# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_nfzh3po4
_database_code_depnum_ccdc_archive 'CCDC 1877008'
_audit_update_record             
;
2018-11-04 deposited with the CCDC.
2019-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H9 N4 O8 P'
_chemical_formula_weight         296.14

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'
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'
P P 0.1023 0.0942 '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                   4.4913(9)
_cell_length_b                   10.893(2)
_cell_length_c                   12.672(3)
_cell_angle_alpha                106.87(3)
_cell_angle_beta                 99.66(3)
_cell_angle_gamma                92.30(3)
_cell_volume                     582.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2646
_cell_measurement_theta_min      1.710
_cell_measurement_theta_max      28.423

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_F_000             304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.290
_exptl_absorpt_coefficient_mu    0.283
_shelx_estimated_absorpt_T_min   0.858
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS, Bruker ASX'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13757
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.710
_diffrn_reflns_theta_max         28.423
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2900
_reflns_number_gt                2646
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0441P)²+0.1751P] 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         2900
_refine_ls_number_parameters     196
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0812
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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 -0.2287(3) 0.09345(11) 0.70954(10) 0.0271(3) Uani 1 1 d . . . . .
O2 O -0.2092(3) 0.01226(10) 0.62183(11) 0.0464(3) Uani 1 1 d . . . . .
O3 O -0.3959(2) 0.08090(10) 0.77429(10) 0.0346(2) Uani 1 1 d . . . . .
C4 C -0.0474(3) 0.21319(12) 0.74095(11) 0.0212(3) Uani 1 1 d . . . . .
O5 O 0.11839(19) 0.23035(8) 0.66602(7) 0.02017(19) Uani 1 1 d . . . . .
C6 C 0.2551(3) 0.35300(11) 0.71276(10) 0.0191(2) Uani 1 1 d . . . . .
C7 C 0.1747(3) 0.40934(13) 0.81387(11) 0.0239(3) Uani 1 1 d . . . . .
H7 H 0.239677 0.493998 0.862361 0.029 Uiso 1 1 calc R U . . .
C8 C -0.0249(3) 0.31660(13) 0.83226(11) 0.0236(3) Uani 1 1 d . . . . .
H8 H -0.121228 0.325480 0.894993 0.028 Uiso 1 1 calc R U . . .
C9 C 0.4545(3) 0.40111(11) 0.65293(10) 0.0189(2) Uani 1 1 d . . . . .
H9 H 0.541989 0.487872 0.681477 0.023 Uiso 1 1 calc R U . . .
N10 N 0.5148(2) 0.32773(10) 0.56148(9) 0.0185(2) Uani 1 1 d . . . . .
N11 N 0.7075(2) 0.38308(10) 0.51205(9) 0.0190(2) Uani 1 1 d . . . . .
H11 H 0.798(4) 0.4613(18) 0.5450(15) 0.035(5) Uiso 1 1 d . . . . .
C12 C 0.7946(3) 0.31125(11) 0.41688(10) 0.0179(2) Uani 1 1 d . . . . .
O13 O 0.9731(2) 0.36813(8) 0.37555(7) 0.0226(2) Uani 1 1 d . . . . .
N14 N 0.6868(3) 0.18964(11) 0.37389(10) 0.0257(2) Uani 1 1 d . . . . .
H15 H 0.742(4) 0.1468(18) 0.3113(17) 0.038(5) Uiso 1 1 d . . . . .
H14 H 0.563(4) 0.1574(17) 0.4037(14) 0.030(4) Uiso 1 1 d . . . . .
P16 P 0.99547(6) 0.18951(3) 0.09545(2) 0.01687(10) Uani 1 1 d . . . . .
O17 O 1.19251(19) 0.14357(8) 0.01013(7) 0.02076(19) Uani 1 1 d . . . . .
O18 O 1.1842(2) 0.28911(9) 0.19988(8) 0.0260(2) Uani 1 1 d . . . . .
H18 H 1.094(5) 0.307(2) 0.253(2) 0.057(6) Uiso 1 1 d . . . . .
O19 O 0.8610(2) 0.08053(9) 0.13460(8) 0.0235(2) Uani 1 1 d . . . . .
H19 H 0.844(5) 0.008(2) 0.0887(19) 0.053(6) Uiso 1 1 d . . . . .
O20 O 0.7289(2) 0.25807(9) 0.05078(8) 0.0239(2) Uani 1 1 d . . . . .
H20 H 0.571(5) 0.220(2) 0.0364(17) 0.044(5) Uiso 1 1 d . . . . .


_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 O2 1.2221(17) . ?
N1 O3 1.2327(15) . ?
N1 C4 1.4237(17) . ?
C4 C8 1.3464(19) . ?
C4 O5 1.3492(15) . ?
O5 C6 1.3658(15) . ?
C6 C7 1.3657(18) . ?
C6 C9 1.4397(16) . ?
C7 C8 1.4187(18) . ?
C9 N10 1.2805(17) . ?
N10 N11 1.3655(14) . ?
N11 C12 1.3619(16) . ?
C12 O13 1.2609(14) . ?
C12 N14 1.3142(16) . ?
P16 O17 1.4983(10) . ?
P16 O18 1.5371(12) . ?
P16 O20 1.5496(11) . ?
P16 O19 1.5507(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 N1 O3 125.21(12) . . ?
O2 N1 C4 118.54(12) . . ?
O3 N1 C4 116.24(12) . . ?
C8 C4 O5 113.63(11) . . ?
C8 C4 N1 130.19(12) . . ?
O5 C4 N1 116.09(12) . . ?
C4 O5 C6 104.45(10) . . ?
C7 C6 O5 110.82(11) . . ?
C7 C6 C9 130.85(12) . . ?
O5 C6 C9 118.33(11) . . ?
C6 C7 C8 106.51(12) . . ?
C4 C8 C7 104.59(11) . . ?
N10 C9 C6 120.44(11) . . ?
C9 N10 N11 115.53(10) . . ?
C12 N11 N10 119.84(10) . . ?
O13 C12 N14 124.63(12) . . ?
O13 C12 N11 116.65(11) . . ?
N14 C12 N11 118.72(11) . . ?
O17 P16 O18 109.14(6) . . ?
O17 P16 O20 111.54(6) . . ?
O18 P16 O20 106.82(6) . . ?
O17 P16 O19 113.60(6) . . ?
O18 P16 O19 107.41(6) . . ?
O20 P16 O19 108.03(6) . . ?

