# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_sh3500
_database_code_depnum_ccdc_archive 'CCDC 1045217'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H5 N5 S'
_chemical_formula_sum            'C5 H5 N5 S'
_chemical_formula_weight         167.20

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

_cell_length_a                   7.5806(3)
_cell_length_b                   14.4950(5)
_cell_length_c                   6.3109(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     693.45(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    132(2)
_cell_measurement_reflns_used    3214
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      29.84

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_F_000             344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.548
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.038
_exptl_absorpt_coefficient_mu    0.398
_shelx_estimated_absorpt_T_min   0.811
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7168
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   'SADABS, BrukerAXS 2010'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      132(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7200
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.810
_diffrn_reflns_theta_max         29.919
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             1891
_reflns_number_gt                1767
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.744
_reflns_Friedel_fraction_max     0.880
_reflns_Friedel_fraction_full    0.945

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0365P)²+0.0183P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 723 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.04(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1891
_refine_ls_number_parameters     120
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0641
_refine_ls_wR_factor_gt          0.0624
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_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
S1 S 0.15983(6) 0.36457(3) 0.33583(8) 0.02141(13) Uani 1 1 d . . . . .
N1 N -0.0048(2) 0.32014(12) 0.7020(2) 0.0191(3) Uani 1 1 d . . . . .
N2 N 0.1002(2) 0.19955(12) 0.4980(2) 0.0179(3) Uani 1 1 d . . . . .
N3 N 0.17896(19) 0.15818(12) 0.3278(4) 0.0228(3) Uani 1 1 d . . . . .
N4 N 0.1743(2) 0.07086(14) 0.3702(3) 0.0283(4) Uani 1 1 d . . . . .
N5 N 0.0968(2) 0.05190(13) 0.5597(3) 0.0256(4) Uani 1 1 d . . . . .
C1 C 0.0752(2) 0.29266(14) 0.5309(3) 0.0175(4) Uani 1 1 d . . . . .
C2 C 0.0503(2) 0.13310(14) 0.6381(3) 0.0190(4) Uani 1 1 d . . . . .
C3 C -0.0341(2) 0.16246(14) 0.8266(4) 0.0216(4) Uani 1 1 d . . . . .
C4 C -0.0582(2) 0.25495(14) 0.8480(4) 0.0206(4) Uani 1 1 d . . . . .
C5 C 0.1150(3) 0.47495(16) 0.4542(3) 0.0248(4) Uani 1 1 d . . . . .
H1 H -0.069(3) 0.1169(16) 0.933(4) 0.027(6) Uiso 1 1 d . . . . .
H2 H -0.112(3) 0.2791(15) 0.969(4) 0.012(5) Uiso 1 1 d . . . . .
H3 H 0.165(3) 0.5205(19) 0.355(5) 0.044(8) Uiso 1 1 d . . . . .
H4 H 0.174(3) 0.478(2) 0.593(5) 0.040(8) Uiso 1 1 d . . . . .
H5 H -0.007(4) 0.4836(19) 0.474(4) 0.035(7) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0232(2) 0.0238(2) 0.01728(18) 0.0016(2) 0.0013(2) -0.00180(17)
N1 0.0200(8) 0.0195(9) 0.0177(7) -0.0001(6) -0.0008(6) 0.0015(6)
N2 0.0160(8) 0.0218(9) 0.0160(7) -0.0036(6) -0.0010(6) 0.0019(6)
N3 0.0213(7) 0.0268(8) 0.0202(7) -0.0067(10) 0.0004(8) 0.0023(6)
N4 0.0260(8) 0.0288(10) 0.0299(11) -0.0090(8) -0.0002(7) 0.0039(7)
N5 0.0269(9) 0.0216(9) 0.0284(9) -0.0040(7) -0.0017(7) 0.0013(8)
C1 0.0150(9) 0.0200(10) 0.0175(7) -0.0010(8) -0.0040(6) -0.0011(7)
C2 0.0184(9) 0.0177(10) 0.0208(8) 0.0006(7) -0.0047(7) 0.0001(7)
C3 0.0236(8) 0.0233(9) 0.0178(7) 0.0014(9) -0.0017(9) -0.0018(7)
C4 0.0208(8) 0.0247(9) 0.0165(7) -0.0013(9) -0.0002(8) 0.0009(7)
C5 0.0295(11) 0.0205(11) 0.0246(10) 0.0020(8) -0.0013(8) -0.0030(9)

