#------------------------------------------------------------------------------
#$Date: 2016-12-05 08:25:31 +0200 (Mon, 05 Dec 2016) $
#$Revision: 188880 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/72/7227230.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_7227230
loop_
_publ_author_name
'Postal, Kahoana'
'Maluf, Daniela Florêncio'
'Valdameri, Glaucio'
'Rüdiger, André Luis'
'Hughes, David L.'
'Sa, Eduardo Lemos de'
'Ribeiro, Ronny R.'
'Souza, Emanuel Maltempi de'
'Fernandes Soares, Jaisa'
'Nunes, Giovana G.'
_publ_section_title
;
 Chemoprotective activity of mixed valence polyoxovanadates against
 diethylsulfate in E. coli cultures: insights from chemichal speciation
 studies
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA15826A
_journal_year                    2016
_chemical_formula_moiety         '0.5K, 3.5(N H4), H6 O42 P V14, 12(H2 O)'
_chemical_formula_structural     '0.5K, 3.5(NH4), {H6O38V14(PO4)}, 12(H2O)'
_chemical_formula_sum            'H44 K0.5 N3.5 O54 P V14'
_chemical_formula_weight         1721.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-01 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.332(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7844(5)
_cell_length_b                   24.2257(11)
_cell_length_c                   16.3820(7)
_cell_measurement_reflns_used    34692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      3.08
_cell_volume                     4585.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP (Johnson, 1976 and Farrugia, 2012)'
_computing_publication_material
'SHELXL-2014 (Sheldrick, 2015) and WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61802
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.474
_diffrn_reflns_theta_min         3.527
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.930
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_description       plate
_exptl_crystal_F_000             3388
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0387P)²+9.6061P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3953
_reflns_number_total             4720
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra15826a2.cif
_cod_data_source_block           kp198-3
_cod_original_formula_sum        'H44 K0.50 N3.50 O54 P V14'
_cod_database_code               7227230
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.19773(3) 0.67946(2) 0.19350(3) 0.00878(10) Uani 1 1 d . . . . .
V2 V 0.33969(4) 0.58450(2) 0.11696(3) 0.00903(10) Uani 1 1 d . . . . .
V3 V 0.46923(4) 0.68607(2) 0.46040(3) 0.01051(10) Uani 1 1 d . . . . .
V4 V 0.36099(3) 0.78028(2) 0.11172(2) 0.00829(10) Uani 1 1 d . . . . .
V5 V 0.33236(3) 0.78250(2) 0.32999(3) 0.00865(10) Uani 1 1 d . . . . .
V6 V 0.32472(3) 0.58596(2) 0.32247(3) 0.01001(10) Uani 1 1 d . . . . .
V7 V 0.5000 0.84457(2) 0.2500 0.00924(13) Uani 1 2 d S T P . .
V8 V 0.5000 0.52648(2) 0.2500 0.00919(13) Uani 1 2 d S T P A .
O1 O 0.06128(15) 0.69046(7) 0.16585(11) 0.0144(4) Uani 1 1 d . . . . .
O2 O 0.29903(15) 0.53685(7) 0.04938(11) 0.0143(4) Uani 1 1 d . . . . .
O3 O 0.46175(16) 0.67681(7) 0.55588(11) 0.0144(4) Uani 1 1 d . . . . .
O4 O 0.28734(14) 0.82857(7) 0.05792(11) 0.0112(4) Uani 1 1 d . . . . .
O5 O 0.24773(15) 0.82978(7) 0.35168(11) 0.0123(4) Uani 1 1 d . . . . .
O6 O 0.27414(15) 0.53708(7) 0.37058(11) 0.0150(4) Uani 1 1 d . . . . .
O7 O 0.5000 0.91126(10) 0.2500 0.0134(5) Uani 1 2 d S T P . .
O8 O 0.5000 0.46013(10) 0.2500 0.0148(5) Uani 1 2 d S T P . .
O11 O 0.21262(14) 0.62056(7) 0.11449(10) 0.0107(4) Uani 1 1 d . . . . .
O12 O 0.58575(14) 0.74643(7) 0.48003(10) 0.0104(4) Uani 1 1 d D . . . .
O13 O 0.25709(14) 0.73210(7) 0.12263(10) 0.0095(3) Uani 1 1 d . . . . .
O14 O 0.40277(15) 0.63793(7) 0.04894(11) 0.0107(4) Uani 1 1 d D . . . .
O15 O 0.19713(14) 0.62081(7) 0.27406(10) 0.0108(4) Uani 1 1 d . . . . .
O16 O 0.33917(14) 0.54409(7) 0.22022(10) 0.0102(3) Uani 1 1 d . . . . .
O17 O 0.36065(14) 0.74661(7) 0.43638(10) 0.0100(3) Uani 1 1 d D . . . .
O18 O 0.51329(14) 0.82446(7) 0.14086(10) 0.0098(4) Uani 1 1 d . . . . .
O19 O 0.35766(14) 0.81133(7) 0.22194(10) 0.0090(3) Uani 1 1 d . . . . .
