#------------------------------------------------------------------------------
#$Date: 2016-02-16 18:55:33 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176466 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/20/8102072.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_8102072
loop_
_publ_author_name
'Li, L.-Z.'
'Jing, B.-Q.'
'Li, L.-W.'
'Xu, T.'
_publ_section_title
;
Crystal structure of (1,10-phenanthroline-κ²N,N')oxo-
(N-salicylideneisoleucinato-κ³O,N,O')vanadium(IV), 
VO(C₁₂H₈N₂)(C₁₃H₁₅NO₃)
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              520
_journal_page_last               522
_journal_volume                  221
_journal_year                    2006
_chemical_formula_structural     VO(C12H8N2)(C13H15NO3)
_chemical_formula_sum            'C25 H23 N3 O4 V'
_chemical_formula_weight         480.40
_chemical_name_systematic
;
(1,10-phenanthroline-κ²N,N')oxo(N-salicylideneisoleucinato-
κ³O,N,O')vanadium(IV)
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   32.593(11)
_cell_length_b                   32.593(11)
_cell_length_c                   10.974(4)
_cell_measurement_reflns_used    1885
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.218
_cell_measurement_theta_min      2.1635
_cell_volume                     10096(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       phi/omega
_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  0.1225
_diffrn_reflns_av_sigmaI/netI    0.1199
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17804
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9718
_exptl_absorpt_correction_T_min  0.8616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS  (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4482
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1534
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0539P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                1713
_reflns_number_total             3950
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            1267-1907.cff
_cod_data_source_block           060317b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C25 H23 N3 O4 V '
_cod_database_code               8102072
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.10850(3) 0.25443(3) 0.18071(7) 0.0486(3) Uani 1 18 f d . . .
N1 N 0.05538(14) 0.18653(13) 0.2112(4) 0.0503(11) Uani 1 18 f d . C .
N2 N 0.14988(13) 0.32065(13) 0.0933(3) 0.0457(10) Uani 1 18 f d . . .
N3 N 0.06308(14) 0.25667(14) 0.0161(3) 0.0461(10) Uani 1 18 f d . . .
O1 O 0.12234(12) 0.22001(13) 0.0534(3) 0.0574(9) Uani 1 18 f d . . .
O2 O 0.09864(14) 0.15280(14) -0.0450(4) 0.0840(13) Uani 1 18 f d . . .
O3 O 0.07246(12) 0.27800(11) 0.2632(3) 0.0580(9) Uani 1 18 f d . C .
O4 O 0.14789(12) 0.26304(12) 0.2782(3) 0.0682(10) Uani 1 18 f d . . .
C1 C 0.09501(19) 0.1753(2) 0.0407(5) 0.0598(15) Uani 1 18 f d . C .
C2 C 0.05817(18) 0.14986(18) 0.1392(5) 0.0590(14) Uani 1 18 f d . . .
H2 H 0.0275 0.1307 0.0989 0.071 Uiso 1 18 f calc R A 1
C4 C 0.1144(3) 0.1410(2) 0.2752(6) 0.108(2) Uani 1 18 f d . . .
H4A H 0.1132 0.1627 0.3337 0.129 Uiso 1 18 f calc R B 1
H4B H 0.1389 0.1598 0.2163 0.129 Uiso 1 18 f calc R B 1
C5 C 0.1286(3) 0.1088(3) 0.3422(9) 0.166(4) Uani 1 18 f d . C .
H5A H 0.1057 0.0914 0.4043 0.250 Uiso 1 18 f calc R . .
H5B H 0.1592 0.1278 0.3789 0.250 Uiso 1 18 f calc R . .
H5C H 0.1299 0.0871 0.2853 0.250 Uiso 1 18 f calc R . .
C3 C 0.0689(2) 0.1163(2) 0.2116(6) 0.0827(19) Uani 1 18 f d P C 1
H3 H 0.0725 0.0964 0.1505 0.099 Uiso 0.540(12) 18 f calc PR C 1
C6 C 0.0300(5) 0.0826(4) 0.2938(15) 0.141(8) Uani 0.540(12) 18 f d P C 1
H6A H 0.0009 0.0666 0.2488 0.211 Uiso 0.540(12) 18 f calc PR C 1
H6B H 0.0265 0.0998 0.3601 0.211 Uiso 0.540(12) 18 f calc PR C 1
H6C H 0.0377 0.0598 0.3252 0.211 Uiso 0.540(12) 18 f calc PR C 1
H3' H 0.0455 0.1052 0.2776 0.099 Uiso 0.460(12) 18 f calc PR C 2
C6' C 0.0569(7) 0.0719(6) 0.1419(18) 0.164(10) Uani 0.460(12) 18 f d P C 2
H6A' H 0.0259 0.0592 0.1066 0.245 Uiso 0.460(12) 18 f calc PR C 2
H6B' H 0.0573 0.0491 0.1963 0.245 Uiso 0.460(12) 18 f calc PR C 2
H6C' H 0.0798 0.0793 0.0785 0.245 Uiso 0.460(12) 18 f calc PR C 2
C7 C 0.01925(18) 0.17448(18) 0.2802(5) 0.0531(14) Uani 1 18 f d . . .
