data_global
#===========================================================================

_audit_creation_date '2018-01-04'
_audit_creation_method  'from SHELXTL CIF, local template and enCIFer'
_audit_update_record
;   

;

#===========================================================================
# 1. SUBMISSION DETAILS
#===========================================================================

_publ_contact_author_name       'Dr Damon A. Parrish'

_publ_contact_author_address
;
Laboratory for the Structure of Matter
Naval Research Laboratory
Washington, DC 20375
;

_publ_contact_author_email        'damon.parrish@nrl.navy.mil'
_publ_contact_author_fax          '202-767-6874'
_publ_contact_author_phone        '202-404-2141'


_publ_requested_journal           ?
_publ_requested_category         ?
_publ_requested_coeditor_name     ?

_publ_contact_letter
;

; 

#===========================================================================
# 2. PROCESSING SUMMARY  (IUCr Office Use Only)
# Do  NOT  alter anthing in this section.
#===========================================================================
_journal_date_recd_electronic  ?
_journal_date_to_coeditor      ?
_journal_date_from_coeditor    ?
_journal_date_accepted         ?
_journal_date_printers_first   ?
_journal_date_printers_final   ?
_journal_date_proofs_out       ?
_journal_date_proofs_in        ?
_journal_coeditor_name         ?
_journal_coeditor_code         ?
_journal_coeditor_notes
; ?
;
_journal_techeditor_code       ?
_journal_techeditor_notes
; ?
;
_journal_coden_ASTM            ?
_journal_name_full             ?
_journal_year                  ?
_journal_volume                ?
_journal_issue                 ?
_journal_page_first            ?
_journal_page_last             ?
_journal_suppl_publ_number      ?
_journal_suppl_publ_pages       ?

#===========================================================================
# 3. TITLE AND AUTHOR LIST
#===========================================================================

_publ_section_title
;
title
;


loop_
 _publ_author_name
 _publ_author_address
 _publ_author_footnote
'Parrish, Damon A.'
;
CBMSE, Code 6910
Naval Research Laboratory
Washington, DC 20375
;
?
'Imler, Gregory H.'
;
CBMSE, Code 6910
Naval Research Laboratory
Washington, DC 20375
;
?
'Shreeve, Jean'ne'
;
Chemistry Department 
University of Idaho
Moscow, ID, 83843
;
?
'Tang, Yongxing'
;
Chemistry Department 
University of Idaho
Moscow, ID, 83843
;
?
#===========================================================================
# 4. TEXT
#===========================================================================

_publ_section_abstract
;

;

_publ_section_comment
;
;

_publ_section_exptl_prep
;
;

_publ_section_exptl_refinement
; 
;

_publ_section_references
;
Bruker (2015). APEX3 v2015.5-2. Bruker AXS Inc., Madison, Wisconsin, 
USA.

Bruker (2013). SAINT v8.34A. Bruker AXS Inc., Madison, Wisconsin, 
USA.

Bruker (2014). SADABS v2014/5, Bruker AXS Inc., Madison, Wisconsin, 
USA.

Bruker (2014). XPREP v2014/2. Bruker AXS Inc., Madison, Wisconsin, 
USA.

Bruker (2014). SHELXTL v2014/7. Bruker AXS Inc., Madison, Wisconsin, 
USA.

Sheldrick, G. M. (2014). SHELXL-2014/7. University of Gottingen, Germany.

Spek, A. L.  (2001) PLATON, A Multipurpose Crystallographic Tool, 
Utrecht University, Utrecht, The Netherlands. 

Spek, A. L. (2015). Acta Cryst. C71, 9-18) SQUEEZE - Procedure
;

_publ_section_figure_captions
;
Fig 1.  View of 1 showing the labeling of the non-hydrogen atoms...   
Thermal ellipsoids are shown at the  ??% probability level.
;


_publ_section_table_legends
; 
;
#  E.g. Table 1.  Selected geometric parameters (\%A, \%) for compound (1)
#
#  E.g. Table 2.  Hydrogen-bond parameters (\%A, \%) for compound (1)
#  No table legends are required for Electronic-Paper submissions.


