# Supplementary Information (SI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

####################################################################### 
# 
# 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_CE4
_database_code_depnum_ccdc_archive 'CCDC 2258327'
loop_
_audit_author_name
_audit_author_address
'Vincent M. Lynch'
;Department of Chemistry, the University of Texas at Austin
United States of America
;
_audit_update_record             
;
2023-04-24 deposited with the CCDC.	2024-09-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63 H69 Cl6 N4 O9'
_chemical_formula_weight         1238.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   20.3119(4)
_cell_length_b                   21.5671(5)
_cell_length_c                   14.0259(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6144.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9993
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      21.36

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_F_000             2596
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.203
_exptl_absorpt_coefficient_mu    0.339
_shelx_estimated_absorpt_T_min   0.910
_shelx_estimated_absorpt_T_max   0.934
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7131
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            97609
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.732
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7836
_reflns_number_gt                4800
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1681P)²+6.9796P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7836
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0919
_refine_ls_wR_factor_ref         0.3085
_refine_ls_wR_factor_gt          0.2701
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.55946(8) 0.31651(7) 0.07717(10) 0.0801(5) Uani 1 1 d . . . . .
Cl2 Cl 0.62857(10) 0.2500 -0.07141(17) 0.0850(6) Uani 1 2 d S T P . .
Cl3 Cl 0.76840(8) 0.2500 0.36859(12) 0.0633(4) Uani 1 2 d S T P . .
Cl4 Cl 0.7110(2) 0.2500 0.1861(2) 0.1428(14) Uani 1 2 d S T P . .
Cl5 Cl 0.8587(3) 0.2500 0.2177(4) 0.239(3) Uani 1 2 d S T P . .
O1 O 0.28127(14) 0.43694(14) 0.5029(2) 0.0542(7) Uani 1 1 d . . . . .
O2 O 0.25653(16) 0.41781(15) 0.3064(2) 0.0617(8) Uani 1 1 d . . . . .
O3 O 0.3456(3) 0.4585(2) 0.1495(4) 0.0817(17) Uani 0.7 1 d . . P A 1
O3A O 0.3409(5) 0.3933(3) 0.1569(5) 0.0373(18) Uani 0.3 1 d . . P A 2
O4 O 0.48667(18) 0.39276(17) 0.27187(19) 0.0667(9) Uani 1 1 d . . . . .
N1 N 0.4384(2) 0.2500 0.8134(3) 0.0400(10) Uani 1 2 d S T P . .
H1 H 0.4561 0.2500 0.7562 0.048 Uiso 1 2 calc R U P . .
N2 N 0.53086(12) 0.35715(13) 0.71528(18) 0.0301(6) Uani 1 1 d . . . . .
H2 H 0.5091 0.3353 0.6727 0.036 Uiso 1 1 calc R U . . .
N3 N 0.62713(18) 0.2500 0.6276(3) 0.0329(8) Uani 1 2 d S T P . .
H3 H 0.5845 0.2500 0.6390 0.039 Uiso 1 2 calc R U P . .
C1 C 0.42240(15) 0.30267(18) 0.8650(2) 0.0368(8) Uani 1 1 d . . . . .
C2 C 0.39636(15) 0.28248(19) 0.9489(2) 0.0385(8) Uani 1 1 d . . . . .
H2A H 0.3808 0.3082 0.9991 0.046 Uiso 1 1 calc R U . . .
C3 C 0.43341(16) 0.36739(18) 0.8272(2) 0.0386(8) Uani 1 1 d . . . . .
C4 C 0.4155(2) 0.4137(2) 0.9066(3) 0.0548(11) Uani 1 1 d . . . . .
H4A H 0.4223 0.4561 0.8835 0.082 Uiso 1 1 calc R U . . .
H4B H 0.3692 0.4081 0.9245 0.082 Uiso 1 1 calc R U . . .
H4C H 0.4435 0.4063 0.9623 0.082 Uiso 1 1 calc R U . . .
C5 C 0.50569(16) 0.37650(16) 0.8020(2) 0.0321(7) Uani 1 1 d . . . . .
C6 C 0.55531(19) 0.40599(18) 0.8481(2) 0.0412(8) Uani 1 1 d . . . . .
H6A H 0.5530 0.4234 0.9102 0.049 Uiso 1 1 calc R U . . .
C7 C 0.61106(18) 0.40634(17) 0.7879(2) 0.0392(8) Uani 1 1 d . . . . .
H7A H 0.6527 0.4240 0.8027 0.047 Uiso 1 1 calc R U . . .
C8 C 0.59501(15) 0.37713(14) 0.7052(2) 0.0292(6) Uani 1 1 d . . . . .
C9 C 0.63462(15) 0.36617(14) 0.6157(2) 0.0306(7) Uani 1 1 d . . . . .
C10 C 0.69075(17) 0.41493(17) 0.6119(3) 0.0429(8) Uani 1 1 d . . . . .
H10A H 0.7170 0.4085 0.5542 0.064 Uiso 1 1 calc R U . . .
H10B H 0.6717 0.4567 0.6109 0.064 Uiso 1 1 calc R U . . .
H10C H 0.7189 0.4104 0.6682 0.064 Uiso 1 1 calc R U . . .
C11 C 0.66515(14) 0.30213(15) 0.6174(2) 0.0300(7) Uani 1 1 d . . . . .
C12 C 0.72796(15) 0.28300(16) 0.6031(2) 0.0339(7) Uani 1 1 d . . . . .
H12A H 0.7653 0.3090 0.5947 0.041 Uiso 1 1 calc R U . . .
C13 C 0.39117(16) 0.38294(18) 0.7397(2) 0.0386(8) Uani 1 1 d . . . . .
C14 C 0.33745(17) 0.34714(19) 0.7120(2) 0.0415(8) Uani 1 1 d . . . . .
H14A H 0.3268 0.3108 0.7470 0.050 Uiso 1 1 calc R U . . .
C15 C 0.29911(18) 0.3637(2) 0.6340(3) 0.0463(9) Uani 1 1 d . . . . .
H15A H 0.2623 0.3390 0.6166 0.056 Uiso 1 1 calc R U . . .
C16 C 0.31430(17) 0.41604(19) 0.5815(3) 0.0416(8) Uani 1 1 d . . . . .
C17 C 0.36768(17) 0.45300(18) 0.6098(3) 0.0432(8) Uani 1 1 d . . . . .
H17A H 0.3782 0.4895 0.5752 0.052 Uiso 1 1 calc R U . . .
C18 C 0.40458(17) 0.43627(18) 0.6875(3) 0.0424(8) Uani 1 1 d . . . . .
H18A H 0.4404 0.4619 0.7062 0.051 Uiso 1 1 calc R U . . .
C19 C 0.2281(2) 0.4000(3) 0.4682(3) 0.0600(12) Uani 1 1 d . . . . .
H19A H 0.1912 0.4003 0.5143 0.072 Uiso 1 1 calc R U . . .
H19B H 0.2427 0.3566 0.4588 0.072 Uiso 1 1 calc R U . . .
C20 C 0.2068(2) 0.4280(3) 0.3747(3) 0.0647(13) Uani 1 1 d . . . . .
H20A H 0.1652 0.4087 0.3533 0.078 Uiso 1 1 calc R U . . .
H20B H 0.1992 0.4730 0.3826 0.078 Uiso 1 1 calc R U . . .
C21 C 0.2399(3) 0.4441(2) 0.2177(3) 0.0676(14) Uani 1 1 d . . . . .
H21A H 0.2369 0.4897 0.2244 0.081 Uiso 1 1 calc R U . . .
H21B H 0.1963 0.4285 0.1973 0.081 Uiso 1 1 calc R U . . .
C22 C 0.2896(4) 0.4287(4) 0.1441(5) 0.114(3) Uani 1 1 d . . . . .
H22A H 0.2989 0.3837 0.1478 0.137 Uiso 0.7 1 calc R U P A 1
H22B H 0.2701 0.4369 0.0807 0.137 Uiso 0.7 1 calc R U P A 1
H22C H 0.2649 0.4103 0.0903 0.137 Uiso 0.3 1 calc R U P A 2
H22D H 0.3069 0.4689 0.1209 0.137 Uiso 0.3 1 calc R U P A 2
C23 C 0.4035(3) 0.4197(4) 0.1661(4) 0.096(2) Uani 1 1 d . . . . .
H23A H 0.4395 0.4326 0.1228 0.116 Uiso 0.7 1 calc R U P A 1
H23B H 0.3926 0.3759 0.1518 0.116 Uiso 0.7 1 calc R U P A 1
H23C H 0.4030 0.4614 0.1368 0.116 Uiso 0.3 1 calc R U P A 2
H23D H 0.4355 0.3940 0.1304 0.116 Uiso 0.3 1 calc R U P A 2
C24 C 0.4262(2) 0.4252(3) 0.2688(3) 0.0672(13) Uani 1 1 d . . . . .
H24A H 0.4324 0.4692 0.2867 0.081 Uiso 1 1 calc R U . . .
H24B H 0.3937 0.4062 0.3126 0.081 Uiso 1 1 calc R U . . .
C25 C 0.5188(2) 0.38859(18) 0.3569(2) 0.0458(9) Uani 1 1 d . . . . .
C26 C 0.5739(2) 0.3499(2) 0.3594(3) 0.0597(12) Uani 1 1 d . . . . .
H26A H 0.5873 0.3289 0.3031 0.072 Uiso 1 1 calc R U . . .
C27 C 0.6089(2) 0.3418(2) 0.4418(3) 0.0477(9) Uani 1 1 d . . . . .
H27A H 0.6452 0.3140 0.4422 0.057 Uiso 1 1 calc R U . . .
C28 C 0.59257(16) 0.37341(15) 0.5253(2) 0.0322(7) Uani 1 1 d . . . . .
C29 C 0.53911(18) 0.41352(15) 0.5202(2) 0.0366(7) Uani 1 1 d . . . . .
H29A H 0.5276 0.4369 0.5752 0.044 Uiso 1 1 calc R U . . .
C30 C 0.50190(19) 0.42065(17) 0.4381(2) 0.0391(8) Uani 1 1 d . . . . .
H30A H 0.4649 0.4476 0.4378 0.047 Uiso 1 1 calc R U . . .
O5 O 0.4687(4) 0.2500 0.5925(4) 0.112(2) Uani 1 2 d S T P . .
C31 C 0.4398(6) 0.2500 0.5114(6) 0.103(3) Uani 1 2 d S T P . .
H31A H 0.4306 0.2928 0.4921 0.154 Uiso 0.5 1 calc R U P . .
H31B H 0.3984 0.2269 0.5162 0.154 Uiso 0.5 1 calc R U P . .
H31C H 0.4684 0.2303 0.4639 0.154 Uiso 0.5 1 calc R U P . .
C32 C 0.5611(3) 0.2500 0.0052(4) 0.0524(14) Uani 1 2 d S T P . .
H32A H 0.5203 0.2500 -0.0347 0.063 Uiso 1 2 calc R U P . .
C33 C 0.7837(8) 0.2701(4) 0.2469(7) 0.097(5) Uani 0.5 1 d . . P . .
H33A H 0.7843 0.3165 0.2463 0.116 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C32 1.754(4) . ?
Cl2 C32 1.742(7) . ?
Cl3 C33 1.789(11) 7_565 ?
Cl3 C33 1.789(11) . ?
Cl4 C33 1.760(14) . ?
Cl4 C33 1.760(14) 7_565 ?
Cl5 C33 1.636(16) 7_565 ?
Cl5 C33 1.636(16) . ?
O1 C16 1.367(4) . ?
O1 C19 1.427(5) . ?
O2 C21 1.409(5) . ?
O2 C20 1.409(6) . ?
O3 C22 1.309(9) . ?
O3 C23 1.462(8) . ?
O3A C22 1.305(11) . ?
O3A C23 1.399(11) . ?
O4 C25 1.362(4) . ?
O4 C24 1.415(6) . ?
N1 C1 1.385(4) . ?
N1 C1 1.385(4) 7_565 ?
N1 H1 0.8800 . ?
N2 C8 1.380(4) . ?
N2 C5 1.384(4) . ?
N2 H2 0.8800 . ?
N3 C11 1.371(4) 7_565 ?
N3 C11 1.371(4) . ?
N3 H3 0.8800 . ?
C1 C2 1.362(5) . ?
C1 C3 1.510(5) . ?
C2 C2 1.401(8) 7_565 ?
C2 H2A 0.9500 . ?
C3 C5 1.523(5) . ?
C3 C13 1.534(5) . ?
C3 C4 1.539(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.356(5) . ?
C6 C7 1.412(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.360(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.509(4) . ?
C9 C11 1.514(4) . ?
