# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shrv429
_database_code_depnum_ccdc_archive 'CCDC 1526400'
_audit_update_record             
;
2017-01-09 deposited with the CCDC.
2017-03-03 downloaded from the CCDC.
;

_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 H3 N7 O2, H2 O'
_chemical_formula_sum            'C3 H5 N7 O3'
_chemical_formula_weight         187.14

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.6446(6)
_cell_length_b                   14.4368(7)
_cell_length_c                   7.7331(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.954(2)
_cell_angle_gamma                90
_cell_volume                     1401.27(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5320
_cell_measurement_theta_min      2.822
_cell_measurement_theta_max      29.732

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_F_000             768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.029
_exptl_absorpt_coefficient_mu    0.155
_shelx_estimated_absorpt_T_min   0.961
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   'SADABS v2014/5 (Bruker, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16794
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.150
_diffrn_reflns_theta_max         26.360
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2858
_reflns_number_gt                2186
_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.
 
 _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          
;
Two part disorder of oxygen atom in water is present with 57:43 ratio 
between two components.  Hydrogen atoms are not disorderd
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0475P)²+0.6801P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2858
_refine_ls_number_parameters     257
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.1011
_refine_ls_wR_factor_gt          0.0928
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.068
_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 0.57926(12) 0.35368(9) 0.6803(2) 0.0413(4) Uani 1 1 d . . . . .
O2 O 0.52973(10) 0.49717(9) 0.70467(19) 0.0315(4) Uani 1 1 d . . . . .
N3 N 0.59191(12) 0.43811(10) 0.6575(2) 0.0253(4) Uani 1 1 d . . . . .
N4 N 0.67693(12) 0.46023(10) 0.5816(2) 0.0228(4) Uani 1 1 d . . . . .
C5 C 0.69427(14) 0.55178(12) 0.5584(2) 0.0199(4) Uani 1 1 d . . . . .
N6 N 0.64857(12) 0.63133(10) 0.5956(2) 0.0239(4) Uani 1 1 d . . . . .
H6 H 0.5906 0.6341 0.6481 0.029 Uiso 1 1 calc R U . . .
N7 N 0.70086(13) 0.70981(10) 0.5439(2) 0.0256(4) Uani 1 1 d . . . . .
C8 C 0.77981(14) 0.67206(12) 0.4726(2) 0.0214(4) Uani 1 1 d . . . . .
N9 N 0.86557(12) 0.69351(10) 0.3888(2) 0.0239(4) Uani 1 1 d . . . . .
H9 H 0.8878 0.7492 0.3640 0.029 Uiso 1 1 calc R U . . .
C10 C 0.90966(15) 0.61051(12) 0.3513(3) 0.0244(4) Uani 1 1 d . . . . .
H10 H 0.9709 0.6062 0.2917 0.029 Uiso 1 1 calc R U . . .
N11 N 0.86105(12) 0.53739(10) 0.4038(2) 0.0237(4) Uani 1 1 d . . . . .
N12 N 0.77978(11) 0.57839(10) 0.4807(2) 0.0201(3) Uani 1 1 d . . . . .
O13 O 0.95317(11) -0.12619(8) 0.30744(18) 0.0271(3) Uani 1 1 d . . . . .
O14 O 0.81779(11) -0.10677(9) 0.45147(18) 0.0302(3) Uani 1 1 d . . . . .
N15 N 0.88995(12) -0.07393(10) 0.3746(2) 0.0207(3) Uani 1 1 d . . . . .
N16 N 0.90379(12) 0.01671(10) 0.3576(2) 0.0211(3) Uani 1 1 d . . . . .
C17 C 0.83359(14) 0.07008(12) 0.4308(2) 0.0188(4) Uani 1 1 d . . . . .
N18 N 0.74897(12) 0.05821(10) 0.5162(2) 0.0221(3) Uani 1 1 d . . . . .
H18 H 0.7252 0.0033 0.5423 0.026 Uiso 1 1 calc R U . . .
N19 N 0.70122(13) 0.14130(10) 0.5608(2) 0.0247(4) Uani 1 1 d . . . . .
C20 C 0.76165(14) 0.20267(12) 0.4957(2) 0.0210(4) Uani 1 1 d . . . . .
N21 N 0.77598(13) 0.29567(10) 0.4798(2) 0.0243(4) Uani 1 1 d . . . . .
H21 H 0.7365 0.3401 0.5164 0.029 Uiso 1 1 calc R U . . .
C22 C 0.86439(15) 0.30574(12) 0.3953(2) 0.0239(4) Uani 1 1 d . . . . .
H22 H 0.8916 0.3647 0.3688 0.029 Uiso 1 1 calc R U . . .
N23 N 0.90861(12) 0.22822(10) 0.3536(2) 0.0226(3) Uani 1 1 d . . . . .
N24 N 0.84169(12) 0.16388(10) 0.41773(19) 0.0191(3) Uani 1 1 d . . . . .
O25 O 0.64377(11) 0.91261(10) 0.6387(2) 0.0333(4) Uani 1 1 d D . . . .
H25A H 0.6385(19) 0.8658(12) 0.578(3) 0.050 Uiso 1 1 d D U . . .
H25B H 0.5833(11) 0.9251(16) 0.660(3) 0.050 Uiso 1 1 d D U . . .
O26A O 0.5116(3) 0.67957(18) 0.8304(9) 0.0362(16) Uani 0.574(12) 1 d D . P A 1
O26B O 0.4698(6) 0.6842(3) 0.7131(13) 0.041(2) Uani 0.426(12) 1 d D . P A 2
H26A H 0.4965(19) 0.7283(7) 0.775(2) 0.061 Uiso 1 1 d D U . . .
H26B H 0.4504(12) 0.6579(16) 0.802(2) 0.061 Uiso 1 1 d D 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 1.245(2) . ?
O2 N3 1.2441(19) . ?
N3 N4 1.325(2) . ?
N4 C5 1.355(2) . ?
C5 N6 1.333(2) . ?
C5 N12 1.355(2) . ?
N6 N7 1.395(2) . ?
N6 H6 0.8800 . ?
N7 C8 1.316(2) . ?
C8 N12 1.354(2) . ?
C8 N9 1.365(2) . ?
N9 C10 1.367(2) . ?
N9 H9 0.8800 . ?
C10 N11 1.310(2) . ?
C10 H10 0.9500 . ?
N11 N12 1.3812(19) . ?
O13 N15 1.2565(18) . ?
O14 N15 1.2417(18) . ?
N15 N16 1.329(2) . ?
N16 C17 1.350(2) . ?
C17 N18 1.335(2) . ?
C17 N24 1.363(2) . ?
N18 N19 1.404(2) . ?
N18 H18 0.8800 . ?
N19 C20 1.310(2) . ?
C20 N24 1.360(2) . ?
C20 N21 1.362(2) . ?
N21 C22 1.369(2) . ?
N21 H21 0.8800 . ?
C22 N23 1.309(2) . ?
C22 H22 0.9500 . ?
N23 N24 1.388(2) . ?
O25 H25A 0.821(10) . ?
O25 H25B 0.823(10) . ?
O26A H26A 0.834(10) . ?
O26A H26B 0.838(10) . ?
O26B H26A 0.842(10) . ?
O26B H26B 0.845(10) . ?