_publ_section_acknowledgements
;
Crystallographic studies were supported in part by the Office of Naval 
Research (ONR) and the Naval Research Laboratory (NRL).
;
 
data_shrv761_a_sq
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C3 H5 N7 O2, 0.667(H2 O)'
_chemical_formula_sum
 'C3 H6.33 N7 O2.67' 
_chemical_formula_weight          183.15

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_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'
 
_cell_length_a                    4.9771(4)
_cell_length_b                    13.1099(9)
_cell_length_c                    16.9277(11)
_cell_angle_alpha                 101.610(4)
_cell_angle_beta                  91.179(5)
_cell_angle_gamma                 90.050(5)
_cell_volume                      1081.68(14)
_cell_formula_units_Z             6
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used      3674
_cell_measurement_theta_min        2.67
_cell_measurement_theta_max       68.38
 
_exptl_crystal_description        block
_exptl_crystal_colour             'clear colorless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.687          
_exptl_crystal_F_000              568
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.134
_exptl_crystal_size_mid           0.049
_exptl_crystal_size_min           0.040
_exptl_absorpt_coefficient_mu     1.273
_shelx_estimated_absorpt_T_min    0.848
_shelx_estimated_absorpt_T_max    0.951
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.5385
_exptl_absorpt_correction_T_max   0.7531
_exptl_absorpt_process_details    'SADABS v2014/5 (Bruker, 2008)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    '1uS microfocus'
_diffrn_radiation_monochromator	  'HELIOS multilayer optics'
_diffrn_measurement_device_type   'Photon 100'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             7269
_diffrn_reflns_av_unetI/netI      0.0675
_diffrn_reflns_av_R_equivalents   0.0653
_diffrn_reflns_limit_h_min        -5
_diffrn_reflns_limit_h_max        5
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          2.665
_diffrn_reflns_theta_max          68.373
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   0.883
_diffrn_measured_fraction_theta_full  0.888
_diffrn_reflns_Laue_measured_fraction_max    0.883
_diffrn_reflns_Laue_measured_fraction_full   0.888
_diffrn_reflns_point_group_measured_fraction_max   0.883
_diffrn_reflns_point_group_measured_fraction_full  0.888
_reflns_number_total              3470
_reflns_number_gt                 2612
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX3 v2015.5-2 (Bruker, 2015)'
_computing_cell_refinement        'Bruker APEX3 v2015.5-2 (Bruker, 2015)'
_computing_data_reduction         
;
Bruker SAINT v8.34A (Bruker, 2013), Bruker XPREP v2014/2 (Bruker, 2014)
;
_computing_structure_solution     'Bruker SHELXTL v2014/7 (Bruker, 2014)' 
_computing_structure_refinement 
'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_computing_publication_material   'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_refine_special_details           
;
The program SQUEEZE was used to treat severely disordered water molecules
in a void that ran parallel to the a-axis.  SQUEEZE calculated that the 
void contained 44 electrons per unit cell which is proposed to be 
four water molecule per unit cell or two water molecule per asymmetric 
unit.  
;
# SQUEEZE RESULTS (Version =  21116)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.040  0.500  1.000       133        44 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1153P)²+0.4542P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      'intrinsic phasing'
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          3470
