# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_tx3993a_sq
_audit_block_doi                 10.5517/ccdc.csd.cc278k69
_database_code_depnum_ccdc_archive 'CCDC 2063800'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1007/s11426-021-1030-7 2021
loop_
_audit_author_name
_audit_author_address
'Yingjie Zhao'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2021-02-19 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-12-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H42 N6 O12, C16 H10, C4 H8 O'
_chemical_formula_sum            'C80 H60 N6 O13'
_chemical_formula_weight         1313.34
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNO
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'
N N 0.0311 0.0180 '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      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   20.1153(3)
_cell_length_b                   24.4281(3)
_cell_length_c                   15.72562(18)
_cell_angle_alpha                90
_cell_angle_beta                 89.9918(11)
_cell_angle_gamma                90
_cell_volume                     7727.24(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17227
_cell_measurement_temperature    220.00(15)
_cell_measurement_theta_max      72.1920
_cell_measurement_theta_min      3.6020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.573
_diffrn_reflns_theta_min         2.810
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(15)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  25.00   0.50    0.80    --  -46.70  19.00 -90.00   96
  2  ω    -16.00  25.00   0.50    0.80    --  -46.70  19.00 -30.00   82
  3  ω    -23.00  28.00   0.50    0.80    --  -46.70  19.00-150.00  102
  4  ω    -22.00  12.00   0.50    0.80    --  -46.70  19.00-180.00   68
  5  ω    -59.00 -27.00   0.50    4.00    --  -99.00  61.00-120.00   64
  6  ω    -76.00 -50.00   0.50    4.00    --  -99.00 117.00 -20.73   52
  7  ω    -90.00 -56.00   0.50    0.80    --  -46.70 134.00  -0.00   68
  8  ω    -96.00 -71.00   0.50    4.00    --  -99.00 134.00  -0.00   50
  9  ω   -107.00 -27.00   0.50    4.00    --  -99.00 110.00  44.90  160
 10  ω    -61.00 -34.00   0.50    0.80    --  -46.70 135.00 178.00   54
 11  ω   -112.00 -70.00   0.50    4.00    --  -99.00 125.00  60.00   84
 12  ω   -109.00 -79.00   0.50    4.00    --  -99.00 117.00 -20.73   60
 13  ω   -111.00 -86.00   0.50    4.00    --  -99.00 125.00 -60.00   50
 14  ω   -119.00 -68.00   0.50    4.00    --  -99.00 135.00 178.00  102
 15  ω    -20.00  27.00   0.50    0.80    --   46.70 -19.00 -90.00   94
 16  ω     62.00 108.00   0.50    4.00    --  103.25 -77.00 -60.00   92
 17  ω     77.00 104.00   0.50    4.00    --  103.25 -94.00-120.00   54
 18  ω     48.00 101.00   0.50    4.00    --  103.25 -94.00 -60.00  106
 19  ω     48.00  75.00   0.50    4.00    --  103.25 -61.00 -90.00   54
 20  ω     31.00  75.00   0.50    4.00    --  103.25 -61.00-120.00   88
 21  ω     33.00  74.00   0.50    4.00    --  103.25 -61.00 -60.00   82
 22  ω     37.00  63.00   0.50    0.80    --   46.70-134.00 -67.00   52
 23  ω     32.00 118.00   0.50    4.00    --  103.25-134.00 -67.00  172
 24  ω     36.00  98.00   0.50    0.80    --   46.70-135.00 112.00  124
 25  ω     83.00 119.00   0.50    4.00    --  103.25-135.00 112.00   72
 26  ω     81.00 109.00   0.50    4.00    --  103.25 -77.00 120.00   56
 27  ω     79.00 106.00   0.50    4.00    --  103.25 -94.00 150.00   54
 28  ω     56.00 104.00   0.50    4.00    --  103.25 -94.00 120.00   96
 29  ω     41.00  80.00   0.50    4.00    --  103.25 -77.00 120.00   78
 30  ω     32.00  73.00   0.50    4.00    --  103.25 -61.00  60.00   82
 31  ω     32.00  75.00   0.50    4.00    --  103.25 -61.00 120.00   86
 32  ω     32.00  98.00   0.50    4.00    --  103.25-125.00 150.00  132
 33  ω     91.00 141.00   0.50    4.00    --  103.25  15.00   0.00  100
 34  ω    126.00 152.00   0.50    4.00    --  103.25  61.00 -90.00   52
 35  ω     95.00 169.00   0.50    4.00    --  103.25  61.00-180.00  148
 36  ω     89.00 115.00   0.50    4.00    --  103.25  61.00 -90.00   52
 37  ω     92.00 122.00   0.50    4.00    --  103.25 134.00  -0.00   60
 38  ω     87.00 162.00   0.50    4.00    --  103.25  61.00  90.00  150
 39  ω    104.00 159.00   0.50    4.00    --  103.25  45.00 120.00  110
 40  ω     75.00 145.00   0.50    4.00    --  103.25 135.00 178.00  140
 41  ω     49.00 115.00   0.50    0.80    --   46.70  77.00-180.00  132
 42  ω   -104.00 -68.00   0.50    0.80    --  -46.70-135.00 112.00   72
 43  ω   -123.00 -78.00   0.50    4.00    --  -99.00-135.00 112.00   90
 44  ω   -118.00 -73.00   0.50    0.80    --  -46.70-134.00 -67.00   90
 45  ω   -142.00-117.00   0.50    4.00    --  -99.00-134.00 -67.00   50
 46  ω   -167.00-106.00   0.50    4.00    --  -99.00 -70.00  42.18  122
 47  ω   -167.00 -85.00   0.50    4.00    --  -99.00 -94.00  60.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0331984000
_diffrn_orient_matrix_UB_12      -0.0518765000
_diffrn_orient_matrix_UB_13      -0.0361651000
_diffrn_orient_matrix_UB_21      0.0472480000
_diffrn_orient_matrix_UB_22      0.0359033000
_diffrn_orient_matrix_UB_23      -0.0532019000
_diffrn_orient_matrix_UB_31      0.0502869000
_diffrn_orient_matrix_UB_32      0.0004552000
_diffrn_orient_matrix_UB_33      0.0738559000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                13684
_reflns_number_total             15270
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 5853 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         15270
_refine_ls_number_restraints     192
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0477
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0978P)²+1.6812P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1442
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O13-C80 = O13-C77 = O13A-C80A = O13A-C77A
 1.47 with sigma of 0.01
 C79-C78 = C78-C77 = C80-C79 = C79A-C78A = C78A-C77A = C80A-C79A
 1.54 with sigma of 0.01
 C78A-C80A
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C78 \\sim O13 \\sim C77 \\sim C80 \\sim C79 \\sim C77A \\sim O13A \\sim C80A
\\sim C78A \\sim C79A: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
Uanis(C78) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C77A) \\sim Ueq, Uanis(O13A) \\sim Ueq,
Uanis(C80A) \\sim Ueq, Uanis(C78A) \\sim Ueq, Uanis(C79A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O13A)=Sof(C77A)=Sof(H77C)=Sof(H77D)=Sof(C78A)=Sof(H78C)=Sof(H78D)=
 Sof(C79A)=Sof(H79C)=Sof(H79D)=Sof(C80A)=Sof(H80C)=Sof(H80D)=1-FVAR(1)
 Sof(O13)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=
 Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80A)=Sof(H80B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C20(H20), C35(H35), C40(H40), C55(H55), C60(H60)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C56(H56A,H56B),
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C77(H77A,H77B), C78(H78A,H78B),
  C79(H79A,H79B), C80(H80A,H80B), C77A(H77C,H77D), C78A(H78C,H78D), C79A(H79C,
 H79D), C80A(H80C,H80D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C23(H23), C24(H24), C29(H29), C30(H30),
 C43(H43), C44(H44), C49(H49), C50(H50), C62(H62), C63(H63), C64(H64), C66(H66),
  C67(H67), C69(H69), C70(H70), C71(H71), C73(H73), C74(H74)
;
_atom_sites_solution_hydrogens   geom
_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
O1 O 0.90650(12) 0.57870(11) 0.58229(19) 0.0610(7) Uani 1 1 d . . . . .
O2 O 0.76060(12) 0.56039(10) 0.36370(14) 0.0495(5) Uani 1 1 d . . . . .
O3 O 0.66106(12) 0.71505(12) 0.82148(15) 0.0588(7) Uani 1 1 d . . . . .
O4 O 0.51215(11) 0.68315(12) 0.61053(16) 0.0569(6) Uani 1 1 d . . . . .
O5 O 0.58387(15) 0.63913(10) 0.95862(18) 0.0635(7) Uani 1 1 d . . . . .
O6 O 0.41402(12) 0.65192(10) 0.76883(17) 0.0538(6) Uani 1 1 d . . . . .
O7 O 0.39494(13) 0.36549(10) 0.75104(17) 0.0564(6) Uani 1 1 d . . . . .
O8 O 0.56624(14) 0.35230(10) 0.93684(17) 0.0556(6) Uani 1 1 d . . . . .
O9 O 0.51890(12) 0.30323(11) 0.63912(15) 0.0520(6) Uani 1 1 d . . . . .
O10 O 0.68557(14) 0.29325(15) 0.83454(18) 0.0711(8) Uani 1 1 d . . . . .
O11 O 0.73448(11) 0.43499(11) 0.35476(15) 0.0519(6) Uani 1 1 d . . . . .
O12 O 0.89549(11) 0.44068(11) 0.55789(17) 0.0568(6) Uani 1 1 d . . . . .
N1 N 0.83081(12) 0.56109(10) 0.47775(17) 0.0387(5) Uani 1 1 d . . . . .
N2 N 0.58495(12) 0.69795(10) 0.71873(15) 0.0361(5) Uani 1 1 d . . . . .
N3 N 0.50433(13) 0.64676(10) 0.85545(16) 0.0388(5) Uani 1 1 d . . . . .
N4 N 0.48782(13) 0.35852(10) 0.83281(16) 0.0387(5) Uani 1 1 d . . . . .
N5 N 0.59917(13) 0.30291(11) 0.74125(16) 0.0401(5) Uani 1 1 d . . . . .
N6 N 0.81353(12) 0.44299(10) 0.45775(17) 0.0373(5) Uani 1 1 d . . . . .
C1 C 0.84977(15) 0.58317(12) 0.5558(2) 0.0425(7) Uani 1 1 d . . . . .
C2 C 0.79774(15) 0.61121(12) 0.6071(2) 0.0384(6) Uani 1 1 d . . . . .
C3 C 0.81199(16) 0.63006(13) 0.6878(2) 0.0453(7) Uani 1 1 d . . . . .
H3 H 0.854213 0.625092 0.710610 0.054 Uiso 1 1 calc R U . . .
C4 C 0.76228(17) 0.65694(15) 0.7357(2) 0.0490(8) Uani 1 1 d . . . . .
H4 H 0.772052 0.669404 0.790186 0.059 Uiso 1 1 calc R U . . .
C5 C 0.69995(15) 0.66487(12) 0.70303(19) 0.0385(6) Uani 1 1 d . . . . .
C6 C 0.64860(15) 0.69462(14) 0.7531(2) 0.0426(7) Uani 1 1 d . . . . .
C7 C 0.56819(14) 0.67871(13) 0.63763(19) 0.0374(6) Uani 1 1 d . . . . .
C8 C 0.62149(14) 0.65352(12) 0.58590(18) 0.0357(6) Uani 1 1 d . . . . .
C9 C 0.60803(15) 0.63752(13) 0.50343(19) 0.0399(6) Uani 1 1 d . . . . .
H9 H 0.566273 0.643915 0.480088 0.048 Uiso 1 1 calc R U . . .
C10 C 0.65738(15) 0.61161(13) 0.45490(19) 0.0398(6) Uani 1 1 d . . . . .
H10 H 0.648181 0.601091 0.399290 0.048 Uiso 1 1 calc R U . . .
C11 C 0.71932(15) 0.60160(12) 0.48884(18) 0.0358(6) Uani 1 1 d . . . . .
C12 C 0.77057(15) 0.57309(11) 0.4373(2) 0.0388(6) Uani 1 1 d . . . . .
C13 C 0.73414(14) 0.61915(11) 0.57232(18) 0.0336(6) Uani 1 1 d . . . . .
C14 C 0.68468(14) 0.64572(11) 0.62099(18) 0.0342(6) Uani 1 1 d . . . . .
C15 C 0.53100(15) 0.72815(12) 0.76398(18) 0.0382(6) Uani 1 1 d . . . . .
H15 H 0.490525 0.723203 0.730158 0.046 Uiso 1 1 calc R U . . .
C16 C 0.54524(18) 0.78969(13) 0.7654(2) 0.0478(7) Uani 1 1 d . . . . .
H16A H 0.584887 0.796591 0.798837 0.057 Uiso 1 1 calc R U . . .
H16B H 0.553455 0.802400 0.707921 0.057 Uiso 1 1 calc R U . . .
C17 C 0.4874(2) 0.82103(14) 0.8029(2) 0.0543(8) Uani 1 1 d . . . . .
H17A H 0.498153 0.859730 0.804923 0.065 Uiso 1 1 calc R U . . .
H17B H 0.448544 0.816420 0.767206 0.065 Uiso 1 1 calc R U . . .
C18 C 0.4724(2) 0.80071(15) 0.8916(2) 0.0563(9) Uani 1 1 d . . . . .
H18A H 0.434718 0.820612 0.914498 0.068 Uiso 1 1 calc R U . . .
H18B H 0.510371 0.807424 0.928174 0.068 Uiso 1 1 calc R U . . .
C19 C 0.45678(19) 0.73941(14) 0.8905(2) 0.0492(8) Uani 1 1 d . . . . .
H19A H 0.417287 0.732946 0.856551 0.059 Uiso 1 1 calc R U . . .
H19B H 0.447872 0.726967 0.947946 0.059 Uiso 1 1 calc R U . . .
C20 C 0.51524(16) 0.70694(13) 0.85334(19) 0.0407(6) Uani 1 1 d . . . . .
H20 H 0.554101 0.714631 0.888965 0.049 Uiso 1 1 calc R U . . .
C21 C 0.45145(15) 0.62357(14) 0.80999(19) 0.0414(6) Uani 1 1 d . . . . .
C22 C 0.44381(15) 0.56299(13) 0.81296(19) 0.0401(6) Uani 1 1 d . . . . .
C23 C 0.39306(16) 0.53776(14) 0.7699(2) 0.0448(7) Uani 1 1 d . . . . .
H23 H 0.360612 0.558894 0.743525 0.054 Uiso 1 1 calc R U . . .
C24 C 0.38942(17) 0.48076(14) 0.7652(2) 0.0460(7) Uani 1 1 d . . . . .
H24 H 0.354823 0.464280 0.735478 0.055 Uiso 1 1 calc R U . . .
C25 C 0.43713(15) 0.44862(13) 0.80456(19) 0.0400(6) Uani 1 1 d . . . . .
C26 C 0.43652(16) 0.38831(14) 0.7933(2) 0.0426(7) Uani 1 1 d . . . . .
C27 C 0.53152(15) 0.38102(13) 0.89191(19) 0.0406(6) Uani 1 1 d . . . . .
C28 C 0.53455(15) 0.44182(13) 0.89709(18) 0.0399(6) Uani 1 1 d . . . . .
C29 C 0.58323(17) 0.46684(14) 0.9448(2) 0.0442(7) Uani 1 1 d . . . . .
H29 H 0.613885 0.445714 0.974468 0.053 Uiso 1 1 calc R U . . .
C30 C 0.58669(17) 0.52422(14) 0.9486(2) 0.0452(7) Uani 1 1 d . . . . .
H30 H 0.619828 0.540864 0.980773 0.054 Uiso 1 1 calc R U . . .
C31 C 0.54147(15) 0.55607(13) 0.90532(18) 0.0390(6) Uani 1 1 d . . . . .
C32 C 0.54550(17) 0.61665(14) 0.9103(2) 0.0435(7) Uani 1 1 d . . . . .
C33 C 0.49100(15) 0.53081(13) 0.85745(19) 0.0387(6) Uani 1 1 d . . . . .
C34 C 0.48755(15) 0.47351(13) 0.85295(18) 0.0381(6) Uani 1 1 d . . . . .
C35 C 0.48711(15) 0.29857(13) 0.8170(2) 0.0413(6) Uani 1 1 d . . . . .
H35 H 0.462045 0.292840 0.764335 0.050 Uiso 1 1 calc R U . . .
C36 C 0.4499(2) 0.26776(15) 0.8871(2) 0.0523(8) Uani 1 1 d . . . . .
H36A H 0.474437 0.270639 0.940015 0.063 Uiso 1 1 calc R U . . .
H36B H 0.406554 0.284273 0.895523 0.063 Uiso 1 1 calc R U . . .
C37 C 0.4415(2) 0.20755(16) 0.8637(3) 0.0620(9) Uani 1 1 d . . . . .
H37A H 0.419466 0.188402 0.909829 0.074 Uiso 1 1 calc R U . . .
H37B H 0.413794 0.204480 0.813395 0.074 Uiso 1 1 calc R U . . .
C38 C 0.5090(2) 0.18134(16) 0.8466(3) 0.0662(10) Uani 1 1 d . . . . .
H38A H 0.502773 0.143630 0.829020 0.079 Uiso 1 1 calc R U . . .
H38B H 0.535080 0.181350 0.898505 0.079 Uiso 1 1 calc R U . . .
C39 C 0.5465(2) 0.21272(14) 0.7770(3) 0.0607(9) Uani 1 1 d . . . . .
H39A H 0.589605 0.195904 0.767603 0.073 Uiso 1 1 calc R U . . .
H39B H 0.521712 0.211007 0.724160 0.073 Uiso 1 1 calc R U . . .
C40 C 0.55586(17) 0.27268(13) 0.8034(2) 0.0450(7) Uani 1 1 d . . . . .
H40 H 0.578778 0.272805 0.858415 0.054 Uiso 1 1 calc R U . . .
C41 C 0.57554(15) 0.31474(12) 0.66010(19) 0.0389(6) Uani 1 1 d . . . . .
C42 C 0.62126(15) 0.34249(11) 0.59966(19) 0.0354(6) Uani 1 1 d . . . . .
C43 C 0.60046(15) 0.35455(13) 0.5188(2) 0.0407(6) Uani 1 1 d . . . . .
H43 H 0.558004 0.344507 0.501329 0.049 Uiso 1 1 calc R U . . .
C44 C 0.64327(15) 0.38221(13) 0.4616(2) 0.0411(6) Uani 1 1 d . . . . .
H44 H 0.629101 0.390134 0.406700 0.049 Uiso 1 1 calc R U . . .
C45 C 0.70607(14) 0.39735(11) 0.48781(19) 0.0348(6) Uani 1 1 d . . . . .
C46 C 0.75059(14) 0.42633(12) 0.4268(2) 0.0377(6) Uani 1 1 d . . . . .
C47 C 0.83863(14) 0.42823(12) 0.5371(2) 0.0406(6) Uani 1 1 d . . . . .
C48 C 0.79443(15) 0.39761(12) 0.5965(2) 0.0398(6) Uani 1 1 d . . . . .
C49 C 0.81573(16) 0.38324(16) 0.6749(2) 0.0509(8) Uani 1 1 d . . . . .
H49 H 0.858442 0.392627 0.692149 0.061 Uiso 1 1 calc R U . . .
C50 C 0.77347(17) 0.35397(16) 0.7310(2) 0.0502(8) Uani 1 1 d . . . . .
H50 H 0.789211 0.343169 0.783988 0.060 Uiso 1 1 calc R U . . .
C51 C 0.70943(16) 0.34145(13) 0.7075(2) 0.0428(7) Uani 1 1 d . . . . .
C52 C 0.66518(17) 0.31065(14) 0.7674(2) 0.0459(7) Uani 1 1 d . . . . .
C53 C 0.68642(14) 0.35604(12) 0.62636(19) 0.0351(6) Uani 1 1 d . . . . .
C54 C 0.72895(14) 0.38439(11) 0.5695(2) 0.0347(6) Uani 1 1 d . . . . .
C55 C 0.85552(15) 0.47381(12) 0.3969(2) 0.0411(6) Uani 1 1 d . . . . .
H55 H 0.827292 0.482988 0.348166 0.049 Uiso 1 1 calc R U . . .
C56 C 0.91343(17) 0.44008(14) 0.3628(3) 0.0516(8) Uani 1 1 d . . . . .
H56A H 0.945336 0.433418 0.407868 0.062 Uiso 1 1 calc R U . . .
H56B H 0.897373 0.405008 0.342434 0.062 Uiso 1 1 calc R U . . .
C57 C 0.94672(19) 0.47113(15) 0.2903(3) 0.0588(9) Uani 1 1 d . . . . .
H57A H 0.983740 0.449844 0.268702 0.071 Uiso 1 1 calc R U . . .
H57B H 0.915144 0.476188 0.244393 0.071 Uiso 1 1 calc R U . . .
C58 C 0.97148(19) 0.52617(15) 0.3199(3) 0.0601(10) Uani 1 1 d . . . . .
H58A H 0.990283 0.545790 0.271981 0.072 Uiso 1 1 calc R U . . .
H58B H 1.006454 0.520901 0.361583 0.072 Uiso 1 1 calc R U . . .
C59 C 0.91573(19) 0.56054(14) 0.3594(3) 0.0561(9) Uani 1 1 d . . . . .
H59A H 0.882862 0.569358 0.316430 0.067 Uiso 1 1 calc R U . . .
H59B H 0.933846 0.594556 0.381251 0.067 Uiso 1 1 calc R U . . .
C60 C 0.88268(15) 0.52819(12) 0.4323(2) 0.0439(7) Uani 1 1 d . . . . .
H60 H 0.917446 0.519220 0.473676 0.053 Uiso 1 1 calc R U . . .
C61 C 0.32515(17) 0.21572(12) 0.4508(2) 0.0456(7) Uani 1 1 d . . . . .
C62 C 0.39011(17) 0.20485(14) 0.4763(3) 0.0528(8) Uani 1 1 d . . . . .
H62 H 0.417987 0.185416 0.439983 0.063 Uiso 1 1 calc R U . . .
C63 C 0.41409(18) 0.22202(16) 0.5534(3) 0.0590(9) Uani 1 1 d . . . . .
H63 H 0.458076 0.215042 0.567975 0.071 Uiso 1 1 calc R U . . .
C64 C 0.37300(18) 0.24978(16) 0.6098(3) 0.0549(8) Uani 1 1 d . . . . .
H64 H 0.389680 0.261052 0.662108 0.066 Uiso 1 1 calc R U . . .
C65 C 0.30708(17) 0.26092(13) 0.5889(2) 0.0445(7) Uani 1 1 d . . . . .
C66 C 0.26328(18) 0.28995(14) 0.6452(2) 0.0500(8) Uani 1 1 d . . . . .
H66 H 0.278728 0.300867 0.698324 0.060 Uiso 1 1 calc R U . . .
C67 C 0.20025(17) 0.30166(13) 0.6226(2) 0.0465(7) Uani 1 1 d . . . . .
H67 H 0.173108 0.320457 0.660590 0.056 Uiso 1 1 calc R U . . .
C68 C 0.17404(15) 0.28585(11) 0.5415(2) 0.0402(6) Uani 1 1 d . . . . .
C69 C 0.10940(17) 0.29782(14) 0.5159(2) 0.0503(8) Uani 1 1 d . . . . .
H69 H 0.081283 0.316824 0.552400 0.060 Uiso 1 1 calc R U . . .
C70 C 0.08654(18) 0.28181(16) 0.4370(3) 0.0582(9) Uani 1 1 d . . . . .
H70 H 0.043316 0.290517 0.420915 0.070 Uiso 1 1 calc R U . . .
C71 C 0.12676(19) 0.25306(17) 0.3813(2) 0.0564(9) Uani 1 1 d . . . . .
H71 H 0.110197 0.241760 0.328970 0.068 Uiso 1 1 calc R U . . .
C72 C 0.19216(16) 0.24107(13) 0.4039(2) 0.0449(7) Uani 1 1 d . . . . .
C73 C 0.2367(2) 0.21140(15) 0.3481(2) 0.0534(8) Uani 1 1 d . . . . .
H73 H 0.221665 0.200115 0.294948 0.064 Uiso 1 1 calc R U . . .
C74 C 0.29857(19) 0.20005(13) 0.3714(2) 0.0518(8) Uani 1 1 d . . . . .
H74 H 0.325622 0.180917 0.333743 0.062 Uiso 1 1 calc R U . . .
C75 C 0.21680(15) 0.25712(12) 0.4842(2) 0.0388(6) Uani 1 1 d . . . . .
C76 C 0.28269(16) 0.24470(12) 0.5086(2) 0.0411(7) Uani 1 1 d . . . . .
O13 O 0.5642(4) 0.5646(2) 0.6928(4) 0.105(2) Uani 0.599(7) 1 d D U P A 1
C77 C 0.5255(6) 0.5403(5) 0.6227(8) 0.115(4) Uani 0.599(7) 1 d D U P A 1
H77A H 0.515782 0.568570 0.581204 0.138 Uiso 0.599(7) 1 calc R U P A 1
H77B H 0.483556 0.527022 0.644964 0.138 Uiso 0.599(7) 1 calc R U P A 1
C78 C 0.5615(7) 0.4932(7) 0.5784(10) 0.144(4) Uani 0.599(7) 1 d D U P A 1
H78A H 0.539894 0.458193 0.587482 0.173 Uiso 0.599(7) 1 calc R U P A 1
H78B H 0.567569 0.499620 0.517989 0.173 Uiso 0.599(7) 1 calc R U P A 1
C79 C 0.6242(5) 0.4985(4) 0.6269(6) 0.098(3) Uani 0.599(7) 1 d D U P A 1
H79A H 0.656058 0.517632 0.591328 0.118 Uiso 0.599(7) 1 calc R U P A 1
H79B H 0.641563 0.462039 0.636731 0.118 Uiso 0.599(7) 1 calc R U P A 1
C80 C 0.6209(6) 0.5286(4) 0.7140(7) 0.111(3) Uani 0.599(7) 1 d D U P A 1
H80A H 0.611039 0.503934 0.760657 0.133 Uiso 0.599(7) 1 calc R U P A 1
H80B H 0.661126 0.549066 0.726150 0.133 Uiso 0.599(7) 1 calc R U P A 1
O13A O 0.5549(6) 0.4380(4) 0.6876(7) 0.109(4) Uani 0.401(7) 1 d D U P A 2
C77A C 0.5173(11) 0.4602(7) 0.6172(12) 0.129(5) Uani 0.401(7) 1 d D U P A 2
H77C H 0.470459 0.459727 0.631804 0.155 Uiso 0.401(7) 1 calc R U P A 2
H77D H 0.523379 0.436700 0.568076 0.155 Uiso 0.401(7) 1 calc R U P A 2
C78A C 0.5372(14) 0.5189(10) 0.5931(18) 0.156(7) Uani 0.401(7) 1 d D U P A 2
H78C H 0.555811 0.521130 0.536300 0.187 Uiso 0.401(7) 1 calc R U P A 2
H78D H 0.500671 0.544475 0.598890 0.187 Uiso 0.401(7) 1 calc R U P A 2
C79A C 0.5899(12) 0.5264(7) 0.6622(14) 0.130(5) Uani 0.401(7) 1 d D U P A 2
H79C H 0.627725 0.545662 0.638295 0.156 Uiso 0.401(7) 1 calc R U P A 2
H79D H 0.571649 0.548920 0.707368 0.156 Uiso 0.401(7) 1 calc R U P A 2
C80A C 0.6130(7) 0.4731(5) 0.6989(10) 0.106(4) Uani 0.401(7) 1 d D U P A 2
H80C H 0.651111 0.458932 0.668235 0.127 Uiso 0.401(7) 1 calc R U P A 2
H80D H 0.624350 0.476868 0.758585 0.127 Uiso 0.401(7) 1 calc R U P A 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
O1 C1 1.220(4) . ?
O2 C12 1.215(4) . ?
O3 C6 1.211(4) . ?
O4 C7 1.210(4) . ?
O5 C32 1.214(4) . ?
O6 C21 1.211(4) . ?
O7 C26 1.205(4) . ?
O8 C27 1.216(4) . ?
O9 C41 1.219(4) . ?
O10 C52 1.210(4) . ?
O11 C46 1.198(4) . ?
O12 C47 1.228(4) . ?
N1 C1 1.394(4) . ?
N1 C12 1.399(4) . ?
N1 C60 1.498(4) . ?
N2 C6 1.392(4) . ?
N2 C7 1.401(4) . ?
N2 C15 1.493(4) . ?
N3 C20 1.487(4) . ?
N3 C21 1.401(4) . ?
N3 C32 1.404(4) . ?
N4 C26 1.407(4) . ?
N4 C27 1.392(4) . ?
N4 C35 1.486(4) . ?
N5 C40 1.503(4) . ?
N5 C41 1.392(4) . ?
N5 C52 1.403(4) . ?
N6 C46 1.416(4) . ?
N6 C47 1.394(4) . ?
N6 C55 1.482(4) . ?
C1 C2 1.488(4) . ?
C2 C3 1.380(4) . ?
C2 C13 1.405(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.414(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.369(4) . ?
C5 C6 1.488(4) . ?
C5 C14 1.406(4) . ?
C7 C8 1.480(4) . ?
C8 C9 1.381(4) . ?
C8 C14 1.399(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.403(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.377(4) . ?
C11 C12 1.484(4) . ?
C11 C13 1.413(4) . ?
C13 C14 1.413(4) . ?
C15 H15 0.9800 . ?
C15 C16 1.531(4) . ?
C15 C20 1.531(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.512(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.510(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.530(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.534(4) . ?
C20 H20 0.9800 . ?
C21 C22 1.488(5) . ?
C22 C23 1.371(4) . ?
C22 C33 1.417(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.396(5) . ?
C24 H24 0.9300 . ?
C24 C25 1.386(4) . ?
