##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# 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 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. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_global
_audit_creation_method     'SHELXL-97 plus manual editing'
_journal_date_recd_electronic     2002-12-02
_journal_date_accepted     2003-01-07
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2003
_journal_volume     59
_journal_issue      2
_journal_page_first     o132
_journal_page_last     o134
_journal_paper_category     EO
_publ_contact_author_name     'Professor Jacek Klinowski'
_publ_contact_author_address
;
Department of Chemistry
University of Cambridge
Lensfield Road
Cambridge CB2 1EW
England
;
_publ_contact_author_email     jk18@cam.ac.uk
_publ_contact_author_fax     '+44 1223 336362'
_publ_contact_author_phone     '+44 1224 336514'
_publ_section_title
;
4-[2-(4-Pyridyl)ethyl]pyridinium nitrate trihydrate
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Almeida Paz, Filipe A.' .
; Department of Chemistry
  University of Cambridge
  Lensfield Road
  Cambridge CB2 1EW
  England
;
    'Khimyak, Yaroslav Z.' .
; Department of Chemistry
  University of Cambridge
  Lensfield Road
  Cambridge CB2 1EW
  England
;
    'Klinowski, Jacek' .
; Department of Chemistry
  University of Cambridge
  Lensfield Road
  Cambridge
  Cambridge CB2 1EW
  England
;
data_I
_chemical_name_systematic
;
4-[2-(4-Pyridyl)ethyl]pyridinium nitrate trihydrate
;
_chemical_name_common     ?
_chemical_formula_moiety     'C12 H13 N2 1+, N O3 1-, 3 H2 O'
_chemical_formula_sum     'C12 H19 N3 O6'
_chemical_formula_iupac     'C12 H13 N2 1+, N O3 1-, 3 H2 O'
_chemical_formula_weight     301.30
_chemical_melting_point     ?
_symmetry_cell_setting     Monoclinic
_symmetry_space_group_name_H-M     'P 21/c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y-1/2, z-1/2'
_cell_length_a     11.7751(4)
_cell_length_b     16.1980(7)
_cell_length_c     15.8787(4)
_cell_angle_alpha     90.00
_cell_angle_beta     90.175(2)
_cell_angle_gamma     90.00
_cell_volume     3028.58(18)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     15908
_cell_measurement_theta_min     1.00
_cell_measurement_theta_max     25.03
_cell_measurement_temperature     180(2)
_exptl_crystal_description     block
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     0.46
_exptl_crystal_size_mid     0.39
_exptl_crystal_size_min     0.12
_exptl_crystal_density_diffrn     1.322
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1280
_exptl_absorpt_coefficient_mu     0.107
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SORTAV; Blessing, 1995)'
_exptl_absorpt_correction_T_min     0.9526
_exptl_absorpt_correction_T_max     0.9873
_exptl_special_details
;
;
_diffrn_ambient_temperature     180(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Nonius KappaCCD'
_diffrn_measurement_method     'Thin-slice ω and φ'
_diffrn_reflns_number     21624
_diffrn_reflns_av_R_equivalents     0.0413
