#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:11:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179279 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/99/4319967.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_4319967
loop_
_publ_author_name
'M. Kaliva'
'T. Giannadaki'
'A. Salifoglou'
'C. P. Raptopoulou'
'A. Terzis'
'V. Tangoulis'
_publ_section_title
;
 pH-Dependent Investigations of Vanadium(V)-Peroxo-Malate Complexes from
 Aqueous Solutions. In Search of Biologically Relevant Vanadium(V)-Peroxo
 Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3711
_journal_page_last               3718
_journal_paper_doi               10.1021/ic000894o
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C8 H28 N4 O19 V2'
_chemical_formula_weight         586.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                104.81(1)
_cell_angle_beta                 90.31(1)
_cell_angle_gamma                115.64(1)
_cell_formula_units_Z            2
_cell_length_a                   9.158(4)
_cell_length_b                   9.669(4)
_cell_length_c                   14.185(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      27
_cell_measurement_theta_min      12
_cell_volume                     1085.0(8)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package, C.E.Strouse 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'P21 Nicolet upgraded by Crystal Logic'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3555
_diffrn_reflns_theta_max         61.98
_diffrn_reflns_theta_min         3.25
_diffrn_standards_decay_%        -0.3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.149
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_meas      1.77
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         3329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_obs          0.0498
_refine_ls_shift/esd_max         0.162
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0855P)²+1.8273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1756
_refine_ls_wR_factor_obs         0.1315
_reflns_number_observed          2730
_reflns_number_total             3329
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000894o_2.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0855P)^2^+1.8273P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0855P)^2^+1.8273P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1085.0(7)
_cod_database_code               4319967
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V1 V 0.4570(1) 0.8569(1) 0.3977(1) 0.038(1) Uani 1 d . .
O1 O 0.5368(4) 0.6960(4) 0.4003(2) 0.047(1) Uani 1 d . .
O3 O 0.5843(4) 0.9527(3) 0.5293(2) 0.040(1) Uani 1 d . .
O5 O 0.2741(4) 0.7202(4) 0.4927(2) 0.044(1) Uani 1 d . .
O6 O 0.5889(4) 0.9457(4) 0.3361(2) 0.049(1) Uani 1 d . .
O7 O 0.2615(4) 0.8094(4) 0.3202(2) 0.049(1) Uani 1 d . .
O8 O 0.3035(4) 0.6797(4) 0.2957(2) 0.051(1) Uani 1 d . .
C1 C 0.6100(5) 0.7106(5) 0.4818(3) 0.043(1) Uani 1 d . .
O2 O 0.6786(4) 0.6286(4) 0.4913(3) 0.051(1) Uani 1 d . .
C2 C 0.6069(5) 0.8415(5) 0.5685(3) 0.043(1) Uani 1 d . .
C3 C 0.4691(6) 0.7663(6) 0.6263(4) 0.047(1) Uani 1 d . .
C4 C 0.2976(5) 0.7130(5) 0.5787(3) 0.039(1) Uani 1 d . .
O4 O 0.1847(4) 0.6605(4) 0.6288(2) 0.053(1) Uani 1 d . .
V2 V 0.1646(1) 0.1614(1) 0.0575(1) 0.039(1) Uani 1 d . .
O11 O 0.3521(4) 0.1177(4) 0.0963(3) 0.051(1) Uani 1 d . .
O13 O 0.0736(4) -0.0760(3) -0.0026(2) 0.039(1) Uani 1 d . .
O15 O 0.0629(4) 0.0659(4) 0.1846(2) 0.050(1) Uani 1 d . .
O16 O 0.2454(4) 0.2158(4) -0.0346(2) 0.054(1) Uani 1 d . .
O17 O 0.2816(4) 0.3472(4) 0.1617(3) 0.057(1) Uani 1 d . .
O18 O 0.1302(4) 0.3367(4) 0.1248(3) 0.056(1) Uani 1 d . .
C11 C 0.3210(6) -0.0272(6) 0.0874(3) 0.045(1) Uani 1 d . .
O12 O 0.4231(4) -0.0676(4) 0.1101(3) 0.058(1) Uani 1 d . .
C12 C 0.1437(6) -0.1482(6) 0.0470(3) 0.048(1) Uani 1 d . .
C13 C 0.0571(6) -0.1977(6) 0.1305(4) 0.049(1) Uani 1 d . .
