# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_LQ191211_1_a
_database_code_depnum_ccdc_archive 'CCDC 1980541'
loop_
_audit_author_name
_audit_author_address
a
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2020-01-29 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H4 N14 O8, 0.125(H4 O2), 5(H2 O)'
_chemical_formula_sum            'C4 H14.50 N14 O13.25'
_chemical_formula_weight         470.80

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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'-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                   8.9398(7)
_cell_length_b                   20.6711(17)
_cell_length_c                   10.4206(7)
_cell_angle_alpha                90
_cell_angle_beta                 102.471(3)
_cell_angle_gamma                90
_cell_volume                     1880.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3191
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      26.02

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_F_000             970
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.162
_shelx_estimated_absorpt_T_min   0.968
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            14578
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.533
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2166
_reflns_number_gt                1492
_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-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick 2018)'
_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)+(0.0928P)²+2.3194P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2166
_refine_ls_number_parameters     150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1739
_refine_ls_wR_factor_gt          0.1529
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
C1 C 0.9629(3) 0.96910(11) 0.4820(2) 0.0256(5) Uani 1 1 d . . . . .
C2 C 0.7873(3) 0.89175(11) 0.4553(2) 0.0274(5) Uani 1 1 d . . . . .
N1 N 0.8179(2) 0.95394(9) 0.49870(18) 0.0260(5) Uani 1 1 d . . . . .
N2 N 1.0216(2) 0.92156(10) 0.4295(2) 0.0323(5) Uani 1 1 d . . . . .
N3 N 0.9116(2) 0.87354(9) 0.4133(2) 0.0311(5) Uani 1 1 d . . . . .
H3 H 0.924135 0.839241 0.368408 0.047 Uiso 1 1 d R U . . .
N4 N 0.7098(2) 0.99264(10) 0.53438(19) 0.0308(5) Uani 1 1 d . . . . .
H4 H 0.635784 1.009914 0.478309 0.037 Uiso 1 1 calc R U . . .
N5 N 0.7298(3) 1.00159(12) 0.6687(2) 0.0402(6) Uani 1 1 d . . . . .
N6 N 0.6561(2) 0.86510(10) 0.4664(2) 0.0358(5) Uani 1 1 d . . . . .
N7 N 0.6287(3) 0.80494(12) 0.4153(3) 0.0492(7) Uani 1 1 d . . . . .
O1 O 0.8146(3) 0.96482(12) 0.74100(19) 0.0579(6) Uani 1 1 d . . . . .
O2 O 0.6546(3) 1.04457(13) 0.7007(2) 0.0663(7) Uani 1 1 d . . . . .
O3 O 0.5101(3) 0.77986(13) 0.4320(3) 0.0801(9) Uani 1 1 d . . . . .
O4 O 0.7173(3) 0.77829(11) 0.3575(3) 0.0649(7) Uani 1 1 d . . . . .
O5 O 0.2356(3) 0.70811(12) 0.3904(3) 0.0725(8) Uani 1 1 d . . . . .
H5A H 0.318704 0.729501 0.403242 0.109 Uiso 1 1 d R U . . .
H5B H 0.172144 0.724131 0.325522 0.109 Uiso 1 1 d R U . . .
O6 O 0.5731(2) 1.09443(9) 0.3903(2) 0.0446(5) Uani 1 1 d . . . . .
H6A H 0.505690 1.104556 0.433133 0.067 Uiso 1 1 d R U . . .
H6B H 0.666620 1.122446 0.410603 0.067 Uiso 1 1 d R U . . .
O7 O 0.500000 0.28361(12) 0.250000 0.0410(6) Uani 1 2 d S T P . .
H7A H 0.588760 0.271373 0.248290 0.061 Uiso 0.5 1 d R U P . .
H7B H 0.440890 0.255453 0.203670 0.061 Uiso 0.5 1 d R U P . .
O8 O 0.523(3) 0.6622(6) 0.237(4) 0.043(5) Uani 0.125 1 d . . P . .
H8A H 0.571639 0.627425 0.239701 0.064 Uiso 0.125 1 d R U P . .
H8B H 0.428929 0.649825 0.232571 0.064 Uiso 0.125 1 d R U P . .


_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
C1 N2 1.290(3) . ?
C1 N1 1.380(3) . ?
C1 C1 1.451(5) 5_776 ?
C2 N6 1.323(3) . ?
C2 N3 1.333(3) . ?
C2 N1 1.370(3) . ?
N1 N4 1.367(3) . ?
N2 N3 1.382(3) . ?
N3 H3 0.8701 . ?
N4 N5 1.385(3) . ?
N4 H4 0.8600 . ?
N5 O2 1.204(3) . ?
N5 O1 1.214(3) . ?
N6 N7 1.354(3) . ?
N7 O4 1.224(3) . ?
N7 O3 1.226(3) . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8500 . ?
O6 H6A 0.8500 . ?
O6 H6B 1.0011 . ?
O7 H7A 0.8367 . ?
O7 H7B 0.8608 . ?
O7 H7A 0.8367 2_655 ?
O7 H7B 0.8608 2_655 ?
O8 O8 0.54(3) 2_655 ?
O8 H8A 0.8398 . ?
O8 H8B 0.8682 . ?
O8 H8B 0.54(7) 2_655 ?

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
N2 C1 N1 111.1(2) . . ?
N2 C1 C1 125.1(3) . 5_776 ?
N1 C1 C1 123.8(3) . 5_776 ?
N6 C2 N3 136.7(2) . . ?
N6 C2 N1 118.7(2) . . ?
N3 C2 N1 104.58(19) . . ?
N4 N1 C2 122.40(19) . . ?
N4 N1 C1 129.80(19) . . ?
C2 N1 C1 107.31(18) . . ?
C1 N2 N3 104.75(19) . . ?
C2 N3 N2 112.27(19) . . ?
C2 N3 H3 128.3 . . ?
N2 N3 H3 118.7 . . ?
N1 N4 N5 114.13(19) . . ?
N1 N4 H4 122.9 . . ?
N5 N4 H4 122.9 . . ?
O2 N5 O1 127.0(2) . . ?
O2 N5 N4 114.9(2) . . ?
O1 N5 N4 118.1(2) . . ?
C2 N6 N7 115.9(2) . . ?
O4 N7 O3 123.4(3) . . ?
O4 N7 N6 121.7(2) . . ?
O3 N7 N6 114.9(2) . . ?
H5A O5 H5B 109.5 . . ?
H6A O6 H6B 113.7 . . ?
H7A O7 H7B 104.7 . . ?
H7A O7 H7A 144.8 . 2_655 ?
H7B O7 H7A 48.5 . 2_655 ?
H7A O7 H7B 48.5 . 2_655 ?
H7B O7 H7B 94.9 . 2_655 ?
H7A O7 H7B 104.7 2_655 2_655 ?
O8 O8 H8A 115.1 2_655 . ?
O8 O8 H8B 37.0 2_655 . ?
H8A O8 H8B 103.8 . . ?
O8 O8 H8B 107(10) 2_655 2_655 ?
H8A O8 H8B 39.8 . 2_655 ?
H8B O8 H8B 121.7 . 2_655 ?

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
N6 C2 N1 N4 -10.0(3) . . . . ?
N3 C2 N1 N4 171.5(2) . . . . ?
N6 C2 N1 C1 177.3(2) . . . . ?
N3 C2 N1 C1 -1.1(2) . . . . ?
N2 C1 N1 N4 -170.7(2) . . . . ?
C1 C1 N1 N4 8.8(4) 5_776 . . . ?
N2 C1 N1 C2 1.3(3) . . . . ?
C1 C1 N1 C2 -179.3(3) 5_776 . . . ?
N1 C1 N2 N3 -0.8(3) . . . . ?
C1 C1 N2 N3 179.8(3) 5_776 . . . ?
N6 C2 N3 N2 -177.3(3) . . . . ?
N1 C2 N3 N2 0.7(3) . . . . ?
C1 N2 N3 C2 0.1(3) . . . . ?
C2 N1 N4 N5 106.0(2) . . . . ?
C1 N1 N4 N5 -83.1(3) . . . . ?
N1 N4 N5 O2 166.6(2) . . . . ?
N1 N4 N5 O1 -16.1(3) . . . . ?
N3 C2 N6 N7 -5.7(4) . . . . ?
N1 C2 N6 N7 176.5(2) . . . . ?
C2 N6 N7 O4 -3.1(4) . . . . ?
C2 N6 N7 O3 176.7(3) . . . . ?

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
_geom_hbond_publ_flag
N3 H3 O7 0.87 1.91 2.749(3) 160.2 3 yes
N4 H4 O6 0.86 2.00 2.717(3) 140.7 . yes
O5 H5A O3 0.85 1.97 2.820(3) 179.4 . yes
O5 H5B O4 0.85 2.59 3.070(3) 117.3 2_655 yes
O5 H5B O7 0.85 1.99 2.771(3) 151.6 3_455 yes
O6 H6A N6 0.85 2.06 2.907(3) 176.5 5_676 yes
O6 H6B O5 1.00 1.90 2.763(3) 142.3 3 yes
O7 H7A O4 0.84 2.25 2.980(2) 145.6 4_645 yes
O7 H7A O5 0.84 2.19 2.771(3) 126.8 3_545 yes
O7 H7B O5 0.86 1.93 2.771(3) 164.0 4_545 yes
O8 H8A O1 0.84 2.15 2.988(17) 175.0 7_666 yes
O8 H8B O1 0.87 2.59 3.224(16) 130.7 8_465 yes

_refine_diff_density_max         0.377
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.067



####################################################################### 
# 
# 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_lq191018_1_a
_database_code_depnum_ccdc_archive 'CCDC 1980543'
loop_
_audit_author_name
_audit_author_address
langqing
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2020-01-29 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H4 K2 N7 O6'
_chemical_formula_sum            'C2 H4 K2 N7 O6'
_chemical_formula_weight         300.32

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'
K K 0.2009 0.2494 '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                   7.197(2)
_cell_length_b                   8.971(3)
_cell_length_c                   9.188(2)
_cell_angle_alpha                61.707(7)
_cell_angle_beta                 72.877(8)
_cell_angle_gamma                81.944(9)
_cell_volume                     499.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2435
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      27.30

