#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:04:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179466 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/63/4336379.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_4336379
loop_
_publ_author_name
'Henry S. La Pierre'
'Stefan G. Minasian'
'Mark Abubekerov'
'Stosh A. Kozimor'
'David K. Shuh'
'Tolek Tyliszczak'
'John Arnold'
'Robert G. Bergman'
'F. Dean Toste'
_publ_section_title
;
 Vanadium Bisimide Bonding Investigated by X-ray Crystallography, 51V and
 13C Nuclear Magnetic Resonance Spectroscopy, and V L3,2-Edge X-ray
 Absorption Near-Edge Structure Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11650
_journal_page_last               11660
_journal_paper_doi               10.1021/ic4020543
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         VPh(PMe3)2(NtBu)2
_chemical_formula_sum            'C20 H41 N2 P2 V'
_chemical_formula_weight         422.43
_chemical_name_common            VPh(PMe3)2(NtBu)2
_chemical_name_systematic        VPh(PMe3)2(NtBu)2
_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                 95.873(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.485(4)
_cell_length_b                   9.550(4)
_cell_length_c                   27.830(11)
_cell_measurement_reflns_used    1569
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      2.48
_cell_volume                     2507.7(18)
_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, 2008)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0781
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22082
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.9589
_exptl_absorpt_correction_T_min  0.8925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.617
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         11343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0958
_refine_ls_shift/su_max          0.005
_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+23.6974P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2211
_refine_ls_wR_factor_ref         0.2259
_reflns_number_gt                9739
_reflns_number_total             11343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4020543_si_004.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2507.6(17)
_cod_database_code               4336379
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9662(6) 0.4001(7) 0.1749(2) 0.0258(14) Uani 1 1 d . . .
C2 C 0.9427(15) 0.5656(15) 0.1604(5) 0.057(4) Uiso 0.587(9) 1 d P A 1
H2A H 0.9534 0.5782 0.1260 0.086 Uiso 0.587(9) 1 calc PR A 1
H2B H 1.0132 0.6228 0.1797 0.086 Uiso 0.587(9) 1 calc PR A 1
H2C H 0.8473 0.5947 0.1668 0.086 Uiso 0.587(9) 1 calc PR A 1
C3 C 1.1192(14) 0.3737(16) 0.1638(5) 0.057(4) Uiso 0.587(9) 1 d P A 1
H3A H 1.1830 0.4389 0.1825 0.086 Uiso 0.587(9) 1 calc PR A 1
H3B H 1.1259 0.3882 0.1292 0.086 Uiso 0.587(9) 1 calc PR A 1
H3C H 1.1463 0.2773 0.1725 0.086 Uiso 0.587(9) 1 calc PR A 1
C4 C 0.9414(15) 0.3880(17) 0.2262(5) 0.060(4) Uiso 0.587(9) 1 d P A 1
H4A H 0.8420 0.4096 0.2298 0.091 Uiso 0.587(9) 1 calc PR A 1
H4B H 1.0028 0.4541 0.2454 0.091 Uiso 0.587(9) 1 calc PR A 1
H4C H 0.9628 0.2924 0.2374 0.091 Uiso 0.587(9) 1 calc PR A 1
C2A C 1.0517(18) 0.483(2) 0.1451(6) 0.042(5) Uiso 0.413(9) 1 d P A 2
H2A1 H 1.1240 0.4230 0.1329 0.063 Uiso 0.413(9) 1 calc PR A 2
H2A2 H 1.0978 0.5588 0.1645 0.063 Uiso 0.413(9) 1 calc PR A 2
H2A3 H 0.9909 0.5224 0.1179 0.063 Uiso 0.413(9) 1 calc PR A 2
C3A C 1.0558(18) 0.2878(19) 0.2086(6) 0.042(5) Uiso 0.413(9) 1 d P A 2
H3A1 H 0.9912 0.2326 0.2264 0.063 Uiso 0.413(9) 1 calc PR A 2
H3A2 H 1.1239 0.3369 0.2315 0.063 Uiso 0.413(9) 1 calc PR A 2
H3A3 H 1.1067 0.2254 0.1884 0.063 Uiso 0.413(9) 1 calc PR A 2
C4A C 0.8797(18) 0.4873(19) 0.2105(6) 0.041(5) Uiso 0.413(9) 1 d P A 2
H4A1 H 0.8142 0.5509 0.1918 0.061 Uiso 0.413(9) 1 calc PR A 2
H4A2 H 0.9456 0.5419 0.2326 0.061 Uiso 0.413(9) 1 calc PR A 2
H4A3 H 0.8260 0.4231 0.2292 0.061 Uiso 0.413(9) 1 calc PR A 2
C5 C 0.5844(6) 0.0380(7) 0.1842(2) 0.0235(14) Uani 1 1 d . . .