C9 C28 1.537(4) . ?
C9 C10 1.552(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.356(4) . ?
C12 C12 1.424(7) 7_565 ?
C12 H12A 0.9500 . ?
C13 C18 1.391(5) . ?
C13 C14 1.392(5) . ?
C14 C15 1.390(5) . ?
C14 H14A 0.9500 . ?
C15 C16 1.382(6) . ?
C15 H15A 0.9500 . ?
C16 C17 1.403(5) . ?
C17 C18 1.371(5) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C19 C20 1.507(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.481(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 H22C 0.9900 . ?
C22 H22D 0.9900 . ?
C23 C24 1.517(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 H23C 0.9900 . ?
C23 H23D 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C30 1.376(5) . ?
C25 C26 1.397(6) . ?
C26 C27 1.368(6) . ?
C26 H26A 0.9500 . ?
C27 C28 1.395(5) . ?
C27 H27A 0.9500 . ?
C28 C29 1.390(5) . ?
C29 C30 1.387(5) . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9500 . ?
O5 C31 1.279(8) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 Cl1 1.754(4) 7_565 ?
C32 H32A 1.0000 . ?
C33 H33A 1.0000 . ?

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
C33 Cl3 C33 28.1(6) 7_565 . ?
C33 Cl4 C33 28.5(6) . 7_565 ?
C33 Cl5 C33 30.7(7) 7_565 . ?
C16 O1 C19 117.5(3) . . ?
C21 O2 C20 111.5(4) . . ?
C22 O3 C23 115.2(6) . . ?
C22 O3A C23 119.9(7) . . ?
C25 O4 C24 118.4(3) . . ?
C1 N1 C1 110.2(4) . 7_565 ?
C1 N1 H1 124.9 . . ?
C1 N1 H1 124.9 7_565 . ?
C8 N2 C5 110.2(3) . . ?
C8 N2 H2 124.9 . . ?
C5 N2 H2 124.9 . . ?
C11 N3 C11 110.1(4) 7_565 . ?
C11 N3 H3 124.9 7_565 . ?
C11 N3 H3 124.9 . . ?
C2 C1 N1 106.3(3) . . ?
C2 C1 C3 131.1(3) . . ?
N1 C1 C3 122.7(3) . . ?
C1 C2 C2 108.6(2) . 7_565 ?
C1 C2 H2A 125.7 . . ?
C2 C2 H2A 125.7 7_565 . ?
C1 C3 C5 110.1(3) . . ?
C1 C3 C13 113.6(3) . . ?
C5 C3 C13 109.0(3) . . ?
C1 C3 C4 108.1(3) . . ?
C5 C3 C4 108.2(3) . . ?
C13 C3 C4 107.7(3) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N2 106.6(3) . . ?
C6 C5 C3 131.8(3) . . ?
N2 C5 C3 121.4(3) . . ?
C5 C6 C7 108.3(3) . . ?
C5 C6 H6A 125.9 . . ?
C7 C6 H6A 125.9 . . ?
C8 C7 C6 108.4(3) . . ?
C8 C7 H7A 125.8 . . ?
C6 C7 H7A 125.8 . . ?
C7 C8 N2 106.5(3) . . ?
C7 C8 C9 130.8(3) . . ?
N2 C8 C9 122.7(3) . . ?
C8 C9 C11 110.4(3) . . ?
C8 C9 C28 112.0(2) . . ?
C11 C9 C28 109.4(3) . . ?
C8 C9 C10 108.3(3) . . ?
C11 C9 C10 108.5(3) . . ?
C28 C9 C10 108.1(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N3 107.2(3) . . ?
C12 C11 C9 131.3(3) . . ?
N3 C11 C9 121.3(3) . . ?
C11 C12 C12 107.7(2) . 7_565 ?
C11 C12 H12A 126.1 . . ?
C12 C12 H12A 126.1 7_565 . ?
C18 C13 C14 117.7(3) . . ?
C18 C13 C3 119.5(3) . . ?
C14 C13 C3 122.7(3) . . ?
C15 C14 C13 121.1(4) . . ?
C15 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
C16 C15 C14 120.2(4) . . ?
C16 C15 H15A 119.9 . . ?
C14 C15 H15A 119.9 . . ?
O1 C16 C15 126.1(4) . . ?
O1 C16 C17 114.8(3) . . ?
C15 C16 C17 119.1(3) . . ?
C18 C17 C16 119.8(4) . . ?
C18 C17 H17A 120.1 . . ?
C16 C17 H17A 120.1 . . ?
C17 C18 C13 122.0(4) . . ?
C17 C18 H18A 119.0 . . ?
C13 C18 H18A 119.0 . . ?
O1 C19 C20 106.9(4) . . ?
O1 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
O1 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.6 . . ?
O2 C20 C19 108.9(4) . . ?
O2 C20 H20A 109.9 . . ?
C19 C20 H20A 109.9 . . ?
O2 C20 H20B 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
O2 C21 C22 111.3(5) . . ?
O2 C21 H21A 109.4 . . ?
C22 C21 H21A 109.4 . . ?
O2 C21 H21B 109.4 . . ?
C22 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
O3A C22 C21 125.4(6) . . ?
O3 C22 C21 116.2(7) . . ?
O3 C22 H22A 108.2 . . ?
C21 C22 H22A 108.2 . . ?
O3 C22 H22B 108.2 . . ?
C21 C22 H22B 108.2 . . ?
H22A C22 H22B 107.4 . . ?
O3A C22 H22C 106.0 . . ?
C21 C22 H22C 106.0 . . ?
O3A C22 H22D 106.0 . . ?
C21 C22 H22D 106.0 . . ?
H22C C22 H22D 106.3 . . ?
O3A C23 C24 113.3(6) . . ?
O3 C23 C24 110.5(5) . . ?
O3 C23 H23A 109.6 . . ?
C24 C23 H23A 109.6 . . ?
O3 C23 H23B 109.6 . . ?
C24 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
O3A C23 H23C 108.9 . . ?
C24 C23 H23C 108.9 . . ?
O3A C23 H23D 108.9 . . ?
C24 C23 H23D 108.9 . . ?
H23C C23 H23D 107.7 . . ?
O4 C24 C23 104.7(4) . . ?
O4 C24 H24A 110.8 . . ?
C23 C24 H24A 110.8 . . ?
O4 C24 H24B 110.8 . . ?
C23 C24 H24B 110.8 . . ?
H24A C24 H24B 108.9 . . ?
O4 C25 C30 124.9(3) . . ?
O4 C25 C26 116.5(3) . . ?
C30 C25 C26 118.7(3) . . ?
C27 C26 C25 120.9(3) . . ?
C27 C26 H26A 119.6 . . ?
C25 C26 H26A 119.6 . . ?
C26 C27 C28 121.6(4) . . ?
C26 C27 H27A 119.2 . . ?
C28 C27 H27A 119.2 . . ?
C29 C28 C27 116.6(3) . . ?
C29 C28 C9 122.6(3) . . ?
C27 C28 C9 120.7(3) . . ?
C30 C29 C28 122.5(3) . . ?
C30 C29 H29A 118.8 . . ?
C28 C29 H29A 118.8 . . ?
C25 C30 C29 119.7(3) . . ?
C25 C30 H30A 120.1 . . ?
C29 C30 H30A 120.1 . . ?
O5 C31 H31A 109.5 . . ?
O5 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O5 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Cl2 C32 Cl1 111.7(2) . 7_565 ?
Cl2 C32 Cl1 111.7(2) . . ?
Cl1 C32 Cl1 109.7(3) 7_565 . ?
Cl2 C32 H32A 107.9 . . ?
Cl1 C32 H32A 107.9 7_565 . ?
Cl1 C32 H32A 107.9 . . ?
Cl5 C33 Cl4 126.6(6) . . ?
Cl5 C33 Cl3 109.7(7) . . ?
Cl4 C33 Cl3 104.8(8) . . ?
Cl5 C33 H33A 104.6 . . ?
Cl4 C33 H33A 104.6 . . ?
Cl3 C33 H33A 104.6 . . ?

_refine_diff_density_max         2.261
_refine_diff_density_min         -1.748
_refine_diff_density_rms         0.095



####################################################################### 
# 
# 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_yjh-3_auto
_database_code_depnum_ccdc_archive 'CCDC 2258328'
loop_
_audit_author_name
_audit_author_address
'Vincent M. Lynch'
;Department of Chemistry, the University of Texas at Austin
United States of America
;
_audit_update_record             
;
2023-04-24 deposited with the CCDC.	2024-09-02 downloaded from the CCDC.
;
_audit_creation_date             2022-12-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C H Cl3), Cl O4, C66 H79 N4 Na O12, 0.612(C3 H6 O), 0.388(C2 H5 O), 1.194(C H4 O), 0.806(H2 O)'
_chemical_formula_sum            'C71.81 H93 Cl7 N4 Na O19'
_chemical_formula_weight         1587.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C73 H42 N4 O18 Cl7 Na'
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 Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.2739(3)
_cell_length_b                   15.65634(16)
_cell_length_c                   19.10054(13)
_cell_angle_alpha                110.4157(8)
_cell_angle_beta                 90.9004(15)
_cell_angle_gamma                103.4262(16)
_cell_volume                     3869.11(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    28767
_cell_measurement_temperature    100.03(12)
_cell_measurement_theta_max      77.0110
_cell_measurement_theta_min      2.4660
_shelx_estimated_absorpt_T_max   0.865
_shelx_estimated_absorpt_T_min   0.478
_exptl_absorpt_coefficient_mu    2.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28080
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.374
_diffrn_reflns_theta_min         2.482
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00 -44.00   0.50    6.57    --  -48.70 -60.00  16.00  152
  2  ω     93.00 142.00   0.50   26.27    --  107.75  60.00 156.00   98
  3  ω   -120.00 -95.00   0.50    6.57    --  -48.70-125.00 120.00   50
  4  ω    -64.00  19.00   0.50    6.57    --  -48.70  60.00 156.00  166
  5  ω    -21.00  51.00   0.50    6.57    --   48.70 -60.00  16.00  144
  6  ω     39.00  93.00   0.50   26.27    --  107.75 -99.00  60.00  108
  7  ω     52.00 120.00   0.50    6.57    --   48.70  60.00 156.00  136
  8  ω     64.00 121.00   0.50   26.27    --  107.75 -60.00  16.00  114
  9  ω   -110.00 -82.00   0.50    6.57    --  -48.70-125.00-180.00   56
 10  ω    -72.00 -18.00   0.50    6.57    --  -48.70 125.00  30.00  108
 11  ω   -110.00 -84.00   0.50    6.57    --  -48.70-125.00 -30.00   52
 12  ω   -119.00 -75.00   0.50    6.57    --  -48.70-125.00  90.00   88
 13  ω     34.00  96.00   0.50    6.57    --   48.70-125.00  30.00  124
 14  ω     35.00  95.00   0.50    6.57    --   48.70-125.00-120.00  120
 15  ω    100.50 140.00   0.50   26.27    --  107.75  77.00 -60.00   79
 16  ω     41.00 106.00   0.50   26.27    --  107.75 -99.00 150.00  130
 17  ω     77.00  91.00   0.50   26.27    --  107.75 -99.00 -30.00   28
 18  ω     35.00  80.00   0.50   26.27    --  107.75 -99.00   0.00   90
 19  ω     35.00  76.00   0.50   26.27    --  107.75 -38.00-120.00   82
 20  ω     80.00 118.00   0.50   26.27    --  107.75 -38.00-120.00   76
 21  ω     65.00  84.00   0.50   26.27    --  107.75 -99.00 -90.00   38
 22  ω    122.00 177.00   0.50   26.27    --  107.75 125.00   0.00  110
 23  ω     37.00 102.00   0.50   26.27    --  107.75 -99.00  30.00  130
 24  ω     39.00 106.00   0.50   26.27    --  107.75 -99.00-150.00  134
 25  ω     79.00 104.00   0.50   26.27    --  107.75 -99.00 120.00   50
 26  ω    127.00 169.00   0.50   26.27    --  107.75  19.00 150.00   84
 27  ω     97.00 176.00   0.50   26.27    --  107.75  19.00  60.00  158
 28  ω     95.00 174.00   0.50   26.27    --  107.75  38.00   0.00  158
 29  ω    150.00 178.00   0.50   26.27    --  107.75  77.00 -60.00   56
 30  ω     96.00 178.00   0.50   26.27    --  107.75  19.00  90.00  164
 31  ω     61.00 115.00   0.50   26.27    --  107.75 -38.00  30.00  108
 32  ω     36.00  62.00   0.50   26.27    --  107.75 -99.00 -30.00   52