_diffrn_reflns_av_sigmaI/netI     0.0366
_diffrn_reflns_theta_min     3.59
_diffrn_reflns_theta_max     25.05
_diffrn_reflns_theta_full     25.05
_diffrn_measured_fraction_theta_max     0.992
_diffrn_measured_fraction_theta_full     0.992
_diffrn_reflns_limit_h_min     -14
_diffrn_reflns_limit_h_max     14
_diffrn_reflns_limit_k_min     -18
_diffrn_reflns_limit_k_max     19
_diffrn_reflns_limit_l_min     -18
_diffrn_reflns_limit_l_max     18
_diffrn_standards_number     0
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     5304
_reflns_number_gt     3982
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0981
_refine_ls_R_factor_gt     0.0756
_refine_ls_wR_factor_gt     0.2045
_refine_ls_wR_factor_ref     0.2223
_refine_ls_goodness_of_fit_ref     1.064
_refine_ls_restrained_S_all     1.063
_refine_ls_number_reflns     5304
_refine_ls_number_parameters     423
_refine_ls_number_restraints     20
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
     'calc w = 1/[σ²(Fo²)+(0.1132P)²+1.9726P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.026
_refine_ls_shift/su_mean     0.003
_refine_diff_density_max     0.707
_refine_diff_density_min     -0.299
_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'
_computing_data_collection     'COLLECT (Nonius, 1998)'
_computing_cell_refinement     'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction
;
HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK
;
_computing_structure_solution     'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement     'SHELXTL (Bruker, 2001)'
_computing_molecular_graphics     'SHELXTL'
_computing_publication_material     'SHELXTL'
loop_
    _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_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    N11 -0.25795(16) 1.01182(13) 0.86038(13) 0.0354(5) Uani d . 1 . . N
    N12 0.51924(16) 1.01354(14) 0.88350(13) 0.0351(5) Uani d D 1 . . N
    H12N 0.5925(11) 1.015(3) 0.871(2) 0.089(4) Uiso d D 1 . . H
    C11 -0.1976(2) 1.08140(16) 0.85559(17) 0.0394(6) Uani d . 1 . . C
    H11A -0.2356 1.1330 0.8595 0.047 Uiso calc R 1 . . H
    C12 -0.0815(2) 1.08024(16) 0.84503(16) 0.0391(6) Uani d . 1 . . C
    H12A -0.0403 1.1306 0.8419 0.047 Uiso calc R 1 . . H
    C13 -0.0250(2) 1.00569(16) 0.83906(15) 0.0336(6) Uani d . 1 . . C
    C14 -0.0889(2) 0.93446(17) 0.84450(18) 0.0422(6) Uani d . 1 . . C
    H14A -0.0532 0.8820 0.8410 0.051 Uiso calc R 1 . . H
    C15 -0.2042(2) 0.93975(17) 0.85495(18) 0.0439(7) Uani d . 1 . . C
    H15A -0.2473 0.8903 0.8584 0.053 Uiso calc R 1 . . H
    C16 0.1025(2) 1.00308(18) 0.83076(16) 0.0389(6) Uani d . 1 . . C
    H16A 0.1282 1.0502 0.7960 0.047 Uiso calc R 1 . . H
    H16B 0.1251 0.9515 0.8019 0.047 Uiso calc R 1 . . H
    C17 0.1595(2) 1.00711(19) 0.91745(16) 0.0411(6) Uani d . 1 . . C
    H17A 0.1335 1.0571 0.9477 0.049 Uiso calc R 1 . . H
    H17B 0.1374 0.9582 0.9510 0.049 Uiso calc R 1 . . H
    C18 0.2861(2) 1.00948(16) 0.90836(14) 0.0334(6) Uani d . 1 . . C