_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
S1 C1 1.736(2) . ?
S1 C5 1.798(2) . ?
N1 C1 1.301(2) . ?
N1 C4 1.381(3) . ?
N2 C2 1.361(3) . ?
N2 N3 1.367(3) . ?
N2 C1 1.379(3) . ?
N3 N4 1.294(3) . ?
N4 N5 1.361(3) . ?
N5 C2 1.324(3) . ?
C2 C3 1.416(3) . ?
C3 C4 1.360(3) . ?
C3 H1 0.98(3) . ?
C4 H2 0.94(2) . ?
C5 H3 0.99(3) . ?
C5 H4 0.98(3) . ?
C5 H5 0.94(3) . ?

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
C1 S1 C5 99.78(10) . . ?
C1 N1 C4 118.75(18) . . ?
C2 N2 N3 108.73(17) . . ?
C2 N2 C1 123.83(16) . . ?
N3 N2 C1 127.43(16) . . ?
N4 N3 N2 104.77(18) . . ?
N3 N4 N5 113.00(18) . . ?
C2 N5 N4 105.28(18) . . ?
N1 C1 N2 119.28(17) . . ?
N1 C1 S1 125.24(16) . . ?
N2 C1 S1 115.47(13) . . ?
N5 C2 N2 108.21(17) . . ?
N5 C2 C3 134.49(19) . . ?
N2 C2 C3 117.29(18) . . ?
C4 C3 C2 116.1(2) . . ?
C4 C3 H1 124.1(15) . . ?
C2 C3 H1 119.8(15) . . ?
C3 C4 N1 124.7(2) . . ?
C3 C4 H2 120.7(14) . . ?
N1 C4 H2 114.6(14) . . ?
S1 C5 H3 105.0(17) . . ?
S1 C5 H4 109.0(17) . . ?
H3 C5 H4 111(2) . . ?
S1 C5 H5 111.1(17) . . ?
H3 C5 H5 112(2) . . ?
H4 C5 H5 109(2) . . ?

_refine_diff_density_max         0.277
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.042

_shelxl_version_number           2014/6

_shelx_res_file                  
; 
TITL sh3500a in Pna2(1) 
CELL 0.71073   7.58060  14.49500   6.31090  90.0000  90.0000  90.0000 
ZERR    4.00   0.00030   0.00050   0.00020   0.0000   0.0000   0.0000 
LATT -1 
SYMM -X, -Y, 0.5+Z 
SYMM 0.5+X, 0.5-Y, Z 
SYMM 0.5-X, 0.5+Y, 0.5+Z 
SFAC C  H  N  S 
UNIT 20  20  20  4 
L.S. 4 
BOND $H 
FMAP 2 
PLAN -5 
ACTA 
SIZE 0.038 0.236 0.548 
TEMP -140.500 
WGHT    0.036500    0.018300 
FVAR       0.66698 
MOLE 1 
S1    4    0.159826    0.364567    0.335833    11.00000    0.02317    0.02379 = 
         0.01728    0.00156    0.00129   -0.00180 
N1    3   -0.004785    0.320141    0.701992    11.00000    0.02003    0.01952 = 
         0.01771   -0.00015   -0.00084    0.00147 
N2    3    0.100189    0.199553    0.497985    11.00000    0.01598    0.02177 = 
         0.01602   -0.00358   -0.00101    0.00191 
N3    3    0.178955    0.158182    0.327825    11.00000    0.02131    0.02683 = 
         0.02017   -0.00671    0.00041    0.00230 
N4    3    0.174294    0.070862    0.370156    11.00000    0.02604    0.02881 = 
         0.02992   -0.00900   -0.00021    0.00387 
N5    3    0.096766    0.051900    0.559703    11.00000    0.02687    0.02162 = 
         0.02842   -0.00397   -0.00171    0.00132 
C1    1    0.075188    0.292655    0.530917    11.00000    0.01499    0.02001 = 
         0.01752   -0.00097   -0.00400   -0.00109 
C2    1    0.050300    0.133101    0.638066    11.00000    0.01845    0.01768 = 
         0.02084    0.00056   -0.00465    0.00007 
C3    1   -0.034139    0.162457    0.826573    11.00000    0.02357    0.02325 = 
         0.01783    0.00137   -0.00173   -0.00181 
C4    1   -0.058205    0.254946    0.848003    11.00000    0.02075    0.02471 = 
         0.01646   -0.00134   -0.00016    0.00085 
C5    1    0.115018    0.474949    0.454210    11.00000    0.02946    0.02051 = 
         0.02456    0.00199   -0.00131   -0.00305 
H1    2   -0.068694    0.116879    0.933442    11.00000    0.02725 
H2    2   -0.112242    0.279144    0.969054    11.00000    0.01162 
H3    2    0.165097    0.520473    0.354975    11.00000    0.04402 
H4    2    0.173767    0.478133    0.592850    11.00000    0.04011 
H5    2   -0.006732    0.483568    0.474219    11.00000    0.03458 
HKLF 4 1 0 1 0 0 0 1 1 0 0 
  