C25 C26 1.484(4) . ?
C25 C34 1.406(4) . ?
C27 C28 1.489(4) . ?
C28 C29 1.376(4) . ?
C28 C34 1.405(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.405(5) . ?
C30 H30 0.9300 . ?
C30 C31 1.377(4) . ?
C31 C32 1.484(5) . ?
C31 C33 1.407(4) . ?
C33 C34 1.403(4) . ?
C35 H35 0.9800 . ?
C35 C36 1.530(4) . ?
C35 C40 1.535(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.526(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.526(6) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.535(5) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.534(5) . ?
C40 H40 0.9800 . ?
C41 C42 1.486(4) . ?
C42 C43 1.371(4) . ?
C42 C53 1.416(4) . ?
C43 H43 0.9300 . ?
C43 C44 1.416(4) . ?
C44 H44 0.9300 . ?
C44 C45 1.379(4) . ?
C45 C46 1.491(4) . ?
C45 C54 1.401(4) . ?
C47 C48 1.491(5) . ?
C48 C49 1.351(5) . ?
C48 C54 1.421(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.419(5) . ?
C50 H50 0.9300 . ?
C50 C51 1.374(5) . ?
C51 C52 1.498(5) . ?
C51 C53 1.404(4) . ?
C53 C54 1.418(4) . ?
C55 H55 0.9800 . ?
C55 C56 1.524(4) . ?
C55 C60 1.540(4) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 C57 1.524(5) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C57 C58 1.507(5) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58 C59 1.532(5) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 C60 1.543(5) . ?
C60 H60 0.9800 . ?
C61 C62 1.393(5) . ?
C61 C74 1.411(5) . ?
C61 C76 1.434(5) . ?
C62 H62 0.9300 . ?
C62 C63 1.371(6) . ?
C63 H63 0.9300 . ?
C63 C64 1.390(6) . ?
C64 H64 0.9300 . ?
C64 C65 1.393(5) . ?
C65 C66 1.437(5) . ?
C65 C76 1.411(5) . ?
C66 H66 0.9300 . ?
C66 C67 1.347(5) . ?
C67 H67 0.9300 . ?
C67 C68 1.433(5) . ?
C68 C69 1.393(5) . ?
C68 C75 1.430(4) . ?
C69 H69 0.9300 . ?
C69 C70 1.380(6) . ?
C70 H70 0.9300 . ?
C70 C71 1.383(6) . ?
C71 H71 0.9300 . ?
C71 C72 1.394(5) . ?
C72 C73 1.448(5) . ?
C72 C75 1.412(5) . ?
C73 H73 0.9300 . ?
C73 C74 1.327(6) . ?
C74 H74 0.9300 . ?
C75 C76 1.413(4) . ?
O13 C77 1.473(11) . ?
O13 C80 1.478(11) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C77 C78 1.529(11) . ?
C78 H78A 0.9700 . ?
C78 H78B 0.9700 . ?
C78 C79 1.479(12) . ?
C79 H79A 0.9700 . ?
C79 H79B 0.9700 . ?
C79 C80 1.556(11) . ?
C80 H80A 0.9700 . ?
C80 H80B 0.9700 . ?
O13A C77A 1.445(13) . ?
O13A C80A 1.459(12) . ?
C77A H77C 0.9700 . ?
C77A H77D 0.9700 . ?
C77A C78A 1.536(14) . ?
C78A H78C 0.9700 . ?
C78A H78D 0.9700 . ?
C78A C79A 1.528(14) . ?
C79A H79C 0.9700 . ?
C79A H79D 0.9700 . ?
C79A C80A 1.499(13) . ?
C80A H80C 0.9700 . ?
C80A H80D 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
C1 N1 C12 123.8(2) . . ?
C1 N1 C60 115.9(2) . . ?
C12 N1 C60 119.9(3) . . ?
C6 N2 C7 123.7(2) . . ?
C6 N2 C15 120.8(2) . . ?
C7 N2 C15 115.1(2) . . ?
C21 N3 C20 120.0(2) . . ?
C21 N3 C32 123.3(3) . . ?
C32 N3 C20 116.4(3) . . ?
C26 N4 C35 115.4(3) . . ?
C27 N4 C26 123.6(3) . . ?
C27 N4 C35 120.5(3) . . ?
C41 N5 C40 120.0(3) . . ?
C41 N5 C52 124.3(3) . . ?
C52 N5 C40 115.1(2) . . ?
C46 N6 C55 115.7(2) . . ?
C47 N6 C46 123.9(3) . . ?
C47 N6 C55 120.2(2) . . ?
O1 C1 N1 121.5(3) . . ?
O1 C1 C2 121.0(3) . . ?
N1 C1 C2 117.6(3) . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 C13 120.1(3) . . ?
C13 C2 C1 119.6(3) . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.9(3) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.9(3) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 C14 119.8(3) . . ?
C14 C5 C6 119.7(3) . . ?
O3 C6 N2 120.7(3) . . ?
O3 C6 C5 121.8(3) . . ?
N2 C6 C5 117.5(3) . . ?
O4 C7 N2 121.0(3) . . ?
O4 C7 C8 121.2(3) . . ?
N2 C7 C8 117.8(2) . . ?
C9 C8 C7 119.5(3) . . ?
C9 C8 C14 120.7(3) . . ?
C14 C8 C7 119.9(2) . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0(3) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.6(3) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 C12 120.0(3) . . ?
C10 C11 C13 119.8(3) . . ?
C13 C11 C12 120.2(3) . . ?
O2 C12 N1 121.5(3) . . ?
O2 C12 C11 121.7(3) . . ?
N1 C12 C11 116.8(3) . . ?
C2 C13 C11 120.8(3) . . ?
C2 C13 C14 119.6(3) . . ?
C14 C13 C11 119.6(2) . . ?
C5 C14 C13 119.7(3) . . ?
C8 C14 C5 121.0(3) . . ?
C8 C14 C13 119.3(3) . . ?
N2 C15 H15 106.5 . . ?
N2 C15 C16 110.9(2) . . ?
N2 C15 C20 114.9(2) . . ?
C16 C15 H15 106.5 . . ?
C16 C15 C20 111.0(2) . . ?
C20 C15 H15 106.5 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 C15 111.1(3) . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C16 C17 H17A 109.6 . . ?
C16 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
C18 C17 C16 110.3(3) . . ?
C18 C17 H17A 109.6 . . ?
C18 C17 H17B 109.6 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 C19 110.6(3) . . ?
H18A C18 H18B 108.1 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 C20 110.7(3) . . ?
H19A C19 H19B 108.1 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
N3 C20 C15 112.7(2) . . ?
N3 C20 C19 112.9(3) . . ?
N3 C20 H20 107.1 . . ?
C15 C20 C19 109.5(3) . . ?
C15 C20 H20 107.1 . . ?
C19 C20 H20 107.1 . . ?
O6 C21 N3 120.9(3) . . ?
O6 C21 C22 121.4(3) . . ?
N3 C21 C22 117.7(3) . . ?
C23 C22 C21 120.6(3) . . ?
C23 C22 C33 119.5(3) . . ?
C33 C22 C21 119.8(3) . . ?
C22 C23 H23 119.5 . . ?
C22 C23 C24 120.9(3) . . ?
C24 C23 H23 119.5 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.3(3) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C26 120.2(3) . . ?
C24 C25 C34 119.8(3) . . ?
C34 C25 C26 120.0(3) . . ?
O7 C26 N4 120.9(3) . . ?
O7 C26 C25 122.0(3) . . ?
N4 C26 C25 117.1(3) . . ?
O8 C27 N4 121.5(3) . . ?
O8 C27 C28 121.4(3) . . ?
N4 C27 C28 117.1(3) . . ?
C29 C28 C27 120.1(3) . . ?
C29 C28 C34 120.2(3) . . ?
C34 C28 C27 119.7(3) . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.1(3) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 119.7 . . ?
C31 C30 C29 120.6(3) . . ?
C31 C30 H30 119.7 . . ?
C30 C31 C32 120.1(3) . . ?
C30 C31 C33 119.6(3) . . ?
C33 C31 C32 120.4(3) . . ?
O5 C32 N3 121.5(3) . . ?
O5 C32 C31 121.2(3) . . ?
N3 C32 C31 117.2(3) . . ?
C31 C33 C22 120.3(3) . . ?
C34 C33 C22 119.7(3) . . ?
C34 C33 C31 120.0(3) . . ?
C28 C34 C25 121.0(3) . . ?
C33 C34 C25 119.6(3) . . ?
C33 C34 C28 119.4(3) . . ?
N4 C35 H35 106.7 . . ?
N4 C35 C36 111.7(3) . . ?
N4 C35 C40 114.9(2) . . ?
C36 C35 H35 106.7 . . ?
C36 C35 C40 109.8(3) . . ?
C40 C35 H35 106.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C37 C36 C35 110.8(3) . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
C36 C37 H37A 109.6 . . ?
C36 C37 H37B 109.6 . . ?
H37A C37 H37B 108.1 . . ?
C38 C37 C36 110.3(3) . . ?
C38 C37 H37A 109.6 . . ?
C38 C37 H37B 109.6 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 C39 110.7(3) . . ?
H38A C38 H38B 108.1 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
H39A C39 H39B 108.2 . . ?
C40 C39 C38 110.1(3) . . ?
C40 C39 H39A 109.6 . . ?
C40 C39 H39B 109.6 . . ?
N5 C40 C35 114.2(2) . . ?
N5 C40 C39 111.3(3) . . ?
N5 C40 H40 107.4 . . ?
C35 C40 H40 107.4 . . ?
C39 C40 C35 108.7(3) . . ?
C39 C40 H40 107.4 . . ?
O9 C41 N5 121.3(3) . . ?
O9 C41 C42 120.7(3) . . ?
N5 C41 C42 118.0(3) . . ?
C43 C42 C41 120.2(3) . . ?
C43 C42 C53 120.5(3) . . ?
C53 C42 C41 119.3(3) . . ?
C42 C43 H43 119.8 . . ?
C42 C43 C44 120.4(3) . . ?
C44 C43 H43 119.8 . . ?
C43 C44 H44 120.2 . . ?
C45 C44 C43 119.7(3) . . ?
C45 C44 H44 120.2 . . ?
C44 C45 C46 119.0(3) . . ?
C44 C45 C54 120.9(3) . . ?
C54 C45 C46 120.0(2) . . ?
O11 C46 N6 121.1(3) . . ?
O11 C46 C45 122.0(3) . . ?
N6 C46 C45 116.9(3) . . ?
O12 C47 N6 120.8(3) . . ?
O12 C47 C48 120.9(3) . . ?
N6 C47 C48 118.3(2) . . ?
C49 C48 C47 120.8(3) . . ?
C49 C48 C54 120.5(3) . . ?
C54 C48 C47 118.7(3) . . ?
C48 C49 H49 119.7 . . ?
C48 C49 C50 120.6(3) . . ?
C50 C49 H49 119.7 . . ?
C49 C50 H50 119.8 . . ?
C51 C50 C49 120.5(3) . . ?
C51 C50 H50 119.8 . . ?
C50 C51 C52 120.0(3) . . ?
C50 C51 C53 119.8(3) . . ?
C53 C51 C52 120.2(3) . . ?
O10 C52 N5 121.9(3) . . ?
O10 C52 C51 121.6(3) . . ?
N5 C52 C51 116.5(3) . . ?
C42 C53 C54 119.1(3) . . ?
C51 C53 C42 121.0(3) . . ?
C51 C53 C54 119.9(3) . . ?
C45 C54 C48 121.8(3) . . ?
C45 C54 C53 119.4(2) . . ?
C53 C54 C48 118.8(3) . . ?
N6 C55 H55 106.9 . . ?
N6 C55 C56 112.8(3) . . ?
N6 C55 C60 114.0(3) . . ?
C56 C55 H55 106.9 . . ?
C56 C55 C60 108.8(2) . . ?
C60 C55 H55 106.9 . . ?
C55 C56 H56A 109.8 . . ?
C55 C56 H56B 109.8 . . ?
H56A C56 H56B 108.3 . . ?
C57 C56 C55 109.3(3) . . ?
C57 C56 H56A 109.8 . . ?
C57 C56 H56B 109.8 . . ?
C56 C57 H57A 109.4 . . ?
C56 C57 H57B 109.4 . . ?
H57A C57 H57B 108.0 . . ?
C58 C57 C56 111.0(3) . . ?
C58 C57 H57A 109.4 . . ?
C58 C57 H57B 109.4 . . ?
C57 C58 H58A 109.2 . . ?
C57 C58 H58B 109.2 . . ?
C57 C58 C59 111.8(3) . . ?
H58A C58 H58B 107.9 . . ?
C59 C58 H58A 109.2 . . ?
C59 C58 H58B 109.2 . . ?
C58 C59 H59A 109.7 . . ?
C58 C59 H59B 109.7 . . ?
C58 C59 C60 109.6(3) . . ?
H59A C59 H59B 108.2 . . ?
C60 C59 H59A 109.7 . . ?
C60 C59 H59B 109.7 . . ?
N1 C60 C55 112.8(2) . . ?
N1 C60 C59 112.3(2) . . ?
N1 C60 H60 107.5 . . ?
C55 C60 C59 109.0(3) . . ?
C55 C60 H60 107.5 . . ?
C59 C60 H60 107.5 . . ?
C62 C61 C74 124.0(3) . . ?
C62 C61 C76 118.1(3) . . ?
C74 C61 C76 118.0(3) . . ?
C61 C62 H62 119.1 . . ?
C63 C62 C61 121.8(3) . . ?
C63 C62 H62 119.1 . . ?
C62 C63 H63 119.8 . . ?
C62 C63 C64 120.3(3) . . ?
C64 C63 H63 119.8 . . ?
C63 C64 H64 119.7 . . ?
C63 C64 C65 120.7(4) . . ?
C65 C64 H64 119.7 . . ?
C64 C65 C66 122.3(3) . . ?
C64 C65 C76 119.2(3) . . ?
C76 C65 C66 118.5(3) . . ?
C65 C66 H66 119.4 . . ?
C67 C66 C65 121.3(3) . . ?
C67 C66 H66 119.4 . . ?
C66 C67 H67 119.2 . . ?
C66 C67 C68 121.6(3) . . ?
C68 C67 H67 119.2 . . ?
C69 C68 C67 123.0(3) . . ?
C69 C68 C75 118.8(3) . . ?
C75 C68 C67 118.2(3) . . ?
C68 C69 H69 119.6 . . ?
C70 C69 C68 120.8(3) . . ?
C70 C69 H69 119.6 . . ?
C69 C70 H70 119.4 . . ?
C69 C70 C71 121.2(3) . . ?
C71 C70 H70 119.4 . . ?
C70 C71 H71 120.1 . . ?
C70 C71 C72 119.9(3) . . ?
C72 C71 H71 120.1 . . ?
C71 C72 C73 122.3(3) . . ?
C71 C72 C75 120.0(3) . . ?
C75 C72 C73 117.6(3) . . ?
C72 C73 H73 119.4 . . ?
C74 C73 C72 121.1(3) . . ?
C74 C73 H73 119.4 . . ?
C61 C74 H74 118.5 . . ?
C73 C74 C61 122.9(3) . . ?
C73 C74 H74 118.5 . . ?
C72 C75 C68 119.3(3) . . ?
C72 C75 C76 120.8(3) . . ?
C76 C75 C68 119.9(3) . . ?
C65 C76 C61 119.9(3) . . ?
C65 C76 C75 120.6(3) . . ?
C75 C76 C61 119.5(3) . . ?
C77 O13 C80 109.7(8) . . ?
O13 C77 H77A 108.9 . . ?
O13 C77 H77B 108.9 . . ?
O13 C77 C78 113.2(10) . . ?
H77A C77 H77B 107.7 . . ?
C78 C77 H77A 108.9 . . ?
C78 C77 H77B 108.9 . . ?
C77 C78 H78A 112.6 . . ?
C77 C78 H78B 112.6 . . ?
H78A C78 H78B 110.1 . . ?
C79 C78 C77 95.8(10) . . ?
C79 C78 H78A 112.6 . . ?
C79 C78 H78B 112.6 . . ?
C78 C79 H79A 108.0 . . ?
C78 C79 H79B 108.0 . . ?
C78 C79 C80 117.4(9) . . ?
H79A C79 H79B 107.2 . . ?
C80 C79 H79A 108.0 . . ?
C80 C79 H79B 108.0 . . ?
O13 C80 C79 96.6(8) . . ?
O13 C80 H80A 112.4 . . ?
O13 C80 H80B 112.4 . . ?
C79 C80 H80A 112.4 . . ?
C79 C80 H80B 112.4 . . ?
H80A C80 H80B 110.0 . . ?
C77A O13A C80A 107.0(13) . . ?
O13A C77A H77C 108.8 . . ?
O13A C77A H77D 108.8 . . ?
O13A C77A C78A 113.7(16) . . ?
H77C C77A H77D 107.7 . . ?
C78A C77A H77C 108.8 . . ?
C78A C77A H77D 108.8 . . ?
C77A C78A H78C 112.4 . . ?
C77A C78A H78D 112.4 . . ?
H78C C78A H78D 110.0 . . ?
C79A C78A C77A 96.8(15) . . ?
C79A C78A H78C 112.4 . . ?
C79A C78A H78D 112.4 . . ?
C78A C79A H79C 109.1 . . ?
C78A C79A H79D 109.1 . . ?
H79C C79A H79D 107.8 . . ?
C80A C79A C78A 112.5(14) . . ?
C80A C79A H79C 109.1 . . ?
C80A C79A H79D 109.1 . . ?
O13A C80A C79A 102.4(12) . . ?
O13A C80A H80C 111.3 . . ?
O13A C80A H80D 111.3 . . ?
C79A C80A H80C 111.3 . . ?
C79A C80A H80D 111.3 . . ?
H80C C80A H80D 109.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -3.6(5) . . . . ?
O1 C1 C2 C13 175.5(3) . . . . ?
O4 C7 C8 C9 3.6(5) . . . . ?
O4 C7 C8 C14 -175.8(3) . . . . ?
O6 C21 C22 C23 -1.1(5) . . . . ?
O6 C21 C22 C33 176.0(3) . . . . ?
O8 C27 C28 C29 8.8(5) . . . . ?
O8 C27 C28 C34 -171.3(3) . . . . ?
O9 C41 C42 C43 -1.2(4) . . . . ?
O9 C41 C42 C53 179.1(3) . . . . ?
O12 C47 C48 C49 0.6(5) . . . . ?
O12 C47 C48 C54 179.7(3) . . . . ?
N1 C1 C2 C3 174.8(3) . . . . ?
N1 C1 C2 C13 -6.1(4) . . . . ?
N2 C7 C8 C9 -175.5(3) . . . . ?
N2 C7 C8 C14 5.0(4) . . . . ?
N2 C15 C16 C17 174.1(3) . . . . ?
N2 C15 C20 N3 -50.4(3) . . . . ?
N2 C15 C20 C19 -177.0(3) . . . . ?
N3 C21 C22 C23 179.9(3) . . . . ?
N3 C21 C22 C33 -2.9(4) . . . . ?
N4 C27 C28 C29 -170.5(3) . . . . ?
N4 C27 C28 C34 9.4(4) . . . . ?
N4 C35 C36 C37 172.2(3) . . . . ?
N4 C35 C40 N5 -48.0(4) . . . . ?
N4 C35 C40 C39 -173.0(3) . . . . ?
N5 C41 C42 C43 179.4(3) . . . . ?
N5 C41 C42 C53 -0.3(4) . . . . ?
N6 C47 C48 C49 -178.6(3) . . . . ?
N6 C47 C48 C54 0.5(4) . . . . ?
N6 C55 C56 C57 170.5(3) . . . . ?
N6 C55 C60 N1 -45.5(4) . . . . ?
N6 C55 C60 C59 -171.0(3) . . . . ?
C1 N1 C12 O2 167.7(3) . . . . ?
C1 N1 C12 C11 -12.8(4) . . . . ?
C1 N1 C60 C55 134.3(3) . . . . ?
C1 N1 C60 C59 -102.0(3) . . . . ?
C1 C2 C3 C4 179.6(3) . . . . ?
C1 C2 C13 C11 -1.0(4) . . . . ?
C1 C2 C13 C14 179.9(3) . . . . ?
C2 C3 C4 C5 -0.3(5) . . . . ?
C2 C13 C14 C5 1.2(4) . . . . ?
C2 C13 C14 C8 179.9(3) . . . . ?
C3 C2 C13 C11 178.1(3) . . . . ?
C3 C2 C13 C14 -1.0(4) . . . . ?
C3 C4 C5 C6 -178.2(3) . . . . ?
C3 C4 C5 C14 0.5(5) . . . . ?
C4 C5 C6 O3 4.0(5) . . . . ?
C4 C5 C6 N2 -175.6(3) . . . . ?
C4 C5 C14 C8 -179.7(3) . . . . ?
C4 C5 C14 C13 -1.0(5) . . . . ?
C6 N2 C7 O4 -179.2(3) . . . . ?
C6 N2 C7 C8 -0.1(4) . . . . ?
C6 N2 C15 C16 67.8(4) . . . . ?
C6 N2 C15 C20 -59.0(4) . . . . ?
C6 C5 C14 C8 -0.9(4) . . . . ?
C6 C5 C14 C13 177.8(3) . . . . ?
C7 N2 C6 O3 175.3(3) . . . . ?
C7 N2 C6 C5 -5.1(4) . . . . ?
C7 N2 C15 C16 -106.3(3) . . . . ?
C7 N2 C15 C20 127.0(3) . . . . ?
C7 C8 C9 C10 -177.5(3) . . . . ?
C7 C8 C14 C5 -4.4(4) . . . . ?
C7 C8 C14 C13 176.9(3) . . . . ?
C8 C9 C10 C11 0.4(5) . . . . ?
C9 C8 C14 C5 176.1(3) . . . . ?
C9 C8 C14 C13 -2.6(4) . . . . ?
C9 C10 C11 C12 178.7(3) . . . . ?
C9 C10 C11 C13 -2.1(5) . . . . ?
C10 C11 C12 O2 3.6(4) . . . . ?
C10 C11 C12 N1 -175.9(3) . . . . ?
C10 C11 C13 C2 -177.6(3) . . . . ?
C10 C11 C13 C14 1.5(4) . . . . ?
C11 C13 C14 C5 -177.9(3) . . . . ?
C11 C13 C14 C8 0.8(4) . . . . ?
C12 N1 C1 O1 -168.1(3) . . . . ?
C12 N1 C1 C2 13.5(4) . . . . ?
C12 N1 C60 C55 -52.7(4) . . . . ?
C12 N1 C60 C59 71.0(4) . . . . ?
C12 C11 C13 C2 1.6(4) . . . . ?
C12 C11 C13 C14 -179.3(2) . . . . ?
C13 C2 C3 C4 0.6(5) . . . . ?
C13 C11 C12 O2 -175.6(3) . . . . ?
C13 C11 C12 N1 4.9(4) . . . . ?
C14 C5 C6 O3 -174.8(3) . . . . ?
C14 C5 C6 N2 5.6(4) . . . . ?
C14 C8 C9 C10 2.0(5) . . . . ?
C15 N2 C6 O3 1.8(5) . . . . ?
C15 N2 C6 C5 -178.6(3) . . . . ?
C15 N2 C7 O4 -5.4(4) . . . . ?
C15 N2 C7 C8 173.8(2) . . . . ?
C15 C16 C17 C18 57.4(4) . . . . ?
C16 C15 C20 N3 -177.2(3) . . . . ?
C16 C15 C20 C19 56.2(3) . . . . ?
C16 C17 C18 C19 -58.0(4) . . . . ?
C17 C18 C19 C20 58.4(4) . . . . ?
C18 C19 C20 N3 176.6(3) . . . . ?
C18 C19 C20 C15 -57.0(4) . . . . ?
C20 N3 C21 O6 -0.2(4) . . . . ?
C20 N3 C21 C22 178.7(3) . . . . ?
C20 N3 C32 O5 6.1(5) . . . . ?
C20 N3 C32 C31 -172.4(3) . . . . ?
C20 C15 C16 C17 -57.0(4) . . . . ?
C21 N3 C20 C15 -62.6(4) . . . . ?
C21 N3 C20 C19 62.1(4) . . . . ?
C21 N3 C32 O5 -168.3(3) . . . . ?
C21 N3 C32 C31 13.3(5) . . . . ?
C21 C22 C23 C24 173.4(3) . . . . ?
C21 C22 C33 C31 5.9(5) . . . . ?
C21 C22 C33 C34 -173.5(3) . . . . ?
C22 C23 C24 C25 0.4(6) . . . . ?
C22 C33 C34 C25 -0.2(5) . . . . ?
C22 C33 C34 C28 179.9(3) . . . . ?
C23 C22 C33 C31 -176.9(3) . . . . ?
C23 C22 C33 C34 3.7(5) . . . . ?
C23 C24 C25 C26 -174.7(3) . . . . ?
C23 C24 C25 C34 3.1(5) . . . . ?
C24 C25 C26 O7 -0.7(5) . . . . ?
C24 C25 C26 N4 177.9(3) . . . . ?
C24 C25 C34 C28 176.7(3) . . . . ?
C24 C25 C34 C33 -3.2(5) . . . . ?
C26 N4 C27 O8 165.2(3) . . . . ?
C26 N4 C27 C28 -15.5(4) . . . . ?
C26 N4 C35 C36 -93.8(3) . . . . ?
C26 N4 C35 C40 140.4(3) . . . . ?
C26 C25 C34 C28 -5.4(5) . . . . ?
C26 C25 C34 C33 174.7(3) . . . . ?
C27 N4 C26 O7 -170.5(3) . . . . ?
C27 N4 C26 C25 10.9(4) . . . . ?
C27 N4 C35 C36 78.1(4) . . . . ?
C27 N4 C35 C40 -47.7(4) . . . . ?
C27 C28 C29 C30 179.1(3) . . . . ?
C27 C28 C34 C25 0.7(5) . . . . ?
C27 C28 C34 C33 -179.4(3) . . . . ?
C28 C29 C30 C31 0.3(6) . . . . ?
C29 C28 C34 C25 -179.4(3) . . . . ?
C29 C28 C34 C33 0.4(5) . . . . ?
C29 C30 C31 C32 179.7(3) . . . . ?
C29 C30 C31 C33 0.6(5) . . . . ?
C30 C31 C32 O5 -7.4(5) . . . . ?
C30 C31 C32 N3 171.1(3) . . . . ?
C30 C31 C33 C22 179.6(3) . . . . ?
C30 C31 C33 C34 -1.0(5) . . . . ?
C31 C33 C34 C25 -179.7(3) . . . . ?
C31 C33 C34 C28 0.5(5) . . . . ?
C32 N3 C20 C15 122.8(3) . . . . ?
C32 N3 C20 C19 -112.5(3) . . . . ?
C32 N3 C21 O6 174.0(3) . . . . ?
C32 N3 C21 C22 -7.1(4) . . . . ?
C32 C31 C33 C22 0.5(5) . . . . ?
C32 C31 C33 C34 179.9(3) . . . . ?
C33 C22 C23 C24 -3.8(5) . . . . ?
C33 C31 C32 O5 171.7(3) . . . . ?
C33 C31 C32 N3 -9.8(5) . . . . ?
C34 C25 C26 O7 -178.6(3) . . . . ?
C34 C25 C26 N4 0.0(4) . . . . ?
C34 C28 C29 C30 -0.8(5) . . . . ?
C35 N4 C26 O7 1.1(4) . . . . ?
C35 N4 C26 C25 -177.5(3) . . . . ?
C35 N4 C27 O8 -6.0(5) . . . . ?
C35 N4 C27 C28 173.3(3) . . . . ?
C35 C36 C37 C38 56.9(4) . . . . ?
C36 C35 C40 N5 -174.8(3) . . . . ?
C36 C35 C40 C39 60.2(4) . . . . ?
C36 C37 C38 C39 -56.3(5) . . . . ?
C37 C38 C39 C40 58.4(5) . . . . ?
C38 C39 C40 N5 173.5(3) . . . . ?
C38 C39 C40 C35 -59.9(4) . . . . ?
C40 N5 C41 O9 3.3(4) . . . . ?
C40 N5 C41 C42 -177.3(3) . . . . ?
C40 N5 C52 O10 1.2(5) . . . . ?
C40 N5 C52 C51 -179.0(3) . . . . ?
C40 C35 C36 C37 -59.2(4) . . . . ?
C41 N5 C40 C35 -53.4(4) . . . . ?
C41 N5 C40 C39 70.1(4) . . . . ?
C41 N5 C52 O10 -170.1(3) . . . . ?
C41 N5 C52 C51 9.7(5) . . . . ?
C41 C42 C43 C44 178.4(3) . . . . ?
C41 C42 C53 C51 2.9(4) . . . . ?
C41 C42 C53 C54 -177.6(2) . . . . ?
C42 C43 C44 C45 -0.4(5) . . . . ?
C42 C53 C54 C45 -1.3(4) . . . . ?
C42 C53 C54 C48 -179.6(3) . . . . ?
C43 C42 C53 C51 -176.7(3) . . . . ?
C43 C42 C53 C54 2.7(4) . . . . ?
C43 C44 C45 C46 179.9(3) . . . . ?
C43 C44 C45 C54 1.8(5) . . . . ?
C44 C45 C46 O11 -3.0(4) . . . . ?
C44 C45 C46 N6 177.5(3) . . . . ?
C44 C45 C54 C48 177.3(3) . . . . ?
C44 C45 C54 C53 -1.0(4) . . . . ?
C46 N6 C47 O12 174.7(3) . . . . ?
C46 N6 C47 C48 -6.1(4) . . . . ?
C46 N6 C55 C56 -106.7(3) . . . . ?
C46 N6 C55 C60 128.5(3) . . . . ?
C46 C45 C54 C48 -0.7(4) . . . . ?
C46 C45 C54 C53 -179.0(2) . . . . ?
