#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:32:16 +0100 (mar 22 de mar de 2016) $
#$Revision: 179115 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/77/4307722.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_4307722
loop_
_publ_author_name
'Peter Schwendt'
'Alan S. Tracey'
'Jozef Tatiersky'
'Jana Gáliková'
'Zdirad Žák'
_publ_section_title
;
Vanadium(V) Tartrato Complexes: Speciation in the
H3O+(OH-)/H2VO4-/(2R,3R)-Tartrate System and X-ray Crystal Structures of
Na4[V4O8(rac-tart)2].12H2O and (NEt4)4[V4O8((R,R)-tart)2].6H2O (tart =
C4H2O64-)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3971
_journal_page_last               3983
_journal_paper_doi               10.1021/ic062223h
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C40 H96 N4 O26 V4'
_chemical_formula_weight         1252.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.225(2)
_cell_length_b                   14.029(3)
_cell_length_c                   18.298(4)
_cell_measurement_reflns_used    5726
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      2.3
_cell_volume                     2971.6(12)
_computing_cell_refinement       'KUMA Crysalis 168'
_computing_data_collection       'KUMA Crysalis 168'
_computing_data_reduction        'KUMA Crysalis 168'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '0.06 mm'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'KUMA KM-4 CCD'
_diffrn_measurement_method       'omega scan'
_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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35252
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'each 100 frames'
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.9036
_exptl_absorpt_correction_T_min  0.7700
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.201
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         9531
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0747P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                7008
_reflns_number_total             9531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062223hsi20061122_084420.cif
_cod_data_source_block           lvina
_cod_original_cell_volume        2971.6(10)
_cod_database_code               4307722
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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_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 0.68265(7) 0.51255(7) 0.17292(5) 0.0232(2) Uani 1 1 d . . .
V2 V 0.65758(7) 0.58528(7) 0.35468(5) 0.0268(2) Uani 1 1 d . . .
V3 V 0.88380(7) 0.64239(7) 0.26826(5) 0.0247(2) Uani 1 1 d . . .
V4 V 0.59134(7) 0.72311(7) 0.21472(5) 0.0257(2) Uani 1 1 d . . .
C1 C 0.5127(5) 0.4319(5) 0.3655(3) 0.0333(15) Uani 1 1 d . . .
C2 C 0.6236(5) 0.3909(4) 0.3576(3) 0.0306(14) Uani 1 1 d . . .
H2 H 0.6446 0.3292 0.3859 0.037 Uiso 1 1 calc R . .
C3 C 0.6112(4) 0.3798(4) 0.2717(3) 0.0256(13) Uani 1 1 d . . .
H3 H 0.5455 0.3359 0.2464 0.031 Uiso 1 1 calc R . .
C4 C 0.7252(5) 0.3383(4) 0.2632(3) 0.0273(13) Uani 1 1 d . . .
C5 C 0.9572(4) 0.7958(4) 0.1923(3) 0.0260(13) Uani 1 1 d . . .
C6 C 0.9116(5) 0.8347(4) 0.2566(3) 0.0306(14) Uani 1 1 d . . .
H6 H 0.9531 0.8945 0.2797 0.037 Uiso 1 1 calc R . .
C7 C 0.7786(4) 0.8532(4) 0.2194(3) 0.0261(13) Uani 1 1 d . . .
H7 H 0.7641 0.9004 0.1763 0.031 Uiso 1 1 calc R . .
C8 C 0.7278(5) 0.8894(5) 0.2808(3) 0.0319(15) Uani 1 1 d . . .
O1 O 0.5114(3) 0.5235(3) 0.3664(2) 0.0301(9) Uani 1 1 d . . .
O2 O 0.4311(3) 0.3785(3) 0.3674(3) 0.0431(11) Uani 1 1 d . . .
O3 O 0.7101(3) 0.4629(3) 0.3891(2) 0.0304(9) Uani 1 1 d . . .
O4 O 0.5895(3) 0.4695(3) 0.2363(2) 0.0283(9) Uani 1 1 d . . .
O5 O 0.7607(3) 0.2584(3) 0.2901(2) 0.0356(10) Uani 1 1 d . . .
O6 O 0.7737(3) 0.3947(3) 0.2288(2) 0.0298(9) Uani 1 1 d . . .
