#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/03/7010333.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_7010333
loop_
_publ_author_name
'Nakamura, Setsuko'
'Ozeki, Tomoji'
_publ_section_title
;
 Hydrogen-bonded aggregates of protonated decavanadate anions in their
 tetraalkylammonium salts † ‡
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              472
_journal_paper_doi               10.1039/b008128k
_journal_year                    2001
_chemical_formula_moiety         '(C16 H36 N +)2, (H4 V10 O28 2-)'
_chemical_formula_sum            'C32 H76 N2 O28 V10'
_chemical_formula_weight         1446.35
_chemical_name_common
;
 Bis(tetra-n-butylammonium) tetrahydrogendecavanadate
;
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.375(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.5633(9)
_cell_length_b                   21.048(3)
_cell_length_c                   15.435(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298
_cell_measurement_theta_max      15.00
_cell_measurement_theta_min      14.93
_cell_volume                     2764.8(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection       'MSC/AFC Diffractometer Control Software'
_computing_data_reduction
'teXsan PROCESS (Molecular Structure Corporation, 1993)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       ω--2q\
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6330
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        1.568
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'de Meulenaar & Tompa (1965)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0835P)²+0.6566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                4518
_reflns_number_total             6330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008128k.txt
_cod_data_source_block           TBAc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2764.9(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7010333
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V2B V 0.54192(7) 0.57165(3) 0.70094(4) 0.02899(15) Uani 1 1 d . . .
V1A V 0.54244(6) 0.54408(3) 0.41839(4) 0.02161(14) Uani 1 1 d . . .
V2A V 0.64607(7) 0.65005(3) 0.54923(4) 0.02623(15) Uani 1 1 d . . .
V3A V 0.79319(6) 0.51003(3) 0.59432(4) 0.02399(14) Uani 1 1 d . . .
V3B V 0.69369(6) 0.39887(3) 0.46161(4) 0.02582(15) Uani 1 1 d . . .
OG2 O 0.5426(3) 0.58136(14) 0.80263(18) 0.0430(7) Uani 1 1 d . . .
OG1 O 0.7245(3) 0.71674(12) 0.53310(18) 0.0371(6) Uani 1 1 d . . .
OF1 O 0.9712(3) 0.48411(13) 0.60585(17) 0.0323(6) Uani 1 1 d . . .
OF2 O 0.8698(3) 0.37102(12) 0.47495(19) 0.0363(6) Uani 1 1 d . . .
OE2 O 0.4649(3) 0.48195(11) 0.68521(15) 0.0275(5) Uani 1 1 d . . .
OE1 O 0.6245(3) 0.61635(11) 0.42247(16) 0.0268(5) Uani 1 1 d . . .
OD1 O 0.6351(3) 0.64522(12) 0.66364(16) 0.0314(5) Uani 1 1 d . . .
OC2 O 0.7481(3) 0.52961(12) 0.69597(16) 0.0295(5) Uani 1 1 d . . .
OB2 O 0.6704(2) 0.43269(11) 0.57936(15) 0.0246(5) Uani 1 1 d . . .
OC3 O 0.5689(3) 0.33384(11) 0.47526(17) 0.0296(5) Uani 1 1 d . . .
OC4 O 0.6524(3) 0.40231(12) 0.34287(17) 0.0309(5) Uani 1 1 d . . .
OB1 O 0.7473(3) 0.49567(11) 0.45623(16) 0.0226(5) Uani 1 1 d . . .
OC1 O 0.8335(4) 0.59640(15) 0.5601(2) 0.0293(6) Uani 1 1 d . . .
OA1 O 0.5482(2) 0.54729(10) 0.55197(14) 0.0231(5) Uani 1 1 d . . .
N1 N 0.5303(4) 0.78538(17) 0.2988(2) 0.0395(8) Uani 1 1 d . . .
C1 C 0.4561(5) 0.7790(2) 0.3831(3) 0.0444(10) Uani 1 1 d . . .
H1A H 0.5318 0.7932 0.4306 0.053 Uiso 1 1 calc R . .
H1B H 0.4359 0.7344 0.3926 0.053 Uiso 1 1 calc R . .
C2 C 0.3040(6) 0.8154(3) 0.3880(4) 0.0622(14) Uani 1 1 d . . .
