#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:59:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179165 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/26/4312616.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_4312616
loop_
_publ_author_name
'Fabien Wolff'
'Christian Lorber'
'Robert Choukroun'
'Bruno Donnadieu'
_publ_contact_author             'Dr. Robert Choukroun, Dr. Christian Lorber'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France   
;
_publ_contact_author_email
'choukrou@lcc-toulouse.fr or lorber@lcc-toulouse.fr'
_publ_contact_author_fax         ' 33 (0) 5 61 55 30 03 '
_publ_section_title
;
 Vanadium(V) Complexes of a Chelating Dianionic [ONNO]-Type Amine
 Bis(Phenolate) Ligand: Synthesis and Solid State and Solution Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7839
_journal_page_last               7845
_journal_paper_doi               10.1021/ic034742f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C25 H37 N2 O4 V'
_chemical_formula_weight         480.51
_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.
_cell_angle_beta                 103.462(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.008(2)
_cell_length_b                   13.075(1)
_cell_length_c                   13.863(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.15
_cell_volume                     2469.3(5)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       φ
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18908
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  5
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0567P)²+0.4841P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                3898
_reflns_number_total             4820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034742fsi20030630_051806_2.cif
_cod_data_source_block           1a
_cod_original_cell_volume        2469.2(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4312616
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
V1 V 0.23971(2) 0.16095(2) 0.97917(2) 0.02354(10) Uani 1 1 d . . .
N1 N 0.12948(10) 0.25052(11) 1.04573(10) 0.0241(3) Uani 1 1 d . . .
N2 N 0.25441(11) 0.07948(12) 1.13525(11) 0.0297(3) Uani 1 1 d . . .
O1 O 0.32477(9) 0.25288(9) 1.05913(9) 0.0277(3) Uani 1 1 d . . .
O2 O 0.12985(9) 0.07152(9) 0.94028(9) 0.0282(3) Uani 1 1 d . . .
O3 O 0.21496(9) 0.22921(10) 0.88098(9) 0.0309(3) Uani 1 1 d . . .
O4 O 0.33056(9) 0.07380(10) 0.95898(9) 0.0295(3) Uani 1 1 d . . .
C1 C 0.13509(13) 0.36044(13) 1.02112(13) 0.0279(4) Uani 1 1 d . . .
H1A H 0.0905 0.3987 1.0540 0.033 Uiso 1 1 calc R . .
H1B H 0.1097 0.3685 0.9487 0.033 Uiso 1 1 calc R . .
C2 C 0.23559(13) 0.41020(13) 1.04950(12) 0.0263(4) Uani 1 1 d . . .
C3 C 0.24007(13) 0.51642(14) 1.06021(12) 0.0280(4) Uani 1 1 d . . .
H3 H 0.1806 0.5538 1.0519 0.034 Uiso 1 1 calc R . .
C4 C 0.32835(14) 0.56922(14) 1.08253(13) 0.0299(4) Uani 1 1 d . . .
C5 C 0.41457(14) 0.51238(14) 1.09437(13) 0.0302(4) Uani 1 1 d . . .
H5 H 0.4757 0.5473 1.1088 0.036 Uiso 1 1 calc R . .
C6 C 0.41404(13) 0.40676(14) 1.08575(12) 0.0271(4) Uani 1 1 d . . .
C7 C 0.32302(13) 0.35524(13) 1.06296(12) 0.0248(3) Uani 1 1 d . . .
C8 C 0.05040(12) 0.10671(13) 0.87374(12) 0.0256(4) Uani 1 1 d . . .
C9 C 0.02096(13) 0.06302(14) 0.77919(13) 0.0291(4) Uani 1 1 d . . .
C10 C -0.06065(14) 0.10387(14) 0.71419(13) 0.0318(4) Uani 1 1 d . . .
H10 H -0.0812 0.0744 0.6501 0.038 Uiso 1 1 calc R . .
C11 C -0.11356(13) 0.18563(14) 0.73827(14) 0.0316(4) Uani 1 1 d . . .
C12 C -0.08353(13) 0.22660(14) 0.83347(14) 0.0294(4) Uani 1 1 d . . .
H12 H -0.1188 0.2824 0.8522 0.035 Uiso 1 1 calc R . .
C13 C -0.00303(13) 0.18727(13) 0.90128(13) 0.0255(4) Uani 1 1 d . . .
C14 C 0.02422(13) 0.21867(14) 1.00838(13) 0.0283(4) Uani 1 1 d . . .
H14A H 0.0106 0.1608 1.0493 0.034 Uiso 1 1 calc R . .