O7 O 0.9588(3) 0.7026(3) 0.1927(2) 0.0260(9) Uani 1 1 d . . .
O8 O 0.9828(3) 0.8471(3) 0.1461(2) 0.0391(10) Uani 1 1 d . . .
O9 O 0.9278(3) 0.7634(3) 0.3124(2) 0.0269(9) Uani 1 1 d . . .
O10 O 0.7295(3) 0.7649(3) 0.1911(2) 0.0259(9) Uani 1 1 d . . .
O11 O 0.7619(3) 0.9660(3) 0.3161(2) 0.0360(10) Uani 1 1 d . . .
O12 O 0.6496(3) 0.8345(3) 0.2916(2) 0.0322(10) Uani 1 1 d . . .
O13 O 0.6417(3) 0.4600(3) 0.0898(2) 0.0327(9) Uani 1 1 d . . .
O14 O 0.7005(3) 0.6445(3) 0.4348(2) 0.0341(9) Uani 1 1 d . . .
015 O 0.9882(3) 0.5780(3) 0.3202(2) 0.0320(9) Uani 1 1 d . . .
O16 O 0.4817(3) 0.7826(3) 0.1609(2) 0.0359(10) Uani 1 1 d . . .
O17 O 0.8155(3) 0.5666(3) 0.1800(2) 0.0273(9) Uani 1 1 d . . .
O18 O 0.5917(3) 0.6190(3) 0.15516(19) 0.0267(9) Uani 1 1 d . . .
O19 O 0.5467(3) 0.6655(3) 0.2873(2) 0.0280(9) Uani 1 1 d . . .
O20 O 0.7661(3) 0.6156(3) 0.3072(2) 0.0298(9) Uani 1 1 d . . .
N1 N 0.3420(4) 0.8183(4) 0.3684(3) 0.0332(12) Uani 1 1 d . . .
C11 C 0.2354(6) 0.7557(6) 0.3335(6) 0.081(3) Uani 1 1 d . . .
H11A H 0.1721 0.7958 0.3005 0.098 Uiso 1 1 calc R . .
H11B H 0.2100 0.7300 0.3758 0.098 Uiso 1 1 calc R . .
C21 C 0.2560(7) 0.6709(8) 0.2844(7) 0.114(4) Uani 1 1 d . . .
H21A H 0.2588 0.6948 0.2347 0.171 Uiso 1 1 calc R . .
H21B H 0.1928 0.6248 0.2756 0.171 Uiso 1 1 calc R . .
H21C H 0.3294 0.6397 0.3121 0.171 Uiso 1 1 calc R . .
C31 C 0.4426(7) 0.7613(5) 0.4200(4) 0.056(2) Uani 1 1 d . . .
H31A H 0.5059 0.8067 0.4444 0.067 Uiso 1 1 calc R . .
H31B H 0.4704 0.7190 0.3864 0.067 Uiso 1 1 calc R . .
C41 C 0.4242(10) 0.7001(7) 0.4838(5) 0.108(4) Uani 1 1 d . . .
H41A H 0.3905 0.7391 0.5155 0.162 Uiso 1 1 calc R . .
H41B H 0.4986 0.6744 0.5161 0.162 Uiso 1 1 calc R . .
H41C H 0.3718 0.6475 0.4608 0.162 Uiso 1 1 calc R . .
C51 C 0.3872(7) 0.8601(6) 0.3076(4) 0.069(2) Uani 1 1 d . . .
H51A H 0.4155 0.8078 0.2822 0.082 Uiso 1 1 calc R . .
H51B H 0.4535 0.9022 0.3330 0.082 Uiso 1 1 calc R . .
C61 C 0.2955(9) 0.9178(7) 0.2456(5) 0.093(3) Uani 1 1 d . . .
H61A H 0.2412 0.8739 0.2104 0.140 Uiso 1 1 calc R . .
H61B H 0.3336 0.9568 0.2165 0.140 Uiso 1 1 calc R . .
H61C H 0.2536 0.9592 0.2706 0.140 Uiso 1 1 calc R . .
C71 C 0.3019(5) 0.8952(5) 0.4145(4) 0.0445(17) Uani 1 1 d . . .
H71A H 0.2277 0.9221 0.3813 0.053 Uiso 1 1 calc R . .