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 122.19(15) . . ?
O2 N3 N4 122.71(14) . . ?
O1 N3 N4 115.09(14) . . ?
N3 N4 C5 116.53(15) . . ?
N6 C5 N12 103.98(14) . . ?
N6 C5 N4 136.94(16) . . ?
N12 C5 N4 119.07(15) . . ?
C5 N6 N7 113.90(14) . . ?
C5 N6 H6 123.0 . . ?
N7 N6 H6 123.0 . . ?
C8 N7 N6 101.17(14) . . ?
N7 C8 N12 112.97(15) . . ?
N7 C8 N9 142.36(17) . . ?
N12 C8 N9 104.66(15) . . ?
C8 N9 C10 105.64(14) . . ?
C8 N9 H9 127.2 . . ?
C10 N9 H9 127.2 . . ?
N11 C10 N9 114.94(16) . . ?
N11 C10 H10 122.5 . . ?
N9 C10 H10 122.5 . . ?
C10 N11 N12 100.91(14) . . ?
C8 N12 C5 107.96(14) . . ?
C8 N12 N11 113.83(14) . . ?
C5 N12 N11 138.14(14) . . ?
O14 N15 O13 120.65(14) . . ?
O14 N15 N16 122.46(14) . . ?
O13 N15 N16 116.89(14) . . ?
N15 N16 C17 114.78(14) . . ?
N18 C17 N16 137.84(16) . . ?
N18 C17 N24 103.66(14) . . ?
N16 C17 N24 118.47(15) . . ?
C17 N18 N19 113.95(14) . . ?
C17 N18 H18 123.0 . . ?
N19 N18 H18 123.0 . . ?
C20 N19 N18 101.27(14) . . ?
N19 C20 N24 113.08(15) . . ?
N19 C20 N21 142.32(17) . . ?
N24 C20 N21 104.58(15) . . ?
C20 N21 C22 105.83(14) . . ?
C20 N21 H21 127.1 . . ?
C22 N21 H21 127.1 . . ?
N23 C22 N21 115.12(16) . . ?
N23 C22 H22 122.4 . . ?
N21 C22 H22 122.4 . . ?
C22 N23 N24 100.80(14) . . ?
C20 N24 C17 108.04(14) . . ?
C20 N24 N23 113.67(14) . . ?
C17 N24 N23 138.26(14) . . ?
H25A O25 H25B 106.5(19) . . ?
H26A O26A H26B 91.8(16) . . ?
H26A O26B H26B 90.8(15) . . ?

