# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 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_201112_TN_KI_2
_database_code_depnum_ccdc_archive 'CCDC 2168840'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Akutagawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C28 H32 I K N8 O14'
_chemical_formula_moiety         'C28 H32 I K N8 O14'
_chemical_formula_weight         870.61
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
_space_group_IT_number           29
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,1/2+Z
3 1/2-X,+Y,1/2+Z
4 1/2+X,-Y,+Z
#------------------------------------------------------------------------------
_cell_length_a                   18.5633(3)
_cell_length_b                   9.31515(17)
_cell_length_c                   21.2695(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3677.91(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    27136
_cell_measurement_theta_min      3.16
_cell_measurement_theta_max      68.21
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1760.00
_exptl_absorpt_coefficient_mu    8.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.239
_exptl_absorpt_correction_T_max  0.427

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            39737
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_theta_max         68.230
_diffrn_reflns_theta_min         4.157
_diffrn_reflns_theta_full        68.230
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6663
_reflns_number_gt                5348
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1468
_refine_ls_wR_factor_gt          0.1378
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6663
_refine_ls_number_parameters     469
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0864P)²+0.8738P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3202 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.574(11)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.3257 6.8362
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
K K 0.3868 1.0657
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.25097(2) 0.24819(4) 0.39937(8) 0.02946(13) Uani 1 1 d . . .
K1 K 0.47027(6) 0.89772(13) 0.65007(7) 0.0268(3) Uani 1 1 d . . .
O1 O 0.5543(2) 0.8620(5) 0.5418(2) 0.0299(10) Uani 1 1 d . . .
O2 O 0.6081(2) 0.7944(5) 0.66448(18) 0.0269(10) Uani 1 1 d . . .
O3 O 0.5294(2) 0.8847(5) 0.77330(19) 0.0294(10) Uani 1 1 d . . .
O4 O 0.4097(2) 1.0178(5) 0.7577(2) 0.0311(10) Uani 1 1 d . . .
O5 O 0.3569(2) 1.0952(4) 0.63551(18) 0.0304(10) Uani 1 1 d . . .
O6 O 0.4379(2) 1.0070(5) 0.52735(18) 0.0311(10) Uani 1 1 d . . .
O7 O 0.3467(3) 0.8697(6) 0.3103(2) 0.0447(13) Uani 1 1 d . . .
O8 O 0.3875(3) 0.6511(7) 0.3057(3) 0.0555(15) Uani 1 1 d . . .
O9 O 0.5343(3) 0.6746(6) 0.2865(2) 0.0522(15) Uani 1 1 d . . .
O10 O 0.5493(3) 0.5128(6) 0.3580(2) 0.0566(15) Uani 1 1 d . . .
O11 O 0.5101(3) 0.6566(6) 0.9889(2) 0.0441(13) Uani 1 1 d . . .
O12 O 0.3940(3) 0.6309(6) 0.9974(2) 0.0481(14) Uani 1 1 d . . .
O13 O 0.3282(3) 0.9007(6) 1.0088(2) 0.0478(14) Uani 1 1 d . . .
O14 O 0.2555(2) 0.8138(7) 0.9391(3) 0.0444(13) Uani 1 1 d . . .
N1 N 0.3872(3) 0.7733(7) 0.3280(3) 0.0398(15) Uani 1 1 d . . .
N2 N 0.5285(3) 0.6307(7) 0.3401(3) 0.0379(14) Uani 1 1 d . . .
N3 N 0.4474(3) 0.6843(7) 0.9723(2) 0.0354(13) Uani 1 1 d . . .
N4 N 0.3141(3) 0.8527(6) 0.9570(3) 0.0342(14) Uani 1 1 d . . .
N5 N 0.5477(3) 1.1715(7) 0.6524(4) 0.0448(14) Uani 1 1 d . . .
N6 N 0.3938(4) 0.6822(7) 0.7234(3) 0.0441(16) Uani 1 1 d . . .
N7 N 0.4037(4) 0.6865(9) 0.5716(3) 0.059(2) Uani 1 1 d . . .
N8 N 0.2336(4) 0.4836(8) 0.6344(4) 0.061(2) Uani 1 1 d . . .
C1 C 0.6204(4) 0.7839(7) 0.5528(3) 0.0300(15) Uani 1 1 d . . .
H1A H 0.6539 0.8003 0.5186 0.036 Uiso 1 1 calc R . .
H1B H 0.6106 0.6818 0.5554 0.036 Uiso 1 1 calc R . .
C2 C 0.6516(3) 0.8358(7) 0.6130(3) 0.0281(15) Uani 1 1 d . . .
H2A H 0.6996 0.7965 0.6182 0.034 Uiso 1 1 calc R . .
H2B H 0.6555 0.9396 0.6119 0.034 Uiso 1 1 calc R . .
C3 C 0.6410(4) 0.8344(9) 0.7224(3) 0.0336(16) Uani 1 1 d . . .
H3A H 0.6499 0.9370 0.7227 0.040 Uiso 1 1 calc R . .
H3B H 0.6870 0.7856 0.7266 0.040 Uiso 1 1 calc R . .
C4 C 0.5928(3) 0.7948(8) 0.7766(3) 0.0312(15) Uani 1 1 d . . .
H4A H 0.5792 0.6944 0.7739 0.037 Uiso 1 1 calc R . .
H4B H 0.6176 0.8102 0.8162 0.037 Uiso 1 1 calc R . .
C5 C 0.4813(3) 0.8704(7) 0.8213(3) 0.0280(15) Uani 1 1 d . . .
C6 C 0.4911(4) 0.7941(8) 0.8751(3) 0.0296(15) Uani 1 1 d . . .
H6 H 0.5351 0.7489 0.8819 0.036 Uiso 1 1 calc R . .
C7 C 0.4382(4) 0.7819(8) 0.9194(3) 0.0295(16) Uani 1 1 d . . .
C8 C 0.3731(3) 0.8528(7) 0.9096(3) 0.0317(15) Uani 1 1 d . . .
C9 C 0.3612(3) 0.9332(7) 0.8566(3) 0.0297(15) Uani 1 1 d . . .
H9 H 0.3175 0.9803 0.8509 0.036 Uiso 1 1 calc R . .
C10 C 0.4144(3) 0.9433(7) 0.8122(3) 0.0294(15) Uani 1 1 d . . .
C11 C 0.3431(3) 1.0948(7) 0.7471(3) 0.0315(15) Uani 1 1 d . . .
H11A H 0.3323 1.1553 0.7830 0.038 Uiso 1 1 calc R . .
H11B H 0.3038 1.0276 0.7415 0.038 Uiso 1 1 calc R . .
C12 C 0.3518(3) 1.1847(8) 0.6895(3) 0.0298(15) Uani 1 1 d . . .
H12A H 0.3108 1.2486 0.6852 0.036 Uiso 1 1 calc R . .
H12B H 0.3949 1.2430 0.6932 0.036 Uiso 1 1 calc R . .
C13 C 0.3641(4) 1.1789(8) 0.5793(3) 0.0315(15) Uani 1 1 d . . .
H13A H 0.4071 1.2379 0.5819 0.038 Uiso 1 1 calc R . .
H13B H 0.3228 1.2418 0.5748 0.038 Uiso 1 1 calc R . .
C14 C 0.3692(3) 1.0805(8) 0.5236(3) 0.0317(15) Uani 1 1 d . . .
H14A H 0.3300 1.0115 0.5242 0.038 Uiso 1 1 calc R . .
H14B H 0.3662 1.1352 0.4849 0.038 Uiso 1 1 calc R . .
C15 C 0.4547(3) 0.9185(8) 0.4791(3) 0.0307(15) Uani 1 1 d . . .
C16 C 0.4142(3) 0.9001(7) 0.4256(3) 0.0298(14) Uani 1 1 d . . .
H16 H 0.3723 0.9532 0.4198 0.036 Uiso 1 1 calc R . .
C17 C 0.4358(4) 0.8023(8) 0.3801(3) 0.0303(16) Uani 1 1 d . . .
C18 C 0.4994(4) 0.7252(7) 0.3888(3) 0.0347(17) Uani 1 1 d . . .
C19 C 0.5411(4) 0.7451(6) 0.4410(3) 0.0313(16) Uani 1 1 d . . .
H19 H 0.5840 0.6947 0.4454 0.038 Uiso 1 1 calc R . .
C20 C 0.5194(3) 0.8399(7) 0.4873(3) 0.0297(15) Uani 1 1 d . . .
C21 C 0.5435(3) 1.2928(7) 0.6532(4) 0.0348(15) Uani 1 1 d . . .
C22 C 0.5358(4) 1.4471(7) 0.6528(4) 0.0461(17) Uani 1 1 d . . .
H22A H 0.5165 1.4773 0.6131 0.055 Uiso 1 1 calc R . .
H22B H 0.5820 1.4909 0.6592 0.055 Uiso 1 1 calc R . .
H22C H 0.5037 1.4757 0.6859 0.055 Uiso 1 1 calc R . .
C23 C 0.3519(4) 0.6305(8) 0.7557(3) 0.0403(18) Uani 1 1 d . . .
C24 C 0.2968(5) 0.5699(9) 0.7957(4) 0.056(2) Uani 1 1 d . . .
H24A H 0.3190 0.5188 0.8298 0.067 Uiso 1 1 calc R . .
H24B H 0.2675 0.5051 0.7717 0.067 Uiso 1 1 calc R . .
H24C H 0.2672 0.6456 0.8122 0.067 Uiso 1 1 calc R . .
C25 C 0.3749(4) 0.6183(8) 0.5354(4) 0.0421(19) Uani 1 1 d . . .
C26 C 0.3388(4) 0.5335(8) 0.4875(4) 0.047(2) Uani 1 1 d . . .
H26A H 0.3147 0.5964 0.4585 0.056 Uiso 1 1 calc R . .
H26B H 0.3041 0.4714 0.5070 0.056 Uiso 1 1 calc R . .
H26C H 0.3736 0.4769 0.4653 0.056 Uiso 1 1 calc R . .
C27 C 0.2332(4) 0.6057(10) 0.6390(4) 0.0438(19) Uani 1 1 d . . .
C28 C 0.2337(5) 0.7629(8) 0.6455(8) 0.056(2) Uani 1 1 d . . .
H28A H 0.2823 0.7957 0.6510 0.068 Uiso 1 1 calc R . .
H28B H 0.2055 0.7899 0.6815 0.068 Uiso 1 1 calc R . .
H28C H 0.2135 0.8057 0.6084 0.068 Uiso 1 1 calc R . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 O2 2.751(4) . ?
K1 O4 2.786(4) . ?
K1 O1 2.802(5) . ?
K1 O5 2.812(4) . ?
K1 O3 2.844(4) . ?
K1 N7 2.860(7) . ?
K1 O6 2.865(4) . ?
K1 N6 2.912(7) . ?
K1 N5 2.928(6) . ?
K1 C2 3.505(6) . ?
O1 C20 1.344(8) . ?
O1 C1 1.444(8) . ?
O2 C2 1.414(7) . ?
O2 C3 1.424(7) . ?
O3 C5 1.362(7) . ?
O3 C4 1.446(7) . ?
O4 C10 1.353(7) . ?
O4 C11 1.446(7) . ?
O5 C12 1.423(7) . ?
O5 C13 1.433(7) . ?
O6 C15 1.353(7) . ?
O6 C14 1.450(7) . ?
O7 N1 1.229(7) . ?
O8 N1 1.234(8) . ?
O9 N2 1.218(7) . ?
O10 N2 1.224(7) . ?
O11 N3 1.243(7) . ?
O12 N3 1.232(7) . ?
O13 N4 1.218(7) . ?
O14 N4 1.208(7) . ?
N1 C17 1.455(9) . ?
N2 C18 1.462(9) . ?
N3 C7 1.456(9) . ?
N4 C8 1.488(8) . ?
N5 C21 1.132(8) . ?
N6 C23 1.144(9) . ?
N7 C25 1.133(9) . ?
N8 C27 1.141(10) . ?
C1 C2 1.486(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.507(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.359(9) . ?
C5 C10 1.429(9) . ?
C6 C7 1.366(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.393(9) . ?
C8 C9 1.372(9) . ?
C9 C10 1.369(8) . ?
C9 H9 0.9300 . ?
C11 C12 1.492(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.502(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.375(8) . ?
C15 C20 1.419(9) . ?
C16 C17 1.388(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.393(10) . ?
C18 C19 1.365(10) . ?
C19 C20 1.383(9) . ?
C19 H19 0.9300 . ?
C21 C22 1.445(9) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.446(11) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.453(10) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.471(11) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?

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 K1 O4 115.12(13) . . ?
O2 K1 O1 62.09(12) . . ?
O4 K1 O1 161.51(14) . . ?
O2 K1 O5 159.57(13) . . ?
O4 K1 O5 61.69(12) . . ?
O1 K1 O5 113.82(13) . . ?
O2 K1 O3 61.55(12) . . ?
O4 K1 O3 54.22(12) . . ?
O1 K1 O3 122.53(13) . . ?
O5 K1 O3 114.71(13) . . ?
O2 K1 N7 103.1(2) . . ?
O4 K1 N7 125.55(17) . . ?
O1 K1 N7 71.28(16) . . ?
O5 K1 N7 93.6(2) . . ?
O3 K1 N7 132.45(19) . . ?
O2 K1 O6 114.89(13) . . ?
O4 K1 O6 121.43(13) . . ?
O1 K1 O6 53.86(12) . . ?
O5 K1 O6 60.68(12) . . ?
O3 K1 O6 159.33(14) . . ?
N7 K1 O6 67.80(19) . . ?
O2 K1 N6 98.78(17) . . ?
O4 K1 N6 68.88(17) . . ?
O1 K1 N6 129.04(17) . . ?
O5 K1 N6 98.36(17) . . ?
O3 K1 N6 70.43(15) . . ?
N7 K1 N6 68.15(16) . . ?
O6 K1 N6 129.09(16) . . ?
O2 K1 N5 81.15(15) . . ?
O4 K1 N5 80.49(17) . . ?
O1 K1 N5 81.02(17) . . ?
O5 K1 N5 78.41(15) . . ?
O3 K1 N5 80.34(17) . . ?
N7 K1 N5 145.2(2) . . ?
O6 K1 N5 78.99(17) . . ?
N6 K1 N5 146.2(2) . . ?
O2 K1 C2 22.20(13) . . ?
O4 K1 C2 129.70(14) . . ?
O1 K1 C2 42.33(13) . . ?
O5 K1 C2 143.27(14) . . ?
O3 K1 C2 80.20(13) . . ?
N7 K1 C2 99.80(19) . . ?
O6 K1 C2 93.16(14) . . ?
N6 K1 C2 118.37(18) . . ?
N5 K1 C2 71.08(16) . . ?
C20 O1 C1 118.2(5) . . ?
C20 O1 K1 117.3(4) . . ?
C1 O1 K1 113.5(3) . . ?
C2 O2 C3 110.7(5) . . ?
C2 O2 K1 110.4(3) . . ?
C3 O2 K1 113.8(3) . . ?
C5 O3 C4 116.1(5) . . ?
C5 O3 K1 116.3(3) . . ?
C4 O3 K1 112.6(3) . . ?
C10 O4 C11 116.4(5) . . ?
C10 O4 K1 118.1(4) . . ?
C11 O4 K1 114.6(3) . . ?
C12 O5 C13 111.1(5) . . ?
C12 O5 K1 110.2(3) . . ?
C13 O5 K1 112.2(4) . . ?
C15 O6 C14 116.6(5) . . ?
C15 O6 K1 115.3(4) . . ?
C14 O6 K1 113.8(3) . . ?
O7 N1 O8 124.0(6) . . ?
O7 N1 C17 118.5(6) . . ?
O8 N1 C17 117.5(7) . . ?
O9 N2 O10 124.4(6) . . ?
O9 N2 C18 119.6(6) . . ?
O10 N2 C18 115.9(6) . . ?
O12 N3 O11 123.2(6) . . ?
O12 N3 C7 119.5(6) . . ?
O11 N3 C7 117.3(6) . . ?
O14 N4 O13 126.0(6) . . ?
O14 N4 C8 116.8(6) . . ?
O13 N4 C8 117.0(6) . . ?
C21 N5 K1 146.7(5) . . ?
C23 N6 K1 160.6(6) . . ?
C25 N7 K1 170.6(7) . . ?
O1 C1 C2 107.9(5) . . ?
O1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
O1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
O2 C2 C1 110.8(5) . . ?
O2 C2 K1 47.3(3) . . ?
C1 C2 K1 82.7(3) . . ?
O2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
K1 C2 H2A 156.8 . . ?
O2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
K1 C2 H2B 85.1 . . ?
H2A C2 H2B 108.1 . . ?
O2 C3 C4 110.1(5) . . ?
O2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
O2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 C3 107.8(5) . . ?
O3 C4 H4A 110.2 . . ?
C3 C4 H4A 110.2 . . ?
O3 C4 H4B 110.2 . . ?
C3 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
C6 C5 O3 126.5(6) . . ?
C6 C5 C10 118.6(6) . . ?
O3 C5 C10 114.9(5) . . ?
C5 C6 C7 121.9(6) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C8 118.8(6) . . ?
C6 C7 N3 120.1(6) . . ?
C8 C7 N3 120.8(6) . . ?
C9 C8 C7 121.4(6) . . ?
C9 C8 N4 116.0(6) . . ?
C7 C8 N4 122.5(6) . . ?
C10 C9 C8 119.2(6) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
O4 C10 C9 125.3(6) . . ?
O4 C10 C5 114.6(5) . . ?
C9 C10 C5 120.0(6) . . ?
O4 C11 C12 108.4(5) . . ?
O4 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
O4 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
O5 C12 C11 109.9(6) . . ?
O5 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
O5 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
O5 C13 C14 109.4(6) . . ?
O5 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
O5 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
O6 C14 C13 107.4(5) . . ?
O6 C14 H14A 110.2 . . ?
C13 C14 H14A 110.2 . . ?
O6 C14 H14B 110.2 . . ?
C13 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O6 C15 C16 125.3(6) . . ?
O6 C15 C20 114.6(5) . . ?
C16 C15 C20 120.0(6) . . ?
C15 C16 C17 120.0(6) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 119.4(6) . . ?
C16 C17 N1 118.2(6) . . ?
C18 C17 N1 122.1(6) . . ?
C19 C18 C17 121.2(6) . . ?
C19 C18 N2 116.6(7) . . ?
C17 C18 N2 122.0(6) . . ?
C18 C19 C20 120.1(7) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
O1 C20 C19 124.9(6) . . ?
O1 C20 C15 115.8(6) . . ?
C19 C20 C15 119.2(6) . . ?
N5 C21 C22 177.9(8) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N6 C23 C24 177.5(9) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N7 C25 C26 178.2(9) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N8 C27 C28 179.1(10) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 K1 O1 C20 154.0(5) . . . . ?
O4 K1 O1 C20 -119.9(5) . . . . ?
O5 K1 O1 C20 -48.3(5) . . . . ?
O3 K1 O1 C20 166.3(4) . . . . ?
N7 K1 O1 C20 37.3(4) . . . . ?
O6 K1 O1 C20 -38.4(4) . . . . ?
N6 K1 O1 C20 76.0(5) . . . . ?
N5 K1 O1 C20 -121.3(4) . . . . ?
C2 K1 O1 C20 167.0(5) . . . . ?
O2 K1 O1 C1 10.5(4) . . . . ?
O4 K1 O1 C1 96.5(6) . . . . ?
O5 K1 O1 C1 168.2(4) . . . . ?
O3 K1 O1 C1 22.7(4) . . . . ?
N7 K1 O1 C1 -106.2(4) . . . . ?
O6 K1 O1 C1 178.0(4) . . . . ?
N6 K1 O1 C1 -67.6(4) . . . . ?
N5 K1 O1 C1 95.2(4) . . . . ?
C2 K1 O1 C1 23.5(4) . . . . ?
O4 K1 O2 C2 -135.9(4) . . . . ?
O1 K1 O2 C2 23.6(4) . . . . ?
O5 K1 O2 C2 -59.9(6) . . . . ?
O3 K1 O2 C2 -144.6(4) . . . . ?
N7 K1 O2 C2 83.9(4) . . . . ?
O6 K1 O2 C2 12.6(4) . . . . ?
N6 K1 O2 C2 153.4(4) . . . . ?
N5 K1 O2 C2 -60.8(4) . . . . ?
O4 K1 O2 C3 -10.7(4) . . . . ?
O1 K1 O2 C3 148.9(4) . . . . ?
O5 K1 O2 C3 65.3(6) . . . . ?
O3 K1 O2 C3 -19.4(4) . . . . ?
N7 K1 O2 C3 -150.9(4) . . . . ?
O6 K1 O2 C3 137.8(4) . . . . ?
N6 K1 O2 C3 -81.4(4) . . . . ?
N5 K1 O2 C3 64.4(4) . . . . ?
C2 K1 O2 C3 125.2(6) . . . . ?
O2 K1 O3 C5 -152.9(5) . . . . ?
O4 K1 O3 C5 36.8(4) . . . . ?
O1 K1 O3 C5 -165.3(4) . . . . ?
O5 K1 O3 C5 49.6(5) . . . . ?
N7 K1 O3 C5 -71.4(5) . . . . ?
O6 K1 O3 C5 121.7(5) . . . . ?
N6 K1 O3 C5 -40.8(4) . . . . ?
N5 K1 O3 C5 122.0(4) . . . . ?
C2 K1 O3 C5 -165.7(4) . . . . ?
O2 K1 O3 C4 -15.5(4) . . . . ?
O4 K1 O3 C4 174.2(5) . . . . ?
O1 K1 O3 C4 -27.9(4) . . . . ?
O5 K1 O3 C4 -173.0(4) . . . . ?
N7 K1 O3 C4 66.0(5) . . . . ?
O6 K1 O3 C4 -101.0(5) . . . . ?
N6 K1 O3 C4 96.6(4) . . . . ?
N5 K1 O3 C4 -100.7(4) . . . . ?
C2 K1 O3 C4 -28.4(4) . . . . ?
O2 K1 O4 C10 -47.9(4) . . . . ?
O1 K1 O4 C10 -124.7(5) . . . . ?
O5 K1 O4 C10 154.7(4) . . . . ?
O3 K1 O4 C10 -38.5(4) . . . . ?
N7 K1 O4 C10 82.1(5) . . . . ?
O6 K1 O4 C10 165.9(4) . . . . ?
N6 K1 O4 C10 42.1(4) . . . . ?
N5 K1 O4 C10 -123.4(4) . . . . ?
C2 K1 O4 C10 -67.9(5) . . . . ?
O2 K1 O4 C11 169.2(4) . . . . ?
O1 K1 O4 C11 92.3(6) . . . . ?
O5 K1 O4 C11 11.8(4) . . . . ?
O3 K1 O4 C11 178.6(5) . . . . ?
N7 K1 O4 C11 -60.9(5) . . . . ?
O6 K1 O4 C11 22.9(4) . . . . ?
N6 K1 O4 C11 -100.8(4) . . . . ?
N5 K1 O4 C11 93.7(4) . . . . ?
C2 K1 O4 C11 149.2(4) . . . . ?
O2 K1 O5 C12 -63.6(5) . . . . ?
O4 K1 O5 C12 22.6(4) . . . . ?
O1 K1 O5 C12 -137.4(4) . . . . ?
O3 K1 O5 C12 10.9(4) . . . . ?
N7 K1 O5 C12 151.5(4) . . . . ?
O6 K1 O5 C12 -146.5(4) . . . . ?
N6 K1 O5 C12 83.1(4) . . . . ?
N5 K1 O5 C12 -62.7(4) . . . . ?
C2 K1 O5 C12 -96.8(4) . . . . ?
O2 K1 O5 C13 60.8(5) . . . . ?
O4 K1 O5 C13 147.1(4) . . . . ?
O1 K1 O5 C13 -12.9(4) . . . . ?
O3 K1 O5 C13 135.3(4) . . . . ?
N7 K1 O5 C13 -84.0(4) . . . . ?
O6 K1 O5 C13 -22.0(4) . . . . ?
N6 K1 O5 C13 -152.5(4) . . . . ?
N5 K1 O5 C13 61.7(4) . . . . ?
C2 K1 O5 C13 27.6(5) . . . . ?
O2 K1 O6 C15 50.5(4) . . . . ?
O4 K1 O6 C15 -163.2(4) . . . . ?
O1 K1 O6 C15 38.4(4) . . . . ?
O5 K1 O6 C15 -152.0(4) . . . . ?
O3 K1 O6 C15 125.5(5) . . . . ?
N7 K1 O6 C15 -44.1(4) . . . . ?
N6 K1 O6 C15 -76.0(5) . . . . ?
N5 K1 O6 C15 125.2(4) . . . . ?
C2 K1 O6 C15 55.2(4) . . . . ?
O2 K1 O6 C14 -171.0(4) . . . . ?
O4 K1 O6 C14 -24.7(5) . . . . ?
O1 K1 O6 C14 176.8(5) . . . . ?
O5 K1 O6 C14 -13.5(4) . . . . ?
O3 K1 O6 C14 -96.0(5) . . . . ?
N7 K1 O6 C14 94.4(4) . . . . ?
N6 K1 O6 C14 62.5(5) . . . . ?
N5 K1 O6 C14 -96.3(4) . . . . ?
C2 K1 O6 C14 -166.3(4) . . . . ?
O2 K1 N5 C21 -173.6(12) . . . . ?
O4 K1 N5 C21 -56.1(12) . . . . ?
O1 K1 N5 C21 123.5(12) . . . . ?
O5 K1 N5 C21 6.8(12) . . . . ?
O3 K1 N5 C21 -111.1(12) . . . . ?
N7 K1 N5 C21 86.3(13) . . . . ?
O6 K1 N5 C21 68.8(12) . . . . ?
N6 K1 N5 C21 -81.0(13) . . . . ?
C2 K1 N5 C21 166.0(12) . . . . ?
O2 K1 N6 C23 146.6(17) . . . . ?
O4 K1 N6 C23 32.9(17) . . . . ?
O1 K1 N6 C23 -152.4(17) . . . . ?
O5 K1 N6 C23 -22.3(17) . . . . ?
O3 K1 N6 C23 91.1(17) . . . . ?
N7 K1 N6 C23 -112.8(17) . . . . ?
O6 K1 N6 C23 -81.0(17) . . . . ?
N5 K1 N6 C23 59.4(18) . . . . ?
C2 K1 N6 C23 157.7(17) . . . . ?
O2 K1 N7 C25 -127(4) . . . . ?
O4 K1 N7 C25 98(4) . . . . ?
O1 K1 N7 C25 -73(4) . . . . ?
O5 K1 N7 C25 41(4) . . . . ?
O3 K1 N7 C25 169(4) . . . . ?
O6 K1 N7 C25 -15(4) . . . . ?
N6 K1 N7 C25 138(4) . . . . ?
N5 K1 N7 C25 -34(4) . . . . ?
C2 K1 N7 C25 -105(4) . . . . ?
C20 O1 C1 C2 175.1(5) . . . . ?
K1 O1 C1 C2 -41.7(6) . . . . ?
C3 O2 C2 C1 175.4(5) . . . . ?
K1 O2 C2 C1 -57.6(6) . . . . ?
C3 O2 C2 K1 -127.0(5) . . . . ?
O1 C1 C2 O2 68.2(7) . . . . ?
O1 C1 C2 K1 29.4(4) . . . . ?
O4 K1 C2 O2 55.0(4) . . . . ?
O1 K1 C2 O2 -148.3(5) . . . . ?
O5 K1 C2 O2 149.7(3) . . . . ?
O3 K1 C2 O2 31.1(4) . . . . ?
N7 K1 C2 O2 -100.6(4) . . . . ?
O6 K1 C2 O2 -168.6(4) . . . . ?
N6 K1 C2 O2 -30.2(4) . . . . ?
N5 K1 C2 O2 114.2(4) . . . . ?
O2 K1 C2 C1 127.3(6) . . . . ?
O4 K1 C2 C1 -177.7(3) . . . . ?
O1 K1 C2 C1 -21.0(3) . . . . ?
O5 K1 C2 C1 -83.0(4) . . . . ?
O3 K1 C2 C1 158.4(4) . . . . ?
N7 K1 C2 C1 26.7(4) . . . . ?
O6 K1 C2 C1 -41.3(4) . . . . ?
N6 K1 C2 C1 97.1(4) . . . . ?
N5 K1 C2 C1 -118.5(4) . . . . ?
C2 O2 C3 C4 177.8(6) . . . . ?
K1 O2 C3 C4 52.7(6) . . . . ?
C5 O3 C4 C3 -175.9(5) . . . . ?
K1 O3 C4 C3 46.6(6) . . . . ?
O2 C3 C4 O3 -67.3(7) . . . . ?
C4 O3 C5 C6 8.6(9) . . . . ?
K1 O3 C5 C6 144.4(6) . . . . ?
C4 O3 C5 C10 -170.8(6) . . . . ?
K1 O3 C5 C10 -34.9(7) . . . . ?
O3 C5 C6 C7 -177.4(6) . . . . ?
C10 C5 C6 C7 2.0(10) . . . . ?
C5 C6 C7 C8 -1.6(10) . . . . ?
C5 C6 C7 N3 172.0(6) . . . . ?
O12 N3 C7 C6 -152.0(7) . . . . ?
O11 N3 C7 C6 26.3(9) . . . . ?
O12 N3 C7 C8 21.5(9) . . . . ?
O11 N3 C7 C8 -160.2(6) . . . . ?
C6 C7 C8 C9 0.4(10) . . . . ?
N3 C7 C8 C9 -173.1(6) . . . . ?
C6 C7 C8 N4 -176.3(6) . . . . ?
N3 C7 C8 N4 10.1(10) . . . . ?
O14 N4 C8 C9 56.9(8) . . . . ?
O13 N4 C8 C9 -118.2(7) . . . . ?
O14 N4 C8 C7 -126.2(7) . . . . ?
O13 N4 C8 C7 58.7(9) . . . . ?
C7 C8 C9 C10 0.3(10) . . . . ?
N4 C8 C9 C10 177.2(6) . . . . ?
C11 O4 C10 C9 1.4(9) . . . . ?
K1 O4 C10 C9 -140.9(5) . . . . ?
C11 O4 C10 C5 -179.1(5) . . . . ?
K1 O4 C10 C5 38.6(7) . . . . ?
C8 C9 C10 O4 179.5(6) . . . . ?
C8 C9 C10 C5 0.1(10) . . . . ?
C6 C5 C10 O4 179.3(6) . . . . ?
O3 C5 C10 O4 -1.3(8) . . . . ?
C6 C5 C10 C9 -1.2(9) . . . . ?
O3 C5 C10 C9 178.2(6) . . . . ?
C10 O4 C11 C12 172.7(5) . . . . ?
K1 O4 C11 C12 -43.7(6) . . . . ?
C13 O5 C12 C11 179.1(5) . . . . ?
K1 O5 C12 C11 -55.9(5) . . . . ?
O4 C11 C12 O5 68.3(7) . . . . ?
C12 O5 C13 C14 -179.8(5) . . . . ?
K1 O5 C13 C14 56.3(6) . . . . ?
C15 O6 C14 C13 -176.4(5) . . . . ?
K1 O6 C14 C13 45.7(6) . . . . ?
O5 C13 C14 O6 -69.1(7) . . . . ?
C14 O6 C15 C16 4.3(9) . . . . ?
K1 O6 C15 C16 141.6(6) . . . . ?
C14 O6 C15 C20 -175.0(6) . . . . ?
K1 O6 C15 C20 -37.7(7) . . . . ?
O6 C15 C16 C17 -177.8(6) . . . . ?
C20 C15 C16 C17 1.4(10) . . . . ?
C15 C16 C17 C18 -1.1(10) . . . . ?
C15 C16 C17 N1 172.6(6) . . . . ?
O7 N1 C17 C16 30.4(9) . . . . ?
O8 N1 C17 C16 -147.2(6) . . . . ?
O7 N1 C17 C18 -156.1(7) . . . . ?
O8 N1 C17 C18 26.3(10) . . . . ?
C16 C17 C18 C19 -0.6(10) . . . . ?
N1 C17 C18 C19 -174.0(6) . . . . ?
C16 C17 C18 N2 -174.3(6) . . . . ?
N1 C17 C18 N2 12.3(10) . . . . ?
O9 N2 C18 C19 -124.9(7) . . . . ?
O10 N2 C18 C19 51.1(9) . . . . ?
O9 N2 C18 C17 49.0(10) . . . . ?
O10 N2 C18 C17 -134.9(7) . . . . ?
C17 C18 C19 C20 1.9(10) . . . . ?
N2 C18 C19 C20 175.9(6) . . . . ?
C1 O1 C20 C19 1.5(9) . . . . ?
K1 O1 C20 C19 -140.3(5) . . . . ?
C1 O1 C20 C15 179.5(6) . . . . ?
K1 O1 C20 C15 37.7(7) . . . . ?
C18 C19 C20 O1 176.4(6) . . . . ?
C18 C19 C20 C15 -1.6(9) . . . . ?
O6 C15 C20 O1 1.1(8) . . . . ?
C16 C15 C20 O1 -178.2(6) . . . . ?
O6 C15 C20 C19 179.2(6) . . . . ?
C16 C15 C20 C19 -0.1(10) . . . . ?
K1 N5 C21 C22 -34(25) . . . . ?
K1 N6 C23 C24 28(20) . . . . ?
K1 N7 C25 C26 40(35) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_210113_TN_NaI
_database_code_depnum_ccdc_archive 'CCDC 2168842'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Akutagawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C26 H29 I N7 Na O14'
_chemical_formula_moiety         'C26 H29 I N7 Na O14'
_chemical_formula_weight         813.45
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_IT_number           61
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,-Z
3 -X,1/2+Y,1/2-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,+Z
7 +X,-1/2-Y,-1/2+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   17.6971(3)
_cell_length_b                   18.6927(3)
_cell_length_c                   20.9582(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     6933.1(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    43948
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      68.28
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3280.00
_exptl_absorpt_coefficient_mu    8.039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_T_max  0.200