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_F_000             302
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.985
_shelx_estimated_absorpt_T_min   0.925
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6186
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ' SADABS-2016/2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            4040
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.579
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             1707
_reflns_number_gt                1352
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0483P)²+1.0467P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1707
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1125
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_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
C1 C 0.5973(5) 0.5905(4) 0.5941(5) 0.0254(8) Uani 1 1 d . . . . .
C2 C 0.9073(5) 0.5420(4) 0.5074(4) 0.0253(8) Uani 1 1 d . . . . .
N1 N 0.8743(4) 0.7036(4) 0.4174(4) 0.0331(8) Uani 1 1 d . . . . .
N2 N 0.6774(4) 0.7352(4) 0.4722(4) 0.0310(8) Uani 1 1 d . . . . .
N3 N 0.7359(4) 0.4642(4) 0.6197(4) 0.0306(8) Uani 1 1 d . . . . .
N4 N 0.6894(5) 0.2863(4) 0.7156(4) 0.0383(8) Uani 1 1 d . . . . .
N5 N 0.7187(5) 0.2317(4) 0.8643(4) 0.0319(8) Uani 1 1 d . . . . .
N6 N 0.4112(4) 0.5384(4) 0.6908(4) 0.0349(8) Uani 1 1 d . . . . .
N7 N 0.2826(4) 0.6550(4) 0.6965(4) 0.0309(7) Uani 1 1 d . . . . .
O1 O 0.7797(6) 0.3244(4) 0.9101(5) 0.0622(10) Uani 1 1 d . . . . .
O2 O 0.6908(5) 0.0807(4) 0.9672(4) 0.0643(11) Uani 1 1 d . . . . .
O3 O 0.1125(4) 0.6035(4) 0.7827(4) 0.0543(9) Uani 1 1 d . . . . .
O4 O 0.3193(4) 0.8102(3) 0.6255(3) 0.0351(7) Uani 1 1 d . . . . .
K1 K 0.44631(14) 1.02334(11) 0.28688(11) 0.0401(3) Uani 1 1 d . . . . .
K2 K 0.15469(17) 0.24372(12) 0.93596(14) 0.0551(4) Uani 1 1 d . . . . .
O5 O 0.3185(6) 1.3450(4) 0.1130(5) 0.0651(10) Uani 1 1 d . . . . .
H5A H 0.215449 1.340510 0.088021 0.098 Uiso 1 1 d R U . . .
H5B H 0.294519 1.394691 0.175661 0.098 Uiso 1 1 d R U . . .
O7 O 0.0515(4) 1.0329(4) 0.2896(4) 0.0545(9) Uani 1 1 d . . . . .
H6A H -0.043595 1.082037 0.334953 0.082 Uiso 1 1 d R U . . .
H6B H 0.008205 0.933737 0.325153 0.082 Uiso 1 1 d 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
C1 N2 1.313(4) . ?
C1 N6 1.372(5) . ?
C1 N3 1.379(4) . ?
C2 N1 1.313(4) . ?
C2 N3 1.372(5) . ?
C2 C2 1.441(7) 2_766 ?
N1 N2 1.395(4) . ?
N1 K2 3.118(4) 2_666 ?
N2 K1 2.939(3) . ?
N3 N4 1.441(4) . ?
N4 N5 1.287(5) . ?
N4 K1 3.083(4) 2_666 ?
N5 O2 1.233(4) . ?
N5 O1 1.267(5) . ?
N5 K2 3.416(4) 1_655 ?
N6 N7 1.306(4) . ?
N6 K2 2.957(3) . ?
N7 O4 1.255(4) . ?
N7 O3 1.257(4) . ?
O1 K2 2.744(4) 1_655 ?
O2 K2 2.778(3) 2_657 ?
O2 K1 2.787(3) 1_546 ?
O2 K1 3.313(4) 2_666 ?
O3 K2 2.857(3) . ?
O4 K1 2.710(3) . ?
O4 K1 2.893(3) 2_676 ?
K1 O5 2.734(3) . ?
K1 O7 2.824(3) . ?
K1 K2 3.9354(15) 1_564 ?
K1 K1 4.031(2) 2_676 ?
K1 K2 4.1757(18) 2_666 ?
K2 O5 2.774(3) 1_546 ?
K2 O7 2.799(4) 1_546 ?
K2 K2 4.666(2) 2_557 ?
K2 H5A 2.124(4) 1_546 ?
O5 H5A 0.8500 . ?
O5 H5B 0.8500 . ?
O7 H6A 0.8705 . ?
O7 H6B 0.8586 . ?

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
N2 C1 N6 134.8(3) . . ?
N2 C1 N3 109.8(3) . . ?
N6 C1 N3 115.4(3) . . ?
N1 C2 N3 109.1(3) . . ?
N1 C2 C2 126.1(4) . 2_766 ?
N3 C2 C2 124.8(4) . 2_766 ?
C2 N1 N2 108.4(3) . . ?
C2 N1 K2 107.4(2) . 2_666 ?
N2 N1 K2 94.1(2) . 2_666 ?
C1 N2 N1 107.0(3) . . ?
C1 N2 K1 122.1(2) . . ?
N1 N2 K1 127.7(2) . . ?
C2 N3 C1 105.7(3) . . ?
C2 N3 N4 129.2(3) . . ?
C1 N3 N4 123.5(3) . . ?
N5 N4 N3 108.0(3) . . ?
N5 N4 K1 105.7(2) . 2_666 ?
N3 N4 K1 146.2(2) . 2_666 ?
O2 N5 O1 117.6(4) . . ?
O2 N5 N4 119.0(4) . . ?
O1 N5 N4 123.4(3) . . ?
O2 N5 K2 94.0(3) . 1_655 ?
O1 N5 K2 48.4(2) . 1_655 ?
N4 N5 K2 124.9(2) . 1_655 ?
N7 N6 C1 117.5(3) . . ?
N7 N6 K2 96.8(2) . . ?
C1 N6 K2 145.5(2) . . ?
O4 N7 O3 119.5(3) . . ?
O4 N7 N6 124.6(3) . . ?
O3 N7 N6 115.9(3) . . ?
N5 O1 K2 111.4(2) . 1_655 ?
N5 O2 K2 145.2(3) . 2_657 ?
N5 O2 K1 114.0(3) . 1_546 ?
K2 O2 K1 97.25(9) 2_657 1_546 ?
N5 O2 K1 95.8(3) . 2_666 ?
K2 O2 K1 79.98(10) 2_657 2_666 ?
K1 O2 K1 120.71(13) 1_546 2_666 ?
N7 O3 K2 103.1(2) . . ?
N7 O4 K1 128.6(2) . . ?
N7 O4 K1 127.1(2) . 2_676 ?
K1 O4 K1 91.94(8) . 2_676 ?
O4 K1 O5 127.18(11) . . ?
O4 K1 O2 148.57(9) . 1_564 ?
O5 K1 O2 84.25(11) . 1_564 ?
O4 K1 O7 84.33(9) . . ?
O5 K1 O7 67.46(10) . . ?
O2 K1 O7 111.27(12) 1_564 . ?
O4 K1 O4 88.06(8) . 2_676 ?
O5 K1 O4 83.32(9) . 2_676 ?
O2 K1 O4 97.58(11) 1_564 2_676 ?
O7 K1 O4 135.54(9) . 2_676 ?
O4 K1 N2 57.20(8) . . ?
O5 K1 N2 162.40(10) . . ?
O2 K1 N2 93.25(10) 1_564 . ?
O7 K1 N2 129.06(9) . . ?
O4 K1 N2 79.74(9) 2_676 . ?
O4 K1 N4 77.65(9) . 2_666 ?
O5 K1 N4 122.92(10) . 2_666 ?
O2 K1 N4 84.26(10) 1_564 2_666 ?
O7 K1 N4 65.51(9) . 2_666 ?
O4 K1 N4 153.67(8) 2_676 2_666 ?
N2 K1 N4 73.93(9) . 2_666 ?
O4 K1 O2 114.54(8) . 2_666 ?
O5 K1 O2 88.26(9) . 2_666 ?
O2 K1 O2 59.29(13) 1_564 2_666 ?
O7 K1 O2 58.66(9) . 2_666 ?
O4 K1 O2 156.16(8) 2_676 2_666 ?
N2 K1 O2 105.46(9) . 2_666 ?
N4 K1 O2 39.49(8) 2_666 2_666 ?
O4 K1 K2 129.61(7) . 1_564 ?
O5 K1 K2 44.81(7) . 1_564 ?
O2 K1 K2 70.08(9) 1_564 1_564 ?
O7 K1 K2 45.32(7) . 1_564 ?
O4 K1 K2 126.57(6) 2_676 1_564 ?
N2 K1 K2 149.40(8) . 1_564 ?
N4 K1 K2 78.87(7) 2_666 1_564 ?
O2 K1 K2 44.04(6) 2_666 1_564 ?
O4 K1 K1 45.83(6) . 2_676 ?
O5 K1 K1 108.83(8) . 2_676 ?
O2 K1 K1 131.95(10) 1_564 2_676 ?
O7 K1 K1 116.48(8) . 2_676 ?
O4 K1 K1 42.22(5) 2_676 2_676 ?
N2 K1 K1 60.53(7) . 2_676 ?
N4 K1 K1 119.97(7) 2_666 2_676 ?
O2 K1 K1 159.36(6) 2_666 2_676 ?
K2 K1 K1 148.90(4) 1_564 2_676 ?
O4 K1 K2 107.34(6) . 2_666 ?
O5 K1 K2 125.29(9) . 2_666 ?
O2 K1 K2 41.30(6) 1_564 2_666 ?
O7 K1 K2 119.49(8) . 2_666 ?
O4 K1 K2 104.60(6) 2_676 2_666 ?
N2 K1 K2 55.82(7) . 2_666 ?
N4 K1 K2 60.20(7) 2_666 2_666 ?
O2 K1 K2 62.83(6) 2_666 2_666 ?
K2 K1 K2 98.32(3) 1_564 2_666 ?
K1 K1 K2 112.42(4) 2_676 2_666 ?
O1 K2 O5 122.18(12) 1_455 1_546 ?
O1 K2 O2 123.96(12) 1_455 2_657 ?
O5 K2 O2 99.29(11) 1_546 2_657 ?
O1 K2 O7 95.21(11) 1_455 1_546 ?
O5 K2 O7 67.29(11) 1_546 1_546 ?
O2 K2 O7 65.97(10) 2_657 1_546 ?
O1 K2 O3 71.15(10) 1_455 . ?
O5 K2 O3 75.18(10) 1_546 . ?
O2 K2 O3 163.09(11) 2_657 . ?
O7 K2 O3 123.89(11) 1_546 . ?
O1 K2 N6 109.85(10) 1_455 . ?
O5 K2 N6 70.37(11) 1_546 . ?
O2 K2 N6 119.26(10) 2_657 . ?
O7 K2 N6 137.54(11) 1_546 . ?
O3 K2 N6 43.86(8) . . ?
O1 K2 N1 70.17(10) 1_455 2_666 ?
O5 K2 N1 147.66(11) 1_546 2_666 ?
O2 K2 N1 95.15(10) 2_657 2_666 ?
O7 K2 N1 144.81(10) 1_546 2_666 ?
O3 K2 N1 82.65(10) . 2_666 ?
N6 K2 N1 77.32(9) . 2_666 ?
O1 K2 N5 20.22(9) 1_455 1_455 ?
O5 K2 N5 141.21(11) 1_546 1_455 ?
O2 K2 N5 106.36(10) 2_657 1_455 ?
O7 K2 N5 97.18(9) 1_546 1_455 ?
O3 K2 N5 86.82(9) . 1_455 ?
N6 K2 N5 118.19(9) . 1_455 ?
N1 K2 N5 58.31(8) 2_666 1_455 ?
O1 K2 K1 140.06(9) 1_455 1_546 ?
O5 K2 K1 43.99(7) 1_546 1_546 ?
O2 K2 K1 55.98(9) 2_657 1_546 ?
O7 K2 K1 45.84(7) 1_546 1_546 ?
O3 K2 K1 118.89(8) . 1_546 ?
N6 K2 K1 99.08(7) . 1_546 ?
N1 K2 K1 145.25(7) 2_666 1_546 ?
N5 K2 K1 141.98(6) 1_455 1_546 ?
O1 K2 K1 126.45(8) 1_455 2_666 ?
O5 K2 K1 111.35(9) 1_546 2_666 ?
O2 K2 K1 41.45(7) 2_657 2_666 ?
O7 K2 K1 107.05(7) 1_546 2_666 ?
O3 K2 K1 125.11(8) . 2_666 ?
N6 K2 K1 85.35(7) . 2_666 ?
N1 K2 K1 63.62(6) 2_666 2_666 ?
N5 K2 K1 107.14(6) 1_455 2_666 ?
K1 K2 K1 81.68(3) 1_546 2_666 ?
O1 K2 K2 71.29(8) 1_455 2_557 ?
O5 K2 K2 135.39(8) 1_546 2_557 ?
O2 K2 K2 52.69(9) 2_657 2_557 ?
O7 K2 K2 69.30(7) 1_546 2_557 ?
O3 K2 K2 141.14(8) . 2_557 ?
N6 K2 K2 150.56(9) . 2_557 ?
N1 K2 K2 75.64(6) 2_666 2_557 ?
N5 K2 K2 54.35(6) 1_455 2_557 ?
K1 K2 K2 96.49(3) 1_546 2_557 ?
K1 K2 K2 72.36(4) 2_666 2_557 ?
O1 K2 H5A 109.29(14) 1_455 1_546 ?
O5 K2 H5A 12.97(3) 1_546 1_546 ?
O2 K2 H5A 108.05(13) 2_657 1_546 ?
O7 K2 H5A 64.46(12) 1_546 1_546 ?
O3 K2 H5A 69.61(12) . 1_546 ?
N6 K2 H5A 74.92(13) . 1_546 ?
N1 K2 H5A 150.06(12) 2_666 1_546 ?
N5 K2 H5A 128.25(13) 1_455 1_546 ?
K1 K2 H5A 52.10(9) 1_546 1_546 ?
K1 K2 H5A 124.26(11) 2_666 1_546 ?
K2 K2 H5A 133.64(11) 2_557 1_546 ?
K1 O5 K2 91.20(10) . 1_564 ?
K1 O5 H5A 109.2 . . ?
K2 O5 H5A 34.1 1_564 . ?
K1 O5 H5B 109.4 . . ?
K2 O5 H5B 143.6 1_564 . ?
H5A O5 H5B 109.5 . . ?
K2 O7 K1 88.84(9) 1_564 . ?
K2 O7 H6A 107.3 1_564 . ?
K1 O7 H6A 126.9 . . ?
K2 O7 H6B 117.7 1_564 . ?
K1 O7 H6B 111.6 . . ?
H6A O7 H6B 104.6 . . ?