H2A H 0.3205 0.8601 0.3770 0.075 Uiso 1 1 calc R . .
H2B H 0.2238 0.7997 0.3439 0.075 Uiso 1 1 calc R . .
C3 C 0.2502(9) 0.8070(4) 0.4775(5) 0.106(3) Uani 1 1 d . . .
H3A H 0.2378 0.7619 0.4877 0.127 Uiso 1 1 calc R . .
H3B H 0.3329 0.8223 0.5205 0.127 Uiso 1 1 calc R . .
C4 C 0.1042(10) 0.8388(5) 0.4927(6) 0.125(3) Uani 1 1 d . . .
H4A H 0.0816 0.8305 0.5512 0.188 Uiso 1 1 calc R . .
H4B H 0.0199 0.8231 0.4522 0.188 Uiso 1 1 calc R . .
H4C H 0.1153 0.8838 0.4847 0.188 Uiso 1 1 calc R . .
C5 C 0.4271(5) 0.7535(2) 0.2243(3) 0.0456(10) Uani 1 1 d . . .
H5A H 0.3242 0.7733 0.2198 0.055 Uiso 1 1 calc R . .
H5B H 0.4717 0.7625 0.1705 0.055 Uiso 1 1 calc R . .
C6 C 0.4048(6) 0.6824(2) 0.2304(4) 0.0584(13) Uani 1 1 d . . .
H6A H 0.3590 0.6723 0.2834 0.070 Uiso 1 1 calc R . .
H6B H 0.5061 0.6614 0.2328 0.070 Uiso 1 1 calc R . .
C7 C 0.2982(6) 0.6582(2) 0.1521(4) 0.0580(13) Uani 1 1 d . . .
H7A H 0.1951 0.6773 0.1523 0.070 Uiso 1 1 calc R . .
H7B H 0.3403 0.6716 0.0992 0.070 Uiso 1 1 calc R . .
C8 C 0.2813(10) 0.5875(3) 0.1512(5) 0.096(2) Uani 1 1 d . . .
H8A H 0.2133 0.5749 0.1005 0.143 Uiso 1 1 calc R . .
H8B H 0.2372 0.5740 0.2027 0.143 Uiso 1 1 calc R . .
H8C H 0.3827 0.5683 0.1498 0.143 Uiso 1 1 calc R . .
C9 C 0.6893(5) 0.7535(2) 0.3144(3) 0.0444(10) Uani 1 1 d . . .
H9A H 0.7519 0.7761 0.3608 0.053 Uiso 1 1 calc R . .
H9B H 0.6741 0.7106 0.3349 0.053 Uiso 1 1 calc R . .
C10 C 0.7817(6) 0.7500(3) 0.2367(4) 0.0668(16) Uani 1 1 d . . .
H10A H 0.7243 0.7248 0.1912 0.080 Uiso 1 1 calc R . .
H10B H 0.7945 0.7924 0.2139 0.080 Uiso 1 1 calc R . .
C11 C 0.9404(7) 0.7209(3) 0.2618(6) 0.094(2) Uani 1 1 d . . .
H11A H 0.9973 0.7220 0.2109 0.113 Uiso 1 1 calc R . .
H11B H 0.9966 0.7480 0.3055 0.113 Uiso 1 1 calc R . .
C12 C 0.9477(9) 0.6581(4) 0.2944(7) 0.133(4) Uani 1 1 d . . .
H12A H 1.0556 0.6461 0.3091 0.200 Uiso 1 1 calc R . .
H12B H 0.8991 0.6297 0.2508 0.200 Uiso 1 1 calc R . .
H12C H 0.8935 0.6558 0.3455 0.200 Uiso 1 1 calc R . .
C13 C 0.5459(5) 0.8552(2) 0.2739(3) 0.0436(10) Uani 1 1 d . . .
H13A H 0.5946 0.8572 0.2201 0.052 Uiso 1 1 calc R . .
H13B H 0.4414 0.8732 0.2623 0.052 Uiso 1 1 calc R . .
C14 C 0.6404(6) 0.8961(2) 0.3415(4) 0.0588(13) Uani 1 1 d . . .
H14A H 0.6024 0.8897 0.3978 0.071 Uiso 1 1 calc R . .
H14B H 0.7498 0.8832 0.3464 0.071 Uiso 1 1 calc R . .