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 N4 C5 0.6(3) . . . . ?
O1 N3 N4 C5 -178.56(17) . . . . ?
N3 N4 C5 N6 1.8(3) . . . . ?
N3 N4 C5 N12 -179.67(16) . . . . ?
N12 C5 N6 N7 0.4(2) . . . . ?
N4 C5 N6 N7 179.0(2) . . . . ?
C5 N6 N7 C8 0.5(2) . . . . ?
N6 N7 C8 N12 -1.1(2) . . . . ?
N6 N7 C8 N9 178.4(3) . . . . ?
N7 C8 N9 C10 -178.9(3) . . . . ?
N12 C8 N9 C10 0.7(2) . . . . ?
C8 N9 C10 N11 -0.4(2) . . . . ?
N9 C10 N11 N12 -0.1(2) . . . . ?
N7 C8 N12 C5 1.5(2) . . . . ?
N9 C8 N12 C5 -178.23(15) . . . . ?
N7 C8 N12 N11 178.94(16) . . . . ?
N9 C8 N12 N11 -0.8(2) . . . . ?
N6 C5 N12 C8 -1.0(2) . . . . ?
N4 C5 N12 C8 -179.99(17) . . . . ?
N6 C5 N12 N11 -177.6(2) . . . . ?
N4 C5 N12 N11 3.5(3) . . . . ?
C10 N11 N12 C8 0.5(2) . . . . ?
C10 N11 N12 C5 176.9(2) . . . . ?
O14 N15 N16 C17 0.2(3) . . . . ?
O13 N15 N16 C17 179.56(15) . . . . ?
N15 N16 C17 N18 -1.9(3) . . . . ?
N15 N16 C17 N24 -179.40(16) . . . . ?
N16 C17 N18 N19 -178.1(2) . . . . ?
N24 C17 N18 N19 -0.3(2) . . . . ?
C17 N18 N19 C20 0.5(2) . . . . ?
N18 N19 C20 N24 -0.6(2) . . . . ?
N18 N19 C20 N21 -178.4(3) . . . . ?
N19 C20 N21 C22 177.3(3) . . . . ?
N24 C20 N21 C22 -0.7(2) . . . . ?
C20 N21 C22 N23 0.4(2) . . . . ?
N21 C22 N23 N24 0.1(2) . . . . ?
N19 C20 N24 C17 0.4(2) . . . . ?
N21 C20 N24 C17 179.08(15) . . . . ?
N19 C20 N24 N23 -177.84(15) . . . . ?
N21 C20 N24 N23 0.8(2) . . . . ?
N18 C17 N24 C20 0.0(2) . . . . ?
N16 C17 N24 C20 178.25(16) . . . . ?
N18 C17 N24 N23 177.54(19) . . . . ?
N16 C17 N24 N23 -4.2(3) . . . . ?
C22 N23 N24 C20 -0.6(2) . . . . ?
C22 N23 N24 C17 -178.1(2) . . . . ?