O20 O 0.50780(14) 0.55944(7) 0.15141(10) 0.0104(4) Uani 1 1 d . . . . .
O21 O 0.24081(14) 0.73237(7) 0.28030(10) 0.0096(3) Uani 1 1 d . . . . .
O22 O 0.37231(14) 0.63752(7) 0.40631(10) 0.0105(4) Uani 1 1 d . . . . .
P1 P 0.5000 0.68463(3) 0.2500 0.00616(17) Uani 1 2 d S T P . .
O23 O 0.39114(14) 0.64837(7) 0.23033(10) 0.0086(3) Uani 1 1 d . . . . .
O24 O 0.50599(14) 0.72141(7) 0.17360(10) 0.0086(3) Uani 1 1 d . . . . .
O31 O 0.14950(16) 0.68111(8) 0.44360(12) 0.0168(4) Uani 1 1 d D . . . .
O32 O 0.0000 0.80339(16) 0.2500 0.0362(8) Uani 1 2 d DS T P . .
O33 O 0.5578(7) 1.0135(2) 0.4168(5) 0.051(2) Uani 0.78(2) 1 d D . P . .
O33A O 0.505(3) 1.0079(7) 0.3912(13) 0.049(6) Uiso 0.22(2) 1 d . . P . .
O34 O 0.5106(2) 0.44965(10) 0.05933(16) 0.0369(6) Uani 1 1 d D . . . .
O35 O 0.21133(19) 0.44880(8) 0.19407(14) 0.0239(5) Uani 1 1 d D . . . .
K41 K 0.2750(12) 0.5827(6) 0.5398(9) 0.055(4) Uani 0.248(6) 1 d . . P A 1
N41 N 0.2527(9) 0.5822(6) 0.5328(9) 0.0164(18) Uani 0.752(6) 1 d D . P A 2
N42 N 0.8548(2) 0.87952(11) 0.31659(16) 0.0210(5) Uani 1 1 d D . . . .
O43 O 0.5000 0.94354(13) 0.7500 0.0307(8) Uani 1 2 d DS T P . .
O44 O 0.5269(2) 0.90830(10) 0.48089(16) 0.0403(6) Uani 1 1 d D . . . .
H411 H 0.3302(18) 0.579(3) 0.540(4) 0.070 Uiso 0.752(6) 1 d D U P A 2
H412 H 0.240(5) 0.576(2) 0.5841(18) 0.066(19) Uiso 0.752(6) 1 d D . P A 2
H413 H 0.220(4) 0.5556(17) 0.500(3) 0.07(2) Uiso 0.752(6) 1 d D . P A 2
H414 H 0.229(5) 0.6151(13) 0.515(3) 0.12(3) Uiso 0.752(6) 1 d D . P A 2
H12 H 0.619(3) 0.7531(15) 0.5278(13) 0.036(10) Uiso 1 1 d D . . . .
H14 H 0.344(2) 0.6522(16) 0.020(2) 0.046(12) Uiso 1 1 d D . . . .
H17 H 0.357(3) 0.7680(13) 0.4756(18) 0.039(11) Uiso 1 1 d D . . . .
H311 H 0.090(2) 0.6800(14) 0.4044(18) 0.035(10) Uiso 1 1 d D . . . .
H312 H 0.201(2) 0.6928(15) 0.420(2) 0.043(12) Uiso 1 1 d D . . . .
H321 H -0.038(6) 0.782(2) 0.214(3) 0.14(3) Uiso 1 1 d D . . . .
H331 H 0.594(5) 0.9912(19) 0.392(3) 0.06(2) Uiso 0.78(2) 1 d D . P . .
H341 H 0.518(4) 0.4833(9) 0.074(3) 0.076(16) Uiso 1 1 d D . . . .
H342 H 0.570(3) 0.438(2) 0.046(4) 0.11(2) Uiso 1 1 d D . . . .
H351 H 0.241(2) 0.4804(9) 0.204(2) 0.025(9) Uiso 1 1 d D . . . .
H352 H 0.1418(18) 0.4494(15) 0.199(2) 0.046(12) Uiso 1 1 d D . . . .
H421 H 0.886(3) 0.9013(13) 0.3563(18) 0.057(13) Uiso 1 1 d D . . . .
H422 H 0.808(3) 0.8582(14) 0.339(2) 0.064(14) Uiso 1 1 d D . . . .
H423 H 0.810(3) 0.8994(13) 0.2798(19) 0.060(13) Uiso 1 1 d D . . . .
H424 H 0.902(3) 0.8591(18) 0.295(3) 0.14(3) Uiso 1 1 d D . . . .
H431 H 0.449(3) 0.9198(13) 0.744(3) 0.051(13) Uiso 1 1 d D . . . .
H441 H 0.501(4) 0.8826(14) 0.445(2) 0.072(16) Uiso 1 1 d D . . . .
H442 H 0.578(3) 0.8936(18) 0.520(2) 0.084(18) Uiso 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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'
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
O1 V1 O21 101.77(8) . .
O1 V1 O15 100.15(8) . .
O21 V1 O15 91.21(7) . .
O1 V1 O13 100.41(8) . .
O21 V1 O13 85.99(7) . .
