##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section E. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section E, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_journal_date_recd_electronic     2023-10-10
_journal_date_accepted     2023-10-15
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2023
_journal_volume     79
_journal_issue      1
_journal_page_first     0
_journal_page_last     0
_journal_paper_category     GM
_journal_paper_doi     10.1107/S2056989023009040
_journal_coeditor_code     NX2001
_publ_contact_author_name     'Shintaro Kodama'
_publ_contact_author_address
;
Department of Applied Chemistry, Graduate School of Engineering, Osaka
Metropolitan University, 1-1 Gakuen-cho, Nakaku, Sakai, Osaka 599-8531,
Japan
;
_publ_contact_author_email     'skodama@omu.ac.jp'
_publ_contact_author_fax     ?
_publ_contact_author_phone     '+81-72-254-9295'
_publ_section_title
;\
Crystal structure of (μ-hydrogen
disulfato)-μ-oxido-bis[(4,4'-di-tert-butyl-2,2'-bipyridine)\
oxidovanadium(IV/V)] acetonitrile monosolvate
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Kodama, Shintaro' .
;
Department of Applied Chemistry, Graduate School of Engineering, Osaka
Metropolitan University, 1-1 Gakuen-cho, Nakaku, Sakai, Osaka 599-8531,
Japan
;
    'Hashiguchi, Terushi' .
;
Department of Applied Chemistry, Graduate School of Engineering, Osaka
Prefecture University, 1-1 Gakuen-cho, Nakaku, Sakai, Osaka 599-8531,
Japan
;
    'Nomoto, Akihiro' .
;
Department of Applied Chemistry, Graduate School of Engineering, Osaka
Metropolitan University, 1-1 Gakuen-cho, Nakaku, Sakai, Osaka 599-8531,
Japan
;
_publ_section_synopsis
;
The crystal structure of a dinuclear oxidovanadium(IV/V) complex
[V₂O₂(μ-O)(μ-H(SO₄)₂)(4,4'-tBubpy)₂] acetonitrile
monosolvate has been determined.
;
_chemical_name_systematic
;\
(μ-Hydrogen disulfato)-μ-oxido-\
bis[(4,4'-di-tert-butyl-2,2'-bipyridine)oxidovanadium(IV/V)]
acetonitrile monosolvate
;
_chemical_name_common     ?
_chemical_formula_moiety     'C36 H49 N4 O11 S2 V2, C2 H3 N'
_chemical_formula_sum     'C38 H52 N5 O11 S2 V2'
_chemical_formula_iupac     '[V2 (H S2 O8) O3 (C18 H24 N2)2], C2 H3 N'
_chemical_formula_weight     920.84
_chemical_melting_point     ?
_space_group_crystal_system     orthorhombic
_space_group_name_H-M_alt     'F d d d'
_space_group_name_Hall     '-F 2uv 2vw'
loop_
    _space_group_symop_operation_xyz
    'x, y, z'
    '-x+3/4, -y+3/4, z'
    '-x+3/4, y, -z+3/4'
    'x, -y+3/4, -z+3/4'
    'x, y+1/2, z+1/2'
    '-x+3/4, -y+5/4, z+1/2'
    '-x+3/4, y+1/2, -z+5/4'
    'x, -y+5/4, -z+5/4'
    'x+1/2, y, z+1/2'
    '-x+5/4, -y+3/4, z+1/2'
    '-x+5/4, y, -z+5/4'
    'x+1/2, -y+3/4, -z+5/4'
    'x+1/2, y+1/2, z'
    '-x+5/4, -y+5/4, z'
    '-x+5/4, y+1/2, -z+3/4'
    'x+1/2, -y+5/4, -z+3/4'
    '-x, -y, -z'
    'x-3/4, y-3/4, -z'
    'x-3/4, -y, z-3/4'
    '-x, y-3/4, z-3/4'
    '-x, -y+1/2, -z+1/2'
    'x-3/4, y-1/4, -z+1/2'
    'x-3/4, -y+1/2, z-1/4'
    '-x, y-1/4, z-1/4'
    '-x+1/2, -y, -z+1/2'
    'x-1/4, y-3/4, -z+1/2'
    'x-1/4, -y, z-1/4'
    '-x+1/2, y-3/4, z-1/4'
    '-x+1/2, -y+1/2, -z'
    'x-1/4, y-1/4, -z'
    'x-1/4, -y+1/2, z-3/4'
    '-x+1/2, y-1/4, z-3/4'
_cell_length_a     13.0134(2)
_cell_length_b     34.9495(5)
_cell_length_c     39.4864(6)
_cell_angle_alpha     90
_cell_angle_beta     90
_cell_angle_gamma     90
_cell_volume     17958.9(5)
_cell_formula_units_Z     16
_cell_measurement_reflns_used     30626
_cell_measurement_theta_min     1.8790
_cell_measurement_theta_max     30.5730