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            73769
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_theta_max         68.240
_diffrn_reflns_theta_min         4.035
_diffrn_reflns_theta_full        68.240
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6336
_reflns_number_gt                4715
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0638
_refine_ls_wR_factor_ref         0.1443
_refine_ls_wR_factor_gt          0.1324
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6336
_refine_ls_number_parameters     442
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0534P)²+15.4208P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.31
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Na Na 0.1353 0.1239
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.3257 6.8362
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.88456(2) 0.246094(17) 0.480275(16) 0.03692(14) Uani 1 1 d . . .
Na1 Na 0.71509(13) 0.01272(11) 0.73175(9) 0.0364(5) Uani 1 1 d . . .
O1 O 0.7469(2) 0.05882(19) 0.61077(16) 0.0362(9) Uani 1 1 d . . .
O2 O 0.7982(2) 0.13423(19) 0.71608(17) 0.0358(9) Uani 1 1 d . . .
O3 O 0.7576(2) 0.08788(19) 0.83799(16) 0.0366(9) Uani 1 1 d . . .
O4 O 0.6877(2) -0.02940(18) 0.85249(16) 0.0353(9) Uani 1 1 d . . .
O5 O 0.6593(2) -0.11434(18) 0.74893(17) 0.0317(8) Uani 1 1 d . . .
O6 O 0.6803(2) -0.05970(17) 0.62686(16) 0.0331(9) Uani 1 1 d . . .
O7 O 0.6620(2) 0.1451(2) 0.39289(18) 0.0464(10) Uani 1 1 d . . .
O8 O 0.5481(2) 0.1026(2) 0.3947(2) 0.0550(12) Uani 1 1 d . . .
O9 O 0.5733(3) -0.0375(3) 0.36694(19) 0.0602(13) Uani 1 1 d . . .
O10 O 0.4981(2) -0.0772(2) 0.44036(18) 0.0431(10) Uani 1 1 d . . .
O11 O 0.6559(3) 0.2421(2) 1.02094(19) 0.0485(11) Uani 1 1 d . . .
O12 O 0.6817(3) 0.1646(2) 1.0949(2) 0.0630(13) Uani 1 1 d . . .
O13 O 0.5437(3) 0.1014(2) 1.0743(2) 0.0566(12) Uani 1 1 d . . .
O14 O 0.5597(2) -0.0129(2) 1.06668(18) 0.0466(10) Uani 1 1 d . . .
N1 N 0.6136(3) 0.1034(3) 0.4127(2) 0.0422(12) Uani 1 1 d . . .
N2 N 0.5533(3) -0.0435(3) 0.4221(2) 0.0387(11) Uani 1 1 d . . .
N3 N 0.6671(3) 0.1811(3) 1.0399(2) 0.0418(12) Uani 1 1 d . . .
N4 N 0.5740(3) 0.0491(3) 1.0512(2) 0.0407(12) Uani 1 1 d . . .
N5 N 0.6085(3) 0.0920(3) 0.7161(3) 0.0613(16) Uani 1 1 d . . .
N6 N 0.8360(3) -0.0438(3) 0.7354(2) 0.0418(12) Uani 1 1 d . . .
N7 N 0.4882(3) 0.2643(3) 0.7838(3) 0.0580(16) Uani 1 1 d . . .
C1 C 0.6999(3) 0.0398(3) 0.5634(2) 0.0337(13) Uani 1 1 d . . .
C2 C 0.6851(3) 0.0805(3) 0.5090(2) 0.0337(13) Uani 1 1 d . . .
H2 H 0.7083 0.1246 0.5034 0.040 Uiso 1 1 calc R . .
C3 C 0.6360(3) 0.0546(3) 0.4640(2) 0.0352(13) Uani 1 1 d . . .
C4 C 0.6023(3) -0.0116(3) 0.4716(2) 0.0347(13) Uani 1 1 d . . .
C5 C 0.6157(3) -0.0525(3) 0.5253(2) 0.0323(12) Uani 1 1 d . . .
H5 H 0.5929 -0.0970 0.5301 0.039 Uiso 1 1 calc R . .
C6 C 0.6634(3) -0.0263(3) 0.5715(2) 0.0309(12) Uani 1 1 d . . .
C7 C 0.7866(3) 0.1256(3) 0.6033(3) 0.0368(13) Uani 1 1 d . . .
H7A H 0.7513 0.1653 0.6036 0.044 Uiso 1 1 calc R . .
H7B H 0.8141 0.1263 0.5633 0.044 Uiso 1 1 calc R . .
C8 C 0.8396(3) 0.1313(3) 0.6579(2) 0.0345(13) Uani 1 1 d . . .
H8A H 0.8732 0.0903 0.6583 0.041 Uiso 1 1 calc R . .
H8B H 0.8702 0.1741 0.6534 0.041 Uiso 1 1 calc R . .
C9 C 0.8456(3) 0.1436(3) 0.7695(2) 0.0350(13) Uani 1 1 d . . .
H9A H 0.8776 0.1851 0.7632 0.042 Uiso 1 1 calc R . .
H9B H 0.8779 0.1020 0.7746 0.042 Uiso 1 1 calc R . .
C10 C 0.7984(3) 0.1534(3) 0.8277(2) 0.0361(13) Uani 1 1 d . . .
H10A H 0.8301 0.1640 0.8642 0.043 Uiso 1 1 calc R . .
H10B H 0.7634 0.1928 0.8217 0.043 Uiso 1 1 calc R . .
C11 C 0.7171(3) 0.0831(3) 0.8925(2) 0.0326(12) Uani 1 1 d . . .
C12 C 0.7117(3) 0.1351(3) 0.9387(2) 0.0350(13) Uani 1 1 d . . .
H12 H 0.7380 0.1778 0.9343 0.042 Uiso 1 1 calc R . .
C13 C 0.6671(3) 0.1236(3) 0.9915(2) 0.0343(13) Uani 1 1 d . . .
C14 C 0.6277(3) 0.0604(3) 0.9994(2) 0.0352(13) Uani 1 1 d . . .
C15 C 0.6339(3) 0.0068(3) 0.9535(2) 0.0340(13) Uani 1 1 d . . .
H15 H 0.6083 -0.0362 0.9588 0.041 Uiso 1 1 calc R . .
C16 C 0.6779(3) 0.0176(3) 0.9006(2) 0.0334(13) Uani 1 1 d . . .
C17 C 0.6563(3) -0.0997(3) 0.8612(2) 0.0335(12) Uani 1 1 d . . .
H17A H 0.6015 -0.0974 0.8609 0.040 Uiso 1 1 calc R . .
H17B H 0.6724 -0.1195 0.9018 0.040 Uiso 1 1 calc R . .
C18 C 0.6837(3) -0.1453(3) 0.8079(2) 0.0348(13) Uani 1 1 d . . .
H18A H 0.7384 -0.1481 0.8088 0.042 Uiso 1 1 calc R . .
H18B H 0.6635 -0.1933 0.8121 0.042 Uiso 1 1 calc R . .
C19 C 0.6816(3) -0.1587(3) 0.6969(2) 0.0308(12) Uani 1 1 d . . .
H19A H 0.6643 -0.2074 0.7039 0.037 Uiso 1 1 calc R . .
H19B H 0.7362 -0.1593 0.6933 0.037 Uiso 1 1 calc R . .
C20 C 0.6475(3) -0.1298(3) 0.6371(2) 0.0335(13) Uani 1 1 d . . .
H20A H 0.6588 -0.1610 0.6014 0.040 Uiso 1 1 calc R . .
H20B H 0.5931 -0.1261 0.6415 0.040 Uiso 1 1 calc R . .
C21 C 0.5858(4) 0.1399(4) 0.6887(3) 0.0497(16) Uani 1 1 d . . .
C22 C 0.5565(4) 0.2022(3) 0.6516(3) 0.0556(18) Uani 1 1 d . . .
H22A H 0.5981 0.2295 0.6353 0.067 Uiso 1 1 calc R . .
H22B H 0.5261 0.2318 0.6789 0.067 Uiso 1 1 calc R . .
H22C H 0.5262 0.1852 0.6167 0.067 Uiso 1 1 calc R . .
C23 C 0.9000(4) -0.0513(3) 0.7369(3) 0.0403(14) Uani 1 1 d . . .
C24 C 0.9817(4) -0.0581(4) 0.7382(3) 0.0564(18) Uani 1 1 d . . .
H24A H 1.0043 -0.0116 0.7345 0.068 Uiso 1 1 calc R . .
H24B H 0.9980 -0.0876 0.7033 0.068 Uiso 1 1 calc R . .
H24C H 0.9969 -0.0797 0.7778 0.068 Uiso 1 1 calc R . .
C25 C 0.5138(4) 0.2395(4) 0.8298(4) 0.0509(17) Uani 1 1 d . . .
C26 C 0.5423(4) 0.2081(4) 0.8882(3) 0.0612(19) Uani 1 1 d . . .
H26A H 0.5966 0.2085 0.8875 0.073 Uiso 1 1 calc R . .
H26B H 0.5246 0.1598 0.8918 0.073 Uiso 1 1 calc R . .
H26C H 0.5246 0.2354 0.9240 0.073 Uiso 1 1 calc R . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N6 2.388(6) . ?
Na1 N5 2.422(6) . ?
Na1 O5 2.597(4) . ?
Na1 O6 2.654(4) . ?
Na1 O4 2.694(4) . ?
Na1 O2 2.726(4) . ?
Na1 O1 2.736(4) . ?
Na1 O3 2.738(4) . ?
O1 C1 1.343(6) . ?
O1 C7 1.441(6) . ?
O2 C9 1.410(6) . ?
O2 C8 1.425(6) . ?
O3 C11 1.351(6) . ?
O3 C10 1.438(6) . ?
O4 C16 1.349(6) . ?
O4 C17 1.439(6) . ?
O5 C19 1.426(6) . ?
O5 C18 1.430(6) . ?
O6 C6 1.351(6) . ?
O6 C20 1.449(6) . ?
O7 N1 1.231(6) . ?
O8 N1 1.219(6) . ?
O9 N2 1.216(5) . ?
O10 N2 1.222(6) . ?
O11 N3 1.223(6) . ?
O12 N3 1.221(6) . ?
O13 N4 1.216(6) . ?
O14 N4 1.231(6) . ?
N1 C3 1.465(7) . ?
N2 C4 1.478(7) . ?
N3 C13 1.479(7) . ?
N4 C14 1.457(7) . ?
N5 C21 1.138(8) . ?
N6 C23 1.142(7) . ?
N7 C25 1.162(8) . ?
C1 C2 1.394(7) . ?
C1 C6 1.405(7) . ?
C2 C3 1.371(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.384(8) . ?
C4 C5 1.380(7) . ?
C5 C6 1.376(7) . ?
C5 H5 0.9300 . ?
C7 C8 1.484(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.490(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.376(7) . ?
C11 C16 1.418(7) . ?
C12 C13 1.375(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.381(8) . ?
C14 C15 1.394(8) . ?
C15 C16 1.369(7) . ?
C15 H15 0.9300 . ?
C17 C18 1.487(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.491(7) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.492(9) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.452(9) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.448(9) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

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
N6 Na1 N5 166.8(2) . . ?
N6 Na1 O5 86.08(16) . . ?
N5 Na1 O5 106.38(19) . . ?
N6 Na1 O6 90.49(15) . . ?
N5 Na1 O6 91.10(18) . . ?
O5 Na1 O6 63.91(12) . . ?
N6 Na1 O4 90.10(15) . . ?
N5 Na1 O4 99.55(18) . . ?
O5 Na1 O4 62.24(12) . . ?
O6 Na1 O4 125.96(13) . . ?
N6 Na1 O2 83.63(16) . . ?
N5 Na1 O2 83.93(18) . . ?
O5 Na1 O2 169.69(15) . . ?
O6 Na1 O2 116.77(13) . . ?
O4 Na1 O2 116.98(13) . . ?
N6 Na1 O1 89.12(15) . . ?
N5 Na1 O1 80.92(17) . . ?
O5 Na1 O1 119.65(13) . . ?
O6 Na1 O1 56.01(11) . . ?
O4 Na1 O1 177.89(14) . . ?
O2 Na1 O1 60.98(11) . . ?
N6 Na1 O3 87.41(15) . . ?
N5 Na1 O3 90.59(18) . . ?
O5 Na1 O3 117.45(13) . . ?
O6 Na1 O3 177.39(15) . . ?
O4 Na1 O3 55.63(11) . . ?
O2 Na1 O3 61.46(11) . . ?
O1 Na1 O3 122.37(13) . . ?
C1 O1 C7 116.7(4) . . ?
C1 O1 Na1 118.4(3) . . ?
C7 O1 Na1 118.3(3) . . ?
C9 O2 C8 112.2(4) . . ?
C9 O2 Na1 109.2(3) . . ?
C8 O2 Na1 110.4(3) . . ?
C11 O3 C10 116.7(4) . . ?
C11 O3 Na1 120.5(3) . . ?
C10 O3 Na1 116.9(3) . . ?
C16 O4 C17 116.7(4) . . ?
C16 O4 Na1 122.4(3) . . ?
C17 O4 Na1 117.1(3) . . ?
C19 O5 C18 110.0(4) . . ?
C19 O5 Na1 108.7(3) . . ?
C18 O5 Na1 112.0(3) . . ?
C6 O6 C20 117.2(4) . . ?
C6 O6 Na1 121.8(3) . . ?
C20 O6 Na1 115.5(3) . . ?
O8 N1 O7 124.4(5) . . ?
O8 N1 C3 118.5(5) . . ?
O7 N1 C3 116.9(5) . . ?
O9 N2 O10 125.3(5) . . ?
O9 N2 C4 117.3(5) . . ?
O10 N2 C4 117.2(4) . . ?
O12 N3 O11 125.2(5) . . ?
O12 N3 C13 117.6(5) . . ?
O11 N3 C13 117.1(5) . . ?
O13 N4 O14 124.2(5) . . ?
O13 N4 C14 117.9(5) . . ?
O14 N4 C14 117.8(5) . . ?
C21 N5 Na1 145.6(5) . . ?
C23 N6 Na1 160.8(5) . . ?
O1 C1 C2 125.2(5) . . ?
O1 C1 C6 115.3(4) . . ?
C2 C1 C6 119.5(5) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.6(5) . . ?
C2 C3 N1 117.3(5) . . ?
C4 C3 N1 121.7(5) . . ?
C5 C4 C3 121.1(5) . . ?
C5 C4 N2 116.7(5) . . ?
C3 C4 N2 122.2(5) . . ?
C6 C5 C4 118.8(5) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
O6 C6 C5 125.2(5) . . ?
O6 C6 C1 114.2(5) . . ?
C5 C6 C1 120.7(5) . . ?
O1 C7 C8 106.6(4) . . ?
O1 C7 H7A 110.4 . . ?
C8 C7 H7A 110.4 . . ?
O1 C7 H7B 110.4 . . ?
C8 C7 H7B 110.4 . . ?
H7A C7 H7B 108.6 . . ?
O2 C8 C7 109.7(4) . . ?
O2 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
O2 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
O2 C9 C10 109.3(5) . . ?
O2 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
O2 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
O3 C10 C9 107.5(4) . . ?
O3 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
O3 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
O3 C11 C12 125.8(5) . . ?
O3 C11 C16 114.7(5) . . ?
C12 C11 C16 119.4(5) . . ?
C11 C12 C13 119.7(5) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 121.4(5) . . ?
C12 C13 N3 116.0(5) . . ?
C14 C13 N3 122.6(5) . . ?
C13 C14 C15 119.4(5) . . ?
C13 C14 N4 122.9(5) . . ?
C15 C14 N4 117.4(5) . . ?
C16 C15 C14 119.9(5) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
O4 C16 C15 125.7(5) . . ?
O4 C16 C11 114.1(5) . . ?
C15 C16 C11 120.2(5) . . ?
O4 C17 C18 107.5(4) . . ?
O4 C17 H17A 110.2 . . ?
C18 C17 H17A 110.2 . . ?
O4 C17 H17B 110.2 . . ?
C18 C17 H17B 110.2 . . ?
H17A C17 H17B 108.5 . . ?
O5 C18 C17 108.6(4) . . ?
O5 C18 H18A 110.0 . . ?
C17 C18 H18A 110.0 . . ?
O5 C18 H18B 110.0 . . ?
C17 C18 H18B 110.0 . . ?
H18A C18 H18B 108.3 . . ?
O5 C19 C20 108.6(4) . . ?
O5 C19 H19A 110.0 . . ?
C20 C19 H19A 110.0 . . ?
O5 C19 H19B 110.0 . . ?
C20 C19 H19B 110.0 . . ?
H19A C19 H19B 108.3 . . ?
O6 C20 C19 106.9(4) . . ?
O6 C20 H20A 110.3 . . ?
C19 C20 H20A 110.3 . . ?
O6 C20 H20B 110.3 . . ?
C19 C20 H20B 110.3 . . ?
H20A C20 H20B 108.6 . . ?
N5 C21 C22 179.0(7) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N6 C23 C24 177.9(7) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N7 C25 C26 177.5(7) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 Na1 O1 C1 122.2(4) . . . . ?
N5 Na1 O1 C1 -66.6(4) . . . . ?
O5 Na1 O1 C1 37.2(4) . . . . ?
O6 Na1 O1 C1 31.0(3) . . . . ?
O4 Na1 O1 C1 -170(4) . . . . ?
O2 Na1 O1 C1 -154.6(4) . . . . ?
O3 Na1 O1 C1 -151.4(3) . . . . ?
N6 Na1 O1 C7 -87.3(4) . . . . ?
N5 Na1 O1 C7 84.0(4) . . . . ?
O5 Na1 O1 C7 -172.2(3) . . . . ?
O6 Na1 O1 C7 -178.4(4) . . . . ?
O4 Na1 O1 C7 -19(4) . . . . ?
O2 Na1 O1 C7 -4.0(3) . . . . ?
O3 Na1 O1 C7 -0.9(4) . . . . ?
N6 Na1 O2 C9 -60.1(3) . . . . ?
N5 Na1 O2 C9 124.4(4) . . . . ?
O5 Na1 O2 C9 -56.2(9) . . . . ?
O6 Na1 O2 C9 -147.4(3) . . . . ?
O4 Na1 O2 C9 26.8(4) . . . . ?
O1 Na1 O2 C9 -152.6(4) . . . . ?
O3 Na1 O2 C9 30.4(3) . . . . ?
N6 Na1 O2 C8 63.7(3) . . . . ?
N5 Na1 O2 C8 -111.8(3) . . . . ?
O5 Na1 O2 C8 67.6(9) . . . . ?
O6 Na1 O2 C8 -23.6(4) . . . . ?
O4 Na1 O2 C8 150.6(3) . . . . ?
O1 Na1 O2 C8 -28.8(3) . . . . ?
O3 Na1 O2 C8 154.2(3) . . . . ?
N6 Na1 O3 C11 -120.8(4) . . . . ?
N5 Na1 O3 C11 72.2(4) . . . . ?
O5 Na1 O3 C11 -36.6(4) . . . . ?
O6 Na1 O3 C11 -157(3) . . . . ?
O4 Na1 O3 C11 -29.0(3) . . . . ?
O2 Na1 O3 C11 155.0(4) . . . . ?
O1 Na1 O3 C11 151.8(3) . . . . ?
N6 Na1 O3 C10 86.9(4) . . . . ?
N5 Na1 O3 C10 -80.0(4) . . . . ?
O5 Na1 O3 C10 171.2(3) . . . . ?
O6 Na1 O3 C10 50(3) . . . . ?
O4 Na1 O3 C10 178.8(4) . . . . ?
O2 Na1 O3 C10 2.8(3) . . . . ?
O1 Na1 O3 C10 -0.4(4) . . . . ?
N6 Na1 O4 C16 116.7(4) . . . . ?
N5 Na1 O4 C16 -54.2(4) . . . . ?
O5 Na1 O4 C16 -157.8(4) . . . . ?
O6 Na1 O4 C16 -152.6(4) . . . . ?
O2 Na1 O4 C16 33.8(4) . . . . ?
O1 Na1 O4 C16 49(4) . . . . ?
O3 Na1 O4 C16 29.9(4) . . . . ?
N6 Na1 O4 C17 -86.0(4) . . . . ?
N5 Na1 O4 C17 103.1(4) . . . . ?
O5 Na1 O4 C17 -0.5(3) . . . . ?
O6 Na1 O4 C17 4.7(4) . . . . ?
O2 Na1 O4 C17 -168.9(3) . . . . ?
O1 Na1 O4 C17 -154(4) . . . . ?
O3 Na1 O4 C17 -172.8(4) . . . . ?
N6 Na1 O5 C19 -61.0(3) . . . . ?
N5 Na1 O5 C19 114.5(3) . . . . ?
O6 Na1 O5 C19 31.5(3) . . . . ?
O4 Na1 O5 C19 -153.1(3) . . . . ?
O2 Na1 O5 C19 -64.8(9) . . . . ?
O1 Na1 O5 C19 25.8(3) . . . . ?
O3 Na1 O5 C19 -146.0(3) . . . . ?
N6 Na1 O5 C18 60.8(3) . . . . ?
N5 Na1 O5 C18 -123.7(3) . . . . ?
O6 Na1 O5 C18 153.3(3) . . . . ?
O4 Na1 O5 C18 -31.4(3) . . . . ?
O2 Na1 O5 C18 56.9(9) . . . . ?
O1 Na1 O5 C18 147.5(3) . . . . ?
O3 Na1 O5 C18 -24.2(4) . . . . ?
N6 Na1 O6 C6 -120.1(4) . . . . ?
N5 Na1 O6 C6 46.8(4) . . . . ?
O5 Na1 O6 C6 154.5(4) . . . . ?
O4 Na1 O6 C6 149.5(3) . . . . ?
O2 Na1 O6 C6 -36.9(4) . . . . ?
O1 Na1 O6 C6 -31.5(3) . . . . ?
O3 Na1 O6 C6 -84(3) . . . . ?
N6 Na1 O6 C20 86.8(3) . . . . ?
N5 Na1 O6 C20 -106.3(3) . . . . ?
O5 Na1 O6 C20 1.4(3) . . . . ?
O4 Na1 O6 C20 -3.6(4) . . . . ?
O2 Na1 O6 C20 169.9(3) . . . . ?
O1 Na1 O6 C20 175.4(4) . . . . ?
O3 Na1 O6 C20 123(3) . . . . ?
N6 Na1 N5 C21 18.6(17) . . . . ?
O5 Na1 N5 C21 -141.4(10) . . . . ?
O6 Na1 N5 C21 -78.3(10) . . . . ?
O4 Na1 N5 C21 154.9(10) . . . . ?
O2 Na1 N5 C21 38.5(10) . . . . ?
O1 Na1 N5 C21 -23.0(10) . . . . ?
O3 Na1 N5 C21 99.7(10) . . . . ?
N5 Na1 N6 C23 27(2) . . . . ?
O5 Na1 N6 C23 -172.7(14) . . . . ?
O6 Na1 N6 C23 123.5(14) . . . . ?
O4 Na1 N6 C23 -110.6(14) . . . . ?
O2 Na1 N6 C23 6.6(14) . . . . ?
O1 Na1 N6 C23 67.5(14) . . . . ?
O3 Na1 N6 C23 -55.0(14) . . . . ?
C7 O1 C1 C2 -2.0(8) . . . . ?
Na1 O1 C1 C2 149.0(4) . . . . ?
C7 O1 C1 C6 178.7(4) . . . . ?
Na1 O1 C1 C6 -30.3(6) . . . . ?
O1 C1 C2 C3 179.8(5) . . . . ?
C6 C1 C2 C3 -1.0(8) . . . . ?
C1 C2 C3 C4 -1.1(8) . . . . ?
C1 C2 C3 N1 171.1(5) . . . . ?
O8 N1 C3 C2 -140.4(5) . . . . ?
O7 N1 C3 C2 36.1(7) . . . . ?
O8 N1 C3 C4 31.8(8) . . . . ?
O7 N1 C3 C4 -151.7(5) . . . . ?
C2 C3 C4 C5 1.6(8) . . . . ?
N1 C3 C4 C5 -170.3(5) . . . . ?
C2 C3 C4 N2 -175.6(5) . . . . ?
N1 C3 C4 N2 12.4(8) . . . . ?
O9 N2 C4 C5 -136.0(5) . . . . ?
O10 N2 C4 C5 40.1(7) . . . . ?
O9 N2 C4 C3 41.4(7) . . . . ?
O10 N2 C4 C3 -142.5(5) . . . . ?
C3 C4 C5 C6 0.0(8) . . . . ?
N2 C4 C5 C6 177.4(4) . . . . ?
C20 O6 C6 C5 2.3(7) . . . . ?
Na1 O6 C6 C5 -150.4(4) . . . . ?
C20 O6 C6 C1 -177.1(4) . . . . ?
Na1 O6 C6 C1 30.2(6) . . . . ?
C4 C5 C6 O6 178.5(5) . . . . ?
C4 C5 C6 C1 -2.2(8) . . . . ?
O1 C1 C6 O6 1.4(7) . . . . ?
C2 C1 C6 O6 -177.9(5) . . . . ?
O1 C1 C6 C5 -178.0(5) . . . . ?
C2 C1 C6 C5 2.6(8) . . . . ?
C1 O1 C7 C8 -174.7(4) . . . . ?
Na1 O1 C7 C8 34.3(5) . . . . ?
C9 O2 C8 C7 -176.8(4) . . . . ?
Na1 O2 C8 C7 61.2(4) . . . . ?
O1 C7 C8 O2 -63.2(5) . . . . ?
C8 O2 C9 C10 174.4(4) . . . . ?
Na1 O2 C9 C10 -62.8(5) . . . . ?
C11 O3 C10 C9 173.3(4) . . . . ?
Na1 O3 C10 C9 -33.4(5) . . . . ?
O2 C9 C10 O3 64.8(6) . . . . ?
C10 O3 C11 C12 -0.1(8) . . . . ?
Na1 O3 C11 C12 -152.3(4) . . . . ?
C10 O3 C11 C16 180.0(4) . . . . ?
Na1 O3 C11 C16 27.7(6) . . . . ?
O3 C11 C12 C13 178.7(5) . . . . ?
C16 C11 C12 C13 -1.3(8) . . . . ?
C11 C12 C13 C14 0.3(8) . . . . ?
C11 C12 C13 N3 177.6(5) . . . . ?
O12 N3 C13 C12 -126.6(6) . . . . ?
O11 N3 C13 C12 50.1(7) . . . . ?
O12 N3 C13 C14 50.7(8) . . . . ?
O11 N3 C13 C14 -132.6(6) . . . . ?
C12 C13 C14 C15 0.9(8) . . . . ?
N3 C13 C14 C15 -176.2(5) . . . . ?
C12 C13 C14 N4 -173.5(5) . . . . ?
N3 C13 C14 N4 9.4(8) . . . . ?
O13 N4 C14 C13 25.4(8) . . . . ?
O14 N4 C14 C13 -157.7(5) . . . . ?
O13 N4 C14 C15 -149.1(5) . . . . ?
O14 N4 C14 C15 27.8(7) . . . . ?
C13 C14 C15 C16 -1.1(8) . . . . ?
N4 C14 C15 C16 173.6(5) . . . . ?
C17 O4 C16 C15 -7.6(8) . . . . ?
Na1 O4 C16 C15 149.9(4) . . . . ?
C17 O4 C16 C11 173.3(4) . . . . ?
Na1 O4 C16 C11 -29.3(6) . . . . ?
C14 C15 C16 O4 -179.0(5) . . . . ?
C14 C15 C16 C11 0.1(8) . . . . ?
O3 C11 C16 O4 0.3(7) . . . . ?
C12 C11 C16 O4 -179.7(5) . . . . ?
O3 C11 C16 C15 -178.9(5) . . . . ?
C12 C11 C16 C15 1.1(8) . . . . ?
C16 O4 C17 C18 -171.4(4) . . . . ?
Na1 O4 C17 C18 30.0(5) . . . . ?
C19 O5 C18 C17 -177.2(4) . . . . ?
Na1 O5 C18 C17 61.8(5) . . . . ?
O4 C17 C18 O5 -59.5(5) . . . . ?
C18 O5 C19 C20 173.3(4) . . . . ?
Na1 O5 C19 C20 -63.7(4) . . . . ?
C6 O6 C20 C19 173.3(4) . . . . ?
Na1 O6 C20 C19 -32.3(5) . . . . ?
O5 C19 C20 O6 64.2(5) . . . . ?
Na1 N5 C21 C22 50(44) . . . . ?
Na1 N6 C23 C24 -10(19) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_210217
_database_code_depnum_ccdc_archive 'CCDC 2168843'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Akutagawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C26 H29 I N7 O14 Rb'
_chemical_formula_moiety         'C26 H29 I N7 O14 Rb'
_chemical_formula_weight         875.93
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   10.6237(3)
_cell_length_b                   11.2609(4)
_cell_length_c                   15.1068(5)
_cell_angle_alpha                88.389(6)
_cell_angle_beta                 82.391(6)
_cell_angle_gamma                74.364(5)
_cell_volume                     1725.01(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10795
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      68.30
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872.00
_exptl_absorpt_coefficient_mu    9.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.151
_exptl_absorpt_correction_T_max  0.381

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            18919
_diffrn_reflns_av_unetI/netI     0.1194
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_theta_max         68.240
_diffrn_reflns_theta_min         2.951
_diffrn_reflns_theta_full        68.240
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6167
_reflns_number_gt                5017
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1217
_refine_ls_wR_factor_gt          0.1170
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6167
_refine_ls_number_parameters     442
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0341P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.62
_refine_diff_density_min         -1.30
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Rb Rb -0.4688 1.6079
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.3257 6.8362
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.40387(3) 0.33028(3) 0.28498(2) 0.02978(13) Uani 1 1 d . . .
Rb1 Rb 0.51219(4) 0.61645(4) 0.22941(3) 0.02523(15) Uani 1 1 d . . .
O1 O 0.5519(3) 0.7504(3) 0.0520(2) 0.0224(8) Uani 1 1 d . . .
O2 O 0.6735(3) 0.4908(3) 0.0720(2) 0.0234(8) Uani 1 1 d . . .
O3 O 0.7414(3) 0.4025(3) 0.2436(2) 0.0222(8) Uani 1 1 d . . .
O4 O 0.6950(3) 0.5512(3) 0.3777(2) 0.0266(8) Uani 1 1 d . . .
O5 O 0.5505(3) 0.8000(3) 0.3602(2) 0.0245(8) Uani 1 1 d . . .
O6 O 0.4771(3) 0.8900(3) 0.1914(2) 0.0246(8) Uani 1 1 d . . .
O7 O 0.2041(3) 1.1533(3) -0.1268(2) 0.0348(9) Uani 1 1 d . . .
O8 O 0.2535(3) 0.9635(3) -0.1738(2) 0.0326(9) Uani 1 1 d . . .
O9 O 0.0287(3) 1.1435(3) 0.0283(3) 0.0404(10) Uani 1 1 d . . .
O10 O 0.1263(3) 1.2646(3) 0.0860(2) 0.0327(9) Uani 1 1 d . . .
O11 O 0.6871(3) 0.0229(3) 0.4983(2) 0.0335(9) Uani 1 1 d . . .
O12 O 0.8412(3) -0.0262(3) 0.3852(2) 0.0364(10) Uani 1 1 d . . .
O13 O 0.8515(4) 0.1076(3) 0.5891(2) 0.0350(9) Uani 1 1 d . . .
O14 O 0.7149(3) 0.2732(3) 0.6503(2) 0.0320(9) Uani 1 1 d . . .
N1 N 0.2465(4) 1.0401(4) -0.1160(3) 0.0271(10) Uani 1 1 d . . .
N2 N 0.1258(4) 1.1674(4) 0.0526(3) 0.0292(11) Uani 1 1 d . . .
N3 N 0.7640(4) 0.0493(4) 0.4370(3) 0.0265(10) Uani 1 1 d . . .
N4 N 0.7711(4) 0.2093(4) 0.5843(3) 0.0276(10) Uani 1 1 d . . .
N5 N 0.2614(4) 0.7017(4) 0.1335(3) 0.0346(12) Uani 1 1 d . . .
N6 N 0.0248(6) 0.6138(6) 0.3913(4) 0.074(2) Uani 1 1 d . . .
N7 N 0.0605(4) 0.1603(4) 0.2677(3) 0.0387(12) Uani 1 1 d . . .
C1 C 0.5838(5) 0.6618(4) -0.0209(3) 0.0254(12) Uani 1 1 d . . .
H1A H 0.6014 0.7018 -0.0771 0.031 Uiso 1 1 calc R . .
H1B H 0.5104 0.6270 -0.0244 0.031 Uiso 1 1 calc R . .
C2 C 0.7032(5) 0.5624(5) -0.0033(3) 0.0266(12) Uani 1 1 d . . .
H2A H 0.7351 0.5092 -0.0555 0.032 Uiso 1 1 calc R . .
H2B H 0.7724 0.5992 0.0076 0.032 Uiso 1 1 calc R . .
C3 C 0.7889(4) 0.3950(5) 0.0851(3) 0.0238(12) Uani 1 1 d . . .
H3A H 0.8607 0.4309 0.0910 0.029 Uiso 1 1 calc R . .
H3B H 0.8147 0.3404 0.0335 0.029 Uiso 1 1 calc R . .
C4 C 0.7637(5) 0.3232(4) 0.1666(3) 0.0240(12) Uani 1 1 d . . .
H4A H 0.6871 0.2930 0.1634 0.029 Uiso 1 1 calc R . .
H4B H 0.8390 0.2529 0.1711 0.029 Uiso 1 1 calc R . .
C5 C 0.7393(4) 0.3499(4) 0.3240(3) 0.0203(11) Uani 1 1 d . . .
C6 C 0.7562(4) 0.2238(5) 0.3400(3) 0.0233(12) Uani 1 1 d . . .
H6 H 0.7661 0.1700 0.2924 0.028 Uiso 1 1 calc R . .
C7 C 0.7582(4) 0.1799(5) 0.4243(3) 0.0218(11) Uani 1 1 d . . .
C8 C 0.7465(4) 0.2580(5) 0.4967(3) 0.0220(11) Uani 1 1 d . . .
C9 C 0.7237(4) 0.3836(4) 0.4838(3) 0.0236(12) Uani 1 1 d . . .
H9 H 0.7124 0.4366 0.5320 0.028 Uiso 1 1 calc R . .
C10 C 0.7178(4) 0.4293(5) 0.3978(3) 0.0218(12) Uani 1 1 d . . .
C11 C 0.6587(5) 0.6360(5) 0.4524(3) 0.0293(13) Uani 1 1 d . . .
H11A H 0.7238 0.6139 0.4936 0.035 Uiso 1 1 calc R . .
H11B H 0.5739 0.6334 0.4840 0.035 Uiso 1 1 calc R . .
C12 C 0.6517(5) 0.7625(5) 0.4166(3) 0.0301(13) Uani 1 1 d . . .
H12A H 0.6343 0.8205 0.4658 0.036 Uiso 1 1 calc R . .
H12B H 0.7359 0.7631 0.3829 0.036 Uiso 1 1 calc R . .
C13 C 0.5405(5) 0.9229(4) 0.3318(3) 0.0240(12) Uani 1 1 d . . .
H13A H 0.6245 0.9278 0.3000 0.029 Uiso 1 1 calc R . .
H13B H 0.5204 0.9770 0.3836 0.029 Uiso 1 1 calc R . .
C14 C 0.4362(5) 0.9648(4) 0.2726(3) 0.0271(13) Uani 1 1 d . . .
H14A H 0.3529 0.9548 0.3021 0.033 Uiso 1 1 calc R . .
H14B H 0.4250 1.0512 0.2583 0.033 Uiso 1 1 calc R . .
C15 C 0.4109(5) 0.9299(4) 0.1208(3) 0.0239(12) Uani 1 1 d . . .
C16 C 0.3072(5) 1.0342(4) 0.1206(3) 0.0235(12) Uani 1 1 d . . .
H16 H 0.2776 1.0830 0.1718 0.028 Uiso 1 1 calc R . .
C17 C 0.2480(5) 1.0659(4) 0.0457(3) 0.0261(12) Uani 1 1 d . . .
C18 C 0.2956(5) 0.9970(4) -0.0318(3) 0.0218(11) Uani 1 1 d . . .
C19 C 0.3976(4) 0.8906(4) -0.0331(3) 0.0216(11) Uani 1 1 d . . .
H19 H 0.4276 0.8439 -0.0852 0.026 Uiso 1 1 calc R . .
C20 C 0.4542(5) 0.8545(4) 0.0433(3) 0.0228(12) Uani 1 1 d . . .
C21 C 0.1735(5) 0.7733(5) 0.1655(3) 0.0301(13) Uani 1 1 d . . .
C22 C 0.0590(5) 0.8687(5) 0.2047(4) 0.0411(15) Uani 1 1 d . . .
H22A H 0.0877 0.9302 0.2330 0.049 Uiso 1 1 calc R . .
H22B H 0.0064 0.8324 0.2483 0.049 Uiso 1 1 calc R . .
H22C H 0.0073 0.9061 0.1587 0.049 Uiso 1 1 calc R . .
C23 C 0.0300(5) 0.5650(6) 0.3258(4) 0.0448(16) Uani 1 1 d . . .
C24 C 0.0367(5) 0.5056(5) 0.2400(3) 0.0457(17) Uani 1 1 d . . .
H24A H 0.1272 0.4718 0.2159 0.055 Uiso 1 1 calc R . .
H24B H -0.0063 0.5654 0.1995 0.055 Uiso 1 1 calc R . .
H24C H -0.0066 0.4407 0.2483 0.055 Uiso 1 1 calc R . .
C25 C 0.0786(5) 0.1880(5) 0.3352(4) 0.0311(13) Uani 1 1 d . . .
C26 C 0.0987(5) 0.2247(5) 0.4218(3) 0.0433(16) Uani 1 1 d . . .
H26A H 0.1915 0.2069 0.4254 0.052 Uiso 1 1 calc R . .
H26B H 0.0589 0.1801 0.4673 0.052 Uiso 1 1 calc R . .
H26C H 0.0591 0.3116 0.4304 0.052 Uiso 1 1 calc R . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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
I1 Rb1 3.7422(6) . ?
Rb1 O14 2.832(3) 2_666 ?
Rb1 O2 2.898(3) . ?
Rb1 O3 2.955(3) . ?
Rb1 O5 3.039(3) . ?
Rb1 O6 3.048(3) . ?
Rb1 O1 3.075(3) . ?
Rb1 O4 3.101(3) . ?
Rb1 N5 3.113(4) . ?
Rb1 C5 3.693(5) . ?
Rb1 C4 3.700(5) . ?
O1 C20 1.357(5) . ?
O1 C1 1.451(5) . ?
O2 C2 1.427(5) . ?
O2 C3 1.430(5) . ?
O3 C5 1.336(5) . ?
O3 C4 1.442(5) . ?
O4 C10 1.361(5) . ?
O4 C11 1.443(5) . ?
O5 C13 1.418(5) . ?
O5 C12 1.427(5) . ?
O6 C15 1.355(5) . ?
O6 C14 1.456(5) . ?
O7 N1 1.246(5) . ?
O8 N1 1.225(4) . ?
O9 N2 1.236(5) . ?
O10 N2 1.219(5) . ?
O11 N3 1.236(5) . ?
O12 N3 1.224(5) . ?
O13 N4 1.238(5) . ?
O14 N4 1.232(4) . ?
O14 Rb1 2.832(3) 2_666 ?
N1 C18 1.459(6) . ?
N2 C17 1.475(6) . ?
N3 C7 1.463(6) . ?
N4 C8 1.447(6) . ?
N5 C21 1.119(6) . ?
N6 C23 1.133(7) . ?
N7 C25 1.131(6) . ?
C1 C2 1.497(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.489(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.400(6) . ?
C5 C10 1.405(6) . ?
C6 C7 1.354(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.394(6) . ?
C8 C9 1.382(6) . ?
C9 C10 1.386(6) . ?
C9 H9 0.9300 . ?
C11 C12 1.496(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.486(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.377(6) . ?
C15 C20 1.417(6) . ?
C16 C17 1.359(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.383(6) . ?
C18 C19 1.380(6) . ?
C19 C20 1.372(6) . ?
C19 H19 0.9300 . ?
C21 C22 1.458(7) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.459(7) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.442(7) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