H71B H 0.2877 0.8646 0.4593 0.053 Uiso 1 1 calc R . .
C81 C 0.3884(7) 0.9770(6) 0.4436(5) 0.070(2) Uani 1 1 d . . .
H81A H 0.4559 0.9665 0.4269 0.105 Uiso 1 1 calc R . .
H81B H 0.4128 0.9793 0.5001 0.105 Uiso 1 1 calc R . .
H81C H 0.3516 1.0375 0.4225 0.105 Uiso 1 1 calc R . .
N2 N 1.0185(4) 0.4211(4) 0.0934(3) 0.0338(12) Uani 1 1 d . . .
C12 C 1.0264(17) 0.4473(15) 0.1649(7) 0.297(16) Uani 1 1 d . . .
H12A H 0.9753 0.4077 0.1849 0.357 Uiso 1 1 calc R . .
H12B H 1.0043 0.5151 0.1660 0.357 Uiso 1 1 calc R . .
C22 C 1.1800(7) 0.4292(7) 0.2232(5) 0.092(3) Uani 1 1 d . . .
H22A H 1.1967 0.3607 0.2290 0.138 Uiso 1 1 calc R . .
H22B H 1.1947 0.4580 0.2743 0.138 Uiso 1 1 calc R . .
H22C H 1.2298 0.4592 0.1972 0.138 Uiso 1 1 calc R . .
C32 C 1.0889(9) 0.4529(7) 0.0450(7) 0.100(3) Uani 1 1 d . . .
H32A H 1.0588 0.4241 -0.0071 0.120 Uiso 1 1 calc R . .
H32B H 1.1702 0.4326 0.0687 0.120 Uiso 1 1 calc R . .
C42 C 1.0815(8) 0.5718(7) 0.0382(6) 0.105(4) Uani 1 1 d . . .
H42A H 1.0102 0.5902 -0.0022 0.158 Uiso 1 1 calc R . .
H42B H 1.1482 0.5959 0.0253 0.158 Uiso 1 1 calc R . .
H42C H 1.0817 0.5987 0.0877 0.158 Uiso 1 1 calc R . .
C52 C 0.8881(7) 0.4482(8) 0.0488(6) 0.092(3) Uani 1 1 d . . .
H52A H 0.8388 0.4193 0.0766 0.110 Uiso 1 1 calc R . .
H52B H 0.8800 0.5182 0.0510 0.110 Uiso 1 1 calc R . .
C62 C 0.8443(7) 0.4188(7) -0.0311(4) 0.078(3) Uani 1 1 d . . .
H62A H 0.8903 0.4486 -0.0600 0.116 Uiso 1 1 calc R . .
H62B H 0.7635 0.4385 -0.0533 0.116 Uiso 1 1 calc R . .
H62C H 0.8496 0.3493 -0.0343 0.116 Uiso 1 1 calc R . .
C72 C 1.0249(8) 0.3128(7) 0.0943(6) 0.085(3) Uani 1 1 d . . .
H72A H 1.1068 0.2931 0.1154 0.103 Uiso 1 1 calc R . .
H72B H 0.9941 0.2889 0.0406 0.103 Uiso 1 1 calc R . .
C82 C 0.9557(5) 0.2666(5) 0.1434(5) 0.057(2) Uani 1 1 d . . .
H82A H 0.9835 0.2921 0.1960 0.086 Uiso 1 1 calc R . .
H82B H 0.9668 0.1973 0.1450 0.086 Uiso 1 1 calc R . .
H82C H 0.8734 0.2812 0.1201 0.086 Uiso 1 1 calc R . .
N3 N 1.0699(4) 0.3365(4) 0.4604(3) 0.0332(12) Uani 1 1 d . . .
C13 C 1.0634(5) 0.3041(5) 0.3795(3) 0.0387(16) Uani 1 1 d . . .
H13A H 0.9844 0.2800 0.3530 0.046 Uiso 1 1 calc R . .
H13B H 1.0756 0.3603 0.3504 0.046 Uiso 1 1 calc R . .
C23 C 1.1485(5) 0.2279(5) 0.3761(4) 0.0488(17) Uani 1 1 d . . .
H23A H 1.2267 0.2480 0.4064 0.073 Uiso 1 1 calc R . .
H23B H 1.1447 0.2178 0.3223 0.073 Uiso 1 1 calc R . .