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
_geom_hbond_publ_flag
O7 H6B N1 0.86 2.08 2.935(4) 174.0 1_455 yes
O7 H6A O4 0.87 2.09 2.910(4) 156.5 2_576 yes
O7 H6A O3 0.87 2.53 3.131(4) 126.8 2_576 yes
O7 H6A N7 0.87 2.67 3.451(4) 150.3 2_576 yes
O5 H5B O1 0.85 2.29 2.871(5) 125.8 2_676 yes
O5 H5B N3 0.85 2.67 3.513(5) 172.5 2_676 yes
O5 H5A O3 0.85 2.41 3.004(5) 127.3 2_576 yes

_refine_diff_density_max         1.032
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.076



####################################################################### 
# 
# 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_LQ191221_a
_database_code_depnum_ccdc_archive 'CCDC 1980546'
loop_
_audit_author_name
_audit_author_address
langqing
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2020-01-29 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H6 N14 Na2 O10'
_chemical_formula_sum            'C4 H6 N14 Na2 O10'
_chemical_formula_weight         456.21

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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                   9.5313(9)
_cell_length_b                   11.5462(12)
_cell_length_c                   14.4382(14)
_cell_angle_alpha                90
_cell_angle_beta                 104.885(3)
_cell_angle_gamma                90
_cell_volume                     1535.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5428
_cell_measurement_theta_min      2.83
_cell_measurement_theta_max      27.62

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.230
_shelx_estimated_absorpt_T_min   0.951
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6351
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            7008
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.829
_diffrn_reflns_theta_max         27.638
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_point_group_measured_fraction_full 0.876
_reflns_number_total             2971
_reflns_number_gt                2775
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.692
_reflns_Friedel_fraction_max     0.682
_reflns_Friedel_fraction_full    0.764

_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0599P)²+0.3222P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1065 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2971
_refine_ls_number_parameters     274
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_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
Na2 Na 0.51542(18) 1.02181(12) 0.21094(14) 0.0497(4) Uani 1 1 d . . . . .
C1 C 0.4268(3) 0.7352(3) 0.4984(2) 0.0210(6) Uani 1 1 d . . . . .
C2 C 0.2239(3) 0.6531(2) 0.5101(2) 0.0188(6) Uani 1 1 d . . . . .
C3 C 0.5790(3) 0.7670(2) 0.5196(2) 0.0204(6) Uani 1 1 d . . . . .
C4 C 0.7812(3) 0.8455(2) 0.50221(19) 0.0183(6) Uani 1 1 d . . . . .
N1 N 0.3673(3) 0.6643(2) 0.55455(17) 0.0181(5) Uani 1 1 d . . . . .
N2 N 0.2033(3) 0.7178(2) 0.43141(19) 0.0232(5) Uani 1 1 d . . . . .
H2 H 0.120681 0.725908 0.390391 0.028 Uiso 1 1 calc R U . . .
N3 N 0.3279(3) 0.7699(2) 0.42325(18) 0.0257(6) Uani 1 1 d . . . . .
N4 N 0.4372(3) 0.6052(2) 0.63903(18) 0.0219(5) Uani 1 1 d . . . . .
N5 N 0.4678(3) 0.6812(2) 0.71059(19) 0.0238(5) Uani 1 1 d . . . . .
N6 N 0.1398(3) 0.5838(2) 0.54872(18) 0.0239(6) Uani 1 1 d . . . . .
N7 N 0.0022(3) 0.5770(2) 0.4984(2) 0.0253(6) Uani 1 1 d . . . . .
N8 N 0.6370(3) 0.8314(2) 0.45858(17) 0.0197(5) Uani 1 1 d . . . . .
N9 N 0.8024(3) 0.7888(2) 0.58505(18) 0.0221(5) Uani 1 1 d . . . . .
H9 H 0.885140 0.783849 0.626406 0.026 Uiso 1 1 calc R U . . .
N10 N 0.6772(3) 0.7391(2) 0.59697(19) 0.0249(6) Uani 1 1 d . . . . .
N11 N 0.5709(3) 0.8744(2) 0.36773(18) 0.0230(5) Uani 1 1 d . . . . .
N12 N 0.5591(3) 0.7887(2) 0.30546(18) 0.0232(5) Uani 1 1 d . . . . .
N13 N 0.8622(3) 0.9121(2) 0.46004(18) 0.0225(5) Uani 1 1 d . . . . .
N14 N 1.0033(3) 0.9164(2) 0.5054(2) 0.0240(5) Uani 1 1 d . . . . .
Na1 Na 0.72317(17) 0.50655(12) 0.36205(11) 0.0387(3) Uani 1 1 d . . . . .
O1 O 0.5326(3) 0.6400(2) 0.79021(15) 0.0323(5) Uani 1 1 d . . . . .
O2 O 0.4371(3) 0.7858(2) 0.70062(19) 0.0380(6) Uani 1 1 d . . . . .
O3 O -0.0772(3) 0.5113(2) 0.5312(2) 0.0375(6) Uani 1 1 d . . . . .
O4 O -0.0483(3) 0.6308(2) 0.42237(19) 0.0377(6) Uani 1 1 d . . . . .
O5 O 0.5938(3) 0.6870(2) 0.3277(2) 0.0465(7) Uani 1 1 d . . . . .
O6 O 0.5060(3) 0.8184(2) 0.22003(16) 0.0354(6) Uani 1 1 d . . . . .
O7 O 1.0766(3) 0.9875(2) 0.47420(19) 0.0360(6) Uani 1 1 d . . . . .
O8 O 1.0572(3) 0.8528(2) 0.57500(18) 0.0330(6) Uani 1 1 d . . . . .
O9 O 0.7652(3) 0.5017(2) 0.20880(19) 0.0368(6) Uani 1 1 d G . . . .
H9A H 0.728955 0.441088 0.178509 0.055 Uiso 1 1 d G U . . .
H9B H 0.727626 0.561291 0.177525 0.055 Uiso 1 1 d G U . . .
O10 O 0.7631(4) 1.0385(3) 0.2678(3) 0.0504(7) Uani 1 1 d . . . . .
H10A H 0.841912 1.024173 0.250727 0.076 Uiso 1 1 d R U . . .
H10B H 0.782612 1.020603 0.329057 0.076 Uiso 1 1 d 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
Na2 O10 2.300(4) . ?
Na2 O2 2.336(3) 2_574 ?
Na2 O6 2.355(3) . ?
Na2 O9 2.389(3) 3_455 ?
Na2 O3 2.546(3) 4_564 ?
Na2 N11 2.773(3) . ?
Na2 N12 2.998(3) . ?
Na2 Na1 3.959(2) 3_455 ?
Na2 H10B 2.6763 . ?
C1 N3 1.304(4) . ?
C1 N1 1.373(4) . ?
C1 C3 1.451(3) . ?
C2 N2 1.331(4) . ?
C2 N6 1.351(4) . ?
C2 N1 1.359(4) . ?
C3 N10 1.301(4) . ?
C3 N8 1.373(4) . ?
C4 N9 1.333(4) . ?
C4 N13 1.341(4) . ?
C4 N8 1.367(4) . ?
N1 N4 1.407(3) . ?
N2 N3 1.363(4) . ?
N2 H2 0.8600 . ?
N3 Na1 2.965(3) 3_455 ?
N4 N5 1.330(4) . ?
N5 O2 1.243(4) . ?
N5 O1 1.251(3) . ?
N6 N7 1.328(4) . ?
N7 O4 1.246(4) . ?
N7 O3 1.248(4) . ?
N7 Na1 2.987(3) 1_455 ?
N8 N11 1.392(3) . ?
N9 N10 1.374(4) . ?
N9 H9 0.8600 . ?
N11 N12 1.322(4) . ?
N12 O5 1.239(4) . ?
N12 O6 1.255(3) . ?
N13 N14 1.338(4) . ?
N14 O7 1.235(4) . ?
N14 O8 1.244(4) . ?
Na1 O9 2.348(3) . ?
Na1 O7 2.405(3) 3_445 ?
Na1 O5 2.407(3) . ?
Na1 O1 2.504(3) 2_564 ?
Na1 O4 2.566(3) 1_655 ?
Na1 O3 2.683(3) 1_655 ?
O9 H9A 0.8500 . ?
O9 H9B 0.8500 . ?
O10 H10A 0.8644 . ?
O10 H10B 0.8810 . ?