_refine_ls_number_parameters      325
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0922
_refine_ls_R_factor_gt            0.0651
_refine_ls_wR_factor_ref          0.2085
_refine_ls_wR_factor_gt           0.1872
_refine_ls_goodness_of_fit_ref    1.091
_refine_ls_restrained_S_all       1.091
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
O1 O 0.3372(7) 0.6286(3) 0.85078(17) 0.0774(10) Uani 1 1 d . . . . .
O2 O 0.6563(6) 0.7219(2) 0.81705(16) 0.0699(9) Uani 1 1 d . . . . .
N3 N 0.4789(6) 0.6520(2) 0.79565(18) 0.0519(8) Uani 1 1 d . . . . .
C4 C 0.4499(7) 0.6055(3) 0.7178(2) 0.0424(8) Uani 1 1 d . . . . .
C5 C 0.2459(7) 0.5227(3) 0.6915(2) 0.0421(8) Uani 1 1 d . . . . .
N7 N 0.2243(6) 0.4777(2) 0.61631(19) 0.0529(8) Uani 1 1 d . . . . .
H7A H 0.1031 0.4308 0.6008 0.063 Uiso 1 1 calc R U . . .
H7B H 0.3312 0.4947 0.5818 0.063 Uiso 1 1 calc R U . . .
N6 N 0.0802(6) 0.4954(3) 0.7431(2) 0.0543(8) Uani 1 1 d . . . . .
H6A H -0.0399 0.4483 0.7267 0.065 Uiso 1 1 calc R U . . .
H6B H 0.0921 0.5246 0.7934 0.065 Uiso 1 1 calc R U . . .
C8 C 0.6258(7) 0.6361(3) 0.6594(2) 0.0420(8) Uani 1 1 d . . . . .
N9 N 0.6200(6) 0.5957(2) 0.58133(18) 0.0512(8) Uani 1 1 d . . . . .
N10 N 0.8150(7) 0.6449(3) 0.54843(18) 0.0551(8) Uani 1 1 d . . . . .
N11 N 0.9379(6) 0.7121(2) 0.60253(18) 0.0496(7) Uani 1 1 d . . . . .
N12 N 0.8205(6) 0.7089(2) 0.67276(17) 0.0459(7) Uani 1 1 d . . . . .
H12 H 0.8632 0.7472 0.7188 0.055 Uiso 1 1 calc R U . . .
O13 O -0.3274(5) 0.3376(2) 0.69622(15) 0.0580(7) Uani 1 1 d . . . . .
O14 O -0.1944(5) 0.3078(2) 0.57287(15) 0.0537(7) Uani 1 1 d . . . . .
N15 N -0.3529(5) 0.2876(2) 0.62484(17) 0.0426(7) Uani 1 1 d . . . . .
C16 C -0.5438(6) 0.2109(3) 0.6022(2) 0.0410(7) Uani 1 1 d . . . . .
C17 C -0.7295(6) 0.1878(3) 0.6622(2) 0.0415(7) Uani 1 1 d . . . . .
N18 N -0.7263(7) 0.2378(3) 0.73697(19) 0.0564(8) Uani 1 1 d . . . . .
H18A H -0.8388 0.2215 0.7703 0.068 Uiso 1 1 calc R U . . .
H18B H -0.6117 0.2871 0.7530 0.068 Uiso 1 1 calc R U . . .
N19 N -0.9083(6) 0.1119(2) 0.63878(19) 0.0499(7) Uani 1 1 d . . . . .
H19A H -1.0196 0.0964 0.6728 0.060 Uiso 1 1 calc R U . . .
H19B H -0.9127 0.0782 0.5896 0.060 Uiso 1 1 calc R U . . .
C20 C -0.5567(6) 0.1578(2) 0.5199(2) 0.0393(7) Uani 1 1 d . . . . .
N21 N -0.7379(6) 0.0850(2) 0.48819(17) 0.0499(7) Uani 1 1 d . . . . .
N22 N -0.6843(7) 0.0545(3) 0.40934(19) 0.0565(8) Uani 1 1 d . . . . .
N23 N -0.4827(6) 0.1052(2) 0.39092(18) 0.0501(7) Uani 1 1 d . . . . .
N24 N -0.3970(6) 0.1679(2) 0.45789(17) 0.0438(7) Uani 1 1 d . . . . .
H24 H -0.2604 0.2090 0.4616 0.053 Uiso 1 1 calc R U . . .
O25 O -1.1199(6) 0.1911(3) 0.85084(17) 0.0684(8) Uani 1 1 d . . . . .
O26 O -1.2820(6) 0.0615(2) 0.76246(15) 0.0601(7) Uani 1 1 d . . . . .
N27 N -1.2881(6) 0.1163(2) 0.83158(17) 0.0473(7) Uani 1 1 d . . . . .
C28 C -1.4734(7) 0.0975(3) 0.8855(2) 0.0449(8) Uani 1 1 d . . . . .
C29 C -1.4850(7) 0.1586(3) 0.9659(2) 0.0469(8) Uani 1 1 d . . . . .
N30 N -1.3110(7) 0.2349(3) 0.9930(2) 0.0659(9) Uani 1 1 d . . . . .
H30A H -1.3230 0.2707 1.0413 0.079 Uiso 1 1 calc R U . . .
H30B H -1.1862 0.2487 0.9623 0.079 Uiso 1 1 calc R U . . .
N31 N -1.6728(6) 0.1404(3) 1.01508(18) 0.0560(8) Uani 1 1 d . . . . .
H31A H -1.6798 0.1774 1.0631 0.067 Uiso 1 1 calc R U . . .
H31B H -1.7885 0.0914 0.9992 0.067 Uiso 1 1 calc R U . . .
C32 C -1.6561(7) 0.0088(3) 0.8577(2) 0.0451(8) Uani 1 1 d . . . . .
N33 N -1.8402(7) -0.0213(3) 0.90405(18) 0.0575(8) Uani 1 1 d . . . . .
N34 N -1.9641(7) -0.1053(3) 0.8580(2) 0.0660(10) Uani 1 1 d . . . . .
N35 N -1.8676(7) -0.1254(3) 0.78725(19) 0.0612(9) Uani 1 1 d . . . . .
N36 N -1.6742(6) -0.0545(2) 0.78614(18) 0.0505(7) Uani 1 1 d . . . . .
H36 H -1.5772 -0.0508 0.7454 0.061 Uiso 1 1 calc R U . . .
 