O15 V1 O13 159.39(7) . .
O1 V1 O11 98.59(8) . .
O21 V1 O11 159.62(7) . .
O15 V1 O11 85.92(7) . .
O13 V1 O11 89.64(7) . .
O1 V1 O23 170.92(8) . .
O21 V1 O23 85.51(7) . .
O15 V1 O23 74.05(6) . .
O13 V1 O23 85.37(6) . .
O11 V1 O23 74.29(6) . .
O2 V2 O11 101.97(9) . .
O2 V2 O14 100.31(8) . .
O11 V2 O14 94.42(8) . .
O2 V2 O16 100.67(8) . .
O11 V2 O16 97.09(8) . .
O14 V2 O16 153.36(7) . .
O2 V2 O20 96.81(8) . .
O11 V2 O20 161.11(8) . .
O14 V2 O20 84.10(7) . .
O16 V2 O20 77.29(7) . .
O2 V2 O23 172.70(8) . .
O11 V2 O23 77.19(7) . .
O14 V2 O23 86.99(7) . .
O16 V2 O23 72.35(6) . .
O20 V2 O23 83.92(6) . .
O2 V2 V8 103.19(7) . .
O11 V2 V8 133.30(6) . .
O14 V2 V8 118.62(5) . .
O16 V2 V8 39.79(5) . .
O20 V2 V8 37.59(5) . .
O23 V2 V8 72.99(4) . .
O3 V3 O22 104.15(9) . .
O3 V3 O17 98.27(8) . .
O22 V3 O17 93.82(8) . .
O3 V3 O14 100.73(8) . 2_655
O22 V3 O14 89.78(8) . 2_655
O17 V3 O14 159.16(7) . 2_655
O3 V3 O12 96.54(8) . .
O22 V3 O12 159.30(8) . .
O17 V3 O12 83.32(7) . .
O14 V3 O12 86.09(7) 2_655 .
O3 V3 O24 166.79(8) . 2_655
O22 V3 O24 87.80(7) . 2_655
O17 V3 O24 74.99(6) . 2_655
O14 V3 O24 84.66(7) 2_655 2_655
O12 V3 O24 71.63(6) . 2_655
O3 V3 K41 54.5(2) . .
O22 V3 K41 49.7(2) . .
O17 V3 K41 98.7(2) . .
O14 V3 K41 99.3(2) 2_655 .
O12 V3 K41 151.0(2) . .
O24 V3 K41 137.0(2) 2_655 .
O4 V4 O13 103.34(8) . .
O4 V4 O12 96.05(8) . 2_655
O13 V4 O12 98.03(8) . 2_655
O4 V4 O19 96.83(8) . .
O13 V4 O19 91.21(7) . .
O12 V4 O19 161.97(7) 2_655 .
O4 V4 O18 95.77(8) . .
O13 V4 O18 158.31(8) . .
O12 V4 O18 89.96(7) 2_655 .
O19 V4 O18 76.25(7) . .
O4 V4 O24 164.50(8) . .
O13 V4 O24 90.90(7) . .
O12 V4 O24 75.64(7) 2_655 .
O19 V4 O24 88.83(7) . .
O18 V4 O24 71.51(6) . .
O4 V4 V7 101.19(6) . .
O13 V4 V7 124.97(6) . .
O12 V4 V7 127.26(5) 2_655 .
O19 V4 V7 37.22(5) . .
O18 V4 V7 39.25(5) . .
O24 V4 V7 74.81(4) . .
O5 V5 O21 104.46(9) . .
O5 V5 O17 97.30(8) . .
O21 V5 O17 95.22(8) . .
O5 V5 O19 98.96(8) . .
O21 V5 O19 90.95(7) . .
O17 V5 O19 160.58(7) . .
O5 V5 O18 98.96(8) . 2_655
O21 V5 O18 154.58(8) . 2_655
O17 V5 O18 91.44(7) . 2_655
O19 V5 O18 75.61(7) . 2_655
O5 V5 O24 165.47(8) . 2_655
O21 V5 O24 88.87(7) . 2_655
O17 V5 O24 75.40(6) . 2_655
O19 V5 O24 86.36(6) . 2_655
O18 V5 O24 69.12(6) 2_655 2_655
O5 V5 V7 103.39(7) . .
O21 V5 V7 123.79(6) . .
O17 V5 V7 128.02(5) . .
O19 V5 V7 36.88(5) . .
O18 V5 V7 38.82(5) 2_655 .
O24 V5 V7 72.87(4) 2_655 .
O6 V6 O15 101.99(9) . .
O6 V6 O22 102.75(9) . .
O15 V6 O22 96.71(8) . .
O6 V6 O16 97.98(8) . .
O15 V6 O16 94.10(7) . .
O22 V6 O16 154.02(7) . .
O6 V6 O20 95.87(8) . 2_655
O15 V6 O20 161.08(8) . 2_655
O22 V6 O20 85.28(7) . 2_655
O16 V6 O20 77.12(7) . 2_655
O6 V6 O23 169.97(8) . .
O15 V6 O23 76.63(7) . .