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
N6 H6 O2 0.88 2.19 2.651(2) 112.6 .
N6 H6 O26A 0.88 1.94 2.747(4) 151.8 .
N6 H6 O26B 0.88 1.82 2.649(4) 157.1 .
N9 H9 O13 0.88 2.05 2.9269(19) 174.9 1_565
N9 H9 O14 0.88 2.39 2.997(2) 126.4 1_565
N9 H9 N15 0.88 2.56 3.375(2) 155.2 1_565
C10 H10 N16 0.95 2.44 3.306(2) 151.5 2_755
C10 H10 N23 0.95 2.67 3.400(2) 134.6 2_755
N18 H18 O14 0.88 2.14 2.6051(19) 112.2 .
N18 H18 O25 0.88 1.88 2.718(2) 159.9 1_545
N21 H21 O1 0.88 2.49 3.198(2) 137.6 .
N21 H21 N3 0.88 2.65 3.508(2) 165.4 .
N21 H21 N4 0.88 1.98 2.841(2) 165.5 .
C22 H22 N11 0.95 2.54 3.345(2) 142.4 .
C22 H22 O13 0.95 2.52 3.102(2) 119.3 2_755
O25 H25A N7 0.821(10) 2.411(16) 3.124(2) 146(2) .
O25 H25A O26A 0.821(10) 2.43(2) 3.047(7) 132(2) 4_575
O25 H25B O2 0.823(10) 2.139(13) 2.9008(19) 154(2) 2_656
O26A H26A O1 0.834(10) 2.096(18) 2.761(3) 136(2) 2_656
O26B H26A O1 0.842(10) 2.096(18) 2.679(4) 126.0(18) 2_656
O26A H26B N19 0.838(10) 2.315(15) 2.967(3) 134.9(17) 2_656
O26B H26B N19 0.845(10) 2.315(15) 3.005(4) 139.2(18) 2_656

_refine_diff_density_max         0.229
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.048

# start Validation Reply Form
_vrf_PLAT015_shrv429             
;
PROBLEM: No _shelx_hkl_file record in SHELXL20xy CIF ....     Please Do ! 
RESPONSE: It is our policy to routinely not supply the HKL file unless 
specifically required.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shrv428
_database_code_depnum_ccdc_archive 'CCDC 1526401'
_audit_update_record             
;
2017-01-09 deposited with the CCDC.
2017-03-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 N6 O5, 2(C3 H6 N7), 2(H2 O)'
_chemical_formula_sum            'C8 H16 N20 O7'
_chemical_formula_weight         504.41

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9443(6)
_cell_length_b                   22.3674(10)
_cell_length_c                   6.8059(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.600(2)
_cell_angle_gamma                90
_cell_volume                     1915.26(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3477
_cell_measurement_theta_min      2.437
_cell_measurement_theta_max      27.126

_exptl_crystal_description       block
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.151
_shelx_estimated_absorpt_T_min   0.957
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6755
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   'SADABS v2014/5 (Bruker, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18805
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.176
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3923
_reflns_number_gt                2751
_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.
 