H14B H -0.0185 0.2763 1.0180 0.034 Uiso 1 1 calc R . .
C15 C 0.15741(14) 0.23367(14) 1.15532(12) 0.0295(4) Uani 1 1 d . . .
H15A H 0.1043 0.2587 1.1854 0.035 Uiso 1 1 calc R . .
H15B H 0.2177 0.2728 1.1844 0.035 Uiso 1 1 calc R . .
C16 C 0.17502(14) 0.12103(15) 1.17826(13) 0.0323(4) Uani 1 1 d . . .
H16A H 0.1927 0.1113 1.2511 0.039 Uiso 1 1 calc R . .
H16B H 0.1137 0.0826 1.1514 0.039 Uiso 1 1 calc R . .
C17 C 0.33269(16) 0.68365(14) 1.09696(16) 0.0381(4) Uani 1 1 d . . .
H17A H 0.2659 0.7112 1.0844 0.057 Uiso 1 1 calc R . .
H17B H 0.3675 0.7146 1.0506 0.057 Uiso 1 1 calc R . .
H17C H 0.3675 0.6995 1.1652 0.057 Uiso 1 1 calc R . .
C18 C 0.50729(14) 0.34563(15) 1.10095(15) 0.0351(4) Uani 1 1 d . . .
H18A H 0.5635 0.3922 1.1096 0.053 Uiso 1 1 calc R . .
H18B H 0.5050 0.3020 1.0430 0.053 Uiso 1 1 calc R . .
H18C H 0.5141 0.3028 1.1602 0.053 Uiso 1 1 calc R . .
C19 C 0.07605(16) -0.02577(16) 0.75128(16) 0.0412(5) Uani 1 1 d . . .
H19A H 0.0420 -0.0511 0.6858 0.062 Uiso 1 1 calc R . .
H19B H 0.0798 -0.0804 0.8005 0.062 Uiso 1 1 calc R . .
H19C H 0.1425 -0.0040 0.7493 0.062 Uiso 1 1 calc R . .
C20 C -0.20247(17) 0.22630(18) 0.66503(17) 0.0465(5) Uani 1 1 d . . .
H20A H -0.1816 0.2754 0.6206 0.070 Uiso 1 1 calc R . .
H20B H -0.2461 0.2604 0.7009 0.070 Uiso 1 1 calc R . .
H20C H -0.2375 0.1695 0.6260 0.070 Uiso 1 1 calc R . .
C21 C 0.35038(15) 0.09854(18) 1.20385(15) 0.0425(5) Uani 1 1 d . . .
H21A H 0.3553 0.0583 1.2645 0.064 Uiso 1 1 calc R . .
H21B H 0.3565 0.1714 1.2206 0.064 Uiso 1 1 calc R . .
H21C H 0.4031 0.0785 1.1720 0.064 Uiso 1 1 calc R . .
C22 C 0.24327(17) -0.03231(15) 1.12174(16) 0.0398(5) Uani 1 1 d . . .
H22A H 0.2963 -0.0588 1.0935 0.060 Uiso 1 1 calc R . .
H22B H 0.1798 -0.0474 1.0767 0.060 Uiso 1 1 calc R . .
H22C H 0.2464 -0.0649 1.1861 0.060 Uiso 1 1 calc R . .
C23 C 0.36168(14) 0.05816(15) 0.86838(13) 0.0330(4) Uani 1 1 d . . .
H23 H 0.3045 0.0692 0.8109 0.040 Uiso 1 1 calc R . .
C24 C 0.39631(19) -0.05090(18) 0.86713(18) 0.0500(6) Uani 1 1 d . . .
H24A H 0.4579 -0.0595 0.9172 0.075 Uiso 1 1 calc R . .
H24B H 0.4071 -0.0670 0.8014 0.075 Uiso 1 1 calc R . .
H24C H 0.3465 -0.0971 0.8819 0.075 Uiso 1 1 calc R . .
C25 C 0.44120(19) 0.1340(2) 0.86255(18) 0.0519(6) Uani 1 1 d . . .
H25A H 0.4165 0.2036 0.8663 0.078 Uiso 1 1 calc R . .
H25B H 0.4608 0.1251 0.7997 0.078 Uiso 1 1 calc R . .
H25C H 0.4980 0.1225 0.9179 0.078 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'
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
O3 V1 O4 104.20(6) . . ?
O3 V1 O1 97.37(7) . . ?
O4 V1 O1 97.18(6) . . ?
O3 V1 O2 95.79(6) . . ?