H7 H -0.0030 0.1423 0.2838 0.064 Uiso 1 18 f calc R C .
C8 C 0.00971(17) 0.20550(19) 0.3523(4) 0.0490(13) Uani 1 18 f d . C .
C9 C 0.03588(19) 0.25616(19) 0.3367(4) 0.0524(13) Uani 1 18 f d . . .
C10 C 0.0205(2) 0.2825(2) 0.4034(5) 0.0694(16) Uani 1 18 f d . C .
H10 H 0.0366 0.3153 0.3948 0.083 Uiso 1 18 f calc R . .
C11 C -0.0172(2) 0.2619(3) 0.4807(5) 0.0755(18) Uani 1 18 f d . . .
H11 H -0.0272 0.2806 0.5202 0.091 Uiso 1 18 f calc R C .
C12 C -0.0407(2) 0.2139(3) 0.5012(5) 0.0751(18) Uani 1 18 f d . C .
H12 H -0.0650 0.2002 0.5583 0.090 Uiso 1 18 f calc R . .
C13 C -0.02743(19) 0.1868(2) 0.4353(5) 0.0674(16) Uani 1 18 f d . . .
H13 H -0.0441 0.1542 0.4468 0.081 Uiso 1 18 f calc R C .
C14 C 0.19355(19) 0.35268(19) 0.1301(5) 0.0574(14) Uani 1 18 f d . . .
H14 H 0.2055 0.3464 0.2001 0.069 Uiso 1 18 f calc R . .
C15 C 0.22186(19) 0.39492(18) 0.0686(5) 0.0640(15) Uani 1 18 f d . . .
H15 H 0.2521 0.4159 0.0972 0.077 Uiso 1 18 f calc R . .
C16 C 0.20564(19) 0.40532(18) -0.0315(5) 0.0634(16) Uani 1 18 f d . . .
H16 H 0.2247 0.4333 -0.0736 0.076 Uiso 1 18 f calc R . .
C17 C 0.15954(19) 0.37357(18) -0.0729(5) 0.0510(13) Uani 1 18 f d . . .
C18 C 0.13317(17) 0.33144(17) -0.0073(4) 0.0453(12) Uani 1 18 f d . . .
C19 C 0.08638(17) 0.29759(17) -0.0480(4) 0.0428(12) Uani 1 18 f d . . .
C20 C 0.06696(19) 0.30732(19) -0.1493(4) 0.0508(13) Uani 1 18 f d . . .
C21 C 0.0214(2) 0.2723(2) -0.1853(5) 0.0641(15) Uani 1 18 f d . . .
H21 H 0.0074 0.2772 -0.2531 0.077 Uiso 1 18 f calc R . .
C22 C -0.00207(19) 0.2314(2) -0.1216(5) 0.0619(15) Uani 1 18 f d . . .
H22 H -0.0323 0.2081 -0.1448 0.074 Uiso 1 18 f calc R . .
C23 C 0.01995(18) 0.22473(19) -0.0205(5) 0.0565(14) Uani 1 18 f d . . .
H23 H 0.0036 0.1966 0.0232 0.068 Uiso 1 18 f calc R . .
C24 C 0.1385(2) 0.3827(2) -0.1752(5) 0.0659(16) Uani 1 18 f d . . .
H24 H 0.1555 0.4110 -0.2175 0.079 Uiso 1 18 f calc R . .
C25 C 0.0943(2) 0.3510(2) -0.2120(5) 0.0688(16) Uani 1 18 f d . . .
H25 H 0.0814 0.3578 -0.2794 0.083 Uiso 1 18 f 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 V1 O3 102.36(17) . . ?
O4 V1 O1 100.55(17) . . ?
O3 V1 O1 156.49(15) . . ?
O4 V1 N1 104.71(16) . . ?
O3 V1 N1 89.98(15) . . ?
O1 V1 N1 79.14(16) . . ?
O4 V1 N2 94.52(16) . . ?
O3 V1 N2 90.62(14) . . ?
O1 V1 N2 92.77(14) . . ?
N1 V1 N2 160.17(16) . . ?
O4 V1 N3 167.58(16) . . ?
O3 V1 N3 80.21(14) . . ?
O1 V1 N3 78.54(13) . . ?
N1 V1 N3 87.36(14) . . ?
N2 V1 N3 73.23(15) . . ?
C7 N1 C2 119.1(4) . . ?
C7 N1 V1 125.3(3) . . ?
C2 N1 V1 115.4(3) . . ?
C14 N2 C18 116.9(4) . . ?
C14 N2 V1 123.0(3) . . ?
C18 N2 V1 120.0(3) . . ?