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
O14 Rb1 O2 159.88(9) 2_666 . ?
O14 Rb1 O3 132.90(10) 2_666 . ?
O2 Rb1 O3 58.57(9) . . ?
O14 Rb1 O5 65.17(9) 2_666 . ?
O2 Rb1 O5 133.17(9) . . ?
O3 Rb1 O5 102.51(9) . . ?
O14 Rb1 O6 78.04(9) 2_666 . ?
O2 Rb1 O6 104.86(9) . . ?
O3 Rb1 O6 134.63(8) . . ?
O5 Rb1 O6 55.72(9) . . ?
O14 Rb1 O1 116.71(9) 2_666 . ?
O2 Rb1 O1 57.70(9) . . ?
O3 Rb1 O1 110.15(8) . . ?
O5 Rb1 O1 100.56(8) . . ?
O6 Rb1 O1 49.64(8) . . ?
O14 Rb1 O4 93.95(9) 2_666 . ?
O2 Rb1 O4 104.05(9) . . ?
O3 Rb1 O4 50.25(8) . . ?
O5 Rb1 O4 54.92(9) . . ?
O6 Rb1 O4 106.20(9) . . ?
O1 Rb1 O4 128.98(8) . . ?
O14 Rb1 N5 68.09(10) 2_666 . ?
O2 Rb1 N5 93.27(10) . . ?
O3 Rb1 N5 141.45(10) . . ?
O5 Rb1 N5 116.02(10) . . ?
O6 Rb1 N5 74.06(10) . . ?
O1 Rb1 N5 65.52(10) . . ?
O4 Rb1 N5 161.78(10) . . ?
O14 Rb1 C5 113.51(10) 2_666 . ?
O2 Rb1 C5 77.12(10) . . ?
O3 Rb1 C5 19.40(8) . . ?
O5 Rb1 C5 93.88(10) . . ?
O6 Rb1 C5 140.95(10) . . ?
O1 Rb1 C5 129.29(9) . . ?
O4 Rb1 C5 38.97(9) . . ?
N5 Rb1 C5 144.91(11) . . ?
O14 Rb1 C4 144.11(10) 2_666 . ?
O2 Rb1 C4 40.40(9) . . ?
O3 Rb1 C4 21.51(9) . . ?
O5 Rb1 C4 122.71(10) . . ?
O6 Rb1 C4 137.06(10) . . ?
O1 Rb1 C4 97.03(9) . . ?
O4 Rb1 C4 71.76(9) . . ?
N5 Rb1 C4 120.93(11) . . ?
C5 Rb1 C4 37.49(10) . . ?
O14 Rb1 I1 82.81(7) 2_666 . ?
O2 Rb1 I1 88.53(6) . . ?
O3 Rb1 I1 69.15(6) . . ?
O5 Rb1 I1 127.02(6) . . ?
O6 Rb1 I1 156.21(6) . . ?
O1 Rb1 I1 132.00(6) . . ?
O4 Rb1 I1 88.98(6) . . ?
N5 Rb1 I1 85.81(8) . . ?
C5 Rb1 I1 60.61(7) . . ?
C4 Rb1 I1 64.68(7) . . ?
C20 O1 C1 116.4(4) . . ?
C20 O1 Rb1 113.5(3) . . ?
C1 O1 Rb1 109.1(2) . . ?
C2 O2 C3 109.2(3) . . ?
C2 O2 Rb1 118.8(3) . . ?
C3 O2 Rb1 117.5(2) . . ?
C5 O3 C4 117.6(4) . . ?
C5 O3 Rb1 113.3(3) . . ?
C4 O3 Rb1 109.8(3) . . ?
C10 O4 C11 116.3(4) . . ?
C10 O4 Rb1 110.1(2) . . ?
C11 O4 Rb1 114.7(3) . . ?
C13 O5 C12 109.8(3) . . ?
C13 O5 Rb1 118.6(2) . . ?
C12 O5 Rb1 119.7(3) . . ?
C15 O6 C14 117.1(4) . . ?
C15 O6 Rb1 113.3(3) . . ?
C14 O6 Rb1 112.1(3) . . ?
N4 O14 Rb1 152.3(3) . 2_666 ?
O8 N1 O7 123.3(4) . . ?
O8 N1 C18 118.4(4) . . ?
O7 N1 C18 118.3(4) . . ?
O10 N2 O9 125.5(4) . . ?
O10 N2 C17 118.2(4) . . ?
O9 N2 C17 116.2(4) . . ?
O12 N3 O11 124.2(4) . . ?
O12 N3 C7 118.4(4) . . ?
O11 N3 C7 117.3(4) . . ?
O14 N4 O13 123.2(4) . . ?
O14 N4 C8 118.4(4) . . ?
O13 N4 C8 118.3(4) . . ?
C21 N5 Rb1 119.7(4) . . ?
O1 C1 C2 107.8(4) . . ?
O1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
O1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.5 . . ?
O2 C2 C1 110.9(4) . . ?
O2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.0 . . ?
O2 C3 C4 110.6(4) . . ?
O2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
O2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
O3 C4 C3 108.7(4) . . ?
O3 C4 Rb1 48.7(2) . . ?
C3 C4 Rb1 81.4(3) . . ?
O3 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
Rb1 C4 H4A 83.1 . . ?
O3 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
Rb1 C4 H4B 158.7 . . ?
H4A C4 H4B 108.3 . . ?
O3 C5 C6 125.5(4) . . ?
O3 C5 C10 116.3(4) . . ?
C6 C5 C10 118.2(4) . . ?
O3 C5 Rb1 47.3(2) . . ?
C6 C5 Rb1 140.8(3) . . ?
C10 C5 Rb1 83.1(3) . . ?
C7 C6 C5 120.4(5) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 121.1(5) . . ?
C6 C7 N3 117.4(4) . . ?
C8 C7 N3 121.3(4) . . ?
C9 C8 C7 120.0(5) . . ?
C9 C8 N4 118.5(4) . . ?
C7 C8 N4 121.2(5) . . ?
C8 C9 C10 119.0(4) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
O4 C10 C9 123.8(4) . . ?
O4 C10 C5 115.1(4) . . ?
C9 C10 C5 121.1(5) . . ?
O4 C11 C12 107.7(4) . . ?
O4 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
O4 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
O5 C12 C11 111.0(4) . . ?
O5 C12 H12A 109.4 . . ?
C11 C12 H12A 109.4 . . ?
O5 C12 H12B 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
O5 C13 C14 111.2(4) . . ?
O5 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
O5 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
O6 C14 C13 107.7(4) . . ?
O6 C14 H14A 110.2 . . ?
C13 C14 H14A 110.2 . . ?
O6 C14 H14B 110.2 . . ?
C13 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O6 C15 C16 125.0(4) . . ?
O6 C15 C20 115.2(4) . . ?
C16 C15 C20 119.9(5) . . ?
C17 C16 C15 120.1(5) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 120.2(5) . . ?
C16 C17 N2 117.9(5) . . ?
C18 C17 N2 121.7(5) . . ?
C19 C18 C17 120.9(5) . . ?
C19 C18 N1 118.2(4) . . ?
C17 C18 N1 120.7(4) . . ?
C20 C19 C18 119.4(4) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
O1 C20 C19 125.4(4) . . ?
O1 C20 C15 115.2(4) . . ?
C19 C20 C15 119.4(5) . . ?
N5 C21 C22 178.3(7) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N6 C23 C24 178.3(7) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N7 C25 C26 178.8(6) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O14 Rb1 O1 C20 -1.0(3) 2_666 . . . ?
O2 Rb1 O1 C20 156.7(3) . . . . ?
O3 Rb1 O1 C20 -176.0(3) . . . . ?
O5 Rb1 O1 C20 -68.4(3) . . . . ?
O6 Rb1 O1 C20 -44.0(3) . . . . ?
O4 Rb1 O1 C20 -121.4(3) . . . . ?
N5 Rb1 O1 C20 45.5(3) . . . . ?
C5 Rb1 O1 C20 -172.4(3) . . . . ?
C4 Rb1 O1 C20 166.4(3) . . . . ?
I1 Rb1 O1 C20 104.3(3) . . . . ?
O14 Rb1 O1 C1 -132.6(3) 2_666 . . . ?
O2 Rb1 O1 C1 25.1(3) . . . . ?
O3 Rb1 O1 C1 52.3(3) . . . . ?
O5 Rb1 O1 C1 160.0(3) . . . . ?
O6 Rb1 O1 C1 -175.6(3) . . . . ?
O4 Rb1 O1 C1 106.9(3) . . . . ?
N5 Rb1 O1 C1 -86.1(3) . . . . ?
C5 Rb1 O1 C1 56.0(3) . . . . ?
C4 Rb1 O1 C1 34.8(3) . . . . ?
I1 Rb1 O1 C1 -27.3(3) . . . . ?
O14 Rb1 O2 C2 89.0(4) 2_666 . . . ?
O3 Rb1 O2 C2 -140.4(3) . . . . ?
O5 Rb1 O2 C2 -63.5(3) . . . . ?
O6 Rb1 O2 C2 -6.8(3) . . . . ?
O1 Rb1 O2 C2 9.3(3) . . . . ?
O4 Rb1 O2 C2 -118.2(3) . . . . ?
N5 Rb1 O2 C2 67.5(3) . . . . ?
C5 Rb1 O2 C2 -146.6(3) . . . . ?
C4 Rb1 O2 C2 -155.8(4) . . . . ?
I1 Rb1 O2 C2 153.2(3) . . . . ?
O14 Rb1 O2 C3 -135.9(3) 2_666 . . . ?
O3 Rb1 O2 C3 -5.3(3) . . . . ?
O5 Rb1 O2 C3 71.7(3) . . . . ?
O6 Rb1 O2 C3 128.3(3) . . . . ?
O1 Rb1 O2 C3 144.5(3) . . . . ?
O4 Rb1 O2 C3 17.0(3) . . . . ?
N5 Rb1 O2 C3 -157.3(3) . . . . ?
C5 Rb1 O2 C3 -11.4(3) . . . . ?
C4 Rb1 O2 C3 -20.6(3) . . . . ?
I1 Rb1 O2 C3 -71.6(3) . . . . ?
O14 Rb1 O3 C5 -2.5(3) 2_666 . . . ?
O2 Rb1 O3 C5 -161.6(3) . . . . ?
O5 Rb1 O3 C5 65.1(3) . . . . ?
O6 Rb1 O3 C5 118.8(3) . . . . ?
O1 Rb1 O3 C5 171.4(3) . . . . ?
O4 Rb1 O3 C5 46.9(3) . . . . ?
N5 Rb1 O3 C5 -112.9(3) . . . . ?
C4 Rb1 O3 C5 -133.7(4) . . . . ?
I1 Rb1 O3 C5 -60.0(3) . . . . ?
O14 Rb1 O3 C4 131.2(2) 2_666 . . . ?
O2 Rb1 O3 C4 -27.9(2) . . . . ?
O5 Rb1 O3 C4 -161.2(3) . . . . ?
O6 Rb1 O3 C4 -107.5(3) . . . . ?
O1 Rb1 O3 C4 -54.9(3) . . . . ?
O4 Rb1 O3 C4 -179.4(3) . . . . ?
N5 Rb1 O3 C4 20.8(3) . . . . ?
C5 Rb1 O3 C4 133.7(4) . . . . ?
I1 Rb1 O3 C4 73.6(2) . . . . ?
O14 Rb1 O4 C10 102.3(3) 2_666 . . . ?
O2 Rb1 O4 C10 -68.6(3) . . . . ?
O3 Rb1 O4 C10 -43.8(3) . . . . ?
O5 Rb1 O4 C10 158.1(3) . . . . ?
O6 Rb1 O4 C10 -179.0(3) . . . . ?
O1 Rb1 O4 C10 -128.2(3) . . . . ?
N5 Rb1 O4 C10 92.9(4) . . . . ?
C5 Rb1 O4 C10 -21.1(3) . . . . ?
C4 Rb1 O4 C10 -44.0(3) . . . . ?
I1 Rb1 O4 C10 19.6(3) . . . . ?
O14 Rb1 O4 C11 -31.1(3) 2_666 . . . ?
O2 Rb1 O4 C11 158.0(3) . . . . ?
O3 Rb1 O4 C11 -177.2(3) . . . . ?
O5 Rb1 O4 C11 24.6(3) . . . . ?
O6 Rb1 O4 C11 47.6(3) . . . . ?
O1 Rb1 O4 C11 98.4(3) . . . . ?
N5 Rb1 O4 C11 -40.6(5) . . . . ?
C5 Rb1 O4 C11 -154.5(3) . . . . ?
C4 Rb1 O4 C11 -177.4(3) . . . . ?
I1 Rb1 O4 C11 -113.8(3) . . . . ?
O14 Rb1 O5 C13 -96.8(3) 2_666 . . . ?
O2 Rb1 O5 C13 73.1(3) . . . . ?
O3 Rb1 O5 C13 131.4(3) . . . . ?
O6 Rb1 O5 C13 -4.6(3) . . . . ?
O1 Rb1 O5 C13 17.8(3) . . . . ?
O4 Rb1 O5 C13 148.5(3) . . . . ?
N5 Rb1 O5 C13 -49.9(3) . . . . ?
C5 Rb1 O5 C13 149.0(3) . . . . ?
C4 Rb1 O5 C13 123.4(3) . . . . ?
I1 Rb1 O5 C13 -155.4(3) . . . . ?
O14 Rb1 O5 C12 124.1(3) 2_666 . . . ?
O2 Rb1 O5 C12 -66.0(3) . . . . ?
O3 Rb1 O5 C12 -7.6(3) . . . . ?
O6 Rb1 O5 C12 -143.7(3) . . . . ?
O1 Rb1 O5 C12 -121.2(3) . . . . ?
O4 Rb1 O5 C12 9.4(3) . . . . ?
N5 Rb1 O5 C12 171.0(3) . . . . ?
C5 Rb1 O5 C12 9.9(3) . . . . ?
C4 Rb1 O5 C12 -15.7(3) . . . . ?
I1 Rb1 O5 C12 65.5(3) . . . . ?
O14 Rb1 O6 C15 -96.2(3) 2_666 . . . ?
O2 Rb1 O6 C15 63.4(3) . . . . ?
O3 Rb1 O6 C15 123.6(3) . . . . ?
O5 Rb1 O6 C15 -164.1(3) . . . . ?
O1 Rb1 O6 C15 45.4(3) . . . . ?
O4 Rb1 O6 C15 173.2(3) . . . . ?
N5 Rb1 O6 C15 -25.8(3) . . . . ?
C5 Rb1 O6 C15 151.1(3) . . . . ?
C4 Rb1 O6 C15 92.7(3) . . . . ?
I1 Rb1 O6 C15 -59.0(3) . . . . ?
O14 Rb1 O6 C14 39.1(3) 2_666 . . . ?
O2 Rb1 O6 C14 -161.3(3) . . . . ?
O3 Rb1 O6 C14 -101.1(3) . . . . ?
O5 Rb1 O6 C14 -28.8(3) . . . . ?
O1 Rb1 O6 C14 -179.3(3) . . . . ?
O4 Rb1 O6 C14 -51.5(3) . . . . ?
N5 Rb1 O6 C14 109.5(3) . . . . ?
C5 Rb1 O6 C14 -73.6(3) . . . . ?
C4 Rb1 O6 C14 -132.0(3) . . . . ?
I1 Rb1 O6 C14 76.3(3) . . . . ?
Rb1 O14 N4 O13 -111.3(7) 2_666 . . . ?
Rb1 O14 N4 C8 71.5(8) 2_666 . . . ?
O14 Rb1 N5 C21 20.7(5) 2_666 . . . ?
O2 Rb1 N5 C21 -167.1(5) . . . . ?
O3 Rb1 N5 C21 152.9(4) . . . . ?
O5 Rb1 N5 C21 -24.9(5) . . . . ?
O6 Rb1 N5 C21 -62.6(5) . . . . ?
O1 Rb1 N5 C21 -115.0(5) . . . . ?
O4 Rb1 N5 C21 30.8(7) . . . . ?
C5 Rb1 N5 C21 120.8(5) . . . . ?
C4 Rb1 N5 C21 161.6(5) . . . . ?
I1 Rb1 N5 C21 104.6(5) . . . . ?
C20 O1 C1 C2 173.3(4) . . . . ?
Rb1 O1 C1 C2 -56.6(4) . . . . ?
C3 O2 C2 C1 178.5(4) . . . . ?
Rb1 O2 C2 C1 -43.0(5) . . . . ?
O1 C1 C2 O2 68.3(5) . . . . ?
C2 O2 C3 C4 176.5(4) . . . . ?
Rb1 O2 C3 C4 37.3(5) . . . . ?
C5 O3 C4 C3 -168.9(4) . . . . ?
Rb1 O3 C4 C3 59.6(4) . . . . ?
C5 O3 C4 Rb1 131.5(4) . . . . ?
O2 C3 C4 O3 -66.1(5) . . . . ?
O2 C3 C4 Rb1 -25.2(3) . . . . ?
O14 Rb1 C4 O3 -70.1(3) 2_666 . . . ?
O2 Rb1 C4 O3 141.9(3) . . . . ?
O5 Rb1 C4 O3 21.9(3) . . . . ?
O6 Rb1 C4 O3 94.9(3) . . . . ?
O1 Rb1 C4 O3 129.3(2) . . . . ?
O4 Rb1 C4 O3 0.5(2) . . . . ?
N5 Rb1 C4 O3 -165.1(2) . . . . ?
C5 Rb1 C4 O3 -23.2(2) . . . . ?
I1 Rb1 C4 O3 -97.3(3) . . . . ?
O14 Rb1 C4 C3 165.6(2) 2_666 . . . ?
O2 Rb1 C4 C3 17.7(2) . . . . ?
O3 Rb1 C4 C3 -124.3(4) . . . . ?
O5 Rb1 C4 C3 -102.3(3) . . . . ?
O6 Rb1 C4 C3 -29.3(3) . . . . ?
O1 Rb1 C4 C3 5.0(3) . . . . ?
O4 Rb1 C4 C3 -123.8(3) . . . . ?
N5 Rb1 C4 C3 70.7(3) . . . . ?
C5 Rb1 C4 C3 -147.5(3) . . . . ?
I1 Rb1 C4 C3 138.5(3) . . . . ?
C4 O3 C5 C6 -0.3(6) . . . . ?
Rb1 O3 C5 C6 129.5(4) . . . . ?
C4 O3 C5 C10 179.8(4) . . . . ?
Rb1 O3 C5 C10 -50.3(4) . . . . ?
C4 O3 C5 Rb1 -129.9(4) . . . . ?
O14 Rb1 C5 O3 178.0(3) 2_666 . . . ?
O2 Rb1 C5 O3 16.0(3) . . . . ?
O5 Rb1 C5 O3 -117.4(3) . . . . ?
O6 Rb1 C5 O3 -81.8(3) . . . . ?
O1 Rb1 C5 O3 -10.4(3) . . . . ?
O4 Rb1 C5 O3 -116.7(3) . . . . ?
N5 Rb1 C5 O3 93.1(3) . . . . ?
C4 Rb1 C5 O3 25.8(3) . . . . ?
I1 Rb1 C5 O3 111.7(3) . . . . ?
O14 Rb1 C5 C6 81.2(5) 2_666 . . . ?
O2 Rb1 C5 C6 -80.8(5) . . . . ?
O3 Rb1 C5 C6 -96.8(6) . . . . ?
O5 Rb1 C5 C6 145.8(5) . . . . ?
O6 Rb1 C5 C6 -178.6(4) . . . . ?
O1 Rb1 C5 C6 -107.2(5) . . . . ?
O4 Rb1 C5 C6 146.5(6) . . . . ?
N5 Rb1 C5 C6 -3.7(6) . . . . ?
C4 Rb1 C5 C6 -71.0(5) . . . . ?
I1 Rb1 C5 C6 14.9(5) . . . . ?
O14 Rb1 C5 C10 -46.0(3) 2_666 . . . ?
O2 Rb1 C5 C10 152.0(3) . . . . ?
O3 Rb1 C5 C10 135.9(4) . . . . ?
O5 Rb1 C5 C10 18.5(3) . . . . ?
O6 Rb1 C5 C10 54.2(3) . . . . ?
O1 Rb1 C5 C10 125.5(3) . . . . ?
O4 Rb1 C5 C10 19.2(2) . . . . ?
N5 Rb1 C5 C10 -131.0(3) . . . . ?
C4 Rb1 C5 C10 161.8(4) . . . . ?
I1 Rb1 C5 C10 -112.4(3) . . . . ?
O3 C5 C6 C7 176.9(4) . . . . ?
C10 C5 C6 C7 -3.2(6) . . . . ?
Rb1 C5 C6 C7 -119.5(5) . . . . ?
C5 C6 C7 C8 -1.4(7) . . . . ?
C5 C6 C7 N3 174.5(4) . . . . ?
O12 N3 C7 C6 44.7(6) . . . . ?
O11 N3 C7 C6 -133.1(5) . . . . ?
O12 N3 C7 C8 -139.4(5) . . . . ?
O11 N3 C7 C8 42.7(6) . . . . ?
C6 C7 C8 C9 4.3(7) . . . . ?
N3 C7 C8 C9 -171.4(4) . . . . ?
C6 C7 C8 N4 -169.3(4) . . . . ?
N3 C7 C8 N4 15.1(7) . . . . ?
O14 N4 C8 C9 33.4(6) . . . . ?
O13 N4 C8 C9 -143.9(4) . . . . ?
O14 N4 C8 C7 -153.0(4) . . . . ?
O13 N4 C8 C7 29.7(6) . . . . ?
C7 C8 C9 C10 -2.4(7) . . . . ?
N4 C8 C9 C10 171.3(4) . . . . ?
C11 O4 C10 C9 -8.1(6) . . . . ?
Rb1 O4 C10 C9 -140.7(4) . . . . ?
C11 O4 C10 C5 173.6(4) . . . . ?
Rb1 O4 C10 C5 41.0(4) . . . . ?
C8 C9 C10 O4 179.5(4) . . . . ?
C8 C9 C10 C5 -2.3(7) . . . . ?
O3 C5 C10 O4 3.3(6) . . . . ?
C6 C5 C10 O4 -176.6(4) . . . . ?
Rb1 C5 C10 O4 -31.4(3) . . . . ?
O3 C5 C10 C9 -175.0(4) . . . . ?
C6 C5 C10 C9 5.1(7) . . . . ?
Rb1 C5 C10 C9 150.3(4) . . . . ?
C10 O4 C11 C12 174.4(4) . . . . ?
Rb1 O4 C11 C12 -55.2(4) . . . . ?
C13 O5 C12 C11 176.3(4) . . . . ?
Rb1 O5 C12 C11 -41.4(5) . . . . ?
O4 C11 C12 O5 63.6(5) . . . . ?
C12 O5 C13 C14 179.7(4) . . . . ?
Rb1 O5 C13 C14 36.9(4) . . . . ?
C15 O6 C14 C13 -166.1(4) . . . . ?
Rb1 O6 C14 C13 60.4(4) . . . . ?
O5 C13 C14 O6 -65.1(5) . . . . ?
C14 O6 C15 C16 -1.1(7) . . . . ?
Rb1 O6 C15 C16 131.9(4) . . . . ?
C14 O6 C15 C20 179.8(4) . . . . ?
Rb1 O6 C15 C20 -47.2(5) . . . . ?
O6 C15 C16 C17 179.8(4) . . . . ?
C20 C15 C16 C17 -1.2(7) . . . . ?
C15 C16 C17 C18 -3.1(8) . . . . ?
C15 C16 C17 N2 171.2(4) . . . . ?
O10 N2 C17 C16 51.4(7) . . . . ?
O9 N2 C17 C16 -124.6(5) . . . . ?
O10 N2 C17 C18 -134.4(5) . . . . ?
O9 N2 C17 C18 49.6(7) . . . . ?
C16 C17 C18 C19 4.4(8) . . . . ?
N2 C17 C18 C19 -169.6(5) . . . . ?
C16 C17 C18 N1 -170.6(4) . . . . ?
N2 C17 C18 N1 15.4(7) . . . . ?
O8 N1 C18 C19 29.8(6) . . . . ?
O7 N1 C18 C19 -147.6(4) . . . . ?
O8 N1 C18 C17 -155.0(4) . . . . ?
O7 N1 C18 C17 27.6(7) . . . . ?
C17 C18 C19 C20 -1.4(7) . . . . ?
N1 C18 C19 C20 173.7(4) . . . . ?
C1 O1 C20 C19 -10.2(7) . . . . ?
Rb1 O1 C20 C19 -138.1(4) . . . . ?
C1 O1 C20 C15 170.4(4) . . . . ?
Rb1 O1 C20 C15 42.5(5) . . . . ?
C18 C19 C20 O1 177.8(4) . . . . ?
C18 C19 C20 C15 -2.8(7) . . . . ?
O6 C15 C20 O1 2.7(6) . . . . ?
C16 C15 C20 O1 -176.4(4) . . . . ?
O6 C15 C20 C19 -176.8(4) . . . . ?
C16 C15 C20 C19 4.1(7) . . . . ?
Rb1 N5 C21 C22 130(20) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_210108_TN_LiI
_database_code_depnum_ccdc_archive 'CCDC 2168847'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Akutagawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H23 N5 O14'
_chemical_formula_moiety         'C22 H23 N5 O14'
_chemical_formula_weight         581.45
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   7.5672(3)
_cell_length_b                   22.2189(8)
_cell_length_c                   15.2555(6)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     2564.97(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12918
_cell_measurement_theta_min      3.52
_cell_measurement_theta_max      68.20
_cell_measurement_temperature    99
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1208.00
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_T_max  0.895

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      99
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            26379
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_theta_max         68.199
_diffrn_reflns_theta_min         3.514
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             2407
_reflns_number_gt                1657
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1395
_refine_ls_wR_factor_gt          0.1251
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         2407
_refine_ls_number_parameters     194
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0636P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
O2 O 0.9575(3) 0.250000 0.15373(15) 0.0367(6) Uani 1 2 d S T P . .
O3 O 0.9703(2) 0.13922(7) 0.42111(11) 0.0391(5) Uani 1 1 d . . . . .
O4 O 0.9809(3) 0.250000 0.52211(16) 0.0399(7) Uani 1 2 d S T P . .
O5 O 0.6143(3) -0.04778(8) 0.17153(12) 0.0489(5) Uani 1 1 d . . . . .
O7 O 0.6743(3) -0.05720(8) 0.50813(13) 0.0575(6) Uani 1 1 d . . . . .
O15 O 0.4858(3) -0.06296(9) 0.40151(14) 0.0568(6) Uani 1 1 d . . . . .
O16 O 0.7125(3) -0.10551(7) 0.27552(13) 0.0578(6) Uani 1 1 d . . . . .
O19 O 0.9636(2) 0.13937(6) 0.25442(11) 0.0365(5) Uani 1 1 d . . . . .
N1 N 0.4927(6) 0.250000 0.5970(3) 0.1034(18) Uani 1 2 d S T P . .
N2 N 0.6236(4) -0.04421(9) 0.43467(17) 0.0463(6) Uani 1 1 d . . . . .
N17 N 0.6813(3) -0.05611(9) 0.24375(16) 0.0441(6) Uani 1 1 d . . . . .
C2 C 0.8870(4) 0.09156(11) 0.29228(17) 0.0364(7) Uani 1 1 d . . . . .
C3 C 0.7340(4) -0.00294(10) 0.29427(17) 0.0366(6) Uani 1 1 d . . . . .
C4 C 0.8114(3) 0.04385(10) 0.24748(17) 0.0380(6) Uani 1 1 d . . . . .
H4 H 0.812259 0.043125 0.186529 0.046 Uiso 1 1 calc R U . . .
C6 C 1.0544(3) 0.19741(10) 0.13147(18) 0.0367(7) Uani 1 1 d . . . . .
H6A H 1.168378 0.197808 0.160543 0.044 Uiso 1 1 calc R U . . .
H6B H 1.074075 0.195997 0.068678 0.044 Uiso 1 1 calc R U . . .
C7 C 0.9721(4) 0.14327(11) 0.51548(16) 0.0405(7) Uani 1 1 d . . . . .
H7A H 1.023515 0.107177 0.540600 0.049 Uiso 1 1 calc R U . . .
H7B H 0.852754 0.147645 0.537739 0.049 Uiso 1 1 calc R U . . .
C8 C 0.7285(4) -0.00126(10) 0.38456(17) 0.0386(7) Uani 1 1 d . . . . .
C9 C 0.8078(4) 0.04538(10) 0.43029(18) 0.0399(7) Uani 1 1 d . . . . .
H9 H 0.805851 0.045716 0.491241 0.048 Uiso 1 1 calc R U . . .
C10 C 1.0809(4) 0.19729(11) 0.53916(18) 0.0422(7) Uani 1 1 d . . . . .
H10A H 1.112814 0.195692 0.600696 0.051 Uiso 1 1 calc R U . . .
H10B H 1.188744 0.197773 0.504789 0.051 Uiso 1 1 calc R U . . .
C11 C 0.8898(4) 0.09137(11) 0.38490(17) 0.0369(6) Uani 1 1 d . . . . .
C12 C 0.7503(6) 0.250000 0.7062(3) 0.0508(11) Uani 1 2 d S T P . .
H12A H 0.777601 0.290650 0.722668 0.061 Uiso 0.5 1 calc R U P . .
H12B H 0.851781 0.231956 0.679101 0.061 Uiso 0.5 1 calc R U P . .
H12C H 0.718389 0.227394 0.757445 0.061 Uiso 0.5 1 calc R U P . .
C13 C 0.6054(7) 0.250000 0.6455(3) 0.0573(12) Uani 1 2 d S T P . .
C14 C 0.9508(4) 0.14384(10) 0.15987(16) 0.0358(6) Uani 1 1 d . . . . .
H14A H 0.828229 0.148191 0.142415 0.043 Uiso 1 1 calc R U . . .
H14B H 0.997844 0.107748 0.132741 0.043 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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
O2 C6 1.420(3) . ?
O2 C6 1.420(3) 7_565 ?
O3 C11 1.344(3) . ?
O3 C7 1.443(3) . ?
O4 C10 1.418(3) . ?
O4 C10 1.418(3) 7_565 ?
O5 N17 1.227(3) . ?
O7 N2 1.219(3) . ?
O15 N2 1.231(3) . ?
O16 N17 1.223(2) . ?
O19 C2 1.341(3) . ?
O19 C14 1.449(3) . ?
N1 C13 1.130(6) . ?
N2 C8 1.458(3) . ?
N17 C3 1.466(3) . ?
C2 C4 1.385(3) . ?
C2 C11 1.413(3) . ?
C3 C8 1.379(3) . ?
C3 C4 1.390(3) . ?
C4 H4 0.9300 . ?
C6 C14 1.490(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C10 1.500(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.386(3) . ?
C9 C11 1.381(3) . ?
C9 H9 0.9300 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C13 1.435(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12 H12A 0.960(3) 7_565 ?
C12 H12B 0.960(17) 7_565 ?
C12 H12C 0.96(2) 7_565 ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?