    C19 0.3429(2) 1.08334(16) 0.89421(16) 0.0387(6) Uani d . 1 . . C
    H19A 0.3018 1.1338 0.8928 0.046 Uiso calc R 1 . . H
    C110 0.4587(2) 1.08349(16) 0.88228(16) 0.0388(6) Uani d . 1 . . C
    H11B 0.4965 1.1345 0.8730 0.047 Uiso calc R 1 . . H
    C111 0.4666(2) 0.94185(16) 0.89694(16) 0.0388(6) Uani d . 1 . . C
    H11C 0.5100 0.8924 0.8975 0.047 Uiso calc R 1 . . H
    C112 0.3508(2) 0.93746(17) 0.91000(16) 0.0401(6) Uani d . 1 . . C
    H11D 0.3155 0.8857 0.9200 0.048 Uiso calc R 1 . . H
    N21 -0.00299(17) 1.00612(13) 0.60946(13) 0.0358(5) Uani d D 1 . . N
    H21N -0.0770(10) 1.001(2) 0.617(2) 0.089(4) Uiso d D 1 . . H
    N22 0.77418(16) 1.00920(13) 0.63403(13) 0.0349(5) Uani d . 1 . . N
    C21 0.0523(2) 1.07773(17) 0.60263(18) 0.0439(7) Uani d . 1 . . C
    H21A 0.0107 1.1279 0.6051 0.053 Uiso calc R 1 . . H
    C22 0.1683(2) 1.08034(17) 0.59213(18) 0.0434(7) Uani d . 1 . . C
    H22A 0.2059 1.1320 0.5871 0.052 Uiso calc R 1 . . H
    C23 0.2299(2) 1.00780(16) 0.58892(14) 0.0327(6) Uani d . 1 . . C
    C24 0.1705(2) 0.93431(16) 0.59563(16) 0.0398(6) Uani d . 1 . . C
    H24A 0.2098 0.8831 0.5930 0.048 Uiso calc R 1 . . H
    C25 0.0537(2) 0.93559(16) 0.60615(17) 0.0398(6) Uani d . 1 . . C
    H25A 0.0136 0.8849 0.6111 0.048 Uiso calc R 1 . . H
    C26 0.3575(2) 1.00845(17) 0.58087(16) 0.0378(6) Uani d . 1 . . C
    H26A 0.3809 1.0544 0.5437 0.045 Uiso calc R 1 . . H
    H26B 0.3832 0.9561 0.5549 0.045 Uiso calc R 1 . . H
    C27 0.4136(2) 1.01861(18) 0.66735(15) 0.0388(6) Uani d . 1 . . C
    H27A 0.3903 1.0719 0.6925 0.047 Uiso calc R 1 . . H
    H27B 0.3884 0.9737 0.7052 0.047 Uiso calc R 1 . . H
    C28 0.54147(19) 1.01622(15) 0.65877(14) 0.0322(6) Uani d . 1 . . C
    C29 0.6045(2) 1.08762(17) 0.64825(16) 0.0405(6) Uani d . 1 . . C
    H29A 0.5685 1.1401 0.6496 0.049 Uiso calc R 1 . . H
    C210 0.7195(2) 1.08194(17) 0.63581(17) 0.0405(6) Uani d . 1 . . C
    H21B 0.7619 1.1312 0.6282 0.049 Uiso calc R 1 . . H
    C211 0.7141(2) 0.94015(17) 0.64531(16) 0.0395(6) Uani d . 1 . . C
    H21C 0.7524 0.8885 0.6448 0.047 Uiso calc R 1 . . H
    C212 0.5986(2) 0.94157(16) 0.65767(16) 0.0373(6) Uani d . 1 . . C
    H21D 0.5581 0.8914 0.6654 0.045 Uiso calc R 1 . . H
    N31 -0.3773(2) 0.74636(14) 0.98086(15) 0.0462(6) Uani d . 1 . . N
    O31 -0.4662(2) 0.74849(15) 0.94000(13) 0.0649(6) Uani d . 1 . . O
    O32 -0.28801(19) 0.76856(15) 0.94417(14) 0.0645(6) Uani d . 1 . . O
    O33 -0.3752(2) 0.72427(14) 1.05453(14) 0.0673(7) Uani d . 1 . . O
    N41 0.1340(2) 0.76654(13) 0.77466(14) 0.0433(6) Uani d . 1 . . N
    O41 0.1325(2) 0.76995(14) 0.69782(13) 0.0599(6) Uani d . 1 . . O
    O42 0.2236(2) 0.77828(16) 0.81497(14) 0.0691(7) Uani d . 1 . . O
    O43 0.04672(18) 0.74937(14) 0.81572(13) 0.0565(6) Uani d . 1 . . O
    O5W 0.4197(2) 0.7775(2) 0.70942(17) 0.0826(9) Uani d D 1 . . O
    H5A 0.365(2) 0.782(3) 0.7367(19) 0.089(4) Uiso d D 1 . . H
    H5B 0.402(3) 0.770(3) 0.6629(12) 0.089(4) Uiso d D 1 . . H
