#------------------------------------------------------------------------------
#$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/51/2005151.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2005151
loop_
_publ_author_name
'Hope, H.'
'Borer, L. L.'
_publ_section_title
;5,5'-(2-Hydroxy-1,3-propandiyldiamino)bis(1-phenyl-1,3-hexanedionato-<i>O</i>,<i>O</i>')oxovanadium(IV),
 [VO(C~27~H~28~N~2~O~5~)]
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1621
_journal_page_last               1624
_journal_paper_doi               10.1107/S0108270196002636
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[V O (C27 H28 N2 O5)]'
_chemical_formula_sum            'C27 H28 N2 O6 V'
_chemical_formula_weight         527.45
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                85.18(2)
_cell_angle_beta                 77.79(2)
_cell_angle_gamma                63.75(2)
_cell_formula_units_Z            2
_cell_length_a                   9.360(2)
_cell_length_b                   9.845(2)
_cell_length_c                   15.216(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    118.0(10)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     1229.0(5)
_diffrn_measurement_device       'Siemens P4/R'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3010
_diffrn_reflns_theta_max         55
_diffrn_standards_decay_%        .0
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.762
_exptl_absorpt_correction_T_max  1.26
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type
'empirical (XABS2; Parkin, Moezzi & Hope, 1995)'
_exptl_crystal_colour            'greenish yellow'
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.48
_refine_ls_extinction_coef       0.0008(4)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_obs   1.054
_refine_ls_hydrogen_treatment    'H atoms included as riding (H on N free)'
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3010
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_obs          0.065
_refine_ls_shift/esd_max         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
w = 1/[\s2(F~o~^2^) + (0.0776P)^2^ + 1.33P], where
P = [Max(F~o~^2^,0) + 2F~c~^2^]/3
;
_refine_ls_wR_factor_all         0.1668
_refine_ls_wR_factor_obs         0.147
_reflns_number_observed          2285
_reflns_number_total             3010
_reflns_observed_criterion       I>2s(I)
_[local]_cod_data_source_file    mu1216.cif
_[local]_cod_data_source_block   borer
_[local]_cod_chemical_formula_sum_orig 'C27 H28 N2 O6 V1'
_cod_database_code               2005151
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