_cell_measurement_temperature     110(2)
_exptl_crystal_description     Block
_exptl_crystal_colour     'clear dark brown'
_exptl_crystal_size_max     0.16
_exptl_crystal_size_mid     0.11
_exptl_crystal_size_min     0.06
_exptl_crystal_density_diffrn     1.362
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     7696
_exptl_absorpt_coefficient_mu     0.569
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_absorpt_correction_T_min     0.81541
_exptl_absorpt_correction_T_max     1.00000
_diffrn_ambient_temperature     110(2)
_diffrn_source     'Rotating Anode'
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type     'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method     'profile data from ω-scans'
_diffrn_detector_area_resol_mean     28.5714
_diffrn_reflns_number     51528
_diffrn_reflns_av_R_equivalents     0.0486
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_theta_min     2.063
_diffrn_reflns_theta_max     30.513
_diffrn_reflns_theta_full     25.242
_diffrn_measured_fraction_theta_max     0.957
_diffrn_measured_fraction_theta_full     0.999
_diffrn_reflns_limit_h_min     -18
_diffrn_reflns_limit_h_max     18
_diffrn_reflns_limit_k_min     -49
_diffrn_reflns_limit_k_max     50
_diffrn_reflns_limit_l_min     -55
_diffrn_reflns_limit_l_max     54
_refine_special_details     ?
_reflns_number_total     6582
_reflns_number_gt     5675
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0534
_refine_ls_R_factor_gt     0.0431
_refine_ls_wR_factor_gt     0.1054
_refine_ls_wR_factor_ref     0.1101
_refine_ls_goodness_of_fit_ref     1.123
_refine_ls_restrained_S_all     1.129
_refine_ls_number_reflns     6582
_refine_ls_number_parameters     287
_refine_ls_number_restraints     27
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
             'w=1/[σ²(Fo²)+(0.0469P)²+46.6480P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary     ?
_refine_ls_shift/su_max     0.003
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.502
_refine_diff_density_min     -0.335
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     .
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'
    'S' 'S' 0.1246 0.1234
                         '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'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_solution
;
olex2.solve 1.5 (Bourhis et al., 2015)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al.,  2009)
;
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    V V1 0.70713(2) 0.54069(2) 0.59096(2) 0.02335(8) Uani d 1 . .
    S S1 0.75306(3) 0.47690(2) 0.64590(2) 0.02120(10) Uani d 1 . .
    O O5 0.66572(10) 0.49435(3) 0.66352(3) 0.0235(2) Uani d 1 . .
    O O3 0.78535(10) 0.50242(4) 0.61695(3) 0.0255(3) Uani d 1 . .
    O O6 0.71873(10) 0.43950(3) 0.63066(3) 0.0258(3) Uani d 1 . .
    O O4 0.84010(10) 0.46966(4) 0.66746(3) 0.0299(3) Uani d 1 . .
    O O1 0.79258(12) 0.57322(4) 0.58859(3) 0.0369(3) Uani d 1 . .
    O O2 0.625000 0.55852(5) 0.625000 0.0394(5) Uani d 1 . .
    N N2 0.75091(11) 0.51363(4) 0.54454(3) 0.0216(3) Uani d 1 . .
    N N1 0.60817(12) 0.56465(4) 0.55441(3) 0.0224(3) Uani d 1 . .
    C C3 0.48418(13) 0.59696(5) 0.50377(4) 0.0225(3) Uani d 1 . .
    C C6 0.69971(13) 0.52426(5) 0.51604(4) 0.0202(3) Uani d 1 . .
    C C7 0.72724(13) 0.51037(5) 0.48439(4) 0.0223(3) Uani d 1 . .
    H H7 0.688735 0.517593 0.464972 0.027 Uiso calc 1 . .
    C C8 0.81169(13) 0.48568(5) 0.48092(4) 0.0252(3) Uani d 1 . .
    C C11 0.41640(14) 0.61383(5) 0.47598(5) 0.0260(3) Uani d 1 . .