C15 C 0.6282(7) 0.9658(2) 0.3177(4) 0.0658(14) Uani 1 1 d . . .
H15A H 0.6672 0.9721 0.2617 0.079 Uiso 1 1 calc R . .
H15B H 0.5185 0.9783 0.3118 0.079 Uiso 1 1 calc R . .
C16 C 0.7189(10) 1.0078(3) 0.3842(5) 0.103(3) Uani 1 1 d . . .
H16A H 0.7076 1.0513 0.3660 0.155 Uiso 1 1 calc R . .
H16B H 0.8280 0.9962 0.3895 0.155 Uiso 1 1 calc R . .
H16C H 0.6791 1.0026 0.4395 0.155 Uiso 1 1 calc R . .
H2 H 0.814(4) 0.4985(17) 0.430(2) 0.013(9) Uiso 1 1 d . . .
H1 H 0.877(6) 0.606(3) 0.547(4) 0.037(19) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.3005 0.5294 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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
OB1 H2 OF1 162(4) . 2_766 ?
OF1 OB1 H2 13(3) 2_766 . ?
OC1 H1 OF2 160(8) . 2_766 ?
OF2 OC1 H1 17(7) 2_766 . ?
V1A OB1 H2 120(3) . . ?
V3A OB1 H2 118(3) . . ?
V3B OB1 H2 107(3) . . ?
V2A OC1 H1 114(7) . . ?
V3A OC1 H1 131(7) . . ?
OG2 V2B OC4 103.50(14) . 3_666 ?
OG2 V2B OD1 104.17(13) . . ?
OC4 V2B OD1 92.30(11) 3_666 . ?
OG2 V2B OC2 101.00(14) . . ?
OC4 V2B OC2 154.91(11) 3_666 . ?
OD1 V2B OC2 86.86(11) . . ?
OG2 V2B OE2 101.93(13) . . ?
OC4 V2B OE2 87.92(11) 3_666 . ?
OD1 V2B OE2 153.08(11) . . ?
OC2 V2B OE2 81.80(10) . . ?
OG2 V2B OA1 174.67(13) . . ?
OC4 V2B OA1 79.70(10) 3_666 . ?
OD1 V2B OA1 79.79(9) . . ?
OC2 V2B OA1 75.47(9) . . ?
OE2 V2B OA1 73.77(9) . . ?
OG2 V2B V2A 135.76(11) . . ?
OC4 V2B V2A 83.41(8) 3_666 . ?
OD1 V2B V2A 31.61(8) . . ?
OC2 V2B V2A 82.84(7) . . ?
OE2 V2B V2A 122.13(7) . . ?
OA1 V2B V2A 48.37(6) . . ?
OG2 V2B V1A 131.90(11) . 3_666 ?
OC4 V2B V1A 82.63(8) 3_666 3_666 ?
OD1 V2B V1A 123.43(8) . 3_666 ?
OC2 V2B V1A 77.03(7) . 3_666 ?
OE2 V2B V1A 30.00(7) . 3_666 ?
OA1 V2B V1A 43.77(6) . 3_666 ?
V2A V2B V1A 92.14(2) . 3_666 ?
OG2 V2B V3B 134.97(12) . 3_666 ?
OC4 V2B V3B 31.69(8) 3_666 3_666 ?
OD1 V2B V3B 81.15(8) . 3_666 ?
OC2 V2B V3B 124.02(7) . 3_666 ?
OE2 V2B V3B 85.12(7) . 3_666 ?
OA1 V2B V3B 48.64(6) . 3_666 ?
V2A V2B V3B 59.64(2) . 3_666 ?
V1A V2B V3B 65.65(2) 3_666 3_666 ?
OE1 V1A OE2 107.61(12) . 3_666 ?
OE1 V1A OB2 99.54(11) . 3_666 ?
OE2 V1A OB2 99.60(11) 3_666 3_666 ?
OE1 V1A OB1 95.65(11) . . ?
OE2 V1A OB1 92.83(11) 3_666 . ?
OB2 V1A OB1 156.40(10) 3_666 . ?
OE1 V1A OA1 88.24(11) . . ?
OE2 V1A OA1 162.88(11) 3_666 . ?
OB2 V1A OA1 83.62(9) 3_666 . ?
OB1 V1A OA1 78.88(9) . . ?