V 0.0350(10) 0.0360(10) 0.0350(10) -0.0010(10) -0.0070(10) -0.0170(10)
O(1) 0.042(3) 0.040(3) 0.055(3) 0.003(2) -0.012(2) -0.022(2)
C(1) 0.040(5) 0.041(6) 0.056(7) 0.010(5) -0.017(5) -0.026(5)
C(2) 0.043(4) 0.047(5) 0.061(5) 0.016(4) -0.016(4) -0.025(4)
N(1) 0.036(3) 0.048(4) 0.046(4) 0.014(3) -0.006(3) -0.021(3)
C(3) 0.032(4) 0.049(5) 0.045(5) 0.012(4) -0.004(3) -0.015(4)
C(4) 0.046(4) 0.057(5) 0.032(4) 0.001(4) -0.003(3) -0.025(4)
C(5) 0.037(4) 0.042(4) 0.041(5) 0.001(4) -0.006(3) -0.016(3)
O(2) 0.042(3) 0.050(3) 0.033(3) -0.001(2) -0.003(2) -0.024(2)
C(6) 0.047(4) 0.044(4) 0.031(4) -0.003(3) -0.006(3) -0.019(4)
C(7) 0.040(4) 0.033(4) 0.038(4) -0.001(3) -0.014(3) -0.014(3)
O(3) 0.041(2) 0.039(3) 0.033(3) -0.010(2) -0.001(2) -0.017(2)
C(8) 0.037(4) 0.037(4) 0.036(4) -0.002(3) -0.007(3) -0.014(3)
C(9) 0.047(4) 0.040(4) 0.042(4) -0.007(3) -0.005(3) -0.020(4)
C(10) 0.045(4) 0.037(4) 0.049(5) -0.005(4) -0.002(3) -0.020(4)
C(11) 0.049(4) 0.036(4) 0.052(5) -0.004(4) -0.013(4) -0.017(4)
C(12) 0.056(4) 0.044(5) 0.041(5) -0.010(4) -0.011(4) -0.021(4)
C(13) 0.053(4) 0.059(5) 0.033(4) -0.001(4) -0.008(3) -0.029(4)
C(14) 0.056(5) 0.065(6) 0.061(6) 0.006(5) 0.003(4) -0.029(4)
C(15) 0.038(4) 0.060(5) 0.066(5) 0.022(4) -0.020(4) -0.028(4)
N(2) 0.039(3) 0.059(4) 0.057(5) 0.011(3) -0.017(3) -0.032(3)
C(16) 0.042(4) 0.037(4) 0.053(5) 0.007(4) -0.022(4) -0.019(3)
C(17) 0.043(4) 0.034(4) 0.049(5) 0.000(3) -0.017(3) -0.013(3)
C(18) 0.036(4) 0.029(4) 0.046(5) 0.003(3) -0.014(3) -0.011(3)
O(4) 0.038(2) 0.044(3) 0.038(3) 0.006(2) -0.011(2) -0.021(2)
C(19) 0.037(3) 0.039(4) 0.035(4) -0.007(3) -0.007(3) -0.015(3)
C(20) 0.029(3) 0.025(4) 0.042(5) 0.004(3) -0.004(3) -0.007(3)
O(5) 0.045(3) 0.039(3) 0.031(3) -0.002(2) -0.004(2) -0.021(2)
C(21) 0.033(3) 0.031(4) 0.034(4) 0.002(3) -0.007(3) -0.006(3)
C(22) 0.041(4) 0.038(4) 0.041(4) 0.004(3) -0.010(3) -0.016(3)
C(23) 0.045(4) 0.051(5) 0.050(5) 0.008(4) -0.010(4) -0.027(4)
C(24) 0.040(4) 0.044(5) 0.058(6) 0.011(4) 0.001(4) -0.012(4)
C(25) 0.058(5) 0.045(5) 0.037(4) -0.002(4) 0.000(4) -0.013(4)
C(26) 0.050(4) 0.043(4) 0.037(5) 0.000(4) -0.007(3) -0.018(4)
C(27) 0.052(4) 0.045(5) 0.071(6) 0.009(4) -0.027(4) -0.028(4)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
V .45450(10) .71810(10) .80640(10) .0340(10)
O(1) .3048(5) .8696(5) .7843(3) .0440(10)
C(1) .9939(8) .9102(9) .7095(4) .042(2)
C(2) .8570(7) .9562(7) .6590(5) .048(2)
N(1) .8080(6) .8423(6) .6412(4) .043(2)
C(3) .8510(7) .7603(8) .5665(4) .044(2)
C(4) .7909(8) .6570(8) .5603(4) .045(2)
C(5) .6784(7) .6284(7) .6278(4) .041(2)
O(2) .6311(5) .6993(5) .7042(3) .0410(10)
C(6) .6219(7) .5219(7) .6133(4) .041(2)