 33  ω     41.00 122.00   0.50   26.27    --  107.75 -57.00-180.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1101519000
_diffrn_orient_matrix_UB_12      -0.0383291000
_diffrn_orient_matrix_UB_13      -0.0219129000
_diffrn_orient_matrix_UB_21      0.0163001000
_diffrn_orient_matrix_UB_22      -0.0908760000
_diffrn_orient_matrix_UB_23      -0.0582296000
_diffrn_orient_matrix_UB_31      -0.0073123000
_diffrn_orient_matrix_UB_32      -0.0453213000
_diffrn_orient_matrix_UB_33      0.0601663000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                26107
_reflns_number_total             28080
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Shelxtl-Plus/XP, Bruker AXS, Inc. 2009'
_computing_publication_material  'Shelxtl-Plus, Bruker AXS, Inc. 2009'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1150
_refine_ls_number_reflns         28080
_refine_ls_number_restraints     1061
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0563
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0789P)²+3.0482P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1529
_refine_special_details          
'There was quite a bit of disordered solvent of various components.  Both molecules of chloroform were disordered.  H-bonded to the pyrrole groups was a mixture of acetone and ethanol.  In the interior of the macrocycle was a disordered mixture of methanol and water molecules H-bound to one of the polyether groups.  The H atoms on some of the oxygen atoms of the methanol and ethanol molecules could not be adequately modeled and were not included in the final refinement model.'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.4599(7)
 0.5401(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All H(H,H) groups, All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 O9A-C55
 1.45 with sigma of 0.03
 O20-C69
 1.45 with sigma of 0.03
 O02O-C02T
 1.45 with sigma of 0.03
 O21-C70
 1.45 with sigma of 0.03
 C02T-H02C
 0.95 with sigma of 0.03
 O02O-H02B
 1.85 with sigma of 0.03
 C02T-H02A
 0.95 with sigma of 0.03
 C02T-H02B
 0.95 with sigma of 0.03
 H02C-O02O
 1.85 with sigma of 0.03
 C55-C54
 1.52 with sigma of 0.03
 H02A-O02O
 1.85 with sigma of 0.03
 O9A-C55A
 1.45 with sigma of 0.03
 C55A-C54
 1.52 with sigma of 0.03
 O9-C55
 1.45 with sigma of 0.03
 H02B-H02A
 1.6 with sigma of 0.03
 H02A-H02C
 1.6 with sigma of 0.03
 H02C-H02B
 1.6 with sigma of 0.03
 C1B-O1B
 1.45 with sigma of 0.02
 C1B-C2B
 1.52 with sigma of 0.02
 O1A-C1A
 1.21 with sigma of 0.02
 C1A-C3A = C1A-C2A
 1.5 with sigma of 0.02
 C54A-C55A
 1.52 with sigma of 0.03
 O8-C54A
 1.45 with sigma of 0.03
 C56A-C57A
 1.52 with sigma of 0.02
 O9A-C54A
 2.3 with sigma of 0.04
 C57-C56
 1.52 with sigma of 0.02
 O10-C57A
 1.45 with sigma of 0.03
 O10-C57
 1.45 with sigma of 0.03
 Cl1A-ClA
 2.85 with sigma of 0.04
 Cl6-Cl7
 2.85 with sigma of 0.04
 Cl6-Cl5
 2.85 with sigma of 0.04
 Cl5-ClA
 2.85 with sigma of 0.04
 Cl5-Cl1A
 2.85 with sigma of 0.04
 Cl7-Cl5
 2.85 with sigma of 0.04
 Cl4-C02D
 1.75 with sigma of 0.02
 Cl2A-Cl3
 2.76 with sigma of 0.05
 Cl2A-Cl4A
 2.76 with sigma of 0.05
 Cl4-Cl3
 2.76 with sigma of 0.05
 Cl4A-C02E
 1.75 with sigma of 0.02
 Cl4-Cl2
 2.76 with sigma of 0.05
 Cl2-C02D
 1.75 with sigma of 0.02
 Cl2-Cl3
 2.76 with sigma of 0.05
 Cl4A-Cl3
 2.76 with sigma of 0.05
 Cl2A-C02E
 1.75 with sigma of 0.02
 O1B-C2B
 2.5 with sigma of 0.04
 O023-H02G
 0.84 with sigma of 0.02
 O023-H02F
 0.84 with sigma of 0.02
 H02F-H02G
 1.3 with sigma of 0.03
 O1A-C3A = O1A-C2A
 2.38 with sigma of 0.04
 O12-H12A \\sim O12-H12B \\sim O12-H12C
 with sigma of 0.03
 O20-H69A \\sim O20-H69B \\sim O20-H69C
 with sigma of 0.02
 C3A-O1A \\sim C2A-O1A
 with sigma of 0.04
 C1A-C3A \\sim C1A-C2A
 with sigma of 0.02
 Cl5-C02S \\sim Cl5-C65
 with sigma of 0.02
 Cl6-C02S \\sim ClA-C65
 with sigma of 0.02
 Cl6-Cl7 \\sim ClA-Cl1A
 with sigma of 0.04
 Cl7-C02S \\sim Cl1A-C65
 with sigma of 0.02
 Cl5-Cl6 \\sim Cl5-ClA
 with sigma of 0.04
 Cl5-Cl7 \\sim Cl5-Cl1A
 with sigma of 0.04
 Cl3-C02D \\sim Cl3-C02E
 with sigma of 0.02
 Cl4-C02D \\sim Cl4A-C02E
 with sigma of 0.02
 Cl2-Cl3 \\sim Cl2A-Cl3
 with sigma of 0.04
 Cl2-Cl4 \\sim Cl2A-Cl4A
 with sigma of 0.04
 Cl3-Cl4 \\sim Cl3-Cl4A
 with sigma of 0.04
 Cl2-C02D \\sim Cl2A-C02E
 with sigma of 0.02
4. Restrained planarity
 O1A, C1A, C2A, C3A
 with sigma of 0.05
5. Uiso/Uaniso restraints and constraints
O02O \\sim O21 \\sim C02T \\sim C70: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O20 \\sim O023: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O9 \\sim O9A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O1A \\sim C1A \\sim C2A \\sim C3A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C55 \\sim C55A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C02S \\sim C65: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
ClA \\sim Cl1A \\sim Cl5 \\sim Cl6 \\sim Cl7: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C56 \\sim C56A \\sim C57 \\sim C57A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Cl2 \\sim Cl2A \\sim Cl4 \\sim Cl4A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C54 \\sim C54A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O1A \\sim O1B \\sim C1A \\sim C1B \\sim C2A \\sim C2B \\sim C3A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
Uanis(C55A) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Cl4) \\sim Ueq, Uanis(Cl4A) \\sim Ueq, Uanis(Cl2A) \\sim Ueq, Uanis(Cl2)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C02E) = Uiso(C02D)
6. Rigid body (RIGU) restrains
 O1A, C1A, C2A, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(ClA)=Sof(Cl1A)=Sof(C65)=Sof(H65)=1-FVAR(1)
 Sof(Cl6)=Sof(Cl7)=Sof(C02S)=Sof(H02S)=FVAR(1)
 Sof(O9A)=Sof(C54A)=Sof(H54C)=Sof(H54D)=Sof(C55A)=Sof(H55A)=Sof(H55B)=
 Sof(C56A)=Sof(H56C)=Sof(H56D)=Sof(C57A)=Sof(H57C)=Sof(H57D)=1-FVAR(2)
 Sof(O9)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(H55C)=Sof(H55D)=Sof(C56)=
 Sof(H56A)=Sof(H56B)=Sof(C57)=Sof(H57A)=Sof(H57B)=FVAR(2)
 Sof(O20)=Sof(H20)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=1-FVAR(3)
 Sof(H02F)=Sof(H02G)=Sof(O023)=FVAR(3)
 Sof(O21)=Sof(H21)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=1-FVAR(4)
 Sof(O02O)=Sof(H02O)=Sof(C02T)=Sof(H02A)=Sof(H02B)=Sof(H02C)=FVAR(4)
 Sof(O1B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=
 1-FVAR(5)
 Sof(O1A)=Sof(C1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=FVAR(5)
 Sof(Cl2A)=Sof(Cl4A)=Sof(C02E)=Sof(H02E)=1-FVAR(6)
 Sof(Cl2)=Sof(Cl4)=Sof(C02D)=Sof(H02D)=FVAR(6)
8.a Free rotating group:
 O02O(H02O), O21(H21), C12A(H12A,H12B,H12C), C69(H69A,H69B,H69C), C70(H70A,
 H70B,H70C)
8.b Ternary CH refined with riding coordinates:
 C02D(H02D), C02E(H02E), C02S(H02S), C65(H65)
8.c Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B),
  C54A(H54C,H54D), C55(H55C,H55D), C55A(H55A,H55B), C56(H56A,H56B), C56A(H56C,
 H56D), C57(H57A,H57B), C57A(H57C,H57D)
8.d Me refined with riding coordinates:
 C2B(H2BA,H2BB,H2BC), C11A(H11A,H11B,H11C)
8.e Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C7(H7), C8(H8), C13(H13), C17(H17), C18(H18), C26(H26),
 C27(H27), C29(H29), C30(H30), C40(H40), C41(H41), C43(H43), C46(H46), C48(H48),
  C49(H49), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64)
8.f Tetrahedral OH refined with riding coordinates:
 O20(H20)
8.g Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
ClA Cl 0.1062(5) 0.9701(5) 0.6982(5) 0.0841(19) Uani 0.331(8) 1 d D U P A 2
Cl1 Cl 0.57030(4) 1.03309(4) 0.76416(4) 0.03213(14) Uani 1 1 d . U . . .
Cl1A Cl 0.1691(6) 0.8852(3) 0.5578(4) 0.084(2) Uani 0.331(8) 1 d D U P A 2
Cl2 Cl 0.8936(6) 1.0478(5) 0.8471(4) 0.0541(12) Uani 0.56(2) 1 d D U P B 1
Cl2A Cl 0.8954(9) 1.0349(8) 0.8252(9) 0.0691(18) Uani 0.44(2) 1 d D U P B 2
Cl3 Cl 0.88450(5) 1.21863(5) 0.82376(4) 0.03670(16) Uani 1 1 d D U . . .
Cl4 Cl 0.8713(5) 1.0478(4) 0.6982(3) 0.0654(15) Uani 0.56(2) 1 d D U P B 1
Cl4A Cl 0.8568(6) 1.0587(7) 0.6876(5) 0.091(2) Uani 0.44(2) 1 d D U P B 2
Cl5 Cl 0.32378(7) 1.00537(6) 0.67996(6) 0.0605(2) Uani 1 1 d D U . . .
Cl6 Cl 0.1221(2) 0.9482(3) 0.6615(3) 0.0895(11) Uani 0.669(8) 1 d D U P A 1
Cl7 Cl 0.2272(4) 0.90077(15) 0.53230(12) 0.0854(11) Uani 0.669(8) 1 d D U P A 1
Na1 Na 0.30035(7) 0.74973(8) 0.83251(6) 0.0289(2) Uani 1 1 d . . . . .
H12 H 0.331(5) 0.581(5) 0.762(4) 0.12(2) Uiso 1 1 d . . . . .
O1 O 0.43198(12) 0.81866(14) 0.95372(10) 0.0282(4) Uani 1 1 d . U . . .
O1A O 0.6781(3) 0.5579(4) 0.7746(3) 0.0459(11) Uani 0.612(7) 1 d D U P C 1
O1B O 0.6501(4) 0.5954(5) 0.7978(3) 0.0299(13) Uani 0.388(7) 1 d D U P C 2
O2 O 0.23231(12) 0.76130(15) 0.94943(10) 0.0304(4) Uani 1 1 d . U . . .
O02O O 0.3167(7) 0.4643(4) 0.6633(3) 0.071(2) Uani 0.599(12) 1 d DG U P D 1
H02O H 0.286413 0.412068 0.664535 0.107 Uiso 0.599(12) 1 d G U P D 1
O3 O 0.12679(12) 0.71112(14) 0.81556(11) 0.0301(4) Uani 1 1 d . U . . .
O4 O 0.23687(12) 0.69130(13) 0.69518(10) 0.0286(4) Uani 1 1 d . U . . .
O5 O 0.42125(13) 0.67268(13) 0.62783(10) 0.0280(4) Uani 1 1 d . U . . .
O6 O 0.39977(12) 0.32737(14) 0.86270(11) 0.0299(4) Uani 1 1 d . U . . .
O7 O 0.22014(13) 0.23040(16) 0.76006(11) 0.0377(5) Uani 1 1 d . U . . .
O8 O 0.11238(16) 0.14600(16) 0.62015(12) 0.0410(5) Uani 1 1 d D U . . .