C47 N6 C46 O11 -171.6(3) . . . . ?
C47 N6 C46 C45 8.0(4) . . . . ?
C47 N6 C55 C56 68.1(4) . . . . ?
C47 N6 C55 C60 -56.7(4) . . . . ?
C47 C48 C49 C50 -179.8(3) . . . . ?
C47 C48 C54 C45 2.7(4) . . . . ?
C47 C48 C54 C53 -179.0(2) . . . . ?
C48 C49 C50 C51 -2.3(6) . . . . ?
C49 C48 C54 C45 -178.2(3) . . . . ?
C49 C48 C54 C53 0.2(4) . . . . ?
C49 C50 C51 C52 -179.8(3) . . . . ?
C49 C50 C51 C53 2.3(5) . . . . ?
C50 C51 C52 O10 -4.7(5) . . . . ?
C50 C51 C52 N5 175.6(3) . . . . ?
C50 C51 C53 C42 178.4(3) . . . . ?
C50 C51 C53 C54 -1.0(5) . . . . ?
C51 C53 C54 C45 178.2(3) . . . . ?
C51 C53 C54 C48 -0.2(4) . . . . ?
C52 N5 C40 C35 134.8(3) . . . . ?
C52 N5 C40 C39 -101.6(3) . . . . ?
C52 N5 C41 O9 174.3(3) . . . . ?
C52 N5 C41 C42 -6.4(4) . . . . ?
C52 C51 C53 C42 0.5(4) . . . . ?
C52 C51 C53 C54 -178.9(3) . . . . ?
C53 C42 C43 C44 -1.9(5) . . . . ?
C53 C51 C52 O10 173.2(3) . . . . ?
C53 C51 C52 N5 -6.5(5) . . . . ?
C54 C45 C46 O11 175.1(3) . . . . ?
C54 C45 C46 N6 -4.4(4) . . . . ?
C54 C48 C49 C50 1.0(5) . . . . ?
C55 N6 C46 O11 3.0(4) . . . . ?
C55 N6 C46 C45 -177.4(2) . . . . ?
C55 N6 C47 O12 0.3(4) . . . . ?
C55 N6 C47 C48 179.6(3) . . . . ?
C55 C56 C57 C58 58.8(4) . . . . ?
C56 C55 C60 N1 -172.4(3) . . . . ?
C56 C55 C60 C59 62.1(4) . . . . ?
C56 C57 C58 C59 -55.9(5) . . . . ?
C57 C58 C59 C60 55.5(5) . . . . ?
C58 C59 C60 N1 176.0(3) . . . . ?
C58 C59 C60 C55 -58.2(4) . . . . ?
C60 N1 C1 O1 4.6(4) . . . . ?
C60 N1 C1 C2 -173.8(3) . . . . ?
C60 N1 C12 O2 -4.7(4) . . . . ?
C60 N1 C12 C11 174.8(2) . . . . ?
C60 C55 C56 C57 -61.9(4) . . . . ?
C61 C62 C63 C64 1.8(6) . . . . ?
C62 C61 C74 C73 -179.2(3) . . . . ?
C62 C61 C76 C65 -0.5(4) . . . . ?
C62 C61 C76 C75 179.0(3) . . . . ?
C62 C63 C64 C65 -0.4(6) . . . . ?
C63 C64 C65 C66 -179.4(3) . . . . ?
C63 C64 C65 C76 -1.4(5) . . . . ?
C64 C65 C66 C67 178.0(3) . . . . ?
C64 C65 C76 C61 1.8(5) . . . . ?
C64 C65 C76 C75 -177.7(3) . . . . ?
C65 C66 C67 C68 -0.1(5) . . . . ?
C66 C65 C76 C61 179.9(3) . . . . ?
C66 C65 C76 C75 0.4(4) . . . . ?
C66 C67 C68 C69 -179.3(3) . . . . ?
C66 C67 C68 C75 -0.2(5) . . . . ?
C67 C68 C69 C70 179.8(3) . . . . ?
C67 C68 C75 C72 180.0(3) . . . . ?
C67 C68 C75 C76 0.6(4) . . . . ?
C68 C69 C70 C71 0.6(6) . . . . ?
C68 C75 C76 C61 179.8(3) . . . . ?
C68 C75 C76 C65 -0.7(4) . . . . ?
C69 C68 C75 C72 -0.9(4) . . . . ?
C69 C68 C75 C76 179.7(3) . . . . ?
C69 C70 C71 C72 -1.7(6) . . . . ?
C70 C71 C72 C73 -179.6(3) . . . . ?
C70 C71 C72 C75 1.5(5) . . . . ?
C71 C72 C73 C74 -179.4(3) . . . . ?
C71 C72 C75 C68 -0.2(5) . . . . ?
C71 C72 C75 C76 179.2(3) . . . . ?
C72 C73 C74 C61 0.0(5) . . . . ?
C72 C75 C76 C61 0.4(4) . . . . ?
C72 C75 C76 C65 179.9(3) . . . . ?
C73 C72 C75 C68 -179.2(3) . . . . ?
C73 C72 C75 C76 0.2(4) . . . . ?
C74 C61 C62 C63 178.5(3) . . . . ?
C74 C61 C76 C65 179.7(3) . . . . ?
C74 C61 C76 C75 -0.8(4) . . . . ?
C75 C68 C69 C70 0.7(5) . . . . ?
C75 C72 C73 C74 -0.4(5) . . . . ?
C76 C61 C62 C63 -1.3(5) . . . . ?
C76 C61 C74 C73 0.6(5) . . . . ?
C76 C65 C66 C67 0.0(5) . . . . ?
O13 C77 C78 C79 -4.6(15) . . . . ?
C77 O13 C80 C79 22.4(10) . . . . ?
C77 C78 C79 C80 21.1(15) . . . . ?
C78 C79 C80 O13 -28.6(13) . . . . ?
C80 O13 C77 C78 -12.9(14) . . . . ?
O13A C77A C78A C79A -2(3) . . . . ?
C77A O13A C80A C79A 25.1(17) . . . . ?
C77A C78A C79A C80A 18(3) . . . . ?
C78A C79A C80A O13A -28(2) . . . . ?
C80A O13A C77A C78A -15(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 1.374
_oxdiff_exptl_absorpt_empirical_full_min 0.755
####################################################################### 
# 
# 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_dca-r
_database_code_depnum_ccdc_archive 'CCDC 2391870'
loop_
_audit_author_name
_audit_author_address
'Jialin Cui'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2024-10-15 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_audit_creation_date             2024-09-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.667(C60 H42 N6 O12), C14 H8 Cl2, C H2 Cl2, 4.2[CH2Cl2]'
_chemical_formula_sum            'C55 H38 Cl4 N4 O8'
_chemical_formula_weight         1024.69
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'

_cell_length_a                   24.6956(4)
_cell_length_b                   24.6956(4)
_cell_length_c                   25.1324(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13274.1(5)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    7478
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7230
_cell_measurement_theta_min      2.6890
_shelx_estimated_absorpt_T_max   0.702
_shelx_estimated_absorpt_T_min   0.663
_exptl_absorpt_coefficient_mu    2.241
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13674
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.489
_diffrn_reflns_theta_min         2.713
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     89.00 168.00   0.50    0.25    --  109.82 111.00  30.00  158
  2  ω     93.00 144.00   0.50    0.25    --  109.82  89.00  -7.00  102
  3  ω     40.00 108.00   0.50    0.25    --  109.82-126.00-108.00  136
  4  ω    -10.00  42.00   0.50    0.06    --  -36.36  19.00 -30.00  104
  5  ω    -47.00 -22.00   0.50    0.25    -- -102.00  45.00 -60.00   50
  6  ω    -22.00  38.00   0.50    0.06    --  -36.36  19.00-180.00  120
  7  ω    -49.00 -22.00   0.50    0.25    -- -102.00  45.00  30.00   54
  8  ω    -48.00 -22.00   0.50    0.25    -- -102.00  45.00  60.00   52
  9  ω    -48.00 -23.00   0.50    0.25    -- -102.00  45.00 120.00   50
 10  ω    -85.00  -2.00   0.50    0.06    --  -36.36 -26.00 -16.00  166
 11  ω    -75.00 -30.00   0.50    0.25    -- -102.00 105.00 154.00   90
 12  ω   -144.00 -50.00   0.50    0.25    -- -102.00 178.00 150.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0177130000
_diffrn_orient_matrix_UB_12      -0.0279452000
_diffrn_orient_matrix_UB_13      0.0563564000
_diffrn_orient_matrix_UB_21      0.0673406000
_diffrn_orient_matrix_UB_22      0.0446485000
_diffrn_orient_matrix_UB_23      0.0189349000
_diffrn_orient_matrix_UB_31      -0.0185218000
_diffrn_orient_matrix_UB_32      0.0490732000
_diffrn_orient_matrix_UB_33      0.0149828000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.918
_reflns_Friedel_fraction_max     0.835
_reflns_number_gt                5006
_reflns_number_total             5487
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 
;
 Flack x determined using 1975 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.101(13)
_refine_ls_extinction_coef       0.00036(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         5487
_refine_ls_number_restraints     675
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0727
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1490P)²+18.5638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2201
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C22A-C21A = C34A-C21A = C34-C21 = C22-C21 = C28-C27 = C29A-C28A = C28A-C27A
 1.39 with sigma of 0.01
 Cl4-C42 = Cl3-C42 = Cl4A-C42A = Cl3A-C42A
 1.79 with sigma of 0.01
 Cl3-Cl4 = Cl3A-Cl4A
 2.924 with sigma of 0.02
3. Restrained planarity
 C21, Cl2, C28, C27, C29, C22, C26, C30, C34, C23, C25, C31, C33, C24, Cl1, C32
 with sigma of 0.1
 Cl1A, C21A, C22A, C34A, C27A, C23A, C29A, C33A, C28A, C26A, C24A, C30A, C32A,
 Cl2A, C25A, C31A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C21A \\sim C22A \\sim C34A \\sim Cl1A \\sim C27A \\sim C23A \\sim C29A \\sim
C33A \\sim C28A \\sim C26A \\sim C24A \\sim C30A \\sim C32A \\sim Cl2A \\sim
C25A \\sim C31A \\sim C21 \\sim Cl2 \\sim C28 \\sim C29 \\sim C27 \\sim C30
\\sim C34 \\sim C22 \\sim C26 \\sim C31 \\sim C33 \\sim C23 \\sim C25 \\sim C32
\\sim Cl1 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C42A \\sim Cl3A \\sim Cl4A \\sim C42 \\sim Cl3 \\sim Cl4: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Sof(C21A)=Sof(Cl2A)=Sof(C28A)=Sof(C23A)=Sof(H23A)=Sof(C22A)=Sof(C27A)=
 Sof(C26A)=Sof(H26A)=Sof(C25A)=Sof(H25A)=Sof(C24A)=Sof(H24A)=Sof(Cl1A)=
 Sof(C32A)=Sof(H32A)=Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(H30A)=Sof(C29A)=
 Sof(C34A)=Sof(C33A)=Sof(H33A)=0.5*(1-FVAR(2))
 Sof(Cl2)=Sof(C23)=Sof(H23)=Sof(C22)=Sof(C27)=Sof(C26)=Sof(H26)=Sof(C25)=
 Sof(H25)=Sof(C24)=Sof(H24)=Sof(C28)=Sof(C32)=Sof(H32)=Sof(C31)=Sof(H31)=
 Sof(C30)=Sof(H30)=Sof(C29)=Sof(C34)=Sof(C33)=Sof(H33)=Sof(C21)=Sof(Cl1)=0.5*
 FVAR(2)
 Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(Cl3A)=Sof(Cl4A)=0.5*(1-FVAR(3))
 Sof(Cl3)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(Cl4)=0.5*FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B), C5(H5A,H5B), C4(H4A,H4B), C42(H42A,H42B), C42A(H42C,
 H42D)
6.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C26(H26), C25(H25), C24(H24), C9(H9), C16(H16), C15(H15), C10(H10),
 C32(H32), C31(H31), C30(H30), C33(H33), C23A(H23A), C26A(H26A), C25A(H25A),
 C24A(H24A), C32A(H32A), C31A(H31A), C30A(H30A), C33A(H33A)
6.d Fitted hexagon refined as free rotating group:
 C23(C22,C27,C26,C25,C24), C32(C31,C30,C29,C34,C33), C23A(C22A,C27A,C26A,C25A,
 C24A), C32A(C31A,C30A,C29A,C34A,C33A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
O1 O 0.28607(18) 0.43717(18) 0.60946(14) 0.0454(9) Uani 1 1 d . . . . .
O2 O 0.56919(15) 0.72102(16) 0.59114(15) 0.0394(8) Uani 1 1 d . . . . .
Cl2 Cl 0.6087(2) 0.6043(2) 0.5538(2) 0.0507(11) Uani 0.368(2) 1 d . U P A -1
O4 O 0.27051(17) 0.42789(18) 0.42954(14) 0.0421(8) Uani 1 1 d . . . . .
C23 C 0.4004(6) 0.3965(6) 0.5644(5) 0.052(4) Uani 0.368(2) 1 d G U P A -1
H23 H 0.364508 0.362670 0.548516 0.062 Uiso 0.368(2) 1 calc R U P A -1
C22 C 0.4461(8) 0.4430(8) 0.5327(4) 0.041(3) Uani 0.368(2) 1 d DG U P A -1
C27 C 0.4986(7) 0.4924(8) 0.5560(5) 0.039(3) Uani 0.368(2) 1 d DG U P A -1
C26 C 0.5055(5) 0.4953(6) 0.6110(5) 0.044(3) Uani 0.368(2) 1 d G U P A -1
H26 H 0.541353 0.529110 0.626947 0.052 Uiso 0.368(2) 1 calc R U P A -1
C25 C 0.4598(6) 0.4488(6) 0.6427(4) 0.052(3) Uani 0.368(2) 1 d G U P A -1
H25 H 0.464471 0.450729 0.680315 0.062 Uiso 0.368(2) 1 calc R U P A -1
C24 C 0.4073(5) 0.3993(5) 0.6194(5) 0.055(3) Uani 0.368(2) 1 d G U P A -1
H24 H 0.376048 0.367509 0.641101 0.066 Uiso 0.368(2) 1 calc R U P A -1
O3 O 0.55313(18) 0.71174(19) 0.41027(15) 0.0471(9) Uani 1 1 d . . . . .
N1 N 0.27336(19) 0.43515(18) 0.51920(16) 0.0335(8) Uani 1 1 d . . . . .
N2 N 0.56095(18) 0.71955(18) 0.50090(17) 0.0336(8) Uani 1 1 d . . . . .
C19 C 0.3897(2) 0.5474(2) 0.51247(18) 0.0302(9) Uani 1 1 d . . . . .
C11 C 0.4802(2) 0.6345(2) 0.55493(17) 0.0302(9) Uani 1 1 d . . . . .
C9 C 0.4013(2) 0.5504(2) 0.60690(17) 0.0330(10) Uani 1 1 d . . . . .
H9 H 0.386321 0.531836 0.640775 0.040 Uiso 1 1 calc R U . . .
C17 C 0.3572(2) 0.5169(2) 0.46477(17) 0.0322(9) Uani 1 1 d . . . . .
C20 C 0.4470(2) 0.6049(2) 0.50740(17) 0.0290(9) Uani 1 1 d . . . . .
C18 C 0.2973(2) 0.4568(2) 0.46884(19) 0.0330(10) Uani 1 1 d . . . . .
C16 C 0.3810(3) 0.5424(2) 0.41590(19) 0.0392(11) Uani 1 1 d . . . . .
H16 H 0.359035 0.521836 0.384424 0.047 Uiso 1 1 calc R U . . .
C8 C 0.3666(2) 0.5211(2) 0.56255(17) 0.0296(9) Uani 1 1 d . . . . .
C14 C 0.4703(2) 0.6303(2) 0.45764(19) 0.0347(10) Uani 1 1 d . . . . .
C7 C 0.3062(2) 0.4619(2) 0.56791(18) 0.0323(10) Uani 1 1 d . . . . .
C12 C 0.5403(2) 0.6953(2) 0.5507(2) 0.0332(9) Uani 1 1 d . . . . .
C13 C 0.5309(2) 0.6897(2) 0.45245(18) 0.0334(10) Uani 1 1 d . . . . .
C15 C 0.4384(3) 0.5996(2) 0.41245(19) 0.0389(11) Uani 1 1 d . . . . .
H15 H 0.454989 0.616859 0.378516 0.047 Uiso 1 1 calc R U . . .
C10 C 0.4575(2) 0.6065(2) 0.60383(18) 0.0355(10) Uani 1 1 d . . . . .
H10 H 0.480470 0.625549 0.635320 0.043 Uiso 1 1 calc R U . . .
C1 C 0.2112(2) 0.3774(2) 0.5260(2) 0.0370(10) Uani 1 1 d . . . . .
H1 H 0.200068 0.375059 0.564535 0.044 Uiso 1 1 calc R U . . .
C2 C 0.1588(2) 0.3783(2) 0.4949(2) 0.0390(11) Uani 1 1 d . . . . .
H2 H 0.165827 0.373629 0.456439 0.047 Uiso 1 1 calc R U . . .
C6 C 0.2136(3) 0.3183(3) 0.5133(3) 0.0475(12) Uani 1 1 d . . . . .
H6A H 0.247184 0.317682 0.534262 0.057 Uiso 1 1 calc R U . . .
H6B H 0.223076 0.317861 0.475046 0.057 Uiso 1 1 calc R U . . .
C3 C 0.0957(3) 0.3217(2) 0.5105(3) 0.0545(16) Uani 1 1 d . . . . .
H3A H 0.061604 0.322031 0.489970 0.065 Uiso 1 1 calc R U . . .
H3B H 0.087622 0.323652 0.548821 0.065 Uiso 1 1 calc R U . . .
C5 C 0.1507(3) 0.2605(2) 0.5265(3) 0.0597(17) Uani 1 1 d . . . . .
H5A H 0.151809 0.222471 0.515999 0.072 Uiso 1 1 calc R U . . .
H5B H 0.143743 0.258724 0.565449 0.072 Uiso 1 1 calc R U . . .
C4 C 0.0975(3) 0.2616(3) 0.4985(4) 0.066(2) Uani 1 1 d . . . . .
H4A H 0.057555 0.224959 0.509818 0.079 Uiso 1 1 calc R U . . .
H4B H 0.101831 0.258291 0.459643 0.079 Uiso 1 1 calc R U . . .
C28 C 0.5431(7) 0.5403(7) 0.5244(7) 0.038(3) Uani 0.368(2) 1 d D U P A -1
C32 C 0.5317(5) 0.5342(5) 0.3571(3) 0.043(3) Uani 0.368(2) 1 d G U P A -1
H32 H 0.528686 0.532206 0.319422 0.052 Uiso 0.368(2) 1 calc R U P A -1
C31 C 0.5828(5) 0.5842(5) 0.3816(4) 0.048(3) Uani 0.368(2) 1 d G U P A -1
H31 H 0.614644 0.616238 0.360545 0.058 Uiso 0.368(2) 1 calc R U P A -1
C30 C 0.5872(5) 0.5871(6) 0.4367(4) 0.044(3) Uani 0.368(2) 1 d G U P A -1
H30 H 0.622110 0.621238 0.453426 0.053 Uiso 0.368(2) 1 calc R U P A -1
C29 C 0.5406(7) 0.5402(7) 0.4675(3) 0.040(3) Uani 0.368(2) 1 d G U P A -1
C34 C 0.4895(7) 0.4903(6) 0.4431(5) 0.039(3) Uani 0.368(2) 1 d DG U P A -1
C33 C 0.4851(6) 0.4873(5) 0.3879(5) 0.042(3) Uani 0.368(2) 1 d G U P A -1
H33 H 0.450194 0.453174 0.371183 0.050 Uiso 0.368(2) 1 calc R U P A -1
C21 C 0.4441(9) 0.4439(8) 0.4768(5) 0.036(3) Uani 0.368(2) 1 d D U P A -1
Cl1 Cl 0.3777(2) 0.3801(2) 0.4464(2) 0.0558(12) Uani 0.368(2) 1 d . U P A -1
C21A C 0.4302(13) 0.4309(13) 0.4941(10) 0.042(4) Uani 0.132(2) 1 d D U P A -2
Cl2A Cl 0.6068(8) 0.6105(9) 0.4916(7) 0.047(4) Uani 0.132(2) 1 d . U P A -2
C28A C 0.5378(18) 0.5399(18) 0.5032(10) 0.038(4) Uani 0.132(2) 1 d D U P A -2
C23A C 0.4214(13) 0.4183(13) 0.5901(14) 0.049(5) Uani 0.132(2) 1 d G U P A -2
H23A H 0.383550 0.379596 0.586467 0.059 Uiso 0.132(2) 1 calc R U P A -2
C22A C 0.4528(15) 0.4522(16) 0.5451(11) 0.041(4) Uani 0.132(2) 1 d DG U P A -2
C27A C 0.5081(15) 0.5089(16) 0.5503(11) 0.039(4) Uani 0.132(2) 1 d DG U P A -2
C26A C 0.5321(12) 0.5317(13) 0.6006(13) 0.041(5) Uani 0.132(2) 1 d G U P A -2
H26A H 0.569900 0.570450 0.604242 0.049 Uiso 0.132(2) 1 calc R U P A -2
C25A C 0.5007(14) 0.4978(15) 0.6457(10) 0.047(5) Uani 0.132(2) 1 d G U P A -2
H25A H 0.517063 0.513435 0.680026 0.057 Uiso 0.132(2) 1 calc R U P A -2
C24A C 0.4453(15) 0.4412(15) 0.6404(11) 0.052(5) Uani 0.132(2) 1 d G U P A -2
H24A H 0.423888 0.418007 0.671140 0.062 Uiso 0.132(2) 1 calc R U P A -2
Cl1A Cl 0.3584(13) 0.3575(12) 0.5066(14) 0.056(5) Uani 0.132(2) 1 d . U P A -2
C32A C 0.4628(14) 0.4692(15) 0.3534(10) 0.042(6) Uani 0.132(2) 1 d G U P A -2
H32A H 0.444129 0.451491 0.320157 0.050 Uiso 0.132(2) 1 calc R U P A -2
C31A C 0.5191(14) 0.5254(14) 0.3551(10) 0.043(5) Uani 0.132(2) 1 d G U P A -2
H31A H 0.538938 0.546100 0.323010 0.052 Uiso 0.132(2) 1 calc R U P A -2
C30A C 0.5465(13) 0.5513(13) 0.4038(13) 0.043(4) Uani 0.132(2) 1 d G U P A -2
H30A H 0.584967 0.589747 0.405007 0.052 Uiso 0.132(2) 1 calc R U P A -2
C29A C 0.5175(16) 0.5211(15) 0.4509(10) 0.040(4) Uani 0.132(2) 1 d DG U P A -2
C34A C 0.4612(16) 0.4649(15) 0.4492(10) 0.041(4) Uani 0.132(2) 1 d DG U P A -2
C33A C 0.4338(12) 0.4389(12) 0.4005(12) 0.040(4) Uani 0.132(2) 1 d G U P A -2
H33A H 0.395350 0.400527 0.399304 0.048 Uiso 0.132(2) 1 calc R U P A -2
Cl3 Cl 0.6195(11) 0.6913(14) 0.2928(8) 0.089(6) Uani 0.258(7) 1 d D U P B -1
C42 C 0.6789(14) 0.7542(12) 0.3315(15) 0.106(8) Uani 0.258(7) 1 d D U P B -1
H42A H 0.706392 0.788434 0.307038 0.127 Uiso 0.258(7) 1 calc R U P B -1
H42B H 0.658395 0.770549 0.355324 0.127 Uiso 0.258(7) 1 calc R U P B -1
Cl4 Cl 0.7265(10) 0.7342(12) 0.3712(9) 0.093(6) Uani 0.258(7) 1 d D U P B -1
C42A C 0.6751(19) 0.7276(15) 0.3430(11) 0.084(7) Uani 0.242(7) 1 d D U P B -2
H42C H 0.713388 0.768590 0.337431 0.101 Uiso 0.242(7) 1 calc R U P B -2
H42D H 0.652198 0.732784 0.373102 0.101 Uiso 0.242(7) 1 calc R U P B -2
Cl3A Cl 0.6277(9) 0.7110(10) 0.2852(7) 0.090(5) Uani 0.242(7) 1 d D U P B -2
Cl4A Cl 0.6991(4) 0.6739(5) 0.3635(3) 0.080(3) Uani 0.242(7) 1 d D U P B -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C7 1.186(6) . ?
O2 C12 1.222(6) . ?
Cl2 C28 1.763(19) . ?
O4 C18 1.204(6) . ?
C23 H23 0.9500 . ?
C23 C22 1.3900 . ?
C23 C24 1.3900 . ?
C22 C27 1.3900 . ?
C22 C21 1.408(11) . ?
C27 C26 1.3900 . ?
C27 C28 1.391(12) . ?
C26 H26 0.9500 . ?
C26 C25 1.3900 . ?
C25 H25 0.9500 . ?
C25 C24 1.3900 . ?
C24 H24 0.9500 . ?
O3 C13 1.193(6) . ?
N1 C18 1.386(6) . ?
N1 C7 1.434(6) . ?
N1 C1 1.493(6) . ?
N2 C12 1.370(6) . ?
N2 C13 1.425(6) . ?
N2 C2 1.510(6) 2_665 ?
C19 C17 1.430(6) . ?
C19 C20 1.423(6) . ?
C19 C8 1.400(6) . ?
C11 C20 1.427(6) . ?
C11 C12 1.497(6) . ?
C11 C10 1.384(7) . ?
C9 H9 0.9500 . ?
C9 C8 1.370(6) . ?
C9 C10 1.389(7) . ?
C17 C18 1.486(7) . ?
C17 C16 1.371(7) . ?
C20 C14 1.389(7) . ?
C16 H16 0.9500 . ?
C16 C15 1.417(8) . ?
C8 C7 1.484(6) . ?
C14 C13 1.488(7) . ?
C14 C15 1.375(7) . ?
C15 H15 0.9500 . ?
C10 H10 0.9500 . ?
C1 H1 1.0000 . ?
C1 C2 1.520(7) . ?
C1 C6 1.525(7) . ?
C2 H2 1.0000 . ?
C2 C3 1.535(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.530(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.538(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C4 1.503(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C28 C29 1.432(17) . ?
C32 H32 0.9500 . ?
C32 C31 1.3900 . ?
C32 C33 1.3900 . ?
C31 H31 0.9500 . ?
C31 C30 1.3900 . ?
C30 H30 0.9500 . ?
C30 C29 1.3900 . ?
C29 C34 1.3900 . ?
C34 C33 1.3900 . ?
C34 C21 1.416(11) . ?
C33 H33 0.9500 . ?
C21 Cl1 1.781(17) . ?
C21A C22A 1.391(14) . ?
C21A Cl1A 1.82(3) . ?
C21A C34A 1.386(14) . ?
Cl2A C28A 1.75(3) . ?
C28A C27A 1.402(14) . ?
C28A C29A 1.401(14) . ?
C23A H23A 0.9500 . ?
C23A C22A 1.3900 . ?
C23A C24A 1.3900 . ?
C22A C27A 1.3900 . ?
C27A C26A 1.3900 . ?
C26A H26A 0.9500 . ?
C26A C25A 1.3900 . ?
C25A H25A 0.9500 . ?
C25A C24A 1.3900 . ?
C24A H24A 0.9500 . ?
C32A H32A 0.9500 . ?
C32A C31A 1.3900 . ?
C32A C33A 1.3900 . ?
C31A H31A 0.9500 . ?
C31A C30A 1.3900 . ?
C30A H30A 0.9500 . ?
C30A C29A 1.3900 . ?
C29A C34A 1.3900 . ?
C34A C33A 1.3900 . ?
C33A H33A 0.9500 . ?
Cl3 C42 1.798(14) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 Cl4 1.791(14) . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C42A Cl3A 1.782(14) . ?
C42A Cl4A 1.777(14) . ?

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
C22 C23 H23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C22 C27 120.0 . . ?
C23 C22 C21 124.4(13) . . ?
C27 C22 C21 115.6(13) . . ?
C22 C27 C28 119.9(12) . . ?
C26 C27 C22 120.0 . . ?
C26 C27 C28 120.0(12) . . ?
C27 C26 H26 120.0 . . ?
C27 C26 C25 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C25 H25 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24 120.0 . . ?
C18 N1 C7 124.6(4) . . ?
C18 N1 C1 120.6(4) . . ?
C7 N1 C1 114.6(4) . . ?
C12 N2 C13 124.8(4) . . ?
C12 N2 C2 119.6(4) . 2_665 ?
C13 N2 C2 115.6(4) . 2_665 ?
C20 C19 C17 117.8(4) . . ?
C8 C19 C17 121.2(4) . . ?
C8 C19 C20 120.9(4) . . ?
C20 C11 C12 118.8(4) . . ?
C10 C11 C20 120.1(4) . . ?
C10 C11 C12 121.1(4) . . ?
C8 C9 H9 119.0 . . ?
C8 C9 C10 122.0(4) . . ?
C10 C9 H9 119.0 . . ?
C19 C17 C18 119.0(4) . . ?
C16 C17 C19 120.7(5) . . ?
C16 C17 C18 120.3(4) . . ?
C19 C20 C11 117.8(4) . . ?
C14 C20 C19 120.8(4) . . ?
C14 C20 C11 121.3(4) . . ?
O4 C18 N1 121.3(5) . . ?
O4 C18 C17 120.9(5) . . ?
N1 C18 C17 117.9(4) . . ?
C17 C16 H16 120.1 . . ?
C17 C16 C15 119.9(4) . . ?
C15 C16 H16 120.1 . . ?
C19 C8 C7 120.9(4) . . ?
C9 C8 C19 119.0(4) . . ?
C9 C8 C7 120.1(4) . . ?
C20 C14 C13 120.7(4) . . ?