C(7) .5187(7) .4818(7) .6774(4) .037(2)
O(3) .4473(5) .5489(5) .7550(3) .0390(10)
C(8) .4843(7) .3521(7) .6616(4) .038(2)
C(9) .4087(8) .2962(7) .7354(4) .042(2)
C(10) .3805(8) .1722(7) .7260(4) .044(2)
C(11) .4285(8) .0999(7) .6437(4) .046(2)
C(12) .5022(8) .1542(7) .5701(4) .046(2)
C(13) .5312(8) .2781(8) .5793(4) .047(2)
C(14) .9645(9) .7857(9) .4883(5) .062(2)
C(15) 1.0036(7) .7826(8) .7765(4) .052(2)
N(2) .8521(6) .8128(7) .8358(4) .047(2)
C(16) .8099(7) .8510(7) .9235(4) .041(2)
C(17) .6812(7) .8372(7) .9794(4) .042(2)
C(18) .5748(7) .7870(7) .9542(4) .038(2)
O(4) .5865(5) .7680(5) .8687(3) .0380(10)
C(19) .4627(7) .7545(7) 1.0197(4) .037(2)
C(20) .3691(7) .6882(7) 1.0010(4) .034(2)
O(5) .3709(5) .6524(5) .9207(3) .0370(10)
C(21) .2574(7) .6519(7) 1.0745(4) .036(2)
C(22) .1716(7) .5792(7) 1.0510(4) .041(2)
C(23) .0600(8) .5501(8) 1.1154(4) .047(2)
C(24) .0325(8) .5923(8) 1.2037(5) .052(2)
C(25) .1184(8) .6614(8) 1.2283(4) .052(2)
C(26) .2293(8) .6919(8) 1.1638(4) .044(2)
C(27) .9119(8) .9084(8) .9591(5) .052(2)
O(6) 1.1392(7) .8596(7) .6448(4) .047(2)
O(6A) 1.023(2) 1.0052(15) .7154(12) .050(7)
C(1A) 1.0187(8) .8711 .6939(5) .050
H(1) .9818(8) .9960(9) .7412(4) .040
H(2A) .7629(7) 1.0346(7) .6937(5) .050
H(2B) .8830(7) .9994(7) .6024(5) .050
H(1N) .742(7) .820(8) .681(4) .05(2)
H(4) .8270(8) .6023(8) .5045(4) .050
H(6) .6569(7) .4753(7) .5548(4) .050
H(9) .3779(8) .3432(7) .7935(4) .050
H(10) .3264(8) .1362(7) .7766(4) .050
H(11) .4101(8) .0129(7) .6376(4) .050
H(12) .5341(8) .1045(7) .5128(4) .050
H(13) .5840(8) .3133(8) .5278(4) .050
H(14A) .9087(9) .8848(9) .4649(5) .070
H(14B) .9980(9) .7124(9) .4413(5) .070
H(14C) 1.0590(9) .7801(9) .5066(5) .070
H(15A) 1.0834(7) .7658(8) .8119(4) .050
H(15B) 1.0393(7) .6916(8) .7426(4) .050
H(2N) .786(7) .779(7) .827(4) .043(19)
H(17) .6634(7) .8625(7) 1.0416(4) .050
H(19) .4492(7) .7812(7) 1.0812(4) .050
H(22) .1909(7) .5479(7) .9898(4) .050
H(23) -.004(8) .5020(8) 1.0991(4) .050
H(24) -.0462(8) .5739(8) 1.2482(5) .050
H(25) .1019(8) .6877(8) 1.2902(4) .050
H(26) .2878(8) .7412(8) 1.1811(4) .050
H(27A) .8654(8) .9384(8) 1.0209(5) .080
H(27B) .9159(8) .9936(8) .9249(5) .080
H(27C) 1.0207(8) .8301(8) .9547(5) .080
H(6O) 1.2170(7) .8498(7) .6691(4) .050
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(1) V O(3) 107.9(2) yes
O(1) V O(5) 104.8(2) yes
O(3) V O(5) 85.9(2) yes
O(1) V O(4) 110.1(2) yes
O(3) V O(4) 141.8(2) yes
O(5) V O(4) 87.6(2) yes
O(1) V O(2) 103.0(2) yes
O(3) V O(2) 87.3(2) yes
O(5) V O(2) 152.1(2) yes
O(4) V O(2) 81.3(2) yes
O(6A) C(1) O(6) 82.3(10) yes
O(6A) C(1) C(2) 111.0(11) yes
O(6) C(1) C(2) 106.9(5) yes