C23 N3 C19 117.9(4) . . ?
C23 N3 V1 130.0(3) . . ?
C19 N3 V1 112.1(3) . . ?
C1 O1 V1 119.7(3) . . ?
C9 O3 V1 130.0(3) . . ?
O2 C1 O1 122.7(5) . . ?
O2 C1 C2 120.2(5) . . ?
O1 C1 C2 117.0(5) . . ?
N1 C2 C1 107.0(4) . . ?
N1 C2 C3 115.5(5) . . ?
C1 C2 C3 111.2(4) . . ?
N1 C2 H2 107.6 . . ?
C1 C2 H2 107.6 . . ?
C3 C2 H2 107.6 . . ?
C3 C4 C5 115.0(6) . . ?
C3 C4 H4A 108.5 . . ?
C5 C4 H4A 108.5 . . ?
C3 C4 H4B 108.5 . . ?
C5 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C3 C6 111.7(8) . . ?
C4 C3 C2 112.7(5) . . ?
C6 C3 C2 115.3(7) . . ?
C4 C3 H3 105.3 . . ?
C6 C3 H3 105.3 . . ?
C2 C3 H3 105.3 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
H6A' C6' H6B' 109.5 . . ?
H6A' C6' H6C' 109.5 . . ?
H6B' C6' H6C' 109.5 . . ?
N1 C7 C8 126.7(5) . . ?
N1 C7 H7 116.6 . . ?
C8 C7 H7 116.6 . . ?
C13 C8 C7 120.1(5) . . ?
C13 C8 C9 117.9(5) . . ?
C7 C8 C9 121.9(4) . . ?
O3 C9 C10 119.7(5) . . ?
O3 C9 C8 123.4(4) . . ?
C10 C9 C8 116.9(5) . . ?
C11 C10 C9 122.4(6) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C10 C11 C12 121.0(6) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 118.2(5) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C12 C13 C8 123.4(6) . . ?
C12 C13 H13 118.3 . . ?
C8 C13 H13 118.3 . . ?
N2 C14 C15 123.1(5) . . ?
N2 C14 H14 118.4 . . ?
C15 C14 H14 118.4 . . ?
C16 C15 C14 120.0(5) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 119.5(5) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 117.5(5) . . ?
C18 C17 C24 119.1(5) . . ?
C16 C17 C24 123.4(5) . . ?
N2 C18 C17 123.0(5) . . ?
N2 C18 C19 117.7(4) . . ?
C17 C18 C19 119.3(5) . . ?
N3 C19 C20 122.9(5) . . ?
N3 C19 C18 116.9(4) . . ?
C20 C19 C18 120.2(5) . . ?
C19 C20 C21 117.1(5) . . ?
C19 C20 C25 119.0(5) . . ?
C21 C20 C25 123.8(5) . . ?
C22 C21 C20 120.3(5) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 118.8(5) . . ?
C21 C22 H22 120.6 . . ?
C23 C22 H22 120.6 . . ?
N3 C23 C22 123.0(5) . . ?
N3 C23 H23 118.5 . . ?
C22 C23 H23 118.5 . . ?
C25 C24 C17 121.3(5) . . ?
C25 C24 H24 119.4 . . ?
C17 C24 H24 119.4 . . ?
C24 C25 C20 121.1(5) . . ?
C24 C25 H25 119.5 . . ?
C20 C25 H25 119.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O4 1.585(3) . ?
V1 O3 1.921(3) . ?
V1 O1 1.980(3) . ?
V1 N1 2.043(4) . ?
V1 N2 2.118(4) . ?
V1 N3 2.360(4) . ?
N1 C7 1.286(5) . ?
N1 C2 1.473(6) . ?
N2 C14 1.339(6) . ?
N2 C18 1.353(5) . ?
N3 C23 1.326(6) . ?
N3 C19 1.355(5) . ?
O1 C1 1.280(6) . ?
O2 C1 1.234(6) . ?
O3 C9 1.315(5) . ?
C1 C2 1.517(7) . ?
C2 C3 1.525(7) . ?
C2 H2 0.9800 . ?
C4 C3 1.464(8) . ?
C4 C5 1.531(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C3 C6 1.495(12) . ?
C3 H3 0.9800 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6' H6A' 0.9600 . ?
C6' H6B' 0.9600 . ?
C6' H6C' 0.9600 . ?
C7 C8 1.435(6) . ?
C7 H7 0.9300 . ?
C8 C13 1.389(6) . ?
C8 C9 1.441(6) . ?
C9 C10 1.399(7) . ?
C10 C11 1.362(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.373(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.368(7) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.390(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.334(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.407(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.401(6) . ?
C17 C24 1.422(7) . ?
C18 C19 1.435(6) . ?
C19 C20 1.392(6) . ?
C20 C21 1.402(7) . ?
C20 C25 1.423(7) . ?
C21 C22 1.354(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.396(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.347(7) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