O22 V6 O23 87.28(7) . .
O16 V6 O23 72.34(6) . .
O20 V6 O23 84.70(6) 2_655 .
O6 V6 V8 101.22(7) . .
O15 V6 V8 130.72(6) . .
O22 V6 V8 119.44(5) . .
O16 V6 V8 39.82(5) . .
O20 V6 V8 37.43(5) 2_655 .
O23 V6 V8 73.21(4) . .
O6 V6 K41 50.9(2) . .
O15 V6 K41 99.2(2) . .
O22 V6 K41 52.3(2) . .
O16 V6 K41 148.0(2) . .
O20 V6 K41 96.9(2) 2_655 .
O23 V6 K41 139.0(2) . .
V8 V6 K41 128.9(2) . .
O7 V7 O19 116.02(5) . .
O7 V7 O19 116.02(6) . 2_655
O19 V7 O19 127.97(11) . 2_655
O7 V7 O18 104.95(5) . .
O19 V7 O18 83.77(7) . .
O19 V7 O18 83.24(7) 2_655 .
O7 V7 O18 104.95(5) . 2_655
O19 V7 O18 83.24(7) . 2_655
O19 V7 O18 83.77(7) 2_655 2_655
O18 V7 O18 150.10(11) . 2_655
O7 V7 V4 121.704(13) . .
O19 V7 V4 40.31(5) . .
O19 V7 V4 107.55(6) 2_655 .
O18 V7 V4 43.71(5) . .
O18 V7 V4 116.85(5) 2_655 .
O7 V7 V4 121.705(13) . 2_655
O19 V7 V4 107.55(6) . 2_655
O19 V7 V4 40.31(5) 2_655 2_655
O18 V7 V4 116.85(5) . 2_655
O18 V7 V4 43.71(5) 2_655 2_655
V4 V7 V4 116.59(3) . 2_655
O7 V7 V5 120.271(13) . .
O19 V7 V5 40.31(5) . .
O19 V7 V5 108.68(6) 2_655 .
O18 V7 V5 118.10(5) . .
O18 V7 V5 43.03(5) 2_655 .
V4 V7 V5 75.908(15) . .
V4 V7 V5 73.361(14) 2_655 .
O7 V7 V5 120.271(13) . 2_655
O19 V7 V5 108.68(6) . 2_655
O19 V7 V5 40.31(5) 2_655 2_655
O18 V7 V5 43.03(5) . 2_655
O18 V7 V5 118.10(5) 2_655 2_655
V4 V7 V5 73.361(15) . 2_655
V4 V7 V5 75.907(15) 2_655 2_655
V5 V7 V5 119.46(3) . 2_655
O8 V8 O20 116.02(6) . 2_655
O8 V8 O20 116.02(6) . .
O20 V8 O20 127.96(11) 2_655 .
O8 V8 O16 102.90(5) . 2_655
O20 V8 O16 84.03(7) 2_655 2_655
O20 V8 O16 84.73(7) . 2_655
O8 V8 O16 102.91(5) . .
O20 V8 O16 84.73(7) 2_655 .
O20 V8 O16 84.03(7) . .
O16 V8 O16 154.19(11) 2_655 .
O8 V8 V2 118.502(13) . 2_655
O20 V8 V2 43.20(5) 2_655 2_655
O20 V8 V2 108.08(6) . 2_655
O16 V8 V2 40.93(5) 2_655 2_655
O16 V8 V2 122.84(5) . 2_655
O8 V8 V2 118.502(13) . .
O20 V8 V2 108.08(6) 2_655 .
O20 V8 V2 43.20(5) . .
O16 V8 V2 122.84(5) 2_655 .
O16 V8 V2 40.93(5) . .
V2 V8 V2 123.00(3) 2_655 .
O8 V8 V6 119.213(13) . 2_655
O20 V8 V6 107.70(6) 2_655 2_655
O20 V8 V6 42.92(5) . 2_655
O16 V8 V6 41.95(5) 2_655 2_655
O16 V8 V6 121.72(5) . 2_655
V2 V8 V6 70.546(14) 2_655 2_655
V2 V8 V6 82.371(15) . 2_655
O8 V8 V6 119.213(13) . .
O20 V8 V6 42.92(5) 2_655 .
O20 V8 V6 107.70(6) . .
O16 V8 V6 121.72(5) 2_655 .
O16 V8 V6 41.95(5) . .
V2 V8 V6 82.372(15) 2_655 .
V2 V8 V6 70.546(14) . .
V6 V8 V6 121.57(3) 2_655 .
V2 O2 K41 139.9(3) . 6_565
V3 O3 K41 101.1(3) . .
V5 O5 K41 145.0(3) . 7_566
V6 O6 K41 104.5(3) . .
V2 O11 V1 122.89(9) . .
V4 O12 V3 120.55(9) 2_655 .
V4 O12 H12 120(3) 2_655 .
V3 O12 H12 119(3) . .
V4 O13 V1 148.30(10) . .
V3 O14 V2 146.73(10) 2_655 .
V3 O14 H14 106(3) 2_655 .
V2 O14 H14 103(3) . .