C15 C14 C20 120.0(5) . . ?
C15 C14 C13 119.2(4) . . ?
O1 C7 N1 121.3(4) . . ?
O1 C7 C8 122.9(4) . . ?
N1 C7 C8 115.8(4) . . ?
O2 C12 N2 122.7(4) . . ?
O2 C12 C11 119.3(4) . . ?
N2 C12 C11 118.0(4) . . ?
O3 C13 N2 121.5(5) . . ?
O3 C13 C14 122.3(4) . . ?
N2 C13 C14 116.2(4) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 C16 120.7(4) . . ?
C14 C15 H15 119.6 . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
N1 C1 H1 106.7 . . ?
N1 C1 C2 113.8(4) . . ?
N1 C1 C6 112.1(4) . . ?
C2 C1 H1 106.7 . . ?
C2 C1 C6 110.3(4) . . ?
C6 C1 H1 106.7 . . ?
N2 C2 C1 112.8(4) 3_565 . ?
N2 C2 H2 107.3 3_565 . ?
N2 C2 C3 111.9(4) 3_565 . ?
C1 C2 H2 107.3 . . ?
C1 C2 C3 109.9(5) . . ?
C3 C2 H2 107.3 . . ?
C1 C6 H6A 109.7 . . ?
C1 C6 H6B 109.7 . . ?
C1 C6 C5 109.9(5) . . ?
H6A C6 H6B 108.2 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
C2 C3 H3A 109.9 . . ?
C2 C3 H3B 109.9 . . ?
C2 C3 C4 108.8(5) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
C4 C5 C6 111.7(5) . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
C5 C4 C3 111.9(5) . . ?
C5 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C27 C28 Cl2 120.2(13) . . ?
C27 C28 C29 123.7(18) . . ?
C29 C28 Cl2 116.0(13) . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.0 . . ?
C33 C32 H32 120.0 . . ?
C32 C31 H31 120.0 . . ?
C30 C31 C32 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 C31 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C29 C28 122.5(13) . . ?
C30 C29 C34 120.0 . . ?
C34 C29 C28 117.5(13) . . ?
C29 C34 C21 117.0(10) . . ?
C33 C34 C29 120.0 . . ?
C33 C34 C21 123.0(10) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C22 C21 C34 126.2(16) . . ?
C22 C21 Cl1 116.0(13) . . ?
C34 C21 Cl1 117.8(10) . . ?
C22A C21A Cl1A 103(2) . . ?
C34A C21A C22A 122(2) . . ?
C34A C21A Cl1A 135(3) . . ?
C27A C28A Cl2A 132(2) . . ?
C29A C28A Cl2A 101(2) . . ?
C29A C28A C27A 128(2) . . ?
C22A C23A H23A 120.0 . . ?
C22A C23A C24A 120.0 . . ?
C24A C23A H23A 120.0 . . ?
C23A C22A C21A 122(3) . . ?
C27A C22A C21A 118(3) . . ?
C27A C22A C23A 120.0 . . ?
C22A C27A C28A 117(3) . . ?
C22A C27A C26A 120.0 . . ?
C26A C27A C28A 123(3) . . ?
C27A C26A H26A 120.0 . . ?
C25A C26A C27A 120.0 . . ?
C25A C26A H26A 120.0 . . ?
C26A C25A H25A 120.0 . . ?
C26A C25A C24A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C25A C24A C23A 120.0 . . ?
C25A C24A H24A 120.0 . . ?
C31A C32A H32A 120.0 . . ?
C31A C32A C33A 120.0 . . ?
C33A C32A H32A 120.0 . . ?
C32A C31A H31A 120.0 . . ?
C30A C31A C32A 120.0 . . ?
C30A C31A H31A 120.0 . . ?
C31A C30A H30A 120.0 . . ?
C31A C30A C29A 120.0 . . ?
C29A C30A H30A 120.0 . . ?
C30A C29A C28A 128(3) . . ?
C30A C29A C34A 120.0 . . ?
C34A C29A C28A 112(3) . . ?
C21A C34A C29A 124(3) . . ?
C21A C34A C33A 116(2) . . ?
C29A C34A C33A 120.0 . . ?
C32A C33A H33A 120.0 . . ?
C34A C33A C32A 120.0 . . ?
C34A C33A H33A 120.0 . . ?
Cl3 C42 H42A 108.5 . . ?
Cl3 C42 H42B 108.5 . . ?
H42A C42 H42B 107.5 . . ?
Cl4 C42 Cl3 115.3(13) . . ?
Cl4 C42 H42A 108.5 . . ?
Cl4 C42 H42B 108.5 . . ?
H42C C42A H42D 107.0 . . ?
Cl3A C42A H42C 107.5 . . ?
Cl3A C42A H42D 107.5 . . ?
Cl4A C42A H42C 107.5 . . ?
Cl4A C42A H42D 107.5 . . ?
Cl4A C42A Cl3A 119.3(14) . . ?

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
Cl2 C28 C29 C30 0.7(11) . . . . ?
Cl2 C28 C29 C34 179.8(7) . . . . ?
C23 C22 C27 C26 0.0 . . . . ?
C23 C22 C27 C28 -177.5(15) . . . . ?
C23 C22 C21 C34 -179.9(13) . . . . ?
C23 C22 C21 Cl1 0.1(13) . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C22 C27 C26 C25 0.0 . . . . ?
C22 C27 C28 Cl2 178.2(7) . . . . ?
C22 C27 C28 C29 -4.4(17) . . . . ?
C27 C22 C21 C34 -1.0(15) . . . . ?
C27 C22 C21 Cl1 179.0(11) . . . . ?
C27 C26 C25 C24 0.0 . . . . ?
C27 C28 C29 C30 -176.9(7) . . . . ?
C27 C28 C29 C34 2.3(13) . . . . ?
C26 C27 C28 Cl2 0.7(12) . . . . ?
C26 C27 C28 C29 178.1(10) . . . . ?
C26 C25 C24 C23 0.0 . . . . ?
C24 C23 C22 C27 0.0 . . . . ?
C24 C23 C22 C21 178.9(12) . . . . ?
N1 C1 C2 N2 -46.4(6) . . . 3_565 ?
N1 C1 C2 C3 -172.1(4) . . . . ?
N1 C1 C6 C5 174.0(5) . . . . ?
N2 C2 C3 C4 174.8(5) 3_565 . . . ?
C19 C17 C18 O4 -175.4(4) . . . . ?
C19 C17 C18 N1 4.7(6) . . . . ?
C19 C17 C16 C15 -0.1(7) . . . . ?
C19 C20 C14 C13 -178.7(4) . . . . ?
C19 C20 C14 C15 -0.7(7) . . . . ?
C19 C8 C7 O1 177.6(4) . . . . ?
C19 C8 C7 N1 -1.7(6) . . . . ?
C11 C20 C14 C13 -0.3(7) . . . . ?
C11 C20 C14 C15 177.7(4) . . . . ?
C9 C8 C7 O1 -1.2(7) . . . . ?
C9 C8 C7 N1 179.6(4) . . . . ?
C17 C19 C20 C11 -178.6(4) . . . . ?
C17 C19 C20 C14 -0.2(7) . . . . ?
C17 C19 C8 C9 176.6(4) . . . . ?
C17 C19 C8 C7 -2.2(7) . . . . ?
C17 C16 C15 C14 -0.7(8) . . . . ?
C20 C19 C17 C18 179.9(4) . . . . ?
C20 C19 C17 C16 0.6(7) . . . . ?
C20 C19 C8 C9 -2.6(7) . . . . ?
C20 C19 C8 C7 178.7(4) . . . . ?
C20 C11 C12 O2 -179.8(4) . . . . ?
C20 C11 C12 N2 -0.6(6) . . . . ?
C20 C11 C10 C9 -2.2(7) . . . . ?
C20 C14 C13 O3 177.6(5) . . . . ?
C20 C14 C13 N2 -3.0(7) . . . . ?
C20 C14 C15 C16 1.1(7) . . . . ?
C18 N1 C7 O1 -171.6(4) . . . . ?
C18 N1 C7 C8 7.7(6) . . . . ?
C18 N1 C1 C2 -52.6(6) . . . . ?
C18 N1 C1 C6 73.4(6) . . . . ?
C18 C17 C16 C15 -179.5(4) . . . . ?
C16 C17 C18 O4 3.9(7) . . . . ?
C16 C17 C18 N1 -176.0(4) . . . . ?
C8 C19 C17 C18 0.7(7) . . . . ?
C8 C19 C17 C16 -178.6(4) . . . . ?
C8 C19 C20 C11 0.6(7) . . . . ?
C8 C19 C20 C14 179.0(4) . . . . ?
C8 C9 C10 C11 0.1(8) . . . . ?
C7 N1 C18 O4 170.9(4) . . . . ?
C7 N1 C18 C17 -9.2(7) . . . . ?
C7 N1 C1 C2 131.7(4) . . . . ?
C7 N1 C1 C6 -102.3(5) . . . . ?
C12 N2 C13 O3 -175.9(5) . . . . ?
C12 N2 C13 C14 4.7(7) . . . . ?
C12 C11 C20 C19 -179.5(4) . . . . ?
C12 C11 C20 C14 2.1(6) . . . . ?
C12 C11 C10 C9 179.1(4) . . . . ?
C13 N2 C12 O2 176.2(4) . . . . ?
C13 N2 C12 C11 -3.0(7) . . . . ?
C13 C14 C15 C16 179.1(5) . . . . ?
C15 C14 C13 O3 -0.4(8) . . . . ?
C15 C14 C13 N2 179.0(4) . . . . ?
C10 C11 C20 C19 1.8(7) . . . . ?
C10 C11 C20 C14 -176.6(4) . . . . ?
C10 C11 C12 O2 -1.1(7) . . . . ?
C10 C11 C12 N2 178.1(4) . . . . ?
C10 C9 C8 C19 2.3(7) . . . . ?
C10 C9 C8 C7 -179.0(4) . . . . ?
C1 N1 C18 O4 -4.3(7) . . . . ?
C1 N1 C18 C17 175.6(4) . . . . ?
C1 N1 C7 O1 3.9(6) . . . . ?
C1 N1 C7 C8 -176.8(4) . . . . ?
C1 C2 C3 C4 -59.0(7) . . . . ?
C1 C6 C5 C4 55.4(8) . . . . ?
C2 N2 C12 O2 -0.2(7) 2_665 . . . ?
C2 N2 C12 C11 -179.3(4) 2_665 . . . ?
C2 N2 C13 O3 0.6(7) 2_665 . . . ?
C2 N2 C13 C14 -178.8(4) 2_665 . . . ?
C2 C1 C6 C5 -58.1(6) . . . . ?
C2 C3 C4 C5 56.6(9) . . . . ?
C6 C1 C2 N2 -173.4(4) . . . 3_565 ?
C6 C1 C2 C3 61.0(6) . . . . ?
C6 C5 C4 C3 -55.4(9) . . . . ?
C28 C27 C26 C25 177.5(15) . . . . ?
C28 C29 C34 C33 -179.1(11) . . . . ?
C28 C29 C34 C21 0.4(12) . . . . ?
C32 C31 C30 C29 0.0 . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C31 C30 C29 C28 179.1(12) . . . . ?
C31 C30 C29 C34 0.0 . . . . ?
C30 C29 C34 C33 0.0 . . . . ?
C30 C29 C34 C21 179.5(13) . . . . ?
C29 C34 C33 C32 0.0 . . . . ?
C29 C34 C21 C22 -0.9(19) . . . . ?
C29 C34 C21 Cl1 179.1(11) . . . . ?
C33 C32 C31 C30 0.0 . . . . ?
C33 C34 C21 C22 178.5(10) . . . . ?
C33 C34 C21 Cl1 -1.5(17) . . . . ?
C21 C22 C27 C26 -179.0(11) . . . . ?
C21 C22 C27 C28 3.5(13) . . . . ?
C21 C34 C33 C32 -179.4(14) . . . . ?
C21A C22A C27A C28A -1(3) . . . . ?
C21A C22A C27A C26A 179.9(9) . . . . ?
C21A C34A C33A C32A -178(2) . . . . ?
Cl2A C28A C27A C22A -180(4) . . . . ?
Cl2A C28A C27A C26A -1(6) . . . . ?
Cl2A C28A C29A C30A 1(5) . . . . ?
Cl2A C28A C29A C34A -179(2) . . . . ?
C28A C27A C26A C25A -179(3) . . . . ?
C28A C29A C34A C21A -2(3) . . . . ?
C28A C29A C34A C33A 180(3) . . . . ?
C23A C22A C27A C28A 179(3) . . . . ?
C23A C22A C27A C26A 0.0 . . . . ?
C22A C21A C34A C29A 2(2) . . . . ?
C22A C21A C34A C33A -179.7(11) . . . . ?
C22A C23A C24A C25A 0.0 . . . . ?
C22A C27A C26A C25A 0.0 . . . . ?
C27A C28A C29A C30A -180(3) . . . . ?
C27A C28A C29A C34A 0(6) . . . . ?
C27A C26A C25A C24A 0.0 . . . . ?
C26A C25A C24A C23A 0.0 . . . . ?
C24A C23A C22A C21A -179.9(9) . . . . ?
C24A C23A C22A C27A 0.0 . . . . ?
Cl1A C21A C22A C23A 0.5(12) . . . . ?
Cl1A C21A C22A C27A -179.4(11) . . . . ?
Cl1A C21A C34A C29A -179.2(11) . . . . ?
Cl1A C21A C34A C33A -1(2) . . . . ?
C32A C31A C30A C29A 0.0 . . . . ?
C31A C32A C33A C34A 0.0 . . . . ?
C31A C30A C29A C28A -180(4) . . . . ?
C31A C30A C29A C34A 0.0 . . . . ?
C30A C29A C34A C21A 178(2) . . . . ?
C30A C29A C34A C33A 0.0 . . . . ?
C29A C28A C27A C22A 1(6) . . . . ?
C29A C28A C27A C26A -180(4) . . . . ?
C29A C34A C33A C32A 0.0 . . . . ?
C34A C21A C22A C23A 179.5(18) . . . . ?
C34A C21A C22A C27A -0.4(18) . . . . ?
C33A C32A C31A C30A 0.0 . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 1601 electrons were 
found in a volume of 3986Å³ in 1 void per unit cell. 
This is consistent with the presence of 
4[CH2Cl2] per Asymmetric Unit 
which account for 1512 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.639 -0.192 -0.622 3985.5 1601.3 '37.8 CH2Cl2'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.824
####################################################################### 
# 
# 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_bei-r
_database_code_depnum_ccdc_archive 'CCDC 2391866'
loop_
_audit_author_name
_audit_author_address
'Jialin Cui'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2024-10-17 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_audit_creation_date             2024-09-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C60 H42 N6 O12), 3(C20 H12), C6 H14, 7(C H Cl3)'
_chemical_formula_sum            'C193 H141 Cl21 N12 O24'
_chemical_formula_weight         3756.62
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'

_cell_length_a                   24.0509(4)
_cell_length_b                   24.0509(4)
_cell_length_c                   25.9832(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13016.2(5)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    24334
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      74.3910
_cell_measurement_theta_min      2.7000
_shelx_estimated_absorpt_T_max   0.839
_shelx_estimated_absorpt_T_min   0.785
_exptl_absorpt_coefficient_mu    3.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             5796
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            74883
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.839
_diffrn_reflns_theta_min         2.719
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00 -45.00   0.50    0.35    --  -41.52  -9.00  34.00   52
  2  ω    -17.00   8.00   0.50    0.35    --  -41.52   9.00-151.00   50
  3  ω     12.00  63.00   0.50    0.35    --   41.52   9.00-151.00  102
  4  ω    -30.00  -5.00   0.50    0.35    --   41.52  -9.00  34.00   50
  5  ω   -125.00-100.00   0.50    1.38    -- -102.00  -9.00  34.00   50
  6  ω     62.00 147.00   0.50    1.38    --  107.17   9.00-151.00  170
  7  ω    -40.00  35.00   0.50    0.35    --  -41.52  37.00-120.00  150
  8  ω     20.00  75.00   0.50    0.35    --   41.52  57.00-120.00  110
  9  ω     14.00 114.00   0.50    0.35    --   41.52  77.00 -90.00  200
 10  ω     90.00 115.00   0.50    0.35    --   41.52  77.00   0.00   50
 11  ω     18.00  44.00   0.50    0.35    --   41.52  77.00 120.00   52
 12  ω     13.00  82.00   0.50    0.35    --   41.52  77.00   0.00  138
 13  ω     82.00 112.00   0.50    0.35    --   41.52  77.00 -60.00   60
 14  ω     22.00  91.00   0.50    0.35    --   41.52-125.00 -90.00  138
 15  ω     81.00 112.00   0.50    0.35    --   41.52  57.00-120.00   62
 16  ω     19.00  44.00   0.50    0.35    --   41.52  77.00 150.00   50
 17  ω     20.00  74.00   0.50    0.35    --   41.52  77.00 -60.00  108
 18  ω     21.00  59.00   0.50    0.35    --   41.52  37.00-120.00   76
 19  ω    -99.00 -73.00   0.50    1.38    -- -102.00 -77.00 -60.00   52
 20  ω   -175.00-121.00   0.50    1.38    -- -102.00 -77.00 -60.00  108
 21  ω   -175.00 -78.00   0.50    1.38    -- -102.00 -61.00  30.00  194
 22  ω   -101.00 -75.00   0.50    1.38    -- -102.00 -71.00 -81.89   52
 23  ω   -104.00 -78.00   0.50    1.38    -- -102.00 -61.00 -90.00   52
 24  ω    -99.00 -74.00   0.50    1.38    -- -102.00 -74.00 -39.56   50
 25  ω   -104.00 -78.00   0.50    1.38    -- -102.00 -61.00   0.00   52
 26  ω   -172.00-147.00   0.50    1.38    -- -102.00 -74.00 -39.56   50
 27  ω   -108.00 -74.00   0.50    1.38    -- -102.00 -77.00-120.00   68
 28  ω   -102.00 -77.00   0.50    1.38    -- -102.00 -67.00  -4.21   50
 29  ω   -159.00-133.00   0.50    1.38    -- -102.00 -61.00  11.74   52
 30  ω   -175.00-147.00   0.50    1.38    -- -102.00 -71.00 -81.89   56
 31  ω   -103.00 -77.00   0.50    1.38    -- -102.00 -77.00 -90.00   52
 32  ω   -170.00-114.00   0.50    1.38    -- -102.00 -45.00-120.00  112
 33  ω   -106.00 -81.00   0.50    1.38    -- -102.00 -39.00-105.69   50
 34  ω   -174.00-148.00   0.50    1.38    -- -102.00 -77.00 -44.55   52
 35  ω    -98.00 -73.00   0.50    1.38    -- -102.00 -77.00 -44.55   50
 36  ω   -102.00 -77.00   0.50    1.38    -- -102.00 -73.00  37.68   50
 37  ω   -124.00 -77.00   0.50    1.38    -- -102.00 -67.00  11.19   94
 38  ω    -99.00 -74.00   0.50    1.38    -- -102.00 -74.00 -17.39   50
 39  ω   -175.00-142.00   0.50    1.38    -- -102.00 -67.00  -4.21   66
 40  ω   -103.00 -78.00   0.50    1.38    -- -102.00 -61.00   3.47   50
 41  ω   -173.00 -80.00   0.50    1.38    -- -102.00 -45.00 -30.00  186
 42  ω   -160.00-135.00   0.50    1.38    -- -102.00 -74.00 -17.39   50
 43  ω    -99.00 -74.00   0.50    1.38    -- -102.00 -77.00  30.00   50
 44  ω    -99.00 -74.00   0.50    1.38    -- -102.00 -75.00 -45.46   50
 45  ω   -114.00 -82.00   0.50    1.38    -- -102.00 -45.00 -90.00   64
 46  ω   -174.00-117.00   0.50    1.38    -- -102.00 -66.00 -68.20  114
 47  ω   -102.00 -77.00   0.50    1.38    -- -102.00 -66.00 -68.20   50
 48  ω    -70.00 -45.00   0.50    1.38    -- -102.00  77.00 -30.00   50
 49  ω   -173.00 -78.00   0.50    1.38    -- -102.00 -65.00-123.16  190
 50  ω   -103.00 -78.00   0.50    1.38    -- -102.00 -61.00-120.00   50
 51  ω   -104.00 -71.00   0.50    1.38    -- -102.00  77.00 -30.00   66
 52  ω   -155.00 -82.00   0.50    1.38    -- -102.00 -57.00 -47.82  146
 53  ω   -102.00 -77.00   0.50    1.38    -- -102.00 -68.00  -8.20   50
 54  ω   -103.00 -78.00   0.50    1.38    -- -102.00 -65.00 -55.40   50
 55  ω   -103.00 -78.00   0.50    1.38    -- -102.00 -61.00  11.74   50
 56  ω   -102.00 -77.00   0.50    1.38    -- -102.00 -66.00   4.34   50
 57  ω   -102.00 -77.00   0.50    1.38    -- -102.00 -70.00 -31.53   50
 58  ω   -100.00 -75.00   0.50    1.38    -- -102.00 -77.00 -30.00   50
 59  ω   -100.00 -75.00   0.50    1.38    -- -102.00 -72.00 -91.57   50
 60  ω   -108.00 -83.00   0.50    1.38    -- -102.00 -45.00-120.00   50
 61  ω    -99.00 -74.00   0.50    1.38    -- -102.00 -77.00   0.00   50
 62  ω   -105.00 -80.00   0.50    1.38    -- -102.00 -41.00 -84.49   50
 63  ω   -105.00 -80.00   0.50    1.38    -- -102.00 -42.00 -19.82   50
 64  ω   -107.00 -82.00   0.50    1.38    -- -102.00 -43.00  -4.89   50
 65  ω   -104.00 -79.00   0.50    1.38    -- -102.00 -44.00 -48.88   50
 66  ω   -104.00 -79.00   0.50    1.38    -- -102.00 -57.00 -45.50   50
 67  ω   -103.00 -78.00   0.50    1.38    -- -102.00 -61.00 -30.00   50
 68  ω     36.00 112.00   0.50    1.38    --  107.17-125.00  30.00  152
 69  ω     35.00  72.00   0.50    1.38    --  107.17 -61.00-150.00   74
 70  ω     38.00  78.00   0.50    1.38    --  107.17 -94.00 150.00   80
 71  ω     79.00 105.00   0.50    1.38    --  107.17 -94.00-120.00   52
 72  ω     75.00 104.00   0.50    1.38    --  107.17 -94.00-150.00   58
 73  ω     36.00  98.00   0.50    1.38    --  107.17 -94.00 -60.00  124
 74  ω     34.00  71.00   0.50    1.38    --  107.17 -94.00-120.00   74
 75  ω    153.00 178.00   0.50    1.38    --  107.17  77.00 -30.00   50
 76  ω     46.00  72.00   0.50    1.38    --  107.17 -94.00-150.00   52
 77  ω     78.00 104.00   0.50    1.38    --  107.17  77.00 -30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0229571667
_diffrn_orient_matrix_UB_12      0.0543777333
_diffrn_orient_matrix_UB_13      0.0401019333
_diffrn_orient_matrix_UB_21      0.0315486333
_diffrn_orient_matrix_UB_22      0.0501536667
_diffrn_orient_matrix_UB_23      -0.0430928333
_diffrn_orient_matrix_UB_31      -0.0628471333
_diffrn_orient_matrix_UB_32      0.0014523333
_diffrn_orient_matrix_UB_33      -0.0070262667
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                5510
_reflns_number_total             5908
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 
;
 Flack x determined using 2198 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.041(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         5908
_refine_ls_number_restraints     370
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0681
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1092P)²+23.9187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.1907
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4-C38 = Cl6-C38 = Cl5-C38
 1.79 with sigma of 0.01
 C33-C32 = C34-C33 = C35-C34 = C36-C35 = C37-C36
 1.54 with sigma of 0.01
 Cl4-Cl5 = Cl4-Cl6 = Cl5-Cl6
 2.924 with sigma of 0.02
 C34-C32 = C33-C35 = C35-C37 = C36-C34
 2.515 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34 \\sim C32 \\sim C33 \\sim C35 \\sim C36 \\sim C37: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C31 \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim C31A \\sim Cl1A \\sim Cl2A \\sim Cl3A
\\sim C31B \\sim Cl2B \\sim Cl3B \\sim Cl1B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Cl4 \\sim C38 \\sim Cl5 \\sim Cl6 \\sim C38A \\sim Cl4A \\sim Cl6A \\sim Cl5A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(Cl4) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(Cl5) \\sim Ueq, Uanis(Cl6)
\\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(Cl4A) \\sim Ueq, Uanis(Cl6A) \\sim Ueq,
Uanis(Cl5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C31B) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
4. Same fragment restrains
{C31A, Cl1A, Cl2A, Cl3A} sigma for 1-2: 0.02, 1-3: 0.02
{C31B, Cl1B, Cl2B, Cl3B} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C31, Cl1, Cl2, Cl3}
{C38A, Cl4A, Cl5A, Cl6A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C38, Cl4, Cl6, Cl5}
5. Others
 1*[Sof(C31)+Sof(H31)+Sof(Cl1)+Sof(Cl2)+Sof(Cl3)]+1*[Sof(C31A)+Sof(H31A)+
 Sof(Cl1A)+Sof(Cl2A)+Sof(Cl3A)]+1*[Sof(C31B)+Sof(H31B)+Sof(Cl1B)+Sof(Cl2B)+
 Sof(Cl3B)]=1 with esd of 0.0001
 Sof(C31)=Sof(H31)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(2)
 Sof(C31B)=Sof(H31B)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=FVAR(3)
 Sof(C38A)=Sof(H38A)=Sof(Cl4A)=Sof(Cl5A)=Sof(Cl6A)=0.16667*(1-FVAR(5))
 Sof(C38)=Sof(H38)=Sof(Cl4)=Sof(Cl6)=Sof(Cl5)=0.16667*FVAR(5)
 Fixed Sof: C32(0.16667) H32A(0.16667) H32B(0.16667) H32C(0.16667)
 C33(0.16667) H33A(0.16667) H33B(0.16667) C34(0.16667) H34A(0.16667)
 H34B(0.16667) C35(0.16667) H35A(0.16667) H35B(0.16667) C36(0.16667)
 H36A(0.16667) H36B(0.16667) C37(0.16667) H37A(0.16667) H37B(0.16667)
 H37C(0.16667)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C1(H1), C2(H2), C31A(H31A), C31B(H31B), C38(H38), C38A(H38A)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C16(H16), C15(H15), C22(H22), C10(H10), C23(H23), C24(H24), C29(H29),
 C30(H30), C28(H28)
6.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C37(H37A,H37B,H37C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
O3 O 0.57843(15) 0.72596(15) 0.59440(13) 0.0420(8) Uani 1 1 d . . . . .
C31 C 0.5573(11) 0.7694(12) 0.3165(10) 0.089(6) Uani 0.350(4) 1 d D U P A -1
H31 H 0.568231 0.773090 0.353913 0.107 Uiso 0.350(4) 1 calc R U P A -1
Cl1 Cl 0.5708(3) 0.7104(2) 0.28968(16) 0.0792(17) Uani 0.350(4) 1 d D U P A -1
Cl2 Cl 0.6050(5) 0.8441(3) 0.2881(2) 0.099(2) Uani 0.350(4) 1 d D U P A -1
Cl3 Cl 0.4749(6) 0.7444(7) 0.3109(5) 0.117(4) Uani 0.350(4) 1 d D U P A -1
O2 O 0.27015(19) 0.42392(19) 0.43841(14) 0.0518(9) Uani 1 1 d . . . . .
O1 O 0.28868(16) 0.43322(16) 0.61220(13) 0.0430(8) Uani 1 1 d . . . . .
O4 O 0.5598(2) 0.7185(2) 0.41960(14) 0.0595(11) Uani 1 1 d . . . . .
C8 C 0.3701(2) 0.5211(2) 0.56675(17) 0.0367(10) Uani 1 1 d . . . . .
N1 N 0.27498(19) 0.43180(19) 0.52525(15) 0.0389(9) Uani 1 1 d . . . . .
N2 N 0.5688(2) 0.7249(2) 0.50698(16) 0.0428(9) Uani 1 1 d . . . . .
C9 C 0.4058(2) 0.5497(2) 0.61027(18) 0.0385(10) Uani 1 1 d . . . . .
H9 H 0.390797 0.529910 0.642863 0.046 Uiso 1 1 calc R U . . .
C17 C 0.3575(3) 0.5188(3) 0.47287(18) 0.0416(11) Uani 1 1 d . . . . .
C19 C 0.3919(2) 0.5496(2) 0.51789(18) 0.0382(10) Uani 1 1 d . . . . .
C18 C 0.2983(2) 0.4552(2) 0.47624(18) 0.0408(10) Uani 1 1 d . . . . .
C7 C 0.3091(2) 0.4593(2) 0.57130(18) 0.0371(10) Uani 1 1 d . . . . .
C12 C 0.5480(2) 0.6988(2) 0.55635(19) 0.0394(10) Uani 1 1 d . . . . .
C1 C 0.2125(2) 0.3710(2) 0.5323(2) 0.0426(10) Uani 1 1 d . . . . .
H1 H 0.201085 0.368472 0.569543 0.051 Uiso 1 1 calc R U . . .
C16 C 0.3807(3) 0.5474(3) 0.42559(19) 0.0452(11) Uani 1 1 d . . . . .
H16 H 0.357195 0.527349 0.395232 0.054 Uiso 1 1 calc R U . . .
C15 C 0.4383(3) 0.6053(3) 0.42197(18) 0.0473(12) Uani 1 1 d . . . . .
H15 H 0.453577 0.623975 0.389075 0.057 Uiso 1 1 calc R U . . .
C20 C 0.4503(2) 0.6081(2) 0.51457(17) 0.0380(10) Uani 1 1 d . . . . .
C22 C 0.6035(3) 0.5983(3) 0.5567(3) 0.0588(14) Uani 1 1 d . . . . .