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 N1 C4 C8 -179.39(15) . . . . ?
O3 N1 C4 C8 1.0(2) . . . . ?
O2 N1 C4 O5 4.37(19) . . . . ?
O3 N1 C4 O5 -175.27(11) . . . . ?
C8 C4 O5 C6 -0.11(14) . . . . ?
N1 C4 O5 C6 176.75(11) . . . . ?
C4 O5 C6 C7 0.04(14) . . . . ?
C4 O5 C6 C9 179.25(11) . . . . ?
O5 C6 C7 C8 0.04(15) . . . . ?
C9 C6 C7 C8 -179.04(13) . . . . ?
O5 C4 C8 C7 0.14(15) . . . . ?
N1 C4 C8 C7 -176.18(13) . . . . ?
C6 C7 C8 C4 -0.10(15) . . . . ?
C7 C6 C9 N10 175.08(13) . . . . ?
O5 C6 C9 N10 -3.95(18) . . . . ?
C6 C9 N10 N11 -179.70(10) . . . . ?
C9 N10 N11 C12 177.39(11) . . . . ?
N10 N11 C12 O13 -179.94(10) . . . . ?
N10 N11 C12 N14 0.83(18) . . . . ?

_refine_diff_density_max         0.317
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.049


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H3PO4'
####################################################################### 
# 
# 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_nfzhclo4
_database_code_depnum_ccdc_archive 'CCDC 1877009'
_audit_update_record             
;
2018-11-04 deposited with the CCDC.
2019-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H27 Cl N16 O21'
_chemical_formula_weight         911.06

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'
Cl Cl 0.1484 0.1585 '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                   7.9863(16)
_cell_length_b                   14.566(3)
_cell_length_c                   16.208(3)
_cell_angle_alpha                77.88(3)
_cell_angle_beta                 80.90(3)
_cell_angle_gamma                87.87(3)
_cell_volume                     1820.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3976
_cell_measurement_theta_min      1.300
_cell_measurement_theta_max      25.073

