# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2022

####################################################################### 
# 
# 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_bwn19040
_database_code_depnum_ccdc_archive 'CCDC 2078916'
loop_
_audit_author_name
_audit_author_address
'Haibo Li'
;Beijing institute of technology
China
;
_audit_update_record             
;
2021-12-09 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_audit_creation_date             2019-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H10 Ca N8 O6'
_chemical_formula_sum            'C3 H10 Ca N8 O6'
_chemical_formula_weight         294.27
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Ca Ca 0.2262 0.3064 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.5466(13)
_cell_length_b                   12.561(3)
_cell_length_c                   13.047(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1072.9(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3924
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      1.5608
_shelx_estimated_absorpt_T_max   0.940
_shelx_estimated_absorpt_T_min   0.923
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4309
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.123
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.575
_reflns_Friedel_fraction_full    0.871
_reflns_Friedel_fraction_max     0.803
_reflns_number_gt                2214
_reflns_number_total             2250
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 
;
 Flack x determined using 785 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.96(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0320P)²+1.0948P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0831
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Ca1 Ca 0.20891(9) 0.24183(5) 0.18253(5) 0.01222(16) Uani 1 1 d . . . . .
O1 O 0.1681(4) 0.11566(18) 0.34868(17) 0.0175(5) Uani 1 1 d . . . . .
O2 O 0.5447(4) 0.20911(18) 0.26024(17) 0.0147(5) Uani 1 1 d . . . . .
H2A H 0.582015 0.260745 0.296628 0.018 Uiso 1 1 d R . . . .
H2B H 0.553635 0.168135 0.310928 0.018 Uiso 1 1 d R . . . .
O3 O -0.0464(4) 0.37520(19) 0.16181(18) 0.0192(6) Uani 1 1 d . . . . .
H3A H -0.082783 0.425258 0.200389 0.023 Uiso 1 1 d R . . . .
H3B H -0.071433 0.403848 0.105009 0.023 Uiso 1 1 d R . . . .
O4 O 0.4357(4) 0.39124(18) 0.13152(19) 0.0186(5) Uani 1 1 d . . . . .
H4A H 0.399376 0.442893 0.094920 0.022 Uiso 1 1 d R . . . .
H4B H 0.523976 0.421503 0.168040 0.022 Uiso 1 1 d R . . . .
O5 O 0.1728(4) 0.2532(2) 0.00147(16) 0.0179(5) Uani 1 1 d . . . . .
H5A H 0.244053 0.291883 -0.036979 0.021 Uiso 1 1 d R . . . .
H5B H 0.123213 0.200553 -0.029509 0.021 Uiso 1 1 d R . . . .
O6 O -0.1039(4) 0.14520(18) 0.15976(18) 0.0164(5) Uani 1 1 d . . . . .
H6A H -0.207088 0.163590 0.193703 0.020 Uiso 1 1 d R . . . .
H6B H -0.125878 0.079350 0.161903 0.020 Uiso 1 1 d R . . . .
N1 N 0.1612(4) 0.3317(2) 0.3583(2) 0.0135(6) Uani 1 1 d . . . . .
N2 N 0.1555(4) 0.4317(2) 0.3912(2) 0.0150(6) Uani 1 1 d . . . . .
N3 N 0.1447(5) 0.4332(2) 0.4930(2) 0.0156(6) Uani 1 1 d . . . . .
N4 N 0.1431(5) 0.3327(2) 0.5279(2) 0.0156(6) Uani 1 1 d . . . . .
N5 N 0.3516(4) -0.1193(2) 0.1243(2) 0.0144(6) Uani 1 1 d . . . . .
N6 N 0.3429(4) -0.0306(2) 0.1800(2) 0.0160(6) Uani 1 1 d . . . . .
N7 N 0.3292(5) 0.0532(2) 0.1179(2) 0.0152(6) Uani 1 1 d . . . . .
N8 N 0.3320(4) 0.0200(2) 0.0209(2) 0.0142(6) Uani 1 1 d . . . . .
C1 C 0.1534(5) 0.2726(2) 0.4439(2) 0.0118(6) Uani 1 1 d . . . . .
C2 C 0.1576(5) 0.1551(2) 0.4350(2) 0.0121(6) Uani 1 1 d . . . . .
C3 C 0.3448(5) -0.0866(2) 0.0265(3) 0.0122(6) 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
Ca1 O1 2.699(2) . ?
Ca1 O2 2.456(2) . ?
Ca1 O3 2.382(3) . ?
Ca1 O4 2.484(2) . ?
Ca1 O5 2.378(2) . ?
Ca1 O6 2.399(2) . ?
Ca1 N1 2.576(3) . ?
Ca1 N7 2.635(3) . ?
O1 C2 1.233(4) . ?
O2 H2A 0.8400 . ?
O2 H2B 0.8401 . ?
O3 H3A 0.8399 . ?
O3 H3B 0.8400 . ?
O4 H4A 0.8399 . ?
O4 H4B 0.8400 . ?
O5 H5A 0.8400 . ?
O5 H5B 0.8401 . ?
O6 H6A 0.8399 . ?
O6 H6B 0.8400 . ?
N1 N2 1.327(4) . ?
N1 C1 1.342(4) . ?
N2 N3 1.329(4) . ?
N3 N4 1.343(4) . ?
N4 C1 1.333(4) . ?
N5 N6 1.332(4) . ?
N5 C3 1.341(4) . ?
N6 N7 1.332(4) . ?
N7 N8 1.333(4) . ?
N8 C3 1.344(4) . ?
C1 C2 1.480(4) . ?
C2 C3 1.471(4) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O1 70.04(8) . . ?
O2 Ca1 O4 72.66(8) . . ?
O2 Ca1 N1 79.29(8) . . ?
O2 Ca1 N7 73.39(8) . . ?
O3 Ca1 O1 115.77(8) . . ?
O3 Ca1 O2 142.45(9) . . ?
O3 Ca1 O4 81.81(8) . . ?
O3 Ca1 O6 75.09(9) . . ?
O3 Ca1 N1 73.00(8) . . ?
O3 Ca1 N7 143.68(9) . . ?
O4 Ca1 O1 135.90(8) . . ?
O4 Ca1 N1 88.84(8) . . ?
O4 Ca1 N7 114.51(9) . . ?
O5 Ca1 O1 145.41(8) . . ?
O5 Ca1 O2 120.61(8) . . ?
O5 Ca1 O3 77.02(8) . . ?
O5 Ca1 O4 75.40(9) . . ?
O5 Ca1 O6 79.78(8) . . ?
O5 Ca1 N1 147.79(9) . . ?
O5 Ca1 N7 76.45(9) . . ?
O6 Ca1 O1 73.61(8) . . ?
O6 Ca1 O2 136.95(8) . . ?
O6 Ca1 O4 149.24(9) . . ?
O6 Ca1 N1 103.22(9) . . ?
O6 Ca1 N7 76.16(9) . . ?
N1 Ca1 O1 61.98(8) . . ?
N1 Ca1 N7 135.69(9) . . ?
N7 Ca1 O1 76.04(8) . . ?
C2 O1 Ca1 120.3(2) . . ?
Ca1 O2 H2A 111.4 . . ?
Ca1 O2 H2B 119.3 . . ?
H2A O2 H2B 90.5 . . ?
Ca1 O3 H3A 131.1 . . ?
Ca1 O3 H3B 122.6 . . ?
H3A O3 H3B 98.8 . . ?
Ca1 O4 H4A 124.5 . . ?
Ca1 O4 H4B 127.0 . . ?
H4A O4 H4B 99.7 . . ?
Ca1 O5 H5A 124.9 . . ?
Ca1 O5 H5B 118.0 . . ?
H5A O5 H5B 112.5 . . ?
Ca1 O6 H6A 118.8 . . ?
Ca1 O6 H6B 129.8 . . ?
H6A O6 H6B 96.7 . . ?
N2 N1 Ca1 134.9(2) . . ?
N2 N1 C1 104.7(3) . . ?
C1 N1 Ca1 120.1(2) . . ?
N1 N2 N3 109.8(3) . . ?
N2 N3 N4 109.0(3) . . ?
C1 N4 N3 104.6(3) . . ?
N6 N5 C3 105.1(2) . . ?
N7 N6 N5 109.4(3) . . ?
N6 N7 Ca1 122.4(2) . . ?
N6 N7 N8 109.2(2) . . ?
N8 N7 Ca1 126.1(2) . . ?
N7 N8 C3 105.1(3) . . ?
N1 C1 C2 119.1(3) . . ?
N4 C1 N1 111.9(3) . . ?
N4 C1 C2 129.0(3) . . ?
O1 C2 C1 118.2(3) . . ?
O1 C2 C3 120.5(3) . 2 ?
C3 C2 C1 121.3(3) 2 . ?
N5 C3 N8 111.1(3) . . ?
N5 C3 C2 126.4(3) . 2_554 ?
N8 C3 C2 122.5(3) . 2_554 ?

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
Ca1 O1 C2 C1 4.2(4) . . . . ?
Ca1 O1 C2 C3 -174.1(2) . . . 2 ?
Ca1 N1 N2 N3 -174.4(2) . . . . ?
Ca1 N1 C1 N4 175.5(2) . . . . ?
Ca1 N1 C1 C2 -4.4(4) . . . . ?
Ca1 N7 N8 C3 -162.4(2) . . . . ?
N1 N2 N3 N4 0.0(4) . . . . ?
N1 C1 C2 O1 0.0(5) . . . . ?
N1 C1 C2 C3 178.3(3) . . . 2 ?
N2 N1 C1 N4 0.0(4) . . . . ?
N2 N1 C1 C2 -179.8(3) . . . . ?
N2 N3 N4 C1 0.0(4) . . . . ?
N3 N4 C1 N1 0.0(4) . . . . ?
N3 N4 C1 C2 179.8(3) . . . . ?
N4 C1 C2 O1 -179.8(3) . . . . ?
N4 C1 C2 C3 -1.5(5) . . . 2 ?
N5 N6 N7 Ca1 163.1(2) . . . . ?
N5 N6 N7 N8 -0.9(4) . . . . ?
N6 N5 C3 N8 0.0(4) . . . . ?
N6 N5 C3 C2 -177.5(3) . . . 2_554 ?
N6 N7 N8 C3 0.8(4) . . . . ?
N7 N8 C3 N5 -0.5(4) . . . . ?
N7 N8 C3 C2 177.1(3) . . . 2_554 ?
C1 N1 N2 N3 0.0(4) . . . . ?
C3 N5 N6 N7 0.6(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_bwn18406
_database_code_depnum_ccdc_archive 'CCDC 2078913'
loop_
_audit_author_name
_audit_author_address
'Haibo Li'
;Beijing institute of technology
China
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_audit_creation_date             2021-12-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 K0.498 N8 O Rb1.502'
_chemical_formula_sum            'C3 K0.50 N8 O Rb1.50'
_chemical_formula_weight         311.86
_chemical_melting_point          ?
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'
K K 0.2009 0.2494 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.4887(9)
_cell_length_b                   7.5710(15)
_cell_length_c                   12.714(3)
_cell_angle_alpha                97.31(3)
_cell_angle_beta                 92.74(3)
_cell_angle_gamma                106.32(3)
_cell_volume                     409.70(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1348
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      1.6211
_shelx_estimated_absorpt_T_max   0.260
_shelx_estimated_absorpt_T_min   0.225
_exptl_absorpt_coefficient_mu    9.226
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             294
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3076
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.834
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1318
_reflns_number_total             1429
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1429
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0301P)²+0.4046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0742
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{Rb1, K1}
{Rb2, K2}
2. Uiso/Uaniso restraints and constraints
Uanis(Rb1) = Uanis(K1)
Uanis(Rb2) = Uanis(K2)
3. Others
 Sof(K1)=1-FVAR(1)
 Sof(Rb1)=FVAR(1)
 Sof(K2)=1-FVAR(2)
 Sof(Rb2)=FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Rb1 Rb 0.60770(9) 0.29246(6) 0.08066(3) 0.01676(18) Uani 0.908(7) 1 d . . P A 1
Rb2 Rb 0.76016(11) 1.20330(7) 0.39987(4) 0.0174(2) Uani 0.593(6) 1 d . . P B 1
O1 O 0.2337(6) 0.5442(4) 0.1215(2) 0.0229(7) Uani 1 1 d . . . . .
N5 N 0.5298(8) 0.8005(5) 0.3805(3) 0.0205(8) Uani 1 1 d . . . . .
N4 N 0.1883(8) 0.9880(5) 0.2456(3) 0.0210(9) Uani 1 1 d . . . . .
N8 N 0.6049(8) 0.5386(5) 0.3011(3) 0.0217(8) Uani 1 1 d . . . . .
N7 N 0.7557(8) 0.5845(5) 0.3982(3) 0.0234(9) Uani 1 1 d . . . . .
N2 N -0.1544(8) 0.9625(5) 0.1108(3) 0.0230(9) Uani 1 1 d . . . . .
N3 N 0.0026(8) 1.0743(5) 0.1984(3) 0.0210(8) Uani 1 1 d . . . . .
N6 N 0.7098(8) 0.7410(5) 0.4457(3) 0.0229(9) Uani 1 1 d . . . . .
N1 N -0.0688(8) 0.8058(5) 0.0993(3) 0.0213(9) Uani 1 1 d . . . . .
C3 C 0.4695(9) 0.6730(5) 0.2919(3) 0.0153(9) Uani 1 1 d . . . . .
C2 C 0.2774(9) 0.6742(6) 0.1950(3) 0.0167(9) Uani 1 1 d . . . . .
C1 C 0.1375(9) 0.8253(6) 0.1829(3) 0.0146(9) Uani 1 1 d . . . . .
K1 K 0.60770(9) 0.29246(6) 0.08066(3) 0.01676(18) Uani 0.092(7) 1 d . . P A 2
K2 K 0.76016(11) 1.20330(7) 0.39987(4) 0.0174(2) Uani 0.407(6) 1 d . . P B 2


_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
Rb1 O1 2.890(3) . ?
Rb1 O1 3.022(3) 2_665 ?
Rb1 O1 2.898(3) 1_655 ?
Rb1 N8 3.165(4) . ?
Rb1 N2 3.039(4) 1_645 ?
Rb1 N2 3.149(4) 2_565 ?
Rb1 N3 3.183(4) 1_645 ?
Rb1 N1 3.109(4) 2_565 ?
Rb2 N5 3.137(3) 2_676 ?
Rb2 N5 2.905(4) . ?
Rb2 N4 3.073(4) . ?
Rb2 N8 3.198(4) 1_565 ?
Rb2 N7 2.894(4) 1_565 ?
Rb2 N3 2.988(3) 1_655 ?
Rb2 N6 3.028(4) 2_676 ?
Rb2 N6 2.910(4) 2_776 ?
O1 C2 1.233(5) . ?
O1 K1 2.890(3) . ?
N5 N6 1.335(5) . ?
N5 C3 1.349(5) . ?
N5 K2 2.905(4) . ?
N4 N3 1.357(5) . ?
N4 C1 1.334(5) . ?
N4 K2 3.073(4) . ?
N8 N7 1.335(5) . ?
N8 C3 1.338(5) . ?
N8 K1 3.165(4) . ?
N7 N6 1.333(5) . ?
N2 N3 1.343(5) . ?
N2 N1 1.339(5) . ?
N1 C1 1.341(5) . ?
C3 C2 1.472(6) . ?
C2 C1 1.472(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Rb1 O1 101.72(9) . 1_655 ?
O1 Rb1 O1 87.74(8) . 2_665 ?
O1 Rb1 O1 73.19(9) 1_655 2_665 ?
O1 Rb1 N8 54.29(9) . . ?
O1 Rb1 N8 122.98(8) 2_665 . ?
O1 Rb1 N8 75.28(9) 1_655 . ?
O1 Rb1 N2 156.11(9) . 1_645 ?
O1 Rb1 N2 70.98(9) 2_665 2_565 ?
O1 Rb1 N2 115.45(9) 2_665 1_645 ?