O4 V1 O2 97.04(6) . . ?
O1 V1 O2 157.62(6) . . ?
O3 V1 N1 91.41(6) . . ?
O4 V1 N1 164.38(5) . . ?
O1 V1 N1 80.14(6) . . ?
O2 V1 N1 81.51(6) . . ?
O3 V1 N2 169.08(6) . . ?
O4 V1 N2 86.71(6) . . ?
O1 V1 N2 80.78(6) . . ?
O2 V1 N2 82.87(5) . . ?
N1 V1 N2 77.68(6) . . ?
C1 N1 C15 111.18(13) . . ?
C1 N1 C14 106.82(13) . . ?
C15 N1 C14 108.24(13) . . ?
C1 N1 V1 108.97(10) . . ?
C15 N1 V1 106.97(11) . . ?
C14 N1 V1 114.70(10) . . ?
C21 N2 C22 107.59(16) . . ?
C21 N2 C16 109.58(16) . . ?
C22 N2 C16 110.29(15) . . ?
C21 N2 V1 112.56(11) . . ?
C22 N2 V1 110.10(11) . . ?
C16 N2 V1 106.73(11) . . ?
C7 O1 V1 130.71(11) . . ?
C8 O2 V1 117.82(11) . . ?
C23 O4 V1 127.06(11) . . ?
N1 C1 C2 116.84(14) . . ?
C7 C2 C3 118.80(16) . . ?
C7 C2 C1 123.15(16) . . ?
C3 C2 C1 118.03(16) . . ?
C4 C3 C2 122.31(17) . . ?
C3 C4 C5 117.62(17) . . ?
C3 C4 C17 121.98(18) . . ?
C5 C4 C17 120.38(17) . . ?
C6 C5 C4 122.26(17) . . ?
C5 C6 C7 118.77(17) . . ?
C5 C6 C18 122.04(16) . . ?
C7 C6 C18 119.19(16) . . ?
O1 C7 C2 122.21(15) . . ?
O1 C7 C6 117.50(15) . . ?
C2 C7 C6 120.23(16) . . ?
O2 C8 C13 118.64(15) . . ?
O2 C8 C9 121.10(16) . . ?
C13 C8 C9 120.25(16) . . ?
C10 C9 C8 117.99(17) . . ?
C10 C9 C19 121.89(17) . . ?
C8 C9 C19 120.12(17) . . ?
C11 C10 C9 123.15(17) . . ?
C10 C11 C12 117.63(17) . . ?
C10 C11 C20 120.93(18) . . ?
C12 C11 C20 121.40(18) . . ?
C13 C12 C11 121.13(17) . . ?
C12 C13 C8 119.81(16) . . ?
C12 C13 C14 123.22(16) . . ?
C8 C13 C14 116.60(15) . . ?
C13 C14 N1 114.80(14) . . ?
N1 C15 C16 110.37(14) . . ?
N2 C16 C15 111.89(15) . . ?
O4 C23 C25 109.36(16) . . ?
O4 C23 C24 107.97(16) . . ?
C25 C23 C24 112.20(18) . . ?
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 O3 1.5969(13) . ?
V1 O4 1.7782(13) . ?
V1 O1 1.8651(13) . ?
V1 O2 1.9078(13) . ?
V1 N1 2.2959(15) . ?
V1 N2 2.3773(16) . ?
N1 C1 1.484(2) . ?
N1 C15 1.494(2) . ?
N1 C14 1.503(2) . ?
N2 C21 1.476(2) . ?
N2 C22 1.477(2) . ?
N2 C16 1.482(2) . ?
O1 C7 1.340(2) . ?
O2 C8 1.350(2) . ?
O4 C23 1.437(2) . ?
C1 C2 1.517(2) . ?
C2 C7 1.395(2) . ?
C2 C3 1.397(3) . ?
C3 C4 1.387(3) . ?
C4 C5 1.395(3) . ?
C4 C17 1.509(3) . ?
C5 C6 1.386(3) . ?
C6 C7 1.411(2) . ?
C6 C18 1.504(3) . ?
C8 C13 1.396(3) . ?
C8 C9 1.401(2) . ?
C9 C10 1.387(3) . ?
C9 C19 1.494(3) . ?
C10 C11 1.385(3) . ?
C11 C12 1.395(3) . ?
C11 C20 1.509(3) . ?
C12 C13 1.388(3) . ?
C13 C14 1.502(2) . ?
C15 C16 1.515(3) . ?
C23 C25 1.507(3) . ?
C23 C24 1.508(3) . ?