H23C H 1.1296 0.1683 0.3973 0.073 Uiso 1 1 calc R . .
C33 C 1.1925(5) 0.3736(5) 0.5045(3) 0.0408(16) Uani 1 1 d . . .
H33A H 1.1935 0.3956 0.5561 0.049 Uiso 1 1 calc R . .
H33B H 1.2473 0.3197 0.5123 0.049 Uiso 1 1 calc R . .
C43 C 1.2359(5) 0.4549(5) 0.4653(4) 0.0505(19) Uani 1 1 d . . .
H43A H 1.2479 0.4312 0.4181 0.076 Uiso 1 1 calc R . .
H43B H 1.3090 0.4792 0.5004 0.076 Uiso 1 1 calc R . .
H43C H 1.1786 0.5063 0.4523 0.076 Uiso 1 1 calc R . .
C53 C 1.0484(5) 0.2534(5) 0.5088(4) 0.0415(16) Uani 1 1 d . . .
H53A H 1.1057 0.2027 0.5110 0.050 Uiso 1 1 calc R . .
H53B H 1.0620 0.2763 0.5622 0.050 Uiso 1 1 calc R . .
C63 C 0.9281(5) 0.2100(5) 0.4792(4) 0.0509(18) Uani 1 1 d . . .
H63A H 0.8702 0.2598 0.4749 0.076 Uiso 1 1 calc R . .
H63B H 0.9204 0.1608 0.5152 0.076 Uiso 1 1 calc R . .
H63C H 0.9163 0.1814 0.4283 0.076 Uiso 1 1 calc R . .
C73 C 0.9801(5) 0.4120(5) 0.4512(3) 0.0386(16) Uani 1 1 d . . .
H73A H 0.9043 0.3850 0.4207 0.046 Uiso 1 1 calc R . .
H73B H 0.9972 0.4648 0.4206 0.046 Uiso 1 1 calc R . .
C83 C 0.9688(6) 0.4539(5) 0.5256(4) 0.0459(17) Uani 1 1 d . . .
H83A H 0.9682 0.4022 0.5615 0.069 Uiso 1 1 calc R . .
H83B H 0.8967 0.4902 0.5137 0.069 Uiso 1 1 calc R . .
H83C H 1.0344 0.4963 0.5494 0.069 Uiso 1 1 calc R . .
N4 N 0.5649(4) 0.7042(3) -0.0506(3) 0.0297(11) Uani 1 1 d . . .
C14 C 0.5432(5) 0.6553(4) -0.1284(3) 0.0348(15) Uani 1 1 d . . .
H14A H 0.6120 0.6643 -0.1450 0.042 Uiso 1 1 calc R . .
H14B H 0.4773 0.6870 -0.1669 0.042 Uiso 1 1 calc R . .
C24 C 0.5170(6) 0.5464(5) -0.1286(4) 0.055(2) Uani 1 1 d . . .
H24A H 0.5838 0.5134 -0.0933 0.083 Uiso 1 1 calc R . .
H24B H 0.5012 0.5210 -0.1809 0.083 Uiso 1 1 calc R . .
H24C H 0.4494 0.5363 -0.1117 0.083 Uiso 1 1 calc R . .
C34 C 0.4685(5) 0.6823(5) -0.0160(4) 0.0388(16) Uani 1 1 d . . .
H34A H 0.4840 0.7184 0.0327 0.047 Uiso 1 1 calc R . .
H34B H 0.4716 0.6136 -0.0031 0.047 Uiso 1 1 calc R . .
C44 C 0.3458(5) 0.7064(5) -0.0687(4) 0.0470(18) Uani 1 1 d . . .
H44A H 0.3423 0.7737 -0.0837 0.071 Uiso 1 1 calc R . .
H44B H 0.2906 0.6945 -0.0410 0.071 Uiso 1 1 calc R . .
H44C H 0.3263 0.6664 -0.1150 0.071 Uiso 1 1 calc R . .
C54 C 0.5695(5) 0.8111(4) -0.0649(3) 0.0336(14) Uani 1 1 d . . .
H54A H 0.6267 0.8225 -0.0919 0.040 Uiso 1 1 calc R . .
H54B H 0.4931 0.8314 -0.1000 0.040 Uiso 1 1 calc R . .