O1 Rb1 N2 139.63(9) 1_655 2_565 ?
O1 Rb1 N2 91.08(9) 1_655 1_645 ?
O1 Rb1 N2 94.89(9) . 2_565 ?
O1 Rb1 N3 142.04(8) . 1_645 ?
O1 Rb1 N3 125.04(8) 2_665 1_645 ?
O1 Rb1 N3 74.49(9) 1_655 1_645 ?
O1 Rb1 N1 136.65(9) 1_655 2_565 ?
O1 Rb1 N1 63.95(9) 2_665 2_565 ?
O1 Rb1 N1 71.31(9) . 2_565 ?
N8 Rb1 N3 89.10(9) . 1_645 ?
N2 Rb1 N8 141.50(9) 2_565 . ?
N2 Rb1 N8 111.38(10) 1_645 . ?
N2 Rb1 N2 87.92(10) 1_645 2_565 ?
N2 Rb1 N3 24.78(9) 1_645 1_645 ?
N2 Rb1 N3 112.51(9) 2_565 1_645 ?
N2 Rb1 N1 112.45(10) 1_645 2_565 ?
N1 Rb1 N8 123.10(9) 2_565 . ?
N1 Rb1 N2 24.70(9) 2_565 2_565 ?
N1 Rb1 N3 136.75(9) 2_565 1_645 ?
N5 Rb2 N5 84.80(10) . 2_676 ?
N5 Rb2 N4 59.75(10) . . ?
N5 Rb2 N8 105.28(9) 2_676 1_565 ?
N5 Rb2 N8 139.33(10) . 1_565 ?
N5 Rb2 N3 76.70(10) . 1_655 ?
N5 Rb2 N6 92.79(10) . 2_676 ?
N5 Rb2 N6 97.96(10) . 2_776 ?
N4 Rb2 N5 101.45(9) . 2_676 ?
N4 Rb2 N8 79.58(10) . 1_565 ?
N7 Rb2 N5 159.41(10) 1_565 . ?
N7 Rb2 N5 90.53(10) 1_565 2_676 ?
N7 Rb2 N4 101.87(10) 1_565 . ?
N7 Rb2 N8 24.68(9) 1_565 1_565 ?
N7 Rb2 N3 108.47(10) 1_565 1_655 ?
N7 Rb2 N6 75.38(10) 1_565 2_676 ?
N7 Rb2 N6 100.35(11) 1_565 2_776 ?
N3 Rb2 N5 160.90(9) 1_655 2_676 ?
N3 Rb2 N4 73.36(9) 1_655 . ?
N3 Rb2 N8 92.03(9) 1_655 1_565 ?
N3 Rb2 N6 158.61(10) 1_655 2_676 ?
N6 Rb2 N5 75.99(9) 2_776 2_676 ?
N6 Rb2 N5 24.92(9) 2_676 2_676 ?
N6 Rb2 N4 85.25(9) 2_676 . ?
N6 Rb2 N4 157.66(10) 2_776 . ?
N6 Rb2 N8 122.67(10) 2_776 1_565 ?
N6 Rb2 N8 83.86(10) 2_676 1_565 ?
N6 Rb2 N3 101.65(10) 2_776 1_655 ?
N6 Rb2 N6 98.19(10) 2_776 2_676 ?
Rb1 O1 Rb1 106.81(9) 1_455 2_665 ?
Rb1 O1 Rb1 101.72(9) . 1_455 ?
Rb1 O1 Rb1 92.26(8) . 2_665 ?
C2 O1 Rb1 107.9(3) . 2_665 ?
C2 O1 Rb1 127.5(3) . . ?
C2 O1 Rb1 116.8(2) . 1_455 ?
C2 O1 K1 127.5(3) . . ?
Rb2 N5 Rb2 95.20(10) . 2_676 ?
N6 N5 Rb2 108.9(2) . . ?
N6 N5 Rb2 73.0(2) . 2_676 ?
N6 N5 C3 104.2(3) . . ?
N6 N5 K2 108.9(2) . . ?
C3 N5 Rb2 128.9(3) . . ?
C3 N5 Rb2 131.7(3) . 2_676 ?
C3 N5 K2 128.9(3) . . ?
Rb2 N4 Rb1 110.05(10) 1_455 1_565 ?
Rb2 N4 Rb1 79.94(8) . 1_565 ?
Rb2 N4 Rb2 87.80(9) . 1_455 ?
N3 N4 Rb1 69.0(2) . 1_565 ?
N3 N4 Rb2 61.31(19) . 1_455 ?
N3 N4 Rb2 122.3(3) . . ?
N3 N4 K2 122.3(3) . . ?
C1 N4 Rb1 100.3(2) . 1_565 ?
C1 N4 Rb2 128.9(2) . . ?
C1 N4 Rb2 136.3(2) . 1_455 ?
C1 N4 N3 104.3(3) . . ?
C1 N4 K2 128.9(2) . . ?
Rb1 N8 Rb2 83.88(8) . 1_545 ?
N7 N8 Rb1 140.1(3) . . ?
N7 N8 Rb2 64.8(2) . 1_545 ?
N7 N8 C3 104.6(3) . . ?
N7 N8 K1 140.1(3) . . ?
C3 N8 Rb1 112.9(3) . . ?
C3 N8 Rb2 157.3(3) . 1_545 ?
C3 N8 K1 112.9(3) . . ?
Rb2 N7 Rb2 101.48(11) 1_545 2_776 ?
N8 N7 Rb2 162.8(3) . 2_776 ?
N8 N7 Rb2 90.5(2) . 1_545 ?
N6 N7 Rb2 150.7(3) . 1_545 ?
N6 N7 Rb2 64.8(2) . 2_776 ?
N6 N7 N8 109.4(3) . . ?
Rb1 N2 Rb1 92.08(10) 1_465 2_565 ?
N3 N2 Rb1 171.9(2) . 2_565 ?
N3 N2 Rb1 83.7(2) . 1_465 ?
N1 N2 Rb1 76.0(2) . 2_565 ?
N1 N2 Rb1 166.4(3) . 1_465 ?
N1 N2 N3 109.0(3) . . ?
Rb1 N3 Rb1 87.73(9) 1_465 1_565 ?
Rb2 N3 Rb1 128.91(12) 1_455 1_565 ?
Rb2 N3 Rb1 87.06(9) 1_455 1_465 ?
N4 N3 Rb1 176.1(3) . 1_465 ?
N4 N3 Rb1 88.3(2) . 1_565 ?
N4 N3 Rb2 95.2(2) . 1_455 ?
N2 N3 Rb1 96.6(2) . 1_565 ?
N2 N3 Rb1 71.6(2) . 1_465 ?
N2 N3 Rb2 129.2(2) . 1_455 ?
N2 N3 N4 109.2(3) . . ?
Rb2 N6 Rb2 102.77(10) 2_776 . ?
Rb2 N6 Rb2 98.19(10) 2_776 2_676 ?
Rb2 N6 Rb2 84.79(9) 2_676 . ?
N5 N6 Rb2 50.4(2) . . ?
N5 N6 Rb2 82.1(2) . 2_676 ?
N5 N6 Rb2 153.1(3) . 2_776 ?
N7 N6 Rb2 140.7(2) . . ?
N7 N6 Rb2 90.7(2) . 2_776 ?
N7 N6 Rb2 130.1(3) . 2_676 ?
N7 N6 N5 109.7(3) . . ?
Rb1 N1 Rb1 88.69(8) 2_565 2_665 ?
N2 N1 Rb1 79.3(2) . 2_565 ?
N2 N1 Rb1 124.1(2) . 2_665 ?
N2 N1 C1 105.1(3) . . ?
C1 N1 Rb1 94.9(2) . 2_665 ?
C1 N1 Rb1 171.2(3) . 2_565 ?
N5 C3 C2 125.9(4) . . ?
N8 C3 N5 112.0(4) . . ?
N8 C3 C2 122.0(4) . . ?
Rb1 C2 Rb1 82.34(9) 2_665 1_455 ?
O1 C2 Rb1 45.6(2) . 1_455 ?
O1 C2 Rb1 53.1(2) . 2_665 ?
O1 C2 C3 118.6(4) . . ?
O1 C2 C1 119.1(4) . . ?
C3 C2 Rb1 123.9(3) . 1_455 ?
C3 C2 Rb1 136.9(2) . 2_665 ?
C3 C2 C1 122.3(3) . . ?
C1 C2 Rb1 81.3(2) . 2_665 ?
C1 C2 Rb1 97.0(2) . 1_455 ?
N4 C1 Rb1 131.4(3) . 2_665 ?
N4 C1 N1 112.4(4) . . ?
N4 C1 C2 128.4(4) . . ?
N1 C1 Rb1 63.8(2) . 2_665 ?
N1 C1 C2 119.1(3) . . ?
C2 C1 Rb1 75.3(2) . 2_665 ?
O1 K1 O1 87.74(8) . 2_665 ?
O1 K1 O1 101.72(9) . 1_655 ?
O1 K1 O1 73.19(9) 1_655 2_665 ?
O1 K1 N8 54.29(9) . . ?
O1 K1 N8 75.28(9) 1_655 . ?
O1 K1 N8 122.98(8) 2_665 . ?
O1 K1 N2 139.63(9) 1_655 2_565 ?
O1 K1 N2 115.45(9) 2_665 1_645 ?
O1 K1 N2 91.08(9) 1_655 1_645 ?
O1 K1 N2 94.89(9) . 2_565 ?
O1 K1 N2 70.98(9) 2_665 2_565 ?
O1 K1 N2 156.11(9) . 1_645 ?
O1 K1 N3 74.49(9) 1_655 1_645 ?
O1 K1 N3 125.04(8) 2_665 1_645 ?
O1 K1 N3 142.04(8) . 1_645 ?
O1 K1 N1 63.95(9) 2_665 2_565 ?
O1 K1 N1 71.31(9) . 2_565 ?
O1 K1 N1 136.65(9) 1_655 2_565 ?
N8 K1 N3 89.10(9) . 1_645 ?
N2 K1 N8 111.38(10) 1_645 . ?
N2 K1 N8 141.50(9) 2_565 . ?
N2 K1 N2 87.92(10) 1_645 2_565 ?
N2 K1 N3 24.78(9) 1_645 1_645 ?
N2 K1 N3 112.51(9) 2_565 1_645 ?
N2 K1 N1 112.45(10) 1_645 2_565 ?
N1 K1 N8 123.10(9) 2_565 . ?
N1 K1 N2 24.70(9) 2_565 2_565 ?
N1 K1 N3 136.75(9) 2_565 1_645 ?
N5 K2 N5 84.80(10) . 2_676 ?
N5 K2 N4 59.75(10) . . ?
N5 K2 N8 105.28(9) 2_676 1_565 ?
N5 K2 N8 139.33(10) . 1_565 ?
N5 K2 N3 76.70(10) . 1_655 ?
N5 K2 N6 92.79(10) . 2_676 ?
N5 K2 N6 97.96(10) . 2_776 ?
N4 K2 N5 101.45(9) . 2_676 ?
N4 K2 N8 79.58(10) . 1_565 ?
N7 K2 N5 90.53(10) 1_565 2_676 ?
N7 K2 N5 159.41(10) 1_565 . ?
N7 K2 N4 101.87(10) 1_565 . ?
N7 K2 N8 24.68(9) 1_565 1_565 ?
N7 K2 N3 108.47(10) 1_565 1_655 ?
N7 K2 N6 100.35(11) 1_565 2_776 ?
N7 K2 N6 75.38(10) 1_565 2_676 ?
N3 K2 N5 160.90(9) 1_655 2_676 ?
N3 K2 N4 73.36(9) 1_655 . ?
N3 K2 N8 92.03(9) 1_655 1_565 ?
N3 K2 N6 158.61(10) 1_655 2_676 ?
N6 K2 N5 24.92(9) 2_676 2_676 ?
N6 K2 N5 75.99(9) 2_776 2_676 ?
N6 K2 N4 85.25(9) 2_676 . ?
N6 K2 N4 157.66(10) 2_776 . ?
N6 K2 N8 122.67(10) 2_776 1_565 ?
N6 K2 N8 83.86(10) 2_676 1_565 ?
N6 K2 N3 101.65(10) 2_776 1_655 ?
N6 K2 N6 98.19(10) 2_776 2_676 ?

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
Rb1 O1 C2 Rb1 -132.4(4) . . . 1_455 ?
Rb1 O1 C2 Rb1 120.2(3) 2_665 . . 1_455 ?
Rb1 O1 C2 Rb1 -120.2(3) 1_455 . . 2_665 ?
Rb1 O1 C2 Rb1 107.4(3) . . . 2_665 ?
Rb1 O1 C2 C3 -129.1(3) 2_665 . . . ?
Rb1 O1 C2 C3 110.8(3) 1_455 . . . ?
Rb1 O1 C2 C3 -21.6(5) . . . . ?
Rb1 O1 C2 C1 50.7(4) 2_665 . . . ?
Rb1 O1 C2 C1 158.2(3) . . . . ?
Rb1 O1 C2 C1 -69.5(4) 1_455 . . . ?
Rb1 N4 N3 Rb2 -128.93(13) 1_565 . . 1_455 ?
Rb1 N4 N3 N2 96.4(3) 1_565 . . . ?
Rb1 N4 C1 Rb1 3.5(3) 1_565 . . 2_665 ?
Rb1 N4 C1 N1 -70.7(3) 1_565 . . . ?
Rb1 N4 C1 C2 109.0(4) 1_565 . . . ?
Rb1 N8 N7 Rb2 92.9(9) . . . 2_776 ?
Rb1 N8 N7 Rb2 -41.8(4) . . . 1_545 ?
Rb1 N8 N7 N6 160.0(3) . . . . ?
Rb1 N8 C3 N5 -166.3(2) . . . . ?
Rb1 N8 C3 C2 14.1(5) . . . . ?
Rb1 N2 N3 Rb1 -85.39(10) 1_465 . . 1_565 ?
Rb1 N2 N3 Rb2 70.0(3) 1_465 . . 1_455 ?
Rb1 N2 N3 N4 -175.9(3) 1_465 . . . ?
Rb1 N2 N1 Rb1 -29.4(11) 1_465 . . 2_565 ?
Rb1 N2 N1 Rb1 81.1(2) 2_565 . . 2_665 ?
Rb1 N2 N1 Rb1 51.7(12) 1_465 . . 2_665 ?
Rb1 N2 N1 C1 -172.2(3) 2_565 . . . ?
Rb1 N2 N1 C1 158.5(10) 1_465 . . . ?
Rb1 N1 C1 N4 126.4(3) 2_665 . . . ?
Rb1 N1 C1 C2 -53.3(4) 2_665 . . . ?
Rb1 C2 C1 Rb1 -81.11(10) 1_455 . . 2_665 ?
Rb1 C2 C1 N4 -131.6(4) 2_665 . . . ?
Rb1 C2 C1 N4 147.3(4) 1_455 . . . ?
Rb1 C2 C1 N1 48.1(3) 2_665 . . . ?
Rb1 C2 C1 N1 -33.1(4) 1_455 . . . ?
Rb2 N5 N6 Rb2 89.74(14) . . . 2_676 ?
Rb2 N5 N6 Rb2 -89.74(14) 2_676 . . . ?
Rb2 N5 N6 Rb2 -92.6(5) 2_676 . . 2_776 ?
Rb2 N5 N6 Rb2 -2.9(6) . . . 2_776 ?
Rb2 N5 N6 N7 -140.4(3) . . . . ?
Rb2 N5 N6 N7 129.8(3) 2_676 . . . ?
Rb2 N5 C3 N8 129.4(3) . . . . ?
Rb2 N5 C3 N8 -79.5(4) 2_676 . . . ?
Rb2 N5 C3 C2 -51.0(5) . . . . ?
Rb2 N5 C3 C2 100.1(4) 2_676 . . . ?
Rb2 N4 N3 Rb1 62.4(2) . . . 1_565 ?