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
C6 O2 C6 110.7(3) . 7_565 ?
C11 O3 C7 117.6(2) . . ?
C10 O4 C10 111.3(3) . 7_565 ?
C2 O19 C14 117.03(19) . . ?
O7 N2 O15 124.3(2) . . ?
O7 N2 C8 117.7(3) . . ?
O15 N2 C8 117.8(2) . . ?
O16 N17 O5 124.8(2) . . ?
O16 N17 C3 117.5(2) . . ?
O5 N17 C3 117.6(2) . . ?
O19 C2 C4 124.9(2) . . ?
O19 C2 C11 115.3(2) . . ?
C4 C2 C11 119.8(2) . . ?
C8 C3 C4 120.4(2) . . ?
C8 C3 N17 122.6(2) . . ?
C4 C3 N17 116.6(2) . . ?
C2 C4 C3 119.5(2) . . ?
C2 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
O2 C6 C14 108.4(2) . . ?
O2 C6 H6A 110.0 . . ?
C14 C6 H6A 110.0 . . ?
O2 C6 H6B 110.0 . . ?
C14 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O3 C7 C10 107.2(2) . . ?
O3 C7 H7A 110.3 . . ?
C10 C7 H7A 110.3 . . ?
O3 C7 H7B 110.3 . . ?
C10 C7 H7B 110.3 . . ?
H7A C7 H7B 108.5 . . ?
C3 C8 C9 120.7(2) . . ?
C3 C8 N2 121.5(2) . . ?
C9 C8 N2 117.5(2) . . ?
C11 C9 C8 119.7(3) . . ?
C11 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
O4 C10 C7 108.9(2) . . ?
O4 C10 H10A 109.9 . . ?
C7 C10 H10A 109.9 . . ?
O4 C10 H10B 109.9 . . ?
C7 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
O3 C11 C9 125.6(2) . . ?
O3 C11 C2 114.5(2) . . ?
C9 C11 C2 119.8(2) . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 C12 H12A 109.47(7) . 7_565 ?
H12A C12 H12A 140.4 . 7_565 ?
H12B C12 H12A 63.1 . 7_565 ?
H12C C12 H12A 49.4 . 7_565 ?
C13 C12 H12B 109.5(4) . 7_565 ?
H12A C12 H12B 63.1 . 7_565 ?
H12B C12 H12B 49.4 . 7_565 ?
H12C C12 H12B 140.4 . 7_565 ?
H12A C12 H12B 109.5 7_565 7_565 ?
C13 C12 H12C 109.5(5) . 7_565 ?
H12A C12 H12C 49.4 . 7_565 ?
H12B C12 H12C 140.4 . 7_565 ?
H12C C12 H12C 63.1 . 7_565 ?
H12A C12 H12C 109.5 7_565 7_565 ?
H12B C12 H12C 109.5 7_565 7_565 ?
N1 C13 C12 179.2(5) . . ?
O19 C14 C6 108.0(2) . . ?
O19 C14 H14A 110.1 . . ?
C6 C14 H14A 110.1 . . ?
O19 C14 H14B 110.1 . . ?
C6 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?

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
C14 O19 C2 C4 6.1(3) . . . . ?
C14 O19 C2 C11 -175.0(2) . . . . ?
O16 N17 C3 C8 -34.6(4) . . . . ?
O5 N17 C3 C8 147.7(2) . . . . ?
O16 N17 C3 C4 137.7(2) . . . . ?
O5 N17 C3 C4 -40.0(3) . . . . ?
O19 C2 C4 C3 -179.3(2) . . . . ?
C11 C2 C4 C3 1.9(4) . . . . ?
C8 C3 C4 C2 1.7(4) . . . . ?
N17 C3 C4 C2 -170.8(2) . . . . ?
C6 O2 C6 C14 177.42(15) 7_565 . . . ?
C11 O3 C7 C10 175.6(2) . . . . ?
C4 C3 C8 C9 -3.4(4) . . . . ?
N17 C3 C8 C9 168.6(2) . . . . ?
C4 C3 C8 N2 169.7(2) . . . . ?
N17 C3 C8 N2 -18.3(4) . . . . ?
O7 N2 C8 C3 150.9(2) . . . . ?
O15 N2 C8 C3 -32.2(3) . . . . ?
O7 N2 C8 C9 -35.8(3) . . . . ?
O15 N2 C8 C9 141.1(2) . . . . ?
C3 C8 C9 C11 1.5(4) . . . . ?
N2 C8 C9 C11 -171.9(2) . . . . ?
C10 O4 C10 C7 -177.01(15) 7_565 . . . ?
O3 C7 C10 O4 75.1(3) . . . . ?
C7 O3 C11 C9 0.1(4) . . . . ?
C7 O3 C11 C2 177.6(2) . . . . ?
C8 C9 C11 O3 179.6(2) . . . . ?
C8 C9 C11 C2 2.1(4) . . . . ?
O19 C2 C11 O3 -0.5(3) . . . . ?
C4 C2 C11 O3 178.5(2) . . . . ?
O19 C2 C11 C9 177.3(2) . . . . ?
C4 C2 C11 C9 -3.8(4) . . . . ?
C2 O19 C14 C6 -176.2(2) . . . . ?
O2 C6 C14 O19 -74.2(3) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_210218
_database_code_depnum_ccdc_archive 'CCDC 2168841'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Akutagawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C20 H20 Cs I N4 O14'
_chemical_formula_moiety         'C20 H20 Cs I N4 O14'
_chemical_formula_weight         800.21
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   9.1532
_cell_length_b                   17.8073
_cell_length_c                   16.9471
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.2000
_cell_angle_gamma                90.0000
_cell_volume                     2665.6320
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21833
_cell_measurement_theta_min      3.67
_cell_measurement_theta_max      68.27
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552.00
_exptl_absorpt_coefficient_mu    20.621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.034
_exptl_absorpt_correction_T_max  0.127

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            28791
_diffrn_reflns_av_unetI/netI     0.1141
_diffrn_reflns_av_R_equivalents  0.1501
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.670
_diffrn_reflns_theta_full        68.250
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             4823
_reflns_number_gt                3968
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1591
_refine_ls_wR_factor_gt          0.1459
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4823
_refine_ls_number_parameters     361
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.65
_refine_diff_density_min         -1.78
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cs Cs -0.7457 7.9052
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.3257 6.8362
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.55766(5) 0.03517(2) 0.27815(3) 0.02337(17) Uani 1 1 d . . .
I1 I 0.79590(5) 0.18834(3) 0.41479(3) 0.02705(18) Uani 1 1 d . . .
O1 O 0.3640(5) 0.1449(3) 0.1349(3) 0.0219(11) Uani 1 1 d . . .
O2 O 0.4038(5) -0.0065(3) 0.0871(3) 0.0250(11) Uani 1 1 d . . .
O3 O 0.4192(5) -0.1214(3) 0.2070(3) 0.0230(11) Uani 1 1 d . . .
O4 O 0.3592(6) -0.0946(3) 0.3430(3) 0.0228(11) Uani 1 1 d . . .
O5 O 0.3352(5) 0.0568(3) 0.3956(3) 0.0232(11) Uani 1 1 d . . .
O6 O 0.3401(5) 0.1760(3) 0.2802(3) 0.0234(11) Uani 1 1 d . . .
O7 O 0.6170(6) 0.4445(3) 0.1252(3) 0.0346(13) Uani 1 1 d . . .
O8 O 0.7249(6) 0.3472(3) 0.0868(3) 0.0318(13) Uani 1 1 d . . .
O9 O 0.5474(7) 0.4417(3) 0.3323(4) 0.0417(15) Uani 1 1 d . . .
O10 O 0.7456(6) 0.4237(3) 0.2884(3) 0.0363(14) Uani 1 1 d . . .
O11 O 0.5807(6) -0.4079(3) 0.2435(3) 0.0326(13) Uani 1 1 d . . .
O12 O 0.7615(5) -0.3739(3) 0.3490(3) 0.0319(13) Uani 1 1 d . . .
O13 O 0.5228(6) -0.4107(3) 0.4224(3) 0.0291(12) Uani 1 1 d . . .
O14 O 0.5105(6) -0.3269(3) 0.5128(3) 0.0345(14) Uani 1 1 d . . .
N1 N 0.6406(6) 0.3764(4) 0.1230(4) 0.0254(14) Uani 1 1 d . . .
N2 N 0.6172(7) 0.4088(4) 0.2910(4) 0.0291(15) Uani 1 1 d . . .
N3 N 0.6345(7) -0.3661(3) 0.3015(4) 0.0261(15) Uani 1 1 d . . .
N4 N 0.5146(6) -0.3451(4) 0.4436(4) 0.0232(14) Uani 1 1 d . . .
C1 C 0.3820(8) 0.1239(4) 0.0553(5) 0.0271(17) Uani 1 1 d . . .
H1A H 0.4887 0.1218 0.0569 0.033 Uiso 1 1 calc R . .
H1B H 0.3335 0.1608 0.0147 0.033 Uiso 1 1 calc R . .
C2 C 0.3104(8) 0.0480(4) 0.0331(5) 0.0249(17) Uani 1 1 d . . .
H2A H 0.2085 0.0476 0.0400 0.030 Uiso 1 1 calc R . .
H2B H 0.3052 0.0362 -0.0234 0.030 Uiso 1 1 calc R . .
C3 C 0.3333(9) -0.0793(4) 0.0704(5) 0.0262(17) Uani 1 1 d . . .
H3A H 0.3204 -0.0922 0.0134 0.031 Uiso 1 1 calc R . .
H3B H 0.2342 -0.0783 0.0810 0.031 Uiso 1 1 calc R . .
C4 C 0.4289(8) -0.1362(4) 0.1230(5) 0.0247(17) Uani 1 1 d . . .
H4A H 0.3925 -0.1863 0.1059 0.030 Uiso 1 1 calc R . .
H4B H 0.5329 -0.1320 0.1198 0.030 Uiso 1 1 calc R . .
C5 C 0.4551(8) -0.1773(4) 0.2622(5) 0.0223(16) Uani 1 1 d . . .
C6 C 0.5244(8) -0.2456(4) 0.2514(5) 0.0215(16) Uani 1 1 d . . .
H6 H 0.5534 -0.2549 0.2036 0.026 Uiso 1 1 calc R . .
C7 C 0.5486(8) -0.2984(4) 0.3130(5) 0.0205(15) Uani 1 1 d . . .
C8 C 0.5041(8) -0.2861(4) 0.3839(5) 0.0225(16) Uani 1 1 d . . .
C9 C 0.4395(8) -0.2188(4) 0.3971(5) 0.0254(17) Uani 1 1 d . . .
H9 H 0.4111 -0.2104 0.4452 0.030 Uiso 1 1 calc R . .
C10 C 0.4175(8) -0.1633(4) 0.3366(5) 0.0254(17) Uani 1 1 d . . .
C11 C 0.3265(9) -0.0758(4) 0.4194(5) 0.0271(18) Uani 1 1 d . . .
H11A H 0.4199 -0.0705 0.4622 0.032 Uiso 1 1 calc R . .
H11B H 0.2665 -0.1152 0.4350 0.032 Uiso 1 1 calc R . .
C12 C 0.2397(9) -0.0025(4) 0.4074(5) 0.0270(18) Uani 1 1 d . . .
H12A H 0.1531 -0.0063 0.3602 0.032 Uiso 1 1 calc R . .
H12B H 0.2030 0.0079 0.4550 0.032 Uiso 1 1 calc R . .
C13 C 0.2564(8) 0.1266(4) 0.3912(5) 0.0230(16) Uani 1 1 d . . .
H13A H 0.2416 0.1386 0.4444 0.028 Uiso 1 1 calc R . .
H13B H 0.1576 0.1223 0.3527 0.028 Uiso 1 1 calc R . .
C14 C 0.3434(8) 0.1874(4) 0.3650(4) 0.0232(17) Uani 1 1 d . . .
H14A H 0.2993 0.2357 0.3717 0.028 Uiso 1 1 calc R . .
H14B H 0.4472 0.1869 0.3984 0.028 Uiso 1 1 calc R . .
C15 C 0.4085(8) 0.2287(4) 0.2450(5) 0.0241(17) Uani 1 1 d . . .
C16 C 0.4655(8) 0.2955(4) 0.2823(5) 0.0219(16) Uani 1 1 d . . .
H16 H 0.4519 0.3076 0.3332 0.026 Uiso 1 1 calc R . .
C17 C 0.5423(8) 0.3439(4) 0.2442(5) 0.0218(16) Uani 1 1 d . . .
C18 C 0.5614(7) 0.3258(4) 0.1672(4) 0.0189(15) Uani 1 1 d . . .
C19 C 0.5028(8) 0.2603(4) 0.1285(5) 0.0237(17) Uani 1 1 d . . .
H19 H 0.5158 0.2488 0.0772 0.028 Uiso 1 1 calc R . .
C20 C 0.4238(8) 0.2114(4) 0.1664(5) 0.0237(16) Uani 1 1 d . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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
Cs1 O10 3.086(5) 2_645 ?
Cs1 O3 3.167(5) . ?
Cs1 O6 3.208(5) . ?
Cs1 O5 3.222(5) . ?
Cs1 O1 3.255(5) . ?
Cs1 O2 3.260(5) . ?
Cs1 O4 3.301(5) . ?
Cs1 O7 3.406(6) 2_645 ?
Cs1 O12 3.447(5) 2_655 ?
Cs1 O11 3.571(5) 2_655 ?
Cs1 C15 3.696(7) . ?
Cs1 C20 3.704(7) . ?
O1 C20 1.354(8) . ?
O1 C1 1.451(8) . ?
O2 C3 1.443(8) . ?
O2 C2 1.449(8) . ?
O3 C5 1.346(8) . ?
O3 C4 1.474(8) . ?
O4 C10 1.351(8) . ?
O4 C11 1.441(8) . ?
O5 C12 1.417(8) . ?
O5 C13 1.430(8) . ?
O6 C15 1.351(8) . ?
O6 C14 1.444(8) . ?
O7 N1 1.234(7) . ?
O7 Cs1 3.406(6) 2_655 ?
O8 N1 1.221(7) . ?
O9 N2 1.215(8) . ?
O10 N2 1.217(8) . ?
O10 Cs1 3.086(5) 2_655 ?
O11 N3 1.228(8) . ?
O11 Cs1 3.571(5) 2_645 ?
O12 N3 1.236(8) . ?
O12 Cs1 3.447(5) 2_645 ?
O13 N4 1.230(7) . ?
O14 N4 1.227(7) . ?
N1 C18 1.478(8) . ?
N2 C17 1.466(9) . ?
N3 C7 1.480(9) . ?
N4 C8 1.443(9) . ?
C1 C2 1.506(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.475(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.406(9) . ?
C5 C10 1.413(10) . ?
C6 C7 1.379(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.385(10) . ?
C8 C9 1.381(10) . ?
C9 C10 1.400(10) . ?
C9 H9 0.9300 . ?
C11 C12 1.515(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.479(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.382(10) . ?
C15 C20 1.409(10) . ?
C16 C17 1.376(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.400(10) . ?
C18 C19 1.376(10) . ?
C19 C20 1.392(10) . ?
C19 H19 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Cs1 O3 60.54(13) 2_645 . ?
O10 Cs1 O6 158.48(14) 2_645 . ?
O3 Cs1 O6 120.31(12) . . ?
O10 Cs1 O5 145.74(14) 2_645 . ?
O3 Cs1 O5 94.91(12) . . ?
O6 Cs1 O5 53.51(12) . . ?
O10 Cs1 O1 111.69(13) 2_645 . ?
O3 Cs1 O1 99.17(12) . . ?
O6 Cs1 O1 47.21(12) . . ?
O5 Cs1 O1 94.61(12) . . ?
O10 Cs1 O2 68.41(13) 2_645 . ?
O3 Cs1 O2 52.84(12) . . ?
O6 Cs1 O2 94.65(12) . . ?
O5 Cs1 O2 117.54(12) . . ?
O1 Cs1 O2 52.20(12) . . ?
O10 Cs1 O4 95.52(14) 2_645 . ?
O3 Cs1 O4 46.39(12) . . ?
O6 Cs1 O4 98.41(12) . . ?
O5 Cs1 O4 52.10(12) . . ?
O1 Cs1 O4 115.41(12) . . ?
O2 Cs1 O4 92.25(12) . . ?
O10 Cs1 O7 49.48(13) 2_645 2_645 ?
O3 Cs1 O7 88.74(13) . 2_645 ?
O6 Cs1 O7 146.33(13) . 2_645 ?
O5 Cs1 O7 111.97(12) . 2_645 ?
O1 Cs1 O7 151.60(12) . 2_645 ?
O2 Cs1 O7 117.73(12) . 2_645 ?
O4 Cs1 O7 89.78(12) . 2_645 ?
O10 Cs1 O12 69.63(14) 2_645 2_655 ?
O3 Cs1 O12 112.68(12) . 2_655 ?
O6 Cs1 O12 92.32(12) . 2_655 ?
O5 Cs1 O12 144.59(12) . 2_655 ?
O1 Cs1 O12 60.55(12) . 2_655 ?
O2 Cs1 O12 68.85(12) . 2_655 ?
O4 Cs1 O12 159.03(12) . 2_655 ?
O7 Cs1 O12 91.19(12) 2_645 2_655 ?
O10 Cs1 O11 59.99(14) 2_645 2_655 ?
O3 Cs1 O11 120.00(12) . 2_655 ?
O6 Cs1 O11 111.94(12) . 2_655 ?
O5 Cs1 O11 141.48(12) . 2_655 ?
O1 Cs1 O11 95.22(12) . 2_655 ?
O2 Cs1 O11 97.66(12) . 2_655 ?
O4 Cs1 O11 147.01(12) . 2_655 ?
O7 Cs1 O11 57.79(12) 2_645 2_655 ?
O12 Cs1 O11 36.13(12) 2_655 2_655 ?
O10 Cs1 C15 140.56(16) 2_645 . ?
O3 Cs1 C15 131.93(15) . . ?
O6 Cs1 C15 21.09(13) . . ?
O5 Cs1 C15 73.41(14) . . ?
O1 Cs1 C15 38.70(14) . . ?
O2 Cs1 C15 90.87(15) . . ?
O4 Cs1 C15 119.34(14) . . ?
O7 Cs1 C15 139.17(15) 2_645 . ?
O12 Cs1 C15 71.66(14) 2_655 . ?
O11 Cs1 C15 91.99(14) 2_655 . ?
O10 Cs1 C20 120.32(15) 2_645 . ?
O3 Cs1 C20 120.37(15) . . ?
O6 Cs1 C20 38.75(14) . . ?
O5 Cs1 C20 92.10(14) . . ?
O1 Cs1 C20 21.20(14) . . ?
O2 Cs1 C20 71.72(15) . . ?
O4 Cs1 C20 128.77(14) . . ?
O7 Cs1 C20 141.06(14) 2_645 . ?
O12 Cs1 C20 55.30(13) 2_655 . ?
O11 Cs1 C20 84.15(14) 2_655 . ?
C15 Cs1 C20 21.96(16) . . ?
C20 O1 C1 117.4(5) . . ?
C20 O1 Cs1 98.4(4) . . ?
C1 O1 Cs1 111.5(4) . . ?
C3 O2 C2 108.6(5) . . ?
C3 O2 Cs1 117.0(4) . . ?
C2 O2 Cs1 120.3(4) . . ?
C5 O3 C4 118.3(5) . . ?
C5 O3 Cs1 112.7(4) . . ?
C4 O3 Cs1 113.9(4) . . ?
C10 O4 C11 117.5(6) . . ?
C10 O4 Cs1 110.1(4) . . ?
C11 O4 Cs1 113.5(4) . . ?
C12 O5 C13 109.5(5) . . ?
C12 O5 Cs1 120.7(4) . . ?
C13 O5 Cs1 117.6(4) . . ?
C15 O6 C14 116.8(6) . . ?
C15 O6 Cs1 100.2(4) . . ?
C14 O6 Cs1 105.6(4) . . ?
N1 O7 Cs1 110.0(4) . 2_655 ?
N2 O10 Cs1 144.6(5) . 2_655 ?
N3 O11 Cs1 93.8(4) . 2_645 ?
N3 O12 Cs1 99.7(4) . 2_645 ?
O8 N1 O7 125.0(6) . . ?
O8 N1 C18 116.9(6) . . ?
O7 N1 C18 118.2(6) . . ?
O10 N2 O9 125.1(7) . . ?
O10 N2 C17 118.1(6) . . ?
O9 N2 C17 116.8(6) . . ?
O12 N3 O11 124.4(6) . . ?
O12 N3 C7 116.5(6) . . ?
O11 N3 C7 118.9(6) . . ?
O14 N4 O13 123.3(6) . . ?
O14 N4 C8 117.7(6) . . ?
O13 N4 C8 118.9(6) . . ?
O1 C1 C2 108.4(6) . . ?
O1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
O1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
O2 C2 C1 107.3(6) . . ?
O2 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
O2 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O2 C3 C4 109.6(6) . . ?
O2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
O2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 C3 106.5(6) . . ?
O3 C4 H4A 110.4 . . ?
C3 C4 H4A 110.4 . . ?
O3 C4 H4B 110.4 . . ?
C3 C4 H4B 110.4 . . ?
H4A C4 H4B 108.6 . . ?
O3 C5 C6 125.8(6) . . ?
O3 C5 C10 114.7(6) . . ?
C6 C5 C10 119.5(7) . . ?
O3 C5 Cs1 48.7(3) . . ?
C6 C5 Cs1 137.9(5) . . ?
C10 C5 Cs1 83.0(4) . . ?
C7 C6 C5 118.6(6) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
C8 C7 C6 121.6(7) . . ?
C8 C7 N3 122.0(7) . . ?
C6 C7 N3 116.2(6) . . ?
C7 C8 C9 120.9(7) . . ?
C7 C8 N4 120.8(6) . . ?
C9 C8 N4 118.1(6) . . ?
C10 C9 C8 118.6(7) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
O4 C10 C9 124.3(7) . . ?
O4 C10 C5 115.2(7) . . ?
C9 C10 C5 120.6(7) . . ?
O4 C11 C12 107.7(6) . . ?
O4 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
O4 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
O5 C12 C11 109.9(6) . . ?
O5 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
O5 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
O5 C13 C14 110.4(6) . . ?
O5 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
O5 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
O6 C14 C13 108.9(6) . . ?
O6 C14 Cs1 53.2(3) . . ?
C13 C14 Cs1 88.2(4) . . ?
O6 C14 H14A 109.9 . . ?
C13 C14 H14A 109.9 . . ?
Cs1 C14 H14A 159.6 . . ?
O6 C14 H14B 109.9 . . ?
C13 C14 H14B 109.9 . . ?
Cs1 C14 H14B 72.4 . . ?
H14A C14 H14B 108.3 . . ?
O6 C15 C16 124.0(7) . . ?
O6 C15 C20 115.9(7) . . ?
C16 C15 C20 120.1(7) . . ?
O6 C15 Cs1 58.7(3) . . ?
C16 C15 Cs1 130.7(5) . . ?
C20 C15 Cs1 79.4(4) . . ?
C17 C16 C15 120.2(7) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 119.7(7) . . ?
C16 C17 N2 117.7(7) . . ?
C18 C17 N2 122.1(6) . . ?
C19 C18 C17 120.8(6) . . ?
C19 C18 N1 117.2(6) . . ?
C17 C18 N1 122.0(6) . . ?
C20 C19 C18 119.6(7) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
O1 C20 C19 124.7(7) . . ?
O1 C20 C15 115.7(6) . . ?
C19 C20 C15 119.5(7) . . ?
O1 C20 Cs1 60.4(3) . . ?
C19 C20 Cs1 128.6(4) . . ?
C15 C20 Cs1 78.7(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
O10 Cs1 O1 C20 -118.5(4) 2_645 . . . ?
O3 Cs1 O1 C20 179.7(4) . . . . ?
O6 Cs1 O1 C20 56.5(4) . . . . ?
O5 Cs1 O1 C20 83.9(4) . . . . ?
O2 Cs1 O1 C20 -154.4(4) . . . . ?
O4 Cs1 O1 C20 133.8(4) . . . . ?
O7 Cs1 O1 C20 -75.8(4) 2_645 . . . ?
O12 Cs1 O1 C20 -69.4(4) 2_655 . . . ?
O11 Cs1 O1 C20 -58.8(4) 2_655 . . . ?
C15 Cs1 O1 C20 27.9(4) . . . . ?
O10 Cs1 O1 C1 5.4(4) 2_645 . . . ?
O3 Cs1 O1 C1 -56.4(4) . . . . ?
O6 Cs1 O1 C1 -179.6(4) . . . . ?
O5 Cs1 O1 C1 -152.2(4) . . . . ?
O2 Cs1 O1 C1 -30.5(4) . . . . ?
O4 Cs1 O1 C1 -102.3(4) . . . . ?
O7 Cs1 O1 C1 48.1(5) 2_645 . . . ?
O12 Cs1 O1 C1 54.5(4) 2_655 . . . ?
O11 Cs1 O1 C1 65.1(4) 2_655 . . . ?
C15 Cs1 O1 C1 151.8(5) . . . . ?
C20 Cs1 O1 C1 123.9(6) . . . . ?
O10 Cs1 O2 C3 75.4(5) 2_645 . . . ?
O3 Cs1 O2 C3 6.7(4) . . . . ?
O6 Cs1 O2 C3 -118.3(4) . . . . ?
O5 Cs1 O2 C3 -67.4(5) . . . . ?
O1 Cs1 O2 C3 -140.5(5) . . . . ?
O4 Cs1 O2 C3 -19.6(4) . . . . ?
O7 Cs1 O2 C3 71.3(5) 2_645 . . . ?
O12 Cs1 O2 C3 151.0(5) 2_655 . . . ?
O11 Cs1 O2 C3 128.8(4) 2_655 . . . ?
C15 Cs1 O2 C3 -139.1(4) . . . . ?
C20 Cs1 O2 C3 -150.0(5) . . . . ?
O10 Cs1 O2 C2 -149.3(5) 2_645 . . . ?
O3 Cs1 O2 C2 142.1(5) . . . . ?
O6 Cs1 O2 C2 17.1(4) . . . . ?
O5 Cs1 O2 C2 68.0(5) . . . . ?
O1 Cs1 O2 C2 -5.2(4) . . . . ?
O4 Cs1 O2 C2 115.7(4) . . . . ?
O7 Cs1 O2 C2 -153.4(4) 2_645 . . . ?
O12 Cs1 O2 C2 -73.6(4) 2_655 . . . ?
O11 Cs1 O2 C2 -95.8(4) 2_655 . . . ?
C15 Cs1 O2 C2 -3.7(4) . . . . ?
C20 Cs1 O2 C2 -14.6(4) . . . . ?
O10 Cs1 O3 C5 83.4(4) 2_645 . . . ?
O6 Cs1 O3 C5 -121.4(4) . . . . ?
O5 Cs1 O3 C5 -71.3(4) . . . . ?
O1 Cs1 O3 C5 -166.8(4) . . . . ?
O2 Cs1 O3 C5 167.6(5) . . . . ?
O4 Cs1 O3 C5 -50.2(4) . . . . ?
O7 Cs1 O3 C5 40.7(4) 2_645 . . . ?
O12 Cs1 O3 C5 131.4(4) 2_655 . . . ?
O11 Cs1 O3 C5 91.7(4) 2_655 . . . ?
C15 Cs1 O3 C5 -143.3(4) . . . . ?
C20 Cs1 O3 C5 -166.6(4) . . . . ?
O10 Cs1 O3 C4 -54.9(4) 2_645 . . . ?
O6 Cs1 O3 C4 100.2(4) . . . . ?
O5 Cs1 O3 C4 150.4(4) . . . . ?
O1 Cs1 O3 C4 54.9(4) . . . . ?
O2 Cs1 O3 C4 29.2(4) . . . . ?
O4 Cs1 O3 C4 171.4(5) . . . . ?
O7 Cs1 O3 C4 -97.7(4) 2_645 . . . ?
O12 Cs1 O3 C4 -6.9(4) 2_655 . . . ?
O11 Cs1 O3 C4 -46.6(4) 2_655 . . . ?
C15 Cs1 O3 C4 78.3(4) . . . . ?
C20 Cs1 O3 C4 55.0(4) . . . . ?
O10 Cs1 O4 C10 7.7(4) 2_645 . . . ?
O3 Cs1 O4 C10 46.9(4) . . . . ?
O6 Cs1 O4 C10 171.3(4) . . . . ?
O5 Cs1 O4 C10 -160.0(5) . . . . ?
O1 Cs1 O4 C10 124.9(4) . . . . ?
O2 Cs1 O4 C10 76.2(4) . . . . ?
O7 Cs1 O4 C10 -41.5(4) 2_645 . . . ?
O12 Cs1 O4 C10 51.2(6) 2_655 . . . ?
O11 Cs1 O4 C10 -31.6(5) 2_655 . . . ?
C15 Cs1 O4 C10 168.5(4) . . . . ?
C20 Cs1 O4 C10 144.4(4) . . . . ?
O10 Cs1 O4 C11 141.8(5) 2_645 . . . ?
O3 Cs1 O4 C11 -179.0(5) . . . . ?
O6 Cs1 O4 C11 -54.7(5) . . . . ?
O5 Cs1 O4 C11 -25.9(4) . . . . ?
O1 Cs1 O4 C11 -101.1(4) . . . . ?
O2 Cs1 O4 C11 -149.7(4) . . . . ?
O7 Cs1 O4 C11 92.5(5) 2_645 . . . ?
O12 Cs1 O4 C11 -174.7(4) 2_655 . . . ?
O11 Cs1 O4 C11 102.5(5) 2_655 . . . ?
C15 Cs1 O4 C11 -57.4(5) . . . . ?
C20 Cs1 O4 C11 -81.5(5) . . . . ?
O10 Cs1 O5 C12 -32.2(6) 2_645 . . . ?
O3 Cs1 O5 C12 9.1(5) . . . . ?
O6 Cs1 O5 C12 133.7(5) . . . . ?
O1 Cs1 O5 C12 108.8(5) . . . . ?
O2 Cs1 O5 C12 59.4(5) . . . . ?
O4 Cs1 O5 C12 -10.1(5) . . . . ?
O7 Cs1 O5 C12 -81.5(5) 2_645 . . . ?
O12 Cs1 O5 C12 151.2(5) 2_655 . . . ?
O11 Cs1 O5 C12 -146.9(5) 2_655 . . . ?
C15 Cs1 O5 C12 141.5(5) . . . . ?
C20 Cs1 O5 C12 129.9(5) . . . . ?
O10 Cs1 O5 C13 -170.7(4) 2_645 . . . ?
O3 Cs1 O5 C13 -129.4(5) . . . . ?
O6 Cs1 O5 C13 -4.9(4) . . . . ?
O1 Cs1 O5 C13 -29.8(5) . . . . ?
O2 Cs1 O5 C13 -79.1(5) . . . . ?
O4 Cs1 O5 C13 -148.6(5) . . . . ?
O7 Cs1 O5 C13 140.0(5) 2_645 . . . ?
O12 Cs1 O5 C13 12.7(6) 2_655 . . . ?
O11 Cs1 O5 C13 74.6(5) 2_655 . . . ?
C15 Cs1 O5 C13 3.0(5) . . . . ?
C20 Cs1 O5 C13 -8.7(5) . . . . ?
O10 Cs1 O6 C15 -43.5(6) 2_645 . . . ?
O3 Cs1 O6 C15 -129.4(4) . . . . ?
O5 Cs1 O6 C15 158.6(5) . . . . ?
O1 Cs1 O6 C15 -56.3(4) . . . . ?
O2 Cs1 O6 C15 -80.3(4) . . . . ?
O4 Cs1 O6 C15 -173.3(4) . . . . ?
O7 Cs1 O6 C15 84.3(5) 2_645 . . . ?
O12 Cs1 O6 C15 -11.4(4) 2_655 . . . ?
O11 Cs1 O6 C15 19.9(4) 2_655 . . . ?
C20 Cs1 O6 C15 -27.5(4) . . . . ?
O10 Cs1 O6 C14 -165.2(4) 2_645 . . . ?
O3 Cs1 O6 C14 108.8(4) . . . . ?
O5 Cs1 O6 C14 36.8(4) . . . . ?
O1 Cs1 O6 C14 -178.0(4) . . . . ?
O2 Cs1 O6 C14 157.9(4) . . . . ?
O4 Cs1 O6 C14 65.0(4) . . . . ?
O7 Cs1 O6 C14 -37.4(5) 2_645 . . . ?
O12 Cs1 O6 C14 -133.1(4) 2_655 . . . ?
O11 Cs1 O6 C14 -101.9(4) 2_655 . . . ?
C15 Cs1 O6 C14 -121.7(6) . . . . ?
C20 Cs1 O6 C14 -149.2(5) . . . . ?
Cs1 O7 N1 O8 -63.8(8) 2_655 . . . ?
Cs1 O7 N1 C18 116.3(5) 2_655 . . . ?
Cs1 O10 N2 O9 -74.9(11) 2_655 . . . ?
Cs1 O10 N2 C17 108.3(8) 2_655 . . . ?
Cs1 O12 N3 O11 27.3(7) 2_645 . . . ?
Cs1 O12 N3 C7 -148.1(5) 2_645 . . . ?
Cs1 O11 N3 O12 -25.9(7) 2_645 . . . ?
Cs1 O11 N3 C7 149.4(5) 2_645 . . . ?
C20 O1 C1 C2 178.9(6) . . . . ?
Cs1 O1 C1 C2 66.5(6) . . . . ?
C3 O2 C2 C1 176.8(6) . . . . ?
Cs1 O2 C2 C1 38.1(7) . . . . ?
O1 C1 C2 O2 -69.6(7) . . . . ?
C2 O2 C3 C4 178.3(6) . . . . ?
Cs1 O2 C3 C4 -41.5(7) . . . . ?
C5 O3 C4 C3 159.4(6) . . . . ?
Cs1 O3 C4 C3 -64.7(6) . . . . ?
O2 C3 C4 O3 70.1(7) . . . . ?
C4 O3 C5 C6 10.7(10) . . . . ?
Cs1 O3 C5 C6 -125.7(6) . . . . ?
C4 O3 C5 C10 -169.2(6) . . . . ?
Cs1 O3 C5 C10 54.4(7) . . . . ?
C4 O3 C5 Cs1 136.4(6) . . . . ?
O10 Cs1 C5 O3 -85.9(4) 2_645 . . . ?
O6 Cs1 C5 O3 70.2(5) . . . . ?
O5 Cs1 C5 O3 109.3(4) . . . . ?
O1 Cs1 C5 O3 14.7(5) . . . . ?
O2 Cs1 C5 O3 -10.4(4) . . . . ?
O4 Cs1 C5 O3 111.5(5) . . . . ?
O7 Cs1 C5 O3 -137.5(4) 2_645 . . . ?
O12 Cs1 C5 O3 -56.6(5) 2_655 . . . ?
O11 Cs1 C5 O3 -98.9(4) 2_655 . . . ?
C15 Cs1 C5 O3 51.6(5) . . . . ?
C20 Cs1 C5 O3 17.5(5) . . . . ?
O10 Cs1 C5 C6 15.1(7) 2_645 . . . ?
O3 Cs1 C5 C6 101.0(9) . . . . ?
O6 Cs1 C5 C6 171.2(7) . . . . ?
O5 Cs1 C5 C6 -149.7(8) . . . . ?
O1 Cs1 C5 C6 115.7(7) . . . . ?
O2 Cs1 C5 C6 90.5(8) . . . . ?
O4 Cs1 C5 C6 -147.6(9) . . . . ?
O7 Cs1 C5 C6 -36.6(7) 2_645 . . . ?
O12 Cs1 C5 C6 44.3(8) 2_655 . . . ?
O11 Cs1 C5 C6 2.1(8) 2_655 . . . ?
C15 Cs1 C5 C6 152.5(7) . . . . ?
C20 Cs1 C5 C6 118.4(7) . . . . ?
O10 Cs1 C5 C10 142.2(5) 2_645 . . . ?
O3 Cs1 C5 C10 -131.9(7) . . . . ?
O6 Cs1 C5 C10 -61.7(5) . . . . ?
O5 Cs1 C5 C10 -22.6(4) . . . . ?
O1 Cs1 C5 C10 -117.2(4) . . . . ?
O2 Cs1 C5 C10 -142.4(5) . . . . ?
O4 Cs1 C5 C10 -20.5(4) . . . . ?
O7 Cs1 C5 C10 90.5(4) 2_645 . . . ?
O12 Cs1 C5 C10 171.4(4) 2_655 . . . ?
O11 Cs1 C5 C10 129.2(4) 2_655 . . . ?
C15 Cs1 C5 C10 -80.3(5) . . . . ?
C20 Cs1 C5 C10 -114.4(4) . . . . ?
O3 C5 C6 C7 -177.6(6) . . . . ?
C10 C5 C6 C7 2.4(10) . . . . ?
Cs1 C5 C6 C7 117.0(7) . . . . ?
C5 C6 C7 C8 1.1(11) . . . . ?
C5 C6 C7 N3 -174.5(6) . . . . ?
O12 N3 C7 C8 -62.9(9) . . . . ?
O11 N3 C7 C8 121.4(8) . . . . ?
O12 N3 C7 C6 112.7(7) . . . . ?
O11 N3 C7 C6 -63.0(8) . . . . ?
C6 C7 C8 C9 -2.8(11) . . . . ?
N3 C7 C8 C9 172.5(7) . . . . ?
C6 C7 C8 N4 172.9(6) . . . . ?
N3 C7 C8 N4 -11.7(10) . . . . ?
O14 N4 C8 C7 162.2(6) . . . . ?
O13 N4 C8 C7 -19.9(10) . . . . ?
O14 N4 C8 C9 -21.9(9) . . . . ?
O13 N4 C8 C9 156.0(6) . . . . ?
C7 C8 C9 C10 1.0(11) . . . . ?
N4 C8 C9 C10 -174.9(6) . . . . ?
C11 O4 C10 C9 4.0(10) . . . . ?
Cs1 O4 C10 C9 136.0(6) . . . . ?
C11 O4 C10 C5 -176.7(6) . . . . ?
Cs1 O4 C10 C5 -44.7(7) . . . . ?
C8 C9 C10 O4 -178.2(6) . . . . ?
C8 C9 C10 C5 2.5(11) . . . . ?
O3 C5 C10 O4 -3.6(9) . . . . ?
C6 C5 C10 O4 176.4(6) . . . . ?
Cs1 C5 C10 O4 34.4(5) . . . . ?
O3 C5 C10 C9 175.8(6) . . . . ?
C6 C5 C10 C9 -4.2(11) . . . . ?
Cs1 C5 C10 C9 -146.3(6) . . . . ?
C10 O4 C11 C12 -170.9(6) . . . . ?
Cs1 O4 C11 C12 58.6(6) . . . . ?
C13 O5 C12 C11 -175.2(6) . . . . ?
Cs1 O5 C12 C11 43.3(7) . . . . ?
O4 C11 C12 O5 -67.8(8) . . . . ?
C12 O5 C13 C14 -170.4(6) . . . . ?
Cs1 O5 C13 C14 -27.5(8) . . . . ?
C15 O6 C14 C13 177.0(6) . . . . ?
Cs1 O6 C14 C13 -72.7(5) . . . . ?
C15 O6 C14 Cs1 -110.4(6) . . . . ?
O5 C13 C14 O6 69.9(8) . . . . ?
O5 C13 C14 Cs1 20.0(6) . . . . ?
O10 Cs1 C14 O6 92.9(17) 2_645 . . . ?
O3 Cs1 C14 O6 -84.6(4) . . . . ?
O5 Cs1 C14 O6 -128.7(5) . . . . ?
O1 Cs1 C14 O6 1.6(3) . . . . ?
O2 Cs1 C14 O6 -24.2(4) . . . . ?
O4 Cs1 C14 O6 -116.3(4) . . . . ?
O7 Cs1 C14 O6 154.6(3) 2_645 . . . ?
O12 Cs1 C14 O6 49.5(4) 2_655 . . . ?
O11 Cs1 C14 O6 87.3(4) 2_655 . . . ?
C15 Cs1 C14 O6 30.8(3) . . . . ?
C20 Cs1 C14 O6 22.3(3) . . . . ?
O10 Cs1 C14 C13 -151.8(15) 2_645 . . . ?
O3 Cs1 C14 C13 30.8(5) . . . . ?
O6 Cs1 C14 C13 115.4(6) . . . . ?
O5 Cs1 C14 C13 -13.3(4) . . . . ?
O1 Cs1 C14 C13 116.9(5) . . . . ?
O2 Cs1 C14 C13 91.2(4) . . . . ?
O4 Cs1 C14 C13 -0.9(4) . . . . ?
O7 Cs1 C14 C13 -90.0(5) 2_645 . . . ?
O12 Cs1 C14 C13 164.9(4) 2_655 . . . ?
O11 Cs1 C14 C13 -157.4(4) 2_655 . . . ?
C15 Cs1 C14 C13 146.2(6) . . . . ?
C20 Cs1 C14 C13 137.6(5) . . . . ?
C14 O6 C15 C16 -7.3(10) . . . . ?
Cs1 O6 C15 C16 -120.7(6) . . . . ?
C14 O6 C15 C20 171.0(6) . . . . ?
Cs1 O6 C15 C20 57.6(6) . . . . ?
C14 O6 C15 Cs1 113.4(5) . . . . ?
O10 Cs1 C15 O6 156.6(4) 2_645 . . . ?
O3 Cs1 C15 O6 63.7(5) . . . . ?
O5 Cs1 C15 O6 -17.9(4) . . . . ?
O1 Cs1 C15 O6 102.5(5) . . . . ?
O2 Cs1 C15 O6 100.7(4) . . . . ?
O4 Cs1 C15 O6 7.6(5) . . . . ?
O7 Cs1 C15 O6 -122.5(4) 2_645 . . . ?
O12 Cs1 C15 O6 168.0(4) 2_655 . . . ?
O11 Cs1 C15 O6 -161.6(4) 2_655 . . . ?
C20 Cs1 C15 O6 129.4(7) . . . . ?
O10 Cs1 C15 C16 -93.6(7) 2_645 . . . ?
O3 Cs1 C15 C16 173.5(6) . . . . ?
O6 Cs1 C15 C16 109.8(8) . . . . ?
O5 Cs1 C15 C16 92.0(6) . . . . ?
O1 Cs1 C15 C16 -147.6(7) . . . . ?
O2 Cs1 C15 C16 -149.5(6) . . . . ?
O4 Cs1 C15 C16 117.5(6) . . . . ?
O7 Cs1 C15 C16 -12.6(7) 2_645 . . . ?
O12 Cs1 C15 C16 -82.1(6) 2_655 . . . ?
O11 Cs1 C15 C16 -51.8(6) 2_655 . . . ?
C20 Cs1 C15 C16 -120.7(8) . . . . ?
O10 Cs1 C15 C20 27.2(5) 2_645 . . . ?
O3 Cs1 C15 C20 -65.8(5) . . . . ?
O6 Cs1 C15 C20 -129.4(7) . . . . ?
O5 Cs1 C15 C20 -147.3(4) . . . . ?
O1 Cs1 C15 C20 -26.9(4) . . . . ?
O2 Cs1 C15 C20 -28.7(4) . . . . ?
O4 Cs1 C15 C20 -121.8(4) . . . . ?
O7 Cs1 C15 C20 108.1(4) 2_645 . . . ?
O12 Cs1 C15 C20 38.6(4) 2_655 . . . ?
O11 Cs1 C15 C20 69.0(4) 2_655 . . . ?
O6 C15 C16 C17 175.8(6) . . . . ?
C20 C15 C16 C17 -2.4(11) . . . . ?
Cs1 C15 C16 C17 100.1(8) . . . . ?
C15 C16 C17 C18 0.6(11) . . . . ?
C15 C16 C17 N2 -172.1(6) . . . . ?
O10 N2 C17 C16 135.0(7) . . . . ?
O9 N2 C17 C16 -42.1(9) . . . . ?
O10 N2 C17 C18 -37.6(10) . . . . ?
O9 N2 C17 C18 145.4(7) . . . . ?
C16 C17 C18 C19 0.7(11) . . . . ?
N2 C17 C18 C19 173.1(6) . . . . ?
C16 C17 C18 N1 178.9(6) . . . . ?
N2 C17 C18 N1 -8.7(10) . . . . ?
O8 N1 C18 C19 -42.0(9) . . . . ?
O7 N1 C18 C19 137.9(7) . . . . ?
O8 N1 C18 C17 139.7(7) . . . . ?
O7 N1 C18 C17 -40.4(9) . . . . ?
C17 C18 C19 C20 -0.1(10) . . . . ?
N1 C18 C19 C20 -178.4(6) . . . . ?
C1 O1 C20 C19 -1.0(10) . . . . ?
Cs1 O1 C20 C19 118.6(7) . . . . ?
C1 O1 C20 C15 -178.0(6) . . . . ?
Cs1 O1 C20 C15 -58.4(6) . . . . ?
C1 O1 C20 Cs1 -119.6(6) . . . . ?
C18 C19 C20 O1 -178.6(6) . . . . ?
C18 C19 C20 C15 -1.7(10) . . . . ?
C18 C19 C20 Cs1 -101.1(7) . . . . ?
O6 C15 C20 O1 1.8(9) . . . . ?
C16 C15 C20 O1 -179.8(6) . . . . ?
Cs1 C15 C20 O1 49.0(5) . . . . ?
O6 C15 C20 C19 -175.4(6) . . . . ?
C16 C15 C20 C19 3.0(11) . . . . ?
Cs1 C15 C20 C19 -128.2(6) . . . . ?
O6 C15 C20 Cs1 -47.2(5) . . . . ?
C16 C15 C20 Cs1 131.2(7) . . . . ?
O10 Cs1 C20 O1 71.1(4) 2_645 . . . ?
O3 Cs1 C20 O1 -0.4(4) . . . . ?
O6 Cs1 C20 O1 -102.2(4) . . . . ?
O5 Cs1 C20 O1 -97.3(4) . . . . ?
O2 Cs1 C20 O1 21.0(3) . . . . ?
O4 Cs1 C20 O1 -56.7(4) . . . . ?
O7 Cs1 C20 O1 132.8(3) 2_645 . . . ?
O12 Cs1 C20 O1 97.5(4) 2_655 . . . ?
O11 Cs1 C20 O1 121.1(4) 2_655 . . . ?
C15 Cs1 C20 O1 -128.5(6) . . . . ?
O10 Cs1 C20 C19 -41.5(7) 2_645 . . . ?
O3 Cs1 C20 C19 -113.0(6) . . . . ?
O6 Cs1 C20 C19 145.2(8) . . . . ?
O5 Cs1 C20 C19 150.0(6) . . . . ?
O1 Cs1 C20 C19 -112.6(8) . . . . ?
O2 Cs1 C20 C19 -91.6(7) . . . . ?
O4 Cs1 C20 C19 -169.3(6) . . . . ?
O7 Cs1 C20 C19 20.2(8) 2_645 . . . ?
O12 Cs1 C20 C19 -15.1(6) 2_655 . . . ?
O11 Cs1 C20 C19 8.5(6) 2_655 . . . ?
C15 Cs1 C20 C19 118.8(8) . . . . ?
O10 Cs1 C20 C15 -160.4(4) 2_645 . . . ?
O3 Cs1 C20 C15 128.2(4) . . . . ?
O6 Cs1 C20 C15 26.4(4) . . . . ?
O5 Cs1 C20 C15 31.2(4) . . . . ?
O1 Cs1 C20 C15 128.5(6) . . . . ?
O2 Cs1 C20 C15 149.6(4) . . . . ?
O4 Cs1 C20 C15 71.8(5) . . . . ?
O7 Cs1 C20 C15 -98.6(4) 2_645 . . . ?
O12 Cs1 C20 C15 -133.9(5) 2_655 . . . ?
O11 Cs1 C20 C15 -110.3(4) 2_655 . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_201028_TA
_database_code_depnum_ccdc_archive 'CCDC 2168845'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Akutagawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C60 H84 N12 O19'
_chemical_formula_moiety         'C60 H84 N12 O19'
_chemical_formula_weight         1277.39
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
_space_group_IT_number           4
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   16.8353(4)
_cell_length_b                   8.4802(2)
_cell_length_c                   23.1290(6)
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.799(8)
_cell_angle_gamma                90.0000
_cell_volume                     3086.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    24544
_cell_measurement_theta_min      4.02
_cell_measurement_theta_max      68.09
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360.00
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_T_max  0.917