O9 O 0.2443(2) 0.1398(2) 0.51647(16) 0.0421(8) Uani 0.723(4) 1 d D U P E 1
O9A O 0.2738(6) 0.0922(6) 0.5310(4) 0.0425(15) Uani 0.277(4) 1 d D U P E 2
O10 O 0.45556(17) 0.16279(18) 0.54118(13) 0.0530(6) Uani 1 1 d D U . . .
O11 O 0.34137(16) 0.90396(15) 0.83318(12) 0.0384(5) Uani 1 1 d . U . . .
H11 H 0.395(4) 0.933(4) 0.821(3) 0.079(15) Uiso 1 1 d . . . . .
H02F H 0.302(6) 0.268(5) 0.689(3) 0.119 Uiso 0.806(8) 1 d D U P F 1
H02G H 0.329(6) 0.248(4) 0.619(3) 0.119 Uiso 0.806(8) 1 d D U P F 1
O12 O 0.3184(3) 0.5997(2) 0.80127(16) 0.0744(10) Uani 1 1 d D U . . .
O14 O 0.62187(17) 0.98612(16) 0.79929(14) 0.0458(5) Uani 1 1 d . U . . .
O15 O 0.63337(15) 1.12255(15) 0.77210(15) 0.0453(5) Uani 1 1 d . U . . .
O16 O 0.48645(16) 1.04957(17) 0.80354(14) 0.0492(6) Uani 1 1 d . U . . .
O17 O 0.54189(18) 0.97710(17) 0.68731(13) 0.0502(6) Uani 1 1 d . U . . .
O20 O 0.3875(17) 0.3000(14) 0.6643(10) 0.071(4) Uani 0.194(8) 1 d D U P F 2
H20 H 0.378830 0.249839 0.673030 0.107 Uiso 0.194(8) 1 calc R U P F 2
O21 O 0.2459(11) 0.4525(6) 0.6733(5) 0.071(3) Uani 0.401(12) 1 d DG U P D 2
H21 H 0.246699 0.492196 0.716428 0.107 Uiso 0.401(12) 1 d G U P D 2
O023 O 0.3255(4) 0.2949(3) 0.6592(2) 0.0630(13) Uani 0.806(8) 1 d D U P F 1
N1 N 0.81846(14) 0.74776(14) 0.80020(11) 0.0197(4) Uani 1 1 d . U . . .
H1 H 0.767(3) 0.714(2) 0.7926(18) 0.033(9) Uiso 1 1 d . . . . .
N2 N 0.81642(14) 0.64172(14) 0.91997(11) 0.0184(4) Uani 1 1 d . U . . .
H2 H 0.781(2) 0.623(2) 0.8825(19) 0.027(8) Uiso 1 1 d . . . . .
N3 N 0.81525(15) 0.42859(14) 0.77740(11) 0.0199(4) Uani 1 1 d . U . . .
H3 H 0.761(2) 0.422(2) 0.7703(16) 0.022(7) Uiso 1 1 d . . . . .
N4 N 0.83453(14) 0.54493(14) 0.66194(11) 0.0199(4) Uani 1 1 d . U . . .
H4 H 0.812(2) 0.552(2) 0.701(2) 0.038(9) Uiso 1 1 d . . . . .
C1 C 0.86967(16) 0.75786(16) 0.74173(13) 0.0202(4) Uani 1 1 d . U . . .
C1A C 0.5938(7) 0.5360(6) 0.7619(4) 0.0497(16) Uani 0.612(7) 1 d D U P C 1
C1B C 0.5869(14) 0.5093(9) 0.7459(9) 0.058(2) Uani 0.388(7) 1 d D U P C 2
H1BA H 0.582968 0.520582 0.698202 0.069 Uiso 0.388(7) 1 calc R U P C 2
H1BB H 0.522354 0.509095 0.764139 0.069 Uiso 0.388(7) 1 calc R U P C 2
C2 C 0.95556(17) 0.82326(18) 0.77330(14) 0.0251(5) Uani 1 1 d . U . . .
H2A H 1.006495 0.843519 0.746777 0.030 Uiso 1 1 calc R U . . .
C2A C 0.5481(5) 0.6094(4) 0.7939(3) 0.0483(14) Uani 0.612(7) 1 d D U P C 1
H2AA H 0.535216 0.613800 0.845133 0.073 Uiso 0.612(7) 1 calc R U P C 1
H2AB H 0.486878 0.596330 0.763536 0.073 Uiso 0.612(7) 1 calc R U P C 1
H2AC H 0.590500 0.669120 0.795282 0.073 Uiso 0.612(7) 1 calc R U P C 1
C2B C 0.5920(8) 0.4023(7) 0.7209(6) 0.060(2) Uani 0.388(7) 1 d D U P C 2
H2BA H 0.536440 0.361798 0.684237 0.089 Uiso 0.388(7) 1 calc R U P C 2
H2BB H 0.652171 0.395430 0.698006 0.089 Uiso 0.388(7) 1 calc R U P C 2
H2BC H 0.590661 0.383773 0.764916 0.089 Uiso 0.388(7) 1 calc R U P C 2
C02D C 0.8407(6) 1.0950(5) 0.7925(5) 0.0350(8) Uiso 0.56(2) 1 d D U P B 1
H02D H 0.768758 1.077835 0.792905 0.042 Uiso 0.56(2) 1 calc R U P B 1
C02E C 0.8421(8) 1.0954(7) 0.7804(6) 0.0350(8) Uiso 0.44(2) 1 d D U P B 2
H02E H 0.770982 1.078967 0.784646 0.042 Uiso 0.44(2) 1 calc R U P B 2
C02S C 0.2240(5) 0.9865(5) 0.6195(4) 0.0529(15) Uani 0.669(8) 1 d D U P A 1
H02S H 0.221695 1.046658 0.613021 0.063 Uiso 0.669(8) 1 calc R U P A 1
C02T C 0.2635(16) 0.4506(16) 0.5957(10) 0.071(4) Uani 0.599(12) 1 d D U P D 1
C3 C 0.95513(16) 0.85533(17) 0.85223(14) 0.0229(5) Uani 1 1 d . U . . .
H3A H 1.005565 0.901080 0.888051 0.028 Uiso 1 1 calc R U . . .
C3A C 0.5389(5) 0.4369(5) 0.7148(4) 0.0646(18) Uani 0.612(7) 1 d D U P C 1
H3AA H 0.583730 0.402899 0.685996 0.097 Uiso 0.612(7) 1 calc R U P C 1
H3AB H 0.488629 0.438715 0.680238 0.097 Uiso 0.612(7) 1 calc R U P C 1
H3AC H 0.508773 0.404660 0.747608 0.097 Uiso 0.612(7) 1 calc R U P C 1
C4 C 0.86891(15) 0.80865(15) 0.86796(13) 0.0178(4) Uani 1 1 d . U . . .
C5 C 0.83156(15) 0.81380(16) 0.94256(12) 0.0184(4) Uani 1 1 d . U . . .
C6 C 0.85284(15) 0.73516(16) 0.96405(12) 0.0175(4) Uani 1 1 d . U . . .
C7 C 0.90290(15) 0.73804(17) 1.02718(13) 0.0200(4) Uani 1 1 d . U . . .
H7 H 0.936819 0.793217 1.067432 0.024 Uiso 1 1 calc R U . . .
C8 C 0.89473(16) 0.64320(17) 1.02135(13) 0.0209(4) Uani 1 1 d . U . . .
H8 H 0.922043 0.623938 1.057220 0.025 Uiso 1 1 calc R U . . .
C9 C 0.84045(16) 0.58471(17) 0.95480(13) 0.0190(4) Uani 1 1 d . U . . .
C10 C 0.81043(16) 0.47854(16) 0.91932(12) 0.0190(4) Uani 1 1 d . U . . .
C11 C 0.85984(16) 0.44845(16) 0.84776(12) 0.0184(4) Uani 1 1 d . U . . .
C11A C 0.2806(3) 0.9624(3) 0.8696(2) 0.0564(9) Uani 1 1 d . U . . .
H11A H 0.304213 1.024833 0.866576 0.085 Uiso 1 1 calc R U . . .
H11B H 0.214262 0.934200 0.844968 0.085 Uiso 1 1 calc R U . . .
H11C H 0.281442 0.968402 0.922460 0.085 Uiso 1 1 calc R U . . .
C12 C 0.95246(17) 0.43983(17) 0.83840(14) 0.0225(5) Uani 1 1 d . U . . .
H12D H 0.997(2) 0.451(2) 0.8746(18) 0.032(8) Uiso 1 1 d . . . . .
C12A C 0.3097(5) 0.5419(4) 0.8463(3) 0.0976(18) Uani 1 1 d G U . . .
H12A H 0.356865 0.503602 0.835290 0.146 Uiso 1 1 d DG U . . .
H12B H 0.321495 0.583530 0.899312 0.146 Uiso 1 1 d DG U . . .
H12C H 0.244066 0.500604 0.836180 0.146 Uiso 1 1 d DG U . . .
C13 C 0.96351(17) 0.41222(17) 0.76060(13) 0.0230(5) Uani 1 1 d . U . . .
H13 H 1.020620 0.401225 0.738163 0.028 Uiso 1 1 calc R U . . .
C14 C 0.87691(16) 0.40421(16) 0.72353(13) 0.0199(4) Uani 1 1 d . U . . .
C15 C 0.84812(17) 0.37905(17) 0.64081(13) 0.0221(5) Uani 1 1 d . U . . .
C16 C 0.86762(16) 0.46768(17) 0.62198(12) 0.0203(4) Uani 1 1 d . U . . .
C17 C 0.90956(17) 0.48608(18) 0.56318(14) 0.0245(5) Uani 1 1 d . U . . .
H17 H 0.938815 0.445434 0.525936 0.029 Uiso 1 1 calc R U . . .
C18 C 0.90177(17) 0.57653(18) 0.56748(14) 0.0244(5) Uani 1 1 d . U . . .
H18 H 0.924787 0.607018 0.533649 0.029 Uiso 1 1 calc R U . . .
C20 C 0.82873(17) 0.70502(17) 0.65998(13) 0.0215(4) Uani 1 1 d . U . . .
C21 C 0.88433(17) 0.90858(17) 1.00309(13) 0.0234(5) Uani 1 1 d . U . . .
H21A H 0.871120 0.960191 0.990041 0.035 Uiso 1 1 calc R U . . .
H21B H 0.954209 0.914061 1.005997 0.035 Uiso 1 1 calc R U . . .
H21C H 0.861321 0.911915 1.051811 0.035 Uiso 1 1 calc R U . . .
C22 C 0.84575(18) 0.43722(18) 0.97445(13) 0.0235(5) Uani 1 1 d . U . . .
H22A H 0.816810 0.458496 1.021650 0.035 Uiso 1 1 calc R U . . .
H22B H 0.916488 0.458716 0.984426 0.035 Uiso 1 1 calc R U . . .
H22C H 0.826341 0.368252 0.952224 0.035 Uiso 1 1 calc R U . . .
C23 C 0.9112(2) 0.3159(2) 0.59516(15) 0.0328(6) Uani 1 1 d . U . . .
H23A H 0.900724 0.258691 0.607217 0.049 Uiso 1 1 calc R U . . .
H23B H 0.979661 0.350275 0.607943 0.049 Uiso 1 1 calc R U . . .
H23C H 0.893295 0.298673 0.541365 0.049 Uiso 1 1 calc R U . . .
C24 C 0.8743(2) 0.76573(19) 0.61464(14) 0.0290(5) Uani 1 1 d . U . . .
H24A H 0.944132 0.771181 0.616017 0.044 Uiso 1 1 calc R U . . .
H24B H 0.862863 0.828611 0.636680 0.044 Uiso 1 1 calc R U . . .
H24C H 0.844748 0.735957 0.562442 0.044 Uiso 1 1 calc R U . . .
C25 C 0.72235(15) 0.80870(16) 0.94123(12) 0.0189(4) Uani 1 1 d . U . . .
C26 C 0.67951(17) 0.85560(18) 0.90427(13) 0.0233(5) Uani 1 1 d . U . . .
H26 H 0.717211 0.886283 0.875258 0.028 Uiso 1 1 calc R U . . .
C27 C 0.58338(17) 0.85812(19) 0.90919(14) 0.0259(5) Uani 1 1 d . U . . .
H27 H 0.555959 0.890549 0.883865 0.031 Uiso 1 1 calc R U . . .
C28 C 0.52694(16) 0.81322(18) 0.95117(14) 0.0240(5) Uani 1 1 d . U . . .
C29 C 0.56765(16) 0.76614(18) 0.98839(13) 0.0230(5) Uani 1 1 d . U . . .