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
O10 Na2 O2 102.99(11) . 2_574 ?
O10 Na2 O6 96.55(11) . . ?
O2 Na2 O6 159.35(13) 2_574 . ?
O10 Na2 O9 160.55(14) . 3_455 ?
O2 Na2 O9 77.89(11) 2_574 3_455 ?
O6 Na2 O9 81.47(10) . 3_455 ?
O10 Na2 O3 115.58(13) . 4_564 ?
O2 Na2 O3 93.23(10) 2_574 4_564 ?
O6 Na2 O3 84.19(10) . 4_564 ?
O9 Na2 O3 83.59(10) 3_455 4_564 ?
O10 Na2 N11 78.30(11) . . ?
O2 Na2 N11 128.82(11) 2_574 . ?
O6 Na2 N11 49.02(8) . . ?
O9 Na2 N11 86.07(10) 3_455 . ?
O3 Na2 N11 133.11(10) 4_564 . ?
O10 Na2 N12 84.44(10) . . ?
O2 Na2 N12 152.57(12) 2_574 . ?
O6 Na2 N12 23.40(7) . . ?
O9 Na2 N12 86.57(9) 3_455 . ?
O3 Na2 N12 107.48(9) 4_564 . ?
N11 Na2 N12 26.11(7) . . ?
O10 Na2 Na1 127.61(12) . 3_455 ?
O2 Na2 Na1 79.58(8) 2_574 3_455 ?
O6 Na2 Na1 83.27(9) . 3_455 ?
O9 Na2 Na1 32.99(7) 3_455 3_455 ?
O3 Na2 Na1 116.49(8) 4_564 3_455 ?
N11 Na2 Na1 62.38(7) . 3_455 ?
N12 Na2 Na1 75.19(7) . 3_455 ?
O10 Na2 H10B 18.5 . . ?
O2 Na2 H10B 106.4 2_574 . ?
O6 Na2 H10B 90.2 . . ?
O9 Na2 H10B 142.3 3_455 . ?
O3 Na2 H10B 132.3 4_564 . ?
N11 Na2 H10B 61.7 . . ?
N12 Na2 H10B 73.0 . . ?
Na1 Na2 H10B 109.7 3_455 . ?
N3 C1 N1 110.8(3) . . ?
N3 C1 C3 124.6(3) . . ?
N1 C1 C3 124.6(2) . . ?
N2 C2 N6 135.4(3) . . ?
N2 C2 N1 105.1(2) . . ?
N6 C2 N1 119.5(3) . . ?
N10 C3 N8 111.4(3) . . ?
N10 C3 C1 125.4(3) . . ?
N8 C3 C1 123.2(2) . . ?
N9 C4 N13 135.8(3) . . ?
N9 C4 N8 104.9(2) . . ?
N13 C4 N8 119.1(2) . . ?
C2 N1 C1 107.2(2) . . ?
C2 N1 N4 124.0(2) . . ?
C1 N1 N4 128.7(2) . . ?
C2 N2 N3 112.3(2) . . ?
C2 N2 H2 123.8 . . ?
N3 N2 H2 123.8 . . ?
C1 N3 N2 104.6(3) . . ?
C1 N3 Na1 130.3(2) . 3_455 ?
N2 N3 Na1 101.40(19) . 3_455 ?
N5 N4 N1 108.3(2) . . ?
O2 N5 O1 121.5(3) . . ?
O2 N5 N4 123.6(3) . . ?
O1 N5 N4 114.9(3) . . ?
N7 N6 C2 114.6(3) . . ?
O4 N7 O3 120.2(3) . . ?
O4 N7 N6 123.8(3) . . ?
O3 N7 N6 116.0(3) . . ?
O4 N7 Na1 58.49(16) . 1_455 ?
O3 N7 Na1 63.90(18) . 1_455 ?
N6 N7 Na1 164.5(2) . 1_455 ?
C4 N8 C3 107.0(2) . . ?
C4 N8 N11 123.3(2) . . ?
C3 N8 N11 129.7(2) . . ?
C4 N9 N10 112.4(3) . . ?
C4 N9 H9 123.8 . . ?
N10 N9 H9 123.8 . . ?
C3 N10 N9 104.2(3) . . ?
N12 N11 N8 108.2(2) . . ?
N12 N11 Na2 86.51(16) . . ?
N8 N11 Na2 158.94(19) . . ?
O5 N12 O6 121.8(3) . . ?
O5 N12 N11 124.2(3) . . ?
O6 N12 N11 114.0(2) . . ?
O5 N12 Na2 164.8(2) . . ?
O6 N12 Na2 48.19(15) . . ?
N11 N12 Na2 67.39(15) . . ?
N14 N13 C4 115.0(2) . . ?
O7 N14 O8 122.1(3) . . ?
O7 N14 N13 115.9(3) . . ?
O8 N14 N13 121.9(3) . . ?
O9 Na1 O7 154.33(10) . 3_445 ?
O9 Na1 O5 91.64(10) . . ?
O7 Na1 O5 82.11(11) 3_445 . ?
O9 Na1 O1 82.80(9) . 2_564 ?
O7 Na1 O1 74.45(9) 3_445 2_564 ?
O5 Na1 O1 102.75(11) . 2_564 ?
O9 Na1 O4 89.88(10) . 1_655 ?
O7 Na1 O4 114.32(10) 3_445 1_655 ?
O5 Na1 O4 86.06(11) . 1_655 ?
O1 Na1 O4 168.64(11) 2_564 1_655 ?
O9 Na1 O3 127.27(10) . 1_655 ?
O7 Na1 O3 77.74(9) 3_445 1_655 ?
O5 Na1 O3 112.08(10) . 1_655 ?
O1 Na1 O3 131.31(9) 2_564 1_655 ?
O4 Na1 O3 48.56(8) 1_655 1_655 ?
O9 Na1 N3 97.64(10) . 3_545 ?
O7 Na1 N3 85.66(9) 3_445 3_545 ?
O5 Na1 N3 167.08(11) . 3_545 ?
O1 Na1 N3 69.74(8) 2_564 3_545 ?
O4 Na1 N3 102.86(9) 1_655 3_545 ?
O3 Na1 N3 69.02(8) 1_655 3_545 ?
O9 Na1 N7 106.81(10) . 1_655 ?
O7 Na1 N7 98.86(10) 3_445 1_655 ?
O5 Na1 N7 102.86(10) . 1_655 ?
O1 Na1 N7 152.30(9) 2_564 1_655 ?
O4 Na1 N7 24.45(8) 1_655 1_655 ?
O3 Na1 N7 24.68(8) 1_655 1_655 ?
N3 Na1 N7 83.09(8) 3_545 1_655 ?
O9 Na1 Na2 33.63(7) . 3_545 ?
O7 Na1 Na2 171.02(9) 3_445 3_545 ?
O5 Na1 Na2 104.10(9) . 3_545 ?
O1 Na1 Na2 109.88(7) 2_564 3_545 ?
O4 Na1 Na2 60.41(8) 1_655 3_545 ?
O3 Na1 Na2 93.79(7) 1_655 3_545 ?
N3 Na1 Na2 88.54(7) 3_545 3_545 ?
N7 Na1 Na2 73.60(7) 1_655 3_545 ?
N5 O1 Na1 140.5(2) . 2_565 ?
N5 O2 Na2 148.8(2) . 2_575 ?
N7 O3 Na2 113.1(2) . 4_465 ?
N7 O3 Na1 91.4(2) . 1_455 ?
Na2 O3 Na1 154.66(11) 4_465 1_455 ?
N7 O4 Na1 97.05(19) . 1_455 ?
N12 O5 Na1 164.1(3) . . ?
N12 O6 Na2 108.41(18) . . ?
N14 O7 Na1 141.9(2) . 3 ?
Na1 O9 Na2 113.38(11) . 3_545 ?
Na1 O9 H9A 111.1 . . ?
Na2 O9 H9A 111.0 3_545 . ?
Na1 O9 H9B 109.3 . . ?
Na2 O9 H9B 102.2 3_545 . ?
H9A O9 H9B 109.5 . . ?
Na2 O10 H10A 140.4 . . ?
Na2 O10 H10B 105.7 . . ?
H10A O10 H10B 105.4 . . ?

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
N3 C1 C3 N10 175.5(4) . . . . ?
N1 C1 C3 N10 -4.6(4) . . . . ?
N3 C1 C3 N8 -4.6(4) . . . . ?
N1 C1 C3 N8 175.3(3) . . . . ?
N2 C2 N1 C1 -0.9(3) . . . . ?
N6 C2 N1 C1 177.6(3) . . . . ?
N2 C2 N1 N4 -176.9(3) . . . . ?
N6 C2 N1 N4 1.6(4) . . . . ?
N3 C1 N1 C2 1.3(3) . . . . ?
C3 C1 N1 C2 -178.6(2) . . . . ?
N3 C1 N1 N4 177.0(3) . . . . ?
C3 C1 N1 N4 -2.9(5) . . . . ?
N6 C2 N2 N3 -177.9(3) . . . . ?
N1 C2 N2 N3 0.3(3) . . . . ?
N1 C1 N3 N2 -1.1(3) . . . . ?
C3 C1 N3 N2 178.8(3) . . . . ?
N1 C1 N3 Na1 118.2(2) . . . 3_455 ?
C3 C1 N3 Na1 -61.9(4) . . . 3_455 ?
C2 N2 N3 C1 0.5(3) . . . . ?
C2 N2 N3 Na1 -136.8(2) . . . 3_455 ?
C2 N1 N4 N5 -108.4(3) . . . . ?
C1 N1 N4 N5 76.6(4) . . . . ?
N1 N4 N5 O2 0.1(4) . . . . ?
N1 N4 N5 O1 -179.0(2) . . . . ?
N2 C2 N6 N7 -0.6(5) . . . . ?
N1 C2 N6 N7 -178.5(2) . . . . ?
C2 N6 N7 O4 -1.1(4) . . . . ?
C2 N6 N7 O3 178.3(3) . . . . ?
C2 N6 N7 Na1 92.4(8) . . . 1_455 ?
N9 C4 N8 C3 0.7(3) . . . . ?
N13 C4 N8 C3 -175.8(3) . . . . ?
N9 C4 N8 N11 -177.6(3) . . . . ?
N13 C4 N8 N11 5.9(4) . . . . ?
N10 C3 N8 C4 -0.9(4) . . . . ?
C1 C3 N8 C4 179.2(3) . . . . ?
N10 C3 N8 N11 177.3(3) . . . . ?
C1 C3 N8 N11 -2.6(5) . . . . ?
N13 C4 N9 N10 175.3(3) . . . . ?
N8 C4 N9 N10 -0.4(3) . . . . ?
N8 C3 N10 N9 0.6(4) . . . . ?
C1 C3 N10 N9 -179.5(3) . . . . ?
C4 N9 N10 C3 -0.1(4) . . . . ?
C4 N8 N11 N12 99.5(3) . . . . ?
C3 N8 N11 N12 -78.4(4) . . . . ?
C4 N8 N11 Na2 -33.2(7) . . . . ?
C3 N8 N11 Na2 148.9(4) . . . . ?
N8 N11 N12 O5 4.1(4) . . . . ?
Na2 N11 N12 O5 168.8(3) . . . . ?
N8 N11 N12 O6 -177.3(2) . . . . ?
Na2 N11 N12 O6 -12.6(2) . . . . ?
N8 N11 N12 Na2 -164.6(2) . . . . ?
N9 C4 N13 N14 8.0(5) . . . . ?
N8 C4 N13 N14 -176.9(3) . . . . ?
C4 N13 N14 O7 -171.9(3) . . . . ?
C4 N13 N14 O8 7.9(4) . . . . ?
O2 N5 O1 Na1 -141.8(3) . . . 2_565 ?
N4 N5 O1 Na1 37.4(4) . . . 2_565 ?
O1 N5 O2 Na2 60.5(6) . . . 2_575 ?
N4 N5 O2 Na2 -118.6(4) . . . 2_575 ?
O4 N7 O3 Na2 -156.7(2) . . . 4_465 ?
N6 N7 O3 Na2 23.8(3) . . . 4_465 ?
Na1 N7 O3 Na2 -173.45(19) 1_455 . . 4_465 ?
O4 N7 O3 Na1 16.8(3) . . . 1_455 ?
N6 N7 O3 Na1 -162.7(2) . . . 1_455 ?
O3 N7 O4 Na1 -17.7(3) . . . 1_455 ?
N6 N7 O4 Na1 161.7(2) . . . 1_455 ?
O6 N12 O5 Na1 87.2(9) . . . . ?
N11 N12 O5 Na1 -94.3(9) . . . . ?
Na2 N12 O5 Na1 42.5(15) . . . . ?
O5 N12 O6 Na2 -165.6(3) . . . . ?
N11 N12 O6 Na2 15.7(3) . . . . ?
O8 N14 O7 Na1 88.7(4) . . . 3 ?
N13 N14 O7 Na1 -91.5(4) . . . 3 ?