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            34844
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_theta_max         68.190
_diffrn_reflns_theta_min         4.019
_diffrn_reflns_theta_full        68.190
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             9990
_reflns_number_gt                6906
_reflns_threshold_expression     F²>2.0σ(F²)

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0707
_refine_ls_wR_factor_ref         0.2282
_refine_ls_wR_factor_gt          0.2034
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         9990
_refine_ls_number_parameters     820
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1405P)²+0.3869P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3995 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.1(3)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5155(2) 0.8808(4) 0.24052(15) 0.0557(8) Uani 1 1 d . . .
O2 O 0.3484(3) 0.7369(5) 0.1849(2) 0.0791(12) Uani 1 1 d . . .
O3 O 0.2169(2) 0.8610(4) 0.21545(16) 0.0601(9) Uani 1 1 d . . .
O4 O 0.24911(19) 1.1110(4) 0.28285(16) 0.0584(9) Uani 1 1 d . . .
O5 O 0.41298(19) 1.1884(4) 0.36473(14) 0.0548(8) Uani 1 1 d . . .
O6 O 0.5484(2) 1.1111(5) 0.31958(16) 0.0640(9) Uani 1 1 d . . .
O7 O 0.3875(3) 0.6447(6) 0.0233(3) 0.1127(18) Uani 1 1 d . . .
O8 O 0.2175(4) 0.6641(14) -0.0532(3) 0.169(4) Uani 1 1 d . . .
O9 O 0.0973(3) 0.5076(6) -0.0018(2) 0.0846(13) Uani 1 1 d . . .
O10 O 0.1629(2) 0.3160(5) 0.08958(18) 0.0723(11) Uani 1 1 d . . .
O11 O 0.3371(3) 0.2293(5) 0.1362(2) 0.0808(12) Uani 1 1 d . . .
O12 O 0.4439(2) 0.3996(5) 0.09165(18) 0.0670(10) Uani 1 1 d . . .
O13 O 0.0105(2) 0.5212(5) 0.32844(16) 0.0714(11) Uani 1 1 d . . .
O14 O -0.1063(2) 0.8049(5) 0.3326(2) 0.0828(12) Uani 1 1 d . . .
O15 O -0.2374(2) 0.5830(5) 0.35260(19) 0.0795(13) Uani 1 1 d . . .
O16 O -0.1884(2) 0.3471(4) 0.42899(15) 0.0549(8) Uani 1 1 d . . .
O17 O -0.0269(2) 0.1824(4) 0.46867(15) 0.0558(8) Uani 1 1 d . . .
O18 O 0.08088(19) 0.2983(4) 0.41244(16) 0.0551(8) Uani 1 1 d . . .
O19 O 0.4269(3) 0.8611(5) 0.33251(18) 0.0782(11) Uani 1 1 d . . .
N1 N 0.7715(3) 1.3096(7) 0.2494(2) 0.0819(16) Uani 1 1 d . . .
H1A H 0.7988 1.3045 0.2243 0.098 Uiso 1 1 calc R . .
H1B H 0.7833 1.3825 0.2770 0.098 Uiso 1 1 calc R . .
N2 N 0.7353(3) 1.0619(7) 0.1643(2) 0.0749(14) Uani 1 1 d . . .
H2A H 0.7772 1.1248 0.1689 0.090 Uiso 1 1 calc R . .
H2B H 0.7236 0.9889 0.1368 0.090 Uiso 1 1 calc R . .
N3 N -0.0802(3) 0.8678(9) 0.1988(3) 0.097(2) Uani 1 1 d . . .
H3A H -0.1194 0.9054 0.2106 0.116 Uiso 1 1 calc R . .
H3B H -0.0911 0.7898 0.1734 0.116 Uiso 1 1 calc R . .
N4 N -0.0415(2) 1.1270(7) 0.2815(2) 0.0693(13) Uani 1 1 d . . .
H4A H -0.0924 1.0903 0.2678 0.083 Uiso 1 1 calc R . .
H4B H -0.0289 1.2050 0.3069 0.083 Uiso 1 1 calc R . .
N5 N 0.7345(3) 0.5726(8) 0.1389(2) 0.0940(18) Uani 1 1 d . . .
H5A H 0.7696 0.6369 0.1320 0.113 Uiso 1 1 calc R . .
H5B H 0.7531 0.4961 0.1646 0.113 Uiso 1 1 calc R . .
N6 N 0.6747(4) 0.8254(8) 0.0572(3) 0.115(2) Uani 1 1 d . . .
H6A H 0.6558 0.9045 0.0329 0.137 Uiso 1 1 calc R . .
H6B H 0.7285 0.8128 0.0757 0.137 Uiso 1 1 calc R . .
N7 N -0.1212(3) 0.6774(8) 0.0754(3) 0.0910(17) Uani 1 1 d . . .
H7A H -0.1423 0.7399 0.0445 0.109 Uiso 1 1 calc R . .
H7B H -0.1440 0.6712 0.1033 0.109 Uiso 1 1 calc R . .
N8 N -0.0503(4) 0.4732(8) 0.1776(3) 0.0916(17) Uani 1 1 d . . .
H8A H -0.0297 0.4096 0.2083 0.110 Uiso 1 1 calc R . .
H8B H -0.0941 0.5295 0.1746 0.110 Uiso 1 1 calc R . .
N9 N 0.3607(3) 0.5323(7) 0.4573(2) 0.0798(15) Uani 1 1 d . . .
H9A H 0.3915 0.6005 0.4473 0.096 Uiso 1 1 calc R . .
H9B H 0.3843 0.4637 0.4855 0.096 Uiso 1 1 calc R . .
N10 N 0.2860(4) 0.7602(8) 0.3685(2) 0.106(2) Uani 1 1 d . . .
H10A H 0.3399 0.7604 0.3887 0.128 Uiso 1 1 calc R . .
H10B H 0.2639 0.8300 0.3404 0.128 Uiso 1 1 calc R . .
N11 N -0.4401(3) 0.7501(7) 0.4487(3) 0.0920(17) Uani 1 1 d . . .
H11C H -0.4590 0.7381 0.4784 0.110 Uiso 1 1 calc R . .
H11D H -0.4591 0.8254 0.4225 0.110 Uiso 1 1 calc R . .
N12 N -0.3853(3) 0.4991(7) 0.5307(2) 0.0749(14) Uani 1 1 d . . .
H12C H -0.4264 0.5583 0.5314 0.090 Uiso 1 1 calc R . .
H12D H -0.3670 0.4247 0.5574 0.090 Uiso 1 1 calc R . .
C1 C 0.4961(4) 0.7521(7) 0.1962(3) 0.0685(15) Uani 1 1 d . . .
H1C H 0.5469 0.6908 0.2017 0.082 Uiso 1 1 calc R . .
H1D H 0.4751 0.7934 0.1544 0.082 Uiso 1 1 calc R . .
C2 C 0.4297(4) 0.6502(8) 0.2070(3) 0.0819(19) Uani 1 1 d . . .
H2C H 0.4242 0.5516 0.1846 0.098 Uiso 1 1 calc R . .
H2D H 0.4458 0.6264 0.2507 0.098 Uiso 1 1 calc R . .
C3 C 0.2856(4) 0.6480(8) 0.1884(3) 0.0760(17) Uani 1 1 d . . .
H3C H 0.3038 0.6009 0.2293 0.091 Uiso 1 1 calc R . .
H3D H 0.2763 0.5628 0.1588 0.091 Uiso 1 1 calc R . .
C4 C 0.2067(3) 0.7245(7) 0.1777(3) 0.0649(15) Uani 1 1 d . . .
H4C H 0.1679 0.6519 0.1864 0.078 Uiso 1 1 calc R . .
H4D H 0.1822 0.7547 0.1345 0.078 Uiso 1 1 calc R . .
C5 C 0.1483(3) 0.9251(6) 0.2265(2) 0.0530(11) Uani 1 1 d . . .
C6 C 0.0665(3) 0.8676(8) 0.2043(2) 0.0622(14) Uani 1 1 d . . .
H6 H 0.0539 0.7822 0.1773 0.075 Uiso 1 1 calc R . .
C7 C 0.0019(3) 0.9338(8) 0.2211(2) 0.0651(15) Uani 1 1 d . . .
C8 C 0.0223(3) 1.0584(7) 0.2618(2) 0.0569(13) Uani 1 1 d . . .
C9 C 0.1039(3) 1.1234(6) 0.2825(2) 0.0509(11) Uani 1 1 d . . .
H9 H 0.1158 1.2115 0.3081 0.061 Uiso 1 1 calc R . .
C10 C 0.1668(3) 1.0572(6) 0.2649(2) 0.0522(12) Uani 1 1 d . . .
C11 C 0.2678(3) 1.2537(7) 0.3166(2) 0.0571(13) Uani 1 1 d . . .
H11A H 0.2620 1.2399 0.3566 0.068 Uiso 1 1 calc R . .
H11B H 0.2289 1.3359 0.2943 0.068 Uiso 1 1 calc R . .
C12 C 0.3578(3) 1.2985(7) 0.3249(2) 0.0579(13) Uani 1 1 d . . .
H12A H 0.3653 1.2986 0.2852 0.069 Uiso 1 1 calc R . .
H12B H 0.3702 1.4035 0.3425 0.069 Uiso 1 1 calc R . .
C13 C 0.4988(3) 1.2411(8) 0.3920(2) 0.0658(15) Uani 1 1 d . . .
H13A H 0.5299 1.1664 0.4237 0.079 Uiso 1 1 calc R . .
H13B H 0.4991 1.3417 0.4120 0.079 Uiso 1 1 calc R . .
C14 C 0.5444(3) 1.2596(8) 0.3473(3) 0.0723(17) Uani 1 1 d . . .
H14A H 0.5147 1.3353 0.3156 0.087 Uiso 1 1 calc R . .
H14B H 0.6014 1.2988 0.3689 0.087 Uiso 1 1 calc R . .
C15 C 0.5953(3) 1.1046(7) 0.2814(2) 0.0552(12) Uani 1 1 d . . .
C16 C 0.6591(3) 1.2115(7) 0.2843(2) 0.0624(14) Uani 1 1 d . . .
H16 H 0.6707 1.2945 0.3123 0.075 Uiso 1 1 calc R . .
C17 C 0.7061(3) 1.1955(8) 0.2453(3) 0.0676(16) Uani 1 1 d . . .
C18 C 0.6866(3) 1.0782(8) 0.2014(2) 0.0611(14) Uani 1 1 d . . .
C19 C 0.6227(3) 0.9729(7) 0.1997(2) 0.0589(13) Uani 1 1 d . . .
H19 H 0.6096 0.8917 0.1709 0.071 Uiso 1 1 calc R . .
C20 C 0.5778(3) 0.9839(6) 0.2389(2) 0.0508(11) Uani 1 1 d . . .
C21 C 0.3482(7) 0.7819(13) 0.0021(5) 0.154(4) Uani 1 1 d . . .
H21A H 0.3572 0.8104 -0.0358 0.184 Uiso 1 1 calc R . .
H21B H 0.3727 0.8642 0.0323 0.184 Uiso 1 1 calc R . .
C22 C 0.2552(6) 0.7707(15) -0.0103(4) 0.143(4) Uani 1 1 d . . .
H22A H 0.2465 0.7433 0.0277 0.171 Uiso 1 1 calc R . .
H22B H 0.2292 0.8728 -0.0237 0.171 Uiso 1 1 calc R . .
C23 C 0.1309(5) 0.6312(11) -0.0814(4) 0.120(3) Uani 1 1 d . . .
H23A H 0.1264 0.5278 -0.1002 0.144 Uiso 1 1 calc R . .
H23B H 0.1082 0.7062 -0.1149 0.144 Uiso 1 1 calc R . .
C24 C 0.0742(5) 0.6322(10) -0.0457(4) 0.106(3) Uani 1 1 d . . .
H24A H 0.0787 0.7325 -0.0246 0.127 Uiso 1 1 calc R . .
H24B H 0.0158 0.6188 -0.0733 0.127 Uiso 1 1 calc R . .
C25 C 0.0583(3) 0.5039(7) 0.0402(3) 0.0673(15) Uani 1 1 d . . .
C26 C -0.0124(3) 0.5945(7) 0.0362(3) 0.0682(14) Uani 1 1 d . . .
H26 H -0.0353 0.6628 0.0030 0.082 Uiso 1 1 calc R . .
C27 C -0.0491(4) 0.5850(8) 0.0806(3) 0.0735(16) Uani 1 1 d . . .
C28 C -0.0124(4) 0.4851(8) 0.1324(3) 0.0759(17) Uani 1 1 d . . .
C29 C 0.0582(4) 0.3966(8) 0.1355(3) 0.0725(16) Uani 1 1 d . . .
H29 H 0.0828 0.3304 0.1692 0.087 Uiso 1 1 calc R . .
C30 C 0.0925(3) 0.4047(7) 0.0899(3) 0.0658(14) Uani 1 1 d . . .
C31 C 0.1995(4) 0.2099(9) 0.1390(3) 0.087(2) Uani 1 1 d . . .
H31A H 0.1569 0.1361 0.1416 0.104 Uiso 1 1 calc R . .
H31B H 0.2215 0.2673 0.1777 0.104 Uiso 1 1 calc R . .
C32 C 0.2674(4) 0.1261(8) 0.1283(4) 0.094(2) Uani 1 1 d . . .
H32A H 0.2856 0.0387 0.1571 0.113 Uiso 1 1 calc R . .
H32B H 0.2473 0.0836 0.0866 0.113 Uiso 1 1 calc R . .
C33 C 0.3975(4) 0.1569(7) 0.1169(3) 0.087(2) Uani 1 1 d . . .
H33A H 0.3724 0.1320 0.0732 0.104 Uiso 1 1 calc R . .
H33B H 0.4158 0.0590 0.1394 0.104 Uiso 1 1 calc R . .
C34 C 0.4715(4) 0.2613(7) 0.1276(3) 0.0681(15) Uani 1 1 d . . .
H34A H 0.4961 0.2885 0.1711 0.082 Uiso 1 1 calc R . .
H34B H 0.5145 0.2080 0.1159 0.082 Uiso 1 1 calc R . .
C35 C 0.5040(4) 0.5006(7) 0.0868(3) 0.0643(14) Uani 1 1 d . . .
C36 C 0.5907(4) 0.4839(7) 0.1180(2) 0.0634(14) Uani 1 1 d . . .
H36 H 0.6114 0.4004 0.1452 0.076 Uiso 1 1 calc R . .
C37 C 0.6465(4) 0.5925(9) 0.1082(3) 0.0824(19) Uani 1 1 d . . .
C38 C 0.6167(5) 0.7154(9) 0.0670(3) 0.084(2) Uani 1 1 d . . .
C39 C 0.5313(5) 0.7330(9) 0.0383(3) 0.089(2) Uani 1 1 d . . .
H39 H 0.5111 0.8167 0.0110 0.106 Uiso 1 1 calc R . .
C40 C 0.4725(4) 0.6292(8) 0.0484(3) 0.0773(17) Uani 1 1 d . . .
C41 C -0.0448(4) 0.5438(8) 0.3639(3) 0.0808(18) Uani 1 1 d . . .
H41A H -0.0208 0.4864 0.4025 0.097 Uiso 1 1 calc R . .
H41B H -0.0995 0.4967 0.3410 0.097 Uiso 1 1 calc R . .
C42 C -0.0595(4) 0.7102(9) 0.3787(3) 0.090(2) Uani 1 1 d . . .
H42A H -0.0864 0.7073 0.4095 0.108 Uiso 1 1 calc R . .
H42B H -0.0044 0.7595 0.3980 0.108 Uiso 1 1 calc R . .
C43 C -0.1880(4) 0.7685(13) 0.3000(5) 0.184(7) Uani 1 1 d . . .
H43A H -0.2093 0.8573 0.2724 0.220 Uiso 1 1 calc R . .
H43B H -0.1851 0.6810 0.2739 0.220 Uiso 1 1 calc R . .
C44 C -0.2501(4) 0.7318(11) 0.3195(4) 0.127(4) Uani 1 1 d . . .
H44A H -0.3028 0.7265 0.2842 0.152 Uiso 1 1 calc R . .
H44B H -0.2560 0.8151 0.3464 0.152 Uiso 1 1 calc R . .
C45 C -0.2771(3) 0.5662(7) 0.3947(3) 0.0650(15) Uani 1 1 d . . .
C46 C -0.3403(3) 0.6668(7) 0.3982(3) 0.0715(16) Uani 1 1 d . . .
H46 H -0.3587 0.7502 0.3705 0.086 Uiso 1 1 calc R . .
C47 C -0.3760(3) 0.6432(8) 0.4428(3) 0.0715(16) Uani 1 1 d . . .
C48 C -0.3474(3) 0.5245(8) 0.4856(3) 0.0672(15) Uani 1 1 d . . .
C49 C -0.2857(3) 0.4218(7) 0.4806(2) 0.0563(12) Uani 1 1 d . . .
H49 H -0.2681 0.3379 0.5081 0.068 Uiso 1 1 calc R . .
C50 C -0.2501(3) 0.4419(6) 0.4357(2) 0.0524(12) Uani 1 1 d . . .
C51 C -0.1698(3) 0.2041(6) 0.4655(2) 0.0563(12) Uani 1 1 d . . .
H51A H -0.2217 0.1445 0.4579 0.068 Uiso 1 1 calc R . .
H51B H -0.1465 0.2304 0.5091 0.068 Uiso 1 1 calc R . .
C52 C -0.1085(3) 0.1086(6) 0.4489(2) 0.0593(13) Uani 1 1 d . . .
H52A H -0.1036 0.0055 0.4680 0.071 Uiso 1 1 calc R . .
H52B H -0.1288 0.0940 0.4044 0.071 Uiso 1 1 calc R . .
C53 C 0.0362(3) 0.0873(6) 0.4579(3) 0.0584(13) Uani 1 1 d . . .
H53A H 0.0129 0.0386 0.4174 0.070 Uiso 1 1 calc R . .
H53B H 0.0540 0.0042 0.4887 0.070 Uiso 1 1 calc R . .
C54 C 0.1098(3) 0.1867(6) 0.4614(2) 0.0571(12) Uani 1 1 d . . .
H54A H 0.1315 0.2404 0.5010 0.069 Uiso 1 1 calc R . .
H54B H 0.1549 0.1225 0.4569 0.069 Uiso 1 1 calc R . .
C55 C 0.1348(3) 0.4124(6) 0.4071(2) 0.0507(11) Uani 1 1 d . . .
C56 C 0.2206(3) 0.4165(6) 0.4393(2) 0.0524(11) Uani 1 1 d . . .
H56 H 0.2456 0.3413 0.4696 0.063 Uiso 1 1 calc R . .
C57 C 0.2706(3) 0.5330(7) 0.4268(2) 0.0624(14) Uani 1 1 d . . .
C58 C 0.2335(4) 0.6442(8) 0.3814(3) 0.0728(17) Uani 1 1 d . . .
C59 C 0.1461(4) 0.6424(8) 0.3511(3) 0.0768(18) Uani 1 1 d . . .
H59 H 0.1207 0.7205 0.3223 0.092 Uiso 1 1 calc R . .
C60 C 0.0966(3) 0.5281(7) 0.3628(2) 0.0632(14) Uani 1 1 d . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C20 1.376(6) . ?
O1 C1 1.452(6) . ?
O2 C3 1.325(7) . ?
O2 C2 1.477(7) . ?
O3 C5 1.379(6) . ?
O3 C4 1.423(6) . ?
O4 C10 1.376(5) . ?
O4 C11 1.413(6) . ?
O5 C12 1.406(6) . ?
O5 C13 1.427(5) . ?
O6 C15 1.379(6) . ?
O6 C14 1.425(7) . ?
O7 C21 1.342(11) . ?
O7 C40 1.346(8) . ?
O8 C22 1.325(13) . ?
O8 C23 1.396(10) . ?
O9 C25 1.352(7) . ?
O9 C24 1.422(8) . ?
O10 C30 1.405(7) . ?
O10 C31 1.413(7) . ?
O11 C33 1.390(8) . ?
O11 C32 1.423(7) . ?
O12 C35 1.359(7) . ?
O12 C34 1.417(6) . ?
O13 C60 1.386(6) . ?
O13 C41 1.455(8) . ?
O14 C42 1.343(7) . ?
O14 C43 1.349(8) . ?
O15 C45 1.370(7) . ?
O15 C44 1.452(7) . ?
O16 C50 1.365(6) . ?
O16 C51 1.447(6) . ?
O17 C53 1.424(6) . ?
O17 C52 1.428(6) . ?
O18 C55 1.361(6) . ?
O18 C54 1.423(6) . ?
N1 C17 1.444(8) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N2 C18 1.388(7) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N3 C7 1.407(7) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N4 C8 1.430(6) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N5 C37 1.406(8) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N6 C38 1.426(8) . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
N7 C27 1.413(8) . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
N8 C28 1.408(8) . ?
N8 H8A 0.8600 . ?
N8 H8B 0.8600 . ?
N9 C57 1.429(7) . ?
N9 H9A 0.8600 . ?
N9 H9B 0.8600 . ?
N10 C58 1.424(7) . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
N11 C47 1.452(8) . ?
N11 H11C 0.8600 . ?
N11 H11D 0.8600 . ?
N12 C48 1.419(8) . ?
N12 H12C 0.8600 . ?
N12 H12D 0.8600 . ?
C1 C2 1.501(8) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C4 1.418(8) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.378(7) . ?
C5 C10 1.394(7) . ?
C6 C7 1.396(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.375(8) . ?
C8 C9 1.397(6) . ?
C9 C10 1.381(7) . ?
C9 H9 0.9300 . ?
C11 C12 1.507(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.497(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C20 1.376(7) . ?
C15 C16 1.389(7) . ?
C16 C17 1.401(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.375(9) . ?
C18 C19 1.388(8) . ?
C19 C20 1.373(7) . ?
C19 H19 0.9300 . ?
C21 C22 1.491(13) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.467(10) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C30 1.376(8) . ?
C25 C26 1.393(8) . ?
C26 C27 1.377(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.417(9) . ?
C28 C29 1.385(9) . ?
C29 C30 1.373(8) . ?
C29 H29 0.9300 . ?
C31 C32 1.439(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.476(8) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.387(8) . ?
C35 C40 1.387(9) . ?
C36 C37 1.391(8) . ?
C36 H36 0.9300 . ?
C37 C38 1.381(10) . ?
C38 C39 1.361(9) . ?
C39 C40 1.405(9) . ?
C39 H39 0.9300 . ?
C41 C42 1.493(10) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.313(10) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C50 1.383(7) . ?
C45 C46 1.390(8) . ?
C46 C47 1.379(9) . ?
C46 H46 0.9300 . ?
C47 C48 1.375(9) . ?
C48 C49 1.391(7) . ?
C49 C50 1.382(7) . ?
C49 H49 0.9300 . ?
C51 C52 1.465(7) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 C54 1.477(7) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.371(6) . ?
C55 C60 1.400(7) . ?
C56 C57 1.393(8) . ?
C56 H56 0.9300 . ?
C57 C58 1.384(8) . ?
C58 C59 1.387(8) . ?
C59 C60 1.366(8) . ?
C59 H59 0.9300 . ?