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.216
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS, BRUKER AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14221
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.300
_diffrn_reflns_theta_max         25.073
_diffrn_reflns_theta_full        25.073
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6451
_reflns_number_gt                3976
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0730P)²] 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         6451
_refine_ls_number_parameters     619
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1408
_refine_ls_wR_factor_gt          0.1198
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.964
_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
N1A N -0.2848(3) -0.12686(18) 0.46140(17) 0.0267(6) Uani 1 1 d . . . . .
O2A O -0.2122(3) -0.16970(15) 0.40875(15) 0.0342(6) Uani 1 1 d . . . . .
O3A O -0.4023(3) -0.15988(16) 0.51906(15) 0.0352(6) Uani 1 1 d . . . . .
C4A C -0.2328(4) -0.0350(2) 0.4601(2) 0.0230(7) Uani 1 1 d . . . . .
O5A O -0.1095(3) 0.00276(14) 0.39572(13) 0.0245(5) Uani 1 1 d . . . . .
C6A C -0.0758(4) 0.0884(2) 0.4129(2) 0.0236(7) Uani 1 1 d . . . . .
C7A C -0.1779(4) 0.1022(2) 0.4849(2) 0.0270(8) Uani 1 1 d . . . . .
H7A H -0.179916 0.155784 0.509926 0.032 Uiso 1 1 calc R U . . .
C8A C -0.2796(4) 0.0218(2) 0.5151(2) 0.0280(8) Uani 1 1 d . . . . .
H8A H -0.364016 0.010113 0.564396 0.034 Uiso 1 1 calc R U . . .
C9A C 0.0522(4) 0.1442(2) 0.3526(2) 0.0246(7) Uani 1 1 d . . . . .
H9A H 0.100709 0.125598 0.301203 0.030 Uiso 1 1 calc R U . . .
N10A N 0.0982(3) 0.21974(18) 0.37091(16) 0.0252(6) Uani 1 1 d . . . . .
N11A N 0.2161(3) 0.27377(19) 0.31246(18) 0.0285(7) Uani 1 1 d . . . . .
H11A H 0.257(4) 0.254(2) 0.268(2) 0.018(8) Uiso 1 1 d . . . . .
C12A C 0.2697(4) 0.3567(2) 0.3278(2) 0.0277(8) Uani 1 1 d . . . . .
O13A O 0.3702(3) 0.40623(15) 0.27180(14) 0.0326(6) Uani 1 1 d . . . . .
N14A N 0.2030(4) 0.3775(2) 0.4018(2) 0.0340(8) Uani 1 1 d . . . . .
H14A H 0.138(4) 0.340(2) 0.437(2) 0.023(10) Uiso 1 1 d . . . . .
H15A H 0.242(4) 0.424(3) 0.416(2) 0.038(11) Uiso 1 1 d . . . . .
N1B N 0.9807(3) 0.35989(19) -0.38589(18) 0.0310(7) Uani 1 1 d . . . . .
O2B O 1.0871(3) 0.42237(18) -0.41532(16) 0.0505(8) Uani 1 1 d . . . . .
O3B O 0.9442(3) 0.30258(16) -0.42606(15) 0.0359(6) Uani 1 1 d . . . . .
C4B C 0.8947(4) 0.3531(2) -0.3013(2) 0.0285(8) Uani 1 1 d . . . . .
O5B O 0.9269(3) 0.42133(15) -0.26083(14) 0.0310(6) Uani 1 1 d . . . . .
C6B C 0.8247(4) 0.3999(2) -0.1824(2) 0.0292(8) Uani 1 1 d . . . . .
C7B C 0.7355(4) 0.3209(2) -0.1765(2) 0.0348(9) Uani 1 1 d . . . . .
H7B H 0.656738 0.291686 -0.128797 0.042 Uiso 1 1 calc R U . . .
C8B C 0.7806(4) 0.2900(2) -0.2536(2) 0.0338(8) Uani 1 1 d . . . . .
H8B H 0.739533 0.236359 -0.268706 0.041 Uiso 1 1 calc R U . . .
C9B C 0.8378(4) 0.4628(2) -0.1263(2) 0.0329(8) Uani 1 1 d . . . . .
H9B H 0.909352 0.516331 -0.143711 0.039 Uiso 1 1 calc R U . . .
N10B N 0.7486(3) 0.44369(19) -0.05134(18) 0.0313(7) Uani 1 1 d . . . . .
N11B N 0.7611(4) 0.5020(2) 0.00236(19) 0.0360(8) Uani 1 1 d . . . . .
H11B H 0.822(5) 0.551(3) -0.015(3) 0.055(13) Uiso 1 1 d . . . . .
C12B C 0.6657(4) 0.4869(2) 0.0822(2) 0.0300(8) Uani 1 1 d . . . . .
O13B O 0.6798(3) 0.54121(16) 0.12973(15) 0.0427(7) Uani 1 1 d . . . . .
N14B N 0.5653(4) 0.4125(2) 0.1028(2) 0.0308(7) Uani 1 1 d . . . . .
H14B H 0.560(4) 0.376(2) 0.067(2) 0.025(9) Uiso 1 1 d . . . . .
H15B H 0.510(5) 0.404(3) 0.151(3) 0.059(14) Uiso 1 1 d . . . . .
N1C N 1.3611(4) 1.21409(19) 0.07160(18) 0.0328(7) Uani 1 1 d . . . . .
O2C O 1.3043(3) 1.25187(16) 0.13124(15) 0.0405(6) Uani 1 1 d . . . . .
O3C O 1.4813(3) 1.24616(18) 0.01555(16) 0.0497(7) Uani 1 1 d . . . . .
C4C C 1.2891(4) 1.1301(2) 0.0638(2) 0.0262(8) Uani 1 1 d . . . . .
O5C O 1.1642(3) 1.09385(15) 0.12910(13) 0.0274(5) Uani 1 1 d . . . . .
C6C C 1.1177(4) 1.0126(2) 0.1093(2) 0.0277(8) Uani 1 1 d . . . . .
C7C C 1.2093(4) 1.0010(2) 0.0336(2) 0.0300(8) Uani 1 1 d . . . . .
H7C H 1.199273 0.950692 0.005782 0.036 Uiso 1 1 calc R U . . .
C8C C 1.3205(4) 1.0767(2) 0.0045(2) 0.0287(8) Uani 1 1 d . . . . .
H8C H 1.401116 1.088071 -0.046241 0.034 Uiso 1 1 calc R U . . .
C9C C 0.9880(4) 0.9587(2) 0.1711(2) 0.0311(8) Uani 1 1 d . . . . .
H9C H 0.939841 0.980148 0.221213 0.037 Uiso 1 1 calc R U . . .
N10C N 0.9401(3) 0.88216(18) 0.15679(17) 0.0272(6) Uani 1 1 d . . . . .
N11C N 0.8189(4) 0.83274(19) 0.21754(19) 0.0327(7) Uani 1 1 d . . . . .
H11C H 0.776(4) 0.857(2) 0.258(2) 0.032(10) Uiso 1 1 d . . . . .
C12C C 0.7604(4) 0.7513(2) 0.2058(2) 0.0286(8) Uani 1 1 d . . . . .
O13C O 0.6454(3) 0.70915(17) 0.26257(15) 0.0440(7) Uani 1 1 d . . . . .
N14C N 0.8245(4) 0.7202(2) 0.13748(19) 0.0306(7) Uani 1 1 d . . . . .
H14C H 0.905(4) 0.753(2) 0.096(2) 0.036(10) Uiso 1 1 d . . . . .
H15C H 0.794(5) 0.669(3) 0.128(2) 0.045(12) Uiso 1 1 d . . . . .
N1D N 0.0697(3) 0.73907(19) 0.93652(17) 0.0284(7) Uani 1 1 d . . . . .
O2D O -0.0314(3) 0.67417(16) 0.96658(15) 0.0392(6) Uani 1 1 d . . . . .
O3D O 0.0982(3) 0.79854(16) 0.97633(15) 0.0362(6) Uani 1 1 d . . . . .
C4D C 0.1547(4) 0.7475(2) 0.8528(2) 0.0253(8) Uani 1 1 d . . . . .
O5D O 0.1200(3) 0.68128(14) 0.81078(13) 0.0262(5) Uani 1 1 d . . . . .
C6D C 0.2238(4) 0.7024(2) 0.7331(2) 0.0254(8) Uani 1 1 d . . . . .
C7D C 0.3173(4) 0.7803(2) 0.7287(2) 0.0291(8) Uani 1 1 d . . . . .
H7D H 0.397730 0.809337 0.681757 0.035 Uiso 1 1 calc R U . . .
C8D C 0.2726(4) 0.8094(2) 0.8063(2) 0.0284(8) Uani 1 1 d . . . . .
H8D H 0.315924 0.861580 0.822760 0.034 Uiso 1 1 calc R U . . .
C9D C 0.2109(4) 0.6401(2) 0.6763(2) 0.0279(8) Uani 1 1 d . . . . .
H9D H 0.136727 0.587691 0.692964 0.033 Uiso 1 1 calc R U . . .
N10D N 0.3031(3) 0.65748(18) 0.60197(17) 0.0267(6) Uani 1 1 d . . . . .
N11D N 0.2901(4) 0.5957(2) 0.55179(18) 0.0284(7) Uani 1 1 d . . . . .
H11D H 0.223(5) 0.547(3) 0.569(3) 0.060(13) Uiso 1 1 d . . . . .
C12D C 0.3811(4) 0.6086(2) 0.4719(2) 0.0265(8) Uani 1 1 d . . . . .
O13D O 0.3621(3) 0.55049(15) 0.42710(14) 0.0311(6) Uani 1 1 d . . . . .
N14D N 0.4854(4) 0.6814(2) 0.4480(2) 0.0343(8) Uani 1 1 d . . . . .
H14D H 0.500(4) 0.721(2) 0.485(2) 0.027(9) Uiso 1 1 d . . . . .
H15D H 0.531(4) 0.691(2) 0.399(2) 0.027(10) Uiso 1 1 d . . . . .
O16 O 0.5777(4) 0.5422(2) 0.29834(19) 0.0448(7) Uani 1 1 d D . . . .
H16A H 0.538(8) 0.502(4) 0.270(4) 0.18(3) Uiso 1 1 d D . . . .
H16B H 0.597(7) 0.6023(14) 0.271(3) 0.11(2) Uiso 1 1 d D . . . .
H16C H 0.500(6) 0.553(5) 0.343(3) 0.15(3) Uiso 1 1 d D . . . .
CL17 Cl 0.44969(11) -0.01792(6) 0.25577(6) 0.0365(2) Uani 1 1 d . . . . .
O18 O 0.3041(4) -0.0753(2) 0.2763(2) 0.0863(11) Uani 1 1 d . . . . .
O19 O 0.3969(3) 0.07375(18) 0.26907(18) 0.0529(8) Uani 1 1 d . . . . .
O20 O 0.5707(3) -0.0522(2) 0.31075(17) 0.0638(9) Uani 1 1 d . . . . .
O21 O 0.5278(4) -0.0108(2) 0.16991(17) 0.0701(10) Uani 1 1 d . . . . .