C14 C 0.0170(6) -0.0694(6) 0.1985(3) 0.049(1) Uani 1 d . .
O14 O -0.0591(5) -0.1096(5) 0.2671(2) 0.078(1) Uani 1 d . .
N1 N 0.8519(6) 0.6221(5) 0.6495(3) 0.050(1) Uani 1 d . .
N2 N 0.7557(7) 0.1097(8) 0.1844(4) 0.078(2) Uani 1 d . .
N3 N -0.0417(7) 0.6734(7) 0.3850(5) 0.072(2) Uani 1 d . .
N4 N 0.4071(8) 0.6296(6) 0.0994(5) 0.082(2) Uani 1 d . .
W1 O 0.6537(7) 0.6236(6) 0.2239(4) 0.099(2) Uani 1 d . .
W2 O 0.6643(6) 0.3598(6) 0.1094(4) 0.092(2) Uani 1 d . .
W3 O 0.0661(7) 0.9123(9) 0.5622(6) 0.127(3) Uani 1 d . .
H2 H 0.7250(52) 0.9007(50) 0.6095(31) 0.033(11) Uiso 1 d . .
H3A H 0.4813(58) 0.8404(59) 0.6883(38) 0.046(13) Uiso 1 d . .
H3B H 0.4733(73) 0.6744(77) 0.6389(45) 0.074(19) Uiso 1 d . .
H12 H 0.1375(59) -0.2501(61) -0.0039(37) 0.050(14) Uiso 1 d . .
H13A H -0.0571(64) -0.2990(62) 0.0985(38) 0.053(14) Uiso 1 d . .
H13B H 0.1212(72) -0.2311(72) 0.1753(45) 0.073(18) Uiso 1 d . .
HN1A H 0.9452(71) 0.6399(65) 0.6390(40) 0.051(16) Uiso 1 d . .
HN1B H 0.8093(98) 0.5117(105) 0.6609(61) 0.117(28) Uiso 1 d . .
HN1C H 0.8608(83) 0.6998(88) 0.7115(56) 0.094(23) Uiso 1 d . .
HN1D H 0.7824(110) 0.6309(102) 0.6029(67) 0.125(31) Uiso 1 d . .
HN2A H 0.6394(85) 0.0596(78) 0.1520(48) 0.079(19) Uiso 1 d . .
HN2B H 0.8276(102) 0.1355(98) 0.1487(62) 0.106(28) Uiso 1 d . .
HN2C H 0.7742(94) 0.1706(92) 0.2267(59) 0.088(27) Uiso 1 d . .
HN3A H 0.0235(198) 0.6925(194) 0.3654(123) 0.258(81) Uiso 1 d . .
HN3B H -0.0323(80) 0.7341(81) 0.4355(52) 0.070(21) Uiso 1 d . .
HN4A H 0.3473(54) 0.6078(54) 0.0372(36) 0.034(12) Uiso 1 d . .
HW1A H 0.7376(243) 0.7560(234) 0.2604(139) 0.182(99) Uiso 1 d . .
HW2A H 0.6717(80) 0.4082(82) 0.1609(51) 0.072(20) Uiso 1 d . .
HW2B H 0.5631(132) 0.2843(127) 0.1056(78) 0.157(42) Uiso 1 d . .
HW3A H 0.0344(145) 0.9720(138) 0.5869(91) 0.166(50) Uiso 1 d . .
HW3B H 0.1720(219) 0.9233(204) 0.5235(132) 0.296(85) Uiso 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'
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'
K K 0.2009 0.2494 '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
O6 V1 O7 101.5(2) . . ?
O6 V1 O8 100.2(2) . . ?
O8 V1 O7 44.8(2) . . ?
O6 V1 O3 98.3(2) . . ?
O7 V1 O3 148.69(14) . . ?
O8 V1 O3 151.9(2) . . ?
O6 V1 O3 97.9(2) . 2_676 ?
O7 V1 O3 81.82(14) . 2_676 ?
O8 V1 O3 126.0(2) . 2_676 ?
O3 V1 O3 71.6(2) . 2_676 ?
O6 V1 O1 92.9(2) . . ?
O7 V1 O1 124.31(14) . . ?
O8 V1 O1 79.9(2) . . ?
O3 V1 O1 78.19(13) . . ?
O3 V1 O1 149.04(13) 2_676 . ?
O6 V1 O5 173.1(2) . . ?
O7 V1 O5 84.53(14) . . ?
O8 V1 O5 81.70(13) . . ?