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
C20 O1 C1 116.2(4) . . ?
C3 O2 C2 111.0(5) . . ?
C5 O3 C4 120.6(4) . . ?
C10 O4 C11 116.9(4) . . ?
C12 O5 C13 114.3(4) . . ?
C15 O6 C14 117.0(4) . . ?
C21 O7 C40 123.5(7) . . ?
C22 O8 C23 129.0(8) . . ?
C25 O9 C24 116.8(5) . . ?
C30 O10 C31 117.6(5) . . ?
C33 O11 C32 110.5(5) . . ?
C35 O12 C34 118.1(4) . . ?
C60 O13 C41 114.8(4) . . ?
C42 O14 C43 120.0(6) . . ?
C45 O15 C44 116.6(5) . . ?
C50 O16 C51 116.3(4) . . ?
C53 O17 C52 112.8(4) . . ?
C55 O18 C54 119.6(4) . . ?
C17 N1 H1A 120.0 . . ?
C17 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C18 N2 H2A 120.0 . . ?
C18 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C7 N3 H3A 120.0 . . ?
C7 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C8 N4 H4A 120.0 . . ?
C8 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C37 N5 H5A 120.0 . . ?
C37 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C38 N6 H6A 120.0 . . ?
C38 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C27 N7 H7A 120.0 . . ?
C27 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
C28 N8 H8A 120.0 . . ?
C28 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
C57 N9 H9A 120.0 . . ?
C57 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
C58 N10 H10A 120.0 . . ?
C58 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C47 N11 H11C 120.0 . . ?
C47 N11 H11D 120.0 . . ?
H11C N11 H11D 120.0 . . ?
C48 N12 H12C 120.0 . . ?
C48 N12 H12D 120.0 . . ?
H12C N12 H12D 120.0 . . ?
O1 C1 C2 108.1(5) . . ?
O1 C1 H1C 110.1 . . ?
C2 C1 H1C 110.1 . . ?
O1 C1 H1D 110.1 . . ?
C2 C1 H1D 110.1 . . ?
H1C C1 H1D 108.4 . . ?
O2 C2 C1 108.0(5) . . ?
O2 C2 H2C 110.1 . . ?
C1 C2 H2C 110.1 . . ?
O2 C2 H2D 110.1 . . ?
C1 C2 H2D 110.1 . . ?
H2C C2 H2D 108.4 . . ?
O2 C3 C4 116.5(6) . . ?
O2 C3 H3C 108.2 . . ?
C4 C3 H3C 108.2 . . ?
O2 C3 H3D 108.2 . . ?
C4 C3 H3D 108.2 . . ?
H3C C3 H3D 107.3 . . ?
C3 C4 O3 111.3(4) . . ?
C3 C4 H4C 109.4 . . ?
O3 C4 H4C 109.4 . . ?
C3 C4 H4D 109.4 . . ?
O3 C4 H4D 109.4 . . ?
H4C C4 H4D 108.0 . . ?
C6 C5 O3 125.6(5) . . ?
C6 C5 C10 119.3(5) . . ?
O3 C5 C10 115.1(4) . . ?
C5 C6 C7 121.9(5) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C8 C7 C6 118.0(5) . . ?
C8 C7 N3 122.1(5) . . ?
C6 C7 N3 119.9(6) . . ?
C7 C8 C9 120.9(5) . . ?
C7 C8 N4 119.8(4) . . ?
C9 C8 N4 119.3(5) . . ?
C10 C9 C8 120.2(5) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
O4 C10 C9 124.9(4) . . ?
O4 C10 C5 115.5(4) . . ?
C9 C10 C5 119.6(4) . . ?
O4 C11 C12 107.6(4) . . ?
O4 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
O4 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
O5 C12 C11 108.5(4) . . ?
O5 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
O5 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O5 C13 C14 114.5(4) . . ?
O5 C13 H13A 108.6 . . ?
C14 C13 H13A 108.6 . . ?
O5 C13 H13B 108.6 . . ?
C14 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
O6 C14 C13 109.6(5) . . ?
O6 C14 H14A 109.7 . . ?
C13 C14 H14A 109.7 . . ?
O6 C14 H14B 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C20 C15 O6 117.5(4) . . ?
C20 C15 C16 119.1(5) . . ?
O6 C15 C16 123.5(5) . . ?
C15 C16 C17 120.6(5) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C18 C17 C16 120.2(5) . . ?
C18 C17 N1 120.6(5) . . ?
C16 C17 N1 119.0(6) . . ?
C17 C18 N2 119.3(5) . . ?
C17 C18 C19 117.7(5) . . ?
N2 C18 C19 122.8(6) . . ?
C20 C19 C18 122.7(5) . . ?
C20 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
C19 C20 C15 119.5(5) . . ?
C19 C20 O1 125.3(5) . . ?
C15 C20 O1 115.2(4) . . ?
O7 C21 C22 111.2(10) . . ?
O7 C21 H21A 109.4 . . ?
C22 C21 H21A 109.4 . . ?
O7 C21 H21B 109.4 . . ?
C22 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
O8 C22 C21 112.3(8) . . ?
O8 C22 H22A 109.2 . . ?
C21 C22 H22A 109.2 . . ?
O8 C22 H22B 109.2 . . ?
C21 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
O8 C23 C24 121.0(8) . . ?
O8 C23 H23A 107.1 . . ?
C24 C23 H23A 107.1 . . ?
O8 C23 H23B 107.1 . . ?
C24 C23 H23B 107.1 . . ?
H23A C23 H23B 106.8 . . ?
O9 C24 C23 109.3(6) . . ?
O9 C24 H24A 109.8 . . ?
C23 C24 H24A 109.8 . . ?
O9 C24 H24B 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.3 . . ?
O9 C25 C30 116.7(5) . . ?
O9 C25 C26 124.2(5) . . ?
C30 C25 C26 119.1(6) . . ?
C27 C26 C25 121.3(6) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C26 C27 N7 120.2(6) . . ?
C26 C27 C28 119.3(6) . . ?
N7 C27 C28 120.5(6) . . ?
C29 C28 N8 122.0(6) . . ?
C29 C28 C27 118.4(6) . . ?
N8 C28 C27 119.6(6) . . ?
C30 C29 C28 121.4(6) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C29 C30 C25 120.5(6) . . ?
C29 C30 O10 124.3(5) . . ?
C25 C30 O10 115.2(5) . . ?
O10 C31 C32 108.7(6) . . ?
O10 C31 H31A 109.9 . . ?
C32 C31 H31A 109.9 . . ?
O10 C31 H31B 109.9 . . ?
C32 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
O11 C32 C31 110.1(6) . . ?
O11 C32 H32A 109.6 . . ?
C31 C32 H32A 109.6 . . ?
O11 C32 H32B 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.2 . . ?
O11 C33 C34 110.5(5) . . ?
O11 C33 H33A 109.5 . . ?
C34 C33 H33A 109.5 . . ?
O11 C33 H33B 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
O12 C34 C33 108.5(4) . . ?
O12 C34 H34A 110.0 . . ?
C33 C34 H34A 110.0 . . ?
O12 C34 H34B 110.0 . . ?
C33 C34 H34B 110.0 . . ?
H34A C34 H34B 108.4 . . ?
O12 C35 C36 124.7(5) . . ?
O12 C35 C40 114.9(5) . . ?
C36 C35 C40 120.3(6) . . ?
C35 C36 C37 119.7(6) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C38 C37 C36 120.7(6) . . ?
C38 C37 N5 119.9(7) . . ?
C36 C37 N5 119.3(7) . . ?
C39 C38 C37 118.8(6) . . ?
C39 C38 N6 121.0(7) . . ?
C37 C38 N6 120.1(7) . . ?
C38 C39 C40 122.3(7) . . ?
C38 C39 H39 118.9 . . ?
C40 C39 H39 118.9 . . ?
O7 C40 C35 117.3(6) . . ?
O7 C40 C39 124.8(6) . . ?
C35 C40 C39 117.9(6) . . ?
O13 C41 C42 116.5(6) . . ?
O13 C41 H41A 108.2 . . ?
C42 C41 H41A 108.2 . . ?
O13 C41 H41B 108.2 . . ?
C42 C41 H41B 108.2 . . ?
H41A C41 H41B 107.3 . . ?
O14 C42 C41 118.7(6) . . ?
O14 C42 H42A 107.6 . . ?
C41 C42 H42A 107.6 . . ?
O14 C42 H42B 107.6 . . ?
C41 C42 H42B 107.6 . . ?
H42A C42 H42B 107.1 . . ?
C44 C43 O14 129.9(10) . . ?
C44 C43 H43A 104.8 . . ?
O14 C43 H43A 104.8 . . ?
C44 C43 H43B 104.8 . . ?
O14 C43 H43B 104.8 . . ?
H43A C43 H43B 105.8 . . ?
C43 C44 O15 113.6(6) . . ?
C43 C44 H44A 108.9 . . ?
O15 C44 H44A 108.9 . . ?
C43 C44 H44B 108.9 . . ?
O15 C44 H44B 108.9 . . ?
H44A C44 H44B 107.7 . . ?
O15 C45 C50 116.3(5) . . ?
O15 C45 C46 123.8(5) . . ?
C50 C45 C46 120.0(6) . . ?
C47 C46 C45 120.1(5) . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
C48 C47 C46 120.8(5) . . ?
C48 C47 N11 118.1(6) . . ?
C46 C47 N11 121.0(6) . . ?
C47 C48 C49 118.6(6) . . ?
C47 C48 N12 120.5(5) . . ?
C49 C48 N12 120.7(6) . . ?
C50 C49 C48 121.4(5) . . ?
C50 C49 H49 119.3 . . ?
C48 C49 H49 119.3 . . ?
O16 C50 C49 124.3(5) . . ?
O16 C50 C45 116.6(5) . . ?
C49 C50 C45 119.0(5) . . ?
O16 C51 C52 109.7(4) . . ?
O16 C51 H51A 109.7 . . ?
C52 C51 H51A 109.7 . . ?
O16 C51 H51B 109.7 . . ?
C52 C51 H51B 109.7 . . ?
H51A C51 H51B 108.2 . . ?
O17 C52 C51 111.1(4) . . ?
O17 C52 H52A 109.4 . . ?
C51 C52 H52A 109.4 . . ?
O17 C52 H52B 109.4 . . ?
C51 C52 H52B 109.4 . . ?
H52A C52 H52B 108.0 . . ?
O17 C53 C54 109.3(4) . . ?
O17 C53 H53A 109.8 . . ?
C54 C53 H53A 109.8 . . ?
O17 C53 H53B 109.8 . . ?
C54 C53 H53B 109.8 . . ?
H53A C53 H53B 108.3 . . ?
O18 C54 C53 107.0(4) . . ?
O18 C54 H54A 110.3 . . ?
C53 C54 H54A 110.3 . . ?
O18 C54 H54B 110.3 . . ?
C53 C54 H54B 110.3 . . ?
H54A C54 H54B 108.6 . . ?
O18 C55 C56 125.2(5) . . ?
O18 C55 C60 114.6(4) . . ?
C56 C55 C60 120.1(5) . . ?
C55 C56 C57 120.2(5) . . ?
C55 C56 H56 119.9 . . ?
C57 C56 H56 119.9 . . ?
C58 C57 C56 119.9(5) . . ?
C58 C57 N9 119.4(5) . . ?
C56 C57 N9 120.6(5) . . ?
C57 C58 C59 119.2(5) . . ?
C57 C58 N10 118.9(5) . . ?
C59 C58 N10 121.9(6) . . ?
C60 C59 C58 121.3(6) . . ?
C60 C59 H59 119.3 . . ?
C58 C59 H59 119.3 . . ?
C59 C60 O13 120.3(5) . . ?
C59 C60 C55 119.3(5) . . ?
O13 C60 C55 120.3(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 O1 C1 C2 177.8(4) . . . . ?
C3 O2 C2 C1 174.9(5) . . . . ?
O1 C1 C2 O2 72.1(6) . . . . ?
C2 O2 C3 C4 170.7(5) . . . . ?
O2 C3 C4 O3 -52.1(8) . . . . ?
C5 O3 C4 C3 -160.4(5) . . . . ?
C4 O3 C5 C6 0.7(8) . . . . ?
C4 O3 C5 C10 179.1(5) . . . . ?
O3 C5 C6 C7 175.7(5) . . . . ?
C10 C5 C6 C7 -2.7(8) . . . . ?
C5 C6 C7 C8 -1.0(9) . . . . ?
C5 C6 C7 N3 -177.9(6) . . . . ?
C6 C7 C8 C9 4.1(8) . . . . ?
N3 C7 C8 C9 -179.0(6) . . . . ?
C6 C7 C8 N4 -178.4(5) . . . . ?
N3 C7 C8 N4 -1.5(8) . . . . ?
C7 C8 C9 C10 -3.7(8) . . . . ?
N4 C8 C9 C10 178.8(5) . . . . ?
C11 O4 C10 C9 -6.6(7) . . . . ?
C11 O4 C10 C5 173.8(4) . . . . ?
C8 C9 C10 O4 -179.6(5) . . . . ?
C8 C9 C10 C5 -0.1(7) . . . . ?
C6 C5 C10 O4 -177.2(5) . . . . ?
O3 C5 C10 O4 4.2(6) . . . . ?
C6 C5 C10 C9 3.2(7) . . . . ?
O3 C5 C10 C9 -175.4(5) . . . . ?
C10 O4 C11 C12 -173.8(4) . . . . ?
C13 O5 C12 C11 -161.4(4) . . . . ?
O4 C11 C12 O5 -68.1(5) . . . . ?
C12 O5 C13 C14 -68.0(6) . . . . ?
C15 O6 C14 C13 -174.2(4) . . . . ?
O5 C13 C14 O6 -61.3(7) . . . . ?
C14 O6 C15 C20 -158.7(5) . . . . ?
C14 O6 C15 C16 22.1(7) . . . . ?
C20 C15 C16 C17 -1.1(8) . . . . ?
O6 C15 C16 C17 178.1(5) . . . . ?
C15 C16 C17 C18 3.4(8) . . . . ?
C15 C16 C17 N1 179.6(5) . . . . ?
C16 C17 C18 N2 -178.4(5) . . . . ?
N1 C17 C18 N2 5.4(8) . . . . ?
C16 C17 C18 C19 -3.4(8) . . . . ?
N1 C17 C18 C19 -179.6(5) . . . . ?
C17 C18 C19 C20 1.3(7) . . . . ?
N2 C18 C19 C20 176.1(5) . . . . ?
C18 C19 C20 C15 0.9(7) . . . . ?
C18 C19 C20 O1 -178.1(4) . . . . ?
O6 C15 C20 C19 179.7(4) . . . . ?
C16 C15 C20 C19 -1.0(7) . . . . ?
O6 C15 C20 O1 -1.1(6) . . . . ?
C16 C15 C20 O1 178.1(4) . . . . ?
C1 O1 C20 C19 -0.8(7) . . . . ?
C1 O1 C20 C15 -179.8(4) . . . . ?
C40 O7 C21 C22 -167.7(7) . . . . ?
C23 O8 C22 C21 -172.9(9) . . . . ?
O7 C21 C22 O8 -61.5(12) . . . . ?
C22 O8 C23 C24 -39.5(16) . . . . ?
C25 O9 C24 C23 171.9(7) . . . . ?
O8 C23 C24 O9 -65.9(12) . . . . ?
C24 O9 C25 C30 -167.0(6) . . . . ?
C24 O9 C25 C26 12.2(9) . . . . ?
O9 C25 C26 C27 179.9(6) . . . . ?
C30 C25 C26 C27 -0.8(9) . . . . ?
C25 C26 C27 N7 -179.6(5) . . . . ?
C25 C26 C27 C28 2.2(9) . . . . ?
C26 C27 C28 C29 -1.9(9) . . . . ?
N7 C27 C28 C29 180.0(5) . . . . ?
C26 C27 C28 N8 -179.2(6) . . . . ?
N7 C27 C28 N8 2.7(9) . . . . ?
N8 C28 C29 C30 177.4(6) . . . . ?
C27 C28 C29 C30 0.2(9) . . . . ?
C28 C29 C30 C25 1.3(9) . . . . ?
C28 C29 C30 O10 -178.7(5) . . . . ?
O9 C25 C30 C29 178.3(5) . . . . ?
C26 C25 C30 C29 -0.9(8) . . . . ?
O9 C25 C30 O10 -1.7(7) . . . . ?
C26 C25 C30 O10 179.0(5) . . . . ?
C31 O10 C30 C29 1.1(8) . . . . ?
C31 O10 C30 C25 -178.8(5) . . . . ?
C30 O10 C31 C32 177.2(5) . . . . ?
C33 O11 C32 C31 -170.8(6) . . . . ?
O10 C31 C32 O11 70.7(8) . . . . ?
C32 O11 C33 C34 -177.5(5) . . . . ?
C35 O12 C34 C33 -169.6(5) . . . . ?
O11 C33 C34 O12 -62.4(7) . . . . ?
C34 O12 C35 C36 -4.5(8) . . . . ?
C34 O12 C35 C40 176.9(5) . . . . ?
O12 C35 C36 C37 178.3(5) . . . . ?
C40 C35 C36 C37 -3.2(8) . . . . ?
C35 C36 C37 C38 -1.2(9) . . . . ?
C35 C36 C37 N5 -178.5(6) . . . . ?
C36 C37 C38 C39 3.2(10) . . . . ?
N5 C37 C38 C39 -179.4(6) . . . . ?
C36 C37 C38 N6 -179.7(6) . . . . ?
N5 C37 C38 N6 -2.4(10) . . . . ?
C37 C38 C39 C40 -1.0(10) . . . . ?
N6 C38 C39 C40 -178.0(6) . . . . ?
C21 O7 C40 C35 158.4(8) . . . . ?
C21 O7 C40 C39 -21.9(12) . . . . ?
O12 C35 C40 O7 3.6(8) . . . . ?
C36 C35 C40 O7 -175.1(6) . . . . ?
O12 C35 C40 C39 -176.1(5) . . . . ?
C36 C35 C40 C39 5.3(9) . . . . ?
C38 C39 C40 O7 177.1(7) . . . . ?
C38 C39 C40 C35 -3.3(10) . . . . ?
C60 O13 C41 C42 80.5(7) . . . . ?
C43 O14 C42 C41 61.2(12) . . . . ?
O13 C41 C42 O14 69.9(8) . . . . ?
C42 O14 C43 C44 50.8(17) . . . . ?
O14 C43 C44 O15 -66.3(17) . . . . ?
C45 O15 C44 C43 154.1(9) . . . . ?
C44 O15 C45 C50 -165.8(6) . . . . ?
C44 O15 C45 C46 13.3(8) . . . . ?
O15 C45 C46 C47 -178.8(5) . . . . ?
C50 C45 C46 C47 0.3(8) . . . . ?
C45 C46 C47 C48 2.6(9) . . . . ?
C45 C46 C47 N11 177.8(5) . . . . ?
C46 C47 C48 C49 -4.3(8) . . . . ?
N11 C47 C48 C49 -179.7(5) . . . . ?
C46 C47 C48 N12 -179.0(5) . . . . ?
N11 C47 C48 N12 5.7(8) . . . . ?
C47 C48 C49 C50 3.3(7) . . . . ?
N12 C48 C49 C50 178.0(5) . . . . ?
C51 O16 C50 C49 9.8(6) . . . . ?
C51 O16 C50 C45 -170.8(4) . . . . ?
C48 C49 C50 O16 178.8(4) . . . . ?
C48 C49 C50 C45 -0.5(7) . . . . ?
O15 C45 C50 O16 -1.5(7) . . . . ?
C46 C45 C50 O16 179.3(4) . . . . ?
O15 C45 C50 C49 177.9(5) . . . . ?
C46 C45 C50 C49 -1.3(7) . . . . ?
C50 O16 C51 C52 174.7(4) . . . . ?
C53 O17 C52 C51 175.2(4) . . . . ?
O16 C51 C52 O17 68.8(5) . . . . ?
C52 O17 C53 C54 163.0(4) . . . . ?
C55 O18 C54 C53 175.7(4) . . . . ?
O17 C53 C54 O18 -63.7(5) . . . . ?
C54 O18 C55 C56 11.0(7) . . . . ?
C54 O18 C55 C60 -171.6(4) . . . . ?
O18 C55 C56 C57 175.3(5) . . . . ?
C60 C55 C56 C57 -1.9(7) . . . . ?
C55 C56 C57 C58 -0.5(8) . . . . ?
C55 C56 C57 N9 -175.9(5) . . . . ?
C56 C57 C58 C59 3.2(9) . . . . ?
N9 C57 C58 C59 178.6(6) . . . . ?
C56 C57 C58 N10 -178.6(5) . . . . ?
N9 C57 C58 N10 -3.2(8) . . . . ?
C57 C58 C59 C60 -3.6(9) . . . . ?
N10 C58 C59 C60 178.3(6) . . . . ?
C58 C59 C60 O13 -174.8(6) . . . . ?
C58 C59 C60 C55 1.3(9) . . . . ?
C41 O13 C60 C59 -117.6(6) . . . . ?
C41 O13 C60 C55 66.4(7) . . . . ?
O18 C55 C60 C59 -175.9(5) . . . . ?
C56 C55 C60 C59 1.5(8) . . . . ?
O18 C55 C60 O13 0.1(7) . . . . ?
C56 C55 C60 O13 177.6(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A N2 . . . 2.793(8) 0.860 2.499 101.0 no
N2 H2A N1 . . . 2.793(8) 0.860 2.460 103.8 no
N2 H2B N6 . . . 3.066(8) 0.860 2.215 170.3 no
N3 H3A N4 . . . 2.833(8) 0.860 2.532 101.6 no
N4 H4A N3 . . . 2.833(8) 0.860 2.527 102.0 no
N5 H5A N6 . . . 2.798(9) 0.860 2.477 102.9 no
N6 H6B N5 . . . 2.798(9) 0.860 2.489 102.1 no
N7 H7B N8 . . . 2.829(8) 0.860 2.517 102.4 no
N8 H8B N7 . . . 2.829(8) 0.860 2.508 103.0 no
N9 H9A N10 . . . 2.775(8) 0.860 2.452 103.0 no
N10 H10A O19 . . . 2.906(8) 0.860 2.433 115.3 no
N10 H10A N9 . . . 2.775(8) 0.860 2.446 103.4 no
N11 H11C N12 . . . 2.782(8) 0.860 2.459 103.0 no
N11 H11D O19 . . 1_455 2.975(6) 0.860 2.296 135.9 no
N12 H12C N11 . . . 2.782(8) 0.860 2.459 103.0 no
N12 H12D N10 . . 2_546 3.093(7) 0.860 2.255 164.9 no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_210530_K
_database_code_depnum_ccdc_archive 'CCDC 2168844'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Akutagawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_SHFSU01_210530_K            
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: This is due to the disordered H2O guest and orientational dosrder of H2SO4- anions
;
_vrf_PLAT080_210530_K            
;
PROBLEM: Maximum Shift/Error ............................       2.58 Why ?
RESPONSE: This is due to the disordered H2O guest and orientational dosrder of H2SO4- anions
;
_vrf_PLAT214_210530_K            
;
PROBLEM: Atom O49       (Anion/Solvent) ADP max/min Ratio       10.4 prolat
RESPONSE: This is due to the disordered H2O guest and orientational dosrder of H2SO4- anions
;
_vrf_PLAT430_210530_K            
;
PROBLEM: Short Inter D...A Contact  O29      ..O47      .       2.53 Ang.
RESPONSE: This is due to the disordered H2O guest and orientational dosrder of H2SO4- anions
;
# Added during the CSD deposition process: Tuesday 26 April 2022 05:29 AM
# end Validation Reply Form


#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C20 H46 K N4 O24 S3'
_chemical_formula_moiety         'C20 H46 K N4 O24 S3'
_chemical_formula_weight         861.87
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
_space_group_IT_number           33
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,1/2+Z
3 1/2-X,1/2+Y,1/2+Z
4 1/2+X,1/2-Y,+Z
#------------------------------------------------------------------------------
_cell_length_a                   11.1964(2)
_cell_length_b                   16.8470(4)
_cell_length_c                   19.1707(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3616.09(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25789
_cell_measurement_theta_min      3.50
_cell_measurement_theta_max      68.27
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1812.00
_exptl_absorpt_coefficient_mu    3.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_T_max  0.685

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            40108
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_theta_max         68.220
_diffrn_reflns_theta_min         3.493
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6508
_reflns_number_gt                5240
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_max     0.962
_reflns_Friedel_fraction_full    0.963

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0722
_refine_ls_wR_factor_ref         0.2239
_refine_ls_wR_factor_gt          0.2073
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6508
_refine_ls_number_parameters     496
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1445P)²+5.5643P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          2.584
_refine_diff_density_max         1.29
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 2081 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.516(8)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.3331 0.5567
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
K K 0.3868 1.0657
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
K15 K -0.02601(16) 0.49880(10) 0.53017(19) 0.0446(5) Uani 1 1 d . . . . .
S1 S 0.0508(2) 0.16352(16) 0.25993(15) 0.0319(7) Uani 1 1 d . . . . .
S3 S 0.5495(2) 0.33758(16) 0.80060(15) 0.0325(7) Uani 1 1 d . . . . .
S4 S 0.30982(18) 0.42813(14) 0.0299(2) 0.0534(6) Uani 1 1 d . . . . .
O2 O 0.4042(19) 0.485(2) 0.0217(19) 0.131(12) Uani 0.5 1 d . . P . .
O5 O -0.0392(7) 0.4172(5) 0.4048(4) 0.0323(19) Uani 1 1 d . . . . .
O6 O 0.5235(8) 0.4181(5) 0.8280(5) 0.046(2) Uani 1 1 d . . . . .
O7 O 0.0419(7) 0.5613(5) 0.4043(4) 0.0310(18) Uani 1 1 d . . . . .
O8 O 0.0449(8) 0.5651(5) 0.6564(5) 0.040(2) Uani 1 1 d . . . . .
O9 O -0.0964(4) 0.3416(3) 0.5302(6) 0.0430(12) Uani 1 1 d . . . . .
O10 O 0.6270(9) 0.3395(5) 0.7396(5) 0.051(3) Uani 1 1 d . . . . .
O11 O 0.0778(5) 0.6457(3) 0.5327(5) 0.0410(12) Uani 1 1 d . . . . .
O12 O 0.0260(7) 0.0814(4) 0.2375(4) 0.0312(18) Uani 1 1 d . . . . .
O13 O 0.6106(10) 0.2944(5) 0.8559(5) 0.055(3) Uani 1 1 d . . . . .
O14 O -0.0637(7) 0.2035(5) 0.2764(5) 0.047(2) Uani 1 1 d . . . . .
O16 O 0.1250(9) 0.1596(4) 0.3223(4) 0.043(2) Uani 1 1 d . . . . .
O18 O 0.1124(10) 0.2078(4) 0.2046(4) 0.046(2) Uani 1 1 d . . . . .
O21 O 0.4401(8) 0.2965(6) 0.7820(6) 0.054(3) Uani 1 1 d . . . . .
O28 O 0.271(2) 0.5021(13) 0.0734(10) 0.089(7) Uani 0.5 1 d . . P . .
O29 O 0.629(4) 0.365(5) 0.9880(18) 0.59(6) Uani 1 1 d . . . . .
O37 O 0.080(2) -0.1442(6) 0.1309(7) 0.181(10) Uani 1 1 d . . . . .
O40 O 0.2393(11) 0.4343(8) -0.0289(5) 0.080(4) Uani 1 1 d . . . . .
O47 O 0.4396(16) 0.4306(12) 0.0313(16) 0.075(6) Uani 0.5 1 d . . P . .
O48 O -0.0347(8) 0.4186(5) 0.6559(5) 0.042(2) Uani 1 1 d . . . . .
O49 O 0.6113(16) 0.567(5) 0.9275(14) 0.74(7) Uani 1 1 d . . . . .
O50 O 0.7899(8) 0.5362(8) 1.0305(9) 0.129(5) Uani 1 1 d . . . . .
O51 O 0.1055(10) 0.0110(5) 0.1237(5) 0.071(3) Uani 1 1 d . . . . .
O52 O 0.2389(11) 0.4333(5) 0.0934(5) 0.013(2) Uani 0.5 1 d . . P . .
O53 O 0.344(3) 0.3453(18) 0.0240(15) 0.191(18) Uani 0.5 1 d . . P . .
O54 O 0.300(2) 0.3635(13) 0.0782(11) 0.085(6) Uani 0.5 1 d . . P . .
O55 O 0.4585(15) 0.6719(17) 1.0413(19) 0.271(15) Uani 1 1 d . . . . .
N19 N 0.2375(10) 0.3418(5) 0.8426(4) 0.033(2) Uani 1 1 d . . . . .
N20 N 0.2330(8) 0.3422(5) 0.2143(5) 0.029(2) Uani 1 1 d . . . . .
N22 N 0.3209(8) 0.5004(5) 0.2171(4) 0.0220(17) Uani 1 1 d . . . . .
N23 N 0.3172(9) 0.5063(6) 0.8506(5) 0.035(2) Uani 1 1 d . . . . .
C17 C 0.0925(10) 0.5117(6) 0.7051(6) 0.026(2) Uani 1 1 d . . . . .
C24 C 0.1828(9) 0.3995(6) 0.7972(6) 0.030(2) Uani 1 1 d . . . . .
C25 C 0.0505(11) 0.4349(7) 0.7025(5) 0.029(3) Uani 1 1 d . . . . .
C26 C 0.2287(10) 0.4789(6) 0.2627(6) 0.029(2) Uani 1 1 d . . . . .
C27 C 0.0948(10) 0.3793(7) 0.3105(6) 0.029(2) Uani 1 1 d . . . . .
H27 H 0.065971 0.327553 0.309562 0.034 Uiso 1 1 calc R U . . .
C30 C 0.0353(14) 0.6842(8) 0.4673(6) 0.044(3) Uani 1 1 d . . . . .
H30A H -0.050812 0.679570 0.463409 0.053 Uiso 1 1 calc R U . . .
H30B H 0.056153 0.740117 0.467241 0.053 Uiso 1 1 calc R U . . .
C31 C -0.1598(13) 0.3328(8) 0.5923(6) 0.042(3) Uani 1 1 d . . . . .
H31A H -0.200374 0.281942 0.592458 0.051 Uiso 1 1 calc R U . . .
H31B H -0.219774 0.374207 0.595797 0.051 Uiso 1 1 calc R U . . .
C32 C 0.2234(9) 0.4782(6) 0.7977(6) 0.026(2) Uani 1 1 d . . . . .
C33 C -0.0842(13) 0.3371(9) 0.4083(7) 0.045(3) Uani 1 1 d . . . . .
H33A H -0.018239 0.300417 0.414457 0.054 Uiso 1 1 calc R U . . .
H33B H -0.124256 0.323934 0.364923 0.054 Uiso 1 1 calc R U . . .
C34 C 0.0918(12) 0.6415(7) 0.6535(6) 0.040(3) Uani 1 1 d . . . . .
H34A H 0.178095 0.638995 0.649777 0.048 Uiso 1 1 calc R U . . .
H34B H 0.071618 0.670134 0.695716 0.048 Uiso 1 1 calc R U . . .
C35 C 0.1868(11) 0.4040(6) 0.2639(5) 0.030(3) Uani 1 1 d . . . . .
C36 C 0.1819(10) 0.5337(6) 0.7511(6) 0.030(2) Uani 1 1 d . . . . .
H36 H 0.213280 0.584784 0.750358 0.035 Uiso 1 1 calc R U . . .
C38 C 0.0943(13) 0.6430(7) 0.4083(6) 0.040(3) Uani 1 1 d . . . . .
H38A H 0.179792 0.640013 0.416164 0.048 Uiso 1 1 calc R U . . .
H38B H 0.080238 0.671492 0.365152 0.048 Uiso 1 1 calc R U . . .
C39 C 0.0996(11) 0.3795(7) 0.7494(6) 0.032(3) Uani 1 1 d . . . . .
H39 H 0.073725 0.327060 0.747403 0.038 Uiso 1 1 calc R U . . .
C41 C 0.0510(11) 0.4324(8) 0.3557(6) 0.036(3) Uani 1 1 d . . . . .
C42 C 0.1776(11) 0.5343(7) 0.3095(5) 0.031(3) Uani 1 1 d . . . . .
H42 H 0.202212 0.586964 0.306763 0.037 Uiso 1 1 calc R U . . .
C43 C 0.0409(13) 0.6839(7) 0.5910(6) 0.038(3) Uani 1 1 d . . . . .
H43A H -0.045692 0.683864 0.593280 0.046 Uiso 1 1 calc R U . . .
H43B H 0.068153 0.738496 0.590271 0.046 Uiso 1 1 calc R U . . .
C44 C -0.0761(13) 0.3377(7) 0.6539(7) 0.041(3) Uani 1 1 d . . . . .
H44A H -0.117734 0.324392 0.696746 0.049 Uiso 1 1 calc R U . . .
H44B H -0.009589 0.301450 0.648077 0.049 Uiso 1 1 calc R U . . .
C45 C -0.1695(13) 0.3289(10) 0.4676(7) 0.050(4) Uani 1 1 d . . . . .
H45A H -0.232475 0.368355 0.464501 0.060 Uiso 1 1 calc R U . . .
H45B H -0.205353 0.276513 0.468071 0.060 Uiso 1 1 calc R U . . .
C46 C 0.0945(13) 0.5148(7) 0.3583(6) 0.035(3) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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
K15 O50 2.708(9) 2_664 ?
K15 O11 2.735(6) . ?
K15 O7 2.741(8) . ?
K15 O9 2.763(5) . ?
K15 O48 2.765(9) . ?
K15 O5 2.773(8) . ?
K15 O8 2.780(9) . ?
K15 O28 2.87(2) 2_565 ?
K15 O40 2.874(13) 2_565 ?
K15 O52 2.908(12) 2_565 ?
K15 C31 3.388(12) . ?
K15 S4 3.408(3) 2_565 ?
S1 O16 1.458(9) . ?
S1 O18 1.469(9) . ?
S1 O12 1.476(8) . ?
S1 O14 1.482(9) . ?
S3 O21 1.451(10) . ?
S3 O13 1.457(10) . ?
S3 O10 1.457(9) . ?
S3 O6 1.484(9) . ?
S4 O40 1.380(10) . ?
S4 O54 1.43(2) . ?
S4 O2 1.44(2) . ?
S4 O53 1.45(2) . ?
S4 O47 1.454(18) . ?
S4 O52 1.456(11) . ?
S4 O28 1.560(19) . ?
O2 O47 1.02(3) . ?
O2 O28 1.81(4) . ?
O5 C41 1.404(14) . ?
O5 C33 1.442(15) . ?
O7 C46 1.318(14) . ?
O7 C38 1.499(14) . ?
O8 C34 1.390(15) . ?
O8 C17 1.402(13) . ?
O9 C31 1.394(13) . ?
O9 C45 1.468(15) . ?
O11 C43 1.354(14) . ?
O11 C30 1.490(13) . ?
O28 O52 1.27(3) . ?
O47 O53 1.80(4) . ?
O48 C25 1.336(14) . ?
O48 C44 1.439(13) . ?
O52 O54 1.39(2) . ?
O53 O54 1.19(3) . ?
N19 C24 1.441(13) . ?
N20 C35 1.502(13) . ?
N22 C26 1.401(14) . ?
N23 C32 1.535(13) . ?
C17 C25 1.379(16) . ?
C17 C36 1.384(16) . ?
C24 C39 1.349(15) . ?
C24 C32 1.402(13) . ?
C25 C39 1.408(15) . ?
C26 C35 1.346(14) . ?
C26 C42 1.416(14) . ?
C27 C41 1.338(17) . ?
C27 C35 1.426(15) . ?
C27 H27 0.9300 . ?
C30 C38 1.482(17) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C44 1.511(17) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C36 1.374(15) . ?
C33 C45 1.492(17) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C43 1.506(15) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C36 H36 0.9300 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39 0.9300 . ?
C41 C46 1.473(17) . ?
C42 C46 1.359(17) . ?
C42 H42 0.9300 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?