OE1 V1A OA1 165.55(11) . 3_666 ?
OE2 V1A OA1 86.24(10) 3_666 3_666 ?
OB2 V1A OA1 81.70(9) 3_666 3_666 ?
OB1 V1A OA1 79.17(9) . 3_666 ?
OA1 V1A OA1 77.55(10) . 3_666 ?
OE1 V1A V2A 39.31(8) . . ?
OE2 V1A V2A 146.87(8) 3_666 . ?
OB2 V1A V2A 90.51(7) 3_666 . ?
OB1 V1A V2A 89.89(7) . . ?
OA1 V1A V2A 49.06(6) . . ?
OA1 V1A V2A 126.61(6) 3_666 . ?
OE1 V1A V3A 136.38(8) . 3_666 ?
OE2 V1A V3A 83.27(8) 3_666 3_666 ?
OB2 V1A V3A 37.03(7) 3_666 3_666 ?
OB1 V1A V3A 126.57(7) . 3_666 ?
OA1 V1A V3A 89.67(6) . 3_666 ?
OA1 V1A V3A 47.43(6) 3_666 3_666 ?
V2A V1A V3A 120.66(2) . 3_666 ?
OE1 V1A V2B 143.90(9) . 3_666 ?
OE2 V1A V2B 36.52(8) 3_666 3_666 ?
OB2 V1A V2B 93.02(7) 3_666 3_666 ?
OB1 V1A V2B 85.08(7) . 3_666 ?
OA1 V1A V2B 126.94(7) . 3_666 ?
OA1 V1A V2B 49.72(6) 3_666 3_666 ?
V2A V1A V2B 174.29(3) . 3_666 ?
V3A V1A V2B 61.022(19) 3_666 3_666 ?
OG1 V2A OD1 105.99(13) . . ?
OG1 V2A OC3 103.42(13) . 3_666 ?
OD1 V2A OC3 92.96(12) . 3_666 ?
OG1 V2A OC1 99.59(14) . . ?
OD1 V2A OC1 90.88(13) . . ?
OC3 V2A OC1 154.61(12) 3_666 . ?
OG1 V2A OE1 98.60(12) . . ?
OD1 V2A OE1 155.27(10) . . ?
OC3 V2A OE1 83.60(11) 3_666 . ?
OC1 V2A OE1 82.49(12) . . ?
OG1 V2A OA1 170.54(12) . . ?
OD1 V2A OA1 82.53(10) . . ?
OC3 V2A OA1 79.81(9) 3_666 . ?
OC1 V2A OA1 75.83(11) . . ?
OE1 V2A OA1 72.76(9) . . ?
OG1 V2A V1A 129.42(11) . . ?
OD1 V2A V1A 124.53(8) . . ?
OC3 V2A V1A 78.04(8) 3_666 . ?
OC1 V2A V1A 79.13(9) . . ?
OE1 V2A V1A 30.82(6) . . ?
OA1 V2A V1A 42.04(6) . . ?
OG1 V2A V3B 134.58(10) . 3_666 ?
OD1 V2A V3B 83.17(8) . 3_666 ?
OC3 V2A V3B 31.17(7) 3_666 3_666 ?
OC1 V2A V3B 125.08(10) . 3_666 ?
OE1 V2A V3B 81.33(7) . 3_666 ?
OA1 V2A V3B 49.25(5) . 3_666 ?
V1A V2A V3B 61.217(19) . 3_666 ?
OG1 V2A V2B 139.20(11) . . ?
OD1 V2A V2B 33.22(8) . . ?
OC3 V2A V2B 83.63(8) 3_666 . ?
OC1 V2A V2B 85.97(10) . . ?
OE1 V2A V2B 122.19(7) . . ?
OA1 V2A V2B 49.51(6) . . ?
V1A V2A V2B 91.37(2) . . ?
V3B V2A V2B 60.60(2) 3_666 . ?
OF1 V3A OC2 106.74(13) . . ?
OF1 V3A OC1 98.79(13) . . ?
OC2 V3A OC1 95.15(13) . . ?
OF1 V3A OB2 102.89(12) . . ?
OC2 V3A OB2 97.89(11) . . ?
OC1 V3A OB2 150.19(11) . . ?
OF1 V3A OB1 97.41(12) . . ?