    C C4 0.55602(13) 0.56814(4) 0.49641(4) 0.0210(3) Uani d 1 . .
    H H4 0.562535 0.558953 0.473872 0.025 Uiso calc 1 . .
    C C5 0.61741(13) 0.55301(4) 0.52172(4) 0.0200(3) Uani d 1 . .
    C C2 0.47668(14) 0.60821(5) 0.53749(5) 0.0265(3) Uani d 1 . .
    H H2 0.428897 0.627475 0.543821 0.032 Uiso calc 1 . .
    C C10 0.83025(13) 0.48947(5) 0.54148(4) 0.0259(3) Uani d 1 . .
    H H10 0.865230 0.481514 0.561393 0.031 Uiso calc 1 . .
    C C9 0.86340(14) 0.47561(5) 0.51049(5) 0.0283(4) Uani d 1 . .
    H H9 0.921500 0.459194 0.509397 0.034 Uiso calc 1 . .
    C C1 0.53844(15) 0.59148(5) 0.56180(4) 0.0266(3) Uani d 1 . .
    H H1 0.531067 0.599365 0.584695 0.032 Uiso calc 1 . .
    C C15 0.84388(15) 0.47210(6) 0.44572(5) 0.0329(4) Uani d 1 . .
    C C12 0.48286(15) 0.62876(5) 0.44658(5) 0.0310(4) Uani d 1 . .
    H H12A 0.524627 0.607783 0.437528 0.047 Uiso calc 1 . .
    H H12B 0.527993 0.649180 0.454815 0.047 Uiso calc 1 . .
    H H12C 0.438268 0.638807 0.428664 0.047 Uiso calc 1 . .
    C C13 0.34999(16) 0.64692(6) 0.48896(6) 0.0375(5) Uani d 1 . .
    H H13A 0.394311 0.666815 0.498583 0.056 Uiso calc 1 . .
    H H13B 0.302988 0.637465 0.506451 0.056 Uiso calc 1 . .
    H H13C 0.310203 0.657649 0.470150 0.056 Uiso calc 1 . .
    C C14 0.34585(16) 0.58193(6) 0.46305(5) 0.0346(4) Uani d 1 . .
    H H14A 0.299790 0.573763 0.481303 0.052 Uiso calc 1 . .
    H H14B 0.387562 0.560154 0.455598 0.052 Uiso calc 1 . .
    H H14C 0.305067 0.591466 0.443967 0.052 Uiso calc 1 . .
    C C18 0.93513(18) 0.44437(7) 0.44714(6) 0.0434(5) Uani d 1 . .
    H H18A 0.915526 0.421472 0.459928 0.065 Uiso calc 1 . .
    H H18B 0.993353 0.456879 0.458329 0.065 Uiso calc 1 . .
    H H18C 0.954806 0.437044 0.424081 0.065 Uiso calc 1 . .
    C C17 0.87660(19) 0.50771(7) 0.42503(5) 0.0437(5) Uani d 1 . .
    H H17A 0.929138 0.521948 0.437572 0.065 Uiso calc 1 . .
    H H17B 0.816724 0.524171 0.421258 0.065 Uiso calc 1 . .
    H H17C 0.904661 0.499545 0.403158 0.065 Uiso calc 1 . .
    C C16 0.75339(19) 0.45218(7) 0.42815(6) 0.0467(6) Uani d 1 . .
    H H16A 0.695186 0.469893 0.426686 0.070 Uiso calc 1 . .
    H H16B 0.733200 0.429568 0.441237 0.070 Uiso calc 1 . .
    H H16C 0.773966 0.444343 0.405306 0.070 Uiso calc 1 . .
    N N3 0.6842(6) 0.5900(2) 0.3294(2) 0.102(2) Uani d 0.5 A -1
    C C19 0.5721(5) 0.64049(17) 0.36076(15) 0.0605(14) Uani d 0.5 A -1
    H H19A 0.549690 0.660308 0.344825 0.091 Uiso calc 0.5 A -1
    H H19B 0.611988 0.652277 0.379037 0.091 Uiso calc 0.5 A -1
    H H19C 0.511740 0.627648 0.370330 0.091 Uiso calc 0.5 A -1
    C C20 0.6367(5) 0.61212(17) 0.34275(17) 0.0616(15) Uani d 0.5 A -1
    H H6 0.659(3) 0.4376(11) 0.6263(12) 0.022(11) Uiso d 0.5 . .