C6 C 0.6491(7) 0.1010(8) 0.23163(19) 0.0373(18) Uani 1 1 d . . .
H6A H 0.7497 0.0761 0.2369 0.056 Uiso 1 1 calc R . .
H6B H 0.5997 0.0644 0.2582 0.056 Uiso 1 1 calc R . .
H6C H 0.6394 0.2031 0.2303 0.056 Uiso 1 1 calc R . .
C7 C 0.4220(6) 0.0609(7) 0.1788(2) 0.0322(17) Uani 1 1 d . . .
H7A H 0.4015 0.1615 0.1778 0.048 Uiso 1 1 calc R . .
H7B H 0.3814 0.0185 0.2063 0.048 Uiso 1 1 calc R . .
H7C H 0.3802 0.0171 0.1488 0.048 Uiso 1 1 calc R . .
C8 C 0.6158(7) -0.1179(7) 0.1835(2) 0.0371(17) Uani 1 1 d . . .
H8A H 0.5794 -0.1571 0.1521 0.056 Uiso 1 1 calc R . .
H8B H 0.5698 -0.1644 0.2092 0.056 Uiso 1 1 calc R . .
H8C H 0.7184 -0.1328 0.1889 0.056 Uiso 1 1 calc R . .
C9 C 0.3988(6) 0.3245(7) 0.0655(2) 0.0269(15) Uani 1 1 d . . .
H9A H 0.3252 0.3958 0.0673 0.040 Uiso 1 1 calc R . .
H9B H 0.3701 0.2380 0.0807 0.040 Uiso 1 1 calc R . .
H9C H 0.4117 0.3062 0.0315 0.040 Uiso 1 1 calc R . .
C10 C 0.6088(6) 0.5386(6) 0.0620(2) 0.0311(16) Uani 1 1 d . . .
H10A H 0.6288 0.5087 0.0297 0.047 Uiso 1 1 calc R . .
H10B H 0.6926 0.5851 0.0783 0.047 Uiso 1 1 calc R . .
H10C H 0.5288 0.6041 0.0592 0.047 Uiso 1 1 calc R . .
C11 C 0.5067(6) 0.4692(7) 0.1511(2) 0.0291(15) Uani 1 1 d . . .
H11A H 0.5829 0.5284 0.1664 0.044 Uiso 1 1 calc R . .
H11B H 0.4835 0.3964 0.1738 0.044 Uiso 1 1 calc R . .
H11C H 0.4225 0.5267 0.1420 0.044 Uiso 1 1 calc R . .
C12 C 0.8358(6) -0.1244(7) 0.0631(2) 0.0259(14) Uani 1 1 d . . .
H12A H 0.7888 -0.0947 0.0317 0.039 Uiso 1 1 calc R . .
H12B H 0.7662 -0.1678 0.0821 0.039 Uiso 1 1 calc R . .
H12C H 0.9103 -0.1924 0.0580 0.039 Uiso 1 1 calc R . .
C13 C 1.0561(6) 0.0784(7) 0.0606(2) 0.0255(15) Uani 1 1 d . . .
H13A H 1.1100 -0.0047 0.0528 0.038 Uiso 1 1 calc R . .
H13B H 1.1190 0.1440 0.0794 0.038 Uiso 1 1 calc R . .
H13C H 1.0165 0.1237 0.0306 0.038 Uiso 1 1 calc R . .
C14 C 1.0104(7) -0.0564(8) 0.1480(2) 0.0379(18) Uani 1 1 d . . .
H14A H 1.0694 -0.1323 0.1374 0.057 Uiso 1 1 calc R . .
H14B H 0.9425 -0.0946 0.1689 0.057 Uiso 1 1 calc R . .
H14C H 1.0708 0.0130 0.1661 0.057 Uiso 1 1 calc R . .
C15 C 0.7322(6) 0.2201(7) 0.03412(18) 0.0197(12) Uani 1 1 d . A .
C16 C 0.8181(6) 0.3132(7) 0.0098(2) 0.0320(16) Uani 1 1 d . . .