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
O50 K15 O11 77.4(3) 2_664 . ?
O50 K15 O7 79.3(3) 2_664 . ?
O11 K15 O7 63.3(3) . . ?
O50 K15 O9 94.0(3) 2_664 . ?
O11 K15 O9 171.36(17) . . ?
O7 K15 O9 116.6(3) . . ?
O50 K15 O48 85.7(3) 2_664 . ?
O11 K15 O48 116.2(3) . . ?
O7 K15 O48 164.8(3) . . ?
O9 K15 O48 61.4(3) . . ?
O50 K15 O5 86.9(5) 2_664 . ?
O11 K15 O5 119.1(3) . . ?
O7 K15 O5 56.1(2) . . ?
O9 K15 O5 60.6(3) . . ?
O48 K15 O5 120.74(16) . . ?
O50 K15 O8 78.8(5) 2_664 . ?
O11 K15 O8 60.0(3) . . ?
O7 K15 O8 122.19(15) . . ?
O9 K15 O8 117.8(3) . . ?
O48 K15 O8 56.5(3) . . ?
O5 K15 O8 165.6(3) . . ?
O50 K15 O28 158.8(5) 2_664 2_565 ?
O11 K15 O28 114.0(5) . 2_565 ?
O7 K15 O28 121.5(4) . 2_565 ?
O9 K15 O28 73.8(5) . 2_565 ?
O48 K15 O28 73.3(4) . 2_565 ?
O5 K15 O28 101.3(5) . 2_565 ?
O8 K15 O28 91.4(5) . 2_565 ?
O50 K15 O40 153.8(4) 2_664 2_565 ?
O11 K15 O40 90.3(3) . 2_565 ?
O7 K15 O40 74.5(3) . 2_565 ?
O9 K15 O40 98.0(3) . 2_565 ?
O48 K15 O40 120.4(3) . 2_565 ?
O5 K15 O40 79.0(3) . 2_565 ?
O8 K15 O40 115.0(3) . 2_565 ?
O28 K15 O40 47.2(4) 2_565 2_565 ?
O50 K15 O52 152.2(5) 2_664 2_565 ?
O11 K15 O52 89.1(2) . 2_565 ?
O7 K15 O52 116.3(3) . 2_565 ?
O9 K15 O52 98.2(2) . 2_565 ?
O48 K15 O52 78.5(3) . 2_565 ?
O5 K15 O52 120.8(3) . 2_565 ?
O8 K15 O52 73.3(3) . 2_565 ?
O28 K15 O52 25.5(5) 2_565 2_565 ?
O40 K15 O52 47.84(19) 2_565 2_565 ?
O50 K15 C31 104.5(3) 2_664 . ?
O11 K15 C31 158.2(3) . . ?
O7 K15 C31 138.5(3) . . ?
O9 K15 C31 23.5(3) . . ?
O48 K15 C31 43.5(3) . . ?
O5 K15 C31 82.6(3) . . ?
O8 K15 C31 98.8(3) . . ?
O28 K15 C31 58.0(5) 2_565 . ?
O40 K15 C31 95.4(4) 2_565 . ?
O52 K15 C31 79.4(3) 2_565 . ?
O50 K15 S4 171.4(3) 2_664 2_565 ?
O11 K15 S4 93.98(13) . 2_565 ?
O7 K15 S4 96.82(19) . 2_565 ?
O9 K15 S4 94.60(12) . 2_565 ?
O48 K15 S4 98.3(2) . 2_565 ?
O5 K15 S4 97.36(19) . 2_565 ?
O8 K15 S4 97.0(2) . 2_565 ?
O28 K15 S4 27.1(4) 2_565 2_565 ?
O40 K15 S4 23.46(19) 2_565 2_565 ?
O52 K15 S4 25.1(2) 2_565 2_565 ?
C31 K15 S4 83.5(3) . 2_565 ?
O16 S1 O18 110.3(6) . . ?
O16 S1 O12 107.7(5) . . ?
O18 S1 O12 110.8(5) . . ?
O16 S1 O14 109.8(6) . . ?
O18 S1 O14 109.2(6) . . ?
O12 S1 O14 109.0(5) . . ?
O21 S3 O13 109.7(6) . . ?
O21 S3 O10 108.4(7) . . ?
O13 S3 O10 108.4(6) . . ?
O21 S3 O6 111.0(5) . . ?
O13 S3 O6 106.9(6) . . ?
O10 S3 O6 112.3(5) . . ?
O40 S4 O54 122.7(11) . . ?
O40 S4 O2 106.3(14) . . ?
O54 S4 O2 129.5(16) . . ?
O40 S4 O53 99.2(15) . . ?
O54 S4 O53 48.7(15) . . ?
O2 S4 O53 116(2) . . ?
O40 S4 O47 125.8(13) . . ?
O54 S4 O47 95.0(13) . . ?
O2 S4 O47 41.3(12) . . ?
O53 S4 O47 76.4(17) . . ?
O40 S4 O52 111.5(4) . . ?
O54 S4 O52 57.6(10) . . ?
O2 S4 O52 116.8(17) . . ?
O53 S4 O52 105.5(13) . . ?
O47 S4 O52 121.9(13) . . ?
O40 S4 O28 102.7(9) . . ?
O54 S4 O28 104.0(12) . . ?
O2 S4 O28 74.0(19) . . ?
O53 S4 O28 151.9(14) . . ?
O47 S4 O28 104.0(15) . . ?
O52 S4 O28 49.8(10) . . ?
O40 S4 K15 56.0(5) . 2_564 ?
O54 S4 K15 101.6(9) . 2_564 ?
O2 S4 K15 116.2(14) . 2_564 ?
O53 S4 K15 126.5(17) . 2_564 ?
O47 S4 K15 157.1(9) . 2_564 ?
O52 S4 K15 57.9(4) . 2_564 ?
O28 S4 K15 56.9(9) . 2_564 ?
O47 O2 S4 70.1(19) . . ?
O47 O2 O28 111(2) . . ?
S4 O2 O28 56.0(11) . . ?
C41 O5 C33 117.0(9) . . ?
C41 O5 K15 116.9(7) . . ?
C33 O5 K15 116.3(6) . . ?
C46 O7 C38 113.9(9) . . ?
C46 O7 K15 119.1(7) . . ?
C38 O7 K15 114.5(6) . . ?
C34 O8 C17 118.5(9) . . ?
C34 O8 K15 116.4(6) . . ?
C17 O8 K15 115.5(7) . . ?
C31 O9 C45 113.4(6) . . ?
C31 O9 K15 104.3(7) . . ?
C45 O9 K15 107.4(7) . . ?
C43 O11 C30 113.0(5) . . ?
C43 O11 K15 108.3(7) . . ?
C30 O11 K15 104.1(7) . . ?
O52 O28 S4 60.8(10) . . ?
O52 O28 O2 105.0(16) . . ?
S4 O28 O2 50.0(12) . . ?
O52 O28 K15 78.9(13) . 2_564 ?
S4 O28 K15 96.0(10) . 2_564 ?
O2 O28 K15 128.9(13) . 2_564 ?
S4 O40 K15 100.5(6) . 2_564 ?
O2 O47 S4 68.6(16) . . ?
O2 O47 O53 119(2) . . ?
S4 O47 O53 51.8(9) . . ?
C25 O48 C44 116.2(10) . . ?
C25 O48 K15 117.2(7) . . ?
C44 O48 K15 116.8(7) . . ?
O28 O52 O54 124.5(16) . . ?
O28 O52 S4 69.3(10) . . ?
O54 O52 S4 60.4(10) . . ?
O28 O52 K15 75.6(11) . 2_564 ?
O54 O52 K15 130.4(11) . 2_564 ?
S4 O52 K15 97.0(5) . 2_564 ?
O54 O53 S4 64.8(13) . . ?
O54 O53 O47 89(2) . . ?
S4 O53 O47 51.9(13) . . ?
O53 O54 O52 127(2) . . ?
O53 O54 S4 66.5(18) . . ?
O52 O54 S4 62.0(10) . . ?
C25 C17 C36 121.4(10) . . ?
C25 C17 O8 116.6(10) . . ?
C36 C17 O8 121.9(10) . . ?
C39 C24 C32 117.7(10) . . ?
C39 C24 N19 122.3(10) . . ?
C32 C24 N19 119.7(10) . . ?
O48 C25 C17 117.5(10) . . ?
O48 C25 C39 124.8(11) . . ?
C17 C25 C39 117.8(10) . . ?
C35 C26 N22 120.6(9) . . ?
C35 C26 C42 117.8(11) . . ?
N22 C26 C42 121.6(10) . . ?
C41 C27 C35 118.4(10) . . ?
C41 C27 H27 120.8 . . ?
C35 C27 H27 120.8 . . ?
C38 C30 O11 107.2(10) . . ?
C38 C30 K15 86.0(7) . . ?
O11 C30 K15 50.9(5) . . ?
C38 C30 H30A 110.3 . . ?
O11 C30 H30A 110.3 . . ?
K15 C30 H30A 75.7 . . ?
C38 C30 H30B 110.3 . . ?
O11 C30 H30B 110.3 . . ?
K15 C30 H30B 159.4 . . ?
H30A C30 H30B 108.5 . . ?
O9 C31 C44 110.3(11) . . ?
O9 C31 K15 52.2(5) . . ?
C44 C31 K15 87.5(7) . . ?
O9 C31 H31A 109.6 . . ?
C44 C31 H31A 109.6 . . ?
K15 C31 H31A 159.6 . . ?
O9 C31 H31B 109.6 . . ?
C44 C31 H31B 109.6 . . ?
K15 C31 H31B 74.8 . . ?
H31A C31 H31B 108.1 . . ?
C36 C32 C24 122.0(10) . . ?
C36 C32 N23 116.8(9) . . ?
C24 C32 N23 121.2(10) . . ?
O5 C33 C45 110.2(11) . . ?
O5 C33 H33A 109.6 . . ?
C45 C33 H33A 109.6 . . ?
O5 C33 H33B 109.6 . . ?
C45 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
O8 C34 C43 109.1(11) . . ?
O8 C34 H34A 109.9 . . ?
C43 C34 H34A 109.9 . . ?
O8 C34 H34B 109.9 . . ?
C43 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
C26 C35 C27 122.4(10) . . ?
C26 C35 N20 121.3(10) . . ?
C27 C35 N20 116.3(9) . . ?
C32 C36 C17 118.5(10) . . ?
C32 C36 H36 120.8 . . ?
C17 C36 H36 120.8 . . ?
C30 C38 O7 107.2(10) . . ?
C30 C38 H38A 110.3 . . ?
O7 C38 H38A 110.3 . . ?
C30 C38 H38B 110.3 . . ?
O7 C38 H38B 110.3 . . ?
H38A C38 H38B 108.5 . . ?
C24 C39 C25 122.5(11) . . ?
C24 C39 H39 118.7 . . ?
C25 C39 H39 118.7 . . ?
C27 C41 O5 125.1(11) . . ?
C27 C41 C46 122.1(11) . . ?
O5 C41 C46 112.8(11) . . ?
C46 C42 C26 123.6(11) . . ?
C46 C42 H42 118.2 . . ?
C26 C42 H42 118.2 . . ?
O11 C43 C34 108.4(9) . . ?
O11 C43 K15 49.5(5) . . ?
C34 C43 K15 85.5(7) . . ?
O11 C43 H43A 110.0 . . ?
C34 C43 H43A 110.0 . . ?
K15 C43 H43A 78.2 . . ?
O11 C43 H43B 110.0 . . ?
C34 C43 H43B 110.0 . . ?
K15 C43 H43B 158.6 . . ?
H43A C43 H43B 108.4 . . ?
O48 C44 C31 105.8(10) . . ?
O48 C44 H44A 110.6 . . ?
C31 C44 H44A 110.6 . . ?
O48 C44 H44B 110.6 . . ?
C31 C44 H44B 110.6 . . ?
H44A C44 H44B 108.7 . . ?
O9 C45 C33 104.6(10) . . ?
O9 C45 K15 49.0(5) . . ?
C33 C45 K15 83.8(8) . . ?
O9 C45 H45A 110.8 . . ?
C33 C45 H45A 110.8 . . ?
K15 C45 H45A 78.1 . . ?
O9 C45 H45B 110.8 . . ?
C33 C45 H45B 110.8 . . ?
K15 C45 H45B 158.8 . . ?
H45A C45 H45B 108.9 . . ?
O7 C46 C42 128.5(11) . . ?
O7 C46 C41 115.7(11) . . ?
C42 C46 C41 115.6(11) . . ?

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
O40 S4 O2 O47 -126(3) . . . . ?
O54 S4 O2 O47 40(4) . . . . ?
O53 S4 O2 O47 -17(4) . . . . ?
O52 S4 O2 O47 109(3) . . . . ?
O28 S4 O2 O47 135(3) . . . . ?
K15 S4 O2 O47 174(2) 2_564 . . . ?
O40 S4 O2 O28 98.8(11) . . . . ?
O54 S4 O2 O28 -95.1(19) . . . . ?
O53 S4 O2 O28 -151.9(16) . . . . ?
O47 S4 O2 O28 -135(3) . . . . ?
O52 S4 O2 O28 -26.3(13) . . . . ?
K15 S4 O2 O28 39.2(13) 2_564 . . . ?
O40 S4 O28 O52 107.5(8) . . . . ?
O54 S4 O28 O52 -21.2(14) . . . . ?
O2 S4 O28 O52 -148.8(17) . . . . ?
O53 S4 O28 O52 -33(4) . . . . ?
O47 S4 O28 O52 -120.1(14) . . . . ?
K15 S4 O28 O52 73.7(11) 2_564 . . . ?
O40 S4 O28 O2 -103.6(15) . . . . ?
O54 S4 O28 O2 127.7(17) . . . . ?
O53 S4 O28 O2 116(4) . . . . ?
O47 S4 O28 O2 28.8(16) . . . . ?
O52 S4 O28 O2 148.8(17) . . . . ?
K15 S4 O28 O2 -137.4(15) 2_564 . . . ?
O40 S4 O28 K15 33.8(10) . . . 2_564 ?
O54 S4 O28 K15 -94.9(11) . . . 2_564 ?
O2 S4 O28 K15 137.4(15) . . . 2_564 ?
O53 S4 O28 K15 -107(4) . . . 2_564 ?
O47 S4 O28 K15 166.2(11) . . . 2_564 ?
O52 S4 O28 K15 -73.7(11) . . . 2_564 ?
O47 O2 O28 O52 -18(4) . . . . ?
S4 O2 O28 O52 27.9(14) . . . . ?
O47 O2 O28 S4 -45(3) . . . . ?
O47 O2 O28 K15 -105(3) . . . 2_564 ?
S4 O2 O28 K15 -59.9(18) . . . 2_564 ?
O54 S4 O40 K15 81.7(13) . . . 2_564 ?
O2 S4 O40 K15 -111.0(17) . . . 2_564 ?
O53 S4 O40 K15 128.1(15) . . . 2_564 ?
O47 S4 O40 K15 -152.1(11) . . . 2_564 ?
O52 S4 O40 K15 17.3(6) . . . 2_564 ?
O28 S4 O40 K15 -34.2(12) . . . 2_564 ?
O28 O2 O47 S4 39(2) . . . . ?
S4 O2 O47 O53 14(3) . . . . ?
O28 O2 O47 O53 53(4) . . . . ?
O40 S4 O47 O2 73(3) . . . . ?
O54 S4 O47 O2 -150(3) . . . . ?
O53 S4 O47 O2 164(3) . . . . ?
O52 S4 O47 O2 -96(3) . . . . ?
O28 S4 O47 O2 -44(3) . . . . ?
K15 S4 O47 O2 -13(5) 2_564 . . . ?
O40 S4 O47 O53 -91.6(15) . . . . ?
O54 S4 O47 O53 45.3(16) . . . . ?
O2 S4 O47 O53 -164(3) . . . . ?
O52 S4 O47 O53 100.0(14) . . . . ?
O28 S4 O47 O53 151.1(15) . . . . ?
K15 S4 O47 O53 -178(3) 2_564 . . . ?
S4 O28 O52 O54 26.0(15) . . . . ?
O2 O28 O52 O54 2(2) . . . . ?
K15 O28 O52 O54 129.4(15) 2_564 . . . ?
O2 O28 O52 S4 -24.2(12) . . . . ?
K15 O28 O52 S4 103.4(5) 2_564 . . . ?
S4 O28 O52 K15 -103.4(5) . . . 2_564 ?
O2 O28 O52 K15 -127.6(14) . . . 2_564 ?
O40 S4 O52 O28 -88.6(12) . . . . ?
O54 S4 O52 O28 155.5(16) . . . . ?
O2 S4 O52 O28 33.9(18) . . . . ?
O53 S4 O52 O28 164.7(19) . . . . ?
O47 S4 O52 O28 81.3(15) . . . . ?
K15 S4 O52 O28 -71.7(11) 2_564 . . . ?
O40 S4 O52 O54 115.9(13) . . . . ?
O2 S4 O52 O54 -121.6(19) . . . . ?
O53 S4 O52 O54 9(2) . . . . ?
O47 S4 O52 O54 -74.2(15) . . . . ?
O28 S4 O52 O54 -155.5(16) . . . . ?
K15 S4 O52 O54 132.9(12) 2_564 . . . ?
O40 S4 O52 K15 -17.0(6) . . . 2_564 ?
O54 S4 O52 K15 -132.9(12) . . . 2_564 ?
O2 S4 O52 K15 105.5(15) . . . 2_564 ?
O53 S4 O52 K15 -123.7(17) . . . 2_564 ?
O47 S4 O52 K15 153.0(10) . . . 2_564 ?
O28 S4 O52 K15 71.7(11) . . . 2_564 ?
O40 S4 O53 O54 -125.8(19) . . . . ?
O2 S4 O53 O54 121(2) . . . . ?
O47 S4 O53 O54 109(2) . . . . ?
O52 S4 O53 O54 -10(2) . . . . ?
O28 S4 O53 O54 15(5) . . . . ?
K15 S4 O53 O54 -72(2) 2_564 . . . ?
O40 S4 O53 O47 124.8(14) . . . . ?
O54 S4 O53 O47 -109(2) . . . . ?
O2 S4 O53 O47 11(2) . . . . ?
O52 S4 O53 O47 -119.8(14) . . . . ?
O28 S4 O53 O47 -94(4) . . . . ?
K15 S4 O53 O47 179.0(14) 2_564 . . . ?
O2 O47 O53 O54 -75(4) . . . . ?
S4 O47 O53 O54 -58.6(16) . . . . ?
O2 O47 O53 S4 -16(3) . . . . ?
S4 O53 O54 O52 13(3) . . . . ?
O47 O53 O54 O52 61(3) . . . . ?
O47 O53 O54 S4 47.9(11) . . . . ?
O28 O52 O54 O53 -42(4) . . . . ?
S4 O52 O54 O53 -14(3) . . . . ?
K15 O52 O54 O53 59(4) 2_564 . . . ?
O28 O52 O54 S4 -28.1(16) . . . . ?
K15 O52 O54 S4 72.7(13) 2_564 . . . ?
O40 S4 O54 O53 72(3) . . . . ?
O2 S4 O54 O53 -92(3) . . . . ?
O47 S4 O54 O53 -67(3) . . . . ?
O52 S4 O54 O53 168(3) . . . . ?
O28 S4 O54 O53 -173(2) . . . . ?
K15 S4 O54 O53 129(2) 2_564 . . . ?
O40 S4 O54 O52 -96.2(10) . . . . ?
O2 S4 O54 O52 100(2) . . . . ?
O53 S4 O54 O52 -168(3) . . . . ?
O47 S4 O54 O52 124.9(14) . . . . ?
O28 S4 O54 O52 19.1(13) . . . . ?
K15 S4 O54 O52 -39.3(9) 2_564 . . . ?
C34 O8 C17 C25 -174.8(10) . . . . ?
K15 O8 C17 C25 -29.8(11) . . . . ?
C34 O8 C17 C36 1.6(15) . . . . ?
K15 O8 C17 C36 146.6(9) . . . . ?
C44 O48 C25 C17 179.5(10) . . . . ?
K15 O48 C25 C17 34.5(13) . . . . ?
C44 O48 C25 C39 -1.1(17) . . . . ?
K15 O48 C25 C39 -146.1(9) . . . . ?
C36 C17 C25 O48 -179.0(10) . . . . ?
O8 C17 C25 O48 -2.6(15) . . . . ?
C36 C17 C25 C39 1.6(16) . . . . ?
O8 C17 C25 C39 178.0(9) . . . . ?
C43 O11 C30 C38 172.9(13) . . . . ?
K15 O11 C30 C38 -69.8(11) . . . . ?
C43 O11 C30 K15 -117.3(8) . . . . ?
C45 O9 C31 C44 173.7(13) . . . . ?
K15 O9 C31 C44 -69.7(11) . . . . ?
C45 O9 C31 K15 -116.5(7) . . . . ?
C39 C24 C32 C36 -0.7(16) . . . . ?
N19 C24 C32 C36 173.9(10) . . . . ?
C39 C24 C32 N23 179.6(10) . . . . ?
N19 C24 C32 N23 -5.8(15) . . . . ?
C41 O5 C33 C45 174.1(11) . . . . ?
K15 O5 C33 C45 29.3(13) . . . . ?
C17 O8 C34 C43 171.6(9) . . . . ?
K15 O8 C34 C43 26.9(11) . . . . ?
N22 C26 C35 C27 178.7(10) . . . . ?
C42 C26 C35 C27 -0.6(16) . . . . ?
N22 C26 C35 N20 -2.9(15) . . . . ?
C42 C26 C35 N20 177.8(9) . . . . ?
C41 C27 C35 C26 -1.6(17) . . . . ?
C41 C27 C35 N20 180.0(10) . . . . ?
C24 C32 C36 C17 3.8(17) . . . . ?
N23 C32 C36 C17 -176.5(10) . . . . ?
C25 C17 C36 C32 -4.2(17) . . . . ?
O8 C17 C36 C32 179.5(10) . . . . ?
O11 C30 C38 O7 69.6(13) . . . . ?
K15 C30 C38 O7 22.7(8) . . . . ?
C46 O7 C38 C30 -173.7(10) . . . . ?
K15 O7 C38 C30 -31.8(12) . . . . ?
C32 C24 C39 C25 -2.1(17) . . . . ?
N19 C24 C39 C25 -176.6(11) . . . . ?
O48 C25 C39 C24 -177.7(11) . . . . ?
C17 C25 C39 C24 1.7(17) . . . . ?
C35 C27 C41 O5 -179.8(10) . . . . ?
C35 C27 C41 C46 0.2(17) . . . . ?
C33 O5 C41 C27 2.6(17) . . . . ?
K15 O5 C41 C27 147.1(10) . . . . ?
C33 O5 C41 C46 -177.5(10) . . . . ?
K15 O5 C41 C46 -32.9(12) . . . . ?
C35 C26 C42 C46 4.4(16) . . . . ?
N22 C26 C42 C46 -174.9(11) . . . . ?
C30 O11 C43 C34 -178.3(12) . . . . ?
K15 O11 C43 C34 66.9(11) . . . . ?
C30 O11 C43 K15 114.8(7) . . . . ?
O8 C34 C43 O11 -63.9(13) . . . . ?
O8 C34 C43 K15 -19.3(8) . . . . ?
C25 O48 C44 C31 -173.4(11) . . . . ?
K15 O48 C44 C31 -28.3(13) . . . . ?
O9 C31 C44 O48 68.1(14) . . . . ?
K15 C31 C44 O48 20.2(9) . . . . ?
C31 O9 C45 C33 -177.3(13) . . . . ?
K15 O9 C45 C33 68.0(11) . . . . ?
C31 O9 C45 K15 114.7(7) . . . . ?
O5 C33 C45 O9 -65.2(14) . . . . ?
O5 C33 C45 K15 -20.5(9) . . . . ?
C38 O7 C46 C42 -9.0(17) . . . . ?
K15 O7 C46 C42 -149.0(10) . . . . ?
C38 O7 C46 C41 176.2(10) . . . . ?
K15 O7 C46 C41 36.2(13) . . . . ?
C26 C42 C46 O7 179.6(11) . . . . ?
C26 C42 C46 C41 -5.5(17) . . . . ?
C27 C41 C46 O7 178.7(11) . . . . ?
O5 C41 C46 O7 -1.3(15) . . . . ?
C27 C41 C46 C42 3.2(18) . . . . ?
O5 C41 C46 C42 -176.8(10) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_210616
_database_code_depnum_ccdc_archive 'CCDC 2168846'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Akutagawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_SHFSU01_210616              
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: This is due to the disordered H2O guests
;
_vrf_PLAT043_210616              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..    1502.71 Check
RESPONSE: This is due to the disordered H2O guests
;
_vrf_PLAT051_210616              
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      95.96 %
RESPONSE: This is due to the disordered H2O guests
;
_vrf_PLAT080_210616              
;
PROBLEM: Maximum Shift/Error ............................       0.55 Why ?
RESPONSE: This is due to the disordered H2O guests
;
_vrf_PLAT430_210616              
;
PROBLEM: Short Inter D...A Contact  O7       ..O100     .       2.16 Ang.
RESPONSE: This is due to the disordered H2O guests
;
# Added during the CSD deposition process: Tuesday 26 April 2022 05:29 AM
# end Validation Reply Form


#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C40 H88 N8 Na Ne0.5 O46 S6'
_chemical_formula_moiety         'C40 H88 N8 Na Ne0.5 O46 S6'
_chemical_formula_weight         1642.60
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
_space_group_IT_number           29
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,1/2+Z
3 1/2-X,+Y,1/2+Z
4 1/2+X,-Y,+Z
#------------------------------------------------------------------------------
_cell_length_a                   34.7439(9)
_cell_length_b                   8.1437(2)
_cell_length_c                   23.0281(6)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     6515.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    35594
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      68.11
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    0.837
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728.00
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_T_max  0.857

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            71878
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_theta_max         68.229
_diffrn_reflns_theta_min         3.187
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             11887
_reflns_number_gt                7407
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.998