REM  sh3500a in Pna2(1) 
REM R1 =  0.0261 for    1767 Fo > 4sig(Fo)  and  0.0292 for all    1891 data 
REM    120 parameters refined using      1 restraints 
  
END 
  
WGHT      0.0364      0.0168 
  
REM Highest difference peak  0.277,  deepest hole -0.159,  1-sigma level  0.042 
Q1    1   0.1077  0.3322  0.4376  11.00000  0.05    0.28 
Q2    1   0.0010  0.2139  0.8410  11.00000  0.05    0.24 
Q3    1   0.1274  0.1833  0.4119  11.00000  0.05    0.22 
Q4    1  -0.0069  0.1470  0.7331  11.00000  0.05    0.21 
Q5    1  -0.0192  0.2861  0.7739  11.00000  0.05    0.20 
;
_shelx_res_checksum              95523
####################################################################### 
# 
# 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_sh3502
_database_code_depnum_ccdc_archive 'CCDC 1045218'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H6 N6'
_chemical_formula_sum            'C5 H6 N6'
_chemical_formula_weight         150.16

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   3.9589(3)
_cell_length_b                   10.9827(8)
_cell_length_c                   15.3508(12)
_cell_angle_alpha                90
_cell_angle_beta                 93.0963(19)
_cell_angle_gamma                90
_cell_volume                     666.47(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    132(2)
_cell_measurement_reflns_used    2464
_cell_measurement_theta_min      3.24
_cell_measurement_theta_max      33.51