C64 C 0.6004(6) 0.8731(5) 0.0061(3) 0.0453(17) Uani 1 1 d . . .
H64A H 0.5408 0.8670 0.0310 0.068 Uiso 1 1 calc R . .
H64B H 0.6055 0.9397 -0.0086 0.068 Uiso 1 1 calc R . .
H64C H 0.6751 0.8528 0.0421 0.068 Uiso 1 1 calc R . .
C74 C 0.6765(4) 0.6690(4) 0.0088(3) 0.0309(14) Uani 1 1 d . . .
H74A H 0.6737 0.5986 0.0112 0.037 Uiso 1 1 calc R . .
H74B H 0.6802 0.6939 0.0601 0.037 Uiso 1 1 calc R . .
C84 C 0.7873(5) 0.6981(5) -0.0077(3) 0.0367(15) Uani 1 1 d . . .
H84A H 0.7860 0.6720 -0.0576 0.055 Uiso 1 1 calc R . .
H84B H 0.8545 0.6731 0.0330 0.055 Uiso 1 1 calc R . .
H84C H 0.7920 0.7678 -0.0090 0.055 Uiso 1 1 calc R . .
OW1 O 0.4092(4) 0.1831(3) 0.3190(3) 0.0558(13) Uani 1 1 d D . .
HW1A H 0.4783 0.1620 0.3487 0.084 Uiso 1 1 d RD . .
HW1B H 0.3974 0.2307 0.3450 0.084 Uiso 1 1 d RD . .
OW2 O 0.3622(3) 0.5300(4) 0.1391(3) 0.0534(13) Uani 1 1 d D . .
HW2A H 0.3977 0.5961 0.1281 0.080 Uiso 1 1 d RD . .
HW2B H 0.4522 0.4870 0.1698 0.080 Uiso 1 1 d RD . .
OW3 O 0.8858(4) 1.1020(4) 0.2631(3) 0.0680(16) Uani 1 1 d D . .
HW3A H 0.8597 1.1708 0.2626 0.102 Uiso 1 1 d RD . .
HW3B H 0.8594 1.0527 0.2869 0.102 Uiso 1 1 d RD . .
OW4 O 0.7809(4) 0.6577(3) -0.1889(2) 0.0509(12) Uani 1 1 d D . .
HW4A H 0.7182 0.6665 -0.2369 0.076 Uiso 1 1 d RD . .
HW4B H 0.8572 0.6380 -0.1978 0.076 Uiso 1 1 d RD . .
OW5 O 0.6365(4) 0.1230(3) 0.3469(3) 0.0543(13) Uani 1 1 d D . .
HW5A H 0.6937 0.1641 0.3213 0.081 Uiso 1 1 d RD . .
HW5B H 0.6629 0.0553 0.3521 0.081 Uiso 1 1 d RD . .
OW6 O 1.0385(6) 1.0360(4) 0.1928(5) 0.118(3) Uani 1 1 d D . .
HW6A H 1.0281 0.9694 0.1706 0.178 Uiso 1 1 d RD . .
HW6B H 0.9762 1.0668 0.2207 0.178 Uiso 1 1 d RD . .
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
O13 V1 O17 105.39(18) . . ?
O13 V1 O18 102.61(18) . . ?
O17 V1 O18 98.93(16) . . ?
O13 V1 O4 110.64(18) . . ?
O17 V1 O4 141.79(16) . . ?
O18 V1 O4 85.49(16) . . ?
O13 V1 O6 93.21(18) . . ?
O17 V1 O6 88.32(16) . . ?
O18 V1 O6 160.06(16) . . ?
O4 V1 O6 77.53(15) . . ?
O13 V1 V3 138.16(14) . . ?
O17 V1 V3 32.89(12) . . ?
O18 V1 V3 86.95(11) . . ?
O4 V1 V3 110.67(12) . . ?
O6 V1 V3 89.30(11) . . ?
O14 V2 O20 103.51(18) . . ?
O14 V2 O3 100.95(19) . . ?
O20 V2 O3 98.52(17) . . ?
O14 V2 O19 104.01(19) . . ?
O20 V2 O19 91.65(17) . . ?
O3 V2 O19 149.97(15) . . ?
O14 V2 O1 99.32(17) . . ?
O20 V2 O1 157.14(17) . . ?