 
_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_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
O1 N3 1.267(4) . ?
O2 N3 1.266(4) . ?
N3 C4 1.340(5) . ?
C4 C8 1.449(5) . ?
C4 C5 1.481(4) . ?
C5 N7 1.292(5) . ?
C5 N6 1.315(5) . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
C8 N9 1.321(5) . ?
C8 N12 1.343(4) . ?
N9 N10 1.354(4) . ?
N10 N11 1.281(4) . ?
N11 N12 1.343(4) . ?
N12 H12 0.8600 . ?
O13 N15 1.257(4) . ?
O14 N15 1.260(4) . ?
N15 C16 1.375(4) . ?
C16 C20 1.426(5) . ?
C16 C17 1.463(5) . ?
C17 N18 1.302(5) . ?
C17 N19 1.329(4) . ?
N18 H18A 0.8600 . ?
N18 H18B 0.8600 . ?
N19 H19A 0.8600 . ?
N19 H19B 0.8600 . ?
C20 N21 1.336(4) . ?
C20 N24 1.357(4) . ?
N21 N22 1.347(5) . ?
N22 N23 1.281(4) . ?
N23 N24 1.322(4) . ?
N24 H24 0.8600 . ?
O25 N27 1.275(4) . ?
O26 N27 1.245(4) . ?
N27 C28 1.367(4) . ?
C28 C29 1.436(5) . ?
C28 C32 1.471(5) . ?
C29 N31 1.318(5) . ?
C29 N30 1.326(5) . ?
N30 H30A 0.8600 . ?
N30 H30B 0.8600 . ?
N31 H31A 0.8600 . ?
N31 H31B 0.8600 . ?
C32 N36 1.325(5) . ?
C32 N33 1.328(4) . ?
N33 N34 1.354(5) . ?
N34 N35 1.277(5) . ?
N35 N36 1.340(4) . ?
N36 H36 0.8600 . ?
 