 _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          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0480P)²+0.2273P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3923
_refine_ls_number_parameters     340
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0850
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.023
_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 0.46417(11) 0.43956(6) 0.1731(2) 0.0264(3) Uani 1 1 d . . . . .
O2 O 0.55332(10) 0.35554(6) 0.2059(2) 0.0271(3) Uani 1 1 d . . . . .
N3 N 0.46715(13) 0.38461(7) 0.2039(2) 0.0198(4) Uani 1 1 d . . . . .
N4 N 0.39034(12) 0.35151(7) 0.2369(2) 0.0189(4) Uani 1 1 d . . . . .
C5 C 0.29301(15) 0.37929(8) 0.2235(3) 0.0179(4) Uani 1 1 d . . . . .
N6 N 0.26345(13) 0.43472(7) 0.1851(2) 0.0227(4) Uani 1 1 d . . . . .
O7 O 0.15554(10) 0.43520(6) 0.1844(2) 0.0255(3) Uani 1 1 d . . . . .
N8 N 0.11996(13) 0.37794(7) 0.2254(3) 0.0231(4) Uani 1 1 d . . . . .
C9 C 0.20413(15) 0.34376(8) 0.2495(3) 0.0179(4) Uani 1 1 d . . . . .
N10 N 0.21840(12) 0.28381(7) 0.2896(2) 0.0198(4) Uani 1 1 d . . . . .
N11 N 0.13479(13) 0.25298(7) 0.3132(2) 0.0208(4) Uani 1 1 d . . . . .
O12 O 0.14893(11) 0.19755(6) 0.3360(2) 0.0263(3) Uani 1 1 d . . . . .
O13 O 0.04725(11) 0.27647(6) 0.3132(2) 0.0307(4) Uani 1 1 d . . . . .
N14 N 0.28106(13) 0.57970(7) 0.8749(3) 0.0245(4) Uani 1 1 d . . . . .
H14A H 0.3473 0.5917 0.8905 0.029 Uiso 1 1 calc R U . . .
H14B H 0.2335 0.6039 0.9054 0.029 Uiso 1 1 calc R U . . .
C15 C 0.25314(15) 0.52555(9) 0.8059(3) 0.0189(4) Uani 1 1 d . . . . .
N16 N 0.30911(12) 0.48116(7) 0.7498(2) 0.0219(4) Uani 1 1 d . . . . .
H16 H 0.3774 0.4841 0.7537 0.026 Uiso 1 1 calc R U . . .
N17 N 0.24909(12) 0.42923(7) 0.6837(2) 0.0217(4) Uani 1 1 d . . . . .
C18 C 0.15503(15) 0.44625(8) 0.7020(3) 0.0180(4) Uani 1 1 d . . . . .
N19 N 0.15384(12) 0.50262(7) 0.7743(2) 0.0184(4) Uani 1 1 d . . . . .
N20 N 0.05471(12) 0.52208(7) 0.7925(2) 0.0203(4) Uani 1 1 d . . . . .
C21 C -0.00255(15) 0.47502(8) 0.7285(3) 0.0192(4) Uani 1 1 d . . . . .
H21 H -0.0765 0.4734 0.7228 0.023 Uiso 1 1 calc R U . . .
N22 N 0.05103(12) 0.42815(7) 0.6701(2) 0.0186(4) Uani 1 1 d . . . . .
N23 N -0.00054(13) 0.37642(7) 0.5769(3) 0.0218(4) Uani 1 1 d . . . . .
H23B H 0.0277(18) 0.3450(10) 0.657(3) 0.033 Uiso 1 1 d . U . . .
H23A H 0.0200(18) 0.3743(10) 0.451(4) 0.033 Uiso 1 1 d . U . . .
N24 N 0.63519(12) 0.68936(8) 0.2486(3) 0.0242(4) Uani 1 1 d . . . . .
H24A H 0.6652 0.7237 0.2316 0.029 Uiso 1 1 calc R U . . .
H24B H 0.6696 0.6556 0.2442 0.029 Uiso 1 1 calc R U . . .
C25 C 0.53929(15) 0.68847(8) 0.2803(3) 0.0193(4) Uani 1 1 d . . . . .
N26 N 0.47369(13) 0.73366(7) 0.2926(2) 0.0229(4) Uani 1 1 d . . . . .
H26 H 0.4915 0.7714 0.2838 0.028 Uiso 1 1 calc R U . . .
N27 N 0.37391(13) 0.71617(7) 0.3208(3) 0.0231(4) Uani 1 1 d . . . . .
C28 C 0.38560(15) 0.65856(8) 0.3264(3) 0.0185(4) Uani 1 1 d . . . . .
N29 N 0.48099(12) 0.63935(7) 0.3029(2) 0.0176(4) Uani 1 1 d . . . . .
N30 N 0.49079(13) 0.57692(7) 0.3072(2) 0.0204(4) Uani 1 1 d . . . . .
C31 C 0.39782(15) 0.56114(8) 0.3340(3) 0.0200(4) Uani 1 1 d . . . . .
H31 H 0.3780 0.5205 0.3428 0.024 Uiso 1 1 calc R U . . .
N32 N 0.33118(12) 0.60752(7) 0.3484(2) 0.0200(4) Uani 1 1 d . . . . .
N33 N 0.22634(14) 0.60165(8) 0.3721(3) 0.0255(4) Uani 1 1 d . . . . .
H33B H 0.2209(19) 0.6261(11) 0.477(4) 0.038 Uiso 1 1 d . U . . .
H33A H 0.1820(19) 0.6168(11) 0.259(4) 0.038 Uiso 1 1 d . U . . .
O34 O 0.17437(15) 0.72877(10) 0.5971(3) 0.0534(5) Uani 1 1 d D . . . .
H34A H 0.2345(12) 0.7363(15) 0.671(4) 0.080 Uiso 1 1 d D U . . .
H34B H 0.1261(16) 0.7213(15) 0.656(4) 0.080 Uiso 1 1 d D U . . .
O35 O 0.11518(13) 0.65213(8) 0.9738(3) 0.0432(4) Uani 1 1 d D . . . .
H35A H 0.129(2) 0.6878(6) 1.010(4) 0.065 Uiso 1 1 d D U . . .
H35B H 0.0520(10) 0.6434(11) 0.923(4) 0.065 Uiso 1 1 d D 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 1.246(2) . ?
O2 N3 1.288(2) . ?
N3 N4 1.301(2) . ?
N4 C5 1.388(2) . ?
C5 N6 1.306(2) . ?
C5 C9 1.443(3) . ?
N6 O7 1.396(2) . ?
O7 N8 1.411(2) . ?
N8 C9 1.309(2) . ?
C9 N10 1.372(2) . ?
N10 N11 1.325(2) . ?
N11 O13 1.249(2) . ?
N11 O12 1.257(2) . ?
N14 C15 1.319(2) . ?
N14 H14A 0.8800 . ?
N14 H14B 0.8800 . ?
C15 N16 1.337(2) . ?
C15 N19 1.353(2) . ?
N16 N17 1.411(2) . ?
N16 H16 0.8800 . ?
N17 C18 1.309(2) . ?
C18 N19 1.355(2) . ?
C18 N22 1.373(2) . ?
N19 N20 1.388(2) . ?
N20 C21 1.302(2) . ?
C21 N22 1.367(2) . ?
C21 H21 0.9500 . ?
N22 N23 1.410(2) . ?
N23 H23B 0.91(2) . ?
N23 H23A 0.96(2) . ?
N24 C25 1.309(2) . ?
N24 H24A 0.8800 . ?
N24 H24B 0.8800 . ?
C25 N26 1.335(2) . ?
C25 N29 1.362(2) . ?
N26 N27 1.405(2) . ?
N26 H26 0.8800 . ?
N27 C28 1.297(2) . ?
C28 N29 1.352(2) . ?
C28 N32 1.368(2) . ?
N29 N30 1.402(2) . ?
N30 C31 1.307(2) . ?
C31 N32 1.367(2) . ?
C31 H31 0.9500 . ?
N32 N33 1.410(2) . ?
N33 H33B 0.91(3) . ?
N33 H33A 0.91(3) . ?
O34 H34A 0.839(10) . ?
O34 H34B 0.835(10) . ?
O35 H35A 0.841(10) . ?
O35 H35B 0.833(10) . ?