_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
N1A O2A 1.222(3) . ?
N1A O3A 1.246(3) . ?
N1A C4A 1.411(4) . ?
C4A C8A 1.343(4) . ?
C4A O5A 1.354(4) . ?
O5A C6A 1.379(3) . ?
C6A C7A 1.361(4) . ?
C6A C9A 1.440(4) . ?
C7A C8A 1.405(4) . ?
C9A N10A 1.279(4) . ?
N10A N11A 1.365(4) . ?
N11A C12A 1.380(4) . ?
C12A O13A 1.235(4) . ?
C12A N14A 1.323(4) . ?
N1B O3B 1.229(3) . ?
N1B O2B 1.235(3) . ?
N1B C4B 1.419(4) . ?
C4B C8B 1.347(5) . ?
C4B O5B 1.352(4) . ?
O5B C6B 1.379(4) . ?
C6B C7B 1.353(5) . ?
C6B C9B 1.438(4) . ?
C7B C8B 1.406(5) . ?
C9B N10B 1.288(4) . ?
N10B N11B 1.355(4) . ?
N11B C12B 1.373(4) . ?
C12B O13B 1.233(4) . ?
C12B N14B 1.326(4) . ?
N1C O2C 1.228(3) . ?
N1C O3C 1.243(4) . ?
N1C C4C 1.408(4) . ?
C4C C8C 1.347(4) . ?
C4C O5C 1.365(4) . ?
O5C C6C 1.369(4) . ?
C6C C7C 1.364(4) . ?
C6C C9C 1.447(5) . ?
C7C C8C 1.395(5) . ?
C9C N10C 1.270(4) . ?
N10C N11C 1.370(4) . ?
N11C C12C 1.352(4) . ?
C12C O13C 1.267(4) . ?
C12C N14C 1.306(4) . ?
N1D O3D 1.230(3) . ?
N1D O2D 1.234(3) . ?
N1D C4D 1.401(4) . ?
C4D C8D 1.349(4) . ?
C4D O5D 1.351(3) . ?
O5D C6D 1.376(4) . ?
C6D C7D 1.364(4) . ?
C6D C9D 1.440(4) . ?
C7D C8D 1.400(4) . ?
C9D N10D 1.289(4) . ?
N10D N11D 1.351(3) . ?
N11D C12D 1.361(4) . ?
C12D O13D 1.252(3) . ?
C12D N14D 1.326(4) . ?
CL17 O18 1.412(3) . ?
CL17 O21 1.416(3) . ?
CL17 O20 1.424(3) . ?
CL17 O19 1.434(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
O2A N1A O3A 124.1(3) . . ?
O2A N1A C4A 119.6(3) . . ?
O3A N1A C4A 116.3(3) . . ?
C8A C4A O5A 112.6(3) . . ?
C8A C4A N1A 130.7(3) . . ?
O5A C4A N1A 116.7(3) . . ?
C4A O5A C6A 104.6(2) . . ?
C7A C6A O5A 110.3(3) . . ?
C7A C6A C9A 133.7(3) . . ?
O5A C6A C9A 115.9(3) . . ?
C6A C7A C8A 106.6(3) . . ?
C4A C8A C7A 105.9(3) . . ?
N10A C9A C6A 117.4(3) . . ?
C9A N10A N11A 117.2(3) . . ?
N10A N11A C12A 120.2(3) . . ?
O13A C12A N14A 125.5(3) . . ?
O13A C12A N11A 118.5(3) . . ?
N14A C12A N11A 115.9(3) . . ?
O3B N1B O2B 123.5(3) . . ?
O3B N1B C4B 117.6(3) . . ?
O2B N1B C4B 118.9(3) . . ?
C8B C4B O5B 113.0(3) . . ?
C8B C4B N1B 130.5(3) . . ?
O5B C4B N1B 116.4(3) . . ?
C4B O5B C6B 104.5(2) . . ?
C7B C6B O5B 110.0(3) . . ?
C7B C6B C9B 134.8(3) . . ?
O5B C6B C9B 115.2(3) . . ?
C6B C7B C8B 107.6(3) . . ?
C4B C8B C7B 104.8(3) . . ?
N10B C9B C6B 117.2(3) . . ?
C9B N10B N11B 117.7(3) . . ?
N10B N11B C12B 120.5(3) . . ?
O13B C12B N14B 124.7(3) . . ?
O13B C12B N11B 119.1(3) . . ?
N14B C12B N11B 116.2(3) . . ?
O2C N1C O3C 123.5(3) . . ?
O2C N1C C4C 120.1(3) . . ?
O3C N1C C4C 116.4(3) . . ?
C8C C4C O5C 112.5(3) . . ?
C8C C4C N1C 132.6(3) . . ?
O5C C4C N1C 114.9(3) . . ?
C4C O5C C6C 104.5(2) . . ?
C7C C6C O5C 110.1(3) . . ?
C7C C6C C9C 134.6(3) . . ?
O5C C6C C9C 115.3(3) . . ?
C6C C7C C8C 107.5(3) . . ?
C4C C8C C7C 105.3(3) . . ?
N10C C9C C6C 118.3(3) . . ?
C9C N10C N11C 116.5(3) . . ?
C12C N11C N10C 119.6(3) . . ?
O13C C12C N14C 123.7(3) . . ?
O13C C12C N11C 117.4(3) . . ?
N14C C12C N11C 118.9(3) . . ?
O3D N1D O2D 123.0(3) . . ?
O3D N1D C4D 117.7(3) . . ?
O2D N1D C4D 119.3(3) . . ?
C8D C4D O5D 112.8(3) . . ?
C8D C4D N1D 131.0(3) . . ?
O5D C4D N1D 116.2(3) . . ?
C4D O5D C6D 104.8(2) . . ?
C7D C6D O5D 109.9(3) . . ?
C7D C6D C9D 134.8(3) . . ?
O5D C6D C9D 115.3(3) . . ?
C6D C7D C8D 107.3(3) . . ?
C4D C8D C7D 105.2(3) . . ?
N10D C9D C6D 118.0(3) . . ?
C9D N10D N11D 115.8(3) . . ?
N10D N11D C12D 120.1(3) . . ?
O13D C12D N14D 125.1(3) . . ?
O13D C12D N11D 117.8(3) . . ?
N14D C12D N11D 117.1(3) . . ?
O18 CL17 O21 112.3(2) . . ?
O18 CL17 O20 111.1(2) . . ?
O21 CL17 O20 109.00(17) . . ?
O18 CL17 O19 107.35(18) . . ?
O21 CL17 O19 109.16(18) . . ?
O20 CL17 O19 107.82(17) . . ?