O3 V2 O1 78.12(16) . . ?
O19 V2 O1 81.58(16) . . ?
O14 V2 V4 110.52(15) . . ?
O20 V2 V4 60.42(12) . . ?
O3 V2 V4 145.14(12) . . ?
O19 V2 V4 31.26(11) . . ?
O1 V2 V4 110.08(12) . . ?
015 V3 O20 103.22(19) . . ?
015 V3 O9 100.99(18) . . ?
O20 V3 O9 99.74(17) . . ?
015 V3 O17 103.79(18) . . ?
O20 V3 O17 91.75(16) . . ?
O9 V3 O17 149.44(16) . . ?
015 V3 O7 100.74(17) . . ?
O20 V3 O7 155.91(16) . . ?
O9 V3 O7 77.96(15) . . ?
O17 V3 O7 80.09(16) . . ?
015 V3 V1 109.78(15) . . ?
O20 V3 V1 61.39(12) . . ?
O9 V3 V1 146.62(11) . . ?
O17 V3 V1 30.37(11) . . ?
O7 V3 V1 107.76(11) . . ?
O16 V4 O19 107.16(19) . . ?
O16 V4 O18 102.18(18) . . ?
O19 V4 O18 98.18(17) . . ?
O16 V4 O10 108.40(18) . . ?
O19 V4 O10 142.20(16) . . ?
O18 V4 O10 86.55(15) . . ?
O16 V4 O12 93.45(19) . . ?
O19 V4 O12 87.53(16) . . ?
O18 V4 O12 160.85(15) . . ?
O10 V4 O12 77.98(15) . . ?
O16 V4 V2 140.33(15) . . ?
O19 V4 V2 33.25(11) . . ?
O18 V4 V2 86.80(11) . . ?
O10 V4 V2 110.68(11) . . ?
O12 V4 V2 88.17(12) . . ?
O2 C1 O1 125.6(5) . . ?
O2 C1 C2 121.1(6) . . ?
O1 C1 C2 113.2(5) . . ?
O3 C2 C1 105.0(5) . . ?
O3 C2 C3 107.3(4) . . ?
C1 C2 C3 109.7(4) . . ?
O4 C3 C2 108.8(4) . . ?
O4 C3 C4 109.3(4) . . ?
C2 C3 C4 110.0(4) . . ?
O5 C4 O6 126.8(5) . . ?
O5 C4 C3 120.2(5) . . ?
O6 C4 C3 113.0(5) . . ?
O8 C5 O7 125.7(5) . . ?
O8 C5 C6 123.4(5) . . ?
O7 C5 C6 110.9(5) . . ?
O9 C6 C5 107.5(4) . . ?
O9 C6 C7 108.6(4) . . ?
C5 C6 C7 107.7(4) . . ?
O10 C7 C8 109.7(4) . . ?
O10 C7 C6 105.9(4) . . ?
C8 C7 C6 110.1(4) . . ?
O11 C8 O12 124.9(5) . . ?
O11 C8 C7 120.9(5) . . ?
O12 C8 C7 114.1(5) . . ?
C1 O1 V2 113.9(3) . . ?
C2 O3 V2 112.3(3) . . ?
C3 O4 V1 119.3(3) . . ?
C4 O6 V1 118.7(4) . . ?
C5 O7 V3 113.7(3) . . ?
C6 O9 V3 112.3(3) . . ?
C7 O10 V4 118.7(3) . . ?
C8 O12 V4 117.1(4) . . ?
V1 O17 V3 116.74(19) . . ?
V4 O18 V1 131.82(19) . . ?
V4 O19 V2 115.49(19) . . ?
V3 O20 V2 174.8(2) . . ?
C51 N1 C31 104.3(5) . . ?
C51 N1 C11 112.3(6) . . ?
C31 N1 C11 111.7(6) . . ?
C51 N1 C71 112.7(5) . . ?
C31 N1 C71 111.5(5) . . ?
C11 N1 C71 104.6(5) . . ?
N1 C11 C21 113.9(6) . . ?
N1 C31 C41 119.0(7) . . ?
N1 C51 C61 113.2(6) . . ?
C81 C71 N1 114.1(5) . . ?
C12 N2 C32 128.9(13) . . ?
C12 N2 C72 106.2(10) . . ?