V6 O15 V1 122.53(9) . .
V8 O16 V2 99.28(7) . .
V8 O16 V6 98.24(7) . .
V2 O16 V6 119.17(9) . .
V5 O17 V3 121.22(9) . .
V5 O17 H17 113(3) . .
V3 O17 H17 117(3) . .
V7 O18 V5 98.15(7) . 2_655
V7 O18 V4 97.04(7) . .
V5 O18 V4 119.14(8) 2_655 .
V7 O19 V4 102.47(8) . .
V7 O19 V5 102.80(8) . .
V4 O19 V5 136.14(9) . .
V8 O20 V6 99.65(7) . 2_655
V8 O20 V2 99.22(8) . .
V6 O20 V2 144.13(9) 2_655 .
V5 O21 V1 151.38(10) . .
V3 O22 V6 153.59(10) . .
V3 O22 K41 103.6(3) . .
V6 O22 K41 98.0(3) . .
O23 P1 O23 110.23(13) . 2_655
O23 P1 O24 109.16(9) . .
O23 P1 O24 109.25(8) 2_655 .
O23 P1 O24 109.25(8) . 2_655
O23 P1 O24 109.16(9) 2_655 2_655
O24 P1 O24 109.77(13) . 2_655
P1 O23 V1 126.53(9) . .
P1 O23 V6 126.64(9) . .
V1 O23 V6 86.75(5) . .
P1 O23 V2 127.18(9) . .
V1 O23 V2 85.62(5) . .
V6 O23 V2 90.96(6) . .
P1 O24 V4 124.36(9) . .
P1 O24 V5 122.14(9) . 2_655
V4 O24 V5 97.47(6) . 2_655
P1 O24 V3 124.09(9) . 2_655
V4 O24 V3 91.78(6) . 2_655
V5 O24 V3 87.62(5) 2_655 2_655
K41 O31 H311 127(2) . .
K41 O31 H312 100(3) . .
H311 O31 H312 103(3) . .
O33A O33 K41 161.1(16) . 3
O33A O33 H331 93(5) . .
K41 O33 H331 102(4) 3 .
O33 O33A H331 48(3) . .
K41 O34 H341 110(3) 6_565 .
K41 O34 H342 137(4) 6_565 .
H341 O34 H342 112(4) . .
K41 O35 H351 104(2) 6_565 .
K41 O35 H352 121(3) 6_565 .
H351 O35 H352 110(3) . .
O5 K41 O34 110.4(5) 7_566 6_566
O5 K41 O35 64.6(3) 7_566 6_566
O34 K41 O35 104.2(4) 6_566 6_566
O5 K41 O2 137.4(5) 7_566 6_566
O34 K41 O2 68.7(3) 6_566 6_566
O35 K41 O2 74.2(3) 6_566 6_566
O5 K41 O22 103.1(5) 7_566 .
O34 K41 O22 72.4(3) 6_566 .
O35 K41 O22 165.7(6) 6_566 .
O2 K41 O22 115.9(5) 6_566 .
O5 K41 O6 152.0(5) 7_566 .
O34 K41 O6 80.1(4) 6_566 .
O35 K41 O6 139.9(5) 6_566 .
O2 K41 O6 70.4(3) 6_566 .
O22 K41 O6 54.1(3) . .
O5 K41 O31 69.1(3) 7_566 .
O34 K41 O31 129.3(5) 6_566 .
O35 K41 O31 118.3(5) 6_566 .
O2 K41 O31 146.3(5) 6_566 .
O22 K41 O31 59.5(3) . .
O6 K41 O31 84.1(4) . .
O5 K41 O3 63.4(3) 7_566 .
O34 K41 O3 62.5(3) 6_566 .
O35 K41 O3 114.7(5) 6_566 .
O2 K41 O3 131.2(5) 6_566 .
O22 K41 O3 51.2(2) . .
O6 K41 O3 102.8(4) . .
O31 K41 O3 74.9(3) . .
O5 K41 O33 126.6(5) 7_566 3_445
O34 K41 O33 122.7(5) 6_566 3_445
O35 K41 O33 95.4(4) 6_566 3_445
O2 K41 O33 66.0(3) 6_566 3_445
O22 K41 O33 98.0(4) . 3_445
O6 K41 O33 53.0(2) . 3_445
O31 K41 O33 81.2(3) . 3_445
O3 K41 O33 147.8(5) . 3_445
O5 K41 V6 129.9(5) 7_566 .
O34 K41 V6 77.3(3) 6_566 .
O35 K41 V6 164.5(5) 6_566 .
O2 K41 V6 92.4(4) 6_566 .
O22 K41 V6 29.67(14) . .
O6 K41 V6 24.63(12) . .
O31 K41 V6 69.1(3) . .
O3 K41 V6 80.0(3) . .
O33 K41 V6 71.5(3) 3_445 .
O5 K41 V3 81.8(3) 7_566 .
O34 K41 V3 65.1(3) 6_566 .
O35 K41 V3 139.1(5) 6_566 .
O2 K41 V3 128.1(4) 6_566 .
O22 K41 V3 26.72(14) . .