H29 H 0.529734 0.735483 1.017317 0.028 Uiso 1 1 calc R U . . .
C30 C 0.66417(16) 0.76435(17) 0.98289(13) 0.0212(4) Uani 1 1 d . U . . .
H30 H 0.691363 0.731891 1.008317 0.025 Uiso 1 1 calc R U . . .
C31 C 0.38606(18) 0.8036(2) 1.01677(15) 0.0318(6) Uani 1 1 d . U . . .
H31A H 0.426963 0.844627 1.064311 0.038 Uiso 1 1 calc R U . . .
H31B H 0.376976 0.737187 1.012262 0.038 Uiso 1 1 calc R U . . .
C32 C 0.28981(18) 0.8267(2) 1.01657(15) 0.0338(6) Uani 1 1 d . U . . .
H32A H 0.257961 0.821477 1.061088 0.041 Uiso 1 1 calc R U . . .
H32B H 0.298443 0.891925 1.017939 0.041 Uiso 1 1 calc R U . . .
C33 C 0.13286(17) 0.7637(2) 0.94773(16) 0.0316(6) Uani 1 1 d . U . . .
H33A H 0.127007 0.826461 0.950194 0.038 Uiso 1 1 calc R U . . .
H33B H 0.104143 0.750996 0.991046 0.038 Uiso 1 1 calc R U . . .
C34 C 0.08186(18) 0.6894(2) 0.87559(17) 0.0331(6) Uani 1 1 d . U . . .
H34A H 0.087049 0.626615 0.873511 0.040 Uiso 1 1 calc R U . . .
H34B H 0.012394 0.688601 0.871668 0.040 Uiso 1 1 calc R U . . .
C35 C 0.09113(19) 0.6388(2) 0.74414(17) 0.0366(6) Uani 1 1 d . U . . .
H35A H 0.019575 0.624393 0.736855 0.044 Uiso 1 1 calc R U . . .
H35B H 0.109794 0.580661 0.741161 0.044 Uiso 1 1 calc R U . . .
C36 C 0.13397(19) 0.6731(2) 0.68476(16) 0.0360(6) Uani 1 1 d . U . . .
H36A H 0.108933 0.624814 0.634407 0.043 Uiso 1 1 calc R U . . .
H36B H 0.115436 0.731373 0.688080 0.043 Uiso 1 1 calc R U . . .
C37 C 0.2799(2) 0.7327(2) 0.64405(16) 0.0323(6) Uani 1 1 d . U . . .
H37A H 0.258533 0.790500 0.650353 0.039 Uiso 1 1 calc R U . . .
H37B H 0.258698 0.688111 0.591833 0.039 Uiso 1 1 calc R U . . .
C38 C 0.38831(19) 0.75673(19) 0.65809(15) 0.0301(5) Uani 1 1 d . U . . .
H38A H 0.417578 0.801908 0.634085 0.036 Uiso 1 1 calc R U . . .
H38B H 0.408558 0.786717 0.712771 0.036 Uiso 1 1 calc R U . . .
C39 C 0.51935(18) 0.68368(18) 0.63715(13) 0.0251(5) Uani 1 1 d . U . . .
C40 C 0.55324(18) 0.60385(18) 0.60215(13) 0.0256(5) Uani 1 1 d . U . . .
H40 H 0.509009 0.545668 0.573455 0.031 Uiso 1 1 calc R U . . .
C41 C 0.65152(18) 0.60968(18) 0.60935(13) 0.0237(5) Uani 1 1 d . U . . .
H41 H 0.673896 0.555192 0.584667 0.028 Uiso 1 1 calc R U . . .
C42 C 0.71845(17) 0.69361(17) 0.65196(13) 0.0220(4) Uani 1 1 d . U . . .
C43 C 0.68270(19) 0.77231(18) 0.68617(14) 0.0273(5) Uani 1 1 d . U . . .
H43 H 0.726727 0.830424 0.715285 0.033 Uiso 1 1 calc R U . . .
C44 C 0.69989(16) 0.43913(16) 0.90222(12) 0.0199(4) Uani 1 1 d . U . . .
C45 C 0.63468(17) 0.49423(18) 0.93010(13) 0.0236(5) Uani 1 1 d . U . . .
C46 C 0.53539(17) 0.45532(18) 0.91479(13) 0.0247(5) Uani 1 1 d . U . . .
H46 H 0.492163 0.494102 0.932769 0.030 Uiso 1 1 calc R U . . .
C47 C 0.49902(17) 0.36011(18) 0.87336(13) 0.0240(5) Uani 1 1 d . U . . .
C48 C 0.56225(17) 0.30341(18) 0.84604(14) 0.0248(5) Uani 1 1 d . U . . .
H48 H 0.537888 0.238045 0.817875 0.030 Uiso 1 1 calc R U . . .
C49 C 0.66143(17) 0.34368(17) 0.86052(13) 0.0228(5) Uani 1 1 d . U . . .
H49 H 0.704408 0.304962 0.841401 0.027 Uiso 1 1 calc R U . . .
C50 C 0.36200(18) 0.2285(2) 0.82459(15) 0.0303(5) Uani 1 1 d . U . . .
H50A H 0.385566 0.193565 0.852535 0.036 Uiso 1 1 calc R U . . .
H50B H 0.383276 0.208640 0.773580 0.036 Uiso 1 1 calc R U . . .
C51 C 0.25385(19) 0.2082(2) 0.81980(16) 0.0336(6) Uani 1 1 d . U . . .
H51A H 0.225739 0.140855 0.811043 0.040 Uiso 1 1 calc R U . . .
H51B H 0.233762 0.246482 0.867572 0.040 Uiso 1 1 calc R U . . .
C52 C 0.1176(2) 0.2135(3) 0.75203(19) 0.0459(7) Uani 1 1 d . U . . .
H52A H 0.096729 0.260930 0.794110 0.055 Uiso 1 1 calc R U . . .
H52B H 0.087083 0.150214 0.752735 0.055 Uiso 1 1 calc R U . . .
C53 C 0.0875(2) 0.2195(3) 0.6796(2) 0.0477(8) Uani 1 1 d . U . . .
H53A H 0.016802 0.212714 0.674309 0.057 Uiso 1 1 calc R U . . .
H53B H 0.120911 0.281537 0.677720 0.057 Uiso 1 1 calc R U . . .
C54 C 0.0885(3) 0.1511(3) 0.5516(2) 0.0365(9) Uani 0.723(4) 1 d D U P E 1
H54A H 0.106444 0.217266 0.554431 0.044 Uiso 0.723(4) 1 calc R U P E 1
H54B H 0.018067 0.125026 0.536298 0.044 Uiso 0.723(4) 1 calc R U P E 1
C54A C 0.1385(10) 0.1593(9) 0.5428(6) 0.0409(17) Uani 0.277(4) 1 d D U P E 2
H54C H 0.078854 0.158201 0.514926 0.049 Uiso 0.277(4) 1 calc R U P E 2
H54D H 0.184479 0.221462 0.553752 0.049 Uiso 0.277(4) 1 calc R U P E 2
C55 C 0.1442(3) 0.0943(3) 0.4971(3) 0.0350(9) Uani 0.723(4) 1 d D U P E 1
H55C H 0.131396 0.030128 0.498809 0.042 Uiso 0.723(4) 1 calc R U P E 1
H55D H 0.124138 0.088633 0.445511 0.042 Uiso 0.723(4) 1 calc R U P E 1
C55A C 0.1825(10) 0.0835(10) 0.4945(7) 0.0398(18) Uani 0.277(4) 1 d D U P E 2
H55A H 0.139087 0.020739 0.486157 0.048 Uiso 0.277(4) 1 calc R U P E 2
H55B H 0.191187 0.089716 0.444992 0.048 Uiso 0.277(4) 1 calc R U P E 2
H02A H 0.304(4) 0.420(4) 0.561(2) 0.060 Uiso 0.599(12) 1 d D U P D 1
H02B H 0.266(4) 0.514(3) 0.600(3) 0.060 Uiso 0.599(12) 1 d D U P D 1
H02C H 0.204(3) 0.411(4) 0.597(3) 0.060 Uiso 0.599(12) 1 d D U P D 1
C56 C 0.3048(3) 0.1021(3) 0.4614(2) 0.0409(9) Uani 0.723(4) 1 d D U P E 1
H56A H 0.277199 0.093919 0.410958 0.049 Uiso 0.723(4) 1 calc R U P E 1
H56B H 0.308969 0.039653 0.461063 0.049 Uiso 0.723(4) 1 calc R U P E 1
C56A C 0.3331(8) 0.0400(10) 0.4842(7) 0.054(2) Uani 0.277(4) 1 d D U P E 2
H56C H 0.335112 0.051061 0.436241 0.065 Uiso 0.277(4) 1 calc R U P E 2
H56D H 0.306034 -0.028154 0.472861 0.065 Uiso 0.277(4) 1 calc R U P E 2
C57 C 0.4041(3) 0.1686(3) 0.4800(2) 0.0394(9) Uani 0.723(4) 1 d D U P E 1
H57A H 0.440654 0.153219 0.435552 0.047 Uiso 0.723(4) 1 calc R U P E 1
H57B H 0.398092 0.233893 0.492497 0.047 Uiso 0.723(4) 1 calc R U P E 1
C57A C 0.4341(9) 0.0708(9) 0.5241(8) 0.054(3) Uani 0.277(4) 1 d D U P E 2
H57C H 0.434880 0.054691 0.569819 0.065 Uiso 0.277(4) 1 calc R U P E 2
H57D H 0.479500 0.041828 0.490738 0.065 Uiso 0.277(4) 1 calc R U P E 2
C58 C 0.5494(2) 0.2161(2) 0.56458(17) 0.0413(7) Uani 1 1 d . U . . .
C59 C 0.5900(2) 0.2877(2) 0.53945(15) 0.0346(6) Uani 1 1 d . U . . .
H59 H 0.553374 0.300668 0.504149 0.042 Uiso 1 1 calc R U . . .
C60 C 0.68460(19) 0.3409(2) 0.56585(14) 0.0288(5) Uani 1 1 d . U . . .
H60 H 0.711441 0.390068 0.548159 0.035 Uiso 1 1 calc R U . . .
C61 C 0.74116(19) 0.32440(18) 0.61728(13) 0.0259(5) Uani 1 1 d . U . . .
C62 C 0.6990(2) 0.2514(2) 0.64201(17) 0.0408(7) Uani 1 1 d . U . . .
H62 H 0.735867 0.238025 0.676925 0.049 Uiso 1 1 calc R U . . .
C63 C 0.6040(3) 0.1978(2) 0.61649(19) 0.0492(8) Uani 1 1 d . U . . .
H63 H 0.576544 0.148924 0.634372 0.059 Uiso 1 1 calc R U . . .
C64 C 0.58449(19) 0.76815(19) 0.67890(15) 0.0291(5) Uani 1 1 d . U . . .
H64 H 0.562173 0.822968 0.702444 0.035 Uiso 1 1 calc R U . . .
C65 C 0.2011(10) 0.9842(12) 0.6394(9) 0.061(2) Uani 0.331(8) 1 d D U P A 2
H65 H 0.198245 1.039569 0.625553 0.073 Uiso 0.331(8) 1 calc R U P A 2
C66 C 0.85512(16) 0.61200(17) 0.62915(13) 0.0204(4) Uani 1 1 d . U . . .
C69 C 0.3420(16) 0.3587(14) 0.7124(11) 0.059(4) Uani 0.194(8) 1 d DG U P F 2
H69A H 0.303685 0.382927 0.684383 0.088 Uiso 0.194(8) 1 d DG U P F 2
H69B H 0.299166 0.324362 0.738741 0.088 Uiso 0.194(8) 1 d DG U P F 2
H69C H 0.390127 0.411308 0.749097 0.088 Uiso 0.194(8) 1 d DG U P F 2
C70 C 0.246(3) 0.461(2) 0.6014(15) 0.067(4) Uani 0.401(12) 1 d DG U P D 2
H70A H 0.239928 0.401620 0.559221 0.101 Uiso 0.401(12) 1 d G U P D 2
H70B H 0.183492 0.476623 0.606242 0.101 Uiso 0.401(12) 1 d G U P D 2
H70C H 0.293715 0.511478 0.592237 0.101 Uiso 0.401(12) 1 d G U P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
ClA C65 1.796(16) . ?
Cl1 O14 1.453(2) . ?
Cl1 O15 1.434(2) . ?
Cl1 O16 1.449(2) . ?
Cl1 O17 1.416(2) . ?
Cl1A C65 1.733(15) . ?
Cl2 C02D 1.725(8) . ?