_refine_diff_density_max         0.287
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.051



####################################################################### 
# 
# 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_LQ191114_a
_database_code_depnum_ccdc_archive 'CCDC 1980542'
loop_
_audit_author_name
_audit_author_address
langqing
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2020-01-29 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 N14 O8, 4(H5 N2), 2(H2 O)'
_chemical_formula_sum            'C4 H24 N22 O10'
_chemical_formula_weight         540.45

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                   7.2053(4)
_cell_length_b                   17.3968(11)
_cell_length_c                   8.5866(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.620(2)
_cell_angle_gamma                90
_cell_volume                     1036.57(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5045
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_F_000             564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.158
_shelx_estimated_absorpt_T_min   0.977
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            8535
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.727
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             2314
_reflns_number_gt                1860
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0626P)²+0.4240P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2314
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1130
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
C1 C 0.0892(2) 0.52150(8) 0.02558(18) 0.0220(3) Uani 1 1 d . . . . .
C2 C 0.3924(2) 0.54813(8) 0.13465(18) 0.0212(3) Uani 1 1 d . . . . .
N1 N 0.26152(18) 0.48947(7) 0.10578(15) 0.0219(3) Uani 1 1 d . . . . .
N2 N 0.11120(19) 0.59524(7) 0.00564(18) 0.0278(3) Uani 1 1 d . . . . .
N3 N 0.30431(19) 0.61289(7) 0.07570(17) 0.0259(3) Uani 1 1 d . . . . .
N4 N 0.30849(19) 0.41154(7) 0.12899(16) 0.0247(3) Uani 1 1 d . . . . .
N5 N 0.28574(18) 0.38917(7) 0.26797(16) 0.0245(3) Uani 1 1 d . . . . .
N6 N 0.57853(19) 0.52842(7) 0.21000(17) 0.0263(3) Uani 1 1 d . . . . .
N7 N 0.70349(19) 0.58482(7) 0.25406(16) 0.0256(3) Uani 1 1 d . . . . .
N8 N 0.5271(2) 0.23599(8) 0.56960(17) 0.0355(4) Uani 1 1 d . . . . .
H8A H 0.429378 0.220028 0.606383 0.053 Uiso 1 1 d R U . . .
H8B H 0.549255 0.201753 0.499704 0.053 Uiso 1 1 d R U . . .
H8C H 0.492280 0.281920 0.516244 0.053 Uiso 1 1 d R U . . .
N9 N 0.6959(2) 0.24345(9) 0.70245(18) 0.0380(4) Uani 1 1 d . . . . .
H9A H 0.797039 0.253226 0.664653 0.057 Uiso 1 1 d R U . . .
H9B H 0.679475 0.282052 0.765414 0.057 Uiso 1 1 d R U . . .
N10 N 0.8281(3) 0.10281(9) 0.8827(2) 0.0427(4) Uani 1 1 d . . . . .
H10A H 0.803897 0.062527 0.816416 0.064 Uiso 1 1 d R U . . .
H10B H 0.953629 0.104758 0.932015 0.064 Uiso 1 1 d R U . . .
H10C H 0.791202 0.146422 0.819899 0.064 Uiso 1 1 d R U . . .
N11 N 0.7223(2) 0.09579(9) 1.0003(2) 0.0405(4) Uani 1 1 d . . . . .
H11A H 0.802503 0.100079 1.098831 0.061 Uiso 1 1 d R U . . .
H11B H 0.664871 0.050069 0.990200 0.061 Uiso 1 1 d R U . . .
O1 O 0.2318(2) 0.43122(8) 0.36371(16) 0.0443(4) Uani 1 1 d . . . . .
O2 O 0.32234(18) 0.31867(7) 0.29862(15) 0.0366(3) Uani 1 1 d . . . . .
O3 O 0.87464(17) 0.56387(7) 0.31346(16) 0.0366(3) Uani 1 1 d . . . . .
O4 O 0.66041(18) 0.65426(6) 0.24126(16) 0.0368(3) Uani 1 1 d . . . . .
O5 O 0.0116(2) 0.24164(8) 0.04226(19) 0.0517(4) Uani 1 1 d . . . . .
H5A H 0.014787 0.292166 0.019158 0.078 Uiso 1 1 d R U . . .
H5B H 0.118542 0.238241 0.115870 0.078 Uiso 1 1 d 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
C1 N2 1.3093(19) . ?
C1 N1 1.366(2) . ?
C1 C1 1.449(3) 3_565 ?
C2 N3 1.3249(19) . ?
C2 N1 1.3661(19) . ?
C2 N6 1.367(2) . ?
N1 N4 1.3986(17) . ?
N2 N3 1.3934(19) . ?
N4 N5 1.3067(19) . ?
N5 O1 1.2388(18) . ?
N5 O2 1.2671(16) . ?
N6 N7 1.3165(18) . ?
N7 O4 1.2447(17) . ?
N7 O3 1.2550(18) . ?
N8 N9 1.432(2) . ?
N8 H8A 0.8900 . ?
N8 H8B 0.8900 . ?
N8 H8C 0.9217 . ?
N9 H9A 0.8900 . ?
N9 H9B 0.8900 . ?
N10 N11 1.425(2) . ?
N10 H10A 0.8900 . ?
N10 H10B 0.8900 . ?
N10 H10C 0.9272 . ?
N11 H11A 0.8900 . ?
N11 H11B 0.8900 . ?
O5 H5A 0.9028 . ?
O5 H5B 0.8568 . ?

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
N2 C1 N1 109.87(13) . . ?
N2 C1 C1 126.50(17) . 3_565 ?
N1 C1 C1 123.62(16) . 3_565 ?
N3 C2 N1 109.25(13) . . ?
N3 C2 N6 134.62(14) . . ?
N1 C2 N6 116.10(13) . . ?
C1 N1 C2 106.03(12) . . ?
C1 N1 N4 128.28(12) . . ?
C2 N1 N4 124.72(12) . . ?
C1 N2 N3 107.55(12) . . ?
C2 N3 N2 107.30(12) . . ?
N5 N4 N1 109.50(12) . . ?
O1 N5 O2 121.25(13) . . ?
O1 N5 N4 124.69(13) . . ?
O2 N5 N4 114.05(12) . . ?
N7 N6 C2 117.20(13) . . ?
O4 N7 O3 120.80(13) . . ?
O4 N7 N6 124.26(13) . . ?
O3 N7 N6 114.93(13) . . ?
N9 N8 H8A 109.2 . . ?
N9 N8 H8B 109.2 . . ?
H8A N8 H8B 109.5 . . ?
N9 N8 H8C 112.1 . . ?
H8A N8 H8C 108.2 . . ?
H8B N8 H8C 108.6 . . ?
N8 N9 H9A 109.3 . . ?
N8 N9 H9B 109.2 . . ?
H9A N9 H9B 109.5 . . ?
N11 N10 H10A 109.6 . . ?
N11 N10 H10B 109.6 . . ?
H10A N10 H10B 109.5 . . ?
N11 N10 H10C 111.0 . . ?
H10A N10 H10C 107.2 . . ?
H10B N10 H10C 110.0 . . ?
N10 N11 H11A 109.4 . . ?
N10 N11 H11B 109.3 . . ?
H11A N11 H11B 109.5 . . ?
H5A O5 H5B 99.1 . . ?

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
N2 C1 N1 C2 0.05(17) . . . . ?
C1 C1 N1 C2 -179.04(18) 3_565 . . . ?
N2 C1 N1 N4 -168.94(14) . . . . ?
C1 C1 N1 N4 12.0(3) 3_565 . . . ?
N3 C2 N1 C1 0.28(17) . . . . ?
N6 C2 N1 C1 -177.87(13) . . . . ?
N3 C2 N1 N4 169.77(13) . . . . ?
N6 C2 N1 N4 -8.4(2) . . . . ?
N1 C1 N2 N3 -0.35(17) . . . . ?
C1 C1 N2 N3 178.71(19) 3_565 . . . ?
N1 C2 N3 N2 -0.49(17) . . . . ?
N6 C2 N3 N2 177.18(17) . . . . ?
C1 N2 N3 C2 0.52(17) . . . . ?
C1 N1 N4 N5 -94.23(18) . . . . ?
C2 N1 N4 N5 98.67(16) . . . . ?
N1 N4 N5 O1 -0.4(2) . . . . ?
N1 N4 N5 O2 179.00(12) . . . . ?
N3 C2 N6 N7 9.3(3) . . . . ?
N1 C2 N6 N7 -173.19(13) . . . . ?
C2 N6 N7 O4 5.0(2) . . . . ?
C2 N6 N7 O3 -175.71(13) . . . . ?