Rb2 N4 N3 Rb1 128.93(13) 1_455 . . 1_565 ?
Rb2 N4 N3 Rb2 -66.6(2) . . . 1_455 ?
Rb2 N4 N3 N2 158.8(2) . . . . ?
Rb2 N4 N3 N2 -134.7(3) 1_455 . . . ?
Rb2 N4 C1 Rb1 -81.9(4) . . . 2_665 ?
Rb2 N4 C1 Rb1 137.5(2) 1_455 . . 2_665 ?
Rb2 N4 C1 N1 -156.0(3) . . . . ?
Rb2 N4 C1 N1 63.4(5) 1_455 . . . ?
Rb2 N4 C1 C2 -116.9(4) 1_455 . . . ?
Rb2 N4 C1 C2 23.7(6) . . . . ?
Rb2 N8 N7 Rb2 134.7(9) 1_545 . . 2_776 ?
Rb2 N8 N7 N6 -158.2(3) 1_545 . . . ?
Rb2 N8 C3 N5 58.7(8) 1_545 . . . ?
Rb2 N8 C3 C2 -120.9(6) 1_545 . . . ?
Rb2 N7 N6 Rb2 67.0(5) 1_545 . . 2_776 ?
Rb2 N7 N6 Rb2 178.4(2) 1_545 . . . ?
Rb2 N7 N6 Rb2 -34.3(7) 1_545 . . 2_676 ?
Rb2 N7 N6 Rb2 -101.4(3) 2_776 . . 2_676 ?
Rb2 N7 N6 Rb2 111.4(4) 2_776 . . . ?
Rb2 N7 N6 N5 162.2(3) 2_776 . . . ?
Rb2 N7 N6 N5 -130.7(5) 1_545 . . . ?
O1 C2 C1 Rb1 -38.8(3) . . . 2_665 ?
O1 C2 C1 N4 -170.4(4) . . . . ?
O1 C2 C1 N1 9.3(6) . . . . ?
N5 C3 C2 Rb1 117.3(4) . . . 2_665 ?
N5 C3 C2 Rb1 -123.9(4) . . . 1_455 ?
N5 C3 C2 O1 -177.4(4) . . . . ?
N5 C3 C2 C1 2.8(6) . . . . ?
N8 N7 N6 Rb2 -162.5(3) . . . 2_776 ?
N8 N7 N6 Rb2 -51.1(5) . . . . ?
N8 N7 N6 Rb2 96.1(4) . . . 2_676 ?
N8 N7 N6 N5 -0.3(4) . . . . ?
N8 C3 C2 Rb1 55.7(5) . . . 1_455 ?
N8 C3 C2 Rb1 -63.2(5) . . . 2_665 ?
N8 C3 C2 O1 2.1(6) . . . . ?
N8 C3 C2 C1 -177.6(4) . . . . ?
N7 N8 C3 N5 -0.3(5) . . . . ?
N7 N8 C3 C2 -179.9(3) . . . . ?
N2 N1 C1 Rb1 -127.2(3) . . . 2_665 ?
N2 N1 C1 N4 -0.8(4) . . . . ?
N2 N1 C1 C2 179.4(3) . . . . ?
N3 N4 C1 Rb1 74.3(4) . . . 2_665 ?
N3 N4 C1 N1 0.1(4) . . . . ?
N3 N4 C1 C2 179.8(4) . . . . ?
N3 N2 N1 Rb1 173.4(3) . . . 2_565 ?
N3 N2 N1 Rb1 -105.6(3) . . . 2_665 ?
N3 N2 N1 C1 1.2(4) . . . . ?
N6 N5 C3 N8 0.2(5) . . . . ?
N6 N5 C3 C2 179.7(4) . . . . ?
N1 N2 N3 Rb1 174.7(3) . . . 1_465 ?
N1 N2 N3 Rb1 89.3(3) . . . 1_565 ?
N1 N2 N3 Rb2 -115.2(3) . . . 1_455 ?
N1 N2 N3 N4 -1.2(4) . . . . ?
C3 N5 N6 Rb2 137.6(5) . . . 2_776 ?
C3 N5 N6 Rb2 -129.8(3) . . . 2_676 ?
C3 N5 N6 Rb2 140.5(4) . . . . ?
C3 N5 N6 N7 0.1(4) . . . . ?
C3 N8 N7 Rb2 158.5(3) . . . 1_545 ?
C3 N8 N7 Rb2 -66.8(10) . . . 2_776 ?
C3 N8 N7 N6 0.4(4) . . . . ?
C3 C2 C1 Rb1 141.0(4) . . . 2_665 ?
C3 C2 C1 N4 9.4(6) . . . . ?
C3 C2 C1 N1 -171.0(3) . . . . ?
C1 N4 N3 Rb1 -95.7(3) . . . 1_565 ?
C1 N4 N3 Rb2 135.3(3) . . . 1_455 ?
C1 N4 N3 N2 0.6(4) . . . . ?
K1 O1 C2 C3 -21.6(5) . . . . ?
K1 O1 C2 C1 158.2(3) . . . . ?
K1 N8 N7 N6 160.0(3) . . . . ?
K1 N8 C3 N5 -166.3(2) . . . . ?
K1 N8 C3 C2 14.1(5) . . . . ?
K2 N5 N6 N7 -140.4(3) . . . . ?
K2 N5 C3 N8 129.4(3) . . . . ?
K2 N5 C3 C2 -51.0(5) . . . . ?
K2 N4 N3 N2 158.8(2) . . . . ?
K2 N4 C1 N1 -156.0(3) . . . . ?
K2 N4 C1 C2 23.7(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_a_pl
_database_code_depnum_ccdc_archive 'CCDC 2078909'
loop_
_audit_author_name
_audit_author_address
'Haibo Li'
;Beijing institute of technology
China
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_audit_creation_date             2021-12-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H16 N16 Na4 O10, H4 O2'
_chemical_formula_sum            'C6 H20 N16 Na4 O12'
_chemical_formula_weight         600.34
_chemical_melting_point          ?
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'
Na Na 0.0362 0.0249 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   6.8000(14)
_cell_length_b                   7.5000(15)
_cell_length_c                   24.200(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1234.2(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2821
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.6926
_shelx_estimated_absorpt_T_max   0.968
_shelx_estimated_absorpt_T_min   0.955
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2553
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         3.112
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1096
_reflns_number_total             1138
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0844
_refine_ls_restrained_S_all      1.264
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+10.7696P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.1878
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H3B(0.5)
3.a Riding coordinates:
 O2(H2A,H2B), O1(H1A,H1B), O3(H3A,H3B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Na1 Na -0.1031(4) 0.250000 0.56896(11) 0.0180(7) Uani 1 2 d S T P . .
Na2 Na 0.1743(4) 0.250000 0.75415(11) 0.0166(7) Uani 1 2 d S T P . .
N2 N 0.3238(10) 0.250000 0.6625(3) 0.0291(19) Uani 1 2 d S T P . .
O2 O -0.0994(5) 0.5353(5) 0.60833(15) 0.0225(9) Uani 1 1 d . . . . .
H2A H -0.205643 0.586432 0.600340 0.027 Uiso 1 1 d R U . . .
H2B H -0.005753 0.590552 0.593510 0.027 Uiso 1 1 d R U . . .
O4 O 0.1654(8) 0.250000 0.5019(2) 0.0239(14) Uani 1 2 d S T P . .
N5 N 0.6857(9) 0.250000 0.4835(3) 0.0221(16) Uani 1 2 d S T P . .
N1 N 0.2341(9) 0.250000 0.6139(3) 0.0252(17) Uani 1 2 d S T P . .
N3 N 0.5167(9) 0.250000 0.6552(3) 0.0231(16) Uani 1 2 d S T P . .
O1 O -0.0624(6) 0.0373(7) 0.72180(16) 0.0363(12) Uani 1 1 d . . . . .
H1A H -0.084364 0.000604 0.689567 0.044 Uiso 1 1 d R U . . .
H1B H -0.146244 0.015304 0.746337 0.044 Uiso 1 1 d R U . . .
N8 N 0.4486(9) 0.250000 0.4213(2) 0.0176(14) Uani 1 2 d S T P . .
N4 N 0.5559(9) 0.250000 0.6006(2) 0.0211(15) Uani 1 2 d S T P . .
N7 N 0.6194(9) 0.250000 0.3951(2) 0.0195(15) Uani 1 2 d S T P . .
C3 C 0.4925(11) 0.250000 0.4751(3) 0.0142(15) Uani 1 2 d S T P . .
N6 N 0.7623(9) 0.250000 0.4322(2) 0.0206(15) Uani 1 2 d S T P . .
C1 C 0.3793(10) 0.250000 0.5767(3) 0.0145(16) Uani 1 2 d S T P . .
C2 C 0.3352(11) 0.250000 0.5174(3) 0.0164(16) Uani 1 2 d S T P . .
O3 O 0.7088(9) 0.250000 0.2815(2) 0.043(2) Uani 1 2 d S T P . .
H3A H 0.683047 0.250000 0.315510 0.052 Uiso 1 2 d R U P . .
H3B H 0.822237 0.277980 0.270920 0.052 Uiso 0.5 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
Na1 O2 2.343(4) 8_565 ?
Na1 O2 2.343(4) . ?
Na1 O4 2.443(6) . ?
Na1 N5 2.518(7) 1_455 ?
Na1 N1 2.538(7) . ?
Na1 N4 2.441(7) 1_455 ?
Na2 Na2 3.4059(8) 6_557 ?
Na2 Na2 3.4060(8) 6_657 ?
Na2 N2 2.439(7) . ?
Na2 N3 2.442(7) 6_557 ?
Na2 O1 2.397(5) 8_565 ?
Na2 O1 2.397(5) . ?
Na2 O1 2.468(5) 6_657 ?
Na2 O1 2.468(5) 3_556 ?
N2 N1 1.324(9) . ?
N2 N3 1.324(9) . ?
O2 H2A 0.8401 . ?
O2 H2B 0.8402 . ?
O4 C2 1.214(9) . ?
N5 C3 1.330(10) . ?
N5 N6 1.346(9) . ?
N1 C1 1.337(9) . ?
N3 N4 1.348(9) . ?
O1 H1A 0.8405 . ?
O1 H1B 0.8398 . ?
N8 N7 1.324(9) . ?
N8 C3 1.334(9) . ?
N4 C1 1.333(9) . ?
N7 N6 1.324(9) . ?
C3 C2 1.482(10) . ?
C1 C2 1.465(10) . ?
O3 H3A 0.8402 . ?
O3 H3B 0.8400 . ?
O3 H3B 0.8401 8_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Na1 O2 132.0(2) 8_565 . ?
O2 Na1 O4 105.20(12) . . ?
O2 Na1 O4 105.20(12) 8_565 . ?
O2 Na1 N5 109.88(11) 8_565 1_455 ?
O2 Na1 N5 109.88(11) . 1_455 ?
O2 Na1 N1 79.40(12) 8_565 . ?
O2 Na1 N1 79.40(12) . . ?
O2 Na1 N4 83.27(12) . 1_455 ?
O2 Na1 N4 83.26(12) 8_565 1_455 ?
O4 Na1 N5 83.1(2) . 1_455 ?
O4 Na1 N1 67.0(2) . . ?
N5 Na1 N1 150.2(2) 1_455 . ?
N4 Na1 O4 156.6(2) 1_455 . ?
N4 Na1 N5 73.5(2) 1_455 1_455 ?
N4 Na1 N1 136.3(2) 1_455 . ?
Na2 Na2 Na2 173.23(18) 6_557 6_657 ?
N2 Na2 Na2 61.99(18) . 6_657 ?
N2 Na2 Na2 111.2(2) . 6_557 ?
N2 Na2 N3 178.6(2) . 6_557 ?
N2 Na2 O1 84.95(17) . 3_556 ?
N2 Na2 O1 84.95(17) . 6_657 ?
N3 Na2 Na2 119.4(2) 6_557 6_657 ?
N3 Na2 Na2 67.36(17) 6_557 6_557 ?
N3 Na2 O1 96.11(17) 6_557 6_657 ?
N3 Na2 O1 96.11(17) 6_557 3_556 ?
O1 Na2 Na2 130.60(13) . 6_657 ?
O1 Na2 Na2 130.60(13) 8_565 6_657 ?
O1 Na2 Na2 46.43(12) 8_565 6_557 ?
O1 Na2 Na2 137.59(12) 6_657 6_557 ?
O1 Na2 Na2 44.73(11) 6_657 6_657 ?
O1 Na2 Na2 46.43(11) . 6_557 ?
O1 Na2 Na2 44.73(11) 3_556 6_657 ?
O1 Na2 Na2 137.59(12) 3_556 6_557 ?
O1 Na2 N2 89.02(17) . . ?
O1 Na2 N2 89.02(17) 8_565 . ?
O1 Na2 N3 89.94(16) 8_565 6_557 ?
O1 Na2 N3 89.94(17) . 6_557 ?
O1 Na2 O1 173.83(16) . 3_556 ?
O1 Na2 O1 80.5(2) 3_556 6_657 ?
O1 Na2 O1 173.83(16) 8_565 6_657 ?
O1 Na2 O1 97.69(19) . 6_657 ?
O1 Na2 O1 83.4(2) . 8_565 ?
O1 Na2 O1 97.69(19) 8_565 3_556 ?
N1 N2 Na2 127.9(5) . . ?
N3 N2 Na2 122.4(5) . . ?
N3 N2 N1 109.7(6) . . ?
Na1 O2 H2A 108.3 . . ?
Na1 O2 H2B 106.5 . . ?
H2A O2 H2B 109.2 . . ?
C2 O4 Na1 120.3(5) . . ?
C3 N5 Na1 133.6(5) . 1_655 ?
C3 N5 N6 104.0(6) . . ?
N6 N5 Na1 122.5(5) . 1_655 ?
N2 N1 Na1 142.8(5) . . ?
N2 N1 C1 105.0(6) . . ?
C1 N1 Na1 112.2(5) . . ?
N2 N3 Na2 108.3(4) . 6_657 ?
N2 N3 N4 109.2(6) . . ?
N4 N3 Na2 142.5(5) . 6_657 ?
Na2 O1 Na2 88.85(16) . 6_557 ?
Na2 O1 H1A 107.5 6_557 . ?
Na2 O1 H1A 129.8 . . ?
Na2 O1 H1B 57.8 6_557 . ?
Na2 O1 H1B 110.8 . . ?
H1A O1 H1B 118.1 . . ?
N7 N8 C3 105.8(6) . . ?
N3 N4 Na1 119.7(5) . 1_655 ?
C1 N4 Na1 136.1(5) . 1_655 ?
C1 N4 N3 104.3(6) . . ?
N8 N7 N6 108.5(5) . . ?
N5 C3 N8 111.7(6) . . ?
N5 C3 C2 127.4(7) . . ?
N8 C3 C2 120.8(7) . . ?
N7 N6 N5 110.0(6) . . ?
N1 C1 C2 120.6(6) . . ?
N4 C1 N1 111.9(6) . . ?
N4 C1 C2 127.5(6) . . ?
O4 C2 C3 118.2(6) . . ?
O4 C2 C1 119.8(7) . . ?
C1 C2 C3 121.9(6) . . ?
H3A O3 H3B 119.4 . . ?
H3A O3 H3B 119.4 . 8_565 ?
H3B O3 H3B 28.9 . 8_565 ?

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
Na1 O4 C2 C3 180.000(2) . . . . ?
Na1 O4 C2 C1 0.000(3) . . . . ?
Na1 N5 C3 N8 180.000(2) 1_655 . . . ?
Na1 N5 C3 C2 0.000(4) 1_655 . . . ?
Na1 N5 N6 N7 180.000(2) 1_655 . . . ?
Na1 N1 C1 N4 180.000(2) . . . . ?
Na1 N1 C1 C2 0.000(3) . . . . ?
Na1 N4 C1 N1 180.000(3) 1_655 . . . ?
Na1 N4 C1 C2 0.000(5) 1_655 . . . ?