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    V1 O5 11 2.2827(12) ?
    V1 O3 . 1.9692(12) ?
    V1 O1 . 1.5932(14) ?
    V1 O2 . 1.8268(7) ?
    V1 N2 . 2.1399(14) ?
    V1 N1 . 2.1077(14) ?
    S1 O5 . 1.4654(13) ?
    S1 O3 . 1.5098(12) ?
    S1 O6 . 1.5066(13) ?
    S1 O4 . 1.4391(13) ?
    O6 H6 . 0.80(4) ?
    N2 C6 . 1.360(2) ?
    N2 C10 . 1.339(2) ?
    N1 C5 . 1.359(2) ?
    N1 C1 . 1.337(2) ?
    C3 C11 . 1.526(2) ?
    C3 C4 . 1.405(2) ?
    C3 C2 . 1.392(2) ?
    C6 C7 . 1.388(2) ?
    C6 C5 . 1.486(2) ?
    C7 H7 . 0.9500 ?
    C7 C8 . 1.404(2) ?
    C8 C9 . 1.393(2) ?
    C8 C15 . 1.527(2) ?
    C11 C12 . 1.539(3) ?
    C11 C13 . 1.532(2) ?
    C11 C14 . 1.532(2) ?
    C4 H4 . 0.9500 ?
    C4 C5 . 1.384(2) ?
    C2 H2 . 0.9500 ?
    C2 C1 . 1.382(3) ?
    C10 H10 . 0.9500 ?
    C10 C9 . 1.385(3) ?
    C9 H9 . 0.9500 ?
    C1 H1 . 0.9500 ?
    C15 C18 . 1.534(3) ?
    C15 C17 . 1.549(3) ?
    C15 C16 . 1.534(3) ?
    C12 H12A . 0.9800 ?
    C12 H12B . 0.9800 ?
    C12 H12C . 0.9800 ?
    C13 H13A . 0.9800 ?
    C13 H13B . 0.9800 ?
    C13 H13C . 0.9800 ?
    C14 H14A . 0.9800 ?
    C14 H14B . 0.9800 ?
    C14 H14C . 0.9800 ?
    C18 H18A . 0.9800 ?
    C18 H18B . 0.9800 ?
    C18 H18C . 0.9800 ?
    C17 H17A . 0.9800 ?
    C17 H17B . 0.9800 ?
    C17 H17C . 0.9800 ?
    C16 H16A . 0.9800 ?
    C16 H16B . 0.9800 ?
    C16 H16C . 0.9800 ?
    N3 C20 . 1.120(9) ?
    C19 H19A . 0.9800 ?
    C19 H19B . 0.9800 ?
    C19 H19C . 0.9800 ?
    C19 C20 . 1.482(8) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O3 V1 O5 . 11 85.44(5) ?
    O3 V1 N2 . . 90.49(5) ?
    O3 V1 N1 . . 160.47(5) ?
    O1 V1 O5 . 11 172.18(6) ?
    O1 V1 O3 . . 98.89(7) ?
    O1 V1 O2 . . 102.02(7) ?
    O1 V1 N2 . . 94.54(7) ?
    O1 V1 N1 . . 95.89(6) ?
    O2 V1 O5 . 11 83.64(5) ?
    O2 V1 O3 . . 98.66(5) ?
    O2 V1 N2 . . 159.52(5) ?
    O2 V1 N1 . . 90.62(5) ?
    N2 V1 O5 . 11 78.84(5) ?
    N1 V1 O5 . 11 78.52(5) ?
    N1 V1 N2 . . 75.63(5) ?
    O5 S1 O3 . . 109.23(7) ?
    O5 S1 O6 . . 108.70(8) ?
    O6 S1 O3 . . 107.02(7) ?
    O4 S1 O5 . . 113.76(8) ?
    O4 S1 O3 . . 109.43(8) ?
    O4 S1 O6 . . 108.49(8) ?
    S1 O5 V1 . 11 143.30(7) ?
    S1 O3 V1 . . 130.69(8) ?
    S1 O6 H6 . . 117(3) ?
    V1 O2 V1 . 11 140.11(10) ?
    C6 N2 V1 . . 117.24(11) ?
    C10 N2 V1 . . 124.13(11) ?
    C10 N2 C6 . . 118.41(14) ?
    C5 N1 V1 . . 118.52(11) ?
    C1 N1 V1 . . 122.95(11) ?