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
_geom_hbond_publ_flag
O5 H5B O4 0.86 2.26 2.9974(18) 143.7 2_645 yes
O5 H5B O2 0.86 2.31 3.0000(19) 137.7 . yes
O5 H5A N2 0.90 2.15 2.9682(19) 151.1 3_565 yes
N11 H11B O1 0.89 2.43 3.076(2) 129.8 2_646 yes
N11 H11B N6 0.89 2.69 3.250(2) 122.0 4_566 yes
N11 H11A O3 0.89 2.33 2.966(2) 128.4 2_746 yes
N10 H10C N9 0.93 1.99 2.914(2) 173.7 . yes
N10 H10B O3 0.89 2.31 2.974(2) 130.8 2_746 yes
N10 H10B O1 0.89 2.32 3.015(2) 134.9 4_666 yes
N10 H10A O3 0.89 2.26 2.997(2) 140.2 4_566 yes
N10 H10A N7 0.89 2.68 3.485(2) 151.3 4_566 yes
N10 H10A N6 0.89 2.28 3.035(2) 143.2 4_566 yes
N9 H9B N3 0.89 2.26 3.143(2) 168.9 3_666 yes
N9 H9A O5 0.89 2.09 2.969(2) 168.3 4_666 yes
N8 H8C O2 0.92 2.04 2.7948(18) 137.9 . yes
N8 H8B O4 0.89 2.36 3.005(2) 129.6 2_645 yes
N8 H8B N3 0.89 2.07 2.904(2) 155.4 2_645 yes
N8 H8A O2 0.89 2.11 2.917(2) 150.1 4_566 yes
N8 H8A N4 0.89 2.48 3.124(2) 130.2 4_566 yes

_refine_diff_density_max         0.319
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.051



####################################################################### 
# 
# 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_LQ191122_a
_database_code_depnum_ccdc_archive 'CCDC 1980544'
loop_
_audit_author_name
_audit_author_address
langqing
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2020-01-29 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H2 N14 O8, 2(H4 N)'
_chemical_formula_sum            'C4 H10 N16 O8'
_chemical_formula_weight         410.28

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/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                   7.3769(14)
_cell_length_b                   13.894(3)
_cell_length_c                   7.3845(13)
_cell_angle_alpha                90
_cell_angle_beta                 99.407(6)
_cell_angle_gamma                90
_cell_volume                     746.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3049
_cell_measurement_theta_min      3.16
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_F_000             420
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.168
_shelx_estimated_absorpt_T_min   0.964
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6267
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            5967
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.157
_diffrn_reflns_theta_max         27.642
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             1711
_reflns_number_gt                1290
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0653P)²+0.4802P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1711
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1414
_refine_ls_wR_factor_gt          0.1301
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
C1 C 0.3775(3) 0.51195(14) 0.1815(3) 0.0280(5) Uani 1 1 d . . . . .
C2 C 0.0884(3) 0.49094(13) 0.0557(3) 0.0286(4) Uani 1 1 d . . . . .
N1 N 0.2335(2) 0.55341(11) 0.0703(2) 0.0275(4) Uani 1 1 d . . . . .
N2 N 0.1327(2) 0.41391(12) 0.1535(3) 0.0350(5) Uani 1 1 d . . . . .
N3 N 0.3126(2) 0.42830(12) 0.2297(3) 0.0336(4) Uani 1 1 d . . . . .
H3 H 0.362554 0.397586 0.321447 0.050 Uiso 1 1 d R U . . .
N4 N 0.2438(3) 0.64120(12) -0.0191(2) 0.0336(4) Uani 1 1 d . . . . .
N5 N 0.1659(3) 0.70771(12) 0.0701(3) 0.0385(5) Uani 1 1 d . . . . .
N6 N 0.5405(2) 0.55666(13) 0.2099(2) 0.0350(4) Uani 1 1 d . . . . .
N7 N 0.6736(3) 0.50953(15) 0.3244(3) 0.0407(5) Uani 1 1 d . . . . .
N8 N 0.1055(4) 0.7236(2) 0.5983(3) 0.0787(9) Uani 1 1 d . . . . .
H8A H 0.199418 0.753468 0.545805 0.118 Uiso 1 1 d R U . . .
H8B H 0.054226 0.753545 0.489314 0.118 Uiso 1 1 d R U . . .
H8C H 0.088981 0.783501 0.651900 0.118 Uiso 1 1 d R U . . .
H8D H 0.113370 0.667779 0.664217 0.118 Uiso 1 1 d R U . . .
O1 O 0.1628(3) 0.78935(11) -0.0025(3) 0.0642(6) Uani 1 1 d . . . . .
O2 O 0.0986(3) 0.69267(13) 0.2101(3) 0.0607(6) Uani 1 1 d . . . . .
O3 O 0.8279(2) 0.54453(17) 0.3395(3) 0.0645(6) Uani 1 1 d . . . . .
O4 O 0.6403(2) 0.43598(13) 0.4092(2) 0.0498(5) 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
C1 N3 1.328(3) . ?
C1 N6 1.340(3) . ?
C1 N1 1.359(3) . ?
C2 N2 1.302(3) . ?
C2 N1 1.369(3) . ?
C2 C2 1.446(4) 3_565 ?
N1 N4 1.395(2) . ?
N2 N3 1.368(3) . ?
N3 H3 0.8337 . ?
N4 N5 1.320(3) . ?
N5 O2 1.235(3) . ?
N5 O1 1.253(2) . ?
N6 N7 1.355(3) . ?
N7 O3 1.226(3) . ?
N7 O4 1.244(3) . ?
N8 H8A 0.9432 . ?
N8 H8B 0.9293 . ?
N8 H8C 0.9380 . ?
N8 H8D 0.9129 . ?

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
N3 C1 N6 135.86(19) . . ?
N3 C1 N1 104.64(17) . . ?
N6 C1 N1 119.40(18) . . ?
N2 C2 N1 110.81(18) . . ?
N2 C2 C2 125.5(2) . 3_565 ?
N1 C2 C2 123.7(2) . 3_565 ?
C1 N1 C2 107.60(16) . . ?
C1 N1 N4 123.98(16) . . ?
C2 N1 N4 128.29(17) . . ?
C2 N2 N3 104.28(16) . . ?
C1 N3 N2 112.66(16) . . ?
C1 N3 H3 122.4 . . ?
N2 N3 H3 122.0 . . ?
N5 N4 N1 108.33(16) . . ?
O2 N5 O1 122.0(2) . . ?
O2 N5 N4 124.50(17) . . ?
O1 N5 N4 113.5(2) . . ?
C1 N6 N7 114.46(19) . . ?
O3 N7 O4 122.5(2) . . ?
O3 N7 N6 115.6(2) . . ?
O4 N7 N6 121.93(19) . . ?
H8A N8 H8B 70.7 . . ?
H8A N8 H8C 86.5 . . ?
H8B N8 H8C 84.6 . . ?
H8A N8 H8D 127.3 . . ?
H8B N8 H8D 145.4 . . ?
H8C N8 H8D 122.0 . . ?

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
N3 C1 N1 C2 -0.7(2) . . . . ?
N6 C1 N1 C2 176.35(18) . . . . ?
N3 C1 N1 N4 -176.85(17) . . . . ?
N6 C1 N1 N4 0.2(3) . . . . ?
N2 C2 N1 C1 1.0(2) . . . . ?
C2 C2 N1 C1 -178.3(2) 3_565 . . . ?
N2 C2 N1 N4 176.90(18) . . . . ?
C2 C2 N1 N4 -2.4(4) 3_565 . . . ?
N1 C2 N2 N3 -0.8(2) . . . . ?
C2 C2 N2 N3 178.5(3) 3_565 . . . ?
N6 C1 N3 N2 -176.1(2) . . . . ?
N1 C1 N3 N2 0.3(2) . . . . ?
C2 N2 N3 C1 0.3(2) . . . . ?
C1 N1 N4 N5 -103.3(2) . . . . ?
C2 N1 N4 N5 81.5(2) . . . . ?
N1 N4 N5 O2 0.9(3) . . . . ?
N1 N4 N5 O1 -178.00(18) . . . . ?
N3 C1 N6 N7 -4.7(3) . . . . ?
N1 C1 N6 N7 179.33(17) . . . . ?
C1 N6 N7 O3 173.65(18) . . . . ?
C1 N6 N7 O4 -6.8(3) . . . . ?

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
_geom_hbond_publ_flag
N3 H3 O1 0.83 2.04 2.774(3) 146.5 2_545 yes
N3 H3 O4 0.83 2.11 2.562(2) 113.4 . yes
N8 H8B O2 0.93 2.30 2.891(3) 120.9 . yes
N8 H8C N6 0.94 2.30 3.219(3) 165.9 4_576 yes
N8 H8C O1 0.94 2.52 3.049(3) 115.8 1_556 yes
N8 H8D N2 0.91 2.68 3.340(4) 129.7 3_566 yes
N8 H8D N4 0.91 2.41 3.065(3) 129.0 1_556 yes
N8 H8D O4 0.91 2.45 2.910(3) 111.5 3_666 yes

_refine_diff_density_max         0.228
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.056



####################################################################### 
# 
# 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_Lq191203_a
_database_code_depnum_ccdc_archive 'CCDC 1980545'
loop_
_audit_author_name
_audit_author_address
langqing
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2020-01-29 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 K2 N14 O11, H2 O'
_chemical_formula_sum            'C4 H10 K2 N14 O12'
_chemical_formula_weight         524.46