H16 H 0.8840 0.3714 0.0285 0.038 Uiso 1 1 calc R . .
C17 C 0.8093(7) 0.3222(7) -0.0406(2) 0.0346(18) Uani 1 1 d . . .
H17 H 0.8689 0.3857 -0.0553 0.041 Uiso 1 1 calc R . .
C18 C 0.7159(7) 0.2407(7) -0.0687(2) 0.0342(18) Uani 1 1 d . . .
H18 H 0.7115 0.2465 -0.1029 0.041 Uiso 1 1 calc R . .
C19 C 0.6265(7) 0.1483(7) -0.0470(2) 0.0339(18) Uani 1 1 d . . .
H19 H 0.5602 0.0916 -0.0661 0.041 Uiso 1 1 calc R . .
C20 C 0.6373(6) 0.1417(7) 0.0032(2) 0.0266(15) Uani 1 1 d . . .
H20 H 0.5756 0.0793 0.0176 0.032 Uiso 1 1 calc R . .
N1 N 0.8681(4) 0.3188(5) 0.14310(16) 0.0182(11) Uani 1 1 d . A .
N2 N 0.6437(4) 0.1038(5) 0.14426(14) 0.0162(10) Uani 1 1 d . A .
P1 P 0.56486(15) 0.38704(17) 0.09686(5) 0.0186(3) Uani 1 1 d . A .
P2 P 0.91414(15) 0.02722(17) 0.09525(5) 0.0193(4) Uani 1 1 d . A .
V1 V 0.74731(10) 0.21007(11) 0.11256(3) 0.0158(2) Uani 1 1 d . . .
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'
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
N1 C1 C2A 107.8(8)
N1 C1 C4 113.2(7)
C2A C1 C4 138.5(10)
N1 C1 C3 110.6(7)
C2A C1 C3 51.6(8)
C4 C1 C3 115.5(8)
N1 C1 C4A 108.9(7)
C2A C1 C4A 115.2(11)
C4 C1 C4A 44.9(8)
C3 C1 C4A 140.6(9)
N1 C1 C3A 105.5(8)
C2A C1 C3A 113.8(10)
C4 C1 C3A 60.8(8)
C3 C1 C3A 63.6(8)
C4A C1 C3A 105.2(9)
N1 C1 C2 107.7(6)
C2A C1 C2 53.5(8)
C4 C1 C2 106.4(9)
C3 C1 C2 102.5(9)
C4A C1 C2 65.3(8)
C3A C1 C2 146.7(9)
C1 C2 H2A 109.5
C1 C2 H2B 109.5
C1 C2 H2C 109.5
C1 C3 H3A 109.5
C1 C3 H3B 109.5
C1 C3 H3C 109.5
C1 C4 H4A 109.5
C1 C4 H4B 109.5
C1 C4 H4C 109.5
C1 C2A H2A1 109.5
C1 C2A H2A2 109.5
H2A1 C2A H2A2 109.5
C1 C2A H2A3 109.5
H2A1 C2A H2A3 109.5
H2A2 C2A H2A3 109.5
C1 C3A H3A1 109.5
C1 C3A H3A2 109.5
H3A1 C3A H3A2 109.5
C1 C3A H3A3 109.5
H3A1 C3A H3A3 109.5
H3A2 C3A H3A3 109.5
C1 C4A H4A1 109.5
C1 C4A H4A2 109.5
H4A1 C4A H4A2 109.5
C1 C4A H4A3 109.5
H4A1 C4A H4A3 109.5
H4A2 C4A H4A3 109.5
N2 C5 C8 109.1(5)
N2 C5 C6 110.0(5)
C8 C5 C6 109.6(5)
N2 C5 C7 109.1(4)
C8 C5 C7 109.4(5)
C6 C5 C7 109.6(5)
C5 C6 H6A 109.5
C5 C6 H6B 109.5
H6A C6 H6B 109.5
C5 C6 H6C 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
C5 C7 H7A 109.5
C5 C7 H7B 109.5
H7A C7 H7B 109.5
C5 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
C5 C8 H8A 109.5
C5 C8 H8B 109.5
H8A C8 H8B 109.5
C5 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
P1 C9 H9A 109.5
P1 C9 H9B 109.5
H9A C9 H9B 109.5
P1 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
P1 C10 H10A 109.5
P1 C10 H10B 109.5
H10A C10 H10B 109.5
P1 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
P1 C11 H11A 109.5