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
O1 N3 O2 119.48(15) . . ?
O1 N3 N4 126.57(16) . . ?
O2 N3 N4 113.95(15) . . ?
N3 N4 C5 116.92(16) . . ?
N6 C5 N4 131.05(18) . . ?
N6 C5 C9 110.05(16) . . ?
N4 C5 C9 118.87(16) . . ?
C5 N6 O7 104.72(15) . . ?
N6 O7 N8 111.41(12) . . ?
C9 N8 O7 104.73(15) . . ?
N8 C9 N10 131.66(18) . . ?
N8 C9 C5 109.09(17) . . ?
N10 C9 C5 119.24(16) . . ?
N11 N10 C9 117.21(16) . . ?
O13 N11 O12 121.36(16) . . ?
O13 N11 N10 123.24(16) . . ?
O12 N11 N10 115.40(16) . . ?
C15 N14 H14A 120.0 . . ?
C15 N14 H14B 120.0 . . ?
H14A N14 H14B 120.0 . . ?
N14 C15 N16 131.50(18) . . ?
N14 C15 N19 125.11(18) . . ?
N16 C15 N19 103.39(16) . . ?
C15 N16 N17 114.06(15) . . ?
C15 N16 H16 123.0 . . ?
N17 N16 H16 123.0 . . ?
C18 N17 N16 100.68(15) . . ?
N17 C18 N19 113.29(17) . . ?
N17 C18 N22 142.97(18) . . ?
N19 C18 N22 103.73(15) . . ?
C15 N19 C18 108.59(16) . . ?
C15 N19 N20 136.94(16) . . ?
C18 N19 N20 114.46(15) . . ?
C21 N20 N19 100.50(15) . . ?
N20 C21 N22 115.44(17) . . ?
N20 C21 H21 122.3 . . ?
N22 C21 H21 122.3 . . ?
C21 N22 C18 105.87(15) . . ?
C21 N22 N23 122.78(15) . . ?
C18 N22 N23 131.00(16) . . ?
N22 N23 H23B 106.3(14) . . ?
N22 N23 H23A 104.0(14) . . ?
H23B N23 H23A 110(2) . . ?
C25 N24 H24A 120.0 . . ?
C25 N24 H24B 120.0 . . ?
H24A N24 H24B 120.0 . . ?
N24 C25 N26 129.83(18) . . ?
N24 C25 N29 127.07(17) . . ?
N26 C25 N29 103.07(16) . . ?
C25 N26 N27 114.60(15) . . ?
C25 N26 H26 122.7 . . ?
N27 N26 H26 122.7 . . ?
C28 N27 N26 100.13(15) . . ?
N27 C28 N29 114.58(17) . . ?
N27 C28 N32 140.60(18) . . ?
N29 C28 N32 104.82(15) . . ?
C28 N29 C25 107.61(15) . . ?
C28 N29 N30 113.27(15) . . ?
C25 N29 N30 139.12(16) . . ?
C31 N30 N29 100.95(15) . . ?
N30 C31 N32 114.98(17) . . ?
N30 C31 H31 122.5 . . ?
N32 C31 H31 122.5 . . ?
C31 N32 C28 105.98(15) . . ?
C31 N32 N33 125.32(16) . . ?
C28 N32 N33 128.64(16) . . ?
N32 N33 H33B 106.6(15) . . ?
N32 N33 H33A 107.5(15) . . ?
H33B N33 H33A 107(2) . . ?
H34A O34 H34B 116(2) . . ?
H35A O35 H35B 117(2) . . ?