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_F_000             312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.681
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.038
_exptl_absorpt_coefficient_mu    0.107
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7153
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_process_details   'SADABS, BrukerAXS 2010'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      132(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19929
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.281
_diffrn_reflns_theta_max         33.689
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2657
_reflns_number_gt                2242
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0747P)²+0.0639P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2657
_refine_ls_number_parameters     124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.1149
_refine_ls_wR_factor_gt          0.1078
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_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
N1 N 0.76249(16) 0.08017(6) 0.92439(4) 0.01886(13) Uani 1 1 d . . . . .
N2 N 1.05152(15) 0.09954(6) 0.79712(4) 0.01660(13) Uani 1 1 d . . . . .
N3 N 1.22897(17) 0.15717(6) 0.73509(4) 0.02224(14) Uani 1 1 d . . . . .
N4 N 1.28201(19) 0.07390(6) 0.67730(4) 0.02453(15) Uani 1 1 d . . . . .
N5 N 1.14910(18) -0.03532(6) 0.69801(4) 0.02220(14) Uani 1 1 d . . . . .
N6 N 0.99936(19) 0.26664(6) 0.88797(4) 0.02259(15) Uani 1 1 d . . . . .
C1 C 0.93329(17) 0.14975(6) 0.87270(4) 0.01671(13) Uani 1 1 d . . . . .
C2 C 1.00453(18) -0.01913(6) 0.77382(4) 0.01757(14) Uani 1 1 d . . . . .
C3 C 0.82825(19) -0.09491(7) 0.82975(5) 0.02072(15) Uani 1 1 d . . . . .
C4 C 0.71557(19) -0.03969(7) 0.90254(5) 0.02008(15) Uani 1 1 d . . . . .
C5 C 0.8928(3) 0.32682(8) 0.96610(6) 0.02780(18) Uani 1 1 d . . . . .
H1 H 0.789(3) -0.1783(11) 0.8177(8) 0.029(3) Uiso 1 1 d . . . . .
H2 H 0.589(3) -0.0859(11) 0.9438(8) 0.027(3) Uiso 1 1 d . . . . .
H3 H 1.114(3) 0.3100(13) 0.8508(9) 0.038(3) Uiso 1 1 d . . . . .
H4 H 0.989(5) 0.296(2) 1.0161(13) 0.081(6) Uiso 1 1 d . . . . .
H5 H 0.659(5) 0.3149(18) 0.9719(13) 0.076(6) Uiso 1 1 d . . . . .
H6 H 0.947(5) 0.405(2) 0.9643(14) 0.086(6) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0221(3) 0.0176(3) 0.0174(3) 0.00020(19) 0.0057(2) -0.0009(2)
N2 0.0195(3) 0.0157(2) 0.0150(2) 0.00075(18) 0.00461(19) 0.00106(19)
N3 0.0279(3) 0.0198(3) 0.0200(3) 0.0028(2) 0.0101(2) 0.0015(2)
N4 0.0318(3) 0.0222(3) 0.0205(3) 0.0021(2) 0.0101(2) 0.0043(2)
N5 0.0286(3) 0.0205(3) 0.0180(3) -0.0007(2) 0.0062(2) 0.0035(2)
N6 0.0324(3) 0.0149(3) 0.0214(3) -0.0018(2) 0.0105(2) -0.0020(2)
C1 0.0189(3) 0.0158(3) 0.0156(3) -0.0001(2) 0.0035(2) 0.0008(2)
C2 0.0196(3) 0.0163(3) 0.0169(3) -0.0012(2) 0.0020(2) 0.0019(2)
C3 0.0245(3) 0.0168(3) 0.0212(3) -0.0010(2) 0.0040(2) -0.0027(2)
C4 0.0222(3) 0.0187(3) 0.0198(3) 0.0014(2) 0.0048(2) -0.0026(2)
C5 0.0390(4) 0.0209(3) 0.0245(4) -0.0061(3) 0.0106(3) -0.0010(3)

_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
N1 C1 1.3148(9) . ?
N1 C4 1.3686(9) . ?
N2 C2 1.3616(9) . ?
N2 N3 1.3685(8) . ?
N2 C1 1.3886(9) . ?
N3 N4 1.2991(9) . ?
N4 N5 1.3546(10) . ?
N5 C2 1.3362(9) . ?
N6 C1 1.3285(9) . ?
N6 C5 1.4518(10) . ?
N6 H3 0.886(15) . ?
C2 C3 1.4077(10) . ?
C3 C4 1.3672(10) . ?
C3 H1 0.946(12) . ?
C4 H2 0.971(13) . ?
C5 H4 0.90(2) . ?
C5 H5 0.94(2) . ?
C5 H6 0.88(2) . ?

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
C1 N1 C4 118.59(6) . . ?
C2 N2 N3 109.14(6) . . ?
C2 N2 C1 123.52(6) . . ?
N3 N2 C1 127.34(6) . . ?
N4 N3 N2 104.92(6) . . ?
N3 N4 N5 112.58(6) . . ?
C2 N5 N4 106.06(6) . . ?
C1 N6 C5 121.49(7) . . ?
C1 N6 H3 120.5(9) . . ?
C5 N6 H3 118.0(9) . . ?
N1 C1 N6 123.92(6) . . ?
N1 C1 N2 118.75(6) . . ?
N6 C1 N2 117.33(6) . . ?
N5 C2 N2 107.29(6) . . ?
N5 C2 C3 134.61(7) . . ?
N2 C2 C3 118.10(6) . . ?
C4 C3 C2 115.51(6) . . ?
C4 C3 H1 122.2(7) . . ?
C2 C3 H1 122.3(7) . . ?
C3 C4 N1 125.52(6) . . ?
C3 C4 H2 120.2(7) . . ?
N1 C4 H2 114.2(7) . . ?
N6 C5 H4 113.8(13) . . ?
N6 C5 H5 110.2(12) . . ?
H4 C5 H5 103.8(17) . . ?
N6 C5 H6 109.4(14) . . ?
H4 C5 H6 107(2) . . ?
H5 C5 H6 112.3(18) . . ?