P1 C11 H11B 109.5
H11A C11 H11B 109.5
P1 C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
P2 C12 H12A 109.5
P2 C12 H12B 109.5
H12A C12 H12B 109.5
P2 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
P2 C13 H13A 109.5
P2 C13 H13B 109.5
H13A C13 H13B 109.5
P2 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
P2 C14 H14A 109.5
P2 C14 H14B 109.5
H14A C14 H14B 109.5
P2 C14 H14C 109.5
H14A C14 H14C 109.5
H14B C14 H14C 109.5
C20 C15 C16 114.0(5)
C20 C15 V1 124.5(5)
C16 C15 V1 121.5(4)
C17 C16 C15 122.5(6)
C17 C16 H16 118.8
C15 C16 H16 118.8
C18 C17 C16 120.6(6)
C18 C17 H17 119.7
C16 C17 H17 119.7
C17 C18 C19 119.8(6)
C17 C18 H18 120.1
C19 C18 H18 120.1
C20 C19 C18 118.3(6)
C20 C19 H19 120.8
C18 C19 H19 120.8
C19 C20 C15 124.7(6)
C19 C20 H20 117.6
C15 C20 H20 117.6
C1 N1 V1 172.0(4)
C5 N2 V1 160.6(4)
C10 P1 C9 103.9(3)
C10 P1 C11 101.7(3)
C9 P1 C11 102.5(3)
C10 P1 V1 117.0(2)
C9 P1 V1 115.1(2)
C11 P1 V1 114.76(19)
C13 P2 C12 104.0(3)
C13 P2 C14 102.1(3)
C12 P2 C14 101.1(3)
C13 P2 V1 116.6(2)
C12 P2 V1 115.3(2)
C14 P2 V1 115.8(2)
N1 V1 N2 119.6(2)
N1 V1 C15 116.4(2)
N2 V1 C15 124.0(2)
N1 V1 P1 95.50(16)
N2 V1 P1 93.96(15)
C15 V1 P1 79.39(15)
N1 V1 P2 96.78(16)
N2 V1 P2 95.47(16)
C15 V1 P2 79.09(15)
P1 V1 P2 158.26(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.444(7)
C1 C2A 1.450(18)
C1 C4 1.474(13)
C1 C3 1.535(15)
C1 C4A 1.587(17)
C1 C3A 1.608(17)
C1 C2 1.641(15)
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
C3 H3A 0.9800
C3 H3B 0.9800
C3 H3C 0.9800
C4 H4A 0.9800
C4 H4B 0.9800
C4 H4C 0.9800
C2A H2A1 0.9800
C2A H2A2 0.9800
C2A H2A3 0.9800
C3A H3A1 0.9800
C3A H3A2 0.9800
C3A H3A3 0.9800
C4A H4A1 0.9800
C4A H4A2 0.9800
C4A H4A3 0.9800
C5 N2 1.440(7)
C5 C8 1.518(8)
C5 C6 1.523(8)
C5 C7 1.548(8)
C6 H6A 0.9800
C6 H6B 0.9800
C6 H6C 0.9800
C7 H7A 0.9800
C7 H7B 0.9800
C7 H7C 0.9800
C8 H8A 0.9800
C8 H8B 0.9800
C8 H8C 0.9800
C9 P1 1.822(6)
C9 H9A 0.9800
C9 H9B 0.9800
C9 H9C 0.9800
C10 P1 1.814(6)
C10 H10A 0.9800
C10 H10B 0.9800
C10 H10C 0.9800
C11 P1 1.835(6)
C11 H11A 0.9800
C11 H11B 0.9800
C11 H11C 0.9800
C12 P2 1.821(6)
C12 H12A 0.9800
C12 H12B 0.9800
C12 H12C 0.9800
C13 P2 1.803(6)
C13 H13A 0.9800
C13 H13B 0.9800
C13 H13C 0.9800
C14 P2 1.831(6)
C14 H14A 0.9800
C14 H14B 0.9800
C14 H14C 0.9800
C15 C20 1.397(8)
C15 C16 1.424(8)
C15 V1 2.175(5)
C16 C17 1.398(7)
C16 H16 0.9500
C17 C18 1.365(9)
C17 H17 0.9500
C18 C19 1.403(9)
C18 H18 0.9500
C19 C20 1.394(7)
C19 H19 0.9500
C20 H20 0.9500
N1 V1 1.707(5)
N2 V1 1.718(5)
P1 V1 2.4264(18)
P2 V1 2.4375(19)