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
O1 N3 N4 C5 4.5(3) . . . . ?
O2 N3 N4 C5 -175.84(16) . . . . ?
N3 N4 C5 N6 -1.0(3) . . . . ?
N3 N4 C5 C9 177.13(16) . . . . ?
N4 C5 N6 O7 177.81(19) . . . . ?
C9 C5 N6 O7 -0.5(2) . . . . ?
C5 N6 O7 N8 0.44(19) . . . . ?
N6 O7 N8 C9 -0.20(19) . . . . ?
O7 N8 C9 N10 -179.0(2) . . . . ?
O7 N8 C9 C5 -0.1(2) . . . . ?
N6 C5 C9 N8 0.4(2) . . . . ?
N4 C5 C9 N8 -178.14(17) . . . . ?
N6 C5 C9 N10 179.48(17) . . . . ?
N4 C5 C9 N10 0.9(3) . . . . ?
N8 C9 N10 N11 -1.5(3) . . . . ?
C5 C9 N10 N11 179.70(16) . . . . ?
C9 N10 N11 O13 -4.6(3) . . . . ?
C9 N10 N11 O12 175.36(16) . . . . ?
N14 C15 N16 N17 179.9(2) . . . . ?
N19 C15 N16 N17 -0.6(2) . . . . ?
C15 N16 N17 C18 0.8(2) . . . . ?
N16 N17 C18 N19 -0.8(2) . . . . ?
N16 N17 C18 N22 177.2(3) . . . . ?
N14 C15 N19 C18 179.64(19) . . . . ?
N16 C15 N19 C18 0.1(2) . . . . ?
N14 C15 N19 N20 1.4(3) . . . . ?
N16 C15 N19 N20 -178.15(19) . . . . ?
N17 C18 N19 C15 0.5(2) . . . . ?
N22 C18 N19 C15 -178.29(15) . . . . ?
N17 C18 N19 N20 179.15(15) . . . . ?
N22 C18 N19 N20 0.4(2) . . . . ?
C15 N19 N20 C21 178.3(2) . . . . ?
C18 N19 N20 C21 0.1(2) . . . . ?
N19 N20 C21 N22 -0.6(2) . . . . ?
N20 C21 N22 C18 0.9(2) . . . . ?
N20 C21 N22 N23 -172.96(17) . . . . ?
N17 C18 N22 C21 -178.8(3) . . . . ?
N19 C18 N22 C21 -0.72(19) . . . . ?
N17 C18 N22 N23 -5.7(4) . . . . ?
N19 C18 N22 N23 172.44(18) . . . . ?
N24 C25 N26 N27 177.67(19) . . . . ?
N29 C25 N26 N27 -0.5(2) . . . . ?
C25 N26 N27 C28 0.7(2) . . . . ?
N26 N27 C28 N29 -0.5(2) . . . . ?
N26 N27 C28 N32 179.8(2) . . . . ?
N27 C28 N29 C25 0.3(2) . . . . ?
N32 C28 N29 C25 -179.93(15) . . . . ?
N27 C28 N29 N30 -179.28(16) . . . . ?
N32 C28 N29 N30 0.5(2) . . . . ?
N24 C25 N29 C28 -178.10(19) . . . . ?
N26 C25 N29 C28 0.15(19) . . . . ?
N24 C25 N29 N30 1.3(4) . . . . ?
N26 C25 N29 N30 179.5(2) . . . . ?
C28 N29 N30 C31 0.0(2) . . . . ?
C25 N29 N30 C31 -179.4(2) . . . . ?
N29 N30 C31 N32 -0.5(2) . . . . ?
N30 C31 N32 C28 0.8(2) . . . . ?
N30 C31 N32 N33 178.25(18) . . . . ?
N27 C28 N32 C31 179.0(3) . . . . ?
N29 C28 N32 C31 -0.7(2) . . . . ?
N27 C28 N32 N33 1.6(4) . . . . ?
N29 C28 N32 N33 -178.07(18) . . . . ?