_refine_diff_density_max         0.452
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.052

_shelxl_version_number           2014/6

_shelx_res_file                  
; 
TITL sh3502 in P2(1)/n 
CELL 0.71073   3.95890  10.98270  15.35080  90.0000  93.0963  90.0000 
ZERR    4.00   0.00030   0.00080   0.00120   0.0000   0.0019   0.0000 
LATT 1 
SYMM 0.5-X, 0.5+Y, 0.5-Z 
SFAC C  H  N 
UNIT 20  24  24 
L.S. 4 
BOND $H 
FMAP 2 
PLAN -5 
ACTA 
SIZE 0.038 0.194 0.681 
TEMP -140.600 
WGHT    0.074700    0.063900 
FVAR       0.85540 
N1    3    0.762492    0.080169    0.924391    11.00000    0.02206    0.01761 = 
         0.01741    0.00020    0.00575   -0.00089 
N2    3    1.051520    0.099540    0.797119    11.00000    0.01954    0.01567 = 
         0.01497    0.00075    0.00461    0.00106 
N3    3    1.228966    0.157169    0.735093    11.00000    0.02786    0.01978 = 
         0.02003    0.00282    0.01008    0.00146 
N4    3    1.282008    0.073903    0.677302    11.00000    0.03180    0.02224 = 
         0.02048    0.00208    0.01010    0.00433 
N5    3    1.149102   -0.035318    0.698010    11.00000    0.02863    0.02054 = 
         0.01798   -0.00071    0.00620    0.00353 
N6    3    0.999360    0.266644    0.887972    11.00000    0.03243    0.01494 = 
         0.02137   -0.00177    0.01049   -0.00200 
C1    1    0.933288    0.149755    0.872704    11.00000    0.01895    0.01584 = 
         0.01562   -0.00007    0.00346    0.00083 
C2    1    1.004533   -0.019132    0.773822    11.00000    0.01963    0.01634 = 
         0.01686   -0.00117    0.00195    0.00186 
C3    1    0.828247   -0.094912    0.829750    11.00000    0.02451    0.01677 = 
         0.02118   -0.00100    0.00405   -0.00269 
C4    1    0.715575   -0.039693    0.902545    11.00000    0.02217    0.01868 = 
         0.01980    0.00140    0.00480   -0.00263 
C5    1    0.892791    0.326820    0.966096    11.00000    0.03901    0.02088 = 
         0.02449   -0.00606    0.01065   -0.00103 
H1    2    0.788986   -0.178329    0.817684    11.00000    0.02857 
H2    2    0.589352   -0.085884    0.943805    11.00000    0.02734 
H3    2    1.113626    0.310022    0.850772    11.00000    0.03840 
H4    2    0.988706    0.296070    1.016087    11.00000    0.08079 
H5    2    0.658981    0.314947    0.971868    11.00000    0.07626 
H6    2    0.947386    0.404699    0.964266    11.00000    0.08612 
HKLF 4 
  
REM  sh3502 in P2(1)/n 
REM R1 =  0.0358 for    2242 Fo > 4sig(Fo)  and  0.0435 for all    2657 data 
REM    124 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0747      0.0639 
  
REM Highest difference peak  0.452,  deepest hole -0.184,  1-sigma level  0.052 
Q1    1   0.7657 -0.0628  0.8595  11.00000  0.05    0.45 
Q2    1   0.9144 -0.0599  0.7993  11.00000  0.05    0.42 
Q3    1   1.0872 -0.0302  0.7379  11.00000  0.05    0.40 
Q4    1   0.8783  0.1084  0.8994  11.00000  0.05    0.40 
Q5    1   0.9535  0.2102  0.8786  11.00000  0.05    0.36 
;
_shelx_res_checksum              62235
####################################################################### 
# 
# 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_sh3503
_database_code_depnum_ccdc_archive 'CCDC 1045219'
_audit_update_record             
;
2015-05-18 deposited with the CCDC.
2015-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H3 N5 O'
_chemical_formula_sum            'C4 H3 N5 O'
_chemical_formula_weight         137.11