H22 H 0.636594 0.634427 0.539245 0.071 Uiso 1 1 calc R U . . .
C21 C 0.5549(3) 0.5516(3) 0.5283(2) 0.0481(12) Uani 1 1 d . . . . .
C3 C 0.0935(3) 0.3108(3) 0.5180(2) 0.0518(13) Uani 1 1 d . . . . .
H3A H 0.057886 0.309493 0.497936 0.062 Uiso 1 1 calc R U . . .
H3B H 0.085365 0.313966 0.554940 0.062 Uiso 1 1 calc R U . . .
C14 C 0.4737(3) 0.6363(3) 0.46546(18) 0.0428(11) Uani 1 1 d . . . . .
C10 C 0.4638(2) 0.6074(2) 0.60692(17) 0.0370(10) Uani 1 1 d . . . . .
H10 H 0.488255 0.626335 0.637142 0.044 Uiso 1 1 calc R U . . .
C11 C 0.4860(2) 0.6374(2) 0.55956(17) 0.0373(10) Uani 1 1 d . . . . .
C26 C 0.5041(3) 0.4980(3) 0.5553(2) 0.0541(12) Uani 1 1 d . . . . .
C23 C 0.6069(4) 0.5953(4) 0.6102(3) 0.0724(19) Uani 1 1 d . . . . .
H23 H 0.642329 0.628345 0.628309 0.087 Uiso 1 1 calc R U . . .
C13 C 0.5361(3) 0.6951(3) 0.46122(18) 0.0471(12) Uani 1 1 d . . . . .
C2 C 0.1573(2) 0.3698(3) 0.5020(2) 0.0463(11) Uani 1 1 d . . . . .
H2 H 0.164334 0.364471 0.464845 0.056 Uiso 1 1 calc R U . . .
C5 C 0.1542(3) 0.2518(2) 0.5351(3) 0.0582(15) Uani 1 1 d . . . . .
H5A H 0.148502 0.251994 0.572849 0.070 Uiso 1 1 calc R U . . .
H5B H 0.156387 0.212841 0.526369 0.070 Uiso 1 1 calc R U . . .
C6 C 0.2168(3) 0.3106(3) 0.5201(2) 0.0523(13) Uani 1 1 d . . . . .
H6A H 0.224916 0.309154 0.482899 0.063 Uiso 1 1 calc R U . . .
H6B H 0.252758 0.311675 0.539525 0.063 Uiso 1 1 calc R U . . .
C24 C 0.5587(4) 0.5444(4) 0.6364(3) 0.075(2) Uani 1 1 d . . . . .
H24 H 0.560685 0.542829 0.672836 0.090 Uiso 1 1 calc R U . . .
C4 C 0.0962(3) 0.2486(3) 0.5083(3) 0.0620(16) Uani 1 1 d . . . . .
H4A H 0.056393 0.211157 0.521389 0.074 Uiso 1 1 calc R U . . .
H4B H 0.098862 0.242712 0.470858 0.074 Uiso 1 1 calc R U . . .
C27 C 0.4512(3) 0.4480(3) 0.5283(3) 0.0617(16) Uani 1 1 d . . . . .
C25 C 0.5069(4) 0.4950(4) 0.6101(2) 0.0683(17) Uani 1 1 d . . . . .
C29 C 0.4068(5) 0.3947(5) 0.6096(4) 0.094(3) Uani 1 1 d . . . . .
H29 H 0.373376 0.359951 0.627968 0.113 Uiso 1 1 calc R U . . .
C30 C 0.4567(6) 0.4422(5) 0.6361(3) 0.090(3) Uani 1 1 d . . . . .
H30 H 0.457797 0.439873 0.672575 0.108 Uiso 1 1 calc R U . . .
C28 C 0.4037(4) 0.3957(4) 0.5568(4) 0.079(2) Uani 1 1 d . . . . .
H28 H 0.369161 0.360933 0.539226 0.094 Uiso 1 1 calc R U . . .
C31A C 0.5684(8) 0.7928(11) 0.3218(8) 0.086(4) Uani 0.453(4) 1 d D U P B -2
H31A H 0.573169 0.798864 0.359976 0.103 Uiso 0.453(4) 1 calc R U P B -2
Cl1A Cl 0.6251(3) 0.7714(3) 0.30133(15) 0.0888(16) Uani 0.453(4) 1 d D U P B -2
Cl2A Cl 0.5855(3) 0.8658(3) 0.29566(16) 0.0920(16) Uani 0.453(4) 1 d D U P B -2
Cl3A Cl 0.4880(4) 0.7358(4) 0.3099(4) 0.107(3) Uani 0.453(4) 1 d D U P B -2
C32 C 0.326(3) 0.658(2) 0.5062(8) 0.057(9) Uani 0.1667 1 d D U P C -1
H32A H 0.281930 0.631566 0.494411 0.085 Uiso 0.1667 1 calc R U P C -1
H32B H 0.345803 0.630789 0.510375 0.085 Uiso 0.1667 1 calc R U P C -1
H32C H 0.350840 0.691456 0.480708 0.085 Uiso 0.1667 1 calc R U P C -1
C33 C 0.327(2) 0.6891(19) 0.5579(8) 0.064(8) Uani 0.1667 1 d D U P C -1
H33A H 0.360399 0.735121 0.556930 0.077 Uiso 0.1667 1 calc R U P C -1
H33B H 0.285101 0.685960 0.563612 0.077 Uiso 0.1667 1 calc R U P C -1
C34 C 0.342(4) 0.656(3) 0.6023(7) 0.057(8) Uani 0.1667 1 d D U P C -1
H34A H 0.311018 0.609454 0.601252 0.068 Uiso 0.1667 1 calc R U P C -1
H34B H 0.385525 0.663188 0.598561 0.068 Uiso 0.1667 1 calc R U P C -1
C35 C 0.336(3) 0.684(2) 0.6539(6) 0.056(8) Uani 0.1667 1 d D U P C -1
H35A H 0.368800 0.729453 0.655939 0.067 Uiso 0.1667 1 calc R U P C -1
H35B H 0.293005 0.680584 0.655763 0.067 Uiso 0.1667 1 calc R U P C -1
C36 C 0.343(3) 0.6479(19) 0.6996(8) 0.070(9) Uani 0.1667 1 d D U P C -1
H36A H 0.384082 0.648090 0.696654 0.084 Uiso 0.1667 1 calc R U P C -1
H36B H 0.307651 0.602655 0.699312 0.084 Uiso 0.1667 1 calc R U P C -1
C37 C 0.342(3) 0.6800(18) 0.7506(9) 0.049(10) Uani 0.1667 1 d D U P C -1
H37A H 0.373315 0.725866 0.749276 0.073 Uiso 0.1667 1 calc R U P C -1
H37B H 0.351831 0.660026 0.779207 0.073 Uiso 0.1667 1 calc R U P C -1
H37C H 0.298699 0.674344 0.755812 0.073 Uiso 0.1667 1 calc R U P C -1
C31B C 0.4288(17) 0.7130(16) 0.2889(16) 0.146(8) Uani 0.197(3) 1 d D U P D -3
H31B H 0.398371 0.696657 0.259204 0.176 Uiso 0.197(3) 1 calc R U P D -3
Cl1B Cl 0.4781(9) 0.6782(7) 0.2833(4) 0.114(4) Uani 0.197(3) 1 d D U P D -3
Cl2B Cl 0.4759(11) 0.7958(7) 0.2806(6) 0.143(5) Uani 0.197(3) 1 d D U P D -3
Cl3B Cl 0.3820(7) 0.6929(6) 0.3440(4) 0.141(5) Uani 0.197(3) 1 d D U P D -3
C38 C -0.0082(14) -0.0052(15) 0.4849(12) 0.117(9) Uani 0.112(4) 1 d D U P E -1
H38 H -0.025694 -0.027614 0.451327 0.141 Uiso 0.112(4) 1 calc R U P E -1
Cl4 Cl 0.0317(16) 0.0798(13) 0.4760(16) 0.136(10) Uani 0.112(4) 1 d D U P E -1
Cl6 Cl 0.0490(13) -0.0250(14) 0.5096(15) 0.114(8) Uani 0.112(4) 1 d D U P E -1
Cl5 Cl -0.0723(13) -0.0233(18) 0.5287(14) 0.128(10) Uani 0.112(4) 1 d D U P E
-1
C38A C -0.020(3) 0.049(3) 0.449(2) 0.123(10) Uani 0.055(4) 1 d D U P E -2
H38A H -0.047712 0.056668 0.474166 0.148 Uiso 0.055(4) 1 calc R U P E -2
Cl4A Cl -0.056(3) -0.035(2) 0.436(3) 0.156(14) Uani 0.055(4) 1 d D U P E -2
Cl5A Cl -0.014(3) 0.090(2) 0.3906(17) 0.109(12) Uani 0.055(4) 1 d D U P E -2
Cl6A Cl 0.055(3) 0.070(3) 0.479(3) 0.112(11) Uani 0.055(4) 1 d D U P E -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
O3 C12 1.209(6) . ?
C31 H31 1.0000 . ?
C31 Cl1 1.75(2) . ?
C31 Cl2 1.74(2) . ?
C31 Cl3 1.77(2) . ?
O2 C18 1.217(6) . ?
O1 C7 1.206(6) . ?
O4 C13 1.221(6) . ?
C8 C9 1.378(7) . ?
C8 C19 1.413(7) . ?
C8 C7 1.483(6) . ?
N1 C18 1.392(6) . ?
N1 C7 1.414(6) . ?
N1 C1 1.495(6) . ?
N2 C12 1.405(6) . ?
N2 C13 1.408(7) . ?
N2 C2 1.497(7) 2_665 ?
C9 H9 0.9500 . ?
C9 C10 1.393(6) . ?
C17 C19 1.410(7) . ?
C17 C18 1.482(7) . ?
C17 C16 1.383(7) . ?
C19 C20 1.408(6) . ?
C12 C11 1.487(7) . ?
C1 H1 1.0000 . ?
C1 C2 1.530(7) . ?
C1 C6 1.540(7) . ?
C16 H16 0.9500 . ?
C16 C15 1.391(8) . ?
C15 H15 0.9500 . ?
C15 C14 1.387(7) . ?
C20 C14 1.422(6) . ?
C20 C11 1.413(7) . ?
C22 H22 0.9500 . ?
C22 C21 1.362(9) . ?
C22 C23 1.396(10) . ?
C21 C21 1.477(11) 4_556 ?
C21 C26 1.440(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.536(8) . ?
C3 C4 1.551(8) . ?
C14 C13 1.464(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.391(6) . ?
C26 C27 1.423(10) . ?
C26 C25 1.429(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.374(12) . ?
C2 H2 1.0000 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.513(8) . ?
C5 C4 1.527(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C24 H24 0.9500 . ?
C24 C25 1.397(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C27 C27 1.479(14) 4_556 ?
C27 C28 1.413(10) . ?
C25 C30 1.411(12) . ?
C29 H29 0.9500 . ?
C29 C30 1.360(15) . ?
C29 C28 1.375(14) . ?
C30 H30 0.9500 . ?
C28 H28 0.9500 . ?
C31A H31A 1.0000 . ?
C31A Cl1A 1.766(19) . ?
C31A Cl2A 1.73(2) . ?
C31A Cl3A 1.751(19) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32 C33 1.533(14) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.531(14) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.531(14) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.526(14) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.543(14) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C31B H31B 1.0000 . ?
C31B Cl1B 1.77(3) . ?
C31B Cl2B 1.74(3) . ?
C31B Cl3B 1.73(3) . ?
C38 H38 1.0000 . ?
C38 Cl4 1.787(15) . ?
C38 Cl6 1.783(15) . ?
C38 Cl5 1.789(14) . ?
C38A H38A 1.0000 . ?
C38A Cl4A 1.79(3) . ?
C38A Cl5A 1.78(3) . ?
C38A Cl6A 1.78(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 C31 H31 108.1 . . ?
Cl1 C31 Cl3 108.9(15) . . ?
Cl2 C31 H31 108.1 . . ?
Cl2 C31 Cl1 112.0(12) . . ?
Cl2 C31 Cl3 111.4(13) . . ?
Cl3 C31 H31 108.1 . . ?
C9 C8 C19 120.5(4) . . ?
C9 C8 C7 119.5(4) . . ?
C19 C8 C7 119.9(4) . . ?
C18 N1 C7 124.3(4) . . ?
C18 N1 C1 120.8(4) . . ?
C7 N1 C1 114.8(4) . . ?
C12 N2 C13 124.1(4) . . ?
C12 N2 C2 118.6(4) . 2_665 ?
C13 N2 C2 117.3(4) . 2_665 ?
C8 C9 H9 119.7 . . ?
C8 C9 C10 120.6(4) . . ?
C10 C9 H9 119.7 . . ?
C19 C17 C18 120.1(4) . . ?
C16 C17 C19 119.3(5) . . ?
C16 C17 C18 120.5(4) . . ?
C17 C19 C8 120.8(5) . . ?
C20 C19 C8 118.8(4) . . ?
C20 C19 C17 120.3(5) . . ?
O2 C18 N1 120.1(5) . . ?
O2 C18 C17 122.7(5) . . ?
N1 C18 C17 117.1(4) . . ?
O1 C7 C8 122.2(4) . . ?
O1 C7 N1 120.8(4) . . ?
N1 C7 C8 117.0(4) . . ?
O3 C12 N2 121.5(4) . . ?
O3 C12 C11 121.7(4) . . ?
N2 C12 C11 116.8(4) . . ?
N1 C1 H1 106.7 . . ?
N1 C1 C2 113.2(4) . . ?
N1 C1 C6 112.8(4) . . ?
C2 C1 H1 106.7 . . ?
C2 C1 C6 110.2(4) . . ?
C6 C1 H1 106.7 . . ?
C17 C16 H16 119.6 . . ?
C17 C16 C15 120.7(5) . . ?
C15 C16 H16 119.6 . . ?
C16 C15 H15 119.4 . . ?
C14 C15 C16 121.3(5) . . ?
C14 C15 H15 119.4 . . ?
C19 C20 C14 119.4(5) . . ?
C19 C20 C11 120.1(4) . . ?
C11 C20 C14 120.5(5) . . ?
C21 C22 H22 118.5 . . ?
C21 C22 C23 123.0(7) . . ?
C23 C22 H22 118.5 . . ?
C22 C21 C21 122.8(4) . 4_556 ?
C22 C21 C26 117.9(6) . . ?
C26 C21 C21 119.3(3) . 4_556 ?
H3A C3 H3B 108.2 . . ?
C2 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
C2 C3 C4 110.1(5) . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C15 C14 C20 119.0(5) . . ?
C15 C14 C13 121.0(4) . . ?
C20 C14 C13 119.9(5) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 H10 119.8 . . ?
C20 C11 C12 120.5(4) . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 C20 119.6(4) . . ?
C27 C26 C21 121.1(5) . . ?
C27 C26 C25 119.5(6) . . ?
C25 C26 C21 119.4(6) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 C22 119.6(7) . . ?
C24 C23 H23 120.2 . . ?
O4 C13 N2 120.0(5) . . ?
O4 C13 C14 122.0(5) . . ?
N2 C13 C14 118.1(4) . . ?
N2 C2 C1 112.5(4) 3_565 . ?
N2 C2 C3 112.6(4) 3_565 . ?
N2 C2 H2 107.3 3_565 . ?
C1 C2 C3 109.5(5) . . ?
C1 C2 H2 107.3 . . ?
C3 C2 H2 107.3 . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
C6 C5 C4 112.7(6) . . ?
C4 C5 H5A 109.0 . . ?
C4 C5 H5B 109.0 . . ?
C1 C6 H6A 109.9 . . ?
C1 C6 H6B 109.9 . . ?
C5 C6 C1 108.9(4) . . ?
C5 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
C23 C24 H24 119.6 . . ?
C23 C24 C25 120.8(7) . . ?
C25 C24 H24 119.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C5 C4 C3 110.8(4) . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C26 C27 C27 119.6(4) . 4_556 ?
C28 C27 C26 118.6(7) . . ?
C28 C27 C27 121.8(5) . 4_556 ?
C24 C25 C26 119.2(7) . . ?
C24 C25 C30 122.0(7) . . ?
C30 C25 C26 118.8(8) . . ?
C30 C29 H29 119.2 . . ?
C30 C29 C28 121.6(8) . . ?
C28 C29 H29 119.2 . . ?
C25 C30 H30 119.6 . . ?
C29 C30 C25 120.7(8) . . ?
C29 C30 H30 119.6 . . ?
C27 C28 H28 119.7 . . ?
C29 C28 C27 120.7(8) . . ?
C29 C28 H28 119.7 . . ?
Cl1A C31A H31A 106.9 . . ?
Cl2A C31A H31A 106.9 . . ?
Cl2A C31A Cl1A 110.6(9) . . ?
Cl2A C31A Cl3A 109.6(11) . . ?
Cl3A C31A H31A 106.9 . . ?
Cl3A C31A Cl1A 115.5(13) . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C34 C33 C32 111.1(18) . . ?
C34 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
C33 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C35 C34 C33 110.2(16) . . ?
C35 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C34 C35 H35A 109.2 . . ?
C34 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
C36 C35 C34 112.2(17) . . ?
C36 C35 H35A 109.2 . . ?
C36 C35 H35B 109.2 . . ?
C35 C36 H36A 109.6 . . ?
C35 C36 H36B 109.6 . . ?
C35 C36 C37 110.5(18) . . ?
H36A C36 H36B 108.1 . . ?
C37 C36 H36A 109.6 . . ?
C37 C36 H36B 109.6 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Cl1B C31B H31B 106.4 . . ?
Cl2B C31B H31B 106.4 . . ?
Cl2B C31B Cl1B 109.0(18) . . ?
Cl3B C31B H31B 106.4 . . ?
Cl3B C31B Cl1B 116(2) . . ?
Cl3B C31B Cl2B 112(2) . . ?
Cl4 C38 H38 110.1 . . ?
Cl4 C38 Cl5 105.3(16) . . ?
Cl6 C38 H38 110.1 . . ?
Cl6 C38 Cl4 107.9(16) . . ?
Cl6 C38 Cl5 113.0(14) . . ?
Cl5 C38 H38 110.1 . . ?
Cl4A C38A H38A 109.4 . . ?
Cl5A C38A H38A 109.4 . . ?
Cl5A C38A Cl4A 108(3) . . ?
Cl5A C38A Cl6A 115(3) . . ?
Cl6A C38A H38A 109.4 . . ?
Cl6A C38A Cl4A 105(3) . . ?

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
O3 C12 C11 C20 177.6(4) . . . . ?
O3 C12 C11 C10 -4.5(7) . . . . ?
C8 C9 C10 C11 0.9(8) . . . . ?
C8 C19 C20 C14 178.1(4) . . . . ?
C8 C19 C20 C11 -0.2(7) . . . . ?
N1 C1 C2 N2 -45.1(5) . . . 3_565 ?
N1 C1 C2 C3 -171.2(4) . . . . ?
N1 C1 C6 C5 172.4(5) . . . . ?
N2 C12 C11 C20 -0.7(7) . . . . ?
N2 C12 C11 C10 177.2(4) . . . . ?
C9 C8 C19 C17 176.3(4) . . . . ?
C9 C8 C19 C20 -0.7(7) . . . . ?
C9 C8 C7 O1 1.3(7) . . . . ?
C9 C8 C7 N1 -179.2(4) . . . . ?
C9 C10 C11 C12 -179.8(4) . . . . ?
C9 C10 C11 C20 -1.8(7) . . . . ?
C17 C19 C20 C14 1.1(8) . . . . ?
C17 C19 C20 C11 -177.3(4) . . . . ?
C17 C16 C15 C14 -0.5(9) . . . . ?
C19 C8 C9 C10 0.4(7) . . . . ?
C19 C8 C7 O1 180.0(4) . . . . ?
C19 C8 C7 N1 -0.5(6) . . . . ?
C19 C17 C18 O2 -173.0(5) . . . . ?
C19 C17 C18 N1 7.2(7) . . . . ?
C19 C17 C16 C15 1.5(8) . . . . ?
C19 C20 C14 C15 -0.1(7) . . . . ?
C19 C20 C14 C13 -176.5(5) . . . . ?
C19 C20 C11 C12 179.5(4) . . . . ?
C19 C20 C11 C10 1.5(7) . . . . ?
C18 N1 C7 O1 -173.1(4) . . . . ?
C18 N1 C7 C8 7.3(6) . . . . ?
C18 N1 C1 C2 -51.2(5) . . . . ?
C18 N1 C1 C6 74.7(6) . . . . ?
C18 C17 C19 C8 -1.0(7) . . . . ?
C18 C17 C19 C20 176.0(4) . . . . ?
C18 C17 C16 C15 -176.3(5) . . . . ?
C7 C8 C9 C10 179.1(5) . . . . ?
C7 C8 C19 C17 -2.4(7) . . . . ?
C7 C8 C19 C20 -179.4(4) . . . . ?
C7 N1 C18 O2 169.6(4) . . . . ?
C7 N1 C18 C17 -10.6(6) . . . . ?
C7 N1 C1 C2 133.4(4) . . . . ?
C7 N1 C1 C6 -100.6(5) . . . . ?
C12 N2 C13 O4 -174.5(5) . . . . ?
C12 N2 C13 C14 5.8(7) . . . . ?
C1 N1 C18 O2 -5.3(7) . . . . ?
C1 N1 C18 C17 174.5(4) . . . . ?
C1 N1 C7 O1 2.1(6) . . . . ?
C1 N1 C7 C8 -177.5(4) . . . . ?
C16 C17 C19 C8 -178.8(4) . . . . ?
C16 C17 C19 C20 -1.8(7) . . . . ?
C16 C17 C18 O2 4.8(8) . . . . ?
C16 C17 C18 N1 -175.0(4) . . . . ?
C16 C15 C14 C20 -0.2(8) . . . . ?
C16 C15 C14 C13 176.2(5) . . . . ?
C15 C14 C13 O4 -1.2(8) . . . . ?
C15 C14 C13 N2 178.5(5) . . . . ?
C20 C14 C13 O4 175.1(5) . . . . ?
C20 C14 C13 N2 -5.1(7) . . . . ?
C22 C21 C26 C27 178.8(5) . . . . ?
C22 C21 C26 C25 -1.0(7) . . . . ?
C22 C23 C24 C25 1.1(10) . . . . ?
C21 C22 C23 C24 -1.8(10) . . . . ?
C21 C21 C26 C27 0.3(8) 4_556 . . . ?
C21 C21 C26 C25 -179.4(5) 4_556 . . . ?
C21 C26 C27 C27 -0.1(8) . . . 4_556 ?
C21 C26 C27 C28 178.3(5) . . . . ?
C21 C26 C25 C24 0.4(8) . . . . ?
C21 C26 C25 C30 179.8(5) . . . . ?
C14 C20 C11 C12 1.1(7) . . . . ?
C14 C20 C11 C10 -176.9(4) . . . . ?
C11 C20 C14 C15 178.3(5) . . . . ?
C11 C20 C14 C13 1.9(7) . . . . ?
C26 C27 C28 C29 3.2(9) . . . . ?
C26 C25 C30 C29 0.6(10) . . . . ?
C23 C22 C21 C21 -179.9(6) . . . 4_556 ?
C23 C22 C21 C26 1.7(8) . . . . ?
C23 C24 C25 C26 -0.4(9) . . . . ?
C23 C24 C25 C30 -179.8(7) . . . . ?
C13 N2 C12 O3 178.8(5) . . . . ?
C13 N2 C12 C11 -2.9(7) . . . . ?
C2 N2 C12 O3 0.3(7) 2_665 . . . ?
C2 N2 C12 C11 178.6(4) 2_665 . . . ?
C2 N2 C13 O4 4.1(8) 2_665 . . . ?
C2 N2 C13 C14 -175.7(4) 2_665 . . . ?
C2 C1 C6 C5 -60.0(6) . . . . ?
C2 C3 C4 C5 54.5(7) . . . . ?
C6 C1 C2 N2 -172.5(4) . . . 3_565 ?
C6 C1 C2 C3 61.5(5) . . . . ?
C6 C5 C4 C3 -54.9(7) . . . . ?
C24 C25 C30 C29 -180.0(7) . . . . ?
C4 C3 C2 N2 176.0(5) . . . 3_565 ?
C4 C3 C2 C1 -58.1(6) . . . . ?
C4 C5 C6 C1 57.0(6) . . . . ?
C27 C26 C25 C24 -179.4(5) . . . . ?
C27 C26 C25 C30 0.0(8) . . . . ?
C27 C27 C28 C29 -178.4(7) 4_556 . . . ?
C25 C26 C27 C27 179.7(6) . . . 4_556 ?
C25 C26 C27 C28 -1.9(7) . . . . ?
C30 C29 C28 C27 -2.7(11) . . . . ?
C28 C29 C30 C25 0.7(11) . . . . ?
C32 C33 C34 C35 -174(6) . . . . ?
C33 C34 C35 C36 174(5) . . . . ?
C34 C35 C36 C37 176(6) . . . . ?

####################################################################### 
# 
# 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_dca-s
_database_code_depnum_ccdc_archive 'CCDC 2391868'
loop_
_audit_author_name
_audit_author_address
'Jialin Cui'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2024-10-15 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_audit_creation_date             2024-09-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.667(C60 H42 N6 O12), C14 H8 Cl2, C H2 Cl2, 3.52[CH2Cl2]'
_chemical_formula_sum            'C55 H38 Cl4 N4 O8'
_chemical_formula_weight         1024.69
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'

_cell_length_a                   24.7120(5)
_cell_length_b                   24.7120(5)
_cell_length_c                   25.1045(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13276.9(6)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    7106
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      73.8040
_cell_measurement_theta_min      2.7000
_shelx_estimated_absorpt_T_max   0.702
_shelx_estimated_absorpt_T_min   0.663
_exptl_absorpt_coefficient_mu    2.241
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15318
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.536
_diffrn_reflns_theta_min         2.713
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     53.00 103.00   0.50    1.63    --  109.82 -94.00 120.00  100
  2  ω     50.00 107.00   0.50    1.63    --  109.82-111.00 -30.00  114
  3  ω     42.00  68.00   0.50    1.63    --  109.82 -61.00-120.00   52
  4  ω     37.00  62.00   0.50    1.63    --  109.82 -61.00-150.00   50
  5  ω    -23.00  46.00   0.50    0.41    --  -36.36  19.00   0.00  138
  6  ω    -29.00   6.00   0.50    0.41    --   36.36 -59.00 -40.00   70
  7  ω     15.00  42.00   0.50    0.41    --   36.36 -59.00 -40.00   54
  8  ω     83.00 108.00   0.50    1.63    --  109.82  43.00-149.00   50
  9  ω    121.00 177.00   0.50    1.63    --  109.82  43.00-149.00  112
 10  ω     87.00 118.00   0.50    0.41    --   36.36 172.00-167.00   62
 11  ω    -47.00 -22.00   0.50    1.63    -- -102.00  45.00-180.00   50
 12  ω    -60.00 -30.00   0.50    1.63    -- -102.00  61.00-150.00   60
 13  ω    -49.00 -23.00   0.50    1.63    -- -102.00  45.00-150.00   52
 14  ω    -49.00 -23.00   0.50    1.63    -- -102.00  45.00-120.00   52
 15  ω    -49.00 -24.00   0.50    1.63    -- -102.00  45.00 -90.00   50
 16  ω    -64.00 -35.00   0.50    1.63    -- -102.00  61.00   0.00   58
 17  ω    -53.00 -27.00   0.50    1.63    -- -102.00  61.00 150.00   52
 18  ω    -49.00 -24.00   0.50    1.63    -- -102.00  45.00 120.00   50
 19  ω    -91.00 -53.00   0.50    0.41    --  -36.36-156.00 -20.00   76
 20  ω   -119.00 -55.00   0.50    1.63    -- -102.00-172.00 179.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0713572000
_diffrn_orient_matrix_UB_12      0.0438525000
_diffrn_orient_matrix_UB_13      -0.0011090000
_diffrn_orient_matrix_UB_21      -0.0028574000
_diffrn_orient_matrix_UB_22      0.0250647000
_diffrn_orient_matrix_UB_23      0.0555275000
_diffrn_orient_matrix_UB_31      0.0091080000
_diffrn_orient_matrix_UB_32      -0.0512890000
_diffrn_orient_matrix_UB_33      0.0260832000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                5108
_reflns_number_total             5536
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 
;
 Flack x determined using 1982 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.112(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         5536
_refine_ls_number_restraints     694
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0749
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1449P)²+28.1671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2266
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C27-C28 = C29-C28 = C21-C34 = C22-C21 = C29A-C28A = C27A-C28A = C21A-C22A =
 C34A-C21A
 1.39 with sigma of 0.01
 Cl4-C35 = Cl3-C35 = Cl3A-C35A = Cl4A-C35A
 1.79 with sigma of 0.01
 Cl1-C21 = Cl2-C28
 1.74 with sigma of 0.01
 Cl2A-C28A = Cl1A-C21A
 1.74 with sigma of 0.01
 Cl3-Cl4 = Cl4A-Cl3A
 2.924 with sigma of 0.02
 Cl2-C29 \\sim Cl2-C27
 with sigma of 0.02
 Cl2A-C27A \\sim Cl2A-C29A
 with sigma of 0.02
 Cl1-C34 \\sim Cl1-C22
 with sigma of 0.02
 C27-C34 \\sim C29-C22
 with sigma of 0.02
 C29-C27 \\sim C22-C34
 with sigma of 0.02
 Cl1A-C22A \\sim Cl1A-C34A
 with sigma of 0.02
 C29A-C22A \\sim C27A-C34A
 with sigma of 0.02
 C27A-C29A \\sim C34A-C22A
 with sigma of 0.02
3. Restrained planarity
 C27, C33, C34, C32, C29, C21, C31, C28, C30, Cl1, C22, Cl2, C23, C26, C24, C25
 with sigma of 0.1
 C30A, C29A, C28A, C34A, C27A, Cl2A, C21A, C33A, C31A, C22A, C26A, Cl1A, C32A,
 C23A, C25A, C24A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Cl3A \\sim C35A \\sim Cl4A \\sim Cl3 \\sim C35 \\sim Cl4: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C33 \\sim C32 \\sim C31 \\sim C30 \\sim C29 \\sim C34 \\sim Cl2 \\sim C28 \\sim
C27 \\sim C26 \\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim Cl1 \\sim
C29A \\sim C23A \\sim C24A \\sim C22A \\sim C25A \\sim C27A \\sim C21A \\sim
Cl1A \\sim C26A \\sim C28A \\sim C34A \\sim Cl2A \\sim C33A \\sim C30A \\sim
C32A \\sim C31A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
5. Others
 Sof(C29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=
 Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(C22A)=Sof(C21A)=
 Sof(Cl1A)=Sof(C28A)=Sof(Cl2A)=0.5*(1-FVAR(2))
 Sof(C33)=Sof(H33)=Sof(C32)=Sof(H32)=Sof(C31)=Sof(H31)=Sof(C30)=Sof(H30)=
 Sof(C29)=Sof(C34)=Sof(Cl2)=Sof(C28)=Sof(C27)=Sof(C26)=Sof(H26)=Sof(C25)=
 Sof(H25)=Sof(C24)=Sof(H24)=Sof(C23)=Sof(H23)=Sof(C22)=Sof(C21)=Sof(Cl1)=0.5*
 FVAR(2)
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(Cl3A)=Sof(Cl4A)=0.5*(1-FVAR(3))
 Sof(Cl3)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(Cl4)=0.5*FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B), C5(H5A,H5B), C4(H4A,H4B), C35(H35A,H35B), C35A(H35C,
 H35D)
6.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C32(H32), C31(H31), C30(H30), C16(H16), C9(H9), C15(H15), C10(H10),
 C26(H26), C25(H25), C24(H24), C23(H23), C30A(H30A), C31A(H31A), C32A(H32A),
 C33A(H33A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A)
6.d Fitted hexagon refined as free rotating group:
 C33(C32,C31,C30,C29,C34), C27(C26,C25,C24,C23,C22), C29A(C30A,C31A,C32A,C33A,
 C34A), C23A(C24A,C25A,C26A,C27A,C22A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.61938(19) 0.5156(2) 0.77598(16) 0.0455(10) Uani 1 1 d . . . . .