    O6W 0.1359(2) 0.7730(2) 0.98979(15) 0.0910(10) Uani d D 1 . . O
    H6A 0.128(3) 0.773(3) 0.9411(11) 0.089(4) Uiso d D 1 . . H
    H6B 0.078(2) 0.762(3) 1.010(2) 0.089(4) Uiso d D 1 . . H
    O7W -0.0855(2) 0.7533(3) 1.0474(2) 0.1004(11) Uani d D 1 . . O
    H7A -0.142(2) 0.754(3) 1.021(2) 0.089(4) Uiso d D 1 . . H
    H7B -0.104(3) 0.752(3) 1.0941(12) 0.089(4) Uiso d D 1 . . H
    O8W -0.6535(2) 0.7428(3) 1.05106(18) 0.1065(12) Uani d D 1 . . O
    H8A -0.610(3) 0.732(3) 1.0166(19) 0.089(4) Uiso d D 1 . . H
    H8B -0.7138(18) 0.747(3) 1.032(2) 0.089(4) Uiso d D 1 . . H
    O9W -0.3625(2) 0.7473(2) 0.76751(14) 0.0777(8) Uani d D 1 . . O
    H9A -0.374(3) 0.753(3) 0.8156(12) 0.089(4) Uiso d D 1 . . H
    H9B -0.4227(19) 0.748(3) 0.747(2) 0.089(4) Uiso d D 1 . . H
    O10W -0.1474(3) 0.7373(3) 0.7077(2) 0.1367(18) Uani d D 1 . . O
    H10A -0.2084(17) 0.735(3) 0.726(2) 0.089(4) Uiso d D 1 . . H
    H10B -0.104(2) 0.724(3) 0.7416(19) 0.089(4) Uiso d D 1 . . H
_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
    N11 C15 . 1.331(3) no
    N11 C11 . 1.335(3) no
    N12 C111 . 1.334(3) no
    N12 C110 . 1.339(3) no
    N12 H12N . 0.887(10) no
    C11 C12 . 1.379(4) no
    C11 H11A . 0.950 no
    C12 C13 . 1.382(4) no
    C12 H12A . 0.950 no
    C13 C14 . 1.381(4) no
    C13 C16 . 1.507(3) no
    C14 C15 . 1.371(4) no
    C14 H14A . 0.950 no
    C15 H15A . 0.950 no
    C16 C17 . 1.531(4) no
    C16 H16A . 0.990 no
    C16 H16B . 0.990 no
    C17 C18 . 1.499(3) no
    C17 H17A . 0.990 no
    C17 H17B . 0.990 no
    C18 C19 . 1.389(4) no
    C18 C112 . 1.393(4) no
    C19 C110 . 1.377(4) no
    C19 H19A . 0.950 no
    C110 H11B . 0.950 no
    C111 C112 . 1.382(4) no
    C111 H11C . 0.950 no
    C112 H11D . 0.950 no
    N21 C25 . 1.324(3) no
    N21 C21 . 1.335(3) no
    N21 H21N . 0.883(10) no
    N22 C211 . 1.336(3) no
    N22 C210 . 1.343(3) no
    C21 C22 . 1.378(4) no
    C21 H21A . 0.950 no
    C22 C23 . 1.382(4) no
    C22 H22A . 0.950 no
    C23 C24 . 1.385(4) no
    C23 C26 . 1.509(3) no
    C24 C25 . 1.387(4) no
    C24 H24A . 0.950 no
    C25 H25A . 0.950 no
    C26 C27 . 1.531(4) no
    C26 H26A . 0.990 no
    C26 H26B . 0.990 no
    C27 C28 . 1.512(3) no
    C27 H27A . 0.990 no
    C27 H27B . 0.990 no
    C28 C212 . 1.384(3) no
    C28 C29 . 1.385(4) no
    C29 C210 . 1.371(4) no
    C29 H29A . 0.950 no
    C210 H21B . 0.950 no
    C211 C212 . 1.376(3) no
    C211 H21C . 0.950 no
    C212 H21D . 0.950 no
    N31 O33 . 1.224(3) yes
    N31 O31 . 1.230(3) yes
    N31 O32 . 1.257(3) yes
    N41 O41 . 1.221(3) yes
    N41 O42 . 1.246(3) yes
    N41 O43 . 1.250(3) yes
    O5W H5A . 0.785(17) no
    O5W H5B . 0.778(17) no
    O6W H6A . 0.779(17) no
    O6W H6B . 0.776(17) no
    O7W H7A . 0.793(17) no
    O7W H7B . 0.774(17) no
    O8W H8A . 0.772(17) no
    O8W H8B . 0.775(17) no
    O9W H9A . 0.782(17) no
    O9W H9B . 0.783(17) no
    O10W H10A . 0.778(17) no
    O10W H10B . 0.771(17) no
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
    C15 N11 C11 . . 118.9(2) no