OC2 V3A OB1 155.75(11) . . ?
OC1 V3A OB1 83.08(12) . . ?
OB2 V3A OB1 74.10(9) . . ?
OF1 V3A OA1 169.59(11) . . ?
OC2 V3A OA1 83.40(10) . . ?
OC1 V3A OA1 77.52(11) . . ?
OB2 V3A OA1 77.51(9) . . ?
OB1 V3A OA1 72.58(9) . . ?
OF1 V3A V1A 138.39(10) . 3_666 ?
OC2 V3A V1A 80.97(8) . 3_666 ?
OC1 V3A V1A 121.61(9) . 3_666 ?
OB2 V3A V1A 36.00(7) . 3_666 ?
OB1 V3A V1A 79.49(7) . 3_666 ?
OA1 V3A V1A 44.09(6) . 3_666 ?
OF2 V3B OC3 105.88(13) . . ?
OF2 V3B OC4 102.52(13) . . ?
OC3 V3B OC4 95.63(12) . . ?
OF2 V3B OB2 101.63(12) . . ?
OC3 V3B OB2 92.60(11) . . ?
OC4 V3B OB2 151.22(11) . . ?
OF2 V3B OB1 98.81(12) . . ?
OC3 V3B OB1 154.05(10) . . ?
OC4 V3B OB1 86.59(11) . . ?
OB2 V3B OB1 74.42(10) . . ?
OF2 V3B OA1 172.29(12) . 3_666 ?
OC3 V3B OA1 81.11(10) . 3_666 ?
OC4 V3B OA1 79.68(10) . 3_666 ?
OB2 V3B OA1 74.41(9) . 3_666 ?
OB1 V3B OA1 73.84(8) . 3_666 ?
OF2 V3B V2A 138.84(10) . 3_666 ?
OC3 V3B V2A 33.28(8) . 3_666 ?
OC4 V3B V2A 83.22(8) . 3_666 ?
OB2 V3B V2A 88.81(7) . 3_666 ?
OB1 V3B V2A 122.31(7) . 3_666 ?
OA1 V3B V2A 48.47(6) 3_666 3_666 ?
OF2 V3B V2B 133.79(11) . 3_666 ?
OC3 V3B V2B 84.47(9) . 3_666 ?
OC4 V3B V2B 31.31(8) . 3_666 ?
OB2 V3B V2B 123.16(7) . 3_666 ?
OB1 V3B V2B 84.20(7) . 3_666 ?
OA1 V3B V2B 48.99(6) 3_666 3_666 ?
V2A V3B V2B 59.75(2) 3_666 3_666 ?
V1A OE2 V2B 113.47(12) 3_666 . ?
V1A OE1 V2A 109.87(12) . . ?
V2A OD1 V2B 115.17(13) . . ?
V3A OC2 V2B 115.86(13) . . ?
V1A OB2 V3A 106.97(11) 3_666 . ?
V1A OB2 V3B 107.75(11) 3_666 . ?
V3A OB2 V3B 107.61(11) . . ?
V3B OC3 V2A 115.54(13) . 3_666 ?
V2B OC4 V3B 117.00(13) 3_666 . ?
V1A OB1 V3B 108.06(10) . . ?
V1A OB1 V3A 105.60(10) . . ?
V3B OB1 V3A 96.58(10) . . ?
V3A OC1 V2A 113.34(16) . . ?
V1A OA1 V1A 102.45(10) . 3_666 ?
V1A OA1 V3A 101.29(9) . . ?
V1A OA1 V3A 88.47(8) 3_666 . ?
V1A OA1 V2A 88.90(8) . . ?
V1A OA1 V2A 168.62(12) 3_666 . ?
V3A OA1 V2A 90.17(8) . . ?
V1A OA1 V3B 90.22(8) . 3_666 ?
V1A OA1 V3B 96.64(8) 3_666 3_666 ?
V3A OA1 V3B 166.14(11) . 3_666 ?
V2A OA1 V3B 82.28(7) . 3_666 ?
V1A OA1 V2B 169.03(12) . . ?
V1A OA1 V2B 86.51(8) 3_666 . ?
V3A OA1 V2B 85.10(8) . . ?
V2A OA1 V2B 82.11(7) . . ?
V3B OA1 V2B 82.37(7) 3_666 . ?