C33 C 0.9194(5) 0.6661(8) 0.7294(4) 0.044(4) Uani 0.372(2) 1 d G U P A -1
H33 H 0.953434 0.665298 0.712657 0.053 Uiso 0.372(2) 1 calc R U P A -1
C32 C 0.9167(5) 0.6679(6) 0.7847(4) 0.045(3) Uani 0.372(2) 1 d G U P A -1
H32 H 0.948931 0.668309 0.805644 0.054 Uiso 0.372(2) 1 calc R U P A -1
C31 C 0.8669(6) 0.6690(6) 0.8093(3) 0.044(3) Uani 0.372(2) 1 d G U P A -1
H31 H 0.865041 0.670214 0.847004 0.053 Uiso 0.372(2) 1 calc R U P A -1
C30 C 0.8197(5) 0.6683(8) 0.7786(4) 0.042(3) Uani 0.372(2) 1 d G U P A -1
H30 H 0.785654 0.669106 0.795378 0.050 Uiso 0.372(2) 1 calc R U P A -1
C29 C 0.8224(5) 0.6665(6) 0.7234(4) 0.035(3) Uani 0.372(2) 1 d DG U P A -1
C34 C 0.8722(6) 0.6654(7) 0.6988(3) 0.035(3) Uani 0.372(2) 1 d DG U P A -1
O4 O 0.90245(17) 0.51475(19) 0.75776(17) 0.0402(9) Uani 1 1 d . . . . .
O1 O 0.60337(18) 0.50904(19) 0.59666(15) 0.0418(9) Uani 1 1 d . . . . .
Cl2 Cl 0.7128(2) 0.6684(2) 0.7208(2) 0.0531(13) Uani 0.372(2) 1 d D U P A -1
O3 O 0.8862(2) 0.5079(2) 0.57708(17) 0.0471(10) Uani 1 1 d . . . . .
N1 N 0.6066(2) 0.5046(2) 0.68605(16) 0.0327(9) Uani 1 1 d . . . . .
N2 N 0.89384(19) 0.5074(2) 0.66730(18) 0.0315(9) Uani 1 1 d . . . . .
C19 C 0.7233(2) 0.5090(2) 0.67880(19) 0.0278(9) Uani 1 1 d . . . . .
C8 C 0.6903(2) 0.5066(2) 0.63098(19) 0.0317(10) Uani 1 1 d . . . . .
C16 C 0.7340(2) 0.5169(2) 0.77353(19) 0.0328(10) Uani 1 1 d . . . . .
H16 H 0.718628 0.519895 0.807438 0.039 Uiso 1 1 calc R U . . .
C14 C 0.8132(2) 0.5122(2) 0.72138(18) 0.0294(10) Uani 1 1 d . . . . .
C9 C 0.7140(3) 0.5053(2) 0.5820(2) 0.0359(11) Uani 1 1 d . . . . .
H9 H 0.692337 0.504498 0.550503 0.043 Uiso 1 1 calc R U . . .
C13 C 0.8732(2) 0.5116(2) 0.7173(2) 0.0325(10) Uani 1 1 d . . . . .
C17 C 0.7002(2) 0.5121(2) 0.72930(19) 0.0276(9) Uani 1 1 d . . . . .
C12 C 0.8640(2) 0.5079(2) 0.61920(19) 0.0329(10) Uani 1 1 d . . . . .
C11 C 0.8038(2) 0.5066(2) 0.6242(2) 0.0339(11) Uani 1 1 d . . . . .
C7 C 0.6309(3) 0.5071(2) 0.6351(2) 0.0341(11) Uani 1 1 d . . . . .
C20 C 0.7803(2) 0.5088(2) 0.67427(19) 0.0291(10) Uani 1 1 d . . . . .
C18 C 0.6398(2) 0.5111(2) 0.73428(19) 0.0301(10) Uani 1 1 d . . . . .
C15 C 0.7906(2) 0.5175(3) 0.7705(2) 0.0358(11) Uani 1 1 d . . . . .
H15 H 0.813634 0.521517 0.802011 0.043 Uiso 1 1 calc R U . . .
C10 C 0.7718(3) 0.5052(3) 0.5789(2) 0.0412(12) Uani 1 1 d . . . . .
H10 H 0.788243 0.504057 0.544947 0.049 Uiso 1 1 calc R U . . .
C1 C 0.5448(2) 0.5003(3) 0.6924(2) 0.0364(12) Uani 1 1 d . . . . .
H1 H 0.533756 0.491774 0.730982 0.044 Uiso 1 1 calc R U . . .
C2 C 0.4919(2) 0.4471(3) 0.6618(2) 0.0376(12) Uani 1 1 d . . . . .
H2 H 0.499016 0.458849 0.623223 0.045 Uiso 1 1 calc R U . . .
C6 C 0.5466(3) 0.5619(3) 0.6797(3) 0.0480(14) Uani 1 1 d . . . . .
H6A H 0.580165 0.596129 0.700660 0.058 Uiso 1 1 calc R U . . .
H6B H 0.556168 0.571831 0.641418 0.058 Uiso 1 1 calc R U . . .
C3 C 0.4292(3) 0.4409(3) 0.6765(3) 0.0521(16) Uani 1 1 d . . . . .
H3A H 0.421181 0.431885 0.715006 0.062 Uiso 1 1 calc R U . . .
H3B H 0.395273 0.405893 0.656397 0.062 Uiso 1 1 calc R U . . .
C5 C 0.4847(3) 0.5573(3) 0.6926(3) 0.0569(17) Uani 1 1 d . . . . .
H5A H 0.486111 0.596647 0.682247 0.068 Uiso 1 1 calc R U . . .
H5B H 0.477193 0.551618 0.731448 0.068 Uiso 1 1 calc R U . . .
C4 C 0.4308(4) 0.5021(3) 0.6629(4) 0.070(2) Uani 1 1 d . . . . .
H4A H 0.390591 0.498923 0.673200 0.084 Uiso 1 1 calc R U . . .
H4B H 0.436280 0.509551 0.624059 0.084 Uiso 1 1 calc R U . . .
C28 C 0.7755(8) 0.6662(11) 0.6907(5) 0.034(3) Uani 0.372(2) 1 d D U P A -1
C27 C 0.7769(7) 0.6636(9) 0.6343(4) 0.035(3) Uani 0.372(2) 1 d DG U P A -1
C26 C 0.7299(5) 0.6621(7) 0.6028(5) 0.045(4) Uani 0.372(2) 1 d G U P A -1
H26 H 0.696123 0.664015 0.618948 0.054 Uiso 0.372(2) 1 calc R U P A -1
C25 C 0.7323(5) 0.6578(6) 0.5477(4) 0.051(3) Uani 0.372(2) 1 d G U P A -1
H25 H 0.700139 0.656752 0.526250 0.062 Uiso 0.372(2) 1 calc R U P A -1
C24 C 0.7817(6) 0.6550(6) 0.5241(4) 0.051(4) Uani 0.372(2) 1 d G U P A -1
H24 H 0.783336 0.652050 0.486493 0.061 Uiso 0.372(2) 1 calc R U P A -1
C23 C 0.8287(6) 0.6565(7) 0.5556(5) 0.045(3) Uani 0.372(2) 1 d G U P A -1
H23 H 0.862518 0.654609 0.539436 0.054 Uiso 0.372(2) 1 calc R U P A -1
C22 C 0.8264(6) 0.6608(9) 0.6106(4) 0.039(3) Uani 0.372(2) 1 d DG U P A -1
C21 C 0.8746(7) 0.6644(9) 0.6427(5) 0.031(3) Uani 0.372(2) 1 d D U P A -1
Cl1 Cl 0.9370(3) 0.6615(2) 0.6125(2) 0.0496(11) Uani 0.372(2) 1 d D U P A -1
C29A C 0.7869(10) 0.6660(14) 0.7132(9) 0.037(4) Uani 0.128(2) 1 d DG U P A -2
C30A C 0.7551(11) 0.6665(17) 0.7587(11) 0.041(5) Uani 0.128(2) 1 d G U P A -2
H30A H 0.716284 0.665547 0.755476 0.049 Uiso 0.128(2) 1 calc R U P A -2
C31A C 0.7800(13) 0.6685(16) 0.8088(9) 0.049(7) Uani 0.128(2) 1 d G U P A -2
H31A H 0.758198 0.668927 0.839809 0.059 Uiso 0.128(2) 1 calc R U P A -2
C32A C 0.8367(14) 0.6700(17) 0.8134(8) 0.048(6) Uani 0.128(2) 1 d G U P A -2
H32A H 0.853746 0.671360 0.847651 0.057 Uiso 0.128(2) 1 calc R U P A -2
C33A C 0.8686(12) 0.6694(18) 0.7680(10) 0.042(4) Uani 0.128(2) 1 d G U P A -2
H33A H 0.907380 0.670414 0.771161 0.051 Uiso 0.128(2) 1 calc R U P A -2
C34A C 0.8437(10) 0.6674(14) 0.7179(9) 0.038(4) Uani 0.128(2) 1 d DG U P A -2
C23A C 0.8796(12) 0.6638(19) 0.5729(10) 0.042(5) Uani 0.128(2) 1 d G U P A -2
H23A H 0.918696 0.665320 0.575143 0.051 Uiso 0.128(2) 1 calc R U P A -2
C24A C 0.8540(14) 0.6630(18) 0.5233(9) 0.048(6) Uani 0.128(2) 1 d G U P A -2
H24A H 0.875668 0.663912 0.491770 0.058 Uiso 0.128(2) 1 calc R U P A -2
C25A C 0.7968(15) 0.6608(18) 0.5200(9) 0.046(5) Uani 0.128(2) 1 d G U P A -2
H25A H 0.779354 0.660215 0.486177 0.055 Uiso 0.128(2) 1 calc R U P A -2
C26A C 0.7652(12) 0.6594(17) 0.5662(10) 0.043(4) Uani 0.128(2) 1 d G U P A -2
H26A H 0.726067 0.657925 0.563958 0.052 Uiso 0.128(2) 1 calc R U P A -2
C27A C 0.7907(11) 0.6603(17) 0.6158(9) 0.040(4) Uani 0.128(2) 1 d DG U P A -2
C22A C 0.8479(12) 0.6625(17) 0.6191(8) 0.038(4) Uani 0.128(2) 1 d DG U P A -2
C21A C 0.8716(19) 0.666(4) 0.6702(9) 0.037(4) Uani 0.128(2) 1 d D U P A -2
Cl1A Cl 0.9441(11) 0.6697(18) 0.6740(8) 0.050(4) Uani 0.128(2) 1 d D U P A -2
C28A C 0.7618(10) 0.6636(16) 0.6626(9) 0.036(4) Uani 0.128(2) 1 d D U P A -2
Cl2A Cl 0.6901(9) 0.6620(15) 0.6592(9) 0.045(4) Uani 0.128(2) 1 d D U P A -2
Cl3 Cl 1.0672(10) 0.6677(16) 0.5336(9) 0.102(7) Uani 0.224(7) 1 d D U P B -1
C35 C 0.996(3) 0.6149(12) 0.500(4) 0.075(7) Uani 0.224(7) 1 d D U P B -1
H35A H 1.004622 0.590930 0.472655 0.090 Uiso 0.224(7) 1 calc R U P B -1
H35B H 0.965479 0.584934 0.525576 0.090 Uiso 0.224(7) 1 calc R U P B -1
Cl4 Cl 0.9664(4) 0.6596(5) 0.4690(3) 0.071(3) Uani 0.224(7) 1 d D U P B -1
C35A C 0.9856(12) 0.5660(10) 0.4960(10) 0.086(8) Uani 0.276(7) 1 d D U P B -2
H35C H 1.010784 0.554560 0.472857 0.104 Uiso 0.276(7) 1 calc R U P B -2
H35D H 0.953558 0.527531 0.513978 0.104 Uiso 0.276(7) 1 calc R U P B -2
Cl3A Cl 1.0352(5) 0.6212(7) 0.5450(4) 0.077(4) Uani 0.276(7) 1 d D U P B -2
Cl4A Cl 0.9484(6) 0.5972(8) 0.4566(6) 0.070(5) Uani 0.276(7) 1 d D U P B -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C18 1.190(6) . ?
C33 H33 0.9500 . ?
C33 C32 1.3900 . ?
C33 C34 1.3900 . ?
C32 H32 0.9500 . ?
C32 C31 1.3900 . ?
C31 H31 0.9500 . ?
C31 C30 1.3900 . ?
C30 H30 0.9500 . ?
C30 C29 1.3900 . ?
C29 C34 1.3900 . ?
C29 C28 1.415(11) . ?
C34 C21 1.411(10) . ?
O4 C13 1.225(7) . ?
O1 C7 1.196(7) . ?
Cl2 C28 1.750(11) . ?
O3 C12 1.191(6) . ?
N1 C7 1.401(7) . ?
N1 C18 1.425(6) . ?
N1 C1 1.486(7) . ?
N2 C13 1.378(7) . ?
N2 C12 1.418(6) . ?
N2 C2 1.515(6) 3_665 ?
C19 C8 1.436(7) . ?
C19 C17 1.408(7) . ?
C19 C20 1.416(7) . ?
C8 C9 1.368(7) . ?
C8 C7 1.477(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.359(7) . ?
C16 C15 1.393(7) . ?
C14 C13 1.495(7) . ?
C14 C20 1.413(7) . ?
C14 C15 1.387(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.432(8) . ?
C17 C18 1.486(7) . ?
C12 C11 1.478(7) . ?
C11 C20 1.398(7) . ?
C11 C10 1.376(8) . ?
C15 H15 0.9500 . ?
C10 H10 0.9500 . ?
C1 H1 1.0000 . ?
C1 C2 1.520(8) . ?
C1 C6 1.533(7) . ?
C2 H2 1.0000 . ?
C2 C3 1.522(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.512(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.534(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C4 1.540(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C28 C27 1.419(10) . ?
C27 C26 1.3900 . ?
C27 C22 1.3900 . ?
C26 H26 0.9500 . ?
C26 C25 1.3900 . ?
C25 H25 0.9500 . ?
C25 C24 1.3900 . ?
C24 H24 0.9500 . ?
C24 C23 1.3900 . ?
C23 H23 0.9500 . ?
C23 C22 1.3900 . ?
C22 C21 1.404(11) . ?
C21 Cl1 1.752(11) . ?
C29A C30A 1.3900 . ?
C29A C34A 1.3900 . ?
C29A C28A 1.403(13) . ?
C30A H30A 0.9500 . ?
C30A C31A 1.3900 . ?
C31A H31A 0.9500 . ?
C31A C32A 1.3900 . ?
C32A H32A 0.9500 . ?
C32A C33A 1.3900 . ?
C33A H33A 0.9500 . ?
C33A C34A 1.3900 . ?
C34A C21A 1.395(13) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.3900 . ?
C23A C22A 1.3900 . ?
C24A H24A 0.9500 . ?
C24A C25A 1.3900 . ?
C25A H25A 0.9500 . ?
C25A C26A 1.3900 . ?
C26A H26A 0.9500 . ?
C26A C27A 1.3900 . ?
C27A C22A 1.3900 . ?
C27A C28A 1.400(13) . ?
C22A C21A 1.397(13) . ?
C21A Cl1A 1.742(13) . ?
C28A Cl2A 1.756(13) . ?
Cl3 C35 1.789(14) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 Cl4 1.785(14) . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?
C35A Cl3A 1.790(14) . ?
C35A Cl4A 1.769(14) . ?

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
C32 C33 H33 120.0 . . ?
C32 C33 C34 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C32 H32 120.0 . . ?
C31 C32 C33 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C31 H31 120.0 . . ?
C32 C31 C30 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 C31 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C29 C34 120.0 . . ?
C30 C29 C28 121.8(8) . . ?
C34 C29 C28 118.2(8) . . ?
C33 C34 C21 120.7(9) . . ?
C29 C34 C33 120.0 . . ?
C29 C34 C21 119.3(9) . . ?
C7 N1 C18 124.1(4) . . ?
C7 N1 C1 120.2(4) . . ?
C18 N1 C1 115.4(4) . . ?
C13 N2 C12 124.2(4) . . ?
C13 N2 C2 119.2(4) . 3_665 ?
C12 N2 C2 116.3(4) . 3_665 ?
C17 C19 C8 121.2(5) . . ?
C17 C19 C20 120.2(4) . . ?
C20 C19 C8 118.6(5) . . ?
C19 C8 C7 119.1(4) . . ?
C9 C8 C19 120.7(5) . . ?
C9 C8 C7 120.1(5) . . ?
C17 C16 H16 119.1 . . ?
C17 C16 C15 121.8(5) . . ?
C15 C16 H16 119.1 . . ?
C20 C14 C13 119.1(4) . . ?
C15 C14 C13 120.7(4) . . ?
C15 C14 C20 120.2(5) . . ?
C8 C9 H9 120.4 . . ?
C8 C9 C10 119.3(5) . . ?
C10 C9 H9 120.4 . . ?
O4 C13 N2 122.1(5) . . ?
O4 C13 C14 119.9(5) . . ?
N2 C13 C14 117.9(4) . . ?
C19 C17 C18 120.4(4) . . ?
C16 C17 C19 119.5(5) . . ?
C16 C17 C18 120.1(4) . . ?
O3 C12 N2 121.0(5) . . ?
O3 C12 C11 122.2(5) . . ?
N2 C12 C11 116.7(4) . . ?
C20 C11 C12 120.5(5) . . ?
C10 C11 C12 119.4(5) . . ?
C10 C11 C20 120.0(5) . . ?
O1 C7 N1 119.9(5) . . ?
O1 C7 C8 122.1(5) . . ?
N1 C7 C8 118.0(4) . . ?
C14 C20 C19 118.4(5) . . ?
C11 C20 C19 120.4(5) . . ?
C11 C20 C14 121.2(5) . . ?
O2 C18 N1 120.8(5) . . ?
O2 C18 C17 122.7(5) . . ?
N1 C18 C17 116.5(4) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 C16 119.8(5) . . ?
C14 C15 H15 120.1 . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.0(5) . . ?
C11 C10 H10 119.5 . . ?
N1 C1 H1 106.3 . . ?
N1 C1 C2 114.6(5) . . ?
N1 C1 C6 112.9(4) . . ?
C2 C1 H1 106.3 . . ?
C2 C1 C6 109.8(4) . . ?
C6 C1 H1 106.3 . . ?
N2 C2 C1 112.3(4) 2_655 . ?
N2 C2 H2 106.7 2_655 . ?
N2 C2 C3 113.0(4) 2_655 . ?
C1 C2 H2 106.7 . . ?
C1 C2 C3 110.9(5) . . ?
C3 C2 H2 106.7 . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C5 C6 C1 110.8(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C2 C3 H3A 109.9 . . ?
C2 C3 H3B 109.9 . . ?
C2 C3 C4 108.9(6) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
C6 C5 C4 111.0(6) . . ?
H5A C5 H5B 108.0 . . ?
C4 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
C3 C4 C5 110.5(6) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C29 C28 Cl2 119.0(8) . . ?
C29 C28 C27 122.7(11) . . ?
C27 C28 Cl2 118.3(10) . . ?
C26 C27 C28 122.0(9) . . ?
C26 C27 C22 120.0 . . ?
C22 C27 C28 118.0(9) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 C27 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C25 H25 120.0 . . ?
C26 C25 C24 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C24 H24 120.0 . . ?
C23 C24 C25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C27 C22 C21 119.5(8) . . ?
C23 C22 C27 120.0 . . ?
C23 C22 C21 120.5(8) . . ?
C34 C21 Cl1 118.6(9) . . ?
C22 C21 C34 122.1(12) . . ?
C22 C21 Cl1 119.2(8) . . ?
C30A C29A C34A 120.0 . . ?
C30A C29A C28A 120.2(13) . . ?
C34A C29A C28A 119.8(13) . . ?
C29A C30A H30A 120.0 . . ?
C31A C30A C29A 120.0 . . ?
C31A C30A H30A 120.0 . . ?
C30A C31A H31A 120.0 . . ?
C30A C31A C32A 120.0 . . ?
C32A C31A H31A 120.0 . . ?
C31A C32A H32A 120.0 . . ?
C33A C32A C31A 120.0 . . ?
C33A C32A H32A 120.0 . . ?
C32A C33A H33A 120.0 . . ?
C32A C33A C34A 120.0 . . ?
C34A C33A H33A 120.0 . . ?
C29A C34A C21A 115.9(13) . . ?
C33A C34A C29A 120.0 . . ?
C33A C34A C21A 124.1(13) . . ?
C24A C23A H23A 120.0 . . ?
C24A C23A C22A 120.0 . . ?
C22A C23A H23A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C25A C24A C23A 120.0 . . ?
C25A C24A H24A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C26A C25A C24A 120.0 . . ?
C26A C25A H25A 120.0 . . ?
C25A C26A H26A 120.0 . . ?
C25A C26A C27A 120.0 . . ?
C27A C26A H26A 120.0 . . ?
C26A C27A C28A 120.7(12) . . ?
C22A C27A C26A 120.0 . . ?
C22A C27A C28A 119.1(12) . . ?
C23A C22A C21A 123.3(13) . . ?
C27A C22A C23A 120.0 . . ?
C27A C22A C21A 116.6(12) . . ?
C34A C21A C22A 126.1(16) . . ?
C34A C21A Cl1A 117.5(13) . . ?
C22A C21A Cl1A 116.3(13) . . ?
C29A C28A Cl2A 117.7(13) . . ?
C27A C28A C29A 122.4(16) . . ?
C27A C28A Cl2A 119.9(13) . . ?
Cl3 C35 H35A 110.1 . . ?
Cl3 C35 H35B 110.1 . . ?
H35A C35 H35B 108.4 . . ?
Cl4 C35 Cl3 108.1(14) . . ?
Cl4 C35 H35A 110.1 . . ?
Cl4 C35 H35B 110.1 . . ?
H35C C35A H35D 108.0 . . ?
Cl3A C35A H35C 109.4 . . ?
Cl3A C35A H35D 109.4 . . ?
Cl4A C35A H35C 109.4 . . ?
Cl4A C35A H35D 109.4 . . ?
Cl4A C35A Cl3A 111.0(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
C33 C32 C31 C30 0.0 . . . . ?
C33 C34 C21 C22 177.1(10) . . . . ?
C33 C34 C21 Cl1 1.9(13) . . . . ?
C32 C33 C34 C29 0.0 . . . . ?
C32 C33 C34 C21 179.2(9) . . . . ?
C32 C31 C30 C29 0.0 . . . . ?
C31 C30 C29 C34 0.0 . . . . ?
C31 C30 C29 C28 -179.6(10) . . . . ?
C30 C29 C34 C33 0.0 . . . . ?
C30 C29 C34 C21 -179.2(9) . . . . ?
C30 C29 C28 Cl2 0.3(16) . . . . ?
C30 C29 C28 C27 -179.2(9) . . . . ?
C29 C34 C21 C22 -3.7(15) . . . . ?
C29 C34 C21 Cl1 -178.9(11) . . . . ?
C29 C28 C27 C26 178.8(12) . . . . ?
C29 C28 C27 C22 0.6(16) . . . . ?
C34 C33 C32 C31 0.0 . . . . ?
C34 C29 C28 Cl2 -179.3(11) . . . . ?
C34 C29 C28 C27 1.1(17) . . . . ?
Cl2 C28 C27 C26 -0.8(14) . . . . ?
Cl2 C28 C27 C22 -179.0(11) . . . . ?
O3 C12 C11 C20 -177.9(5) . . . . ?
O3 C12 C11 C10 0.2(8) . . . . ?
N1 C1 C2 N2 44.7(6) . . . 2_655 ?
N1 C1 C2 C3 172.2(5) . . . . ?
N1 C1 C6 C5 -173.7(5) . . . . ?
N2 C12 C11 C20 3.8(7) . . . . ?
N2 C12 C11 C10 -178.1(5) . . . . ?
N2 C2 C3 C4 -173.0(6) 2_655 . . . ?
C19 C8 C9 C10 1.2(8) . . . . ?
C19 C8 C7 O1 175.3(5) . . . . ?
C19 C8 C7 N1 -5.3(7) . . . . ?
C19 C17 C18 O2 -177.7(5) . . . . ?
C19 C17 C18 N1 2.3(7) . . . . ?
C8 C19 C17 C16 -177.4(4) . . . . ?
C8 C19 C17 C18 1.7(7) . . . . ?
C8 C19 C20 C14 179.0(4) . . . . ?
C8 C19 C20 C11 0.4(7) . . . . ?
C8 C9 C10 C11 -0.3(9) . . . . ?
C16 C17 C18 O2 1.4(8) . . . . ?
C16 C17 C18 N1 -178.6(4) . . . . ?
C9 C8 C7 O1 -3.2(8) . . . . ?
C9 C8 C7 N1 176.2(5) . . . . ?
C13 N2 C12 O3 175.5(5) . . . . ?
C13 N2 C12 C11 -6.2(7) . . . . ?
C13 C14 C20 C19 179.6(4) . . . . ?
C13 C14 C20 C11 -1.8(7) . . . . ?
C13 C14 C15 C16 -178.9(5) . . . . ?
C17 C19 C8 C9 178.2(5) . . . . ?
C17 C19 C8 C7 -0.3(7) . . . . ?
C17 C19 C20 C14 -0.4(7) . . . . ?
C17 C19 C20 C11 -179.0(4) . . . . ?
C17 C16 C15 C14 -1.0(8) . . . . ?
C12 N2 C13 O4 -175.5(5) . . . . ?
C12 N2 C13 C14 4.4(7) . . . . ?
C12 C11 C20 C19 178.5(5) . . . . ?
C12 C11 C20 C14 0.0(7) . . . . ?
C12 C11 C10 C9 -178.6(5) . . . . ?
C7 N1 C18 O2 171.6(5) . . . . ?
C7 N1 C18 C17 -8.4(7) . . . . ?
C7 N1 C1 C2 53.3(6) . . . . ?
C7 N1 C1 C6 -73.3(6) . . . . ?
C7 C8 C9 C10 179.7(5) . . . . ?
C20 C19 C8 C9 -1.3(7) . . . . ?
C20 C19 C8 C7 -179.7(4) . . . . ?
C20 C19 C17 C16 2.1(7) . . . . ?
C20 C19 C17 C18 -178.8(4) . . . . ?
C20 C14 C13 O4 179.7(5) . . . . ?
C20 C14 C13 N2 -0.2(7) . . . . ?
C20 C14 C15 C16 2.6(8) . . . . ?
C20 C11 C10 C9 -0.5(8) . . . . ?
C18 N1 C7 O1 -170.6(5) . . . . ?
C18 N1 C7 C8 10.0(7) . . . . ?
C18 N1 C1 C2 -131.7(5) . . . . ?
C18 N1 C1 C6 101.6(5) . . . . ?
C15 C16 C17 C19 -1.4(8) . . . . ?
C15 C16 C17 C18 179.5(5) . . . . ?
C15 C14 C13 O4 1.2(8) . . . . ?
C15 C14 C13 N2 -178.7(5) . . . . ?
C15 C14 C20 C19 -1.9(7) . . . . ?
C15 C14 C20 C11 176.7(5) . . . . ?
C10 C11 C20 C19 0.4(8) . . . . ?
C10 C11 C20 C14 -178.1(5) . . . . ?
C1 N1 C7 O1 3.9(7) . . . . ?
C1 N1 C7 C8 -175.6(4) . . . . ?
C1 N1 C18 O2 -3.2(7) . . . . ?