Na2 N2 N1 Na1 0.000(5) . . . . ?
Na2 N2 N1 C1 180.000(3) . . . . ?
Na2 N2 N3 Na2 0.000(3) . . . 6_657 ?
Na2 N2 N3 N4 180.000(3) . . . . ?
Na2 N3 N4 Na1 0.000(4) 6_657 . . 1_655 ?
Na2 N3 N4 C1 180.000(4) 6_657 . . . ?
N2 N1 C1 N4 0.000(3) . . . . ?
N2 N1 C1 C2 180.000(3) . . . . ?
N2 N3 N4 Na1 180.000(3) . . . 1_655 ?
N2 N3 N4 C1 0.000(4) . . . . ?
N5 C3 C2 O4 180.000(3) . . . . ?
N5 C3 C2 C1 0.000(4) . . . . ?
N1 N2 N3 Na2 180.000(2) . . . 6_657 ?
N1 N2 N3 N4 0.000(4) . . . . ?
N1 C1 C2 O4 0.000(4) . . . . ?
N1 C1 C2 C3 180.000(3) . . . . ?
N3 N2 N1 Na1 180.000(3) . . . . ?
N3 N2 N1 C1 0.000(4) . . . . ?
N3 N4 C1 N1 0.000(3) . . . . ?
N3 N4 C1 C2 180.000(3) . . . . ?
N8 N7 N6 N5 0.000(2) . . . . ?
N8 C3 C2 O4 0.000(4) . . . . ?
N8 C3 C2 C1 180.000(3) . . . . ?
N4 C1 C2 O4 180.000(3) . . . . ?
N4 C1 C2 C3 0.000(4) . . . . ?
N7 N8 C3 N5 0.000(3) . . . . ?
N7 N8 C3 C2 180.000(3) . . . . ?
C3 N5 N6 N7 0.000(2) . . . . ?
C3 N8 N7 N6 0.000(2) . . . . ?
N6 N5 C3 N8 0.000(2) . . . . ?
N6 N5 C3 C2 180.000(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_bwn18008
_database_code_depnum_ccdc_archive 'CCDC 2078919'
loop_
_audit_author_name
_audit_author_address
'Haibo Li'
;Beijing institute of technology
China
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_audit_creation_date             2021-12-13
_audit_creation_method           
;
Olex2 1.5-dev
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H2 K2 N8 O2'
_chemical_formula_sum            'C3 H2 K2 N8 O2'
_chemical_formula_weight         260.33
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
K K 0.2009 0.2494 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.1376(14)
_cell_length_b                   17.029(3)
_cell_length_c                   7.6232(15)
_cell_angle_alpha                90
_cell_angle_beta                 111.38(3)
_cell_angle_gamma                90
_cell_volume                     862.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3519
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4662
_cell_measurement_theta_min      2.2429
_shelx_estimated_absorpt_T_max   0.862
_shelx_estimated_absorpt_T_min   0.803
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6315
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.464
_diffrn_reflns_theta_min         3.109
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.744
_reflns_Friedel_fraction_full    0.835
_reflns_Friedel_fraction_max     0.783
_reflns_number_gt                3419
_reflns_number_total             3493
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 
;
 Flack x determined using 1377 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.0035(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3493
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0219P)²+0.7564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0675
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O4(H4A,H4B)
2.b Secondary CH2 refined with riding coordinates:
 O3(H3A,H3B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
K1 K 0.41658(13) 0.69837(5) 0.73024(11) 0.01803(19) Uani 1 1 d . . . . .
K2 K 0.67146(12) 0.44466(5) -0.00943(11) 0.01646(19) Uani 1 1 d . . . . .
K3 K 1.27831(13) 0.30698(5) 0.60464(12) 0.0194(2) Uani 1 1 d . . . . .
K4 K 0.96351(13) 0.05529(5) 0.64772(11) 0.01726(19) Uani 1 1 d . . . . .
O1 O 0.8139(4) 0.96627(17) 1.3056(4) 0.0197(6) Uani 1 1 d . . . . .
O2 O 0.5167(4) 0.53626(18) 0.6482(4) 0.0197(6) Uani 1 1 d . . . . .
O3 O 0.7814(5) 0.29450(19) 0.0687(4) 0.0264(7) Uani 1 1 d . . . . .
H3A H 0.927567 0.293897 0.143601 0.032 Uiso 1 1 calc R U . . .
H3B H 0.762054 0.267884 -0.052085 0.032 Uiso 1 1 calc R U . . .
O4 O 1.0671(4) 0.20834(19) 0.7445(4) 0.0206(6) Uani 1 1 d . . . . .
H4A H 0.951202 0.225909 0.724837 0.025 Uiso 1 1 d R U . . .
H4B H 1.157882 0.211119 0.851847 0.025 Uiso 1 1 d R U . . .
N1 N 0.9946(5) 1.1118(2) 1.3105(5) 0.0173(7) Uani 1 1 d . . . . .
N2 N 1.1040(5) 1.1687(2) 1.2723(5) 0.0184(7) Uani 1 1 d . . . . .
N3 N 1.1463(5) 1.1478(2) 1.1223(5) 0.0182(7) Uani 1 1 d . . . . .
N4 N 1.0654(5) 1.0780(2) 1.0581(5) 0.0169(7) Uani 1 1 d . . . . .
N5 N 0.6913(5) 0.8672(2) 0.9982(5) 0.0172(7) Uani 1 1 d . . . . .
N6 N 0.6703(5) 0.8333(2) 0.8341(5) 0.0193(7) Uani 1 1 d . . . . .
N7 N 0.7755(5) 0.8733(2) 0.7514(5) 0.0196(7) Uani 1 1 d . . . . .
N8 N 0.8642(5) 0.9350(2) 0.8593(4) 0.0175(7) Uani 1 1 d . . . . .
N9 N 0.4243(5) 0.6427(2) 0.3578(4) 0.0178(7) Uani 1 1 d . . . . .
N10 N 0.4024(5) 0.6775(2) 0.1928(5) 0.0199(8) Uani 1 1 d . . . . .
N11 N 0.4827(5) 0.6319(2) 0.0965(5) 0.0192(7) Uani 1 1 d . . . . .
N12 N 0.5588(5) 0.5664(2) 0.1965(5) 0.0181(7) Uani 1 1 d . . . . .
N13 N 0.6710(5) 0.3866(2) 0.6316(5) 0.0170(7) Uani 1 1 d . . . . .
N14 N 0.7821(5) 0.3309(2) 0.5950(5) 0.0186(8) Uani 1 1 d . . . . .
N15 N 0.8446(5) 0.3543(2) 0.4591(5) 0.0174(7) Uani 1 1 d . . . . .
N16 N 0.7742(5) 0.42710(19) 0.4037(5) 0.0159(7) Uani 1 1 d . . . . .
C1 C 0.9735(5) 1.0571(3) 1.1768(5) 0.0126(7) Uani 1 1 d . . . . .
C2 C 0.8637(6) 0.9830(2) 1.1729(5) 0.0132(8) Uani 1 1 d . . . . .
C7 C 0.8107(5) 0.9291(2) 1.0097(5) 0.0120(8) Uani 1 1 d . . . . .
C4 C 0.5206(6) 0.5753(2) 0.3557(5) 0.0142(8) Uani 1 1 d . . . . .
C5 C 0.5669(6) 0.5202(2) 0.5144(5) 0.0140(7) Uani 1 1 d . . . . .
C6 C 0.6698(5) 0.4450(3) 0.5122(5) 0.0127(7) 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
K1 K3 4.3281(15) 2_756 y
K1 K4 3.9874(16) 2_656 y
K1 O2 2.975(3) . y
K1 O3 2.933(3) 2_656 y
K1 N1 3.196(4) 2_647 y
K1 N2 3.466(3) 2_747 y
K1 N3 3.030(4) 2_747 y
K1 N6 2.852(4) . y
K1 N9 3.012(3) . y
K1 N11 2.888(4) 1_556 y
K1 N14 3.269(4) 2_656 y
K1 N15 3.263(4) 2_656 y
K2 K3 4.0010(16) 1_454 y
K2 K4 3.5642(15) 2_756 y
K2 O1 3.396(3) 2_646 y
K2 O2 2.892(3) 1_554 y
K2 O3 2.677(3) . y
K2 N4 3.054(3) 2_746 y
K2 N5 2.935(4) 2_646 y
K2 N8 3.091(4) 2_746 y
K2 N12 2.887(4) . y
K2 N13 2.908(3) 1_554 y
K2 N16 2.977(3) . y
K2 C7 3.451(4) 2_646 y
K3 K4 4.7052(15) 2_756 y
K3 O1 2.930(3) 2_747 y
K3 O4 2.721(3) . y
K3 H4B 2.8524 . y
K3 N2 3.349(4) 1_544 y
K3 N5 3.129(3) 2_747 y
K3 N7 2.833(3) 2_746 y
K3 N9 3.460(4) 2_746 y
K3 N10 3.142(4) 2_746 y
K3 N13 3.052(4) 1_655 y
K3 N15 2.994(4) . y
K4 O1 2.865(3) 1_544 y
K4 O2 3.362(3) 2_646 y
K4 O4 2.736(3) . y
K4 H4A 2.9719 . y
K4 N1 2.828(3) 1_544 y
K4 N4 2.968(3) 1_545 y
K4 N8 2.852(3) 1_545 y
K4 N9 3.129(4) 2_646 y
K4 N12 3.182(4) 2_746 y
K4 N16 2.993(4) 2_746 y
K4 C4 3.462(4) 2_646 y
O1 C2 1.222(5) . ?
O2 C5 1.228(4) . ?
O3 H3A 0.9900 . ?
O3 H3B 0.9900 . ?
O4 H4A 0.8399 . ?
O4 H4B 0.8400 . ?
N1 N2 1.341(5) . ?
N1 C1 1.349(5) . ?
N2 N3 1.333(5) . ?
N3 N4 1.335(5) . ?
N4 C1 1.344(5) . ?
N5 N6 1.336(5) . ?
N5 C7 1.338(5) . ?
N6 N7 1.331(5) . ?
N7 N8 1.342(5) . ?
N8 C7 1.338(5) . ?
N9 N10 1.348(5) . ?
N9 C4 1.340(5) . ?
N10 N11 1.334(5) . ?
N11 N12 1.347(5) . ?
N12 C4 1.346(5) . ?
N13 N14 1.330(5) . ?
N13 C6 1.346(5) . ?
N14 N15 1.329(5) . ?
N15 N16 1.346(5) . ?
N16 C6 1.335(5) . ?
C1 C2 1.480(6) . ?
C2 C7 1.479(5) . ?
C4 C5 1.471(5) . ?
C5 C6 1.478(6) . ?

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
K4 K1 K3 101.01(3) 2_656 2_756 y
O2 K1 K3 93.52(6) . 2_756 y
O2 K1 K4 55.48(6) . 2_656 y
O2 K1 N1 80.46(9) . 2_647 y
O2 K1 N2 63.26(8) . 2_747 y
O2 K1 N3 61.34(9) . 2_747 y
O2 K1 N9 54.65(8) . . y
O2 K1 N14 123.52(8) . 2_656 y
O2 K1 N15 143.56(9) . 2_656 y
O3 K1 K3 120.76(7) 2_656 2_756 y
O3 K1 K4 112.83(7) 2_656 2_656 y
O3 K1 O2 145.72(8) 2_656 . y
O3 K1 N1 73.02(9) 2_656 2_647 y
O3 K1 N2 138.50(9) 2_656 2_747 y
O3 K1 N3 126.28(9) 2_656 2_747 y
O3 K1 N9 147.75(9) 2_656 . y
O3 K1 N14 81.52(9) 2_656 2_656 y
O3 K1 N15 58.04(8) 2_656 2_656 y
N1 K1 K3 141.37(7) 2_647 2_756 y
N1 K1 K4 44.71(6) 2_647 2_656 y
N1 K1 N2 143.67(9) 2_647 2_747 y
N1 K1 N14 96.63(9) 2_647 2_656 y
N1 K1 N15 88.63(10) 2_647 2_656 y
N2 K1 K3 49.38(6) 2_747 2_756 y
N2 K1 K4 108.66(6) 2_747 2_656 y
N3 K1 K3 70.66(7) 2_747 2_756 y
N3 K1 K4 115.57(7) 2_747 2_656 y
N3 K1 N1 133.61(10) 2_747 2_647 y
N3 K1 N2 22.42(8) 2_747 2_747 y
N3 K1 N14 125.51(9) 2_747 2_656 y
N3 K1 N15 137.75(10) 2_747 2_656 y
N6 K1 K3 54.17(7) . 2_756 y
N6 K1 K4 152.68(8) . 2_656 y
N6 K1 O2 128.95(9) . . y
N6 K1 O3 77.50(9) . 2_656 y
N6 K1 N1 149.97(10) . 2_647 y
N6 K1 N2 65.84(9) . 2_747 y
N6 K1 N3 70.26(10) . 2_747 y
N6 K1 N9 106.69(10) . . y
N6 K1 N11 100.60(11) . 1_556 y
N6 K1 N14 73.17(10) . 2_656 y
N6 K1 N15 70.73(10) . 2_656 y
N9 K1 K3 52.61(7) . 2_756 y
N9 K1 K4 50.81(7) . 2_656 y
N9 K1 N1 95.44(10) . 2_647 y
N9 K1 N2 65.90(9) . 2_747 y
N9 K1 N3 83.69(10) . 2_747 y
N9 K1 N14 69.79(9) . 2_656 y
N9 K1 N15 92.47(9) . 2_656 y
N11 K1 K3 142.91(8) 1_556 2_756 y
N11 K1 K4 106.70(8) 1_556 2_656 y
N11 K1 O2 82.66(9) 1_556 . y
N11 K1 O3 69.75(9) 1_556 2_656 y
N11 K1 N1 74.57(10) 1_556 2_647 y
N11 K1 N2 97.73(10) 1_556 2_747 y
N11 K1 N3 75.32(10) 1_556 2_747 y
N11 K1 N9 137.30(10) 1_556 . y
N11 K1 N14 151.25(10) 1_556 2_656 y
N11 K1 N15 127.77(10) 1_556 2_656 y
N14 K1 K3 55.26(6) 2_656 2_756 y
N14 K1 K4 83.17(7) 2_656 2_656 y
N14 K1 N2 104.63(9) 2_656 2_747 y
N15 K1 K3 73.76(6) 2_656 2_756 y
N15 K1 K4 92.82(7) 2_656 2_656 y