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
N14 H14A O2 0.88 1.97 2.748(2) 146.7 3_666
N14 H14A N3 0.88 2.68 3.517(2) 158.9 3_666
N14 H14B O35 0.88 2.02 2.893(2) 174.3 .
N16 H16 O1 0.88 2.63 3.363(2) 142.0 3_666
N16 H16 N30 0.88 2.30 3.003(2) 137.2 3_666
C21 H21 O7 0.95 2.44 2.976(2) 116.0 3_566
C21 H21 N33 0.95 2.53 3.297(3) 137.8 3_566
N23 H23B N11 0.91(2) 2.68(2) 3.565(2) 164.9(19) 4_566
N23 H23B O12 0.91(2) 1.99(2) 2.826(2) 152(2) 4_566
N23 H23A N8 0.96(2) 2.23(2) 3.148(3) 160.7(19) .
N23 H23A O13 0.96(2) 2.44(2) 3.021(2) 119.1(17) .
N24 H24A N10 0.88 2.05 2.890(2) 159.4 2_655
N24 H24B N17 0.88 2.17 3.028(2) 164.7 3_666
N26 H26 O2 0.88 1.98 2.749(2) 145.8 2_655
N26 H26 N3 0.88 2.59 3.461(2) 172.7 2_655
N26 H26 N4 0.88 2.38 3.202(2) 155.2 2_655
C31 H31 O1 0.95 2.54 3.126(2) 120.0 .
C31 H31 N6 0.95 2.51 3.350(3) 147.8 .
N33 H33B O34 0.91(3) 2.56(3) 3.371(3) 149(2) .
N33 H33A O35 0.91(3) 2.09(3) 2.977(3) 166(2) 1_554
O34 H34A N27 0.839(10) 2.135(14) 2.942(2) 161(3) 4_576
O34 H34B O13 0.835(10) 2.303(15) 3.072(2) 154(3) 3_566
O35 H35A O34 0.841(10) 2.005(10) 2.844(3) 175(3) 4_576
O35 H35B N8 0.833(10) 2.268(10) 3.101(2) 178(3) 3_566
O35 H35B O13 0.833(10) 2.54(3) 2.976(2) 113(2) 3_566

_refine_diff_density_max         0.253
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.050

# start Validation Reply Form
_vrf_PLAT015_shrv428             
;
PROBLEM: No _shelx_hkl_file record in SHELXL20xy CIF ....     Please Do ! 
RESPONSE: It is our policy to routinely not supply the HKL file unless 
specifically required.
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