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
O2A N1A C4A C8A -172.4(3) . . . . ?
O3A N1A C4A C8A 6.1(5) . . . . ?
O2A N1A C4A O5A 4.0(4) . . . . ?
O3A N1A C4A O5A -177.6(3) . . . . ?
C8A C4A O5A C6A 0.9(3) . . . . ?
N1A C4A O5A C6A -176.1(3) . . . . ?
C4A O5A C6A C7A -0.8(3) . . . . ?
C4A O5A C6A C9A -179.6(3) . . . . ?
O5A C6A C7A C8A 0.5(4) . . . . ?
C9A C6A C7A C8A 178.9(4) . . . . ?
O5A C4A C8A C7A -0.7(4) . . . . ?
N1A C4A C8A C7A 175.8(3) . . . . ?
C6A C7A C8A C4A 0.1(4) . . . . ?
C7A C6A C9A N10A 8.3(6) . . . . ?
O5A C6A C9A N10A -173.4(3) . . . . ?
C6A C9A N10A N11A -178.2(3) . . . . ?
C9A N10A N11A C12A 179.3(3) . . . . ?
N10A N11A C12A O13A -176.4(3) . . . . ?
N10A N11A C12A N14A 1.4(5) . . . . ?
O3B N1B C4B C8B 3.4(5) . . . . ?
O2B N1B C4B C8B -176.7(4) . . . . ?
O3B N1B C4B O5B -174.9(3) . . . . ?
O2B N1B C4B O5B 5.0(4) . . . . ?
C8B C4B O5B C6B -0.5(4) . . . . ?
N1B C4B O5B C6B 178.1(3) . . . . ?
C4B O5B C6B C7B 0.4(4) . . . . ?
C4B O5B C6B C9B 179.3(3) . . . . ?
O5B C6B C7B C8B -0.2(4) . . . . ?
C9B C6B C7B C8B -178.8(4) . . . . ?
O5B C4B C8B C7B 0.4(4) . . . . ?
N1B C4B C8B C7B -177.9(3) . . . . ?
C6B C7B C8B C4B -0.1(4) . . . . ?
C7B C6B C9B N10B 0.8(6) . . . . ?
O5B C6B C9B N10B -177.8(3) . . . . ?
C6B C9B N10B N11B 179.4(3) . . . . ?
C9B N10B N11B C12B 178.2(3) . . . . ?
N10B N11B C12B O13B 180.0(3) . . . . ?
N10B N11B C12B N14B 1.0(5) . . . . ?
O2C N1C C4C C8C 176.9(4) . . . . ?
O3C N1C C4C C8C -2.8(6) . . . . ?
O2C N1C C4C O5C -4.0(4) . . . . ?
O3C N1C C4C O5C 176.3(3) . . . . ?
C8C C4C O5C C6C 0.9(4) . . . . ?
N1C C4C O5C C6C -178.4(3) . . . . ?
C4C O5C C6C C7C -1.1(4) . . . . ?
C4C O5C C6C C9C 178.3(3) . . . . ?
O5C C6C C7C C8C 1.0(4) . . . . ?
C9C C6C C7C C8C -178.3(4) . . . . ?
O5C C4C C8C C7C -0.3(4) . . . . ?
N1C C4C C8C C7C 178.8(4) . . . . ?
C6C C7C C8C C4C -0.5(4) . . . . ?
C7C C6C C9C N10C -0.2(6) . . . . ?
O5C C6C C9C N10C -179.5(3) . . . . ?
C6C C9C N10C N11C 179.1(3) . . . . ?
C9C N10C N11C C12C 179.1(3) . . . . ?
N10C N11C C12C O13C -178.3(3) . . . . ?
N10C N11C C12C N14C 1.9(5) . . . . ?
O3D N1D C4D C8D 3.1(5) . . . . ?
O2D N1D C4D C8D -178.1(3) . . . . ?
O3D N1D C4D O5D -179.7(3) . . . . ?
O2D N1D C4D O5D -0.9(4) . . . . ?
C8D C4D O5D C6D 0.6(4) . . . . ?
N1D C4D O5D C6D -177.2(3) . . . . ?
C4D O5D C6D C7D -0.6(3) . . . . ?
C4D O5D C6D C9D 179.4(3) . . . . ?
O5D C6D C7D C8D 0.5(4) . . . . ?
C9D C6D C7D C8D -179.6(4) . . . . ?
O5D C4D C8D C7D -0.3(4) . . . . ?
N1D C4D C8D C7D 177.0(3) . . . . ?
C6D C7D C8D C4D -0.1(4) . . . . ?
C7D C6D C9D N10D -1.2(6) . . . . ?
O5D C6D C9D N10D 178.8(3) . . . . ?
C6D C9D N10D N11D 178.3(3) . . . . ?
C9D N10D N11D C12D 179.3(3) . . . . ?
N10D N11D C12D O13D -178.5(3) . . . . ?
N10D N11D C12D N14D 2.4(5) . . . . ?

_refine_diff_density_max         0.511
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.065


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: HClO4'
####################################################################### 
# 
# 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_NFZ_PPA
_database_code_depnum_ccdc_archive 'CCDC 1877010'
_audit_update_record             
;
2018-11-04 deposited with the CCDC.
2019-01-11 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H12 N4 O6'
_chemical_formula_weight         272.22

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                   15.801(3)
_cell_length_b                   12.931(3)
_cell_length_c                   24.475(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.04(3)
_cell_angle_gamma                90
_cell_volume                     5000.8(17)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7474
_cell_measurement_theta_min      1.289
_cell_measurement_theta_max      28.308