N15 K1 N2 121.47(9) 2_656 2_747 y
N15 K1 N14 23.48(8) 2_656 2_656 y
K4 K2 K3 176.02(3) 2_756 1_454 y
O1 K2 K3 45.78(5) 2_646 1_454 y
O1 K2 K4 137.56(6) 2_646 2_756 y
O1 K2 C7 39.87(8) 2_646 2_646 y
O2 K2 K3 73.60(7) 1_554 1_454 y
O2 K2 K4 110.13(7) 1_554 2_756 y
O2 K2 O1 51.69(7) 1_554 2_646 y
O2 K2 N4 62.54(9) 1_554 2_746 y
O2 K2 N5 102.60(9) 1_554 2_646 y
O2 K2 N8 111.60(9) 1_554 2_746 y
O2 K2 N13 57.65(9) 1_554 1_554 y
O2 K2 N16 151.01(9) 1_554 . y
O2 K2 C7 89.32(9) 1_554 2_646 y
O3 K2 K3 70.98(7) . 1_454 y
O3 K2 K4 105.09(7) . 2_756 y
O3 K2 O1 113.37(9) . 2_646 y
O3 K2 O2 134.47(9) . 1_554 y
O3 K2 N4 126.41(10) . 2_746 y
O3 K2 N5 75.78(10) . 2_646 y
O3 K2 N8 71.27(10) . 2_746 y
O3 K2 N12 133.02(10) . . y
O3 K2 N13 77.56(10) . 1_554 y
O3 K2 N16 74.30(9) . . y
O3 K2 C7 97.95(10) . 2_646 y
N4 K2 K3 130.07(7) 2_746 1_454 y
N4 K2 K4 52.60(6) 2_746 2_756 y
N4 K2 O1 111.24(8) 2_746 2_646 y
N4 K2 N8 57.37(9) 2_746 2_746 y
N4 K2 C7 135.59(10) 2_746 2_646 y
N5 K2 K3 50.83(7) 2_646 1_454 y
N5 K2 K4 128.23(7) 2_646 2_756 y
N5 K2 O1 51.03(8) 2_646 2_646 y
N5 K2 N4 157.80(9) 2_646 2_746 y
N5 K2 N8 143.45(10) 2_646 2_746 y
N5 K2 N16 78.67(10) 2_646 . y
N5 K2 C7 22.38(10) 2_646 2_646 y
N8 K2 K3 127.66(7) 2_746 1_454 y
N8 K2 K4 50.13(7) 2_746 2_756 y
N8 K2 O1 161.48(8) 2_746 2_646 y
N8 K2 C7 158.51(9) 2_746 2_646 y
N12 K2 K3 124.13(8) . 1_454 y
N12 K2 K4 57.96(7) . 2_756 y
N12 K2 O1 82.23(9) . 2_646 y
N12 K2 O2 90.74(9) . 1_554 y
N12 K2 N4 80.67(10) . 2_746 y
N12 K2 N5 83.29(10) . 2_646 y
N12 K2 N8 108.10(10) . 2_746 y
N12 K2 N13 148.30(10) . 1_554 y
N12 K2 N16 60.45(9) . . y
N12 K2 C7 65.15(10) . 2_646 y
N13 K2 K3 49.39(7) 1_554 1_454 y
N13 K2 K4 131.10(7) 1_554 2_756 y
N13 K2 O1 76.13(8) 1_554 2_646 y
N13 K2 N4 85.87(9) 1_554 2_746 y
N13 K2 N5 100.16(10) 1_554 2_646 y
N13 K2 N8 87.92(10) 1_554 2_746 y
N13 K2 N16 151.24(10) 1_554 . y
N13 K2 C7 108.32(10) 1_554 2_646 y
N16 K2 K3 123.73(7) . 1_454 y
N16 K2 K4 53.55(7) . 2_756 y
N16 K2 O1 120.83(9) . 2_646 y
N16 K2 N4 106.14(10) . 2_746 y
N16 K2 N8 77.61(10) . 2_746 y
N16 K2 C7 81.60(10) . 2_646 y
C7 K2 K3 61.49(7) 2_646 1_454 y
C7 K2 K4 119.25(7) 2_646 2_756 y
K1 K3 K4 109.35(2) 2_746 2_756 y
K1 K3 H4B 118.9 2_746 . y
K2 K3 K1 108.38(3) 1_656 2_746 y
K2 K3 K4 80.12(3) 1_656 2_756 y
K2 K3 H4B 98.6 1_656 . y
K4 K3 H4B 129.1 2_756 . y
O1 K3 K1 137.51(6) 2_747 2_746 y
O1 K3 K2 56.14(6) 2_747 1_656 y
O1 K3 K4 35.27(5) 2_747 2_756 y
O1 K3 H4B 103.2 2_747 . y
O1 K3 N2 140.76(9) 2_747 1_544 y
O1 K3 N5 54.04(8) 2_747 2_747 y
O1 K3 N9 155.83(9) 2_747 2_746 y
O1 K3 N10 135.97(9) 2_747 2_746 y
O1 K3 N13 81.48(9) 2_747 1_655 y
O1 K3 N15 63.08(9) 2_747 . y
O4 K3 K1 115.92(7) . 2_746 y
O4 K3 K2 114.45(7) . 1_656 y
O4 K3 K4 122.81(7) . 2_756 y
O4 K3 O1 106.04(9) . 2_747 y
O4 K3 H4B 17.1 . . y
O4 K3 N2 75.89(9) . 1_544 y
O4 K3 N5 71.10(9) . 2_747 y
O4 K3 N7 136.08(10) . 2_746 y
O4 K3 N9 83.07(9) . 2_746 y
O4 K3 N10 77.33(9) . 2_746 y
O4 K3 N13 150.96(9) . 1_655 y
O4 K3 N15 70.46(9) . . y
N2 K3 K1 51.78(6) 1_544 2_746 y
N2 K3 K2 159.38(6) 1_544 1_656 y
N2 K3 K4 110.05(7) 1_544 2_756 y
N2 K3 H4B 88.8 1_544 . y
N2 K3 N9 62.71(8) 1_544 2_746 y
N5 K3 K1 146.99(7) 2_747 2_746 y
N5 K3 K2 46.65(7) 2_747 1_656 y
N5 K3 K4 89.24(7) 2_747 2_756 y
N5 K3 H4B 58.6 2_747 . y
N5 K3 N2 146.96(9) 2_747 1_544 y
N5 K3 N9 111.16(9) 2_747 2_746 y
N5 K3 N10 88.42(9) 2_747 2_746 y
N7 K3 K1 61.76(8) 2_746 2_746 y
N7 K3 K2 106.54(8) 2_746 1_656 y
N7 K3 K4 49.38(8) 2_746 2_756 y
N7 K3 O1 83.77(10) 2_746 2_747 y
N7 K3 H4B 153.2 2_746 . y
N7 K3 N2 70.87(10) 2_746 1_544 y
N7 K3 N5 137.21(11) 2_746 2_747 y
N7 K3 N9 105.43(10) 2_746 2_746 y
N7 K3 N10 124.82(10) 2_746 2_746 y
N7 K3 N13 71.82(10) 2_746 1_655 y
N7 K3 N15 77.12(10) 2_746 . y
N9 K3 K1 43.77(6) 2_746 2_746 y
N9 K3 K2 99.69(6) 2_746 1_656 y
N9 K3 K4 152.00(6) 2_746 2_756 y
N9 K3 H4B 78.8 2_746 . y
N10 K3 K1 63.85(7) 2_746 2_746 y
N10 K3 K2 82.01(7) 2_746 1_656 y
N10 K3 K4 157.47(7) 2_746 2_756 y
N10 K3 H4B 67.2 2_746 . y
N10 K3 N2 83.18(9) 2_746 1_544 y
N10 K3 N9 22.91(8) 2_746 2_746 y
N13 K3 K1 65.33(7) 1_655 2_746 y
N13 K3 K2 46.32(7) 1_655 1_656 y
N13 K3 K4 79.58(7) 1_655 2_756 y
N13 K3 H4B 134.4 1_655 . y
N13 K3 N2 116.25(9) 1_655 1_544 y
N13 K3 N5 92.93(10) 1_655 2_747 y
N13 K3 N9 80.39(9) 1_655 2_746 y
N13 K3 N10 78.17(9) 1_655 2_746 y
N15 K3 K1 124.84(7) . 2_746 y
N15 K3 K2 117.91(8) . 1_656 y
N15 K3 K4 55.30(7) . 2_756 y
N15 K3 H4B 83.0 . . y
N15 K3 N2 81.97(10) . 1_544 y
N15 K3 N5 88.16(10) . 2_747 y
N15 K3 N9 140.25(9) . 2_746 y
N15 K3 N10 146.93(9) . 2_746 y
N15 K3 N13 134.86(10) . 1_655 y
K1 K4 H4A 58.9 2_646 . y
K2 K4 K1 174.24(3) 2_746 2_646 y
K2 K4 H4A 115.4 2_746 . y
O1 K4 K1 74.69(7) 1_544 2_646 y
O1 K4 K2 110.45(7) 1_544 2_746 y
O1 K4 O2 52.25(7) 1_544 2_646 y
O1 K4 H4A 132.0 1_544 . y
O1 K4 N4 153.53(9) 1_544 1_545 y
O1 K4 N9 101.82(9) 1_544 2_646 y
O1 K4 N12 111.37(9) 1_544 2_746 y
O1 K4 N16 62.50(9) 1_544 2_746 y
O1 K4 C4 90.31(9) 1_544 2_646 y
O2 K4 K1 46.80(6) 2_646 2_646 y
O2 K4 K2 138.33(6) 2_646 2_746 y
O2 K4 H4A 97.5 2_646 . y
O2 K4 C4 40.00(8) 2_646 2_646 y
O4 K4 K1 70.03(7) . 2_646 y
O4 K4 K2 104.21(7) . 2_746 y
O4 K4 O1 136.37(9) . 1_544 y
O4 K4 O2 112.45(9) . 2_646 y
O4 K4 H4A 16.3 . . y
O4 K4 N1 79.50(10) . 1_544 y
O4 K4 N4 69.73(9) . 1_545 y
O4 K4 N8 129.08(9) . 1_545 y
O4 K4 N9 72.62(9) . 2_646 y
O4 K4 N12 72.25(9) . 2_746 y
O4 K4 N16 127.57(9) . 2_746 y
O4 K4 C4 94.52(10) . 2_646 y
N1 K4 K1 52.66(8) 1_544 2_646 y
N1 K4 K2 127.28(8) 1_544 2_746 y
N1 K4 O1 58.64(9) 1_544 1_544 y
N1 K4 O2 79.73(9) 1_544 2_646 y
N1 K4 H4A 82.2 1_544 . y
N1 K4 N4 147.52(10) 1_544 1_545 y
N1 K4 N8 151.21(10) 1_544 1_545 y
N1 K4 N9 100.83(10) 1_544 2_646 y
N1 K4 N12 83.70(10) 1_544 2_746 y
N1 K4 N16 82.48(10) 1_544 2_746 y
N1 K4 C4 111.60(10) 1_544 2_646 y
N4 K4 K1 121.53(7) 1_545 2_646 y
N4 K4 K2 54.84(7) 1_545 2_746 y
N4 K4 O2 121.19(8) 1_545 2_646 y
N4 K4 H4A 71.2 1_545 . y
N4 K4 N9 80.10(9) 1_545 2_646 y
N4 K4 N12 77.38(9) 1_545 2_746 y
N4 K4 N16 107.96(10) 1_545 2_746 y
N4 K4 C4 81.69(10) 1_545 2_646 y
N8 K4 K1 127.14(7) 1_545 2_646 y
N8 K4 K2 56.29(7) 1_545 2_746 y
N8 K4 O1 92.73(9) 1_545 1_544 y
N8 K4 O2 84.69(9) 1_545 2_646 y
N8 K4 H4A 124.0 1_545 . y
N8 K4 N4 60.88(9) 1_545 1_545 y
N8 K4 N9 87.05(9) 1_545 2_646 y
N8 K4 N12 106.58(10) 1_545 2_746 y
N8 K4 N16 81.16(10) 1_545 2_746 y
N8 K4 C4 67.80(10) 1_545 2_646 y
N9 K4 K1 48.25(6) 2_646 2_646 y
N9 K4 K2 130.95(7) 2_646 2_746 y
N9 K4 O2 49.94(8) 2_646 2_646 y
N9 K4 H4A 56.5 2_646 . y
N9 K4 N12 143.04(9) 2_646 2_746 y
N9 K4 C4 22.74(9) 2_646 2_646 y
N12 K4 K1 125.98(7) 2_746 2_646 y
N12 K4 K2 50.29(7) 2_746 2_746 y
N12 K4 O2 161.44(8) 2_746 2_646 y
N12 K4 H4A 88.4 2_746 . y
N12 K4 C4 158.09(9) 2_746 2_646 y
N16 K4 K1 130.11(7) 2_746 2_646 y
N16 K4 K2 53.14(7) 2_746 2_746 y
N16 K4 O2 112.03(9) 2_746 2_646 y
N16 K4 H4A 143.5 2_746 . y
N16 K4 N9 159.63(9) 2_746 2_646 y
N16 K4 N12 57.04(9) 2_746 2_746 y
N16 K4 C4 137.81(10) 2_746 2_646 y
C4 K4 K1 61.32(7) 2_646 2_646 y
C4 K4 K2 120.27(7) 2_646 2_746 y
C4 K4 H4A 78.7 2_646 . y
K3 O1 K2 78.08(7) 2_757 2_656 ?
K4 O1 K2 127.87(10) 1_566 2_656 ?
K4 O1 K3 108.54(9) 1_566 2_757 ?
C2 O1 K2 90.5(2) . 2_656 ?
C2 O1 K3 124.5(3) . 2_757 ?
C2 O1 K4 120.4(3) . 1_566 ?
K1 O2 K4 77.72(7) . 2_656 ?
K2 O2 K1 110.65(9) 1_556 . ?
K2 O2 K4 128.17(10) 1_556 2_656 ?
C5 O2 K1 123.1(3) . . ?
C5 O2 K2 119.9(3) . 1_556 ?
C5 O2 K4 89.9(2) . 2_656 ?
K1 O3 H3A 107.5 2_646 . ?
K1 O3 H3B 107.5 2_646 . ?
K2 O3 K1 119.43(12) . 2_646 ?
K2 O3 H3A 107.5 . . ?
K2 O3 H3B 107.5 . . ?
H3A O3 H3B 107.0 . . ?
K3 O4 K4 128.04(11) . . ?
K3 O4 H4A 111.1 . . ?
K3 O4 H4B 90.3 . . ?
K4 O4 H4A 98.0 . . ?
K4 O4 H4B 110.7 . . ?
H4A O4 H4B 120.9 . . ?
K4 N1 K1 82.64(9) 1_566 2_657 ?
N2 N1 K1 103.5(2) . 2_657 ?
N2 N1 K4 133.5(2) . 1_566 ?
N2 N1 C1 104.4(3) . . ?
C1 N1 K1 113.6(2) . 2_657 ?
C1 N1 K4 115.3(3) . 1_566 ?
K3 N2 K1 78.84(8) 1_566 2_757 ?
N1 N2 K1 139.5(3) . 2_757 ?
N1 N2 K3 115.4(2) . 1_566 ?
N3 N2 K1 60.1(2) . 2_757 ?
N3 N2 K3 134.3(2) . 1_566 ?
N3 N2 N1 109.0(3) . . ?
N2 N3 K1 97.5(2) . 2_757 ?
N2 N3 N4 110.4(3) . . ?
N4 N3 K1 129.7(2) . 2_757 ?
K4 N4 K2 72.57(8) 1_565 2_756 ?
N3 N4 K2 120.2(2) . 2_756 ?
N3 N4 K4 114.2(2) . 1_565 ?
N3 N4 C1 103.9(3) . . ?
C1 N4 K2 110.9(3) . 2_756 ?
C1 N4 K4 133.1(2) . 1_565 ?
K2 N5 K3 82.51(9) 2_656 2_757 ?
N6 N5 K2 115.0(2) . 2_656 ?
N6 N5 K3 135.1(3) . 2_757 ?
N6 N5 C7 104.7(3) . . ?
C7 N5 K2 101.0(2) . 2_656 ?
C7 N5 K3 112.1(2) . 2_757 ?
N5 N6 K1 116.8(2) . . ?
N7 N6 K1 133.8(3) . . ?
N7 N6 N5 109.4(3) . . ?
N6 N7 K3 110.3(2) . 2_756 ?
N6 N7 N8 109.4(3) . . ?
N8 N7 K3 140.1(3) . 2_756 ?
K4 N8 K2 73.57(8) 1_565 2_756 ?
N7 N8 K2 118.1(2) . 2_756 ?
N7 N8 K4 112.0(2) . 1_565 ?
C7 N8 K2 106.8(2) . 2_756 ?
C7 N8 K4 138.2(3) . 1_565 ?
C7 N8 N7 104.4(3) . . ?
K1 N9 K3 83.63(9) . 2_756 ?
K1 N9 K4 80.94(9) . 2_656 ?
K4 N9 K3 153.98(11) 2_656 2_756 ?
N10 N9 K1 134.9(3) . . ?
N10 N9 K3 65.2(2) . 2_756 ?
N10 N9 K4 113.3(2) . 2_656 ?
C4 N9 K1 117.8(2) . . ?
C4 N9 K3 113.0(2) . 2_756 ?
C4 N9 K4 92.7(2) . 2_656 ?
C4 N9 N10 104.5(3) . . ?