C9 N1 C1 106.3(3) . . ?
C9 N1 C5 111.1(3) . . ?
C1 N1 C5 110.2(3) . . ?
C9 N1 C13 111.3(3) . . ?
C1 N1 C13 111.0(3) . . ?
C5 N1 C13 107.0(3) . . ?
N1 C1 C2 116.2(4) . . ?
C3 C2 C1 109.7(4) . . ?
C4 C3 C2 116.5(6) . . ?
C6 C5 N1 117.0(4) . . ?
C5 C6 C7 110.5(4) . . ?
C8 C7 C6 113.0(5) . . ?
C10 C9 N1 115.9(4) . . ?
C11 C10 C9 110.7(5) . . ?
C12 C11 C10 118.5(6) . . ?
C14 C13 N1 115.3(4) . . ?
C15 C14 C13 111.5(4) . . ?
C16 C15 C14 112.8(5) . . ?
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
OB1 H2 0.74(4) . ?
H2 OF1 2.01(4) 2_766 ?
OB1 OF1 2.725(3) 2_766 ?
OC1 H1 0.48(5) . ?
H1 OF2 2.29(5) 2_766 ?
OC1 OF2 2.742(4) 2_766 ?
V2B OG2 1.582(3) . ?
V2B OC4 1.810(3) 3_666 ?
V2B OD1 1.862(3) . ?
V2B OC2 1.984(3) . ?
V2B OE2 2.006(2) . ?
V2B OA1 2.362(2) . ?
V2B V2A 3.0766(9) . ?
V2B V1A 3.0908(9) 3_666 ?
V2B V3B 3.1027(9) 3_666 ?
V1A OE1 1.674(2) . ?
V1A OE2 1.685(2) 3_666 ?
V1A OB2 1.891(2) 3_666 ?
V1A OB1 2.056(2) . ?
V1A OA1 2.058(2) . ?
V1A OA1 2.142(2) 3_666 ?
V1A V2A 3.0729(9) . ?
V1A V3A 3.0774(8) 3_666 ?
V1A V2B 3.0908(9) 3_666 ?
V2A OG1 1.588(3) . ?
V2A OD1 1.782(3) . ?
V2A OC3 1.869(2) 3_666 ?
V2A OC1 1.955(3) . ?
V2A OE1 2.070(3) . ?
V2A OA1 2.322(2) . ?
V2A V3B 3.0732(8) 3_666 ?
V3A OF1 1.610(2) . ?
V3A OC2 1.707(3) . ?
V3A OC1 1.935(3) . ?
V3A OB2 1.938(2) . ?
V3A OB1 2.145(3) . ?
V3A OA1 2.267(2) . ?
V3A V1A 3.0774(8) 3_666 ?
V3B OF2 1.610(2) . ?
V3B OC3 1.763(2) . ?
V3B OC4 1.829(3) . ?
V3B OB2 1.982(2) . ?
V3B OB1 2.092(2) . ?
V3B OA1 2.350(2) 3_666 ?
V3B V2A 3.0732(8) 3_666 ?
V3B V2B 3.1028(9) 3_666 ?
OE2 V1A 1.685(2) 3_666 ?
OB2 V1A 1.891(2) 3_666 ?
OC3 V2A 1.869(2) 3_666 ?
OC4 V2B 1.810(3) 3_666 ?
OA1 V1A 2.142(2) 3_666 ?
OA1 V3B 2.350(2) 3_666 ?
N1 C9 1.513(5) . ?
N1 C1 1.516(5) . ?
N1 C5 1.526(6) . ?
N1 C13 1.528(5) . ?
C1 C2 1.519(6) . ?
C2 C3 1.514(7) . ?
C3 C4 1.459(9) . ?
C5 C6 1.514(6) . ?
C6 C7 1.519(7) . ?
C7 C8 1.495(8) . ?
C9 C10 1.510(6) . ?
C10 C11 1.502(8) . ?
C11 C12 1.414(9) . ?
C13 C14 1.516(7) . ?
C14 C15 1.513(7) . ?
C15 C16 1.504(8) . ?
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_publ_flag
OB1 H2 OF1 0.74(4) 2.01(4) 2.725(3) 162(4) ?
OC1 H1 OF2 0.48(5) 2.29(5) 2.742(4) 160(8) ?