O6 K41 V3 79.5(3) . .
O31 K41 V3 64.8(3) . .
O3 K41 V3 24.47(12) . .
O33 K41 V3 124.2(4) 3_445 .
V6 K41 V3 55.8(2) . .
H411 N41 H412 103(3) . .
H411 N41 H413 109(3) . .
H412 N41 H413 108(3) . .
H411 N41 H414 111(3) . .
H412 N41 H414 112(3) . .
H413 N41 H414 113(3) . .
H421 N42 H422 105(3) . .
H421 N42 H423 107(3) . .
H422 N42 H423 105(3) . .
H421 N42 H424 116(3) . .
H422 N42 H424 109(3) . .
H423 N42 H424 113(3) . .
H441 O44 H442 108(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.6048(17) .
V1 O21 1.9077(17) .
V1 O15 1.9402(17) .
V1 O13 1.9449(17) .
V1 O11 1.9573(17) .
V1 O23 2.3635(16) .
V2 O2 1.6061(18) .
V2 O11 1.7272(17) .
V2 O14 1.9482(18) .
V2 O16 1.9554(17) .
V2 O20 2.0427(17) .
V2 O23 2.4016(17) .
V2 V8 2.9456(5) .
V3 O3 1.5997(18) .
V3 O22 1.7536(17) .
V3 O17 1.9352(18) .
V3 O14 1.9364(18) 2_655
V3 O12 1.9883(18) .
V3 O24 2.4267(16) 2_655
V3 K41 3.791(15) .
V4 O4 1.6119(17) .
V4 O13 1.7261(17) .
V4 O12 1.9227(18) 2_655
V4 O19 1.9634(17) .
V4 O18 2.0634(17) .
V4 O24 2.3023(17) .
V4 V7 2.9635(5) .
V5 O5 1.6038(17) .
V5 O21 1.7194(17) .
V5 O17 1.9174(17) .
V5 O19 1.9791(17) .
V5 O18 2.0563(17) 2_655
V5 O24 2.4221(17) 2_655
V5 V7 2.9829(5) .
V6 O6 1.6012(18) .
V6 O15 1.7702(17) .
V6 O22 1.8597(17) .
V6 O16 1.9940(17) .
V6 O20 2.0394(17) 2_655
V6 O23 2.3752(17) .
V6 V8 2.9523(5) .
V6 K41 3.720(15) .
V7 O7 1.616(2) .
V7 O19 1.8359(16) .
V7 O19 1.8359(16) 2_655
V7 O18 1.8891(17) .
V7 O18 1.8891(17) 2_655
V7 V4 2.9635(5) 2_655
V7 V5 2.9830(5) 2_655
V8 O8 1.608(2) .
V8 O20 1.8201(17) 2_655
V8 O20 1.8201(17) .
V8 O16 1.9101(16) 2_655
V8 O16 1.9101(16) .
V8 V2 2.9455(5) 2_655
V8 V6 2.9523(5) 2_655
O2 K41 2.911(14) 6_565
O3 K41 3.144(15) .
O5 K41 2.814(15) 7_566
O6 K41 2.982(15) .
O12 V4 1.9227(18) 2_655
O12 H12 0.818(18) .
O14 V3 1.9364(18) 2_655
O14 H14 0.832(19) .
O17 H17 0.833(18) .
O18 V5 2.0563(17) 2_655
O20 V6 2.0394(17) 2_655
O22 K41 2.974(15) .
P1 O23 1.5357(17) .
P1 O23 1.5358(17) 2_655
P1 O24 1.5493(17) .
P1 O24 1.5493(17) 2_655
O24 V5 2.4221(16) 2_655
O24 V3 2.4267(16) 2_655
O31 K41 3.072(13) .
O31 H311 0.855(18) .
O31 H312 0.830(18) .
O32 H321 0.84(2) .
O33 O33A 0.69(3) .
O33 K41 3.374(18) 3
O33 H331 0.83(2) .
O33A H331 1.12(5) .
O34 K41 2.842(14) 6_565
O34 H341 0.850(19) .
O34 H342 0.835(19) .
O35 K41 2.878(15) 6_565
O35 H351 0.842(17) .
O35 H352 0.840(18) .
K41 O5 2.814(15) 7_566
K41 O34 2.842(14) 6_566
K41 O35 2.878(15) 6_566
K41 O2 2.911(14) 6_566
K41 O33 3.374(18) 3_445
N41 H411 0.901(18) .
N41 H412 0.898(18) .
N41 H413 0.882(18) .
N41 H414 0.876(18) .
N42 H421 0.862(17) .
N42 H422 0.886(17) .
N42 H423 0.864(17) .
N42 H424 0.864(17) .
O43 H431 0.822(18) .
O44 H441 0.868(19) .
O44 H442 0.869(19) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N41 H411 O34 0.901(18) 2.20(2) 3.083(11) 167(6) 6_566
N41 H412 O35 0.898(18) 1.99(2) 2.879(15) 173(5) 6_566
N41 H413 O2 0.882(18) 2.50(5) 2.937(15) 111(4) 6_566
N41 H413 O6 0.882(18) 2.37(5) 2.929(15) 121(4) .