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
O2 N3 O1 116.9(3) . . ?
O2 N3 C4 120.1(3) . . ?
O1 N3 C4 123.0(3) . . ?
N3 C4 C8 118.9(3) . . ?
N3 C4 C5 121.1(3) . . ?
C8 C4 C5 120.1(3) . . ?
N7 C5 N6 118.9(3) . . ?
N7 C5 C4 120.0(3) . . ?
N6 C5 C4 121.0(3) . . ?
C5 N7 H7A 120.0 . . ?
C5 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
C5 N6 H6A 120.0 . . ?
C5 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
N9 C8 N12 107.2(3) . . ?
N9 C8 C4 124.9(3) . . ?
N12 C8 C4 127.9(3) . . ?
C8 N9 N10 106.4(3) . . ?
N11 N10 N9 110.9(3) . . ?
N10 N11 N12 106.5(3) . . ?
C8 N12 N11 108.9(3) . . ?
C8 N12 H12 125.5 . . ?
N11 N12 H12 125.5 . . ?
O13 N15 O14 118.5(3) . . ?
O13 N15 C16 122.2(3) . . ?
O14 N15 C16 119.2(3) . . ?
N15 C16 C20 118.4(3) . . ?
N15 C16 C17 119.4(3) . . ?
C20 C16 C17 122.3(3) . . ?
N18 C17 N19 119.0(3) . . ?
N18 C17 C16 123.1(3) . . ?
N19 C17 C16 117.9(3) . . ?
C17 N18 H18A 120.0 . . ?
C17 N18 H18B 120.0 . . ?
H18A N18 H18B 120.0 . . ?
C17 N19 H19A 120.0 . . ?
C17 N19 H19B 120.0 . . ?
H19A N19 H19B 120.0 . . ?
N21 C20 N24 105.3(3) . . ?
N21 C20 C16 125.2(3) . . ?
N24 C20 C16 129.5(3) . . ?
C20 N21 N22 107.3(3) . . ?
N23 N22 N21 110.4(3) . . ?
N22 N23 N24 107.2(3) . . ?
N23 N24 C20 109.8(3) . . ?
N23 N24 H24 125.1 . . ?
C20 N24 H24 125.1 . . ?
O26 N27 O25 118.7(3) . . ?
O26 N27 C28 120.7(3) . . ?
O25 N27 C28 120.6(3) . . ?
N27 C28 C29 122.2(3) . . ?
N27 C28 C32 116.4(3) . . ?
C29 C28 C32 121.3(3) . . ?
N31 C29 N30 117.9(3) . . ?
N31 C29 C28 120.3(3) . . ?
N30 C29 C28 121.8(3) . . ?
C29 N30 H30A 120.0 . . ?
C29 N30 H30B 120.0 . . ?
H30A N30 H30B 120.0 . . ?
C29 N31 H31A 120.0 . . ?
C29 N31 H31B 120.0 . . ?
H31A N31 H31B 120.0 . . ?
N36 C32 N33 107.4(3) . . ?
N36 C32 C28 129.2(3) . . ?
N33 C32 C28 123.4(3) . . ?
C32 N33 N34 105.9(3) . . ?
N35 N34 N33 110.8(3) . . ?
N34 N35 N36 106.5(3) . . ?
C32 N36 N35 109.3(3) . . ?
C32 N36 H36 125.3 . . ?
N35 N36 H36 125.3 . . ?
 