C1 N1 C18 C17 176.9(4) . . . . ?
C1 C2 C3 C4 59.9(7) . . . . ?
C1 C6 C5 C4 -56.0(8) . . . . ?
C2 N2 C13 O4 -1.3(7) 3_665 . . . ?
C2 N2 C13 C14 178.7(4) 3_665 . . . ?
C2 N2 C12 O3 1.1(7) 3_665 . . . ?
C2 N2 C12 C11 179.4(4) 3_665 . . . ?
C2 C1 C6 C5 57.2(7) . . . . ?
C2 C3 C4 C5 -57.8(9) . . . . ?
C6 C1 C2 N2 172.9(5) . . . 2_655 ?
C6 C1 C2 C3 -59.5(6) . . . . ?
C6 C5 C4 C3 56.8(10) . . . . ?
C28 C29 C34 C33 179.7(9) . . . . ?
C28 C29 C34 C21 0.4(14) . . . . ?
C28 C27 C26 C25 -178.1(10) . . . . ?
C28 C27 C22 C23 178.2(10) . . . . ?
C28 C27 C22 C21 -3.8(14) . . . . ?
C27 C26 C25 C24 0.0 . . . . ?
C27 C22 C21 C34 5.4(18) . . . . ?
C27 C22 C21 Cl1 -179.4(8) . . . . ?
C26 C27 C22 C23 0.0 . . . . ?
C26 C27 C22 C21 178.0(15) . . . . ?
C26 C25 C24 C23 0.0 . . . . ?
C25 C24 C23 C22 0.0 . . . . ?
C24 C23 C22 C27 0.0 . . . . ?
C24 C23 C22 C21 -178.0(15) . . . . ?
C23 C22 C21 C34 -176.5(9) . . . . ?
C23 C22 C21 Cl1 -1.4(17) . . . . ?
C22 C27 C26 C25 0.0 . . . . ?
C29A C30A C31A C32A 0.0 . . . . ?
C29A C34A C21A C22A 0(8) . . . . ?
C29A C34A C21A Cl1A 178(3) . . . . ?
C30A C29A C34A C33A 0.0 . . . . ?
C30A C29A C34A C21A 179(3) . . . . ?
C30A C29A C28A C27A -177.2(17) . . . . ?
C30A C29A C28A Cl2A 0(2) . . . . ?
C30A C31A C32A C33A 0.0 . . . . ?
C31A C32A C33A C34A 0.0 . . . . ?
C32A C33A C34A C29A 0.0 . . . . ?
C32A C33A C34A C21A -179(4) . . . . ?
C33A C34A C21A C22A 179(4) . . . . ?
C33A C34A C21A Cl1A -3(7) . . . . ?
C34A C29A C30A C31A 0.0 . . . . ?
C34A C29A C28A C27A 2(2) . . . . ?
C34A C29A C28A Cl2A -180(2) . . . . ?
C23A C24A C25A C26A 0.0 . . . . ?
C23A C22A C21A C34A 177(4) . . . . ?
C23A C22A C21A Cl1A -1(7) . . . . ?
C24A C23A C22A C27A 0.0 . . . . ?
C24A C23A C22A C21A -178(4) . . . . ?
C24A C25A C26A C27A 0.0 . . . . ?
C25A C26A C27A C22A 0.0 . . . . ?
C25A C26A C27A C28A 175(3) . . . . ?
C26A C27A C22A C23A 0.0 . . . . ?
C26A C27A C22A C21A 178(4) . . . . ?
C26A C27A C28A C29A -178.5(14) . . . . ?
C26A C27A C28A Cl2A 4(3) . . . . ?
C27A C22A C21A C34A -1(8) . . . . ?
C27A C22A C21A Cl1A -179(3) . . . . ?
C22A C23A C24A C25A 0.0 . . . . ?
C22A C27A C28A C29A -3(3) . . . . ?
C22A C27A C28A Cl2A 179(2) . . . . ?
C28A C29A C30A C31A 179.7(11) . . . . ?
C28A C29A C34A C33A -179.7(10) . . . . ?
C28A C29A C34A C21A -1(4) . . . . ?
C28A C27A C22A C23A -175(3) . . . . ?
C28A C27A C22A C21A 2(4) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 1335 electrons were 
found in a volume of 3920Å³ in 1 void per unit cell. 
This is consistent with the presence of 
3.52[CH2Cl2] per Asymmetric Unit 
which account for 1331 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.419 -0.348 -0.268 3920.3 1335.2 '31.68 CH2Cl2'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.562
####################################################################### 
# 
# 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_cjlc
_database_code_depnum_ccdc_archive 'CCDC 2391869'
loop_
_audit_author_name
_audit_author_address
'Jialin Cui'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2024-10-15 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_audit_creation_date             2024-09-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C20 H14 N2 O4), C H2 Cl2, C16 H10, 3.88[CH2Cl2]'
_chemical_formula_sum            'C57 H40 Cl2 N4 O8'
_chemical_formula_weight         979.83
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   24.6536(8)
_cell_length_b                   24.6536(8)
_cell_length_c                   25.2258(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13278.1(11)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.776
_cell_measurement_theta_min      2.422
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.976
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1294 before and 0.0728 after correction.
The Ratio of minimum to maximum transmission is 0.8742.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4572
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            83542
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.868
_diffrn_reflns_theta_min         1.875
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.936
_reflns_number_gt                8828
_reflns_number_total             13557
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SMART APEX II diffractometer'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 
;
 Flack x determined using 3438 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.24(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         13557
_refine_ls_number_restraints     1073
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0558
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0857P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1607
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl2-C59 = Cl2A-C59A = Cl1A-C59A = Cl1-C59
 1.79 with sigma of 0.01
 C51-C50 = C52-C51 = C53-C52 = C55-C54 = C54-C53 = C54-C41
 1.39 with sigma of 0.01
 C44-C43 = C45-C44 = C46-C45 = C47-C46
 1.39 with sigma of 0.01
 Cl1-Cl2 = Cl2A-Cl1A
 2.924 with sigma of 0.02
3. Restrained planarity
 C42A, C43A, C50A, C51A, C53A, C54A, C55A, C56A, C52A, C41A, C47A, C48A, C49A,
 C44A, C45A, C46A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
5. Same fragment restrains
{C41A, C42A, C43A, C44A, C45A, C46A, C47A, C48A, C49A, C50A, C51A, C52A, C53A,
C54A, C55A, C56A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C41, C42, C43, C44, C45, C46, C47, C48, C49, C50, C51, C52, C53, C54, C55, C56}
6. Others
 Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(C44A)=Sof(H44A)=
 Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(C48A)=Sof(H48A)=
 Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(C51A)=Sof(H51A)=Sof(C52A)=Sof(H52A)=
 Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(C55A)=Sof(C56A)=1-FVAR(1)
 Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(C44)=Sof(H44)=Sof(C45)=
 Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=
 Sof(C50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=
 Sof(C55)=Sof(C56)=FVAR(1)
 Sof(Cl2A)=Sof(C59A)=Sof(H59C)=Sof(H59D)=Sof(Cl1A)=1-FVAR(2)
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(Cl1)=Sof(Cl2)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C21(H21), C22(H22)
7.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C59(H59A,H59B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C59A(H59C,H59D)
7.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C15(H15), C16(H16), C29(H29), C30(H30), C35(H35), C36(H36),
 C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51),
  C52(H52), C53(H53), C41A(H41A), C42A(H42A), C44A(H44A), C45A(H45A),
 C46A(H46A), C48A(H48A), C49A(H49A), C51A(H51A), C52A(H52A), C53A(H53A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.44960(18) 0.49392(18) 0.34760(17) 0.0317(9) Uani 1 1 d . U . . .
H1 H 0.461214 0.500606 0.385178 0.038 Uiso 1 1 calc R U . . .
C2 C 0.50261(18) 0.54694(18) 0.31604(16) 0.0283(8) Uani 1 1 d . U . . .
H2 H 0.494070 0.535881 0.278449 0.034 Uiso 1 1 calc R U . . .
C3 C 0.5645(2) 0.5499(2) 0.32909(18) 0.0387(10) Uani 1 1 d . U . . .
H3A H 0.598003 0.583062 0.308630 0.046 Uiso 1 1 calc R U . . .
H3B H 0.574011 0.559462 0.366403 0.046 Uiso 1 1 calc R U . . .
C4 C 0.5603(2) 0.4883(2) 0.3164(2) 0.0442(11) Uani 1 1 d . U . . .
H4A H 0.598960 0.490047 0.327154 0.053 Uiso 1 1 calc R U . . .
H4B H 0.555970 0.481645 0.278416 0.053 Uiso 1 1 calc R U . . .
C5 C 0.5055(2) 0.4334(2) 0.3440(2) 0.0439(11) Uani 1 1 d . U . . .
H5A H 0.512298 0.437121 0.382058 0.053 Uiso 1 1 calc R U . . .
H5B H 0.502930 0.394578 0.332654 0.053 Uiso 1 1 calc R U . . .
C6 C 0.4432(2) 0.43137(19) 0.33117(19) 0.0392(10) Uani 1 1 d . U . . .
H6A H 0.434346 0.424497 0.293521 0.047 Uiso 1 1 calc R U . . .
H6B H 0.408956 0.397384 0.350363 0.047 Uiso 1 1 calc R U . . .
C7 C 0.36308(19) 0.48813(19) 0.29179(16) 0.0318(9) Uani 1 1 d . U . . .
C8 C 0.30247(18) 0.48825(18) 0.28646(15) 0.0267(8) Uani 1 1 d . U . . .
C9 C 0.2749(2) 0.4823(2) 0.23943(16) 0.0338(9) Uani 1 1 d . U . . .
H9 H 0.293571 0.477393 0.209121 0.041 Uiso 1 1 calc R U . . .
C10 C 0.21828(19) 0.4832(2) 0.23463(15) 0.0333(9) Uani 1 1 d . U . . .
H10 H 0.200642 0.480422 0.201443 0.040 Uiso 1 1 calc R U . . .
C11 C 0.18915(18) 0.48821(18) 0.28018(15) 0.0277(8) Uani 1 1 d . U . . .
C12 C 0.12843(17) 0.48702(18) 0.27458(14) 0.0260(8) Uani 1 1 d . U . . .
C13 C 0.12351(19) 0.49090(19) 0.37281(15) 0.0310(9) Uani 1 1 d . U . . .
C14 C 0.18430(18) 0.49196(18) 0.37679(14) 0.0266(8) Uani 1 1 d . U . . .
C15 C 0.20964(19) 0.4924(2) 0.42538(15) 0.0328(9) Uani 1 1 d . U . . .
H15 H 0.189109 0.492704 0.456210 0.039 Uiso 1 1 calc R U . . .
C16 C 0.26627(19) 0.4924(2) 0.42859(15) 0.0332(9) Uani 1 1 d . U . . .
H16 H 0.282620 0.492228 0.461777 0.040 Uiso 1 1 calc R U . . .
C17 C 0.29794(18) 0.49263(18) 0.38462(14) 0.0281(8) Uani 1 1 d . U . . .
C18 C 0.35697(18) 0.49166(18) 0.38889(15) 0.0287(8) Uani 1 1 d . U . . .
C19 C 0.27323(18) 0.49250(17) 0.33386(13) 0.0243(8) Uani 1 1 d . U . . .
C20 C 0.21603(19) 0.49103(18) 0.33042(14) 0.0270(8) Uani 1 1 d . U . . .
N1 N 0.38782(15) 0.49296(15) 0.34153(12) 0.0260(7) Uani 1 1 d . U . . .
N2 N 0.10248(14) 0.49397(15) 0.32302(12) 0.0267(7) Uani 1 1 d . U . . .
O1 O 0.38905(14) 0.48447(16) 0.25147(10) 0.0400(7) Uani 1 1 d . U . . .
O2 O 0.37831(15) 0.48937(16) 0.43134(11) 0.0440(8) Uani 1 1 d . U . . .
O3 O 0.10267(14) 0.48003(16) 0.23340(11) 0.0437(8) Uani 1 1 d . U . . .
O4 O 0.09339(14) 0.48820(14) 0.41192(11) 0.0388(7) Uani 1 1 d . U . . .
C59 C 0.3349(4) 0.2494(4) 0.1780(3) 0.085(3) Uani 0.762(11) 1 d D U P A 1
H59A H 0.308752 0.213822 0.200492 0.102 Uiso 0.762(11) 1 calc R U P A 1
H59B H 0.361891 0.239066 0.157585 0.102 Uiso 0.762(11) 1 calc R U P A 1
Cl1 Cl 0.3815(3) 0.3152(3) 0.2181(3) 0.1026(19) Uani 0.762(11) 1 d D U P A 1
Cl2 Cl 0.28684(19) 0.2627(2) 0.13424(12) 0.0958(13) Uani 0.762(11) 1 d D U P A
1
C21 C -0.11972(18) 0.16930(18) 0.37106(16) 0.0289(8) Uani 1 1 d . U . . .
H21 H -0.130620 0.161051 0.408700 0.035 Uiso 1 1 calc R U . . .
C22 C -0.17274(18) 0.11584(19) 0.33918(16) 0.0311(9) Uani 1 1 d . U . . .
H22 H -0.165940 0.127518 0.301617 0.037 Uiso 1 1 calc R U . . .
C23 C -0.23425(19) 0.1112(2) 0.35580(19) 0.0377(10) Uani 1 1 d . U . . .
H23A H -0.240859 0.102657 0.393496 0.045 Uiso 1 1 calc R U . . .
H23B H -0.268750 0.077140 0.336939 0.045 Uiso 1 1 calc R U . . .
C24 C -0.2321(2) 0.1728(2) 0.3432(2) 0.0503(12) Uani 1 1 d . U . . .
H24A H -0.227542 0.179854 0.305250 0.060 Uiso 1 1 calc R U . . .
H24B H -0.271324 0.169727 0.353830 0.060 Uiso 1 1 calc R U . . .
C25 C -0.1783(2) 0.2281(2) 0.3713(2) 0.0472(11) Uani 1 1 d . U . . .
H25A H -0.176601 0.266718 0.360553 0.057 Uiso 1 1 calc R U . . .
H25B H -0.184720 0.223657 0.409395 0.057 Uiso 1 1 calc R U . . .
C26 C -0.1173(2) 0.2304(2) 0.35711(18) 0.0376(10) Uani 1 1 d . U . . .
H26A H -0.109455 0.238381 0.319433 0.045 Uiso 1 1 calc R U . . .
H26B H -0.082995 0.264614 0.376080 0.045 Uiso 1 1 calc R U . . .
C27 C -0.03435(18) 0.17532(18) 0.31360(15) 0.0291(8) Uani 1 1 d . U . . .
C28 C 0.02558(19) 0.17394(18) 0.31037(14) 0.0283(8) Uani 1 1 d . U . . .
C29 C 0.05033(19) 0.1739(2) 0.26235(15) 0.0342(9) Uani 1 1 d . U . . .
H29 H 0.029247 0.173787 0.231729 0.041 Uiso 1 1 calc R U . . .
C30 C 0.1072(2) 0.1741(2) 0.25807(15) 0.0338(9) Uani 1 1 d . U . . .
H30 H 0.123596 0.174145 0.224868 0.041 Uiso 1 1 calc R U . . .
C31 C 0.13792(18) 0.17435(18) 0.30236(15) 0.0289(8) Uani 1 1 d . U . . .
C32 C 0.19888(18) 0.17431(18) 0.29728(15) 0.0283(8) Uani 1 1 d . U . . .
C33 C 0.20836(19) 0.17860(18) 0.39509(15) 0.0298(9) Uani 1 1 d . U . . .
C34 C 0.14758(18) 0.17867(19) 0.40006(15) 0.0285(8) Uani 1 1 d . U . . .
C35 C 0.1258(2) 0.1835(2) 0.44798(16) 0.0358(10) Uani 1 1 d . U . . .
H35 H 0.148767 0.187343 0.478402 0.043 Uiso 1 1 calc R U . . .
C36 C 0.06809(19) 0.1827(2) 0.45200(15) 0.0330(9) Uani 1 1 d . U . . .
H36 H 0.052297 0.184156 0.485124 0.040 Uiso 1 1 calc R U . . .
C37 C 0.03535(19) 0.17983(18) 0.40670(15) 0.0277(8) Uani 1 1 d . U . . .
C38 C -0.02495(18) 0.17989(18) 0.41255(15) 0.0267(8) Uani 1 1 d . U . . .
C39 C 0.05760(18) 0.17582(18) 0.35654(14) 0.0257(8) Uani 1 1 d . U . . .
C40 C 0.11540(18) 0.17494(17) 0.35277(14) 0.0251(8) Uani 1 1 d . U . . .
N3 N -0.05867(15) 0.17317(15) 0.36371(12) 0.0274(7) Uani 1 1 d . U . . .
N4 N 0.22885(15) 0.17399(15) 0.34509(12) 0.0285(7) Uani 1 1 d . U . . .
O5 O -0.06139(14) 0.17801(15) 0.27471(11) 0.0394(7) Uani 1 1 d . U . . .
O6 O -0.04363(14) 0.18617(16) 0.45317(11) 0.0425(8) Uani 1 1 d . U . . .
O7 O 0.22185(14) 0.17713(15) 0.25569(11) 0.0427(8) Uani 1 1 d . U . . .
O8 O 0.23741(13) 0.18206(16) 0.43444(11) 0.0395(7) Uani 1 1 d . U . . .
C41 C 0.0735(6) 0.3363(6) 0.3039(6) 0.061(3) Uani 0.531(9) 1 d D U P B 1
H41 H 0.045209 0.340463 0.282316 0.073 Uiso 0.531(9) 1 calc R U P B 1
C42 C 0.0662(6) 0.3338(6) 0.3614(6) 0.057(3) Uani 0.531(9) 1 d D U P B 1
H42 H 0.030269 0.330778 0.376433 0.069 Uiso 0.531(9) 1 calc R U P B 1
C43 C 0.1098(6) 0.3359(7) 0.3916(5) 0.059(3) Uani 0.531(9) 1 d D U P B 1
C44 C 0.0978(7) 0.3366(6) 0.4449(5) 0.076(3) Uani 0.531(9) 1 d D U P B 1
H44 H 0.062881 0.337463 0.457840 0.091 Uiso 0.531(9) 1 calc R U P B 1
C45 C 0.1441(8) 0.3359(7) 0.4779(5) 0.073(4) Uani 0.531(9) 1 d D U P B 1
H45 H 0.138657 0.335940 0.514415 0.088 Uiso 0.531(9) 1 calc R U P B 1
C46 C 0.1981(7) 0.3352(7) 0.4591(4) 0.072(4) Uani 0.531(9) 1 d D U P B 1
H46 H 0.225859 0.333537 0.483110 0.087 Uiso 0.531(9) 1 calc R U P B 1
C47 C 0.2096(6) 0.3370(8) 0.4043(4) 0.059(3) Uani 0.531(9) 1 d D U P B 1
C48 C 0.2641(6) 0.3380(7) 0.3815(6) 0.061(3) Uani 0.531(9) 1 d D U P B 1
H48 H 0.296787 0.342955 0.403143 0.073 Uiso 0.531(9) 1 calc R U P B 1
C49 C 0.2675(5) 0.3310(6) 0.3233(6) 0.054(3) Uani 0.531(9) 1 d D U P B 1
H49 H 0.300031 0.327498 0.308339 0.064 Uiso 0.531(9) 1 calc R U P B 1
C50 C 0.2181(6) 0.3298(7) 0.2902(4) 0.056(3) Uani 0.531(9) 1 d D U P B 1
C51 C 0.2212(6) 0.3334(6) 0.2349(4) 0.065(3) Uani 0.531(9) 1 d D U P B 1
H51 H 0.257023 0.339617 0.217303 0.078 Uiso 0.531(9) 1 calc R U P B 1
C52 C 0.1700(7) 0.3275(6) 0.2062(5) 0.067(4) Uani 0.531(9) 1 d D U P B 1
H52 H 0.169585 0.320357 0.170003 0.080 Uiso 0.531(9) 1 calc R U P B 1
C53 C 0.1187(7) 0.3313(7) 0.2269(5) 0.073(4) Uani 0.531(9) 1 d D U P B 1
H53 H 0.087604 0.332709 0.207205 0.088 Uiso 0.531(9) 1 calc R U P B 1
C54 C 0.1228(6) 0.3324(7) 0.2814(4) 0.056(3) Uani 0.531(9) 1 d D U P B 1
C55 C 0.1667(7) 0.3316(11) 0.3144(4) 0.042(3) Uani 0.531(9) 1 d D U P B 1
C56 C 0.1610(7) 0.3358(12) 0.3702(4) 0.048(3) Uani 0.531(9) 1 d D U P B 1
C41A C 0.0635(6) 0.3311(6) 0.3290(7) 0.052(3) Uani 0.469(9) 1 d D U P B 2
H41A H 0.027897 0.330076 0.315487 0.063 Uiso 0.469(9) 1 calc R U P B 2
C42A C 0.0750(7) 0.3341(6) 0.3858(7) 0.060(3) Uani 0.469(9) 1 d D U P B 2
H42A H 0.045948 0.335398 0.408488 0.072 Uiso 0.469(9) 1 calc R U P B 2
C43A C 0.1239(6) 0.3353(5) 0.4065(5) 0.058(3) Uani 0.469(9) 1 d D U P B 2
C44A C 0.1272(8) 0.3388(8) 0.4607(5) 0.067(4) Uani 0.469(9) 1 d D U P B 2
H44A H 0.097003 0.340693 0.481540 0.080 Uiso 0.469(9) 1 calc R U P B 2
C45A C 0.1808(8) 0.3394(6) 0.4824(5) 0.063(4) Uani 0.469(9) 1 d D U P B 2
H45A H 0.185135 0.340628 0.519120 0.076 Uiso 0.469(9) 1 calc R U P B 2
C46A C 0.2286(7) 0.3383(6) 0.4508(5) 0.059(3) Uani 0.469(9) 1 d D U P B 2
H46A H 0.262659 0.338760 0.467146 0.071 Uiso 0.469(9) 1 calc R U P B 2
C47A C 0.2243(7) 0.3365(9) 0.3948(5) 0.052(3) Uani 0.469(9) 1 d D U P B 2
C48A C 0.2686(6) 0.3328(6) 0.3594(6) 0.048(3) Uani 0.469(9) 1 d D U P B 2
H48A H 0.303425 0.332596 0.373312 0.057 Uiso 0.469(9) 1 calc R U P B 2
C49A C 0.2588(7) 0.3294(8) 0.3010(7) 0.065(4) Uani 0.469(9) 1 d D U P B 2
H49A H 0.286953 0.327035 0.277842 0.078 Uiso 0.469(9) 1 calc R U P B 2
C50A C 0.2031(7) 0.3299(6) 0.2814(4) 0.060(3) Uani 0.469(9) 1 d D U P B 2
C51A C 0.1893(9) 0.3274(7) 0.2276(5) 0.074(4) Uani 0.469(9) 1 d D U P B 2
H51A H 0.216466 0.326022 0.202761 0.089 Uiso 0.469(9) 1 calc R U P B 2
C52A C 0.1353(9) 0.3270(8) 0.2107(6) 0.073(4) Uani 0.469(9) 1 d D U P B 2
H52A H 0.127915 0.324560 0.174403 0.088 Uiso 0.469(9) 1 calc R U P B 2
C53A C 0.0905(7) 0.3300(6) 0.2443(6) 0.077(4) Uani 0.469(9) 1 d D U P B 2
H53A H 0.055504 0.331862 0.233123 0.093 Uiso 0.469(9) 1 calc R U P B 2
C54A C 0.1076(7) 0.3296(8) 0.2960(5) 0.059(3) Uani 0.469(9) 1 d D U P B 2
C55A C 0.1599(8) 0.3324(13) 0.3175(4) 0.049(3) Uani 0.469(9) 1 d D U P B 2
C56A C 0.1673(8) 0.3332(13) 0.3734(4) 0.046(3) Uani 0.469(9) 1 d D U P B 2
Cl2A Cl 0.2890(7) 0.2947(10) 0.1422(6) 0.114(5) Uani 0.238(11) 1 d D U P A 2
C59A C 0.3596(12) 0.2901(17) 0.1469(8) 0.094(6) Uani 0.238(11) 1 d D U P A 2
H59C H 0.354078 0.251792 0.131117 0.113 Uiso 0.238(11) 1 calc R U P A 2
H59D H 0.394661 0.325750 0.130123 0.113 Uiso 0.238(11) 1 calc R U P A 2
Cl1A Cl 0.3703(9) 0.2907(9) 0.2172(7) 0.081(4) Uani 0.238(11) 1 d D U P A 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
C1 H1 0.9800 . ?
C1 C2 1.530(6) . ?
C1 C6 1.527(6) . ?
C1 N1 1.519(5) . ?
C2 H2 0.9800 . ?
C2 C3 1.526(6) . ?
C2 N2 1.488(5) 2_665 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.505(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.523(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.547(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.502(5) . ?
C7 N1 1.374(5) . ?
C7 O1 1.229(5) . ?
C8 C9 1.338(6) . ?
C8 C19 1.427(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.413(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.393(5) . ?
C11 C12 1.489(5) . ?
C11 C20 1.416(5) . ?
C12 N2 1.429(5) . ?
C12 O3 1.184(5) . ?
C13 C14 1.489(6) . ?
C13 N2 1.375(5) . ?
C13 O4 1.216(5) . ?
C14 C15 1.373(5) . ?
C14 C20 1.414(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.398(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.355(5) . ?
C17 C18 1.471(6) . ?
C17 C19 1.417(5) . ?
C18 N1 1.408(5) . ?
C18 O2 1.207(5) . ?
C19 C20 1.395(5) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 Cl1 1.764(9) . ?
C59 Cl2 1.766(9) . ?
C21 H21 0.9800 . ?
C21 C22 1.540(6) . ?
C21 C26 1.520(6) . ?
C21 N3 1.472(5) . ?
C22 H22 0.9800 . ?
C22 C23 1.522(6) . ?
C22 N4 1.496(5) 2 ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.525(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.521(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.520(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.497(5) . ?
C27 N3 1.389(5) . ?
C27 O5 1.206(5) . ?
C28 C29 1.356(5) . ?
C28 C39 1.395(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.404(6) . ?
C30 H30 0.9300 . ?
C30 C31 1.349(5) . ?
C31 C32 1.509(6) . ?
C31 C40 1.390(5) . ?
C32 N4 1.417(5) . ?
C32 O7 1.178(5) . ?
C33 C34 1.505(6) . ?
C33 N4 1.384(5) . ?
C33 O8 1.202(5) . ?
C34 C35 1.352(6) . ?
C34 C40 1.410(5) . ?
C35 H35 0.9300 . ?
C35 C36 1.417(6) . ?
C36 H36 0.9300 . ?
C36 C37 1.380(5) . ?
C37 C38 1.495(5) . ?
C37 C39 1.402(5) . ?
C38 N3 1.449(5) . ?
C38 O6 1.165(5) . ?
C39 C40 1.439(5) . ?
C41 H41 0.9300 . ?
C41 C42 1.461(15) . ?
C41 C54 1.386(10) . ?
C42 H42 0.9300 . ?
C42 C43 1.299(16) . ?
C43 C44 1.378(10) . ?
C43 C56 1.374(12) . ?
C44 H44 0.9300 . ?
C44 C45 1.420(12) . ?
C45 H45 0.9300 . ?
C45 C46 1.422(12) . ?
C46 H46 0.9300 . ?
C46 C47 1.407(10) . ?
C47 C48 1.451(14) . ?
C47 C56 1.465(12) . ?
C48 H48 0.9300 . ?
C48 C49 1.484(15) . ?
C49 H49 0.9300 . ?
C49 C50 1.464(14) . ?
C50 C51 1.397(10) . ?
C50 C55 1.428(12) . ?
C51 H51 0.9300 . ?
C51 C52 1.399(11) . ?
C52 H52 0.9300 . ?
C52 C53 1.413(12) . ?
C53 H53 0.9300 . ?
C53 C54 1.377(10) . ?
C54 C55 1.374(9) . ?
C55 C56 1.422(9) . ?
C41A H41A 0.9300 . ?
C41A C42A 1.455(15) . ?
C41A C54A 1.384(14) . ?
C42A H42A 0.9300 . ?
C42A C43A 1.301(16) . ?
C43A C44A 1.371(13) . ?
C43A C56A 1.377(12) . ?
C44A H44A 0.9300 . ?
C44A C45A 1.425(16) . ?
C45A H45A 0.9300 . ?
C45A C46A 1.435(15) . ?
C46A H46A 0.9300 . ?
C46A C47A 1.415(12) . ?
C47A C48A 1.447(15) . ?
C47A C56A 1.469(13) . ?
C48A H48A 0.9300 . ?
C48A C49A 1.489(15) . ?
C49A H49A 0.9300 . ?
C49A C50A 1.467(15) . ?
C50A C51A 1.393(13) . ?
C50A C55A 1.424(12) . ?
C51A H51A 0.9300 . ?
C51A C52A 1.394(16) . ?
C52A H52A 0.9300 . ?
C52A C53A 1.424(16) . ?
C53A H53A 0.9300 . ?
C53A C54A 1.371(13) . ?
C54A C55A 1.369(11) . ?
C55A C56A 1.423(10) . ?
Cl2A C59A 1.803(14) . ?
C59A H59C 0.9700 . ?
C59A H59D 0.9700 . ?
C59A Cl1A 1.789(14) . ?

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
C2 C1 H1 107.9 . . ?
C6 C1 H1 107.9 . . ?
C6 C1 C2 109.5(3) . . ?
N1 C1 H1 107.9 . . ?
N1 C1 C2 112.5(3) . . ?
N1 C1 C6 111.1(3) . . ?
C1 C2 H2 107.0 . . ?
C3 C2 C1 109.6(3) . . ?
C3 C2 H2 107.0 . . ?
N2 C2 C1 113.5(3) 2_665 . ?
N2 C2 H2 107.0 2_665 . ?