Cl2A C02E 1.758(10) . ?
Cl3 C02D 1.765(8) . ?
Cl3 C02E 1.760(10) . ?
Cl4 C02D 1.798(8) . ?
Cl4A C02E 1.696(10) . ?
Cl5 C02S 1.722(7) . ?
Cl5 C65 1.813(14) . ?
Cl6 C02S 1.756(7) . ?
Cl7 C02S 1.746(7) . ?
Na1 H12 2.66(7) . ?
Na1 O1 2.689(2) . ?
Na1 O2 2.415(2) . ?
Na1 O3 2.3980(19) . ?
Na1 O4 2.531(2) . ?
Na1 O11 2.344(2) . ?
Na1 O12 2.291(3) . ?
O1 C28 1.378(3) . ?
O1 C31 1.445(3) . ?
O1A C1A 1.168(10) . ?
O1B C1B 1.445(14) . ?
O2 C32 1.424(3) . ?
O2 C33 1.429(3) . ?
O02O H02O 0.8402 . ?
O02O C02T 1.41(2) . ?
O3 C34 1.427(3) . ?
O3 C35 1.426(3) . ?
O4 C36 1.426(3) . ?
O4 C37 1.424(3) . ?
O5 C38 1.433(3) . ?
O5 C39 1.371(3) . ?
O6 C47 1.376(3) . ?
O6 C50 1.425(3) . ?
O7 C51 1.411(3) . ?
O7 C52 1.422(3) . ?
O8 C53 1.425(4) . ?
O8 C54 1.381(4) . ?
O8 C54A 1.600(12) . ?
O9 C55 1.419(5) . ?
O9 C56 1.426(5) . ?
O9A C55A 1.423(14) . ?
O9A C56A 1.421(16) . ?
O10 C57 1.411(5) . ?
O10 C57A 1.319(14) . ?
O10 C58 1.375(4) . ?
O11 H11 0.88(5) . ?
O11 C11A 1.420(4) . ?
O12 H12 0.75(6) . ?
O12 C12A 1.438(5) . ?
O20 H20 0.8400 . ?
O20 C69 1.35(2) . ?
O21 H21 0.8401 . ?
O21 C70 1.43(3) . ?
O023 H02F 0.86(3) . ?
O023 H02G 0.86(3) . ?
N1 H1 0.78(4) . ?
N1 C1 1.379(3) . ?
N1 C4 1.376(3) . ?
N2 H2 0.79(3) . ?
N2 C6 1.376(3) . ?
N2 C9 1.381(3) . ?
N3 H3 0.76(3) . ?
N3 C11 1.378(3) . ?
N3 C14 1.375(3) . ?
N4 H4 0.79(4) . ?
N4 C16 1.379(3) . ?
N4 C66 1.379(3) . ?
C1 C2 1.370(3) . ?
C1 C20 1.520(3) . ?
C1A C2A 1.410(10) . ?
C1A C3A 1.507(9) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C1B C2B 1.594(16) . ?
C2 H2A 0.9500 . ?
C2 C3 1.414(3) . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C02D H02D 1.0000 . ?
C02E H02E 1.0000 . ?
C02S H02S 1.0000 . ?
C02T H02A 0.96(3) . ?
C02T H02B 0.96(3) . ?
C02T H02C 0.93(3) . ?
C3 H3A 0.9500 . ?
C3 C4 1.373(3) . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4 C5 1.512(3) . ?
C5 C6 1.516(3) . ?
C5 C21 1.537(3) . ?
C5 C25 1.542(3) . ?
C6 C7 1.374(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.427(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.372(3) . ?
C9 C10 1.510(3) . ?
C10 C11 1.524(3) . ?
C10 C22 1.547(3) . ?
C10 C44 1.539(3) . ?
C11 C12 1.368(3) . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11C 0.9800 . ?
C12 H12D 0.88(3) . ?
C12 C13 1.418(3) . ?
C12A H12A 0.9801 . ?
C12A H12B 0.9801 . ?
C12A H12C 0.9798 . ?
C13 H13 0.9500 . ?
C13 C14 1.372(3) . ?
C14 C15 1.514(3) . ?
C15 C16 1.518(3) . ?
C15 C23 1.545(3) . ?
C15 C61 1.539(3) . ?
C16 C17 1.367(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.420(4) . ?
C18 H18 0.9500 . ?
C18 C66 1.371(3) . ?
C20 C24 1.543(3) . ?
C20 C42 1.542(3) . ?
C20 C66 1.508(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.403(3) . ?
C25 C30 1.394(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.386(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.392(3) . ?
C28 C29 1.392(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.389(3) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.500(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.496(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.497(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.501(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.397(3) . ?
C39 C64 1.385(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.386(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.396(3) . ?
C42 C43 1.395(3) . ?
C43 H43 0.9500 . ?
C43 C64 1.391(4) . ?
C44 C45 1.401(3) . ?
C44 C49 1.394(3) . ?
C45 C46 1.388(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.387(4) . ?
C47 C48 1.392(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.389(3) . ?
C49 H49 0.9500 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.497(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.484(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C55 1.488(7) . ?
C54A H54C 0.9900 . ?
C54A H54D 0.9900 . ?
C54A C55A 1.502(17) . ?
C55 H55C 0.9900 . ?
C55 H55D 0.9900 . ?
C55A H55A 0.9900 . ?
C55A H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.504(5) . ?
C56A H56C 0.9900 . ?
C56A H56D 0.9900 . ?
C56A C57A 1.508(15) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57A H57C 0.9900 . ?
C57A H57D 0.9900 . ?
C58 C59 1.381(4) . ?
C58 C63 1.397(4) . ?
C59 H59 0.9500 . ?
C59 C60 1.391(4) . ?
C60 H60 0.9500 . ?
C60 C61 1.390(4) . ?
C61 C62 1.400(4) . ?
C62 H62 0.9500 . ?
C62 C63 1.395(4) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
C65 H65 1.0000 . ?
C69 H69A 0.9801 . ?
C69 H69B 0.9802 . ?
C69 H69C 0.9799 . ?
C70 H70A 0.9799 . ?
C70 H70B 0.9799 . ?
C70 H70C 0.9799 . ?

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
O15 Cl1 O14 108.21(14) . . ?
O15 Cl1 O16 108.38(13) . . ?
O16 Cl1 O14 108.78(15) . . ?
O17 Cl1 O14 110.12(14) . . ?
O17 Cl1 O15 110.60(15) . . ?
O17 Cl1 O16 110.68(15) . . ?
O1 Na1 H12 101.7(15) . . ?
O2 Na1 H12 112.4(14) . . ?
O2 Na1 O1 65.55(6) . . ?
O2 Na1 O4 136.62(7) . . ?
O3 Na1 H12 100.4(15) . . ?
O3 Na1 O1 133.78(7) . . ?
O3 Na1 O2 68.58(7) . . ?
O3 Na1 O4 68.44(7) . . ?
O4 Na1 H12 70.4(14) . . ?
O4 Na1 O1 157.75(7) . . ?
O11 Na1 H12 141.2(14) . . ?
O11 Na1 O1 84.91(8) . . ?
O11 Na1 O2 105.21(8) . . ?
O11 Na1 O3 101.95(8) . . ?
O11 Na1 O4 89.06(8) . . ?
O12 Na1 H12 15.4(14) . . ?
O12 Na1 O1 93.18(10) . . ?
O12 Na1 O2 97.26(11) . . ?
O12 Na1 O3 97.89(12) . . ?
O12 Na1 O4 83.03(9) . . ?
O12 Na1 O11 154.20(13) . . ?
C28 O1 Na1 124.11(14) . . ?
C28 O1 C31 115.59(18) . . ?
C31 O1 Na1 109.47(14) . . ?
C32 O2 Na1 116.99(15) . . ?
C32 O2 C33 113.6(2) . . ?
C33 O2 Na1 113.99(15) . . ?
C02T O02O H02O 93.3 . . ?
C34 O3 Na1 113.83(15) . . ?
C35 O3 Na1 110.41(15) . . ?
C35 O3 C34 112.4(2) . . ?
C36 O4 Na1 112.03(15) . . ?
C37 O4 Na1 123.19(16) . . ?
C37 O4 C36 110.3(2) . . ?
C39 O5 C38 116.2(2) . . ?
C47 O6 C50 116.5(2) . . ?
C51 O7 C52 112.3(2) . . ?
C53 O8 C54A 120.5(5) . . ?
C54 O8 C53 110.3(3) . . ?
C55 O9 C56 114.3(3) . . ?
C56A O9A C55A 114.6(9) . . ?
C57A O10 C58 120.6(6) . . ?
C58 O10 C57 119.6(3) . . ?
Na1 O11 H11 127(3) . . ?
C11A O11 Na1 116.3(2) . . ?
C11A O11 H11 116(3) . . ?
Na1 O12 H12 111(5) . . ?
C12A O12 Na1 129.1(3) . . ?
C12A O12 H12 120(5) . . ?
C69 O20 H20 109.5 . . ?
C70 O21 H21 131.2 . . ?
H02F O023 H02G 103(4) . . ?
C1 N1 H1 121(2) . . ?
C4 N1 H1 128(2) . . ?
C4 N1 C1 110.32(19) . . ?
C6 N2 H2 125(2) . . ?
C6 N2 C9 110.44(19) . . ?
C9 N2 H2 124(2) . . ?
C11 N3 H3 122(2) . . ?
C14 N3 H3 126(2) . . ?
C14 N3 C11 110.60(19) . . ?
C16 N4 H4 124(3) . . ?
C16 N4 C66 110.38(19) . . ?
C66 N4 H4 125(3) . . ?
N1 C1 C20 122.3(2) . . ?
C2 C1 N1 106.8(2) . . ?
C2 C1 C20 130.9(2) . . ?
O1A C1A C2A 114.8(8) . . ?
O1A C1A C3A 122.1(8) . . ?
C2A C1A C3A 123.1(8) . . ?
O1B C1B H1BA 104.4 . . ?
O1B C1B H1BB 104.4 . . ?
O1B C1B C2B 131.6(14) . . ?
H1BA C1B H1BB 105.6 . . ?
C2B C1B H1BA 104.4 . . ?
C2B C1B H1BB 104.4 . . ?
C1 C2 H2A 126.0 . . ?
C1 C2 C3 108.1(2) . . ?
C3 C2 H2A 126.0 . . ?
C1A C2A H2AA 109.5 . . ?
C1A C2A H2AB 109.5 . . ?
C1A C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C1B C2B H2BA 109.5 . . ?
C1B C2B H2BB 109.5 . . ?
C1B C2B H2BC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
Cl2 C02D Cl3 111.9(5) . . ?
Cl2 C02D Cl4 108.5(5) . . ?
Cl2 C02D H02D 109.8 . . ?
Cl3 C02D Cl4 107.2(4) . . ?
Cl3 C02D H02D 109.8 . . ?
Cl4 C02D H02D 109.8 . . ?
Cl2A C02E Cl3 112.6(6) . . ?
Cl2A C02E H02E 107.2 . . ?
Cl3 C02E H02E 107.2 . . ?
Cl4A C02E Cl2A 110.9(7) . . ?
Cl4A C02E Cl3 111.4(6) . . ?
Cl4A C02E H02E 107.2 . . ?
Cl5 C02S Cl6 106.5(4) . . ?
Cl5 C02S Cl7 110.7(5) . . ?
Cl5 C02S H02S 109.8 . . ?
Cl6 C02S H02S 109.8 . . ?
Cl7 C02S Cl6 110.2(4) . . ?
Cl7 C02S H02S 109.8 . . ?
O02O C02T H02A 99(3) . . ?
O02O C02T H02B 102(3) . . ?
O02O C02T H02C 104(3) . . ?
H02A C02T H02B 116(4) . . ?
H02A C02T H02C 114(4) . . ?
H02B C02T H02C 118(4) . . ?
C2 C3 H3A 126.0 . . ?
C4 C3 C2 107.9(2) . . ?
C4 C3 H3A 126.0 . . ?
C1A C3A H3AA 109.5 . . ?
C1A C3A H3AB 109.5 . . ?
C1A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N1 C4 C5 122.78(19) . . ?
C3 C4 N1 106.8(2) . . ?
C3 C4 C5 130.3(2) . . ?
C4 C5 C6 109.43(18) . . ?
C4 C5 C21 109.03(18) . . ?
C4 C5 C25 112.26(18) . . ?
C6 C5 C21 108.50(18) . . ?
C6 C5 C25 110.41(18) . . ?
C21 C5 C25 107.11(18) . . ?
N2 C6 C5 122.07(19) . . ?
C7 C6 N2 107.1(2) . . ?
C7 C6 C5 130.7(2) . . ?