O(6A) C(1) C(15) 128.2(12) yes
O(6) C(1) C(15) 108.8(6) yes
C(2) C(1) C(15) 113.2(5) yes
N(1) C(2) C(1) 118.4(5) yes
C(3) N(1) C(2) 128.5(5) yes
N(1) C(3) C(4) 121.1(5) yes
N(1) C(3) C(14) 118.1(5) yes
C(4) C(3) C(14) 120.7(6) yes
C(3) C(4) C(5) 125.7(6) yes
O(2) C(5) C(4) 118.4(5) yes
O(2) C(5) C(6) 120.8(5) yes
C(4) C(5) C(6) 120.9(6) yes
C(5) O(2) V 131.2(3) yes
C(7) C(6) C(5) 124.3(5) yes
O(3) C(7) C(6) 124.1(5) yes
O(3) C(7) C(8) 114.8(4) yes
C(6) C(7) C(8) 121.1(5) yes
C(7) O(3) V 130.3(3) yes
C(13) C(8) C(9) 117.9(5) yes
C(13) C(8) C(7) 123.8(5) yes
C(9) C(8) C(7) 118.1(5) yes
C(10) C(9) C(8) 120.9(5) yes
C(11) C(10) C(9) 120.3(5) yes
C(10) C(11) C(12) 119.6(5) yes
C(11) C(12) C(13) 120.3(6) yes
C(12) C(13) C(8) 121.0(5) yes
N(2) C(15) C(1A) 123.2(6) yes
N(2) C(15) C(1) 113.1(5) yes
C(1A) C(15) C(1) 15.6(4) yes
C(16) N(2) C(15) 127.6(5) yes
N(2) C(16) C(17) 122.2(5) yes
N(2) C(16) C(27) 117.1(5) yes
C(17) C(16) C(27) 120.7(6) yes
C(16) C(17) C(18) 126.2(6) yes
O(4) C(18) C(19) 121.0(5) yes
O(4) C(18) C(17) 117.9(5) yes
C(19) C(18) C(17) 121.1(6) yes
C(18) O(4) V 130.7(3) yes
C(20) C(19) C(18) 124.3(5) yes
O(5) C(20) C(19) 123.8(5) yes
O(5) C(20) C(21) 115.0(4) yes
C(19) C(20) C(21) 121.2(5) yes
C(20) O(5) V 128.8(3) yes
C(26) C(21) C(22) 118.3(5) yes
C(26) C(21) C(20) 123.6(5) yes
C(22) C(21) C(20) 118.1(5) yes
C(23) C(22) C(21) 120.6(6) yes
C(24) C(23) C(22) 120.2(5) yes
C(23) C(24) C(25) 119.9(5) yes
C(24) C(25) C(26) 120.1(6) yes
C(21) C(26) C(25) 120.9(6) yes
O(6A) C(1A) C(15) 110.3(9) yes
O(6A) C(1A) C(2) 93.7(8) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
V O(1) 1.602(5) yes
V O(3) 1.932(4) yes
V O(5) 1.933(4) yes
V O(4) 1.943(4) yes
V O(2) 1.969(4) yes
C(1) O(6) 1.408(8) yes
C(1) C(2) 1.510(4) yes
C(1) C(15) 1.533(4) yes
C(2) N(1) 1.449(7) yes
C(2) C(1A) 1.555(5) yes
N(1) C(3) 1.334(7) yes
C(3) C(4) 1.380(7) yes
C(3) C(14) 1.503(7) yes
C(4) C(5) 1.414(7) yes
C(5) O(2) 1.296(7) yes
C(5) C(6) 1.417(7) yes
C(6) C(7) 1.383(7) yes
C(7) O(3) 1.299(6) yes
C(7) C(8) 1.496(7) yes
C(8) C(13) 1.389(7) yes
C(8) C(9) 1.403(7) yes
C(9) C(10) 1.382(7) yes
C(10) C(11) 1.380(8) yes
C(11) C(12) 1.384(8) yes
C(12) C(13) 1.385(8) yes
C(15) N(2) 1.430(7) yes
C(15) C(1A) 1.486(5) yes
N(2) C(16) 1.345(7) yes
C(16) C(17) 1.373(7) yes
C(16) C(27) 1.507(7) yes
C(17) C(18) 1.418(7) yes
C(18) O(4) 1.305(7) yes
C(18) C(19) 1.414(7) yes
C(19) C(20) 1.385(7) yes
C(20) O(5) 1.294(6) yes
C(20) C(21) 1.498(7) yes
C(21) C(26) 1.385(7) yes
C(21) C(22) 1.400(7) yes
C(22) C(23) 1.385(7) yes
C(23) C(24) 1.377(8) yes
C(24) C(25) 1.379(8) yes
C(25) C(26) 1.388(8) yes
O(6A) C(1A) 1.406(9) yes