 0.2781(2) 0.2657(3) 0.09436(9) 0.0309(7) Uani 1 1 d .
N1 N 0.0709(2) 0.1399(3) 0.17725(9) 0.0139(6) Uani 1 1 d .
N2 N -0.0332(3) 0.3403(3) 0.16810(10) 0.0177(7) Uani 1 1 d .
C1 C -0.0326(3) 0.0599(3) 0.07804(12) 0.0177(8) Uani 1 1 d .
C2 C 0.1354(3) 0.0843(4) 0.03817(12) 0.0212(9) Uani 1 1 d .
C3 C 0.1892(3) 0.2457(3) 0.08360(12) 0.0197(8) Uani 1 1 d .
C4 C -0.1104(3) 0.2610(4) 0.02286(12) 0.0233(9) Uani 1 1 d .
H4 H -0.1764 0.2150 0.0247 0.028 Uiso 1 1 calc R
C5 C -0.0237(3) 0.2405(4) -0.00703(12) 0.0244(9) Uani 1 1 d .
H5 H -0.0209 0.1784 -0.0293 0.029 Uiso 1 1 calc R
C6 C 0.0580(3) 0.3276(4) 0.00174(12) 0.0240(9) Uani 1 1 d .
H6 H 0.1260 0.3346 -0.0135 0.029 Uiso 1 1 calc R
C7 C 0.0218(3) 0.4031(4) 0.03703(12) 0.0216(9) Uani 1 1 d .
H7 H 0.0610 0.4698 0.0499 0.026 Uiso 1 1 calc R
C8 C -0.0816(3) 0.3622(3) 0.04968(12) 0.0202(8) Uani 1 1 d .
H8 H -0.1256 0.3969 0.0726 0.024 Uiso 1 1 calc R
C9 C 0.1272(3) 0.0250(3) 0.16280(12) 0.0156(8) Uani 1 1 d .
H9 H 0.1255 0.0230 0.1294 0.019 Uiso 1 1 calc R
C10 C 0.2473(3) 0.0259(4) 0.17697(13) 0.0241(9) Uani 1 1 d .
H10C H 0.2523 0.0153 0.2094 0.029 Uiso 1 1 calc R
H10B H 0.2807 0.1045 0.1685 0.029 Uiso 1 1 calc R
H10A H 0.2862 -0.0413 0.1620 0.029 Uiso 1 1 calc R
C11 C 0.0677(3) -0.0886(3) 0.17932(13) 0.0213(9) Uani 1 1 d .
H11C H -0.0104 -0.0822 0.1720 0.026 Uiso 1 1 calc R
H11B H 0.0764 -0.0955 0.2118 0.026 Uiso 1 1 calc R
H11A H 0.0986 -0.1617 0.1649 0.026 Uiso 1 1 calc R
C12 C 0.0663(3) 0.1571(3) 0.22693(11) 0.0165(8) Uani 1 1 d .
H12 H 0.1060 0.0851 0.2399 0.020 Uiso 1 1 calc R
C13 C 0.1292(3) 0.2695(3) 0.24221(12) 0.0211(8) Uani 1 1 d .
H13C H 0.0897 0.3438 0.2331 0.025 Uiso 1 1 calc R
H13B H 0.2022 0.2693 0.2286 0.025 Uiso 1 1 calc R
H13A H 0.1364 0.2681 0.2748 0.025 Uiso 1 1 calc R
C14 C -0.0489(3) 0.1498(3) 0.24513(12) 0.0208(8) Uani 1 1 d .
H14C H -0.0861 0.0781 0.2324 0.025 Uiso 1 1 calc R
H14B H -0.0891 0.2245 0.2370 0.025 Uiso 1 1 calc R
H14A H -0.0462 0.1420 0.2777 0.025 Uiso 1 1 calc R
C15 C -0.0792(3) 0.4520(3) 0.15562(11) 0.0147(8) Uani 1 1 d .
C16 C -0.0198(3) 0.5432(3) 0.13361(11) 0.0165(8) Uani 1 1 d .
H16 H 0.0553 0.5298 0.1268 0.020 Uiso 1 1 calc R
C17 C -0.0688(3) 0.6528(4) 0.12164(12) 0.0218(9) Uani 1 1 d .
H17 H -0.0274 0.7134 0.1062 0.026 Uiso 1 1 calc R
C18 C -0.1768(4) 0.6752(4) 0.13173(13) 0.0274(10) Uani 1 1 d .
H18 H -0.2105 0.7502 0.1230 0.033 Uiso 1 1 calc R
C19 C -0.2353(4) 0.5877(4) 0.15463(12) 0.0257(9) Uani 1 1 d .
H19 H -0.3097 0.6031 0.1621 0.031 Uiso 1 1 calc R
C20 C -0.1878(3) 0.4776(4) 0.16698(12) 0.0213(9) Uani 1 1 d .