N41 H413 O33 0.882(18) 2.34(3) 3.152(16) 152(5) 3_445
N41 H414 O31 0.876(18) 2.09(3) 2.943(13) 164(5) .
O12 H12 O13 0.818(18) 2.05(2) 2.820(2) 156(3) 8_566
O14 H14 O4 0.832(19) 1.86(2) 2.683(2) 168(4) 7_565
O17 H17 O31 0.833(18) 1.821(19) 2.653(3) 176(4) 7_566
O31 H311 O1 0.855(18) 1.937(19) 2.772(3) 165(3) 2
O31 H312 O17 0.830(18) 2.26(2) 2.973(3) 144(3) .
O31 H312 O21 0.830(18) 2.61(3) 3.315(3) 144(3) .
O31 H312 O22 0.830(18) 2.47(3) 3.002(2) 123(3) .
O33 H331 O6 0.83(2) 2.49(6) 2.856(6) 108(5) 3
O33A H331 O6 1.12(5) 2.49(6) 3.33(3) 131(4) 3
O34 H341 O20 0.850(19) 2.25(2) 3.061(3) 159(4) .
O34 H342 O2 0.835(19) 2.47(4) 3.143(3) 138(5) 5_665
O34 H342 O14 0.835(19) 2.46(4) 3.066(3) 131(5) 5_665
O35 H351 O16 0.842(17) 1.918(18) 2.744(3) 167(3) .
O35 H352 O7 0.840(18) 2.21(2) 2.961(2) 149(3) 3_445
O35 H352 O33A 0.840(18) 2.49(5) 3.02(3) 122(3) 4_545
N42 H421 O34 0.862(17) 2.025(18) 2.875(4) 168(4) 4_655
N42 H422 O4 0.886(17) 2.32(2) 3.148(3) 155(3) 2_655
N42 H422 O19 0.886(17) 2.30(3) 2.963(3) 131(3) 2_655
N42 H423 O35 0.864(17) 2.030(17) 2.893(3) 177(4) 3
N42 H424 O32 0.864(17) 2.013(18) 2.873(4) 173(5) 1_655
O43 H431 O15 0.822(18) 1.96(2) 2.761(2) 166(4) 7_566
O44 H441 O18 0.868(19) 1.98(2) 2.821(3) 164(5) 2_655
O44 H442 O11 0.869(19) 2.01(2) 2.862(3) 165(4) 8_566
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O11 V2 O2 K41 -115.2(5) . 6_565
O14 V2 O2 K41 147.9(5) . 6_565
O16 V2 O2 K41 -15.5(5) . 6_565
O20 V2 O2 K41 62.7(5) . 6_565
V8 V2 O2 K41 25.1(5) . 6_565
O22 V3 O3 K41 -1.3(3) . .
O17 V3 O3 K41 94.8(3) . .
O14 V3 O3 K41 -93.8(3) 2_655 .
O12 V3 O3 K41 179.0(3) . .
O24 V3 O3 K41 153.1(4) 2_655 .
O21 V5 O5 K41 153.7(5) . 7_566
O17 V5 O5 K41 56.3(5) . 7_566
O19 V5 O5 K41 -113.0(5) . 7_566
O18 V5 O5 K41 -36.3(5) 2_655 7_566
O24 V5 O5 K41 -2.4(7) 2_655 7_566
V7 V5 O5 K41 -75.7(5) . 7_566
O15 V6 O6 K41 -92.1(3) . .
O22 V6 O6 K41 7.7(3) . .
O16 V6 O6 K41 171.9(3) . .
O20 V6 O6 K41 94.1(3) 2_655 .
O23 V6 O6 K41 -173.1(5) . .
V8 V6 O6 K41 131.6(3) . .
O2 V2 O11 V1 172.17(11) . .
O14 V2 O11 V1 -86.30(11) . .
O16 V2 O11 V1 69.63(11) . .
O20 V2 O11 V1 -1.6(3) . .
O23 V2 O11 V1 -0.40(9) . .
V8 V2 O11 V1 50.82(14) . .
O4 V4 O13 V1 -139.34(19) . .
O12 V4 O13 V1 122.45(19) 2_655 .
O19 V4 O13 V1 -42.02(19) . .
O18 V4 O13 V1 11.8(4) . .
O24 V4 O13 V1 46.83(19) . .
V7 V4 O13 V1 -25.2(2) . .
O6 V6 O15 V1 -171.79(11) . .
O22 V6 O15 V1 83.60(11) . .
O16 V6 O15 V1 -72.73(11) . .
O20 V6 O15 V1 -11.4(3) 2_655 .
O23 V6 O15 V1 -1.98(9) . .
V8 V6 O15 V1 -55.36(13) . .
K41 V6 O15 V1 136.4(2) . .
O7 V7 O18 V5 118.59(5) . 2_655
O19 V7 O18 V5 -126.10(8) . 2_655
O19 V7 O18 V5 3.41(7) 2_655 2_655
O18 V7 O18 V5 -61.41(5) 2_655 2_655
V4 V7 O18 V5 -120.88(10) . 2_655
V4 V7 O18 V5 -19.55(8) 2_655 2_655
V5 V7 O18 V5 -104.19(6) . 2_655
O7 V7 O18 V4 -120.52(5) . .