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0861
_refine_ls_wR_factor_ref         0.2615
_refine_ls_wR_factor_gt          0.2255
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         11887
_refine_ls_number_parameters     910
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1512P)²+2.2430P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.547
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 2447 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.065(16)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.3331 0.5567
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Na Na 0.1353 0.1239
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ne Ne 0.1019 0.0833
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.58814(9) 0.2983(4) 0.85504(15) 0.0491(8) Uani 1 1 d . . . . .
S2 S 0.35158(9) 1.2765(4) 0.44727(15) 0.0501(8) Uani 1 1 d . . . . .
S3 S 0.46841(13) 0.2133(5) 0.61728(17) 0.0661(10) Uani 1 1 d . . . . .
S4 S 0.69511(14) 1.2135(5) 0.68614(17) 0.0684(11) Uani 1 1 d . . . . .
S5 S 0.37476(12) -0.2126(6) 0.58667(18) 0.0741(12) Uani 1 1 d . . . . .
S6 S 0.61191(13) 0.8230(6) 0.71333(18) 0.0783(13) Uani 1 1 d . . . . .
Na39 Na 0.6309(5) 1.3687(17) 0.3932(9) 0.105(5) Uani 0.5 1 d . . P . .
O7 O 0.6317(2) 0.8631(7) 0.3950(4) 0.0304(14) Uani 1 1 d . . . . .
O8 O 0.5666(2) 1.3417(10) 0.4519(4) 0.046(2) Uani 1 1 d . . . . .
O9 O 0.6641(2) 0.8882(9) 0.4978(4) 0.0418(19) Uani 1 1 d . . . . .
O10 O 0.5845(2) 0.9105(10) 0.4960(4) 0.0452(19) Uani 1 1 d . . . . .
O11 O 0.7040(2) 1.4051(10) 0.4509(4) 0.045(2) Uani 1 1 d . . . . .
O12 O 0.5977(2) 0.8640(10) 0.2939(4) 0.0426(19) Uani 1 1 d . . . . .
O13 O 0.7061(2) 0.8365(10) 0.3960(4) 0.044(2) Uani 1 1 d . . . . .
O14 O 0.5553(2) 0.8315(10) 0.3979(4) 0.046(2) Uani 1 1 d . . . . .
O15 O 0.6357(2) 1.3903(10) 0.5155(4) 0.047(2) Uani 1 1 d . . . . .
O16 O 0.6273(2) 1.3690(10) 0.2784(4) 0.0400(19) Uani 1 1 d . . . . .
O17 O 0.6973(2) 1.3474(10) 0.3407(4) 0.043(2) Uani 1 1 d . . . . .
O18 O 0.6770(2) 0.8910(10) 0.2957(3) 0.0404(19) Uani 1 1 d . . . . .
O19 O 0.6946(3) 1.3523(10) 0.7257(4) 0.064(3) Uani 1 1 d . . . . .
O20 O 0.5590(2) 1.3830(10) 0.3407(4) 0.045(2) Uani 1 1 d . . . . .
O21 O 0.3874(2) 1.3032(11) 0.4799(4) 0.053(2) Uani 1 1 d . . . . .
O22 O 0.5965(2) 0.1929(10) 0.9059(4) 0.050(2) Uani 1 1 d . . . . .
O23 O 0.3612(2) 1.1772(9) 0.3947(4) 0.049(2) Uani 1 1 d . . . . .
O24 O 0.5716(2) 0.4546(11) 0.8741(4) 0.056(2) Uani 1 1 d . . . . .
O25 O 0.3346(2) 1.4318(10) 0.4294(4) 0.052(2) Uani 1 1 d . . . . .
O26 O 0.6236(2) 0.3234(11) 0.8212(4) 0.053(2) Uani 1 1 d . . . . .
O27 O 0.5601(2) 0.2069(11) 0.8187(4) 0.056(2) Uani 1 1 d . . . . .
O28 O 0.7025(3) 1.0618(10) 0.7167(4) 0.060(2) Uani 1 1 d . . . . .
O29 O 0.6320(3) 0.7293(18) 0.6703(5) 0.089(4) Uani 1 1 d . . . . .
O31 O 0.6321(3) 1.5973(14) 0.3929(5) 0.075(3) Uani 1 1 d . . . . .
O32 O 0.4627(3) 0.0636(12) 0.5839(5) 0.078(3) Uani 1 1 d . . . . .
O34 O 0.5375(5) 0.3720(19) 0.7267(7) 0.138(6) Uani 1 1 d . . . . .
O35 O 0.3238(3) 1.1803(11) 0.4815(4) 0.059(2) Uani 1 1 d . . . . .
O36 O 0.6352(3) 0.8432(13) 0.7664(4) 0.064(3) Uani 1 1 d . . . . .
O38 O 0.3977(3) -0.1731(13) 0.5364(5) 0.068(3) Uani 1 1 d . . . . .
O46 O 0.7149(9) 0.503(6) 0.1138(17) 0.44(3) Uani 1 1 d . . . . .
O49 O 0.7231(4) 1.0331(19) 0.1031(10) 0.151(7) Uani 1 1 d . . . . .
O63 O 0.3388(4) -0.287(2) 0.5674(7) 0.120(5) Uani 1 1 d . . . . .
O64 O 0.6556(5) 1.2049(15) 0.6588(6) 0.113(5) Uani 1 1 d . . . . .
O71 O 0.4717(4) 0.3525(12) 0.5804(5) 0.089(4) Uani 1 1 d . . . . .
O74 O 0.5741(3) 0.751(2) 0.7297(6) 0.112(5) Uani 1 1 d . . . . .
O83 O 0.6016(4) 0.9864(18) 0.6900(6) 0.124(5) Uani 1 1 d . . . . .
O88 O 0.3607(6) -0.066(3) 0.6160(7) 0.173(9) Uani 1 1 d . . . . .
O92 O 0.7176(6) 1.2369(19) 0.6375(6) 0.142(7) Uani 1 1 d . . . . .
O93 O 0.4358(6) 0.243(2) 0.6543(7) 0.152(7) Uani 1 1 d . . . . .
O94 O 0.5962(6) 0.431(3) 0.6705(10) 0.181(8) Uani 1 1 d . . . . .
O95 O 0.3967(3) -0.312(3) 0.6246(7) 0.159(9) Uani 1 1 d . . . . .
O96 O 0.3715(6) 0.277(5) 0.6072(11) 0.250(15) Uani 1 1 d . . . . .
O97 O 0.4986(6) 0.192(2) 0.6584(8) 0.157(8) Uani 1 1 d . . . . .
O99 O 0.5046(3) 0.8593(13) 0.6917(4) 0.068(3) Uani 1 1 d . . . . .
O100 O 0.6296(3) 1.1285(13) 0.3946(5) 0.072(3) Uani 1 1 d . . . . .
O101 O 0.7495(4) 0.7280(16) 0.0994(5) 0.088(4) Uani 1 1 d . . . . .
N30 N 0.4744(3) 0.6855(14) 0.6030(5) 0.058(3) Uani 1 1 d . . . . .
N33 N 0.8317(3) 1.1534(14) 0.4570(5) 0.052(3) Uani 1 1 d . . . . .
N37 N 0.8238(3) 1.0804(14) 0.3334(5) 0.050(3) Uani 1 1 d . . . . .
N40 N 0.7905(3) 0.6721(13) 0.1982(4) 0.052(3) Uani 1 1 d . . . . .
N41 N 0.4415(3) 1.0718(13) 0.4657(4) 0.048(3) Uani 1 1 d . . . . .
N42 N 0.4319(3) 1.1312(13) 0.3419(5) 0.051(3) Uani 1 1 d . . . . .
N43 N 0.4431(3) 0.5739(13) 0.4907(5) 0.051(3) Uani 1 1 d . . . . .
N44 N 0.8213(3) 0.5887(13) 0.3103(5) 0.047(3) Uani 1 1 d . . . . .
C45 C 0.5340(3) 0.7859(14) 0.4443(5) 0.040(3) Uani 1 1 d . . . . .
C47 C 0.7122(3) 0.8205(14) 0.2952(5) 0.037(3) Uani 1 1 d . . . . .
C48 C 0.7637(4) 0.7096(14) 0.3548(6) 0.043(3) Uani 1 1 d . . . . .
H48 H 0.773918 0.686941 0.391234 0.052 Uiso 1 1 calc R U . . .
C50 C 0.7927(3) 1.1634(15) 0.3677(6) 0.043(3) Uani 1 1 d . . . . .
C51 C 0.5047(4) 1.2028(14) 0.4582(6) 0.045(3) Uani 1 1 d . . . . .
H51 H 0.507862 1.183545 0.497686 0.054 Uiso 1 1 calc R U . . .
C52 C 0.5502(3) 0.8323(13) 0.4987(5) 0.038(3) Uani 1 1 d . . . . .
C53 C 0.7837(3) 0.6684(14) 0.3041(5) 0.041(3) Uani 1 1 d . . . . .
C54 C 0.6674(3) 1.4935(14) 0.5333(6) 0.043(3) Uani 1 1 d . . . . .
H54A H 0.667464 1.506205 0.575201 0.052 Uiso 1 1 calc R U . . .
H54B H 0.665161 1.601368 0.515762 0.052 Uiso 1 1 calc R U . . .
C55 C 0.5585(3) 0.9182(16) 0.3004(6) 0.048(3) Uani 1 1 d . . . . .
H55A H 0.545745 0.916405 0.262965 0.057 Uiso 1 1 calc R U . . .
H55B H 0.558191 1.030126 0.314768 0.057 Uiso 1 1 calc R U . . .
C56 C 0.7246(3) 0.8414(15) 0.4516(5) 0.045(3) Uani 1 1 d . . . . .
H56A H 0.750661 0.882243 0.447760 0.053 Uiso 1 1 calc R U . . .
H56B H 0.725541 0.732251 0.468386 0.053 Uiso 1 1 calc R U . . .
C57 C 0.5581(3) 1.3873(16) 0.2783(5) 0.043(3) Uani 1 1 d . . . . .
H57A H 0.536565 1.453001 0.265054 0.052 Uiso 1 1 calc R U . . .
H57B H 0.555303 1.277117 0.262930 0.052 Uiso 1 1 calc R U . . .
C58 C 0.5303(3) 0.7943(14) 0.5496(6) 0.045(3) Uani 1 1 d . . . . .
H58 H 0.541038 0.820789 0.585386 0.054 Uiso 1 1 calc R U . . .
C59 C 0.7593(3) 1.2077(14) 0.3368(6) 0.044(3) Uani 1 1 d . . . . .
H59 H 0.756831 1.182318 0.297630 0.053 Uiso 1 1 calc R U . . .
C60 C 0.6437(3) 0.9982(15) 0.5374(6) 0.045(3) Uani 1 1 d . . . . .
H60A H 0.640494 1.105379 0.519644 0.055 Uiso 1 1 calc R U . . .
H60B H 0.658133 1.011403 0.573126 0.055 Uiso 1 1 calc R U . . .
C61 C 0.6565(3) 0.8992(14) 0.2420(5) 0.041(3) Uani 1 1 d . . . . .
H61A H 0.654148 0.790533 0.225120 0.049 Uiso 1 1 calc R U . . .
H61B H 0.670042 0.969222 0.214714 0.049 Uiso 1 1 calc R U . . .
C62 C 0.5289(4) 1.3075(14) 0.3679(6) 0.042(3) Uani 1 1 d . . . . .
C65 C 0.7691(3) 0.7078(16) 0.2515(6) 0.045(3) Uani 1 1 d . . . . .
C66 C 0.6001(3) 1.4732(16) 0.5283(6) 0.048(3) Uani 1 1 d . . . . .
H66A H 0.598091 1.572858 0.505422 0.058 Uiso 1 1 calc R U . . .
H66B H 0.599223 1.502837 0.569075 0.058 Uiso 1 1 calc R U . . .
C67 C 0.5335(3) 1.2829(14) 0.4279(5) 0.039(3) Uani 1 1 d . . . . .
C68 C 0.7680(4) 1.2769(15) 0.4541(6) 0.047(3) Uani 1 1 d . . . . .
H68 H 0.770663 1.296077 0.493730 0.057 Uiso 1 1 calc R U . . .
C69 C 0.5949(3) 1.4606(14) 0.2581(5) 0.041(3) Uani 1 1 d . . . . .
H69A H 0.595158 1.463435 0.216032 0.049 Uiso 1 1 calc R U . . .
H69B H 0.596736 1.572630 0.272128 0.049 Uiso 1 1 calc R U . . .
C70 C 0.7969(4) 1.2010(15) 0.4243(6) 0.046(3) Uani 1 1 d . . . . .
C72 C 0.6957(4) 1.3351(16) 0.2783(5) 0.045(3) Uani 1 1 d . . . . .
H72A H 0.691840 1.221898 0.266612 0.054 Uiso 1 1 calc R U . . .
H72B H 0.719527 1.374302 0.261237 0.054 Uiso 1 1 calc R U . . .
C73 C 0.4804(3) 0.6658(15) 0.4948(5) 0.043(3) Uani 1 1 d . . . . .
C75 C 0.6053(3) 0.9235(15) 0.5498(5) 0.042(3) Uani 1 1 d . . . . .
H75A H 0.608614 0.815636 0.566906 0.051 Uiso 1 1 calc R U . . .
H75B H 0.591201 0.991700 0.576929 0.051 Uiso 1 1 calc R U . . .
C76 C 0.7018(3) 0.9518(15) 0.4889(5) 0.043(3) Uani 1 1 d . . . . .
H76A H 0.714615 0.964477 0.526103 0.051 Uiso 1 1 calc R U . . .
H76B H 0.700091 1.059212 0.470912 0.051 Uiso 1 1 calc R U . . .
C77 C 0.6627(3) 1.4389(16) 0.2587(6) 0.044(3) Uani 1 1 d . . . . .
H77A H 0.665410 1.549050 0.274160 0.053 Uiso 1 1 calc R U . . .
H77B H 0.662580 1.445866 0.216662 0.053 Uiso 1 1 calc R U . . .
C78 C 0.4714(3) 1.1507(14) 0.4315(5) 0.039(3) Uani 1 1 d . . . . .
C79 C 0.6171(3) 0.9691(14) 0.2551(5) 0.040(3) Uani 1 1 d . . . . .
H79A H 0.619735 1.077278 0.272300 0.049 Uiso 1 1 calc R U . . .
H79B H 0.602484 0.979671 0.219470 0.049 Uiso 1 1 calc R U . . .
C80 C 0.7036(3) 1.4111(16) 0.5136(5) 0.044(3) Uani 1 1 d . . . . .
H80A H 0.725786 1.471646 0.527538 0.053 Uiso 1 1 calc R U . . .
H80B H 0.704806 1.300627 0.529278 0.053 Uiso 1 1 calc R U . . .
C81 C 0.4949(4) 0.7179(15) 0.5475(6) 0.048(3) Uani 1 1 d . . . . .
C82 C 0.4664(3) 1.1803(14) 0.3745(6) 0.044(3) Uani 1 1 d . . . . .
C84 C 0.5679(4) 1.3610(16) 0.5142(6) 0.047(3) Uani 1 1 d . . . . .
H84A H 0.571819 1.255348 0.532656 0.057 Uiso 1 1 calc R U . . .
H84B H 0.543778 1.406572 0.528105 0.057 Uiso 1 1 calc R U . . .
C85 C 0.5377(3) 0.8097(15) 0.3416(5) 0.042(3) Uani 1 1 d . . . . .
H85A H 0.510700 0.839145 0.343008 0.051 Uiso 1 1 calc R U . . .
H85B H 0.539813 0.696055 0.329342 0.051 Uiso 1 1 calc R U . . .
C86 C 0.7276(3) 0.7864(15) 0.3489(6) 0.043(3) Uani 1 1 d . . . . .
C87 C 0.4956(3) 1.2558(15) 0.3398(6) 0.046(3) Uani 1 1 d . . . . .
H87 H 0.492519 1.269621 0.299963 0.055 Uiso 1 1 calc R U . . .
C89 C 0.4999(3) 0.6981(13) 0.4428(6) 0.040(3) Uani 1 1 d . . . . .
H89 H 0.490114 0.660742 0.407636 0.048 Uiso 1 1 calc R U . . .
C90 C 0.7328(4) 0.7838(16) 0.2456(6) 0.048(3) Uani 1 1 d . . . . .
H90 H 0.723040 0.808641 0.209070 0.058 Uiso 1 1 calc R U . . .
C91 C 0.7338(3) 1.3267(15) 0.4250(6) 0.043(3) Uani 1 1 d . . . . .
C98 C 0.7298(4) 1.2906(15) 0.3661(6) 0.046(3) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O24 1.465(9) . ?
S1 O26 1.470(9) . ?
S1 O22 1.480(9) . ?
S1 O27 1.485(9) . ?
S2 O25 1.454(9) . ?
S2 O21 1.468(9) . ?
S2 O35 1.472(9) . ?
S2 O23 1.494(9) . ?
S3 O71 1.422(11) . ?
S3 O97 1.424(14) . ?
S3 O93 1.441(15) . ?
S3 O32 1.454(11) . ?
S4 O92 1.378(14) . ?
S4 O28 1.445(9) . ?
S4 O19 1.452(9) . ?
S4 O64 1.513(15) . ?
S5 O95 1.413(13) . ?
S5 O38 1.442(11) . ?
S5 O88 1.453(16) . ?
S5 O63 1.457(14) . ?
S6 O29 1.432(12) . ?
S6 O36 1.476(10) . ?
S6 O83 1.480(13) . ?
S6 O74 1.489(14) . ?
Na39 O31 1.862(18) . ?
Na39 O100 1.957(17) . ?
Na39 O17 2.611(18) . ?
Na39 O8 2.621(19) . ?
Na39 O16 2.65(2) . ?
Na39 O20 2.78(2) . ?
Na39 O15 2.83(2) . ?
Na39 O11 2.88(2) . ?
O8 C67 1.363(13) . ?
O8 C84 1.443(15) . ?
O9 C76 1.422(12) . ?
O9 C60 1.462(13) . ?
O10 C52 1.353(14) . ?
O10 C75 1.439(14) . ?
O11 C91 1.356(14) . ?
O11 C80 1.446(15) . ?
O12 C79 1.408(13) . ?
O12 C55 1.439(13) . ?
O13 C86 1.378(15) . ?
O13 C56 1.433(14) . ?
O14 C45 1.350(14) . ?
O14 C85 1.445(14) . ?
O15 C66 1.439(13) . ?
O15 C54 1.446(13) . ?
O16 C69 1.428(13) . ?
O16 C77 1.429(13) . ?
O17 C98 1.351(15) . ?
O17 C72 1.442(15) . ?
O18 C47 1.350(13) . ?
O18 C61 1.429(14) . ?
O20 C62 1.367(14) . ?
O20 C57 1.436(15) . ?
N30 C81 1.487(17) . ?
N33 C70 1.478(16) . ?
N37 C50 1.499(15) . ?
N40 C65 1.465(16) . ?
N41 C78 1.455(14) . ?
N42 C82 1.470(15) . ?
N43 C73 1.497(15) . ?
N44 C53 1.465(15) . ?
C45 C89 1.383(16) . ?
C45 C52 1.424(17) . ?
C47 C86 1.377(17) . ?
C47 C90 1.380(16) . ?
C48 C53 1.400(17) . ?
C48 C86 1.407(17) . ?
C48 H48 0.9300 . ?
C50 C70 1.347(18) . ?
C50 C59 1.408(16) . ?
C51 C78 1.376(17) . ?
C51 C67 1.383(17) . ?
C51 H51 0.9300 . ?
C52 C58 1.396(17) . ?
C53 C65 1.352(17) . ?
C54 C80 1.496(15) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C85 1.483(17) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 C76 1.473(16) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 C69 1.484(16) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 C81 1.380(17) . ?
C58 H58 0.9300 . ?
C59 C98 1.400(17) . ?
C59 H59 0.9300 . ?
C60 C75 1.492(16) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 C79 1.513(16) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 C87 1.390(17) . ?
C62 C67 1.406(17) . ?
C65 C90 1.409(17) . ?
C66 C84 1.481(16) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C68 C70 1.364(18) . ?
C68 C91 1.422(17) . ?
C68 H68 0.9300 . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C72 C77 1.495(15) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C73 C81 1.380(18) . ?
C73 C89 1.402(17) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C78 C82 1.345(17) . ?
C79 H79A 0.9700 . ?
C79 H79B 0.9700 . ?
C80 H80A 0.9700 . ?
C80 H80B 0.9700 . ?
C82 C87 1.432(17) . ?
C84 H84A 0.9700 . ?
C84 H84B 0.9700 . ?
C85 H85A 0.9700 . ?
C85 H85B 0.9700 . ?
C87 H87 0.9300 . ?
C89 H89 0.9300 . ?
C90 H90 0.9300 . ?
C91 C98 1.397(18) . ?

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
O24 S1 O26 111.5(6) . . ?
O24 S1 O22 110.1(5) . . ?
O26 S1 O22 109.6(5) . . ?
O24 S1 O27 110.3(5) . . ?
O26 S1 O27 108.7(6) . . ?
O22 S1 O27 106.5(5) . . ?
O25 S2 O21 111.1(5) . . ?
O25 S2 O35 110.4(5) . . ?
O21 S2 O35 111.1(6) . . ?
O25 S2 O23 109.4(5) . . ?
O21 S2 O23 107.8(5) . . ?
O35 S2 O23 107.0(5) . . ?
O71 S3 O97 115.9(10) . . ?
O71 S3 O93 106.4(9) . . ?
O97 S3 O93 102.0(12) . . ?
O71 S3 O32 111.3(7) . . ?
O97 S3 O32 110.4(8) . . ?
O93 S3 O32 110.3(10) . . ?
O92 S4 O28 114.4(8) . . ?
O92 S4 O19 114.1(9) . . ?
O28 S4 O19 111.3(6) . . ?
O92 S4 O64 100.6(11) . . ?
O28 S4 O64 108.9(7) . . ?
O19 S4 O64 106.6(7) . . ?
O95 S5 O38 109.0(7) . . ?
O95 S5 O88 111.2(12) . . ?
O38 S5 O88 112.1(10) . . ?
O95 S5 O63 114.4(11) . . ?
O38 S5 O63 108.8(8) . . ?
O88 S5 O63 101.2(11) . . ?
O29 S6 O36 111.5(6) . . ?
O29 S6 O83 110.2(8) . . ?
O36 S6 O83 109.5(9) . . ?
O29 S6 O74 113.2(9) . . ?
O36 S6 O74 108.6(7) . . ?
O83 S6 O74 103.5(9) . . ?
O31 Na39 O100 179.2(15) . . ?
O31 Na39 O17 92.5(7) . . ?
O100 Na39 O17 87.8(6) . . ?
O31 Na39 O8 96.1(8) . . ?
O100 Na39 O8 83.6(7) . . ?
O17 Na39 O8 170.7(7) . . ?
O31 Na39 O16 89.8(8) . . ?
O100 Na39 O16 90.9(8) . . ?
O17 Na39 O16 65.1(5) . . ?
O8 Na39 O16 118.3(8) . . ?
O31 Na39 O20 88.7(7) . . ?
O100 Na39 O20 91.6(8) . . ?
O17 Na39 O20 126.6(8) . . ?
O8 Na39 O20 57.4(4) . . ?
O16 Na39 O20 61.4(5) . . ?
O31 Na39 O15 86.6(8) . . ?
O100 Na39 O15 92.7(8) . . ?
O17 Na39 O15 114.4(7) . . ?
O8 Na39 O15 62.7(5) . . ?
O16 Na39 O15 176.3(7) . . ?
O20 Na39 O15 119.0(6) . . ?
O31 Na39 O11 83.0(7) . . ?
O100 Na39 O11 96.6(7) . . ?
O17 Na39 O11 56.0(4) . . ?
O8 Na39 O11 121.5(8) . . ?
O16 Na39 O11 120.1(7) . . ?
O20 Na39 O11 171.5(6) . . ?
O15 Na39 O11 58.9(5) . . ?
C67 O8 C84 117.8(10) . . ?
C67 O8 Na39 122.7(8) . . ?
C84 O8 Na39 118.5(8) . . ?
C76 O9 C60 108.3(8) . . ?
C52 O10 C75 116.0(9) . . ?
C91 O11 C80 117.4(9) . . ?
C91 O11 Na39 115.1(8) . . ?
C80 O11 Na39 117.1(7) . . ?
C79 O12 C55 109.5(9) . . ?
C86 O13 C56 117.9(9) . . ?
C45 O14 C85 116.5(9) . . ?
C66 O15 C54 108.9(9) . . ?
C66 O15 Na39 100.6(8) . . ?
C54 O15 Na39 111.4(8) . . ?
C69 O16 C77 111.5(8) . . ?
C69 O16 Na39 111.3(7) . . ?
C77 O16 Na39 106.0(8) . . ?
C98 O17 C72 116.1(9) . . ?
C98 O17 Na39 124.1(9) . . ?
C72 O17 Na39 115.6(8) . . ?
C47 O18 C61 117.6(9) . . ?
C62 O20 C57 117.0(9) . . ?
C62 O20 Na39 118.0(8) . . ?
C57 O20 Na39 117.1(7) . . ?
O14 C45 C89 126.2(11) . . ?
O14 C45 C52 114.0(10) . . ?
C89 C45 C52 119.8(11) . . ?
O18 C47 C86 115.4(10) . . ?
O18 C47 C90 124.7(11) . . ?
C86 C47 C90 119.9(11) . . ?
C53 C48 C86 118.0(12) . . ?
C53 C48 H48 121.0 . . ?
C86 C48 H48 121.0 . . ?
C70 C50 C59 121.2(12) . . ?
C70 C50 N37 122.3(11) . . ?
C59 C50 N37 116.4(11) . . ?
C78 C51 C67 121.9(12) . . ?
C78 C51 H51 119.0 . . ?
C67 C51 H51 119.0 . . ?
O10 C52 C58 125.4(11) . . ?
O10 C52 C45 115.6(11) . . ?
C58 C52 C45 119.0(11) . . ?
C65 C53 C48 120.2(11) . . ?
C65 C53 N44 121.9(11) . . ?
C48 C53 N44 117.9(11) . . ?
O15 C54 C80 107.1(9) . . ?
O15 C54 H54A 110.3 . . ?
C80 C54 H54A 110.3 . . ?
O15 C54 H54B 110.3 . . ?
C80 C54 H54B 110.3 . . ?
H54A C54 H54B 108.6 . . ?
O12 C55 C85 110.2(10) . . ?
O12 C55 H55A 109.6 . . ?
C85 C55 H55A 109.6 . . ?
O12 C55 H55B 109.6 . . ?
C85 C55 H55B 109.6 . . ?
H55A C55 H55B 108.1 . . ?
O13 C56 C76 107.4(10) . . ?
O13 C56 H56A 110.2 . . ?
C76 C56 H56A 110.2 . . ?
O13 C56 H56B 110.2 . . ?
C76 C56 H56B 110.2 . . ?
H56A C56 H56B 108.5 . . ?
O20 C57 C69 107.7(10) . . ?
O20 C57 H57A 110.2 . . ?
C69 C57 H57A 110.2 . . ?
O20 C57 H57B 110.2 . . ?
C69 C57 H57B 110.2 . . ?
H57A C57 H57B 108.5 . . ?
C81 C58 C52 120.7(12) . . ?
C81 C58 H58 119.6 . . ?
C52 C58 H58 119.6 . . ?
C98 C59 C50 119.0(12) . . ?
C98 C59 H59 120.5 . . ?
C50 C59 H59 120.5 . . ?
O9 C60 C75 107.7(9) . . ?
O9 C60 H60A 110.2 . . ?
C75 C60 H60A 110.2 . . ?
O9 C60 H60B 110.2 . . ?
C75 C60 H60B 110.2 . . ?
H60A C60 H60B 108.5 . . ?
O18 C61 C79 107.2(10) . . ?
O18 C61 H61A 110.3 . . ?
C79 C61 H61A 110.3 . . ?
O18 C61 H61B 110.3 . . ?
C79 C61 H61B 110.3 . . ?
H61A C61 H61B 108.5 . . ?
O20 C62 C87 123.9(11) . . ?
O20 C62 C67 115.4(11) . . ?
C87 C62 C67 120.6(12) . . ?
C53 C65 C90 121.8(12) . . ?
C53 C65 N40 120.9(10) . . ?
C90 C65 N40 117.3(11) . . ?
O15 C66 C84 108.3(10) . . ?
O15 C66 H66A 110.0 . . ?
C84 C66 H66A 110.0 . . ?
O15 C66 H66B 110.0 . . ?
C84 C66 H66B 110.0 . . ?
H66A C66 H66B 108.4 . . ?
O8 C67 C51 125.0(11) . . ?
O8 C67 C62 116.3(11) . . ?
C51 C67 C62 118.7(11) . . ?
C70 C68 C91 120.4(12) . . ?
C70 C68 H68 119.8 . . ?
C91 C68 H68 119.8 . . ?
O16 C69 C57 111.5(9) . . ?
O16 C69 H69A 109.3 . . ?
C57 C69 H69A 109.3 . . ?
O16 C69 H69B 109.3 . . ?
C57 C69 H69B 109.3 . . ?
H69A C69 H69B 108.0 . . ?
C50 C70 C68 120.8(13) . . ?
C50 C70 N33 121.5(12) . . ?
C68 C70 N33 117.6(12) . . ?
O17 C72 C77 106.9(10) . . ?
O17 C72 H72A 110.3 . . ?
C77 C72 H72A 110.3 . . ?
O17 C72 H72B 110.3 . . ?
C77 C72 H72B 110.3 . . ?
H72A C72 H72B 108.6 . . ?
C81 C73 C89 121.0(11) . . ?
C81 C73 N43 121.7(11) . . ?
C89 C73 N43 117.3(11) . . ?
O10 C75 C60 108.4(10) . . ?
O10 C75 H75A 110.0 . . ?
C60 C75 H75A 110.0 . . ?
O10 C75 H75B 110.0 . . ?
C60 C75 H75B 110.0 . . ?
H75A C75 H75B 108.4 . . ?
O9 C76 C56 110.8(9) . . ?
O9 C76 H76A 109.5 . . ?
C56 C76 H76A 109.5 . . ?
O9 C76 H76B 109.5 . . ?
C56 C76 H76B 109.5 . . ?
H76A C76 H76B 108.1 . . ?
O16 C77 C72 109.9(10) . . ?
O16 C77 H77A 109.7 . . ?
C72 C77 H77A 109.7 . . ?
O16 C77 H77B 109.7 . . ?
C72 C77 H77B 109.7 . . ?
H77A C77 H77B 108.2 . . ?
C82 C78 C51 119.3(12) . . ?
C82 C78 N41 121.0(11) . . ?
C51 C78 N41 119.6(10) . . ?
O12 C79 C61 109.4(9) . . ?
O12 C79 H79A 109.8 . . ?
C61 C79 H79A 109.8 . . ?
O12 C79 H79B 109.8 . . ?
C61 C79 H79B 109.8 . . ?
H79A C79 H79B 108.3 . . ?
O11 C80 C54 109.0(10) . . ?
O11 C80 H80A 109.9 . . ?
C54 C80 H80A 109.9 . . ?
O11 C80 H80B 109.9 . . ?
C54 C80 H80B 109.9 . . ?
H80A C80 H80B 108.3 . . ?
C58 C81 C73 119.8(12) . . ?
C58 C81 N30 118.4(12) . . ?
C73 C81 N30 121.7(11) . . ?
C78 C82 C87 122.0(12) . . ?
C78 C82 N42 123.7(12) . . ?
C87 C82 N42 114.2(11) . . ?
O8 C84 C66 108.0(11) . . ?
O8 C84 H84A 110.1 . . ?
C66 C84 H84A 110.1 . . ?
O8 C84 H84B 110.1 . . ?
C66 C84 H84B 110.1 . . ?
H84A C84 H84B 108.4 . . ?
O14 C85 C55 107.2(9) . . ?
O14 C85 H85A 110.3 . . ?
C55 C85 H85A 110.3 . . ?
O14 C85 H85B 110.3 . . ?
C55 C85 H85B 110.3 . . ?
H85A C85 H85B 108.5 . . ?
C47 C86 O13 115.9(10) . . ?
C47 C86 C48 121.4(12) . . ?
O13 C86 C48 122.6(11) . . ?
C62 C87 C82 117.3(12) . . ?
C62 C87 H87 121.3 . . ?
C82 C87 H87 121.3 . . ?
C45 C89 C73 119.4(12) . . ?
C45 C89 H89 120.3 . . ?
C73 C89 H89 120.3 . . ?
C47 C90 C65 118.6(12) . . ?
C47 C90 H90 120.7 . . ?
C65 C90 H90 120.7 . . ?
O11 C91 C98 116.6(11) . . ?
O11 C91 C68 124.5(11) . . ?
C98 C91 C68 118.8(12) . . ?
O17 C98 C91 115.6(11) . . ?
O17 C98 C59 124.6(12) . . ?
C91 C98 C59 119.7(12) . . ?

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
C85 O14 C45 C89 10.6(16) . . . . ?
C85 O14 C45 C52 -171.2(10) . . . . ?
C61 O18 C47 C86 -167.8(10) . . . . ?
C61 O18 C47 C90 12.8(17) . . . . ?
C75 O10 C52 C58 13.7(16) . . . . ?
C75 O10 C52 C45 -165.9(10) . . . . ?
O14 C45 C52 O10 -1.6(14) . . . . ?
C89 C45 C52 O10 176.7(10) . . . . ?
O14 C45 C52 C58 178.8(10) . . . . ?
C89 C45 C52 C58 -2.9(16) . . . . ?
C86 C48 C53 C65 2.5(18) . . . . ?
C86 C48 C53 N44 179.9(10) . . . . ?
C66 O15 C54 C80 -174.2(10) . . . . ?
Na39 O15 C54 C80 -64.2(11) . . . . ?
C79 O12 C55 C85 -179.4(9) . . . . ?
C86 O13 C56 C76 159.6(10) . . . . ?
C62 O20 C57 C69 -175.0(9) . . . . ?
Na39 O20 C57 C69 -26.4(12) . . . . ?
O10 C52 C58 C81 178.3(11) . . . . ?
C45 C52 C58 C81 -2.2(17) . . . . ?
C70 C50 C59 C98 -0.8(18) . . . . ?
N37 C50 C59 C98 -177.8(10) . . . . ?
C76 O9 C60 C75 -175.9(10) . . . . ?
C47 O18 C61 C79 175.2(9) . . . . ?
C57 O20 C62 C87 -9.0(16) . . . . ?
Na39 O20 C62 C87 -157.2(10) . . . . ?
C57 O20 C62 C67 170.5(11) . . . . ?
Na39 O20 C62 C67 22.3(14) . . . . ?
C48 C53 C65 C90 -3(2) . . . . ?
N44 C53 C65 C90 179.7(11) . . . . ?
C48 C53 C65 N40 177.2(11) . . . . ?
N44 C53 C65 N40 -0.1(19) . . . . ?
C54 O15 C66 C84 -175.5(11) . . . . ?
Na39 O15 C66 C84 67.4(11) . . . . ?
C84 O8 C67 C51 -16.8(17) . . . . ?
Na39 O8 C67 C51 151.6(10) . . . . ?
C84 O8 C67 C62 162.9(11) . . . . ?
Na39 O8 C67 C62 -28.6(14) . . . . ?
C78 C51 C67 O8 178.1(11) . . . . ?
C78 C51 C67 C62 -1.7(18) . . . . ?
O20 C62 C67 O8 2.2(16) . . . . ?
C87 C62 C67 O8 -178.3(10) . . . . ?
O20 C62 C67 C51 -178.1(10) . . . . ?
C87 C62 C67 C51 1.5(18) . . . . ?
C77 O16 C69 C57 179.7(10) . . . . ?
Na39 O16 C69 C57 -62.1(11) . . . . ?
O20 C57 C69 O16 58.2(13) . . . . ?
C59 C50 C70 C68 3.0(19) . . . . ?
N37 C50 C70 C68 179.9(11) . . . . ?
C59 C50 C70 N33 179.4(11) . . . . ?
N37 C50 C70 N33 -3.7(19) . . . . ?
C91 C68 C70 C50 -3.9(19) . . . . ?
C91 C68 C70 N33 179.6(11) . . . . ?
C98 O17 C72 C77 -166.7(10) . . . . ?
Na39 O17 C72 C77 35.5(12) . . . . ?
C52 O10 C75 C60 174.7(9) . . . . ?
O9 C60 C75 O10 -61.4(12) . . . . ?
C60 O9 C76 C56 177.2(10) . . . . ?
O13 C56 C76 O9 63.4(12) . . . . ?
C69 O16 C77 C72 -177.2(10) . . . . ?
Na39 O16 C77 C72 61.4(11) . . . . ?
O17 C72 C77 O16 -66.8(13) . . . . ?
C67 C51 C78 C82 -0.9(18) . . . . ?
C67 C51 C78 N41 -178.0(11) . . . . ?
C55 O12 C79 C61 -172.4(10) . . . . ?
O18 C61 C79 O12 -61.1(12) . . . . ?
C91 O11 C80 C54 -176.7(9) . . . . ?
Na39 O11 C80 C54 -33.3(12) . . . . ?
O15 C54 C80 O11 64.3(13) . . . . ?
C52 C58 C81 C73 5.5(19) . . . . ?
C52 C58 C81 N30 -177.9(11) . . . . ?
C89 C73 C81 C58 -3.9(19) . . . . ?
N43 C73 C81 C58 176.5(11) . . . . ?
C89 C73 C81 N30 179.6(11) . . . . ?
N43 C73 C81 N30 0.0(19) . . . . ?
C51 C78 C82 C87 3.9(19) . . . . ?
N41 C78 C82 C87 -179.2(10) . . . . ?
C51 C78 C82 N42 -179.5(11) . . . . ?
N41 C78 C82 N42 -2.5(19) . . . . ?
C67 O8 C84 C66 -161.9(10) . . . . ?
Na39 O8 C84 C66 29.1(13) . . . . ?
O15 C66 C84 O8 -68.8(13) . . . . ?
C45 O14 C85 C55 160.0(10) . . . . ?
O12 C55 C85 O14 65.7(12) . . . . ?
O18 C47 C86 O13 -3.4(16) . . . . ?
C90 C47 C86 O13 176.0(11) . . . . ?
O18 C47 C86 C48 178.6(10) . . . . ?
C90 C47 C86 C48 -2.0(18) . . . . ?
C56 O13 C86 C47 -164.9(10) . . . . ?
C56 O13 C86 C48 13.1(16) . . . . ?
C53 C48 C86 C47 0.0(18) . . . . ?
C53 C48 C86 O13 -177.9(11) . . . . ?
O20 C62 C87 C82 -179.3(10) . . . . ?
C67 C62 C87 C82 1.2(18) . . . . ?
C78 C82 C87 C62 -4.0(18) . . . . ?
N42 C82 C87 C62 179.1(11) . . . . ?
O14 C45 C89 C73 -177.4(11) . . . . ?
C52 C45 C89 C73 4.5(17) . . . . ?
C81 C73 C89 C45 -1.1(18) . . . . ?
N43 C73 C89 C45 178.5(10) . . . . ?
O18 C47 C90 C65 -179.1(11) . . . . ?
C86 C47 C90 C65 1.6(18) . . . . ?
C53 C65 C90 C47 1(2) . . . . ?
N40 C65 C90 C47 -179.3(11) . . . . ?
C80 O11 C91 C98 166.5(11) . . . . ?
Na39 O11 C91 C98 22.3(14) . . . . ?
C80 O11 C91 C68 -12.1(17) . . . . ?
Na39 O11 C91 C68 -156.3(10) . . . . ?
C70 C68 C91 O11 -178.8(11) . . . . ?
C70 C68 C91 C98 2.6(19) . . . . ?
C72 O17 C98 C91 170.1(11) . . . . ?
Na39 O17 C98 C91 -34.3(15) . . . . ?
C72 O17 C98 C59 -6.8(17) . . . . ?
Na39 O17 C98 C59 148.9(10) . . . . ?
O11 C91 C98 O17 3.9(17) . . . . ?
C68 C91 C98 O17 -177.4(10) . . . . ?
O11 C91 C98 C59 -179.1(10) . . . . ?
C68 C91 C98 C59 -0.4(19) . . . . ?
C50 C59 C98 O17 176.3(11) . . . . ?
C50 C59 C98 C91 -0.5(18) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