C32 N2 C72 105.5(6) . . ?
C12 N2 C52 100.5(8) . . ?
C32 N2 C52 107.4(7) . . ?
C72 N2 C52 106.5(6) . . ?
N2 C12 C22 105.5(8) . . ?
N2 C32 C42 108.3(7) . . ?
C62 C52 N2 115.8(7) . . ?
N2 C72 C82 112.7(7) . . ?
C73 N3 C13 107.0(4) . . ?
C73 N3 C53 110.3(4) . . ?
C13 N3 C53 111.6(5) . . ?
C73 N3 C33 111.9(5) . . ?
C13 N3 C33 110.3(4) . . ?
C53 N3 C33 105.8(4) . . ?
C23 C13 N3 115.5(5) . . ?
C43 C33 N3 115.5(5) . . ?
C63 C53 N3 115.0(5) . . ?
N3 C73 C83 116.4(5) . . ?
C14 N4 C54 106.7(4) . . ?
C14 N4 C74 111.5(4) . . ?
C54 N4 C74 111.5(4) . . ?
C14 N4 C34 111.6(4) . . ?
C54 N4 C34 110.1(4) . . ?
C74 N4 C34 105.7(4) . . ?
N4 C14 C24 114.7(5) . . ?
N4 C34 C44 114.8(5) . . ?
C64 C54 N4 115.6(5) . . ?
N4 C74 C84 114.7(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 O13 1.618(4) . ?
V1 O17 1.759(4) . ?
V1 O18 1.828(4) . ?
V1 O4 1.963(4) . ?
V1 O6 2.070(4) . ?
V1 V3 3.1064(15) . ?
V2 O14 1.618(4) . ?
V2 O20 1.854(4) . ?
V2 O3 1.869(4) . ?
V2 O19 1.884(4) . ?
V2 O1 2.059(4) . ?
V2 V4 3.1017(15) . ?
V3 015 1.602(4) . ?
V3 O20 1.838(4) . ?
V3 O9 1.882(4) . ?
V3 O17 1.889(4) . ?
V3 O7 2.070(4) . ?
V4 O16 1.617(4) . ?
V4 O19 1.783(4) . ?
V4 O18 1.823(4) . ?
V4 O10 1.962(4) . ?
V4 O12 2.070(4) . ?
C1 O2 1.257(7) . ?
C1 O1 1.285(7) . ?
C1 C2 1.522(8) . ?
C2 O3 1.442(7) . ?
C2 C3 1.538(8) . ?
C3 O4 1.401(7) . ?
C3 C4 1.563(7) . ?
C4 O5 1.245(7) . ?
C4 O6 1.269(7) . ?
C5 O8 1.225(7) . ?
C5 O7 1.308(7) . ?
C5 C6 1.553(8) . ?
C6 O9 1.398(7) . ?
C6 C7 1.570(7) . ?
C7 O10 1.402(6) . ?
C7 C8 1.535(8) . ?
C8 O11 1.254(7) . ?
C8 O12 1.291(7) . ?
N1 C51 1.510(8) . ?
N1 C31 1.515(8) . ?
N1 C11 1.531(8) . ?
N1 C71 1.542(7) . ?
C11 C21 1.560(11) . ?
C31 C41 1.523(11) . ?
C51 C61 1.542(11) . ?
C71 C81 1.535(10) . ?
N2 C12 1.331(13) . ?
N2 C32 1.490(11) . ?
N2 C72 1.520(10) . ?
N2 C52 1.586(10) . ?
C12 C22 1.856(19) . ?
C32 C42 1.672(12) . ?
C52 C62 1.447(11) . ?
C72 C82 1.561(11) . ?
N3 C73 1.497(7) . ?
N3 C13 1.525(7) . ?
N3 C53 1.536(8) . ?
N3 C33 1.546(8) . ?
C13 C23 1.508(9) . ?
C33 C43 1.530(9) . ?
C53 C63 1.521(9) . ?
C73 C83 1.530(8) . ?
N4 C14 1.525(7) . ?
N4 C54 1.526(8) . ?
N4 C74 1.527(7) . ?
N4 C34 1.537(7) . ?
C14 C24 1.560(9) . ?
C34 C44 1.538(8) . ?
C54 C64 1.508(8) . ?
C74 C84 1.534(8) . ?