    C111 N12 C110 . . 119.4(2) no
    C111 N12 H12N . . 121(3) no
    C110 N12 H12N . . 119(3) no
    N11 C11 C12 . . 121.6(2) no
    N11 C11 H11A . . 119.2 no
    C12 C11 H11A . . 119.2 no
    C11 C12 C13 . . 119.9(2) no
    C11 C12 H12A . . 120.1 no
    C13 C12 H12A . . 120.1 no
    C14 C13 C12 . . 117.6(2) no
    C14 C13 C16 . . 121.7(2) no
    C12 C13 C16 . . 120.7(2) no
    C15 C14 C13 . . 119.7(2) no
    C15 C14 H14A . . 120.1 no
    C13 C14 H14A . . 120.1 no
    N11 C15 C14 . . 122.3(2) no
    N11 C15 H15A . . 118.9 no
    C14 C15 H15A . . 118.9 no
    C13 C16 C17 . . 110.7(2) no
    C13 C16 H16A . . 109.5 no
    C17 C16 H16A . . 109.5 no
    C13 C16 H16B . . 109.5 no
    C17 C16 H16B . . 109.5 no
    H16A C16 H16B . . 108.1 no
    C18 C17 C16 . . 110.4(2) no
    C18 C17 H17A . . 109.6 no
    C16 C17 H17A . . 109.6 no
    C18 C17 H17B . . 109.6 no
    C16 C17 H17B . . 109.6 no
    H17A C17 H17B . . 108.1 no
    C19 C18 C112 . . 117.4(2) no
    C19 C18 C17 . . 121.1(2) no
    C112 C18 C17 . . 121.4(2) no
    C110 C19 C18 . . 120.1(2) no
    C110 C19 H19A . . 120.0 no
    C18 C19 H19A . . 120.0 no
    N12 C110 C19 . . 121.6(2) no
    N12 C110 H11B . . 119.2 no
    C19 C110 H11B . . 119.2 no
    N12 C111 C112 . . 121.9(2) no
    N12 C111 H11C . . 119.1 no
    C112 C111 H11C . . 119.1 no
    C111 C112 C18 . . 119.6(2) no
    C111 C112 H11D . . 120.2 no
    C18 C112 H11D . . 120.2 no
    C25 N21 C21 . . 120.1(2) no
    C25 N21 H21N . . 115(3) no
    C21 N21 H21N . . 125(3) no
    C211 N22 C210 . . 118.5(2) no
    N21 C21 C22 . . 121.4(2) no
    N21 C21 H21A . . 119.3 no
    C22 C21 H21A . . 119.3 no
    C21 C22 C23 . . 120.0(2) no
    C21 C22 H22A . . 120.0 no
    C23 C22 H22A . . 120.0 no
    C22 C23 C24 . . 117.6(2) no
    C22 C23 C26 . . 121.4(2) no
    C24 C23 C26 . . 121.0(2) no
    C23 C24 C25 . . 119.8(2) no
    C23 C24 H24A . . 120.1 no
    C25 C24 H24A . . 120.1 no
    N21 C25 C24 . . 121.2(2) no
    N21 C25 H25A . . 119.4 no
    C24 C25 H25A . . 119.4 no
    C23 C26 C27 . . 110.6(2) no
    C23 C26 H26A . . 109.5 no
    C27 C26 H26A . . 109.5 no
    C23 C26 H26B . . 109.5 no
    C27 C26 H26B . . 109.5 no
    H26A C26 H26B . . 108.1 no
    C28 C27 C26 . . 110.1(2) no
    C28 C27 H27A . . 109.6 no
    C26 C27 H27A . . 109.6 no
    C28 C27 H27B . . 109.6 no
    C26 C27 H27B . . 109.6 no
    H27A C27 H27B . . 108.2 no
    C212 C28 C29 . . 117.9(2) no
    C212 C28 C27 . . 120.5(2) no
    C29 C28 C27 . . 121.6(2) no
    C210 C29 C28 . . 119.4(2) no
    C210 C29 H29A . . 120.3 no
    C28 C29 H29A . . 120.3 no
    N22 C210 C29 . . 122.4(2) no
    N22 C210 H21B . . 118.8 no
    C29 C210 H21B . . 118.8 no
    N22 C211 C212 . . 122.0(2) no
    N22 C211 H21C . . 119.0 no
    C212 C211 H21C . . 119.0 no
    C211 C212 C28 . . 119.8(2) no
    C211 C212 H21D . . 120.1 no
    C28 C212 H21D . . 120.1 no
    O33 N31 O31 . . 121.9(3) yes
    O33 N31 O32 . . 120.8(3) yes
    O31 N31 O32 . . 117.3(2) yes
    O41 N41 O42 . . 121.0(2) yes