C6 C7 H7 126.2 . . ?
C6 C7 C8 107.6(2) . . ?
C8 C7 H7 126.2 . . ?
C7 C8 H8 126.0 . . ?
C9 C8 C7 107.9(2) . . ?
C9 C8 H8 126.0 . . ?
N2 C9 C10 122.2(2) . . ?
C8 C9 N2 106.9(2) . . ?
C8 C9 C10 130.9(2) . . ?
C9 C10 C11 108.41(18) . . ?
C9 C10 C22 108.63(18) . . ?
C9 C10 C44 112.75(18) . . ?
C11 C10 C22 108.66(18) . . ?
C11 C10 C44 110.61(18) . . ?
C44 C10 C22 107.69(18) . . ?
N3 C11 C10 123.15(19) . . ?
C12 C11 N3 106.7(2) . . ?
C12 C11 C10 130.1(2) . . ?
O11 C11A H11A 109.5 . . ?
O11 C11A H11B 109.5 . . ?
O11 C11A H11C 109.5 . . ?
H11A C11A H11B 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
C11 C12 H12D 126(2) . . ?
C11 C12 C13 108.2(2) . . ?
C13 C12 H12D 126(2) . . ?
O12 C12A H12A 111.0 . . ?
O12 C12A H12B 108.1 . . ?
O12 C12A H12C 109.2 . . ?
H12A C12A H12B 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C12 C13 H13 126.1 . . ?
C14 C13 C12 107.7(2) . . ?
C14 C13 H13 126.1 . . ?
N3 C14 C15 122.6(2) . . ?
C13 C14 N3 106.8(2) . . ?
C13 C14 C15 130.5(2) . . ?
C14 C15 C16 109.98(19) . . ?
C14 C15 C23 108.37(19) . . ?
C14 C15 C61 112.18(19) . . ?
C16 C15 C23 108.1(2) . . ?
C16 C15 C61 110.02(19) . . ?
C61 C15 C23 108.1(2) . . ?
N4 C16 C15 122.4(2) . . ?
C17 C16 N4 106.8(2) . . ?
C17 C16 C15 130.5(2) . . ?
C16 C17 H17 125.9 . . ?
C16 C17 C18 108.1(2) . . ?
C18 C17 H17 125.9 . . ?
C17 C18 H18 126.1 . . ?
C66 C18 C17 107.8(2) . . ?
C66 C18 H18 126.1 . . ?
C1 C20 C24 107.8(2) . . ?
C1 C20 C42 109.93(18) . . ?
C42 C20 C24 107.35(19) . . ?
C66 C20 C1 110.96(19) . . ?
C66 C20 C24 108.19(19) . . ?
C66 C20 C42 112.4(2) . . ?
C5 C21 H21A 109.5 . . ?
C5 C21 H21B 109.5 . . ?
C5 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C22 H22A 109.5 . . ?
C10 C22 H22B 109.5 . . ?
C10 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C15 C23 H23A 109.5 . . ?
C15 C23 H23B 109.5 . . ?
C15 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 H24A 109.5 . . ?
C20 C24 H24B 109.5 . . ?
C20 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C5 121.7(2) . . ?
C30 C25 C5 120.7(2) . . ?
C30 C25 C26 117.3(2) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 C25 121.4(2) . . ?
C27 C26 H26 119.3 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 120.1(2) . . ?
C28 C27 H27 120.0 . . ?
O1 C28 C27 117.0(2) . . ?
O1 C28 C29 123.3(2) . . ?
C27 C28 C29 119.7(2) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 C28 119.5(2) . . ?
C30 C29 H29 120.3 . . ?
C25 C30 H30 119.0 . . ?
C29 C30 C25 122.0(2) . . ?
C29 C30 H30 119.0 . . ?
O1 C31 H31A 110.1 . . ?
O1 C31 H31B 110.1 . . ?
O1 C31 C32 107.8(2) . . ?
H31A C31 H31B 108.5 . . ?
C32 C31 H31A 110.1 . . ?
C32 C31 H31B 110.1 . . ?
O2 C32 C31 107.3(2) . . ?
O2 C32 H32A 110.2 . . ?
O2 C32 H32B 110.2 . . ?
C31 C32 H32A 110.2 . . ?
C31 C32 H32B 110.2 . . ?
H32A C32 H32B 108.5 . . ?
O2 C33 H33A 110.3 . . ?
O2 C33 H33B 110.3 . . ?
O2 C33 C34 107.2(2) . . ?
H33A C33 H33B 108.5 . . ?
C34 C33 H33A 110.3 . . ?
C34 C33 H33B 110.3 . . ?
O3 C34 C33 107.6(2) . . ?
O3 C34 H34A 110.2 . . ?
O3 C34 H34B 110.2 . . ?
C33 C34 H34A 110.2 . . ?
C33 C34 H34B 110.2 . . ?
H34A C34 H34B 108.5 . . ?
O3 C35 H35A 110.1 . . ?
O3 C35 H35B 110.1 . . ?
O3 C35 C36 108.1(2) . . ?
H35A C35 H35B 108.4 . . ?
C36 C35 H35A 110.1 . . ?
C36 C35 H35B 110.1 . . ?
O4 C36 C35 109.2(2) . . ?
O4 C36 H36A 109.8 . . ?
O4 C36 H36B 109.8 . . ?
C35 C36 H36A 109.8 . . ?
C35 C36 H36B 109.8 . . ?
H36A C36 H36B 108.3 . . ?
O4 C37 H37A 109.6 . . ?
O4 C37 H37B 109.6 . . ?
O4 C37 C38 110.1(2) . . ?
H37A C37 H37B 108.2 . . ?
C38 C37 H37A 109.6 . . ?
C38 C37 H37B 109.6 . . ?
O5 C38 C37 109.6(2) . . ?
O5 C38 H38A 109.8 . . ?
O5 C38 H38B 109.8 . . ?
C37 C38 H38A 109.8 . . ?
C37 C38 H38B 109.8 . . ?
H38A C38 H38B 108.2 . . ?
O5 C39 C40 116.7(2) . . ?
O5 C39 C64 123.7(2) . . ?
C64 C39 C40 119.6(2) . . ?
C39 C40 H40 120.1 . . ?
C41 C40 C39 119.9(2) . . ?
C41 C40 H40 120.1 . . ?
C40 C41 H41 119.2 . . ?
C40 C41 C42 121.6(2) . . ?
C42 C41 H41 119.2 . . ?
C41 C42 C20 123.9(2) . . ?
C43 C42 C20 118.7(2) . . ?
C43 C42 C41 117.3(2) . . ?
C42 C43 H43 119.0 . . ?
C64 C43 C42 121.9(2) . . ?
C64 C43 H43 119.0 . . ?
C45 C44 C10 122.8(2) . . ?
C49 C44 C10 119.5(2) . . ?
C49 C44 C45 117.6(2) . . ?
C46 C45 C44 120.9(2) . . ?
C45 C46 H46 119.9 . . ?
C47 C46 C45 120.3(2) . . ?
C47 C46 H46 119.9 . . ?
O6 C47 C46 116.2(2) . . ?
O6 C47 C48 123.9(2) . . ?
C46 C47 C48 119.9(2) . . ?
C47 C48 H48 120.4 . . ?
C49 C48 C47 119.1(2) . . ?
C49 C48 H48 120.4 . . ?
C44 C49 H49 119.0 . . ?
C48 C49 C44 122.1(2) . . ?
C48 C49 H49 119.0 . . ?
O6 C50 H50A 110.2 . . ?
O6 C50 H50B 110.2 . . ?
O6 C50 C51 107.6(2) . . ?
H50A C50 H50B 108.5 . . ?
C51 C50 H50A 110.2 . . ?
C51 C50 H50B 110.2 . . ?
O7 C51 C50 108.9(2) . . ?
O7 C51 H51A 109.9 . . ?
O7 C51 H51B 109.9 . . ?
C50 C51 H51A 109.9 . . ?
C50 C51 H51B 109.9 . . ?
H51A C51 H51B 108.3 . . ?
O7 C52 H52A 110.0 . . ?
O7 C52 H52B 110.0 . . ?
O7 C52 C53 108.4(3) . . ?
H52A C52 H52B 108.4 . . ?
C53 C52 H52A 110.0 . . ?
C53 C52 H52B 110.0 . . ?
O8 C53 C52 108.4(3) . . ?
O8 C53 H53A 110.0 . . ?
O8 C53 H53B 110.0 . . ?
C52 C53 H53A 110.0 . . ?
C52 C53 H53B 110.0 . . ?
H53A C53 H53B 108.4 . . ?
O8 C54 H54A 110.5 . . ?
O8 C54 H54B 110.5 . . ?
O8 C54 C55 106.1(3) . . ?
H54A C54 H54B 108.7 . . ?
C55 C54 H54A 110.5 . . ?
C55 C54 H54B 110.5 . . ?
O8 C54A H54C 109.2 . . ?
O8 C54A H54D 109.2 . . ?
H54C C54A H54D 107.9 . . ?
C55A C54A O8 112.0(9) . . ?
C55A C54A H54C 109.2 . . ?
C55A C54A H54D 109.2 . . ?
O9 C55 C54 108.6(4) . . ?
O9 C55 H55C 110.0 . . ?
O9 C55 H55D 110.0 . . ?
C54 C55 H55C 110.0 . . ?
C54 C55 H55D 110.0 . . ?
H55C C55 H55D 108.4 . . ?
O9A C55A C54A 109.1(10) . . ?
O9A C55A H55A 109.9 . . ?
O9A C55A H55B 109.9 . . ?
C54A C55A H55A 109.9 . . ?
C54A C55A H55B 109.9 . . ?
H55A C55A H55B 108.3 . . ?
O9 C56 H56A 109.9 . . ?
O9 C56 H56B 109.9 . . ?
O9 C56 C57 108.9(3) . . ?
H56A C56 H56B 108.3 . . ?
C57 C56 H56A 109.9 . . ?
C57 C56 H56B 109.9 . . ?
O9A C56A H56C 109.9 . . ?
O9A C56A H56D 109.9 . . ?
O9A C56A C57A 109.1(10) . . ?
H56C C56A H56D 108.3 . . ?
C57A C56A H56C 109.9 . . ?
C57A C56A H56D 109.9 . . ?
O10 C57 C56 111.2(3) . . ?
O10 C57 H57A 109.4 . . ?
O10 C57 H57B 109.4 . . ?
C56 C57 H57A 109.4 . . ?
C56 C57 H57B 109.4 . . ?
H57A C57 H57B 108.0 . . ?
O10 C57A C56A 102.2(11) . . ?
O10 C57A H57C 111.3 . . ?
O10 C57A H57D 111.3 . . ?
C56A C57A H57C 111.3 . . ?
C56A C57A H57D 111.3 . . ?
H57C C57A H57D 109.2 . . ?
O10 C58 C59 122.1(3) . . ?
O10 C58 C63 118.5(3) . . ?
C59 C58 C63 119.4(3) . . ?
C58 C59 H59 120.0 . . ?
C58 C59 C60 119.9(3) . . ?
C60 C59 H59 120.0 . . ?
C59 C60 H60 118.9 . . ?
C61 C60 C59 122.1(3) . . ?
C61 C60 H60 118.9 . . ?
C60 C61 C15 121.0(2) . . ?
C60 C61 C62 117.2(2) . . ?
C62 C61 C15 121.6(2) . . ?
C61 C62 H62 119.3 . . ?
C63 C62 C61 121.4(3) . . ?
C63 C62 H62 119.3 . . ?
C58 C63 H63 120.1 . . ?
C62 C63 C58 119.9(3) . . ?
C62 C63 H63 120.1 . . ?
C39 C64 C43 119.7(2) . . ?
C39 C64 H64 120.2 . . ?
C43 C64 H64 120.2 . . ?
ClA C65 Cl5 116.8(9) . . ?
ClA C65 H65 107.1 . . ?
Cl1A C65 ClA 105.7(8) . . ?
Cl1A C65 Cl5 112.6(9) . . ?
Cl1A C65 H65 107.1 . . ?
Cl5 C65 H65 107.1 . . ?
N4 C66 C20 123.2(2) . . ?
C18 C66 N4 106.8(2) . . ?
C18 C66 C20 130.0(2) . . ?
O20 C69 H69A 109.4 . . ?
O20 C69 H69B 109.5 . . ?
O20 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
O21 C70 H70A 114.2 . . ?
O21 C70 H70B 90.8 . . ?
O21 C70 H70C 121.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 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
Na1 O1 C28 C27 61.5(3) . . . . ?
Na1 O1 C28 C29 -118.9(2) . . . . ?
Na1 O1 C31 C32 -42.6(3) . . . . ?