_exptl_crystal_description       chunk
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_F_000             2272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.123
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS, Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            92691
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.289
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12422
_reflns_number_gt                7474
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0522P)²+0.5579P] 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         12422
_refine_ls_number_parameters     705
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_ref         0.1264
_refine_ls_wR_factor_gt          0.1037
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
N1A N -0.17675(10) 0.40334(13) 0.32899(6) 0.0359(4) Uani 1 1 d . . . . .
N1B N 0.76718(10) 0.34520(12) 0.88377(6) 0.0349(4) Uani 1 1 d . . . . .
N1C N 0.32979(9) 0.39611(12) 0.38884(6) 0.0336(4) Uani 1 1 d . . . . .
N1D N 1.26089(10) 0.33109(12) -0.17131(6) 0.0336(4) Uani 1 1 d . . . . .
O2A O -0.23910(8) 0.38834(12) 0.35823(6) 0.0448(4) Uani 1 1 d . . . . .
O2B O 0.82896(8) 0.33749(11) 0.85319(6) 0.0436(4) Uani 1 1 d . . . . .
O2C O 0.26564(8) 0.40091(12) 0.36020(6) 0.0438(4) Uani 1 1 d . . . . .
O2D O 1.32407(8) 0.33230(11) -0.14195(6) 0.0410(3) Uani 1 1 d . . . . .
O3A O -0.17918(9) 0.41922(13) 0.27932(6) 0.0545(4) Uani 1 1 d . . . . .
O3B O 0.77122(9) 0.34972(12) 0.93405(5) 0.0503(4) Uani 1 1 d . . . . .
O3C O 0.32993(9) 0.39051(12) 0.43919(5) 0.0456(4) Uani 1 1 d . . . . .
O3D O 1.26215(9) 0.32435(12) -0.22150(5) 0.0480(4) Uani 1 1 d . . . . .
C4A C -0.09473(11) 0.40292(14) 0.35324(7) 0.0282(4) Uani 1 1 d . . . . .
C4B C 0.68489(11) 0.34911(14) 0.86032(7) 0.0286(4) Uani 1 1 d . . . . .
C4C C 0.41043(10) 0.39720(14) 0.36305(7) 0.0269(4) Uani 1 1 d . . . . .
C4D C 1.17927(11) 0.33833(14) -0.14699(7) 0.0276(4) Uani 1 1 d . . . . .
O5A O -0.09266(7) 0.38816(9) 0.40774(5) 0.0280(3) Uani 1 1 d . . . . .
O5B O 0.68164(7) 0.34176(9) 0.80535(4) 0.0281(3) Uani 1 1 d . . . . .
O5C O 0.41019(7) 0.40092(9) 0.30800(4) 0.0272(3) Uani 1 1 d . . . . .
O5D O 1.17831(7) 0.34586(9) -0.09183(4) 0.0272(3) Uani 1 1 d . . . . .
C6A C -0.00830(10) 0.39396(13) 0.42165(7) 0.0247(4) Uani 1 1 d . . . . .
C6B C 0.59740(10) 0.35143(13) 0.79243(7) 0.0250(4) Uani 1 1 d . . . . .
C6C C 0.49430(10) 0.40098(13) 0.29334(7) 0.0244(4) Uani 1 1 d . . . . .
C6D C 1.09397(10) 0.35362(13) -0.07822(7) 0.0249(4) Uani 1 1 d . . . . .
C7A C 0.03947(11) 0.41107(14) 0.37617(7) 0.0288(4) Uani 1 1 d . . . . .
H7A H 0.099305 0.417755 0.374792 0.035 Uiso 1 1 calc R U . . .
C7B C 0.55091(11) 0.36511(14) 0.83875(7) 0.0293(4) Uani 1 1 d . . . . .
H7B H 0.491295 0.373824 0.840765 0.035 Uiso 1 1 calc R U . . .
C7C C 0.54427(10) 0.39754(14) 0.33888(7) 0.0271(4) Uani 1 1 d . . . . .
H7C H 0.604373 0.396952 0.339769 0.033 Uiso 1 1 calc R U . . .
C7D C 1.04530(11) 0.35009(14) -0.12429(7) 0.0285(4) Uani 1 1 d . . . . .
H7D H 0.985298 0.353557 -0.125892 0.034 Uiso 1 1 calc R U . . .
C8A C -0.01702(11) 0.41697(14) 0.33147(7) 0.0312(4) Uani 1 1 d . . . . .
H8A H -0.003298 0.428344 0.294167 0.037 Uiso 1 1 calc R U . . .
C8B C 0.60784(11) 0.36392(14) 0.88311(7) 0.0307(4) Uani 1 1 d . . . . .
H8B H 0.594925 0.371803 0.920788 0.037 Uiso 1 1 calc R U . . .
C8C C 0.48941(11) 0.39502(14) 0.38438(7) 0.0297(4) Uani 1 1 d . . . . .
H8C H 0.504678 0.392355 0.421904 0.036 Uiso 1 1 calc R U . . .
C8D C 1.10094(11) 0.34030(14) -0.16913(7) 0.0305(4) Uani 1 1 d . . . . .
H8D H 1.086421 0.336031 -0.206734 0.037 Uiso 1 1 calc R U . . .
C9A C 0.00880(10) 0.38043(13) 0.47889(7) 0.0257(4) Uani 1 1 d . . . . .
H9A H -0.036519 0.370752 0.503857 0.031 Uiso 1 1 calc R U . . .
C9B C 0.57892(10) 0.34555(13) 0.73481(7) 0.0260(4) Uani 1 1 d . . . . .
H9B H 0.623446 0.339301 0.708961 0.031 Uiso 1 1 calc R U . . .
C9C C 0.50932(10) 0.40408(13) 0.23529(7) 0.0264(4) Uani 1 1 d . . . . .
H9C H 0.463240 0.402483 0.210360 0.032 Uiso 1 1 calc R U . . .
C9D C 1.07757(10) 0.36453(13) -0.02074(7) 0.0261(4) Uani 1 1 d . . . . .
H9D H 1.123072 0.366430 0.004627 0.031 Uiso 1 1 calc R U . . .
N10A N 0.08563(8) 0.38147(11) 0.49617(5) 0.0245(3) Uani 1 1 d . . . . .
N10B N 0.50149(8) 0.34888(11) 0.71889(5) 0.0246(3) Uani 1 1 d . . . . .
N10C N 0.58584(8) 0.40901(11) 0.21766(5) 0.0257(3) Uani 1 1 d . . . . .
N10D N 1.00063(9) 0.37169(11) -0.00401(5) 0.0249(3) Uani 1 1 d . . . . .
N11A N 0.09484(9) 0.36860(12) 0.55116(6) 0.0282(3) Uani 1 1 d . . . . .
H11A H 0.049381 0.359064 0.573723 0.044(6) Uiso 1 1 d R . . . .
N11B N 0.49027(9) 0.34376(12) 0.66371(6) 0.0291(3) Uani 1 1 d . . . . .