N9 N10 K3 91.9(2) . 2_756 ?
N11 N10 K3 107.4(2) . 2_756 ?
N11 N10 N9 109.3(3) . . ?
N10 N11 K1 110.6(2) . 1_554 ?
N10 N11 N12 109.6(3) . . ?
N12 N11 K1 139.6(2) . 1_554 ?
K2 N12 K4 71.75(8) . 2_756 ?
N11 N12 K2 114.9(2) . . ?
N11 N12 K4 114.6(2) . 2_756 ?
C4 N12 K2 139.4(3) . . ?
C4 N12 K4 102.2(2) . 2_756 ?
C4 N12 N11 104.2(3) . . ?
K2 N13 K3 84.29(9) 1_556 1_455 ?
N14 N13 K2 130.1(2) . 1_556 ?
N14 N13 K3 105.8(2) . 1_455 ?
N14 N13 C6 104.0(3) . . ?
C6 N13 K2 112.5(3) . 1_556 ?
C6 N13 K3 120.2(2) . 1_455 ?
N13 N14 K1 121.7(2) . 2_646 ?
N15 N14 K1 78.0(2) . 2_646 ?
N15 N14 N13 110.2(3) . . ?
K3 N15 K1 106.95(11) . 2_646 ?
N14 N15 K1 78.5(2) . 2_646 ?
N14 N15 K3 103.0(2) . . ?
N14 N15 N16 109.1(3) . . ?
N16 N15 K1 121.5(2) . 2_646 ?
N16 N15 K3 125.5(2) . . ?
K2 N16 K4 73.31(8) . 2_756 ?
N15 N16 K2 110.1(2) . . ?
N15 N16 K4 122.2(2) . 2_756 ?
C6 N16 K2 130.9(3) . . ?
C6 N16 K4 115.6(3) . 2_756 ?
C6 N16 N15 104.2(3) . . ?
N1 C1 C2 121.1(3) . . ?
N4 C1 N1 112.2(4) . . ?
N4 C1 C2 126.6(4) . . ?
O1 C2 C1 119.6(3) . . ?
O1 C2 C7 119.3(4) . . ?
C7 C2 C1 121.1(3) . . ?
N5 C7 K2 56.6(2) . 2_656 ?
N5 C7 C2 120.4(3) . . ?
N8 C7 K2 126.2(2) . 2_656 ?
N8 C7 N5 112.1(3) . . ?
N8 C7 C2 127.5(3) . . ?
C2 C7 K2 84.4(2) . 2_656 ?
N9 C4 K4 64.5(2) . 2_656 ?
N9 C4 N12 112.4(3) . . ?
N9 C4 C5 119.9(3) . . ?
N12 C4 K4 120.8(3) . 2_656 ?
N12 C4 C5 127.7(4) . . ?
C5 C4 K4 82.4(2) . 2_656 ?
O2 C5 C4 119.6(4) . . ?
O2 C5 C6 119.9(4) . . ?
C4 C5 C6 120.5(3) . . ?
N13 C6 C5 120.8(3) . . ?
N16 C6 N13 112.5(4) . . ?
N16 C6 C5 126.7(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
K1 O2 C5 C4 -18.8(5) . . . . ?
K1 O2 C5 C6 162.3(2) . . . . ?
K1 N1 N2 K1 174.8(2) 2_657 . . 2_757 ?
K1 N1 N2 K3 71.7(2) 2_657 . . 1_566 ?
K1 N1 N2 N3 -119.4(3) 2_657 . . . ?
K1 N1 C1 N4 111.9(3) 2_657 . . . ?
K1 N1 C1 C2 -69.4(4) 2_657 . . . ?
K1 N2 N3 N4 137.4(3) 2_757 . . . ?
K1 N3 N4 K2 -6.0(4) 2_757 . . 2_756 ?
K1 N3 N4 K4 -89.2(3) 2_757 . . 1_565 ?
K1 N3 N4 C1 118.9(3) 2_757 . . . ?
K1 N6 N7 K3 1.0(4) . . . 2_756 ?
K1 N6 N7 N8 177.5(3) . . . . ?
K1 N9 N10 K3 50.7(3) . . . 2_756 ?
K1 N9 N10 N11 159.9(3) . . . . ?
K1 N9 C4 K4 81.20(18) . . . 2_656 ?
K1 N9 C4 N12 -164.2(3) . . . . ?
K1 N9 C4 C5 17.5(5) . . . . ?
K1 N11 N12 K2 -5.9(5) 1_554 . . . ?
K1 N11 N12 K4 74.5(4) 1_554 . . 2_756 ?
K1 N11 N12 C4 -174.6(3) 1_554 . . . ?
K1 N14 N15 K3 -104.97(13) 2_646 . . . ?
K1 N14 N15 N16 119.6(3) 2_646 . . . ?
K1 N15 N16 K2 -56.1(3) 2_646 . . . ?
K1 N15 N16 K4 -138.54(16) 2_646 . . 2_756 ?
K1 N15 N16 C6 88.2(3) 2_646 . . . ?
K2 O1 C2 C1 125.6(3) 2_656 . . . ?
K2 O1 C2 C7 -53.6(3) 2_656 . . . ?
K2 O2 C5 C4 -168.2(2) 1_556 . . . ?
K2 O2 C5 C6 12.9(5) 1_556 . . . ?
K2 N4 C1 N1 130.9(3) 2_756 . . . ?
K2 N4 C1 C2 -47.7(4) 2_756 . . . ?
K2 N5 N6 K1 -68.3(3) 2_656 . . . ?
K2 N5 N6 N7 110.5(3) 2_656 . . . ?
K2 N5 C7 N8 -119.7(3) 2_656 . . . ?
K2 N5 C7 C2 58.6(4) 2_656 . . . ?
K2 N8 C7 K2 169.48(16) 2_756 . . 2_656 ?
K2 N8 C7 N5 -126.6(3) 2_756 . . . ?
K2 N8 C7 C2 55.3(4) 2_756 . . . ?
K2 N12 C4 K4 -91.2(4) . . . 2_656 ?
K2 N12 C4 N9 -163.9(3) . . . . ?
K2 N12 C4 C5 14.2(7) . . . . ?
K2 N13 N14 K1 135.1(2) 1_556 . . 2_646 ?
K2 N13 N14 N15 -136.8(3) 1_556 . . . ?
K2 N13 C6 N16 145.7(3) 1_556 . . . ?
K2 N13 C6 C5 -32.3(4) 1_556 . . . ?
K2 N16 C6 N13 133.1(3) . . . . ?
K2 N16 C6 C5 -49.1(5) . . . . ?
K3 O1 C2 C1 -158.6(2) 2_757 . . . ?
K3 O1 C2 C7 22.2(5) 2_757 . . . ?
K3 N2 N3 K1 29.0(4) 1_566 . . 2_757 ?
K3 N2 N3 N4 166.5(3) 1_566 . . . ?
K3 N5 N6 K1 37.1(4) 2_757 . . . ?
K3 N5 N6 N7 -144.1(3) 2_757 . . . ?
K3 N5 C7 K2 -86.33(17) 2_757 . . 2_656 ?
K3 N5 C7 N8 154.0(2) 2_757 . . . ?
K3 N5 C7 C2 -27.8(4) 2_757 . . . ?
K3 N7 N8 K2 -65.6(4) 2_756 . . 2_756 ?
K3 N7 N8 K4 16.9(5) 2_756 . . 1_565 ?
K3 N7 N8 C7 176.0(3) 2_756 . . . ?
K3 N9 N10 N11 109.2(3) 2_756 . . . ?
K3 N9 C4 K4 176.2(2) 2_756 . . 2_656 ?
K3 N9 C4 N12 -69.1(4) 2_756 . . . ?
K3 N9 C4 C5 112.6(3) 2_756 . . . ?
K3 N10 N11 K1 -85.4(2) 2_756 . . 1_554 ?
K3 N10 N11 N12 98.4(3) 2_756 . . . ?
K3 N13 N14 K1 39.2(3) 1_455 . . 2_646 ?
K3 N13 N14 N15 127.3(3) 1_455 . . . ?
K3 N13 C6 N16 -117.6(3) 1_455 . . . ?
K3 N13 C6 C5 64.4(4) 1_455 . . . ?
K3 N15 N16 K2 93.1(2) . . . . ?
K3 N15 N16 K4 10.6(4) . . . 2_756 ?
K3 N15 N16 C6 -122.6(3) . . . . ?
K4 O1 C2 C1 -10.3(5) 1_566 . . . ?
K4 O1 C2 C7 170.6(2) 1_566 . . . ?
K4 O2 C5 C4 56.4(3) 2_656 . . . ?
K4 O2 C5 C6 -122.5(3) 2_656 . . . ?
K4 N1 N2 K1 82.2(4) 1_566 . . 2_757 ?
K4 N1 N2 K3 -20.9(4) 1_566 . . 1_566 ?
K4 N1 N2 N3 148.0(3) 1_566 . . . ?
K4 N1 C1 N4 -155.1(2) 1_566 . . . ?
K4 N1 C1 C2 23.6(4) 1_566 . . . ?
K4 N4 C1 N1 -143.7(3) 1_565 . . . ?
K4 N4 C1 C2 37.7(6) 1_565 . . . ?
K4 N8 C7 K2 85.5(4) 1_565 . . 2_656 ?
K4 N8 C7 N5 149.5(3) 1_565 . . . ?
K4 N8 C7 C2 -28.6(6) 1_565 . . . ?
K4 N9 N10 K3 151.50(13) 2_656 . . 2_756 ?
K4 N9 N10 N11 -99.3(3) 2_656 . . . ?
K4 N9 C4 N12 114.6(3) 2_656 . . . ?
K4 N9 C4 C5 -63.7(3) 2_656 . . . ?
K4 N12 C4 K4 -167.34(15) 2_756 . . 2_656 ?
K4 N12 C4 N9 119.9(3) 2_756 . . . ?
K4 N12 C4 C5 -62.0(4) 2_756 . . . ?
K4 N16 C6 N13 -137.3(3) 2_756 . . . ?
K4 N16 C6 C5 40.5(5) 2_756 . . . ?
K4 C4 C5 O2 -54.7(3) 2_656 . . . ?
K4 C4 C5 C6 124.2(3) 2_656 . . . ?
O1 C2 C7 K2 52.8(3) . . . 2_656 ?
O1 C2 C7 N5 7.1(6) . . . . ?
O1 C2 C7 N8 -175.0(4) . . . . ?
O2 C5 C6 N13 14.7(6) . . . . ?
O2 C5 C6 N16 -163.0(4) . . . . ?
N1 N2 N3 K1 -136.9(3) . . . 2_757 ?
N1 N2 N3 N4 0.5(4) . . . . ?
N1 C1 C2 O1 -9.6(6) . . . . ?
N1 C1 C2 C7 169.6(4) . . . . ?
N2 N1 C1 N4 0.0(4) . . . . ?
N2 N1 C1 C2 178.6(3) . . . . ?
N2 N3 N4 K2 -125.4(3) . . . 2_756 ?
N2 N3 N4 K4 151.5(3) . . . 1_565 ?
N2 N3 N4 C1 -0.5(4) . . . . ?
N3 N4 C1 N1 0.3(4) . . . . ?
N3 N4 C1 C2 -178.3(4) . . . . ?
N4 C1 C2 O1 168.9(4) . . . . ?
N4 C1 C2 C7 -12.0(6) . . . . ?
N5 N6 N7 K3 -177.6(2) . . . 2_756 ?
N5 N6 N7 N8 -1.0(5) . . . . ?
N6 N5 C7 K2 119.8(3) . . . 2_656 ?
N6 N5 C7 N8 0.1(4) . . . . ?
N6 N5 C7 C2 178.3(3) . . . . ?
N6 N7 N8 K2 119.5(3) . . . 2_756 ?
N6 N7 N8 K4 -158.0(2) . . . 1_565 ?
N6 N7 N8 C7 1.1(4) . . . . ?
N7 N8 C7 K2 -64.6(4) . . . 2_656 ?
N7 N8 C7 N5 -0.7(4) . . . . ?
N7 N8 C7 C2 -178.8(4) . . . . ?
N9 N10 N11 K1 176.1(2) . . . 1_554 ?
N9 N10 N11 N12 -0.1(5) . . . . ?
N9 C4 C5 O2 0.0(6) . . . . ?
N9 C4 C5 C6 178.9(3) . . . . ?
N10 N9 C4 K4 -114.9(3) . . . 2_656 ?
N10 N9 C4 N12 -0.3(4) . . . . ?
N10 N9 C4 C5 -178.6(4) . . . . ?
N10 N11 N12 K2 168.6(2) . . . . ?
N10 N11 N12 K4 -111.0(3) . . . 2_756 ?
N10 N11 N12 C4 -0.1(4) . . . . ?
N11 N12 C4 K4 73.0(4) . . . 2_656 ?
N11 N12 C4 N9 0.3(4) . . . . ?
N11 N12 C4 C5 178.4(4) . . . . ?
N12 C4 C5 O2 -178.0(4) . . . . ?
N12 C4 C5 C6 0.9(6) . . . . ?
N13 N14 N15 K1 -119.6(3) . . . 2_646 ?
N13 N14 N15 K3 135.5(3) . . . . ?
N13 N14 N15 N16 0.1(4) . . . . ?
N14 N13 C6 N16 0.4(4) . . . . ?
N14 N13 C6 C5 -177.5(3) . . . . ?
N14 N15 N16 K2 -144.1(3) . . . . ?
N14 N15 N16 K4 133.4(3) . . . 2_756 ?
N14 N15 N16 C6 0.2(4) . . . . ?
N15 N16 C6 N13 -0.4(4) . . . . ?
N15 N16 C6 C5 177.4(3) . . . . ?
C1 N1 N2 K1 -66.2(4) . . . 2_757 ?
C1 N1 N2 K3 -169.2(2) . . . 1_566 ?
C1 N1 N2 N3 -0.3(4) . . . . ?
C1 C2 C7 K2 -126.4(3) . . . 2_656 ?
C1 C2 C7 N5 -172.1(4) . . . . ?
C1 C2 C7 N8 5.9(6) . . . . ?
C7 N5 N6 K1 -178.3(2) . . . . ?
C7 N5 N6 N7 0.6(4) . . . . ?
C4 N9 N10 K3 -109.0(3) . . . 2_756 ?
C4 N9 N10 N11 0.2(4) . . . . ?
C4 C5 C6 N13 -164.2(4) . . . . ?
C4 C5 C6 N16 18.1(6) . . . . ?
C6 N13 N14 K1 -88.3(3) . . . 2_646 ?
C6 N13 N14 N15 -0.3(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_bwn17286
_database_code_depnum_ccdc_archive 'CCDC 2078900'
loop_
_audit_author_name
_audit_author_address
'Haibo Li'
;Beijing institute of technology
China
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_audit_creation_date             2018-01-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H6 N8 Na2 O4'
_chemical_formula_sum            'C3 H6 N8 Na2 O4'
_chemical_formula_weight         264.14
_chemical_melting_point          ?
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'
Na Na 0.0362 0.0249 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.5949(13)
_cell_length_b                   8.7129(17)
_cell_length_c                   9.1609(18)
_cell_angle_alpha                102.33(3)
_cell_angle_beta                 90.26(3)
_cell_angle_gamma                105.15(3)
_cell_volume                     495.34(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1820
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4623
_cell_measurement_theta_min      2.2804
_shelx_estimated_absorpt_T_max   0.954
_shelx_estimated_absorpt_T_min   0.948
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3918
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         2.280
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2067
_reflns_number_total             2206
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2206
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0407
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0493P)²+0.3870P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1110
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Na1 Na 0.08554(12) 0.22564(8) 0.62495(7) 0.01799(19) Uani 1 1 d . . . . .
Na2 Na 0.42389(12) 0.28386(8) 0.93448(8) 0.01795(19) Uani 1 1 d . . . . .
O1 O 0.3888(2) 0.49495(15) 0.18024(13) 0.0186(3) Uani 1 1 d . . . . .