H20 H -0.2293 0.4189 0.1833 0.026 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C2 V1 C3 74.10(16)
C2 V1 C1 76.59(16)
C3 V1 C1 122.12(16)
C2 V1 C6 93.11(15)
C3 V1 C6 94.48(16)
C1 V1 C6 136.02(15)
C2 V1 C7 127.46(15)
C3 V1 C7 91.78(15)
C1 V1 C7 144.53(15)
C6 V1 C7 36.67(14)
C2 V1 C5 88.18(15)
C3 V1 C5 127.39(15)
C1 V1 C5 99.91(15)
C6 V1 C5 36.39(15)
C7 V1 C5 60.67(14)
C2 V1 C8 147.93(15)
C3 V1 C8 121.73(15)
C1 V1 C8 109.47(15)
C6 V1 C8 60.09(14)
C7 V1 C8 35.75(14)
C5 V1 C8 59.88(14)
C2 V1 C4 117.28(15)
C3 V1 C4 151.49(15)
C1 V1 C4 86.39(15)
C6 V1 C4 60.32(15)
C7 V1 C4 60.21(14)
C5 V1 C4 35.96(14)
C8 V1 C4 35.89(14)
C2 V1 P1 121.94(11)
C3 V1 P1 75.80(11)
C1 V1 P1 79.32(11)
C6 V1 P1 137.78(11)
C7 V1 P1 101.73(10)
C5 V1 P1 148.07(11)
C8 V1 P1 89.96(10)
C4 V1 P1 112.86(10)
N2 P1 N1 105.24(16)
N2 P1 V1 132.00(12)
N1 P1 V1 122.74(11)
C9 N1 C12 114.2(3)
C9 N1 P1 120.9(2)
C12 N1 P1 124.9(2)
C15 N2 P1 131.6(3)
O1 C1 V1 176.4(3)
O2 C2 V1 179.1(4)
O3 C3 V1 176.9(3)
C5 C4 C8 107.5(4)
C5 C4 V1 70.9(2)
C8 C4 V1 71.9(2)
C5 C4 H4 126.3
C8 C4 H4 126.3
V1 C4 H4 122.6
C6 C5 C4 108.0(3)
C6 C5 V1 70.7(2)
C4 C5 V1 73.1(2)
C6 C5 H5 126.0
C4 C5 H5 126.0
V1 C5 H5 121.9
C5 C6 C7 108.2(4)
C5 C6 V1 73.0(2)
C7 C6 V1 72.4(2)
C5 C6 H6 125.9
C7 C6 H6 125.9
V1 C6 H6 120.5
C8 C7 C6 107.6(4)
C8 C7 V1 73.4(2)
C6 C7 V1 70.9(2)
C8 C7 H7 126.2
C6 C7 H7 126.2
V1 C7 H7 121.2
C7 C8 C4 108.8(3)
C7 C8 V1 70.8(2)
C4 C8 V1 72.2(2)
C7 C8 H8 125.6
C4 C8 H8 125.6
V1 C8 H8 123.0
N1 C9 C11 111.7(3)
N1 C9 C10 110.9(3)
C11 C9 C10 112.0(3)
N1 C9 H9 107.3
C11 C9 H9 107.3
C10 C9 H9 107.3
C9 C10 H10C 109.5
C9 C10 H10B 109.5
H10C C10 H10B 109.5
C9 C10 H10A 109.5
H10C C10 H10A 109.5
H10B C10 H10A 109.5
C9 C11 H11C 109.5
C9 C11 H11B 109.5
H11C C11 H11B 109.5
C9 C11 H11A 109.5
H11C C11 H11A 109.5
H11B C11 H11A 109.5
N1 C12 C14 112.7(3)
N1 C12 C13 112.4(3)
C14 C12 C13 113.9(3)
N1 C12 H12 105.6
C14 C12 H12 105.6
C13 C12 H12 105.6
C12 C13 H13C 109.5
C12 C13 H13B 109.5
H13C C13 H13B 109.5
C12 C13 H13A 109.5
H13C C13 H13A 109.5
H13B C13 H13A 109.5
C12 C14 H14C 109.5
C12 C14 H14B 109.5
H14C C14 H14B 109.5
C12 C14 H14A 109.5
H14C C14 H14A 109.5
H14B C14 H14A 109.5
N2 C15 C16 122.6(3)
N2 C15 C20 119.5(3)
C16 C15 C20 117.9(3)
C17 C16 C15 120.7(4)
C17 C16 H16 119.6
C15 C16 H16 119.6
C18 C17 C16 120.8(4)
C18 C17 H17 119.6
C16 C17 H17 119.6
C17 C18 C19 119.0(4)
C17 C18 H18 120.5
C19 C18 H18 120.5
C18 C19 C20 121.2(4)
C18 C19 H19 119.4
C20 C19 H19 119.4
C19 C20 C15 120.4(4)
C19 C20 H20 119.8
C15 C20 H20 119.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
V1 C2 1.914(4)
V1 C3 1.929(4)
V1 C1 1.937(4)
V1 C6 2.228(4)
V1 C7 2.248(4)
V1 C5 2.257(4)
V1 C8 2.281(4)
V1 C4 2.285(4)
V1 P1 2.3620(12)
P1 N2 1.547(3)
P1 N1 1.646(3)
O1 C1 1.151(5)
O2 C2 1.150(5)
O3 C3 1.152(5)
N1 C9 1.491(4)
N1 C12 1.499(4)
N2 C15 1.391(5)
C4 C5 1.402(6)
C4 C8 1.407(5)
C4 H4 0.9500
C5 C6 1.401(6)
C5 H5 0.9500
C6 C7 1.408(6)
C6 H6 0.9500
C7 C8 1.391(6)
C7 H7 0.9500
C8 H8 0.9500
C9 C11 1.517(5)
C9 C10 1.526(5)
C9 H9 1.0000
C10 H10C 0.9800
C10 H10B 0.9800
C10 H10A 0.9800
C11 H11C 0.9800
C11 H11B 0.9800
C11 H11A 0.9800
C12 C14 1.509(5)
C12 C13 1.515(5)
C12 H12 1.0000
C13 H13C 0.9800
C13 H13B 0.9800
C13 H13A 0.9800
C14 H14C 0.9800
C14 H14B 0.9800
C14 H14A 0.9800
C15 C16 1.394(5)
C15 C20 1.396(5)
C16 C17 1.382(5)
C16 H16 0.9500
C17 C18 1.373(6)
C17 H17 0.9500
C18 C19 1.374(6)
C18 H18 0.9500
C19 C20 1.381(6)
C19 H19 0.9500
C20 H20 0.9500