H11B H 0.536197 0.345203 0.638668 0.043(6) Uiso 1 1 d R . . . .
N11C N 0.59441(8) 0.40832(12) 0.16220(6) 0.0297(3) Uani 1 1 d . . . . .
H11C H 0.548174 0.404982 0.138008 0.057(7) Uiso 1 1 d R . . . .
N11D N 0.99095(9) 0.38034(11) 0.05118(5) 0.0271(3) Uani 1 1 d . . . . .
H11D H 1.036724 0.385579 0.075212 0.055(6) Uiso 1 1 d R . . . .
C12A C 0.17330(10) 0.37005(13) 0.57460(7) 0.0252(4) Uani 1 1 d . . . . .
C12B C 0.41164(10) 0.36038(14) 0.64151(7) 0.0264(4) Uani 1 1 d . . . . .
C12C C 0.67323(10) 0.41390(14) 0.13902(7) 0.0259(4) Uani 1 1 d . . . . .
C12D C 0.91215(10) 0.39450(13) 0.07336(7) 0.0243(4) Uani 1 1 d . . . . .
O13A O 0.17874(7) 0.36444(10) 0.62559(5) 0.0310(3) Uani 1 1 d . . . . .
O13B O 0.40568(7) 0.36728(11) 0.59063(5) 0.0348(3) Uani 1 1 d . . . . .
O13C O 0.67906(7) 0.40999(10) 0.08811(5) 0.0317(3) Uani 1 1 d . . . . .
O13D O 0.90598(7) 0.40695(10) 0.12390(5) 0.0283(3) Uani 1 1 d . . . . .
N14A N 0.23967(9) 0.37671(13) 0.54190(6) 0.0352(4) Uani 1 1 d . . . . .
H14A H 0.234065 0.382085 0.505696 0.053(7) Uiso 1 1 d R . . . .
H14B H 0.289415 0.376435 0.556576 0.050(6) Uiso 1 1 d R . . . .
N14B N 0.34645(9) 0.36848(12) 0.67523(6) 0.0339(4) Uani 1 1 d . . . . .
H14C H 0.354674 0.360237 0.711000 0.049(6) Uiso 1 1 d R . . . .
H14D H 0.296584 0.370517 0.661690 0.048(6) Uiso 1 1 d R . . . .
N14C N 0.73930(9) 0.42484(12) 0.17218(6) 0.0312(4) Uani 1 1 d . . . . .
H14F H 0.790887 0.422447 0.156913 0.048(6) Uiso 1 1 d R . . . .
H14E H 0.730147 0.422547 0.208423 0.035(5) Uiso 1 1 d R . . . .
N14D N 0.84655(9) 0.39577(12) 0.03949(6) 0.0326(4) Uani 1 1 d . . . . .
H14H H 0.854874 0.383086 0.003994 0.043(6) Uiso 1 1 d R . . . .
H14G H 0.794664 0.401696 0.053594 0.041(6) Uiso 1 1 d R . . . .
O15A O 0.05533(8) 0.32310(11) 0.69495(5) 0.0386(3) Uani 1 1 d . . . . .
H15A H 0.095537 0.338987 0.666836 0.082(9) Uiso 1 1 d R . . . .
O15B O 0.53204(8) 0.37843(11) 0.52019(5) 0.0390(3) Uani 1 1 d . . . . .
H15B H 0.491555 0.374159 0.548659 0.083(9) Uiso 1 1 d R . . . .
O15C O 0.55599(8) 0.37583(11) 0.01747(5) 0.0397(3) Uani 1 1 d . . . . .
H15C H 0.594616 0.385392 0.045723 0.062(7) Uiso 1 1 d R . . . .
O15D O 1.03122(8) 0.43370(11) 0.19425(5) 0.0388(3) Uani 1 1 d . . . . .
H15D H 0.989123 0.422626 0.164172 0.062(7) Uiso 1 1 d R . . . .
C16A C -0.02247(11) 0.32472(14) 0.67349(7) 0.0301(4) Uani 1 1 d . . . . .
C16B C 0.60940(11) 0.36962(14) 0.54079(8) 0.0313(4) Uani 1 1 d . . . . .
C16C C 0.47803(11) 0.38041(15) 0.03765(8) 0.0319(4) Uani 1 1 d . . . . .
C16D C 1.10830(11) 0.41541(15) 0.17467(7) 0.0328(4) Uani 1 1 d . . . . .
O17A O -0.03585(8) 0.33729(10) 0.62524(5) 0.0369(3) Uani 1 1 d . . . . .
O17B O 0.62281(8) 0.36264(11) 0.58956(5) 0.0419(3) Uani 1 1 d . . . . .
O17C O 0.46374(8) 0.39965(12) 0.08516(5) 0.0464(4) Uani 1 1 d . . . . .
O17D O 1.12215(8) 0.40050(12) 0.12675(5) 0.0479(4) Uani 1 1 d . . . . .
C18A C -0.09053(12) 0.30857(17) 0.71506(8) 0.0418(5) Uani 1 1 d . . . . .
H18A H -0.080255 0.355049 0.746510 0.050 Uiso 1 1 calc R U . . .
H18B H -0.087787 0.236445 0.728514 0.050 Uiso 1 1 calc R U . . .
C18B C 0.67711(12) 0.36956(17) 0.49835(8) 0.0410(5) Uani 1 1 d . . . . .
H18C H 0.669843 0.431088 0.474737 0.049 Uiso 1 1 calc R U . . .
H18D H 0.670348 0.307442 0.475115 0.049 Uiso 1 1 calc R U . . .
C18C C 0.41048(12) 0.35916(16) -0.00413(8) 0.0386(5) Uani 1 1 d . . . . .
H18E H 0.412044 0.284949 -0.014030 0.046 Uiso 1 1 calc R U . . .
H18F H 0.422729 0.399658 -0.037527 0.046 Uiso 1 1 calc R U . . .
C18D C 1.17559(12) 0.41536(19) 0.21757(8) 0.0460(5) Uani 1 1 d . . . . .
H18G H 1.160937 0.363256 0.245656 0.055 Uiso 1 1 calc R U . . .
H18H H 1.176417 0.483912 0.235580 0.055 Uiso 1 1 calc R U . . .
C19A C -0.17848(12) 0.32920(18) 0.69240(9) 0.0479(6) Uani 1 1 d . . . . .
H19B H -0.182713 0.401720 0.681095 0.072 Uiso 1 1 calc R U . . .
H19A H -0.220779 0.314914 0.720679 0.072 Uiso 1 1 calc R U . . .
H19C H -0.188664 0.284274 0.660831 0.072 Uiso 1 1 calc R U . . .
C19B C 0.76586(12) 0.37036(19) 0.52186(9) 0.0489(6) Uani 1 1 d . . . . .
H19E H 0.774077 0.433311 0.543518 0.073 Uiso 1 1 calc R U . . .
H19D H 0.807152 0.368702 0.492013 0.073 Uiso 1 1 calc R U . . .
H19F H 0.773731 0.309592 0.545239 0.073 Uiso 1 1 calc R U . . .
C19C C 0.32243(12) 0.38621(19) 0.01601(9) 0.0518(6) Uani 1 1 d . . . . .
H19I H 0.309785 0.346154 0.048997 0.078 Uiso 1 1 calc R U . . .
H19G H 0.280878 0.369740 -0.012429 0.078 Uiso 1 1 calc R U . . .
H19H H 0.319768 0.460221 0.024463 0.078 Uiso 1 1 calc R U . . .
C19D C 1.26289(12) 0.39218(18) 0.19605(9) 0.0472(5) Uani 1 1 d . . . . .
H19J H 1.262779 0.324476 0.178054 0.071 Uiso 1 1 calc R U . . .