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_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
O2 N3 C4 C8 0.5(5) . . . . ?
O1 N3 C4 C8 -178.7(4) . . . . ?
O2 N3 C4 C5 179.4(3) . . . . ?
O1 N3 C4 C5 0.1(6) . . . . ?
N3 C4 C5 N7 -178.9(3) . . . . ?
C8 C4 C5 N7 -0.1(5) . . . . ?
N3 C4 C5 N6 2.8(5) . . . . ?
C8 C4 C5 N6 -178.5(3) . . . . ?
N3 C4 C8 N9 179.3(3) . . . . ?
C5 C4 C8 N9 0.4(5) . . . . ?
N3 C4 C8 N12 -1.1(5) . . . . ?
C5 C4 C8 N12 -179.9(3) . . . . ?
N12 C8 N9 N10 0.4(4) . . . . ?
C4 C8 N9 N10 -179.8(3) . . . . ?
C8 N9 N10 N11 0.3(4) . . . . ?
N9 N10 N11 N12 -0.9(4) . . . . ?
N9 C8 N12 N11 -1.0(4) . . . . ?
C4 C8 N12 N11 179.3(3) . . . . ?
N10 N11 N12 C8 1.1(4) . . . . ?
O13 N15 C16 C20 -179.6(3) . . . . ?
O14 N15 C16 C20 -0.8(5) . . . . ?
O13 N15 C16 C17 1.7(5) . . . . ?
O14 N15 C16 C17 -179.5(3) . . . . ?
N15 C16 C17 N18 1.0(5) . . . . ?
C20 C16 C17 N18 -177.7(3) . . . . ?
N15 C16 C17 N19 -178.7(3) . . . . ?
C20 C16 C17 N19 2.6(5) . . . . ?
N15 C16 C20 N21 -176.9(3) . . . . ?
C17 C16 C20 N21 1.8(5) . . . . ?
N15 C16 C20 N24 3.2(5) . . . . ?
C17 C16 C20 N24 -178.1(3) . . . . ?
N24 C20 N21 N22 -0.4(4) . . . . ?
C16 C20 N21 N22 179.7(3) . . . . ?
C20 N21 N22 N23 -0.7(4) . . . . ?
N21 N22 N23 N24 1.6(4) . . . . ?
N22 N23 N24 C20 -1.8(4) . . . . ?
N21 C20 N24 N23 1.3(4) . . . . ?
C16 C20 N24 N23 -178.7(3) . . . . ?
O26 N27 C28 C29 179.5(3) . . . . ?
O25 N27 C28 C29 -1.3(5) . . . . ?
O26 N27 C28 C32 1.5(5) . . . . ?
O25 N27 C28 C32 -179.3(3) . . . . ?
N27 C28 C29 N31 177.6(3) . . . . ?
C32 C28 C29 N31 -4.5(5) . . . . ?
N27 C28 C29 N30 -2.0(6) . . . . ?
C32 C28 C29 N30 176.0(4) . . . . ?
N27 C28 C32 N36 -2.6(6) . . . . ?
C29 C28 C32 N36 179.3(4) . . . . ?
N27 C28 C32 N33 177.6(3) . . . . ?
C29 C28 C32 N33 -0.5(6) . . . . ?
N36 C32 N33 N34 1.0(4) . . . . ?
C28 C32 N33 N34 -179.2(4) . . . . ?
C32 N33 N34 N35 -1.0(5) . . . . ?
N33 N34 N35 N36 0.6(5) . . . . ?
N33 C32 N36 N35 -0.6(4) . . . . ?
C28 C32 N36 N35 179.5(4) . . . . ?
N34 N35 N36 C32 0.0(5) . . . . ?
 
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 
N7 H7A O14  0.86 2.16 3.019(4) 174.4 .
N7 H7B N9  0.86 1.95 2.652(4) 137.4 .
N6 H6A O13  0.86 2.02 2.880(4) 176.1 .
N6 H6B O1  0.86 1.93 2.574(4) 131.1 .
N12 H12 O2  0.86 2.06 2.565(4) 117.0 .
N12 H12 N35  0.86 2.25 3.010(4) 146.7 1_865
N18 H18A O25  0.86 2.07 2.925(4) 176.5 .
N18 H18B O13  0.86 1.92 2.558(4) 130.3 .
N19 H19A O26  0.86 2.14 2.999(4) 176.9 .
N19 H19B N21  0.86 1.96 2.659(4) 137.8 .
N24 H24 N11  0.86 2.31 3.079(4) 148.5 2_666
N24 H24 O14  0.86 2.08 2.578(4) 116.2 .
N30 H30A O1  0.86 2.03 2.885(4) 172.5 2_467
N30 H30B O25  0.86 1.92 2.562(4) 130.3 .
N31 H31A O2  0.86 2.19 3.044(4) 174.0 2_467
N31 H31B N33  0.86 1.97 2.655(4) 136.2 .
N36 H36 N23  0.86 2.30 3.055(4) 146.7 2_356
N36 H36 O26  0.86 2.05 2.561(4) 117.0 .
 
_refine_diff_density_max    0.278
_refine_diff_density_min   -0.317
_refine_diff_density_rms    0.065

# start Validation Reply Form
_vrf_PLAT029_shrv761_a_sq
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.888 Why?  
RESPONSE: Low data completeness is often encountered in triclinic unit 
cells when utilizing Cu radiation.
;
# end Validation Reply Form