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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   13.1418(10)
_cell_length_b                   5.9625(5)
_cell_length_c                   6.7680(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     530.33(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    132(2)
_cell_measurement_reflns_used    1728
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      30.80

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_F_000             280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.054
_exptl_absorpt_coefficient_mu    0.135
_shelx_estimated_absorpt_T_min   0.948
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7064
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   'SADABS, BrukerAXS 2010'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      132(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6832
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.100
_diffrn_reflns_theta_max         33.179
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1096
_reflns_number_gt                803
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0531P)²+0.0931P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1096
_refine_ls_number_parameters     70
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.0993
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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
N1 N 1.02446(10) 0.2500 0.2865(2) 0.0188(3) Uani 1 2 d S T P . .
N2 N 0.89648(10) 0.2500 0.05929(18) 0.0160(3) Uani 1 2 d S T P . .
N3 N 0.85212(11) 0.2500 -0.1222(2) 0.0224(3) Uani 1 2 d S T P . .
N4 N 0.75538(11) 0.2500 -0.0893(2) 0.0244(3) Uani 1 2 d S T P . .
N5 N 0.73423(10) 0.2500 0.1089(2) 0.0212(3) Uani 1 2 d S T P . .
O1 O 1.06280(9) 0.2500 -0.04437(18) 0.0257(3) Uani 1 2 d S T P . .
C1 C 1.00262(12) 0.2500 0.0908(2) 0.0171(3) Uani 1 2 d S T P . .
C2 C 0.82319(11) 0.2500 0.1998(2) 0.0158(3) Uani 1 2 d S T P . .
C3 C 0.85267(12) 0.2500 0.4018(2) 0.0177(3) Uani 1 2 d S T P . .
C4 C 0.95352(12) 0.2500 0.4363(2) 0.0176(3) Uani 1 2 d S T P . .
H1 H 0.8009(14) 0.2500 0.505(3) 0.022(5) Uiso 1 2 d S . P . .
H2 H 0.9780(15) 0.2500 0.570(3) 0.024(5) Uiso 1 2 d S . P . .
H3 H 1.0902(17) 0.2500 0.322(3) 0.033(6) Uiso 1 2 d S . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0160(6) 0.0224(6) 0.0181(7) 0.000 -0.0004(5) 0.000
N2 0.0181(6) 0.0193(6) 0.0107(5) 0.000 0.0022(5) 0.000
N3 0.0259(7) 0.0281(7) 0.0133(6) 0.000 -0.0021(5) 0.000
N4 0.0248(7) 0.0293(7) 0.0191(6) 0.000 -0.0046(6) 0.000
N5 0.0172(6) 0.0271(7) 0.0193(6) 0.000 -0.0016(5) 0.000
O1 0.0236(6) 0.0299(6) 0.0235(6) 0.000 0.0117(5) 0.000
C1 0.0170(7) 0.0167(7) 0.0177(7) 0.000 0.0032(6) 0.000
C2 0.0169(7) 0.0167(6) 0.0139(6) 0.000 0.0023(5) 0.000
C3 0.0196(7) 0.0211(7) 0.0123(6) 0.000 0.0016(5) 0.000
C4 0.0216(7) 0.0177(7) 0.0134(6) 0.000 -0.0003(6) 0.000

_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
N1 C1 1.356(2) . ?
N1 C4 1.378(2) . ?
N1 H3 0.90(2) . ?
N2 C2 1.3533(19) . ?
N2 N3 1.3595(18) . ?
N2 C1 1.411(2) . ?
N3 N4 1.291(2) . ?
N4 N5 1.3700(19) . ?
N5 C2 1.321(2) . ?
O1 C1 1.2090(18) . ?
C2 C3 1.422(2) . ?
C3 C4 1.346(2) . ?
C3 H1 0.974(19) . ?
C4 H2 0.96(2) . ?