Na1 O2 C32 C31 -54.6(3) . . . . ?
Na1 O2 C33 C34 44.5(2) . . . . ?
Na1 O3 C34 C33 46.8(2) . . . . ?
Na1 O3 C35 C36 -58.2(2) . . . . ?
Na1 O4 C36 C35 -33.1(3) . . . . ?
Na1 O4 C37 C38 40.8(3) . . . . ?
O1 C28 C29 C30 -179.9(2) . . . . ?
O1 C31 C32 O2 63.8(3) . . . . ?
O2 C33 C34 O3 -59.5(3) . . . . ?
O3 C35 C36 O4 61.1(3) . . . . ?
O4 C37 C38 O5 76.5(3) . . . . ?
O5 C39 C40 C41 -179.8(2) . . . . ?
O5 C39 C64 C43 179.0(2) . . . . ?
O6 C47 C48 C49 -179.6(2) . . . . ?
O6 C50 C51 O7 79.9(3) . . . . ?
O7 C52 C53 O8 63.8(4) . . . . ?
O8 C54 C55 O9 -66.5(4) . . . . ?
O8 C54A C55A O9A -65.6(13) . . . . ?
O9 C56 C57 O10 75.2(5) . . . . ?
O9A C56A C57A O10 -53.8(13) . . . . ?
O10 C58 C59 C60 178.8(3) . . . . ?
O10 C58 C63 C62 -179.2(3) . . . . ?
N1 C1 C2 C3 -1.7(3) . . . . ?
N1 C1 C20 C24 151.1(2) . . . . ?
N1 C1 C20 C42 34.4(3) . . . . ?
N1 C1 C20 C66 -90.6(3) . . . . ?
N1 C4 C5 C6 81.2(2) . . . . ?
N1 C4 C5 C21 -160.2(2) . . . . ?
N1 C4 C5 C25 -41.7(3) . . . . ?
N2 C6 C7 C8 -1.1(2) . . . . ?
N2 C9 C10 C11 64.2(3) . . . . ?
N2 C9 C10 C22 -177.9(2) . . . . ?
N2 C9 C10 C44 -58.6(3) . . . . ?
N3 C11 C12 C13 -1.3(3) . . . . ?
N3 C14 C15 C16 86.6(3) . . . . ?
N3 C14 C15 C23 -155.5(2) . . . . ?
N3 C14 C15 C61 -36.2(3) . . . . ?
N4 C16 C17 C18 0.0(3) . . . . ?
C1 N1 C4 C3 -2.4(3) . . . . ?
C1 N1 C4 C5 -179.7(2) . . . . ?
C1 C2 C3 C4 0.3(3) . . . . ?
C1 C20 C42 C41 -135.0(2) . . . . ?
C1 C20 C42 C43 48.1(3) . . . . ?
C1 C20 C66 N4 55.0(3) . . . . ?
C1 C20 C66 C18 -124.6(3) . . . . ?
C2 C1 C20 C24 -26.3(3) . . . . ?
C2 C1 C20 C42 -143.0(3) . . . . ?
C2 C1 C20 C66 92.0(3) . . . . ?
C2 C3 C4 N1 1.3(3) . . . . ?
C2 C3 C4 C5 178.3(2) . . . . ?
C3 C4 C5 C6 -95.4(3) . . . . ?
C3 C4 C5 C21 23.1(3) . . . . ?
C3 C4 C5 C25 141.6(2) . . . . ?
C4 N1 C1 C2 2.6(3) . . . . ?
C4 N1 C1 C20 -175.4(2) . . . . ?
C4 C5 C6 N2 -60.3(3) . . . . ?
C4 C5 C6 C7 123.6(2) . . . . ?
C4 C5 C25 C26 -40.1(3) . . . . ?
C4 C5 C25 C30 146.0(2) . . . . ?
C5 C6 C7 C8 175.5(2) . . . . ?
C5 C25 C26 C27 -173.8(2) . . . . ?
C5 C25 C30 C29 173.9(2) . . . . ?
C6 N2 C9 C8 -1.2(2) . . . . ?
C6 N2 C9 C10 -179.76(19) . . . . ?
C6 C5 C25 C26 -162.5(2) . . . . ?
C6 C5 C25 C30 23.6(3) . . . . ?
C6 C7 C8 C9 0.3(3) . . . . ?
C7 C8 C9 N2 0.6(2) . . . . ?
C7 C8 C9 C10 178.9(2) . . . . ?
C8 C9 C10 C11 -113.9(3) . . . . ?
C8 C9 C10 C22 4.0(3) . . . . ?
C8 C9 C10 C44 123.3(3) . . . . ?
C9 N2 C6 C5 -175.50(19) . . . . ?
C9 N2 C6 C7 1.4(2) . . . . ?
C9 C10 C11 N3 -96.8(2) . . . . ?
C9 C10 C11 C12 79.7(3) . . . . ?
C9 C10 C44 C45 -11.8(3) . . . . ?
C9 C10 C44 C49 171.6(2) . . . . ?
C10 C11 C12 C13 -178.2(2) . . . . ?
C10 C44 C45 C46 -178.5(2) . . . . ?
C10 C44 C49 C48 177.3(2) . . . . ?
C11 N3 C14 C13 -2.3(3) . . . . ?
C11 N3 C14 C15 -179.7(2) . . . . ?
C11 C10 C44 C45 -133.4(2) . . . . ?
C11 C10 C44 C49 50.0(3) . . . . ?
C11 C12 C13 C14 -0.1(3) . . . . ?
C12 C13 C14 N3 1.4(3) . . . . ?
C12 C13 C14 C15 178.6(2) . . . . ?
C13 C14 C15 C16 -90.1(3) . . . . ?
C13 C14 C15 C23 27.8(4) . . . . ?
C13 C14 C15 C61 147.1(3) . . . . ?
C14 N3 C11 C10 179.5(2) . . . . ?
C14 N3 C11 C12 2.2(3) . . . . ?
C14 C15 C16 N4 -51.4(3) . . . . ?
C14 C15 C16 C17 135.2(3) . . . . ?
C14 C15 C61 C60 141.4(2) . . . . ?
C14 C15 C61 C62 -43.6(3) . . . . ?
C15 C16 C17 C18 174.2(2) . . . . ?
C15 C61 C62 C63 -175.5(3) . . . . ?
C16 N4 C66 C18 0.1(3) . . . . ?
C16 N4 C66 C20 -179.6(2) . . . . ?
C16 C15 C61 C60 18.6(3) . . . . ?
C16 C15 C61 C62 -166.4(2) . . . . ?
C16 C17 C18 C66 0.1(3) . . . . ?
C17 C18 C66 N4 -0.1(3) . . . . ?
C17 C18 C66 C20 179.5(2) . . . . ?
C20 C1 C2 C3 176.0(2) . . . . ?
C20 C42 C43 C64 177.4(2) . . . . ?
C21 C5 C6 N2 -179.15(19) . . . . ?
C21 C5 C6 C7 4.7(3) . . . . ?
C21 C5 C25 C26 79.6(3) . . . . ?
C21 C5 C25 C30 -94.3(3) . . . . ?
C22 C10 C11 N3 145.3(2) . . . . ?
C22 C10 C11 C12 -38.2(3) . . . . ?
C22 C10 C44 C45 108.0(2) . . . . ?
C22 C10 C44 C49 -68.6(3) . . . . ?
C23 C15 C16 N4 -169.5(2) . . . . ?
C23 C15 C16 C17 17.1(3) . . . . ?
C23 C15 C61 C60 -99.2(3) . . . . ?
C23 C15 C61 C62 75.8(3) . . . . ?
C24 C20 C42 C41 108.1(3) . . . . ?
C24 C20 C42 C43 -68.8(3) . . . . ?
C24 C20 C66 N4 173.0(2) . . . . ?
C24 C20 C66 C18 -6.6(4) . . . . ?
C25 C5 C6 N2 63.8(3) . . . . ?
C25 C5 C6 C7 -112.4(3) . . . . ?
C25 C26 C27 C28 -0.3(4) . . . . ?
C26 C25 C30 C29 -0.2(4) . . . . ?
C26 C27 C28 O1 179.9(2) . . . . ?
C26 C27 C28 C29 0.3(4) . . . . ?
C27 C28 C29 C30 -0.2(4) . . . . ?
C28 O1 C31 C32 171.4(2) . . . . ?
C28 C29 C30 C25 0.2(4) . . . . ?
C30 C25 C26 C27 0.3(4) . . . . ?
C31 O1 C28 C27 -158.1(2) . . . . ?
C31 O1 C28 C29 21.5(4) . . . . ?
C32 O2 C33 C34 -178.1(2) . . . . ?
C33 O2 C32 C31 169.4(2) . . . . ?
C34 O3 C35 C36 173.6(2) . . . . ?
C35 O3 C34 C33 173.3(2) . . . . ?
C36 O4 C37 C38 176.8(2) . . . . ?
C37 O4 C36 C35 -174.3(2) . . . . ?
C38 O5 C39 C40 -174.4(2) . . . . ?
C38 O5 C39 C64 5.8(3) . . . . ?
C39 O5 C38 C37 -179.4(2) . . . . ?
C39 C40 C41 C42 1.0(4) . . . . ?
C40 C39 C64 C43 -0.7(4) . . . . ?
C40 C41 C42 C20 -178.0(2) . . . . ?
C40 C41 C42 C43 -1.1(3) . . . . ?
C41 C42 C43 C64 0.3(4) . . . . ?
C42 C20 C66 N4 -68.6(3) . . . . ?
C42 C20 C66 C18 111.8(3) . . . . ?
C42 C43 C64 C39 0.6(4) . . . . ?
C44 C10 C11 N3 27.3(3) . . . . ?
C44 C10 C11 C12 -156.2(2) . . . . ?
C44 C45 C46 C47 2.0(4) . . . . ?
C45 C44 C49 C48 0.4(3) . . . . ?
C45 C46 C47 O6 178.3(2) . . . . ?
C45 C46 C47 C48 -0.9(4) . . . . ?
C46 C47 C48 C49 -0.4(4) . . . . ?
C47 O6 C50 C51 179.4(2) . . . . ?
C47 C48 C49 C44 0.6(4) . . . . ?
C49 C44 C45 C46 -1.8(3) . . . . ?
C50 O6 C47 C46 -175.9(2) . . . . ?
C50 O6 C47 C48 3.3(3) . . . . ?
C51 O7 C52 C53 -168.5(3) . . . . ?
C52 O7 C51 C50 -179.7(3) . . . . ?
C53 O8 C54 C55 162.2(3) . . . . ?
C53 O8 C54A C55A 167.9(7) . . . . ?
C54 O8 C53 C52 -178.0(3) . . . . ?
C54A O8 C53 C52 -150.2(6) . . . . ?
C55 O9 C56 C57 167.5(4) . . . . ?
C55A O9A C56A C57A 168.2(11) . . . . ?
C56 O9 C55 C54 -169.5(4) . . . . ?
C56A O9A C55A C54A -165.7(11) . . . . ?
C57 O10 C58 C59 11.8(5) . . . . ?
C57 O10 C58 C63 -169.4(4) . . . . ?
C57A O10 C58 C59 137.8(8) . . . . ?
C57A O10 C58 C63 -43.4(8) . . . . ?
C58 O10 C57 C56 177.6(3) . . . . ?
C58 O10 C57A C56A -166.5(7) . . . . ?
C58 C59 C60 C61 0.2(4) . . . . ?
C59 C58 C63 C62 -0.4(6) . . . . ?
C59 C60 C61 C15 175.1(2) . . . . ?
C59 C60 C61 C62 0.0(4) . . . . ?
C60 C61 C62 C63 -0.4(5) . . . . ?
C61 C15 C16 N4 72.7(3) . . . . ?
C61 C15 C16 C17 -100.7(3) . . . . ?
C61 C62 C63 C58 0.6(6) . . . . ?
C63 C58 C59 C60 0.0(5) . . . . ?
C64 C39 C40 C41 0.0(4) . . . . ?
C66 N4 C16 C15 -174.8(2) . . . . ?
C66 N4 C16 C17 -0.1(3) . . . . ?
C66 C20 C42 C41 -10.8(3) . . . . ?
C66 C20 C42 C43 172.3(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.048
_oxdiff_exptl_absorpt_empirical_full_min 0.474
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4599(7) 29945 17301 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.5401(7) 29840 17301 nmt 0.9995 0.4954 0.1651 0.0013 -0.9992 0.0010 0.0007
-0.0003 -1.0000

_twin_special_details            
;
Component 2 rotated by -179.9782° 
around [1.00 0.00 0.00] (reciprocal) or [0.97 0.24 0.08] (direct)
;