O2 O 0.1240(2) 0.37179(15) 0.87327(14) 0.0197(3) Uani 1 1 d . . . . .
H2A H 0.1459 0.4728 0.8820 0.024 Uiso 1 1 d R . . . .
H2B H 0.0406 0.3551 0.9407 0.024 Uiso 1 1 d R . . . .
O3 O 0.3601(2) 0.11091(15) 0.69970(14) 0.0193(3) Uani 1 1 d . . . . .
H3A H 0.3338 0.0093 0.6692 0.023 Uiso 1 1 d R . . . .
H3B H 0.4636 0.1420 0.6500 0.023 Uiso 1 1 d R . . . .
O4 O 0.7599(2) 0.27392(15) 1.03054(14) 0.0207(3) Uani 1 1 d . . . . .
H4A H 0.7640 0.2760 1.1226 0.025 Uiso 1 1 d R . . . .
H4B H 0.7571 0.1783 0.9865 0.025 Uiso 1 1 d R . . . .
N1 N 0.3098(2) 0.70332(17) 0.43859(16) 0.0172(3) Uani 1 1 d . . . . .
N2 N 0.2761(2) 0.76023(18) 0.58095(17) 0.0181(3) Uani 1 1 d . . . . .
N3 N 0.2290(2) 0.63864(18) 0.65138(16) 0.0177(3) Uani 1 1 d . . . . .
N4 N 0.2307(2) 0.49872(17) 0.55637(16) 0.0153(3) Uani 1 1 d . . . . .
N5 N 0.1765(2) 0.16976(17) 0.36775(16) 0.0158(3) Uani 1 1 d . . . . .
N6 N 0.1495(3) 0.01459(18) 0.29674(17) 0.0181(3) Uani 1 1 d . . . . .
N7 N 0.2066(3) 0.00942(18) 0.15666(17) 0.0196(3) Uani 1 1 d . . . . .
N8 N 0.2720(3) 0.15986(18) 0.13439(16) 0.0181(3) Uani 1 1 d . . . . .
C1 C 0.2812(3) 0.54237(19) 0.42629(18) 0.0131(3) Uani 1 1 d . . . . .
C2 C 0.3126(3) 0.4353(2) 0.28436(18) 0.0139(3) Uani 1 1 d . . . . .
C3 C 0.2521(3) 0.25656(19) 0.26606(18) 0.0136(3) 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
Na1 Na1 3.973(2) 2_556 ?
Na1 Na2 3.4660(15) . ?
Na1 O2 2.3343(16) . ?
Na1 O3 2.4445(16) . ?
Na1 N1 2.9158(18) 2_566 ?
Na1 N4 2.5349(17) . ?
Na1 N5 2.4133(17) . ?
Na1 N6 2.5007(18) 2_556 ?
Na2 Na2 3.5659(18) 2_667 ?
Na2 O1 2.6388(17) 1_556 ?
Na2 O1 2.4448(16) 2_666 ?
Na2 O2 2.4036(16) . ?
Na2 O3 2.3129(16) . ?
Na2 O4 2.4097(17) . ?
Na2 H4B 2.6712 . ?
Na2 N8 2.4126(17) 1_556 ?
O1 Na2 2.6389(17) 1_554 ?
O1 Na2 2.4448(16) 2_666 ?
O1 C2 1.230(2) . ?
O2 H2A 0.8401 . ?
O2 H2B 0.8400 . ?
O3 H3A 0.8401 . ?
O3 H3B 0.8400 . ?
O4 H4A 0.8400 . ?
O4 H4B 0.8400 . ?
N1 Na1 2.9158(18) 2_566 ?
N1 N2 1.334(2) . ?
N1 C1 1.345(2) . ?
N2 N3 1.325(2) . ?
N3 N4 1.341(2) . ?
N4 C1 1.344(2) . ?
N5 N6 1.334(2) . ?
N5 C3 1.340(2) . ?
N6 Na1 2.5007(18) 2_556 ?
N6 N7 1.334(2) . ?
N7 N8 1.329(2) . ?
N8 Na2 2.4126(17) 1_554 ?
N8 C3 1.344(2) . ?
C1 C2 1.479(2) . ?
C2 C3 1.475(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Na2 Na1 Na1 115.34(4) . 2_556 ?
O2 Na1 Na1 142.09(5) . 2_556 ?
O2 Na1 Na2 43.77(4) . . ?
O2 Na1 O3 85.09(6) . . ?
O2 Na1 N1 94.09(6) . 2_566 ?
O2 Na1 N4 86.39(6) . . ?
O2 Na1 N5 155.37(6) . . ?
O2 Na1 N6 89.36(6) . 2_556 ?
O3 Na1 Na1 78.15(5) . 2_556 ?
O3 Na1 Na2 41.76(4) . . ?
O3 Na1 N1 165.96(5) . 2_566 ?
O3 Na1 N4 113.11(6) . . ?
O3 Na1 N6 82.28(5) . 2_556 ?
N1 Na1 Na1 94.32(5) 2_566 2_556 ?
N1 Na1 Na2 137.42(4) 2_566 . ?
N4 Na1 Na1 131.47(5) . 2_556 ?
N4 Na1 Na2 98.73(5) . . ?
N4 Na1 N1 80.78(5) . 2_566 ?
N5 Na1 Na1 59.39(5) . 2_556 ?
N5 Na1 Na2 125.18(5) . . ?
N5 Na1 O3 90.66(6) . . ?
N5 Na1 N1 95.69(6) . 2_566 ?
N5 Na1 N4 73.00(6) . . ?
N5 Na1 N6 114.13(6) . 2_556 ?
N6 Na1 Na1 55.05(4) 2_556 2_556 ?
N6 Na1 Na2 89.05(5) 2_556 . ?
N6 Na1 N1 83.69(6) 2_556 2_566 ?
N6 Na1 N4 163.55(6) 2_556 . ?
Na1 Na2 Na2 103.04(4) . 2_667 ?
Na1 Na2 H4B 134.6 . . ?
Na2 Na2 H4B 106.9 2_667 . ?
O1 Na2 Na1 118.62(5) 1_556 . ?
O1 Na2 Na1 79.17(5) 2_666 . ?
O1 Na2 Na2 43.27(4) 1_556 2_667 ?
O1 Na2 Na2 47.72(4) 2_666 2_667 ?
O1 Na2 O1 91.00(5) 2_666 1_556 ?
O1 Na2 H4B 96.7 2_666 . ?
O1 Na2 H4B 106.5 1_556 . ?
O2 Na2 Na1 42.21(4) . . ?
O2 Na2 Na2 74.84(5) . 2_667 ?
O2 Na2 O1 76.57(5) . 1_556 ?
O2 Na2 O1 82.49(5) . 2_666 ?
O2 Na2 O4 164.11(5) . . ?
O2 Na2 H4B 176.8 . . ?
O2 Na2 N8 96.40(6) . 1_556 ?
O3 Na2 Na1 44.75(4) . . ?
O3 Na2 Na2 134.12(5) . 2_667 ?
O3 Na2 O1 89.06(5) . 2_666 ?
O3 Na2 O1 162.91(6) . 1_556 ?
O3 Na2 O2 86.50(6) . . ?
O3 Na2 O4 106.29(6) . . ?
O3 Na2 H4B 90.4 . . ?
O3 Na2 N8 114.52(6) . 1_556 ?
O4 Na2 Na1 147.86(4) . . ?
O4 Na2 Na2 89.37(5) . 2_667 ?
O4 Na2 O1 88.24(6) . 2_666 ?
O4 Na2 O1 90.79(6) . 1_556 ?
O4 Na2 H4B 18.1 . . ?
O4 Na2 N8 86.93(6) . 1_556 ?
N8 Na2 Na1 115.67(5) 1_556 . ?
N8 Na2 Na2 109.04(5) 1_556 2_667 ?
N8 Na2 O1 65.93(5) 1_556 1_556 ?
N8 Na2 O1 156.33(6) 1_556 2_666 ?
N8 Na2 H4B 85.6 1_556 . ?
Na2 O1 Na2 89.00(5) 2_666 1_554 ?
C2 O1 Na2 115.56(11) . 1_554 ?
C2 O1 Na2 154.83(11) . 2_666 ?
Na1 O2 Na2 94.02(6) . . ?
Na1 O2 H2A 113.5 . . ?
Na1 O2 H2B 127.1 . . ?
Na2 O2 H2A 115.3 . . ?
Na2 O2 H2B 105.8 . . ?
H2A O2 H2B 101.4 . . ?
Na1 O3 H3A 113.7 . . ?
Na1 O3 H3B 106.0 . . ?
Na2 O3 Na1 93.49(6) . . ?
Na2 O3 H3A 133.8 . . ?
Na2 O3 H3B 107.0 . . ?
H3A O3 H3B 100.6 . . ?
Na2 O4 H4A 113.1 . . ?
Na2 O4 H4B 98.9 . . ?
H4A O4 H4B 106.3 . . ?
N2 N1 Na1 84.04(10) . 2_566 ?
N2 N1 C1 104.65(14) . . ?
C1 N1 Na1 110.89(11) . 2_566 ?
N3 N2 N1 109.60(14) . . ?
N2 N3 N4 109.74(14) . . ?
N3 N4 Na1 121.24(11) . . ?
N3 N4 C1 104.27(14) . . ?
C1 N4 Na1 133.21(11) . . ?
N6 N5 Na1 118.28(11) . . ?
N6 N5 C3 104.81(13) . . ?
C3 N5 Na1 136.91(11) . . ?
N5 N6 Na1 124.85(11) . 2_556 ?
N7 N6 Na1 122.65(11) . 2_556 ?
N7 N6 N5 109.12(14) . . ?
N8 N7 N6 109.84(14) . . ?
N7 N8 Na2 136.39(12) . 1_554 ?
N7 N8 C3 104.53(14) . . ?
C3 N8 Na2 118.93(11) . 1_554 ?
N1 C1 C2 121.26(15) . . ?
N4 C1 N1 111.73(15) . . ?
N4 C1 C2 126.97(15) . . ?
O1 C2 C1 120.10(15) . . ?
O1 C2 C3 119.42(15) . . ?
C3 C2 C1 120.48(14) . . ?
N5 C3 N8 111.70(14) . . ?
N5 C3 C2 128.21(15) . . ?
N8 C3 C2 120.09(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Na1 N1 N2 N3 109.99(13) 2_566 . . . ?
Na1 N1 C1 N4 -88.97(14) 2_566 . . . ?
Na1 N1 C1 C2 93.14(16) 2_566 . . . ?
Na1 N4 C1 N1 166.52(12) . . . . ?
Na1 N4 C1 C2 -15.7(3) . . . . ?
Na1 N5 N6 Na1 19.91(18) . . . 2_556 ?
Na1 N5 N6 N7 179.48(11) . . . . ?
Na1 N5 C3 N8 -179.45(13) . . . . ?
Na1 N5 C3 C2 1.0(3) . . . . ?
Na1 N6 N7 N8 160.32(12) 2_556 . . . ?
Na2 O1 C2 C1 -178.63(11) 1_554 . . . ?
Na2 O1 C2 C1 14.9(4) 2_666 . . . ?
Na2 O1 C2 C3 -165.3(2) 2_666 . . . ?
Na2 O1 C2 C3 1.1(2) 1_554 . . . ?
Na2 N8 C3 N5 -176.47(11) 1_554 . . . ?
Na2 N8 C3 C2 3.1(2) 1_554 . . . ?
O1 C2 C3 N5 176.64(17) . . . . ?
O1 C2 C3 N8 -2.9(3) . . . . ?
N1 N2 N3 N4 0.0(2) . . . . ?
N1 C1 C2 O1 8.4(3) . . . . ?
N1 C1 C2 C3 -171.35(15) . . . . ?
N2 N1 C1 N4 0.17(19) . . . . ?
N2 N1 C1 C2 -177.72(15) . . . . ?
N2 N3 N4 Na1 -168.57(11) . . . . ?
N2 N3 N4 C1 0.11(19) . . . . ?
N3 N4 C1 N1 -0.18(19) . . . . ?
N3 N4 C1 C2 177.57(16) . . . . ?
N4 C1 C2 O1 -169.14(16) . . . . ?
N4 C1 C2 C3 11.1(3) . . . . ?
N5 N6 N7 N8 0.2(2) . . . . ?
N6 N5 C3 N8 0.2(2) . . . . ?
N6 N5 C3 C2 -179.34(16) . . . . ?
N6 N7 N8 Na2 175.34(13) . . . 1_554 ?
N6 N7 N8 C3 -0.1(2) . . . . ?
N7 N8 C3 N5 -0.1(2) . . . . ?
N7 N8 C3 C2 179.51(15) . . . . ?
C1 N1 N2 N3 -0.09(19) . . . . ?
C1 C2 C3 N5 -3.6(3) . . . . ?
C1 C2 C3 N8 176.90(15) . . . . ?
C3 N5 N6 Na1 -159.81(12) . . . 2_556 ?
C3 N5 N6 N7 -0.25(19) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_bwn19041
_database_code_depnum_ccdc_archive 'CCDC 2078917'
loop_
_audit_author_name
_audit_author_address
'Haibo Li'
;Beijing institute of technology
China
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_audit_creation_date             2019-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H10 N8 O6 Sr'
_chemical_formula_sum            'C3 H10 N8 O6 Sr'
_chemical_formula_weight         341.81
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.6230(13)
_cell_length_b                   12.839(3)
_cell_length_c                   13.282(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1129.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4326
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.5332
_shelx_estimated_absorpt_T_max   0.446
_shelx_estimated_absorpt_T_min   0.404
_exptl_absorpt_coefficient_mu    4.814
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4560
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         3.067
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.689
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                2478
_reflns_number_total             2529
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 
;
 Flack x determined using 983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2529
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0312
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0363P)²+0.1127P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0732
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Sr1 Sr 0.71411(6) 0.25917(3) 0.17977(3) 0.01049(12) Uani 1 1 d . . . . .
O1 O 0.6672(5) 0.3806(2) 0.3518(2) 0.0167(7) Uani 1 1 d . . . . .
O2 O 0.3867(5) 0.3610(2) 0.1572(2) 0.0162(7) Uani 1 1 d . . . . .
H2A H 0.290950 0.340863 0.193868 0.019 Uiso 1 1 d R . . . .
H2B H 0.356030 0.424443 0.155778 0.019 Uiso 1 1 d R . . . .
O3 O 0.6559(5) 0.2473(3) -0.0085(2) 0.0186(7) Uani 1 1 d . . . . .
H3A H 0.651423 0.204383 -0.056242 0.022 Uiso 1 1 d R . . . .
H3B H 0.673013 0.305283 -0.036442 0.022 Uiso 1 1 d R . . . .
O4 O 0.4435(6) 0.1214(2) 0.1626(2) 0.0195(8) Uani 1 1 d . . . . .
H4A H 0.423465 0.095176 0.105567 0.023 Uiso 1 1 d R . . . .
H4B H 0.403035 0.081196 0.208297 0.023 Uiso 1 1 d R . . . .
O5 O 0.9429(5) 0.0990(3) 0.1338(2) 0.0186(7) Uani 1 1 d . . . . .
H5A H 1.008718 0.069568 0.179705 0.022 Uiso 1 1 d R . . . .
H5B H 0.927058 0.054888 0.087775 0.022 Uiso 1 1 d R . . . .
O6 O 1.0617(5) 0.2910(2) 0.2649(2) 0.0147(7) Uani 1 1 d . . . . .
H6A H 1.027580 0.325983 0.315532 0.018 Uiso 1 1 d R . . . .
H6B H 1.102510 0.237413 0.294942 0.018 Uiso 1 1 d R . . . .
N1 N 0.6564(6) 0.5148(3) 0.5179(3) 0.0138(8) Uani 1 1 d . . . . .
N2 N 0.6618(6) 0.5493(3) 0.6123(3) 0.0137(8) Uani 1 1 d . . . . .