H19L H 1.303333 0.391442 0.226425 0.071 Uiso 1 1 calc R U . . .
H19K H 1.279343 0.445539 0.169683 0.071 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
N1A O2A 1.2335(19) . ?
N1A O3A 1.2334(19) . ?
N1A C4A 1.425(2) . ?
N1B O3B 1.2336(19) . ?
N1B O2B 1.2347(19) . ?
N1B C4B 1.422(2) . ?
N1C O2C 1.2337(19) . ?
N1C O3C 1.2343(19) . ?
N1C C4C 1.422(2) . ?
N1D O2D 1.2298(19) . ?
N1D O3D 1.2318(19) . ?
N1D C4D 1.424(2) . ?
C4A O5A 1.348(2) . ?
C4A C8A 1.351(2) . ?
C4B O5B 1.350(2) . ?
C4B C8B 1.353(2) . ?
C4C O5C 1.3482(19) . ?
C4C C8C 1.353(2) . ?
C4D C8D 1.351(2) . ?
C4D O5D 1.3539(19) . ?
O5A C6A 1.3776(18) . ?
O5B C6B 1.3736(19) . ?
O5C C6C 1.3768(18) . ?
O5D C6D 1.3775(19) . ?
C6A C7A 1.363(2) . ?
C6A C9A 1.437(2) . ?
C6B C7B 1.363(2) . ?
C6B C9B 1.442(2) . ?
C6C C7C 1.366(2) . ?
C6C C9C 1.441(2) . ?
C6D C7D 1.365(2) . ?
C6D C9D 1.438(2) . ?
C7A C8A 1.414(2) . ?
C7B C8B 1.410(2) . ?
C7C C8C 1.412(2) . ?
C7D C8D 1.412(2) . ?
C9A N10A 1.286(2) . ?
C9B N10B 1.285(2) . ?
C9C N10C 1.286(2) . ?
C9D N10D 1.286(2) . ?
N10A N11A 1.3638(18) . ?
N10B N11B 1.3636(19) . ?
N10C N11C 1.3643(18) . ?
N10D N11D 1.3641(18) . ?
N11A C12A 1.366(2) . ?
N11B C12B 1.373(2) . ?
N11C C12C 1.371(2) . ?
N11D C12D 1.371(2) . ?
C12A O13A 1.2530(19) . ?
C12A N14A 1.323(2) . ?
C12B O13B 1.252(2) . ?
C12B N14B 1.324(2) . ?
C12C O13C 1.2507(19) . ?
C12C N14C 1.329(2) . ?
C12D O13D 1.2512(19) . ?
C12D N14D 1.327(2) . ?
O15A C16A 1.337(2) . ?
O15B C16B 1.327(2) . ?
O15C C16C 1.329(2) . ?
O15D C16D 1.330(2) . ?
C16A O17A 1.211(2) . ?
C16A C18A 1.495(2) . ?
C16B O17B 1.215(2) . ?
C16B C18B 1.492(2) . ?
C16C O17C 1.211(2) . ?
C16C C18C 1.503(2) . ?
C16D O17D 1.209(2) . ?
C16D C18D 1.494(3) . ?
C18A C19A 1.519(3) . ?
C18B C19B 1.515(3) . ?
C18C C19C 1.517(3) . ?
C18D C19D 1.507(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
O2A N1A O3A 125.01(16) . . ?
O2A N1A C4A 118.96(15) . . ?
O3A N1A C4A 116.04(16) . . ?
O3B N1B O2B 124.62(15) . . ?
O3B N1B C4B 116.60(16) . . ?
O2B N1B C4B 118.78(15) . . ?
O2C N1C O3C 124.83(15) . . ?
O2C N1C C4C 118.90(15) . . ?
O3C N1C C4C 116.27(15) . . ?
O2D N1D O3D 124.74(15) . . ?
O2D N1D C4D 119.35(15) . . ?
O3D N1D C4D 115.90(15) . . ?
O5A C4A C8A 112.82(15) . . ?
O5A C4A N1A 115.74(15) . . ?
C8A C4A N1A 131.42(16) . . ?
O5B C4B C8B 112.78(15) . . ?
O5B C4B N1B 115.72(15) . . ?
C8B C4B N1B 131.41(16) . . ?
O5C C4C C8C 112.86(15) . . ?
O5C C4C N1C 116.22(15) . . ?
C8C C4C N1C 130.91(16) . . ?
C8D C4D O5D 112.81(15) . . ?
C8D C4D N1D 131.57(16) . . ?
O5D C4D N1D 115.61(15) . . ?
C4A O5A C6A 105.06(13) . . ?
C4B O5B C6B 105.02(13) . . ?
C4C O5C C6C 104.97(13) . . ?
C4D O5D C6D 104.94(13) . . ?
C7A C6A O5A 110.07(14) . . ?
C7A C6A C9A 135.37(16) . . ?
O5A C6A C9A 114.56(14) . . ?
C7B C6B O5B 110.07(14) . . ?
C7B C6B C9B 135.36(16) . . ?
O5B C6B C9B 114.57(14) . . ?
C7C C6C O5C 110.17(14) . . ?
C7C C6C C9C 135.21(15) . . ?
O5C C6C C9C 114.62(14) . . ?
C7D C6D O5D 110.02(14) . . ?
C7D C6D C9D 135.21(15) . . ?
O5D C6D C9D 114.76(14) . . ?
C6A C7A C8A 106.92(15) . . ?
C6B C7B C8B 107.18(15) . . ?
C6C C7C C8C 106.82(15) . . ?
C6D C7D C8D 107.11(15) . . ?
C4A C8A C7A 105.13(15) . . ?
C4B C8B C7B 104.95(15) . . ?
C4C C8C C7C 105.18(15) . . ?
C4D C8D C7D 105.11(15) . . ?
N10A C9A C6A 119.77(15) . . ?
N10B C9B C6B 119.16(16) . . ?
N10C C9C C6C 119.20(15) . . ?
N10D C9D C6D 119.32(16) . . ?
C9A N10A N11A 115.07(14) . . ?
C9B N10B N11B 114.97(14) . . ?
C9C N10C N11C 115.32(14) . . ?
C9D N10D N11D 115.32(14) . . ?
N10A N11A C12A 120.60(14) . . ?
N10B N11B C12B 120.10(14) . . ?
N10C N11C C12C 120.15(14) . . ?
N10D N11D C12D 120.36(14) . . ?
O13A C12A N14A 123.55(15) . . ?
O13A C12A N11A 118.63(15) . . ?
N14A C12A N11A 117.82(15) . . ?
O13B C12B N14B 123.79(16) . . ?
O13B C12B N11B 118.19(15) . . ?
N14B C12B N11B 118.02(15) . . ?
O13C C12C N14C 123.65(15) . . ?
O13C C12C N11C 118.54(15) . . ?
N14C C12C N11C 117.80(15) . . ?
O13D C12D N14D 123.69(15) . . ?
O13D C12D N11D 118.68(15) . . ?
N14D C12D N11D 117.62(15) . . ?
O17A C16A O15A 123.05(16) . . ?
O17A C16A C18A 123.85(17) . . ?
O15A C16A C18A 113.09(16) . . ?
O17B C16B O15B 122.65(16) . . ?
O17B C16B C18B 124.00(17) . . ?
O15B C16B C18B 113.35(16) . . ?
O17C C16C O15C 122.67(16) . . ?
O17C C16C C18C 123.94(17) . . ?
O15C C16C C18C 113.40(16) . . ?
O17D C16D O15D 122.98(16) . . ?
O17D C16D C18D 123.57(17) . . ?
O15D C16D C18D 113.46(16) . . ?
C16A C18A C19A 112.66(17) . . ?
C16B C18B C19B 113.55(17) . . ?
C16C C18C C19C 112.82(16) . . ?
C16D C18D C19D 113.93(17) . . ?

_refine_diff_density_max         0.176
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.059


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: propanoic acid'