    C1 N1 C5 . . 118.51(15) ?
    C4 C3 C11 . . 120.86(15) ?
    C2 C3 C11 . . 122.56(15) ?
    C2 C3 C4 . . 116.56(15) ?
    N2 C6 C7 . . 121.55(15) ?
    N2 C6 C5 . . 114.41(14) ?
    C7 C6 C5 . . 123.97(14) ?
    C6 C7 H7 . . 119.8 ?
    C6 C7 C8 . . 120.33(15) ?
    C8 C7 H7 . . 119.8 ?
    C7 C8 C15 . . 119.64(15) ?
    C9 C8 C7 . . 116.86(16) ?
    C9 C8 C15 . . 123.49(16) ?
    C3 C11 C12 . . 110.40(15) ?
    C3 C11 C13 . . 112.15(15) ?
    C3 C11 C14 . . 107.75(14) ?
    C13 C11 C12 . . 108.28(16) ?
    C14 C11 C12 . . 109.39(15) ?
    C14 C11 C13 . . 108.84(16) ?
    C3 C4 H4 . . 119.7 ?
    C5 C4 C3 . . 120.58(15) ?
    C5 C4 H4 . . 119.7 ?
    N1 C5 C6 . . 114.19(14) ?
    N1 C5 C4 . . 121.35(15) ?
    C4 C5 C6 . . 124.43(14) ?
    C3 C2 H2 . . 119.9 ?
    C1 C2 C3 . . 120.28(16) ?
    C1 C2 H2 . . 119.9 ?
    N2 C10 H10 . . 118.7 ?
    N2 C10 C9 . . 122.69(15) ?
    C9 C10 H10 . . 118.7 ?
    C8 C9 H9 . . 119.9 ?
    C10 C9 C8 . . 120.11(16) ?
    C10 C9 H9 . . 119.9 ?
    N1 C1 C2 . . 122.68(16) ?
    N1 C1 H1 . . 118.7 ?
    C2 C1 H1 . . 118.7 ?
    C8 C15 C18 . . 112.05(16) ?
    C8 C15 C17 . . 107.79(16) ?
    C8 C15 C16 . . 110.01(17) ?
    C18 C15 C17 . . 108.31(18) ?
    C18 C15 C16 . . 108.92(18) ?
    C16 C15 C17 . . 109.72(18) ?
    C11 C12 H12A . . 109.5 ?
    C11 C12 H12B . . 109.5 ?
    C11 C12 H12C . . 109.5 ?
    H12A C12 H12B . . 109.5 ?
    H12A C12 H12C . . 109.5 ?
    H12B C12 H12C . . 109.5 ?
    C11 C13 H13A . . 109.5 ?
    C11 C13 H13B . . 109.5 ?
    C11 C13 H13C . . 109.5 ?
    H13A C13 H13B . . 109.5 ?
    H13A C13 H13C . . 109.5 ?
    H13B C13 H13C . . 109.5 ?
    C11 C14 H14A . . 109.5 ?
    C11 C14 H14B . . 109.5 ?
    C11 C14 H14C . . 109.5 ?
    H14A C14 H14B . . 109.5 ?
    H14A C14 H14C . . 109.5 ?
    H14B C14 H14C . . 109.5 ?
    C15 C18 H18A . . 109.5 ?
    C15 C18 H18B . . 109.5 ?
    C15 C18 H18C . . 109.5 ?
    H18A C18 H18B . . 109.5 ?
    H18A C18 H18C . . 109.5 ?
    H18B C18 H18C . . 109.5 ?
    C15 C17 H17A . . 109.5 ?
    C15 C17 H17B . . 109.5 ?
    C15 C17 H17C . . 109.5 ?
    H17A C17 H17B . . 109.5 ?
    H17A C17 H17C . . 109.5 ?
    H17B C17 H17C . . 109.5 ?
    C15 C16 H16A . . 109.5 ?
    C15 C16 H16B . . 109.5 ?
    C15 C16 H16C . . 109.5 ?
    H16A C16 H16B . . 109.5 ?
    H16A C16 H16C . . 109.5 ?
    H16B C16 H16C . . 109.5 ?
    H19A C19 H19B . . 109.5 ?
    H19A C19 H19C . . 109.5 ?
    H19B C19 H19C . . 109.5 ?
    C20 C19 H19A . . 109.5 ?
    C20 C19 H19B . . 109.5 ?
    C20 C19 H19C . . 109.5 ?