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'
K K 0.2009 0.2494 '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                   7.1556(18)
_cell_length_b                   9.681(3)
_cell_length_c                   14.024(4)
_cell_angle_alpha                100.925(8)
_cell_angle_beta                 95.155(8)
_cell_angle_gamma                104.206(8)
_cell_volume                     915.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6841
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_F_000             532
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    0.616
_shelx_estimated_absorpt_T_min   0.827
_shelx_estimated_absorpt_T_max   0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6276
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            13490
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.393
_diffrn_reflns_theta_max         27.533
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             4169
_reflns_number_gt                3261
_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 (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)+(0.0510P)²+0.6749P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4169
_refine_ls_number_parameters     294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1129
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
C1 C 0.5149(3) 0.1970(2) 0.68489(15) 0.0225(4) Uani 1 1 d . . . . .
C2 C 0.4938(3) 0.0605(2) 0.53802(15) 0.0240(4) Uani 1 1 d . . . . .
C3 C 0.0140(3) 0.4482(2) 0.95827(14) 0.0225(4) Uani 1 1 d . . . . .
C4 C 0.0135(3) 0.3418(2) 0.80556(15) 0.0232(4) Uani 1 1 d . . . . .
K1 K -0.07867(8) -0.17673(6) 0.62208(4) 0.03847(16) Uani 1 1 d . . . . .
K2 K 0.60143(8) 0.72128(6) 0.90470(4) 0.03862(16) Uani 1 1 d . . . . .
N1 N 0.5423(2) 0.07001(18) 0.63610(12) 0.0221(4) Uani 1 1 d . . . . .
N2 N 0.4379(3) 0.17382(19) 0.52302(13) 0.0281(4) Uani 1 1 d . . . . .
N3 N 0.4525(3) 0.25800(19) 0.61510(13) 0.0260(4) Uani 1 1 d . . . . .
H3 H 0.424569 0.340555 0.626533 0.031 Uiso 1 1 calc R U . . .
N4 N 0.6253(3) -0.02379(19) 0.68018(13) 0.0272(4) Uani 1 1 d . . . . .
N5 N 0.4855(3) -0.1411(2) 0.68271(14) 0.0297(4) Uani 1 1 d . . . . .
N6 N 0.5537(3) 0.23268(19) 0.78331(13) 0.0270(4) Uani 1 1 d . . . . .
N7 N 0.5124(3) 0.3549(2) 0.82633(13) 0.0287(4) Uani 1 1 d . . . . .
N8 N 0.0723(3) 0.33274(19) 0.96345(13) 0.0271(4) Uani 1 1 d . . . . .
N9 N 0.0709(3) 0.26715(19) 0.86764(13) 0.0265(4) Uani 1 1 d . . . . .
H9 H 0.103334 0.187263 0.849801 0.032 Uiso 1 1 calc R U . . .
N10 N -0.0202(2) 0.46017(18) 0.86287(12) 0.0226(4) Uani 1 1 d . . . . .
N11 N -0.0226(3) 0.3215(2) 0.70727(13) 0.0306(4) Uani 1 1 d . . . . .
N12 N 0.0137(3) 0.2012(2) 0.65657(14) 0.0337(4) Uani 1 1 d . . . . .
N13 N -0.0985(3) 0.5626(2) 0.82691(13) 0.0280(4) Uani 1 1 d . . . . .
N14 N 0.0373(3) 0.6878(2) 0.84374(14) 0.0290(4) Uani 1 1 d . . . . .
O1 O 0.5452(3) -0.23843(19) 0.71244(13) 0.0434(4) Uani 1 1 d . . . . .
O2 O 0.3118(3) -0.1568(2) 0.65500(17) 0.0527(5) Uani 1 1 d . . . . .
O3 O 0.5471(3) 0.3884(2) 0.91723(12) 0.0423(4) Uani 1 1 d . . . . .
O4 O 0.4436(2) 0.43159(18) 0.77866(12) 0.0370(4) Uani 1 1 d . . . . .
O5 O 0.0878(3) 0.12043(18) 0.69700(13) 0.0394(4) Uani 1 1 d . . . . .
O6 O -0.0314(3) 0.1758(2) 0.56630(13) 0.0544(5) Uani 1 1 d . . . . .
O7 O -0.0221(3) 0.78986(19) 0.81930(14) 0.0427(4) Uani 1 1 d . . . . .
O8 O 0.2066(2) 0.7084(2) 0.88402(15) 0.0445(5) Uani 1 1 d . . . . .
O9 O -0.1101(6) -0.4707(3) 0.5909(2) 0.1237(14) Uani 1 1 d . . . . .
H9A H -0.214181 -0.516906 0.552089 0.186 Uiso 1 1 d R U . . .
H9B H -0.114431 -0.496666 0.645409 0.186 Uiso 1 1 d R U . . .
O10 O 0.6369(4) 1.0281(3) 0.91132(18) 0.0815(8) Uani 1 1 d . . . . .
H10A H 0.680196 1.049678 0.860010 0.122 Uiso 1 1 d R U . . .
H10B H 0.724190 1.080133 0.958247 0.122 Uiso 1 1 d R U . . .
O11 O 0.7591(3) 0.9416(2) 1.10006(15) 0.0541(5) Uani 1 1 d . . . . .
H11A H 0.666941 0.972179 1.122822 0.081 Uiso 1 1 d R U . . .
H11B H 0.837199 1.017240 1.089767 0.081 Uiso 1 1 d R U . . .
O12 O 0.3415(5) 0.4958(2) 0.5829(2) 0.0845(9) Uani 1 1 d G . . . .
H12A H 0.444076 0.501541 0.555978 0.127 Uiso 1 1 d G U . . .
H12B H 0.367004 0.574438 0.626571 0.127 Uiso 1 1 d G 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
C1 N3 1.333(3) . ?
C1 N6 1.343(3) . ?
C1 N1 1.357(3) . ?
C2 N2 1.302(3) . ?
C2 N1 1.368(3) . ?
C2 C2 1.453(4) 2_656 ?
C3 N8 1.298(3) . ?
C3 N10 1.370(3) . ?
C3 C3 1.453(4) 2_567 ?
C4 N9 1.330(3) . ?
C4 N11 1.347(3) . ?
C4 N10 1.356(3) . ?
K1 O2 2.7436(19) . ?
K1 O9 2.745(3) . ?
K1 O5 2.7832(19) . ?
K1 O6 2.825(2) 2_556 ?
K1 O7 2.850(2) 1_545 ?
K1 N4 2.9555(19) 1_455 ?
K1 O1 3.053(2) 1_455 ?
K1 N2 3.141(2) 2_556 ?
K1 N5 3.386(2) 1_455 ?
K1 K2 4.8917(13) 1_445 ?
K2 O8 2.7836(18) . ?
K2 O1 2.8044(19) 1_565 ?
K2 O10 2.901(3) . ?
K2 O4 2.9108(18) . ?
K2 O7 3.022(2) 1_655 ?
K2 N8 3.055(2) 2_667 ?
K2 O11 3.062(2) . ?
K2 O3 3.069(2) 2_667 ?
K2 N13 3.093(2) 1_655 ?
K2 O3 3.191(2) . ?
K2 N14 3.381(2) 1_655 ?
N1 N4 1.404(2) . ?
N2 N3 1.370(2) . ?
N3 H3 0.8600 . ?
N4 N5 1.325(3) . ?
N5 O2 1.231(3) . ?
N5 O1 1.249(2) . ?
N6 N7 1.336(3) . ?
N7 O3 1.241(2) . ?
N7 O4 1.244(2) . ?
N8 N9 1.371(2) . ?
N9 H9 0.8600 . ?
N10 N13 1.401(2) . ?
N11 N12 1.341(3) . ?
N12 O5 1.237(3) . ?
N12 O6 1.240(3) . ?
N13 N14 1.319(3) . ?
N14 O8 1.242(2) . ?
N14 O7 1.258(2) . ?
O9 H9A 0.8501 . ?
O9 H9B 0.8499 . ?
O10 H10A 0.8499 . ?
O10 H10B 0.8500 . ?
O11 H11A 0.8500 . ?
O11 H11B 0.8500 . ?
O12 H12A 0.8500 . ?
O12 H12B 0.8500 . ?

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
N3 C1 N6 135.77(19) . . ?
N3 C1 N1 105.03(17) . . ?
N6 C1 N1 119.20(18) . . ?
N2 C2 N1 110.99(17) . . ?
N2 C2 C2 125.4(2) . 2_656 ?
N1 C2 C2 123.6(2) . 2_656 ?
N8 C3 N10 111.12(17) . . ?
N8 C3 C3 125.1(2) . 2_567 ?
N10 C3 C3 123.7(2) . 2_567 ?
N9 C4 N11 135.4(2) . . ?
N9 C4 N10 105.29(17) . . ?
N11 C4 N10 119.26(19) . . ?
O2 K1 O9 82.62(9) . . ?
O2 K1 O5 76.86(6) . . ?
O9 K1 O5 157.32(8) . . ?
O2 K1 O6 77.59(6) . 2_556 ?
O9 K1 O6 89.58(9) . 2_556 ?
O5 K1 O6 95.27(6) . 2_556 ?
O2 K1 O7 76.96(6) . 1_545 ?
O9 K1 O7 79.54(7) . 1_545 ?
O5 K1 O7 86.47(6) . 1_545 ?
O6 K1 O7 153.37(6) 2_556 1_545 ?
O2 K1 N4 142.67(6) . 1_455 ?
O9 K1 N4 128.01(10) . 1_455 ?
O5 K1 N4 68.39(5) . 1_455 ?
O6 K1 N4 117.92(6) 2_556 1_455 ?
O7 K1 N4 87.46(5) 1_545 1_455 ?
O2 K1 O1 143.29(6) . 1_455 ?
O9 K1 O1 87.33(10) . 1_455 ?
O5 K1 O1 103.42(5) . 1_455 ?
O6 K1 O1 137.74(6) 2_556 1_455 ?
O7 K1 O1 66.50(5) 1_545 1_455 ?
N4 K1 O1 42.12(5) 1_455 1_455 ?
O2 K1 N2 148.20(6) . 2_556 ?
O9 K1 N2 100.99(8) . 2_556 ?
O5 K1 N2 101.53(5) . 2_556 ?
O6 K1 N2 70.90(6) 2_556 2_556 ?
O7 K1 N2 134.84(5) 1_545 2_556 ?
N4 K1 N2 56.35(5) 1_455 2_556 ?
O1 K1 N2 68.41(5) 1_455 2_556 ?
O2 K1 N5 156.05(6) . 1_455 ?
O9 K1 N5 105.16(10) . 1_455 ?
O5 K1 N5 90.34(5) . 1_455 ?
O6 K1 N5 124.30(5) 2_556 1_455 ?
O7 K1 N5 82.18(5) 1_545 1_455 ?
N4 K1 N5 22.85(5) 1_455 1_455 ?
O1 K1 N5 21.57(4) 1_455 1_455 ?
N2 K1 N5 53.74(5) 2_556 1_455 ?
O2 K1 K2 111.55(5) . 1_445 ?
O9 K1 K2 81.51(8) . 1_445 ?
O5 K1 K2 97.05(4) . 1_445 ?
O6 K1 K2 166.09(5) 2_556 1_445 ?
O7 K1 K2 34.72(4) 1_545 1_445 ?
N4 K1 K2 61.51(4) 1_455 1_445 ?
O1 K1 K2 31.80(3) 1_455 1_445 ?
N2 K1 K2 100.21(4) 2_556 1_445 ?
N5 K1 K2 49.33(3) 1_455 1_445 ?
O8 K2 O1 79.73(6) . 1_565 ?
O8 K2 O10 81.83(7) . . ?
O1 K2 O10 70.99(6) 1_565 . ?
O8 K2 O4 80.04(5) . . ?
O1 K2 O4 73.50(5) 1_565 . ?
O10 K2 O4 142.38(6) . . ?
O8 K2 O7 146.67(6) . 1_655 ?
O1 K2 O7 67.47(5) 1_565 1_655 ?
O10 K2 O7 82.08(7) . 1_655 ?
O4 K2 O7 95.59(5) . 1_655 ?
O8 K2 N8 143.24(6) . 2_667 ?
O1 K2 N8 136.13(6) 1_565 2_667 ?
O10 K2 N8 113.62(7) . 2_667 ?
O4 K2 N8 100.44(5) . 2_667 ?
O7 K2 N8 70.09(5) 1_655 2_667 ?
O8 K2 O11 102.39(6) . . ?
O1 K2 O11 131.11(6) 1_565 . ?
O10 K2 O11 61.28(6) . . ?
O4 K2 O11 155.39(6) . . ?
O7 K2 O11 95.09(6) 1_655 . ?
N8 K2 O11 62.85(5) 2_667 . ?
O8 K2 O3 74.73(6) . 2_667 ?
O1 K2 O3 152.24(6) 1_565 2_667 ?
O10 K2 O3 115.16(6) . 2_667 ?
O4 K2 O3 91.32(5) . 2_667 ?
O7 K2 O3 138.59(5) 1_655 2_667 ?
N8 K2 O3 68.50(5) 2_667 2_667 ?
O11 K2 O3 66.30(6) . 2_667 ?
O8 K2 N13 143.15(6) . 1_655 ?
O1 K2 N13 84.06(5) 1_565 1_655 ?
O10 K2 N13 123.40(7) . 1_655 ?
O4 K2 N13 63.63(5) . 1_655 ?
O7 K2 N13 41.32(5) 1_655 1_655 ?
N8 K2 N13 56.19(5) 2_667 1_655 ?
O11 K2 N13 113.13(6) . 1_655 ?
O3 K2 N13 110.32(5) 2_667 1_655 ?
O8 K2 O3 96.04(5) . . ?
O1 K2 O3 113.74(5) 1_565 . ?
O10 K2 O3 174.48(6) . . ?
O4 K2 O3 41.32(5) . . ?
O7 K2 O3 102.22(5) 1_655 . ?
N8 K2 O3 65.30(5) 2_667 . ?
O11 K2 O3 114.52(5) . . ?
O3 K2 O3 59.32(5) 2_667 . ?
N13 K2 O3 60.98(5) 1_655 . ?
O8 K2 N14 159.68(6) . 1_655 ?
O1 K2 N14 82.64(5) 1_565 1_655 ?
O10 K2 N14 101.90(7) . 1_655 ?
O4 K2 N14 85.34(5) . 1_655 ?
O7 K2 N14 21.74(4) 1_655 1_655 ?
N8 K2 N14 53.49(5) 2_667 1_655 ?
O11 K2 N14 96.79(6) . 1_655 ?
O3 K2 N14 119.93(5) 2_667 1_655 ?
N13 K2 N14 22.96(5) 1_655 1_655 ?
O3 K2 N14 81.87(5) . 1_655 ?
O8 K2 K1 114.62(4) . 1_665 ?
O1 K2 K1 35.00(4) 1_565 1_665 ?
O10 K2 K1 74.88(5) . 1_665 ?
O4 K2 K1 83.20(4) . 1_665 ?
O7 K2 K1 32.48(3) 1_655 1_665 ?
N8 K2 K1 101.82(4) 2_667 1_665 ?
O11 K2 K1 116.63(5) . 1_665 ?
O3 K2 K1 167.92(4) 2_667 1_665 ?
N13 K2 K1 57.61(4) 1_655 1_665 ?
O3 K2 K1 110.60(3) . 1_665 ?
N14 K2 K1 49.06(3) 1_655 1_665 ?
C1 N1 C2 107.45(16) . . ?
C1 N1 N4 124.69(17) . . ?
C2 N1 N4 127.54(16) . . ?
C2 N2 N3 104.44(16) . . ?
C2 N2 K1 127.40(14) . 2_556 ?
N3 N2 K1 113.78(12) . 2_556 ?
C1 N3 N2 112.09(17) . . ?
C1 N3 H3 124.0 . . ?
N2 N3 H3 124.0 . . ?
N5 N4 N1 108.62(16) . . ?
N5 N4 K1 97.13(12) . 1_655 ?
N1 N4 K1 131.43(12) . 1_655 ?
O2 N5 O1 122.1(2) . . ?
O2 N5 N4 123.69(18) . . ?
O1 N5 N4 114.16(18) . . ?
O2 N5 K1 147.53(16) . 1_655 ?
O1 N5 K1 64.02(12) . 1_655 ?
N4 N5 K1 60.01(11) . 1_655 ?
N7 N6 C1 115.65(17) . . ?
O3 N7 O4 121.54(19) . . ?
O3 N7 N6 116.04(19) . . ?
O4 N7 N6 122.42(18) . . ?
C3 N8 N9 104.49(16) . . ?
C3 N8 K2 132.96(14) . 2_667 ?
N9 N8 K2 110.11(12) . 2_667 ?
C4 N9 N8 111.94(17) . . ?
C4 N9 H9 124.0 . . ?
N8 N9 H9 124.0 . . ?
C4 N10 C3 107.13(16) . . ?
C4 N10 N13 124.28(17) . . ?
C3 N10 N13 128.16(17) . . ?
N12 N11 C4 115.11(19) . . ?
O5 N12 O6 121.9(2) . . ?
O5 N12 N11 122.31(19) . . ?
O6 N12 N11 115.8(2) . . ?
N14 N13 N10 108.82(16) . . ?
N14 N13 K2 90.89(12) . 1_455 ?
N10 N13 K2 130.40(12) . 1_455 ?
O8 N14 O7 121.60(19) . . ?
O8 N14 N13 124.59(18) . . ?
O7 N14 N13 113.73(18) . . ?
O8 N14 K2 139.15(15) . 1_455 ?
O7 N14 K2 62.85(11) . 1_455 ?
N13 N14 K2 66.14(11) . 1_455 ?
N5 O1 K2 128.75(14) . 1_545 ?
N5 O1 K1 94.41(13) . 1_655 ?
K2 O1 K1 113.20(6) 1_545 1_655 ?
N5 O2 K1 171.47(18) . . ?
N7 O3 K2 139.49(14) . 2_667 ?
N7 O3 K2 88.26(13) . . ?
K2 O3 K2 120.68(5) 2_667 . ?
N7 O4 K2 101.61(12) . . ?
N12 O5 K1 114.56(14) . . ?
N12 O6 K1 149.84(16) . 2_556 ?
N14 O7 K1 123.75(14) . 1_565 ?
N14 O7 K2 95.40(12) . 1_455 ?
K1 O7 K2 112.80(6) 1_565 1_455 ?
N14 O8 K2 159.45(16) . . ?
K1 O9 H9A 109.1 . . ?
K1 O9 H9B 109.0 . . ?
H9A O9 H9B 109.5 . . ?
K2 O10 H10A 109.1 . . ?
K2 O10 H10B 109.6 . . ?
H10A O10 H10B 104.5 . . ?
K2 O11 H11A 109.6 . . ?
K2 O11 H11B 109.2 . . ?
H11A O11 H11B 104.5 . . ?
H12A O12 H12B 104.5 . . ?