O19 V7 O18 V4 -5.21(7) . .
O19 V7 O18 V4 124.29(8) 2_655 .
O18 V7 O18 V4 59.48(5) 2_655 .
V4 V7 O18 V4 101.33(6) 2_655 .
V5 V7 O18 V4 16.70(8) . .
V5 V7 O18 V4 120.88(10) 2_655 .
O7 V7 O19 V4 109.19(6) . .
O19 V7 O19 V4 -70.81(6) 2_655 .
O18 V7 O19 V4 5.57(8) . .
O18 V7 O19 V4 -147.45(9) 2_655 .
V4 V7 O19 V4 -110.67(6) 2_655 .
V5 V7 O19 V4 -143.85(12) . .
V5 V7 O19 V4 -30.03(8) 2_655 .
O7 V7 O19 V5 -106.96(6) . .
O19 V7 O19 V5 73.04(6) 2_655 .
O18 V7 O19 V5 149.42(9) . .
O18 V7 O19 V5 -3.60(8) 2_655 .
V4 V7 O19 V5 143.85(12) . .
V4 V7 O19 V5 33.18(8) 2_655 .
V5 V7 O19 V5 113.82(6) 2_655 .
O8 V8 O20 V6 -105.82(6) . 2_655
O20 V8 O20 V6 74.18(6) 2_655 2_655
O16 V8 O20 V6 -4.02(8) 2_655 2_655
O16 V8 O20 V6 152.71(8) . 2_655
V2 V8 O20 V6 30.06(8) 2_655 2_655
V2 V8 O20 V6 149.35(11) . 2_655
V6 V8 O20 V6 117.64(6) . 2_655
O8 V8 O20 V2 104.83(6) . .
O20 V8 O20 V2 -75.17(6) 2_655 .
O16 V8 O20 V2 -153.37(8) 2_655 .
O16 V8 O20 V2 3.36(7) . .
V2 V8 O20 V2 -119.29(5) 2_655 .
V6 V8 O20 V2 -149.35(11) 2_655 .
V6 V8 O20 V2 -31.72(7) . .
O5 V5 O21 V1 137.1(2) . .
O17 V5 O21 V1 -123.9(2) . .
O19 V5 O21 V1 37.6(2) . .
O18 V5 O21 V1 -19.4(3) 2_655 .
O24 V5 O21 V1 -48.7(2) 2_655 .
V7 V5 O21 V1 19.7(2) . .
O3 V3 O22 V6 -142.6(2) . .
O17 V3 O22 V6 117.9(2) . .
O14 V3 O22 V6 -41.5(2) 2_655 .
O12 V3 O22 V6 36.7(4) . .
O24 V3 O22 V6 43.1(2) 2_655 .
K41 V3 O22 V6 -143.9(4) . .
O3 V3 O22 K41 1.4(3) . .
O17 V3 O22 K41 -98.1(3) . .
O14 V3 O22 K41 102.4(3) 2_655 .
O12 V3 O22 K41 -179.3(3) . .
O24 V3 O22 K41 -172.9(3) 2_655 .
O6 V6 O22 V3 137.2(2) . .
O15 V6 O22 V3 -118.9(2) . .
O16 V6 O22 V3 -4.9(4) . .
O20 V6 O22 V3 42.2(2) 2_655 .
O23 V6 O22 V3 -42.7(2) . .
V8 V6 O22 V3 26.3(3) . .
K41 V6 O22 V3 144.7(4) . .
O6 V6 O22 K41 -7.5(3) . .
O15 V6 O22 K41 96.4(3) . .
O16 V6 O22 K41 -149.6(3) . .
O20 V6 O22 K41 -102.5(3) 2_655 .
O23 V6 O22 K41 172.6(3) . .
V8 V6 O22 K41 -118.4(3) . .
O23 P1 O23 V1 -179.07(14) 2_655 .
O24 P1 O23 V1 -59.07(13) . .
O24 P1 O23 V1 60.98(13) 2_655 .
O23 P1 O23 V6 63.35(9) 2_655 .
O24 P1 O23 V6 -176.65(10) . .
O24 P1 O23 V6 -56.60(14) 2_655 .
O23 P1 O23 V2 -62.81(9) 2_655 .
O24 P1 O23 V2 57.19(14) . .
O24 P1 O23 V2 177.24(10) 2_655 .
O23 P1 O24 V4 55.62(13) . .
O23 P1 O24 V4 176.21(10) 2_655 .
O24 P1 O24 V4 -64.11(8) 2_655 .
O23 P1 O24 V5 -176.40(9) . 2_655
O23 P1 O24 V5 -55.80(13) 2_655 2_655
O24 P1 O24 V5 63.87(8) 2_655 2_655
O23 P1 O24 V3 -64.93(12) . 2_655
O23 P1 O24 V3 55.67(12) 2_655 2_655
O24 P1 O24 V3 175.35(13) 2_655 2_655