N3 N 0.6607(6) 0.4681(3) 0.6754(3) 0.0159(8) Uani 1 1 d . . . . .
N4 N 0.6554(6) 0.3797(3) 0.6219(3) 0.0134(8) Uani 1 1 d . . . . .
N5 N 0.6327(6) 0.1695(3) 0.5288(3) 0.0137(8) Uani 1 1 d . . . . .
N6 N 0.6363(7) 0.0709(3) 0.4957(3) 0.0146(8) Uani 1 1 d . . . . .
N7 N 0.6541(6) 0.0700(3) 0.3962(3) 0.0135(8) Uani 1 1 d . . . . .
N8 N 0.6633(6) 0.1678(3) 0.3632(3) 0.0116(8) Uani 1 1 d . . . . .
C1 C 0.6501(7) 0.2276(3) 0.4458(3) 0.0112(8) Uani 1 1 d . . . . .
C2 C 0.6562(7) 0.3416(3) 0.4361(3) 0.0102(8) Uani 1 1 d . . . . .
C3 C 0.6526(7) 0.4105(3) 0.5250(3) 0.0116(9) 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
Sr1 O1 2.784(3) . ?
Sr1 O2 2.550(3) . ?
Sr1 O3 2.535(3) . ?
Sr1 O4 2.529(3) . ?
Sr1 O5 2.626(3) . ?
Sr1 O6 2.597(3) . ?
Sr1 N2 2.743(4) 2_664 ?
Sr1 N8 2.724(4) . ?
O1 C2 1.229(5) . ?
N1 N2 1.331(4) . ?
N1 C3 1.343(5) . ?
N2 N3 1.337(5) . ?
N3 N4 1.340(5) . ?
N4 C3 1.346(5) . ?
N5 N6 1.341(5) . ?
N5 C1 1.336(5) . ?
N6 N7 1.326(5) . ?
N7 N8 1.332(5) . ?
N8 C1 1.342(5) . ?
C1 C2 1.469(6) . ?
C2 C3 1.475(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Sr1 O1 73.41(10) . . ?
O2 Sr1 O5 149.86(11) . . ?
O2 Sr1 O6 136.42(10) . . ?
O2 Sr1 N2 75.93(11) . 2_664 ?
O2 Sr1 N8 102.74(11) . . ?
O3 Sr1 O1 145.77(10) . . ?
O3 Sr1 O2 77.63(10) . . ?
O3 Sr1 O5 79.10(11) . . ?
O3 Sr1 O6 125.01(10) . . ?
O3 Sr1 N2 77.15(11) . 2_664 ?
O3 Sr1 N8 146.85(11) . . ?
O4 Sr1 O1 112.74(10) . . ?
O4 Sr1 O2 75.24(11) . . ?
O4 Sr1 O3 76.18(10) . . ?
O4 Sr1 O5 80.81(11) . . ?
O4 Sr1 O6 141.03(10) . . ?
O4 Sr1 N2 144.11(11) . 2_664 ?
O4 Sr1 N8 72.04(11) . . ?
O5 Sr1 O1 133.93(10) . . ?
O5 Sr1 N2 116.94(11) . 2_664 ?
O5 Sr1 N8 86.69(10) . . ?
O6 Sr1 O1 69.73(10) . . ?
O6 Sr1 O5 73.32(10) . . ?
O6 Sr1 N2 74.67(10) . 2_664 ?
O6 Sr1 N8 77.76(10) . . ?
N2 Sr1 O1 78.44(10) 2_664 . ?
N8 Sr1 O1 59.55(10) . . ?
N8 Sr1 N2 135.63(11) . 2_664 ?
C2 O1 Sr1 121.8(3) . . ?
N2 N1 C3 105.4(3) . . ?
N1 N2 Sr1 127.9(3) . 2_665 ?
N1 N2 N3 109.3(3) . . ?
N3 N2 Sr1 119.7(3) . 2_665 ?
N2 N3 N4 109.2(3) . . ?
N3 N4 C3 105.0(3) . . ?
C1 N5 N6 104.8(3) . . ?
N7 N6 N5 109.7(4) . . ?
N6 N7 N8 108.9(3) . . ?
N7 N8 Sr1 134.9(3) . . ?
N7 N8 C1 105.5(3) . . ?
C1 N8 Sr1 119.5(3) . . ?
N5 C1 N8 111.2(4) . . ?
N5 C1 C2 129.1(4) . . ?
N8 C1 C2 119.8(4) . . ?
O1 C2 C1 119.1(4) . . ?
O1 C2 C3 119.1(4) . . ?
C1 C2 C3 121.8(4) . . ?
N1 C3 N4 111.1(4) . . ?
N1 C3 C2 122.8(4) . . ?
N4 C3 C2 126.0(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
Sr1 O1 C2 C1 -5.4(6) . . . . ?
Sr1 O1 C2 C3 173.7(3) . . . . ?
Sr1 N2 N3 N4 -161.5(3) 2_665 . . . ?
Sr1 N8 C1 N5 -177.8(3) . . . . ?
Sr1 N8 C1 C2 2.1(5) . . . . ?
O1 C2 C3 N1 1.5(7) . . . . ?
O1 C2 C3 N4 -175.0(4) . . . . ?
N1 N2 N3 N4 0.3(5) . . . . ?
N2 N1 C3 N4 0.0(5) . . . . ?
N2 N1 C3 C2 -176.9(4) . . . . ?
N2 N3 N4 C3 -0.2(5) . . . . ?
N3 N4 C3 N1 0.1(5) . . . . ?
N3 N4 C3 C2 176.9(4) . . . . ?
N5 N6 N7 N8 0.3(5) . . . . ?
N5 C1 C2 O1 -177.9(4) . . . . ?
N5 C1 C2 C3 3.0(8) . . . . ?
N6 N5 C1 N8 0.3(5) . . . . ?
N6 N5 C1 C2 -179.6(5) . . . . ?
N6 N7 N8 Sr1 177.1(3) . . . . ?
N6 N7 N8 C1 -0.1(5) . . . . ?
N7 N8 C1 N5 -0.1(5) . . . . ?
N7 N8 C1 C2 179.8(4) . . . . ?
N8 C1 C2 O1 2.2(7) . . . . ?
N8 C1 C2 C3 -176.9(4) . . . . ?
C1 N5 N6 N7 -0.4(5) . . . . ?
C1 C2 C3 N1 -179.4(4) . . . . ?
C1 C2 C3 N4 4.1(7) . . . . ?
C3 N1 N2 Sr1 159.7(3) . . . 2_665 ?
C3 N1 N2 N3 -0.2(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_bwn17285a
_database_code_depnum_ccdc_archive 'CCDC 2078915'
loop_
_audit_author_name
_audit_author_address
'Haibo Li'
;Beijing institute of technology
China
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_audit_creation_date             2018-01-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C3 H8 Mg N8 O5, 2(H O0.5)'
_chemical_formula_sum            'C3 H10 Mg N8 O6'
_chemical_formula_weight         278.50
_chemical_melting_point          ?
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'
Mg Mg 0.0486 0.0363 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   11.890(2)
_cell_length_b                   16.700(3)
_cell_length_c                   11.228(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2229.4(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4933
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      1.7127
_shelx_estimated_absorpt_T_max   0.961
_shelx_estimated_absorpt_T_min   0.954
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5924
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         2.439
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2187
_reflns_number_total             2515
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2515
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0589
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0460P)²+2.7335P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1363
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B), O6(H6), O7(H7)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Mg1 Mg 0.28034(7) 0.32704(5) 0.53265(7) 0.0172(2) Uani 1 1 d . . . . .
O1 O 0.31341(18) 0.60088(10) 0.67870(17) 0.0277(4) Uani 1 1 d . . . . .
O2 O 0.42213(15) 0.38004(10) 0.45826(16) 0.0218(4) Uani 1 1 d . . . . .
H2A H 0.4706 0.3876 0.5115 0.026 Uiso 1 1 d R . . . .
H2B H 0.4042 0.4252 0.4314 0.026 Uiso 1 1 d R . . . .
O3 O 0.24104(17) 0.28976(10) 0.36644(16) 0.0263(4) Uani 1 1 d . . . . .
H3A H 0.2055 0.2523 0.3335 0.032 Uiso 1 1 d R . . . .
H3B H 0.2807 0.3048 0.3087 0.032 Uiso 1 1 d R . . . .
O4 O 0.37457(16) 0.22989(10) 0.57564(17) 0.0242(4) Uani 1 1 d . . . . .
H4A H 0.3529 0.1856 0.5485 0.029 Uiso 1 1 d R . . . .
H4B H 0.4133 0.2153 0.6343 0.029 Uiso 1 1 d R . . . .
O5 O 0.13804(17) 0.27352(11) 0.60111(19) 0.0293(5) Uani 1 1 d . . . . .
H5A H 0.0975 0.2969 0.6516 0.035 Uiso 1 1 d R . . . .
H5B H 0.1387 0.2232 0.6021 0.035 Uiso 1 1 d R . . . .
N1 N 0.31866(18) 0.38655(12) 0.70252(18) 0.0175(4) Uani 1 1 d . . . . .
N2 N 0.36809(18) 0.34891(12) 0.79426(18) 0.0192(5) Uani 1 1 d . . . . .
N3 N 0.40737(19) 0.40272(12) 0.87006(18) 0.0198(4) Uani 1 1 d . . . . .
N4 N 0.38577(18) 0.47644(12) 0.82923(18) 0.0184(4) Uani 1 1 d . . . . .
N5 N 0.19334(18) 0.44230(12) 0.50306(19) 0.0183(4) Uani 1 1 d . . . . .
N6 N 0.12506(19) 0.45713(12) 0.41079(19) 0.0204(5) Uani 1 1 d . . . . .
N7 N 0.10585(19) 0.53522(12) 0.40501(19) 0.0222(5) Uani 1 1 d . . . . .
N8 N 0.16128(19) 0.57295(12) 0.49180(19) 0.0206(5) Uani 1 1 d . . . . .
C1 C 0.3308(2) 0.46457(14) 0.7271(2) 0.0172(5) Uani 1 1 d . . . . .
C2 C 0.2886(2) 0.53164(14) 0.6537(2) 0.0183(5) Uani 1 1 d . . . . .
C3 C 0.2146(2) 0.51435(14) 0.5509(2) 0.0168(5) Uani 1 1 d . . . . .
O6 O 0.0000 0.35633(15) 0.7500 0.0258(6) Uani 1 2 d S T P . .
H6 H -0.0332 0.3881 0.7039 0.031 Uiso 1 1 d R . . . .
O7 O 0.5000 0.15278(14) 0.7500 0.0218(5) Uani 1 2 d S T P . .
H7 H 0.5363 0.1197 0.7089 0.026 Uiso 1 1 d R . . . .


_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
Mg1 O2 2.079(2) . ?
Mg1 O3 2.022(2) . ?
Mg1 O4 2.0299(19) . ?
Mg1 O5 2.062(2) . ?
Mg1 N1 2.198(2) . ?
Mg1 N5 2.210(2) . ?
O1 C2 1.226(3) . ?
O2 H2A 0.8400 . ?
O2 H2B 0.8400 . ?
O3 H3A 0.8402 . ?
O3 H3B 0.8400 . ?
O4 H4A 0.8400 . ?
O4 H4B 0.8399 . ?
O5 H5A 0.8400 . ?
O5 H5B 0.8399 . ?
N1 N2 1.342(3) . ?
N1 C1 1.340(3) . ?
N2 N3 1.323(3) . ?
N3 N4 1.338(3) . ?
N4 C1 1.335(3) . ?
N5 N6 1.339(3) . ?
N5 C3 1.342(3) . ?
N6 N7 1.325(3) . ?
N7 N8 1.335(3) . ?
N8 C3 1.341(3) . ?
C1 C2 1.479(3) . ?
C2 C3 1.480(3) . ?
O6 H6 0.8398 . ?
O7 H7 0.8397 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mg1 N1 89.31(8) . . ?
O2 Mg1 N5 87.04(8) . . ?
O3 Mg1 O2 87.00(8) . . ?
O3 Mg1 O4 95.80(8) . . ?
O3 Mg1 O5 91.20(9) . . ?
O3 Mg1 N1 171.04(8) . . ?
O3 Mg1 N5 91.22(8) . . ?
O4 Mg1 O2 89.32(8) . . ?
O4 Mg1 O5 91.02(8) . . ?
O4 Mg1 N1 92.32(8) . . ?
O4 Mg1 N5 171.92(9) . . ?
O5 Mg1 O2 178.20(9) . . ?
O5 Mg1 N1 92.44(9) . . ?
O5 Mg1 N5 92.83(8) . . ?
N1 Mg1 N5 80.43(8) . . ?
Mg1 O2 H2A 109.6 . . ?
Mg1 O2 H2B 108.7 . . ?
H2A O2 H2B 107.1 . . ?
Mg1 O3 H3A 138.7 . . ?
Mg1 O3 H3B 119.4 . . ?
H3A O3 H3B 99.5 . . ?
Mg1 O4 H4A 116.6 . . ?
Mg1 O4 H4B 136.2 . . ?
H4A O4 H4B 101.3 . . ?
Mg1 O5 H5A 121.4 . . ?
Mg1 O5 H5B 115.5 . . ?
H5A O5 H5B 117.5 . . ?
N2 N1 Mg1 123.01(15) . . ?
C1 N1 Mg1 129.85(16) . . ?
C1 N1 N2 104.48(19) . . ?
N3 N2 N1 109.28(18) . . ?
N2 N3 N4 109.67(19) . . ?
C1 N4 N3 104.58(19) . . ?
N6 N5 Mg1 124.12(16) . . ?
N6 N5 C3 104.9(2) . . ?
C3 N5 Mg1 129.26(17) . . ?
N7 N6 N5 108.9(2) . . ?
N6 N7 N8 110.1(2) . . ?
N7 N8 C3 104.47(19) . . ?
N1 C1 C2 125.8(2) . . ?
N4 C1 N1 112.0(2) . . ?
N4 C1 C2 122.2(2) . . ?
O1 C2 C1 120.3(2) . . ?
O1 C2 C3 120.4(2) . . ?
C1 C2 C3 119.3(2) . . ?
N5 C3 C2 126.8(2) . . ?
N8 C3 N5 111.6(2) . . ?
N8 C3 C2 121.6(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 N1 N2 N3 163.40(16) . . . . ?
Mg1 N1 C1 N4 -161.28(17) . . . . ?
Mg1 N1 C1 C2 19.6(4) . . . . ?
Mg1 N5 N6 N7 -166.95(17) . . . . ?
Mg1 N5 C3 N8 165.83(17) . . . . ?
Mg1 N5 C3 C2 -12.7(4) . . . . ?
O1 C2 C3 N5 169.9(2) . . . . ?
O1 C2 C3 N8 -8.6(4) . . . . ?
N1 N2 N3 N4 -0.7(3) . . . . ?
N1 C1 C2 O1 -173.2(2) . . . . ?
N1 C1 C2 C3 7.8(4) . . . . ?
N2 N1 C1 N4 0.3(3) . . . . ?
N2 N1 C1 C2 -178.9(2) . . . . ?
N2 N3 N4 C1 0.8(3) . . . . ?
N3 N4 C1 N1 -0.7(3) . . . . ?
N3 N4 C1 C2 178.5(2) . . . . ?
N4 C1 C2 O1 7.7(4) . . . . ?
N4 C1 C2 C3 -171.3(2) . . . . ?
N5 N6 N7 N8 0.5(3) . . . . ?
N6 N5 C3 N8 0.4(3) . . . . ?
N6 N5 C3 C2 -178.2(2) . . . . ?
N6 N7 N8 C3 -0.3(3) . . . . ?
N7 N8 C3 N5 -0.1(3) . . . . ?
N7 N8 C3 C2 178.6(2) . . . . ?
C1 N1 N2 N3 0.3(3) . . . . ?
C1 C2 C3 N5 -11.1(4) . . . . ?
C1 C2 C3 N8 170.4(2) . . . . ?
C3 N5 N6 N7 -0.5(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