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
N3 C1 N1 C2 -0.2(2) . . . . ?
N6 C1 N1 C2 -179.69(19) . . . . ?
N3 C1 N1 N4 173.71(18) . . . . ?
N6 C1 N1 N4 -5.8(3) . . . . ?
N2 C2 N1 C1 0.0(2) . . . . ?
C2 C2 N1 C1 179.3(3) 2_656 . . . ?
N2 C2 N1 N4 -173.69(19) . . . . ?
C2 C2 N1 N4 5.7(4) 2_656 . . . ?
N1 C2 N2 N3 0.2(2) . . . . ?
C2 C2 N2 N3 -179.1(3) 2_656 . . . ?
N1 C2 N2 K1 -135.93(15) . . . 2_556 ?
C2 C2 N2 K1 44.7(4) 2_656 . . 2_556 ?
N6 C1 N3 N2 179.7(2) . . . . ?
N1 C1 N3 N2 0.3(2) . . . . ?
C2 N2 N3 C1 -0.3(2) . . . . ?
K1 N2 N3 C1 142.69(14) 2_556 . . . ?
C1 N1 N4 N5 106.6(2) . . . . ?
C2 N1 N4 N5 -80.8(2) . . . . ?
C1 N1 N4 K1 -135.23(17) . . . 1_655 ?
C2 N1 N4 K1 37.4(3) . . . 1_655 ?
N1 N4 N5 O2 -3.6(3) . . . . ?
K1 N4 N5 O2 -141.8(2) 1_655 . . . ?
N1 N4 N5 O1 173.84(17) . . . . ?
K1 N4 N5 O1 35.60(18) 1_655 . . . ?
N1 N4 N5 K1 138.23(16) . . . 1_655 ?
N3 C1 N6 N7 4.4(4) . . . . ?
N1 C1 N6 N7 -176.26(18) . . . . ?
C1 N6 N7 O3 179.73(19) . . . . ?
C1 N6 N7 O4 -0.4(3) . . . . ?
N10 C3 N8 N9 -1.3(2) . . . . ?
C3 C3 N8 N9 178.1(3) 2_567 . . . ?
N10 C3 N8 K2 135.21(16) . . . 2_667 ?
C3 C3 N8 K2 -45.4(4) 2_567 . . 2_667 ?
N11 C4 N9 N8 -175.6(2) . . . . ?
N10 C4 N9 N8 1.0(2) . . . . ?
C3 N8 N9 C4 0.2(2) . . . . ?
K2 N8 N9 C4 -147.37(14) 2_667 . . . ?
N9 C4 N10 C3 -1.7(2) . . . . ?
N11 C4 N10 C3 175.49(19) . . . . ?
N9 C4 N10 N13 -174.68(18) . . . . ?
N11 C4 N10 N13 2.5(3) . . . . ?
N8 C3 N10 C4 2.0(2) . . . . ?
C3 C3 N10 C4 -177.4(2) 2_567 . . . ?
N8 C3 N10 N13 174.58(19) . . . . ?
C3 C3 N10 N13 -4.9(4) 2_567 . . . ?
N9 C4 N11 N12 -3.4(4) . . . . ?
N10 C4 N11 N12 -179.57(18) . . . . ?
C4 N11 N12 O5 -4.8(3) . . . . ?
C4 N11 N12 O6 175.2(2) . . . . ?
C4 N10 N13 N14 -111.7(2) . . . . ?
C3 N10 N13 N14 76.9(2) . . . . ?
C4 N10 N13 K2 140.17(16) . . . 1_455 ?
C3 N10 N13 K2 -31.3(3) . . . 1_455 ?
N10 N13 N14 O8 0.8(3) . . . . ?
K2 N13 N14 O8 134.4(2) 1_455 . . . ?
N10 N13 N14 O7 -175.97(17) . . . . ?
K2 N13 N14 O7 -42.33(17) 1_455 . . . ?
N10 N13 N14 K2 -133.64(16) . . . 1_455 ?
O2 N5 O1 K2 -92.0(3) . . . 1_545 ?
N4 N5 O1 K2 90.5(2) . . . 1_545 ?
K1 N5 O1 K2 124.64(17) 1_655 . . 1_545 ?
O2 N5 O1 K1 143.3(2) . . . 1_655 ?
N4 N5 O1 K1 -34.12(18) . . . 1_655 ?
O4 N7 O3 K2 111.9(2) . . . 2_667 ?
N6 N7 O3 K2 -68.2(3) . . . 2_667 ?
O4 N7 O3 K2 -26.7(2) . . . . ?
N6 N7 O3 K2 153.18(16) . . . . ?
O3 N7 O4 K2 30.2(2) . . . . ?
N6 N7 O4 K2 -149.70(16) . . . . ?
O6 N12 O5 K1 -42.1(3) . . . . ?
N11 N12 O5 K1 137.98(17) . . . . ?
O5 N12 O6 K1 -76.3(4) . . . 2_556 ?
N11 N12 O6 K1 103.6(3) . . . 2_556 ?
O8 N14 O7 K1 104.9(2) . . . 1_565 ?
N13 N14 O7 K1 -78.3(2) . . . 1_565 ?
K2 N14 O7 K1 -122.10(15) 1_455 . . 1_565 ?
O8 N14 O7 K2 -133.04(19) . . . 1_455 ?
N13 N14 O7 K2 43.80(18) . . . 1_455 ?
O7 N14 O8 K2 -94.3(4) . . . . ?
N13 N14 O8 K2 89.2(4) . . . . ?
K2 N14 O8 K2 -178.2(2) 1_455 . . . ?

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
_geom_hbond_publ_flag
N3 H3 O4 0.86 2.13 2.590(2) 113.3 . yes
N3 H3 O12 0.86 1.93 2.713(3) 151.6 . yes
N9 H9 O5 0.86 2.10 2.570(2) 113.6 . yes
N9 H9 O11 0.86 1.96 2.688(3) 142.0 2_667 yes
O9 H9A O12 0.85 2.09 2.756(4) 134.3 2_556 yes
O9 H9B N11 0.85 2.31 2.964(3) 134.1 1_545 yes
O9 H9B N13 0.85 2.49 3.256(4) 150.9 1_545 yes
O10 H10A N4 0.85 2.45 3.175(3) 143.0 1_565 yes
O10 H10A N6 0.85 2.54 3.039(3) 118.5 1_565 yes
O10 H10B O8 0.85 2.63 3.353(3) 143.7 2_677 yes
O10 H10B O11 0.85 2.63 3.042(3) 111.4 . yes
O11 H11A O10 0.85 2.18 2.913(4) 143.9 2_677 yes
O11 H11B O7 0.85 2.11 2.771(3) 134.5 2_677 yes

_refine_diff_density_max         0.637
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.061