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
C1 N1 C4 125.18(14) . . ?
C1 N1 H3 117.9(14) . . ?
C4 N1 H3 116.9(14) . . ?
C2 N2 N3 109.23(13) . . ?
C2 N2 C1 126.69(13) . . ?
N3 N2 C1 124.08(12) . . ?
N4 N3 N2 105.46(12) . . ?
N3 N4 N5 111.64(13) . . ?
C2 N5 N4 106.03(13) . . ?
O1 C1 N1 126.93(15) . . ?
O1 C1 N2 122.17(14) . . ?
N1 C1 N2 110.91(13) . . ?
N5 C2 N2 107.64(14) . . ?
N5 C2 C3 133.55(14) . . ?
N2 C2 C3 118.81(14) . . ?
C4 C3 C2 115.81(14) . . ?
C4 C3 H1 124.3(11) . . ?
C2 C3 H1 119.8(11) . . ?
C3 C4 N1 122.60(14) . . ?
C3 C4 H2 119.5(12) . . ?
N1 C4 H2 117.9(12) . . ?

_refine_diff_density_max         0.483
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.066

_shelxl_version_number           2014/6

_shelx_res_file                  
; 
TITL sh3503a in Pnma 
CELL  0.71073  13.1418   5.9625   6.7680   90.000   90.000   90.000 
ZERR    4.00   0.00100   0.00050   0.00060   0.0000   0.0000   0.0000 
LATT 1 
SYMM 1/2-X, -Y, 1/2+Z 
SYMM -X, 1/2+Y, -Z 
SYMM 1/2+X, 1/2-Y, 1/2-Z 
SFAC C  H  N  O 
UNIT 16  12  20  4 
L.S. 10 
BOND $H 
FMAP 2 
PLAN -5 
ACTA 
SIZE 0.054 0.218 0.398 
TEMP -140.500 
WGHT    0.053100    0.093100 
FVAR       0.51402 
N1    3    1.024464    0.250000    0.286509    10.50000    0.01598    0.02240 = 
         0.01809    0.00000   -0.00045    0.00000 
N2    3    0.896480    0.250000    0.059286    10.50000    0.01807    0.01928 = 
         0.01073    0.00000    0.00222    0.00000 
N3    3    0.852119    0.250000   -0.122181    10.50000    0.02590    0.02808 = 
         0.01333    0.00000   -0.00207    0.00000 
N4    3    0.755381    0.250000   -0.089278    10.50000    0.02476    0.02929 = 
         0.01910    0.00000   -0.00463    0.00000 
N5    3    0.734228    0.250000    0.108939    10.50000    0.01722    0.02707 = 
         0.01931    0.00000   -0.00162    0.00000 
O1    4    1.062796    0.250000   -0.044370    10.50000    0.02365    0.02992 = 
         0.02354    0.00000    0.01169    0.00000 
C1    1    1.002622    0.250000    0.090759    10.50000    0.01697    0.01675 = 
         0.01772    0.00000    0.00319    0.00000 
C2    1    0.823190    0.250000    0.199754    10.50000    0.01692    0.01666 = 
         0.01389    0.00000    0.00230    0.00000 
C3    1    0.852667    0.250000    0.401838    10.50000    0.01959    0.02113 = 
         0.01233    0.00000    0.00159    0.00000 
C4    1    0.953520    0.250000    0.436342    10.50000    0.02163    0.01774 = 
         0.01336    0.00000   -0.00032    0.00000 
H1    2    0.800862    0.250000    0.504780    10.50000    0.02215 
H2    2    0.977963    0.250000    0.570451    10.50000    0.02440 
H3    2    1.090219    0.250000    0.322440    10.50000    0.03346 
HKLF 4 1 0 0 1 1 0 0 0 1 0 
  
REM  sh3503a in Pnma 
REM R1 =  0.0429 for     803 Fo > 4sig(Fo)  and  0.0674 for all    1096 data 
REM     70 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0530      0.0923 
  
REM Highest difference peak  0.483,  deepest hole -0.227,  1-sigma level  0.066 
Q1    1   0.8347  0.2500  0.3116  10.50000  0.05    0.48 
Q2    1   0.9008  0.2500  0.4380  10.50000  0.05    0.46 
Q3    1   1.0090  0.2500  0.2032  10.50000  0.05    0.43 
Q4    1   0.9547  0.2500  0.0709  10.50000  0.05    0.43 
Q5    1   0.7777  0.2500  0.1577  10.50000  0.05    0.42 
;
_shelx_res_checksum              49935