    N3 C20 C19 . . 178.4(7) ?
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_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    V1 N2 C6 C7 . . . . 175.43(12) ?
    V1 N2 C6 C5 . . . . -1.51(18) ?
    V1 N2 C10 C9 . . . . -172.91(14) ?
    V1 N1 C5 C6 . . . . -0.61(18) ?
    V1 N1 C5 C4 . . . . -178.82(12) ?
    V1 N1 C1 C2 . . . . 177.27(13) ?
    O5 V1 O2 V1 11 . . 11 36.88(3) ?
    O5 S1 O3 V1 . . . . -24.59(12) ?
    O3 V1 O2 V1 . . . 11 -47.50(4) ?
    O3 S1 O5 V1 . . . 11 14.21(15) ?
    O6 S1 O5 V1 . . . 11 -102.23(13) ?
    O6 S1 O3 V1 . . . . 92.92(11) ?
    O4 S1 O5 V1 . . . 11 136.79(12) ?
    O4 S1 O3 V1 . . . . -149.72(10) ?
    O1 V1 O2 V1 . . . 11 -148.59(5) ?
    N2 V1 O2 V1 . . . 11 68.14(17) ?
    N2 C6 C7 C8 . . . . -2.1(3) ?
    N2 C6 C5 N1 . . . . 1.4(2) ?
    N2 C6 C5 C4 . . . . 179.52(15) ?
    N2 C10 C9 C8 . . . . -2.1(3) ?
    N1 V1 O2 V1 . . . 11 115.25(4) ?
    C3 C4 C5 N1 . . . . 1.9(2) ?
    C3 C4 C5 C6 . . . . -176.08(15) ?
    C3 C2 C1 N1 . . . . 1.0(3) ?
    C6 N2 C10 C9 . . . . 1.4(3) ?
    C6 C7 C8 C9 . . . . 1.3(3) ?
    C6 C7 C8 C15 . . . . -177.25(17) ?
    C7 C6 C5 N1 . . . . -175.49(16) ?
    C7 C6 C5 C4 . . . . 2.7(3) ?
    C7 C8 C9 C10 . . . . 0.7(3) ?
    C7 C8 C15 C18 . . . . -178.11(18) ?
    C7 C8 C15 C17 . . . . 62.8(2) ?
    C7 C8 C15 C16 . . . . -56.8(2) ?
    C11 C3 C4 C5 . . . . 179.87(15) ?
    C11 C3 C2 C1 . . . . 178.68(16) ?
    C4 C3 C11 C12 . . . . -54.6(2) ?
    C4 C3 C11 C13 . . . . -175.46(16) ?
    C4 C3 C11 C14 . . . . 64.8(2) ?
    C4 C3 C2 C1 . . . . 0.4(3) ?
    C5 N1 C1 C2 . . . . -1.0(3) ?
    C5 C6 C7 C8 . . . . 174.54(16) ?
    C2 C3 C11 C12 . . . . 127.22(18) ?
    C2 C3 C11 C13 . . . . 6.4(2) ?
    C2 C3 C11 C14 . . . . -113.38(19) ?
    C2 C3 C4 C5 . . . . -1.9(2) ?
    C10 N2 C6 C7 . . . . 0.7(2) ?
    C10 N2 C6 C5 . . . . -176.23(15) ?
    C9 C8 C15 C18 . . . . 3.4(3) ?
    C9 C8 C15 C17 . . . . -115.7(2) ?
    C9 C8 C15 C16 . . . . 124.7(2) ?
    C1 N1 C5 C6 . . . . 177.74(15) ?
    C1 N1 C5 C4 . . . . -0.5(2) ?
    C15 C8 C9 C10 . . . . 179.22(18) ?
loop_
    _geom_hbond_atom_site_label_d
    _geom_hbond_atom_site_label_h
    _geom_hbond_atom_site_label_a
    _geom_hbond_site_symmetry_d
    _geom_hbond_site_symmetry_h
    _geom_hbond_site_symmetry_a
    _geom_hbond_distance_dh
    _geom_hbond_distance_ha
    _geom_hbond_distance_da
    _geom_hbond_angle_dha
    _geom_hbond_publ_flag
    C14 H14A Cg2 1_555 1_555 17_666 0.98 2.784 3.431(2) 124 yes
_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.
;
_shelx_estimated_absorpt_T_min     ?
_shelx_estimated_absorpt_T_max     ?