O3 V1 O5 77.61(12) . . ?
O3 V1 O5 86.14(12) 2_676 . ?
O1 V1 O5 80.91(13) . . ?
C1 O1 V1 117.7(3) . . ?
C2 O3 V1 114.3(2) . . ?
C2 O3 V1 127.9(3) . 2_676 ?
V1 O3 V1 108.4(2) . 2_676 ?
C4 O5 V1 131.2(3) . . ?
O8 O7 V1 68.6(2) . . ?
O7 O8 V1 66.5(2) . . ?
O2 C1 O1 123.9(4) . . ?
O2 C1 C2 122.2(4) . . ?
O1 C1 C2 113.9(4) . . ?
O3 C2 C3 111.4(4) . . ?
O3 C2 C1 107.5(4) . . ?
C3 C2 C1 109.5(4) . . ?
C4 C3 C2 116.0(4) . . ?
O4 C4 O5 123.5(4) . . ?
O4 C4 C3 116.2(4) . . ?
O5 C4 C3 120.3(4) . . ?
O16 V2 O17 101.7(2) . . ?
O16 V2 O18 102.1(2) . . ?
O17 V2 O18 44.9(2) . . ?
O16 V2 O13 97.9(2) . . ?
O17 V2 O13 151.0(2) . . ?
O18 V2 O13 148.52(14) . . ?
O16 V2 O13 98.0(2) . 2 ?
O17 V2 O13 125.2(2) . 2 ?
O18 V2 O13 81.26(14) . 2 ?
O13 V2 O13 72.03(14) . 2 ?
O16 V2 O11 92.3(2) . . ?
O17 V2 O11 80.3(2) . . ?
O18 V2 O11 124.9(2) . . ?
O13 V2 O11 77.78(13) . . ?
O13 V2 O11 149.13(13) 2 . ?
O16 V2 O15 173.7(2) . . ?
O17 V2 O15 80.78(14) . . ?
O18 V2 O15 83.8(2) . . ?
O13 V2 O15 77.73(12) . . ?
O13 V2 O15 85.02(13) 2 . ?
O11 V2 O15 82.39(14) . . ?
C11 O11 V2 117.6(3) . . ?
C12 O13 V2 113.1(2) . . ?
C12 O13 V2 127.9(3) . 2 ?
V2 O13 V2 107.96(14) . 2 ?
C14 O15 V2 132.4(3) . . ?
O18 O17 V2 67.6(2) . . ?
O17 O18 V2 67.5(2) . . ?
O12 C11 O11 123.4(4) . . ?
O12 C11 C12 122.3(4) . . ?
O11 C11 C12 114.3(4) . . ?
O13 C12 C13 111.8(4) . . ?
O13 C12 C11 108.1(4) . . ?
C13 C12 C11 109.7(4) . . ?
C12 C13 C14 114.5(4) . . ?
O14 C14 O15 124.0(5) . . ?
O14 C14 C13 114.8(5) . . ?
O15 C14 C13 121.2(4) . . ?
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 O6 1.599(3) . ?
V1 O7 1.859(3) . ?
V1 O8 1.887(3) . ?
V1 O3 1.987(3) . ?
V1 O3 2.026(3) 2_676 ?
V1 O1 2.034(3) . ?
V1 O5 2.294(3) . ?
O1 C1 1.277(6) . ?
O3 C2 1.416(6) . ?
O3 V1 2.026(3) 2_676 ?
O5 C4 1.263(5) . ?
O7 O8 1.428(5) . ?
C1 O2 1.236(6) . ?
C1 C2 1.533(6) . ?
C2 C3 1.522(7) . ?
C3 C4 1.516(7) . ?
C4 O4 1.252(5) . ?
V2 O16 1.599(3) . ?
V2 O17 1.876(3) . ?
V2 O18 1.877(4) . ?
V2 O13 2.007(3) . ?
V2 O13 2.035(3) 2 ?
V2 O11 2.042(4) . ?
V2 O15 2.257(3) . ?
O11 C11 1.273(6) . ?
O13 C12 1.423(6) . ?
O13 V2 2.035(3) 2 ?
O15 C14 1.259(6) . ?
O17 O18 1.432(5) . ?
C11 O12 1.229(6) . ?
C11 C12 1.528(6) . ?
C12 C13 1.515(7) . ?
C13 C14 1.517(7) . ?
C14 O14 1.245(6) . ?