    O41 N41 O43 . . 121.4(3) yes
    O42 N41 O43 . . 117.5(2) yes
    H5A O5W H5B . . 108(3) no
    H6A O6W H6B . . 108(3) no
    H7A O7W H7B . . 106(2) no
    H8A O8W H8B . . 111(3) no
    H9A O9W H9B . . 105(2) no
    H10A O10W H10B . . 109(3) no
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
    C15 N11 C11 C12 . . . . 0.1(4) no
    N11 C11 C12 C13 . . . . 0.1(4) no
    C11 C12 C13 C14 . . . . -0.3(4) no
    C11 C12 C13 C16 . . . . -177.7(2) no
    C12 C13 C14 C15 . . . . 0.4(4) no
    C16 C13 C14 C15 . . . . 177.7(2) no
    C11 N11 C15 C14 . . . . -0.1(4) no
    C13 C14 C15 N11 . . . . -0.2(4) no
    C14 C13 C16 C17 . . . . -92.2(3) no
    C12 C13 C16 C17 . . . . 85.0(3) no
    C13 C16 C17 C18 . . . . -176.7(2) no
    C16 C17 C18 C19 . . . . 84.4(3) no
    C16 C17 C18 C112 . . . . -92.7(3) no
    C112 C18 C19 C110 . . . . 0.1(4) no
    C17 C18 C19 C110 . . . . -177.1(2) no
    C111 N12 C110 C19 . . . . -0.3(4) no
    C18 C19 C110 N12 . . . . 0.3(4) no
    C110 N12 C111 C112 . . . . -0.2(4) no
    N12 C111 C112 C18 . . . . 0.7(4) no
    C19 C18 C112 C111 . . . . -0.6(4) no
    C17 C18 C112 C111 . . . . 176.6(2) no
    C25 N21 C21 C22 . . . . 0.0(4) no
    N21 C21 C22 C23 . . . . -0.3(4) no
    C21 C22 C23 C24 . . . . 0.7(4) no
    C21 C22 C23 C26 . . . . -177.6(2) no
    C22 C23 C24 C25 . . . . -0.7(4) no
    C26 C23 C24 C25 . . . . 177.6(2) no
    C21 N21 C25 C24 . . . . 0.0(4) no
    C23 C24 C25 N21 . . . . 0.4(4) no
    C22 C23 C26 C27 . . . . 84.1(3) no
    C24 C23 C26 C27 . . . . -94.2(3) no
    C23 C26 C27 C28 . . . . 178.1(2) no
    C26 C27 C28 C212 . . . . -85.0(3) no
    C26 C27 C28 C29 . . . . 92.3(3) no
    C212 C28 C29 C210 . . . . 1.1(4) no
    C27 C28 C29 C210 . . . . -176.2(2) no
    C211 N22 C210 C29 . . . . -0.4(4) no
    C28 C29 C210 N22 . . . . -0.5(4) no
    C210 N22 C211 C212 . . . . 0.7(4) no
    N22 C211 C212 C28 . . . . -0.1(4) no
    C29 C28 C212 C211 . . . . -0.8(4) no
    C27 C28 C212 C211 . . . . 176.5(2) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    N12 H12N N11 1_655 0.880(10)
                               1.770(10)
                                       2.650(3) 171(4)
    N21 H21N N22 1_455 0.880(10)
                               1.780(10)
                                       2.654(3) 171(4)
    O5W H5A O42 . 0.78(2) 2.08(2) 2.858(3) 172(4)
    O5W H5B O8W 4_675 0.78(2) 1.90(2) 2.676(4) 176(4)
    O6W H6A O43 . 0.78(2) 2.24(2) 2.979(3) 158(4)
    O6W H6A O42 . 0.78(2) 2.30(2) 2.966(3) 144(3)
    O6W H6B O7W . 0.78(2) 2.02(2) 2.785(4) 169(4)
    O7W H7A O32 . 0.78(2) 2.11(2) 2.900(4) 173(4)
    O7W H7B O10W 4_576 0.77(2) 1.88(2) 2.654(5) 174(5)
    O8W H8A O31 . 0.77(2) 2.10(2) 2.829(4) 157(4)
    O8W H8B O6W 1_455 0.78(2) 1.94(2) 2.705(4) 172(4)
    O9W H9A O31 . 0.78(2) 2.26(2) 3.003(3) 160(4)
    O9W H9A O32 . 0.78(2) 2.29(2) 2.957(3) 144(3)
    O9W H9B O5W 1_455 0.78(2) 2.00(2) 2.767(3) 165(4)
    O10W H10A O9W . 0.78(2) 1.94(2) 2.713(4) 172(4)
    O10W H10B O43 . 0.77(2) 2.17(3) 2.860(4) 150(4)