N2 C2 C3 112.3(3) 2_665 . ?
C2 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 C2 110.1(3) . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
C3 C4 C5 112.5(4) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C4 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
C4 C5 C6 111.0(4) . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
C1 C6 C5 108.1(4) . . ?
C1 C6 H6A 110.1 . . ?
C1 C6 H6B 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
N1 C7 C8 118.7(3) . . ?
O1 C7 C8 118.8(3) . . ?
O1 C7 N1 122.5(4) . . ?
C9 C8 C7 122.0(3) . . ?
C9 C8 C19 120.3(4) . . ?
C19 C8 C7 117.7(3) . . ?
C8 C9 H9 119.2 . . ?
C8 C9 C10 121.7(4) . . ?
C10 C9 H9 119.2 . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.2(4) . . ?
C11 C10 H10 120.4 . . ?
C10 C11 C12 118.6(3) . . ?
C10 C11 C20 119.5(4) . . ?
C20 C11 C12 121.8(3) . . ?
N2 C12 C11 115.0(3) . . ?
O3 C12 C11 123.1(3) . . ?
O3 C12 N2 121.9(3) . . ?
N2 C13 C14 117.7(3) . . ?
O4 C13 C14 121.9(4) . . ?
O4 C13 N2 120.5(4) . . ?
C15 C14 C13 120.7(3) . . ?
C15 C14 C20 119.0(4) . . ?
C20 C14 C13 120.3(3) . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.1(4) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 119.1 . . ?
C17 C16 C15 121.7(4) . . ?
C17 C16 H16 119.1 . . ?
C16 C17 C18 120.8(4) . . ?
C16 C17 C19 119.6(4) . . ?
C19 C17 C18 119.6(3) . . ?
N1 C18 C17 117.7(3) . . ?
O2 C18 C17 121.6(4) . . ?
O2 C18 N1 120.7(4) . . ?
C17 C19 C8 121.7(4) . . ?
C20 C19 C8 119.2(3) . . ?
C20 C19 C17 118.9(3) . . ?
C14 C20 C11 119.5(4) . . ?
C19 C20 C11 120.0(3) . . ?
C19 C20 C14 120.6(3) . . ?
C7 N1 C1 119.4(3) . . ?
C7 N1 C18 124.2(3) . . ?
C18 N1 C1 116.1(3) . . ?
C12 N2 C2 114.0(3) . 3_565 ?
C13 N2 C2 120.8(3) . 3_565 ?
C13 N2 C12 124.8(3) . . ?
H59A C59 H59B 107.9 . . ?
Cl1 C59 H59A 109.2 . . ?
Cl1 C59 H59B 109.2 . . ?
Cl1 C59 Cl2 112.1(5) . . ?
Cl2 C59 H59A 109.2 . . ?
Cl2 C59 H59B 109.2 . . ?
C22 C21 H21 107.5 . . ?
C26 C21 H21 107.5 . . ?
C26 C21 C22 108.9(3) . . ?
N3 C21 H21 107.5 . . ?
N3 C21 C22 113.1(3) . . ?
N3 C21 C26 112.0(3) . . ?
C21 C22 H22 107.8 . . ?
C23 C22 C21 107.9(3) . . ?
C23 C22 H22 107.8 . . ?
N4 C22 C21 113.0(3) 2 . ?
N4 C22 H22 107.8 2 . ?
N4 C22 C23 112.2(3) 2 . ?
C22 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C22 C23 C24 109.3(4) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
C23 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C25 C24 C23 112.2(4) . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C24 C25 H25A 109.9 . . ?
C24 C25 H25B 109.9 . . ?
H25A C25 H25B 108.3 . . ?
C26 C25 C24 109.0(4) . . ?
C26 C25 H25A 109.9 . . ?
C26 C25 H25B 109.9 . . ?
C21 C26 C25 111.1(4) . . ?
C21 C26 H26A 109.4 . . ?
C21 C26 H26B 109.4 . . ?
C25 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
N3 C27 C28 117.4(3) . . ?
O5 C27 C28 122.4(3) . . ?
O5 C27 N3 120.2(4) . . ?
C29 C28 C27 119.9(3) . . ?
C29 C28 C39 119.9(4) . . ?
C39 C28 C27 120.2(3) . . ?
C28 C29 H29 119.4 . . ?
C28 C29 C30 121.1(4) . . ?
C30 C29 H29 119.4 . . ?
C29 C30 H30 120.2 . . ?
C31 C30 C29 119.6(4) . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C32 119.2(3) . . ?
C30 C31 C40 122.1(4) . . ?
C40 C31 C32 118.7(3) . . ?
N4 C32 C31 116.8(3) . . ?
O7 C32 C31 121.7(4) . . ?
O7 C32 N4 121.5(4) . . ?
N4 C33 C34 118.7(3) . . ?
O8 C33 C34 119.3(3) . . ?
O8 C33 N4 122.0(4) . . ?
C35 C34 C33 120.9(3) . . ?
C35 C34 C40 121.8(4) . . ?
C40 C34 C33 117.2(3) . . ?
C34 C35 H35 119.9 . . ?
C34 C35 C36 120.2(4) . . ?
C36 C35 H35 119.9 . . ?
C35 C36 H36 120.0 . . ?
C37 C36 C35 119.9(4) . . ?
C37 C36 H36 120.0 . . ?
C36 C37 C38 118.3(3) . . ?
C36 C37 C39 120.8(4) . . ?
C39 C37 C38 120.9(3) . . ?
N3 C38 C37 115.5(3) . . ?
O6 C38 C37 123.1(3) . . ?
O6 C38 N3 121.4(4) . . ?
C28 C39 C37 121.4(3) . . ?
C28 C39 C40 119.5(3) . . ?
C37 C39 C40 119.1(3) . . ?
C31 C40 C34 124.0(4) . . ?
C31 C40 C39 117.7(3) . . ?
C34 C40 C39 118.2(3) . . ?
C27 N3 C21 121.7(3) . . ?
C27 N3 C38 123.9(3) . . ?
C38 N3 C21 114.2(3) . . ?
C32 N4 C22 115.9(3) . 3 ?
C33 N4 C22 119.7(3) . 3 ?
C33 N4 C32 124.2(3) . . ?
C42 C41 H41 120.1 . . ?
C54 C41 H41 120.1 . . ?
C54 C41 C42 119.9(10) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 C41 119.8(10) . . ?
C43 C42 H42 120.1 . . ?
C42 C43 C44 113.1(11) . . ?
C42 C43 C56 120.9(10) . . ?
C56 C43 C44 126.1(12) . . ?
C43 C44 H44 123.5 . . ?
C43 C44 C45 113.1(12) . . ?
C45 C44 H44 123.5 . . ?
C44 C45 H45 117.7 . . ?
C44 C45 C46 124.6(12) . . ?
C46 C45 H45 117.7 . . ?
C45 C46 H46 119.9 . . ?
C47 C46 C45 120.2(12) . . ?
C47 C46 H46 119.9 . . ?
C46 C47 C48 124.2(11) . . ?
C46 C47 C56 115.3(11) . . ?
C48 C47 C56 120.5(9) . . ?
C47 C48 H48 120.1 . . ?
C47 C48 C49 119.7(10) . . ?
C49 C48 H48 120.1 . . ?
C48 C49 H49 120.9 . . ?
C50 C49 C48 118.2(10) . . ?
C50 C49 H49 120.9 . . ?
C51 C50 C49 123.4(11) . . ?
C51 C50 C55 116.5(10) . . ?
C55 C50 C49 119.7(8) . . ?
C50 C51 H51 120.3 . . ?
C50 C51 C52 119.5(11) . . ?
C52 C51 H51 120.3 . . ?
C51 C52 H52 116.8 . . ?
C51 C52 C53 126.4(12) . . ?
C53 C52 H52 116.8 . . ?
C52 C53 H53 125.9 . . ?
C54 C53 C52 108.2(12) . . ?
C54 C53 H53 125.9 . . ?
C53 C54 C41 110.6(10) . . ?
C55 C54 C41 118.5(9) . . ?
C55 C54 C53 130.9(11) . . ?
C54 C55 C50 117.3(9) . . ?
C54 C55 C56 119.4(9) . . ?
C56 C55 C50 123.2(8) . . ?
C43 C56 C47 120.7(9) . . ?
C43 C56 C55 120.9(9) . . ?
C55 C56 C47 118.3(8) . . ?
C42A C41A H41A 121.4 . . ?
C54A C41A H41A 121.4 . . ?
C54A C41A C42A 117.3(11) . . ?
C41A C42A H42A 118.3 . . ?
C43A C42A C41A 123.5(12) . . ?
C43A C42A H42A 118.3 . . ?
C42A C43A C44A 115.2(12) . . ?
C42A C43A C56A 119.0(11) . . ?
C44A C43A C56A 125.8(13) . . ?
C43A C44A H44A 122.9 . . ?
C43A C44A C45A 114.1(13) . . ?
C45A C44A H44A 122.9 . . ?
C44A C45A H45A 118.2 . . ?
C44A C45A C46A 123.6(12) . . ?
C46A C45A H45A 118.2 . . ?
C45A C46A H46A 119.8 . . ?
C47A C46A C45A 120.5(12) . . ?
C47A C46A H46A 119.8 . . ?
C46A C47A C48A 124.8(11) . . ?
C46A C47A C56A 115.0(11) . . ?
C48A C47A C56A 120.1(9) . . ?
C47A C48A H48A 119.7 . . ?
C47A C48A C49A 120.6(10) . . ?
C49A C48A H48A 119.7 . . ?
C48A C49A H49A 121.4 . . ?
C50A C49A C48A 117.2(11) . . ?
C50A C49A H49A 121.4 . . ?
C51A C50A C49A 122.4(12) . . ?
C51A C50A C55A 117.0(12) . . ?
C55A C50A C49A 120.7(10) . . ?
C50A C51A H51A 119.7 . . ?
C50A C51A C52A 120.6(14) . . ?
C52A C51A H51A 119.7 . . ?
C51A C52A H52A 117.2 . . ?
C51A C52A C53A 125.5(13) . . ?
C53A C52A H52A 117.2 . . ?
C52A C53A H53A 125.8 . . ?
C54A C53A C52A 108.5(13) . . ?
C54A C53A H53A 125.8 . . ?
C53A C54A C41A 108.9(12) . . ?
C55A C54A C41A 119.5(10) . . ?
C55A C54A C53A 131.4(13) . . ?
C54A C55A C50A 116.8(10) . . ?
C54A C55A C56A 120.3(10) . . ?
C56A C55A C50A 122.7(9) . . ?
C43A C56A C47A 121.0(10) . . ?
C43A C56A C55A 120.3(10) . . ?
C55A C56A C47A 118.5(9) . . ?
Cl2A C59A H59C 111.4 . . ?
Cl2A C59A H59D 111.4 . . ?
H59C C59A H59D 109.2 . . ?
Cl1A C59A Cl2A 102.0(11) . . ?
Cl1A C59A H59C 111.4 . . ?
Cl1A C59A H59D 111.4 . . ?

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
C1 C2 C3 C4 58.3(5) . . . . ?
C2 C1 C6 C5 61.1(4) . . . . ?
C2 C1 N1 C7 57.2(4) . . . . ?
C2 C1 N1 C18 -128.2(3) . . . . ?
C2 C3 C4 C5 -55.0(5) . . . . ?
C3 C4 C5 C6 54.9(5) . . . . ?
C4 C5 C6 C1 -57.0(5) . . . . ?
C6 C1 C2 C3 -62.6(4) . . . . ?
C6 C1 C2 N2 170.9(3) . . . 2_665 ?
C6 C1 N1 C7 -66.0(4) . . . . ?
C6 C1 N1 C18 108.6(4) . . . . ?
C7 C8 C9 C10 -179.2(4) . . . . ?
C7 C8 C19 C17 -3.9(5) . . . . ?
C7 C8 C19 C20 -178.3(3) . . . . ?
C8 C7 N1 C1 -179.1(3) . . . . ?
C8 C7 N1 C18 6.8(6) . . . . ?
C8 C9 C10 C11 -2.3(6) . . . . ?
C8 C19 C20 C11 -2.8(5) . . . . ?
C8 C19 C20 C14 176.8(3) . . . . ?
C9 C8 C19 C17 173.7(4) . . . . ?
C9 C8 C19 C20 -0.7(6) . . . . ?
C9 C10 C11 C12 -178.1(4) . . . . ?
C9 C10 C11 C20 -1.3(6) . . . . ?
C10 C11 C12 N2 -178.5(3) . . . . ?
C10 C11 C12 O3 2.4(6) . . . . ?
C10 C11 C20 C14 -175.8(4) . . . . ?
C10 C11 C20 C19 3.8(6) . . . . ?
C11 C12 N2 C2 175.7(3) . . . 3_565 ?
C11 C12 N2 C13 -11.4(5) . . . . ?
C12 C11 C20 C14 0.8(6) . . . . ?
C12 C11 C20 C19 -179.6(3) . . . . ?
C13 C14 C15 C16 179.0(4) . . . . ?
C13 C14 C20 C11 -0.9(6) . . . . ?
C13 C14 C20 C19 179.5(3) . . . . ?
C14 C13 N2 C2 -175.9(3) . . . 3_565 ?
C14 C13 N2 C12 11.6(6) . . . . ?
C14 C15 C16 C17 0.7(6) . . . . ?
C15 C14 C20 C11 177.7(4) . . . . ?
C15 C14 C20 C19 -2.0(6) . . . . ?
C15 C16 C17 C18 -179.1(4) . . . . ?
C15 C16 C17 C19 -0.4(6) . . . . ?
C16 C17 C18 N1 -179.0(4) . . . . ?
C16 C17 C18 O2 1.5(6) . . . . ?
C16 C17 C19 C8 -175.5(4) . . . . ?
C16 C17 C19 C20 -1.1(6) . . . . ?
C17 C18 N1 C1 178.2(3) . . . . ?
C17 C18 N1 C7 -7.5(6) . . . . ?
C17 C19 C20 C11 -177.4(4) . . . . ?
C17 C19 C20 C14 2.3(5) . . . . ?
C18 C17 C19 C8 3.2(6) . . . . ?
C18 C17 C19 C20 177.6(3) . . . . ?
C19 C8 C9 C10 3.3(6) . . . . ?
C19 C17 C18 N1 2.3(5) . . . . ?
C19 C17 C18 O2 -177.2(4) . . . . ?
C20 C11 C12 N2 4.8(5) . . . . ?
C20 C11 C12 O3 -174.2(4) . . . . ?
C20 C14 C15 C16 0.5(6) . . . . ?
N1 C1 C2 C3 173.3(3) . . . . ?
N1 C1 C2 N2 46.9(4) . . . 2_665 ?
N1 C1 C6 C5 -174.0(3) . . . . ?
N1 C7 C8 C9 -178.4(4) . . . . ?
N1 C7 C8 C19 -0.9(5) . . . . ?
N2 C2 C3 C4 -174.6(3) 2_665 . . . ?
N2 C13 C14 C15 176.5(4) . . . . ?
N2 C13 C14 C20 -5.0(5) . . . . ?
O1 C7 C8 C9 2.4(6) . . . . ?
O1 C7 C8 C19 180.0(4) . . . . ?
O1 C7 N1 C1 0.0(6) . . . . ?
O1 C7 N1 C18 -174.1(4) . . . . ?
O2 C18 N1 C1 -2.3(5) . . . . ?
O2 C18 N1 C7 172.0(4) . . . . ?
O3 C12 N2 C2 -5.3(5) . . . 3_565 ?
O3 C12 N2 C13 167.7(4) . . . . ?
O4 C13 C14 C15 -2.6(6) . . . . ?
O4 C13 C14 C20 175.9(4) . . . . ?
O4 C13 N2 C2 3.2(6) . . . 3_565 ?
O4 C13 N2 C12 -169.3(4) . . . . ?
C21 C22 C23 C24 60.9(4) . . . . ?
C22 C21 C26 C25 61.1(4) . . . . ?
C22 C21 N3 C27 51.8(5) . . . . ?
C22 C21 N3 C38 -133.2(3) . . . . ?
C22 C23 C24 C25 -58.9(5) . . . . ?
C23 C24 C25 C26 55.6(5) . . . . ?
C24 C25 C26 C21 -56.7(5) . . . . ?
C26 C21 C22 C23 -62.3(4) . . . . ?
C26 C21 C22 N4 173.0(3) . . . 2 ?
C26 C21 N3 C27 -71.7(4) . . . . ?
C26 C21 N3 C38 103.3(4) . . . . ?
C27 C28 C29 C30 178.5(4) . . . . ?
C27 C28 C39 C37 -0.8(6) . . . . ?
C27 C28 C39 C40 -179.5(3) . . . . ?
C28 C27 N3 C21 -175.1(3) . . . . ?
C28 C27 N3 C38 10.4(5) . . . . ?
C28 C29 C30 C31 0.0(7) . . . . ?
C28 C39 C40 C31 2.1(5) . . . . ?
C28 C39 C40 C34 178.2(4) . . . . ?
C29 C28 C39 C37 176.0(4) . . . . ?
C29 C28 C39 C40 -2.7(6) . . . . ?
C29 C30 C31 C32 179.8(4) . . . . ?
C29 C30 C31 C40 -0.6(6) . . . . ?
C30 C31 C32 N4 -179.5(4) . . . . ?
C30 C31 C32 O7 3.7(6) . . . . ?
C30 C31 C40 C34 -176.3(4) . . . . ?
C30 C31 C40 C39 -0.5(6) . . . . ?
C31 C32 N4 C22 178.9(3) . . . 3 ?
C31 C32 N4 C33 -5.2(5) . . . . ?
C32 C31 C40 C34 3.3(6) . . . . ?
C32 C31 C40 C39 179.2(3) . . . . ?
C33 C34 C35 C36 -179.2(4) . . . . ?
C33 C34 C40 C31 -3.3(6) . . . . ?
C33 C34 C40 C39 -179.1(3) . . . . ?
C34 C33 N4 C22 -179.0(3) . . . 3 ?
C34 C33 N4 C32 5.3(5) . . . . ?
C34 C35 C36 C37 -2.9(6) . . . . ?
C35 C34 C40 C31 175.3(4) . . . . ?
C35 C34 C40 C39 -0.5(6) . . . . ?
C35 C36 C37 C38 -179.3(4) . . . . ?
C35 C36 C37 C39 1.8(6) . . . . ?
C36 C37 C38 N3 -176.6(4) . . . . ?
C36 C37 C38 O6 4.9(6) . . . . ?
C36 C37 C39 C28 -178.9(4) . . . . ?
C36 C37 C39 C40 -0.2(6) . . . . ?
C37 C38 N3 C21 176.2(3) . . . . ?
C37 C38 N3 C27 -8.9(5) . . . . ?
C37 C39 C40 C31 -176.6(4) . . . . ?
C37 C39 C40 C34 -0.5(5) . . . . ?
C38 C37 C39 C28 2.2(6) . . . . ?
C38 C37 C39 C40 -179.0(3) . . . . ?
C39 C28 C29 C30 1.7(6) . . . . ?
C39 C37 C38 N3 2.3(5) . . . . ?
C39 C37 C38 O6 -176.2(4) . . . . ?
C40 C31 C32 N4 0.9(5) . . . . ?
C40 C31 C32 O7 -176.0(4) . . . . ?
C40 C34 C35 C36 2.2(6) . . . . ?
N3 C21 C22 C23 172.4(3) . . . . ?
N3 C21 C22 N4 47.8(4) . . . 2 ?
N3 C21 C26 C25 -173.0(3) . . . . ?
N3 C27 C28 C29 177.9(4) . . . . ?
N3 C27 C28 C39 -5.3(5) . . . . ?
N4 C22 C23 C24 -174.0(3) 2 . . . ?
N4 C33 C34 C35 -179.5(4) . . . . ?
N4 C33 C34 C40 -0.9(5) . . . . ?
O5 C27 C28 C29 -1.9(6) . . . . ?
O5 C27 C28 C39 174.9(4) . . . . ?
O5 C27 N3 C21 4.7(6) . . . . ?
O5 C27 N3 C38 -169.8(4) . . . . ?
O6 C38 N3 C21 -5.3(5) . . . . ?
O6 C38 N3 C27 169.6(4) . . . . ?
O7 C32 N4 C22 -4.3(5) . . . 3 ?
O7 C32 N4 C33 171.6(4) . . . . ?
O8 C33 C34 C35 1.0(6) . . . . ?
O8 C33 C34 C40 179.6(4) . . . . ?
O8 C33 N4 C22 0.5(6) . . . 3 ?
O8 C33 N4 C32 -175.3(4) . . . . ?
C41 C42 C43 C44 176.6(12) . . . . ?
C41 C42 C43 C56 -5(2) . . . . ?
C41 C54 C55 C50 -177.9(14) . . . . ?
C41 C54 C55 C56 -1(3) . . . . ?
C42 C41 C54 C53 175.8(13) . . . . ?
C42 C41 C54 C55 -5(2) . . . . ?
C42 C43 C44 C45 177.2(12) . . . . ?
C42 C43 C56 C47 -178.9(16) . . . . ?
C42 C43 C56 C55 -2(3) . . . . ?
C43 C44 C45 C46 1(2) . . . . ?
C44 C43 C56 C47 -1(3) . . . . ?
C44 C43 C56 C55 176.6(18) . . . . ?
C44 C45 C46 C47 2(2) . . . . ?
C45 C46 C47 C48 178.4(14) . . . . ?
C45 C46 C47 C56 -3(2) . . . . ?
C46 C47 C48 C49 171.6(14) . . . . ?
C46 C47 C56 C43 3(3) . . . . ?
C46 C47 C56 C55 -174.3(19) . . . . ?
C47 C48 C49 C50 6.2(18) . . . . ?
C48 C47 C56 C43 -178.9(17) . . . . ?
C48 C47 C56 C55 4(3) . . . . ?
C48 C49 C50 C51 169.6(12) . . . . ?
C48 C49 C50 C55 -3.6(19) . . . . ?
C49 C50 C51 C52 175.5(12) . . . . ?
C49 C50 C55 C54 178.0(15) . . . . ?
C49 C50 C55 C56 1(3) . . . . ?
C50 C51 C52 C53 14(2) . . . . ?
C50 C55 C56 C43 -178.5(17) . . . . ?
C50 C55 C56 C47 -1(3) . . . . ?
C51 C50 C55 C54 4(2) . . . . ?
C51 C50 C55 C56 -172.5(19) . . . . ?
C51 C52 C53 C54 -9(2) . . . . ?
C52 C53 C54 C41 179.8(12) . . . . ?
C52 C53 C54 C55 1(2) . . . . ?
C53 C54 C55 C50 1(3) . . . . ?
C53 C54 C55 C56 177.5(19) . . . . ?
C54 C41 C42 C43 8.6(18) . . . . ?
C54 C55 C56 C43 5(3) . . . . ?
C54 C55 C56 C47 -177.9(18) . . . . ?
C55 C50 C51 C52 -11.0(19) . . . . ?
C56 C43 C44 C45 -1(2) . . . . ?
C56 C47 C48 C49 -6(2) . . . . ?
C41A C42A C43A C44A 179.4(12) . . . . ?
C41A C42A C43A C56A -0.3(15) . . . . ?
C41A C54A C55A C50A 179.2(15) . . . . ?
C41A C54A C55A C56A 3(3) . . . . ?
C42A C41A C54A C53A -177.0(11) . . . . ?
C42A C41A C54A C55A -1(2) . . . . ?
C42A C43A C44A C45A 179.5(9) . . . . ?
C42A C43A C56A C47A 177.9(15) . . . . ?
C42A C43A C56A C55A 2(3) . . . . ?
C43A C44A C45A C46A 1.8(19) . . . . ?
C44A C43A C56A C47A -2(3) . . . . ?
C44A C43A C56A C55A -177.1(19) . . . . ?
C44A C45A C46A C47A 0(2) . . . . ?
C45A C46A C47A C48A -177.5(14) . . . . ?
C45A C46A C47A C56A -2(2) . . . . ?
C46A C47A C48A C49A 178.3(14) . . . . ?
C46A C47A C56A C43A 3(3) . . . . ?
C46A C47A C56A C55A 179(2) . . . . ?
C47A C48A C49A C50A 0.0(19) . . . . ?
C48A C47A C56A C43A 178.6(17) . . . . ?
C48A C47A C56A C55A -6(3) . . . . ?
C48A C49A C50A C51A 179.5(12) . . . . ?
C48A C49A C50A C55A -1.2(19) . . . . ?
C49A C50A C51A C52A 179.0(13) . . . . ?
C49A C50A C55A C54A -177.0(16) . . . . ?
C49A C50A C55A C56A -1(3) . . . . ?
C50A C51A C52A C53A 1(2) . . . . ?
C50A C55A C56A C43A -179.7(17) . . . . ?
C50A C55A C56A C47A 5(4) . . . . ?
C51A C50A C55A C54A 2(2) . . . . ?
C51A C50A C55A C56A 178(2) . . . . ?
C51A C52A C53A C54A -3(2) . . . . ?
C52A C53A C54A C41A -178.6(13) . . . . ?
C52A C53A C54A C55A 6(3) . . . . ?
C53A C54A C55A C50A -6(3) . . . . ?
C53A C54A C55A C56A 178(2) . . . . ?
C54A C41A C42A C43A -0.4(15) . . . . ?
C54A C55A C56A C43A -4(4) . . . . ?
C54A C55A C56A C47A -180(2) . . . . ?
C55A C50A C51A C52A 0(2) . . . . ?
C56A C43A C44A C45A -1(2) . . . . ?
C56A C47A C48A C49A 4(2) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 1465 electrons were 
found in a volume of 4334Å³ in 1 void per unit cell. 
This is consistent with the presence of 
3.88[CH2Cl2] per Asymmetric Unit 
which account for 1467 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.050 -0.060 -0.106 4334.3 1464.6 '34.92 CH2Cl2'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bei-s-2
_database_code_depnum_ccdc_archive 'CCDC 2391867'
loop_
_audit_author_name
_audit_author_address
'Jialin Cui'
;Qingdao University of Science and Technology
China
;
_audit_update_record             
;
2024-10-15 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_audit_creation_date             2024-09-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C60 H42 N6 O12), 3(C20 H12)'
_chemical_formula_sum            'C180 H120 N12 O24'
_chemical_formula_weight         2834.87
_chemical_absolute_configuration syn
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
N N 0.0311 0.0180 '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      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'

_cell_length_a                   24.0472(4)
_cell_length_b                   24.0472(4)
_cell_length_c                   25.9660(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13003.6(5)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    8493
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.4830
_cell_measurement_theta_min      2.7110
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4428
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1261
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27636
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.078
_diffrn_reflns_theta_max         65.078
_diffrn_reflns_theta_min         2.720
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     43.00 104.00   0.50    1.81    --  107.17 -94.00 120.00  122
  2  ω     62.00 108.00   0.50    1.81    --  107.17-115.00  84.00   92
  3  ω     35.00 103.00   0.50    1.81    --  107.17 -94.00   0.00  136
  4  ω     53.00  93.00   0.50    1.81    --  107.17 -94.00 -30.00   80
  5  ω     49.00 103.00   0.50    1.81    --  107.17 -94.00-180.00  108
  6  ω    -31.00  18.00   0.50    0.45    --   41.52 -19.00 -90.00   98
  7  ω     43.00  73.00   0.50    1.81    --  107.17 -61.00  30.00   60
  8  ω     40.00  69.00   0.50    1.81    --  107.17 -61.00 120.00   58
  9  ω     33.00  66.00   0.50    1.81    --  107.17 -61.00 150.00   66
 10  ω     54.00 114.00   0.50    0.45    --   41.52 168.00 -40.00  120
 11  ω     83.00 164.00   0.50    1.81    --  107.17  70.00 -66.00  162
 12  ω     36.00  70.00   0.50    1.81    --  107.17 -61.00-180.00   68
 13  ω     61.00  90.00   0.50    0.45    --   41.52-125.00-180.00   58
 14  ω     25.00  53.00   0.50    0.45    --   41.52-125.00-180.00   56
 15  ω     12.00  87.00   0.50    0.45    --   41.52-115.00  84.00  150
 16  ω    -25.00  29.00   0.50    0.45    --  -41.52  37.00-150.00  108
 17  ω    -16.00  23.00   0.50    0.45    --  -41.52  19.00-180.00   78
 18  ω    -85.00 -28.00   0.50    1.81    -- -102.00  70.00 -66.00  114
 19  ω    -68.00 -30.00   0.50    1.81    -- -102.00  61.00 120.00   76
 20  ω    -69.00 -37.00   0.50    1.81    -- -102.00  61.00  60.00   64
 21  ω    -69.00 -30.00   0.50    1.81    -- -102.00 125.00 -30.00   78
 22  ω    -67.00 -28.00   0.50    1.81    -- -102.00 140.00-111.00   78
 23  ω   -121.00 -88.00   0.50    1.81    -- -102.00 140.00-111.00   66
 24  ω   -114.00 -72.00   0.50    1.81    -- -102.00 129.00  75.00   84
 25  ω    -66.00 -35.00   0.50    1.81    -- -102.00 129.00  75.00   62
 26  ω   -171.00 -85.00   0.50    1.81    -- -102.00 -30.00-180.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0239112000
_diffrn_orient_matrix_UB_12      0.0332546000
_diffrn_orient_matrix_UB_13      0.0374674000
_diffrn_orient_matrix_UB_21      -0.0332693000
_diffrn_orient_matrix_UB_22      0.0136435000
_diffrn_orient_matrix_UB_23      -0.0449691000
_diffrn_orient_matrix_UB_31      -0.0615497000
_diffrn_orient_matrix_UB_32      -0.0646347000
_diffrn_orient_matrix_UB_33      0.0097428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4241
_reflns_number_total             4937
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro system (CCD 42.84a 64-bit (release 16-02-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 
;
 Flack x determined using 1575 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.9(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4937
_refine_ls_number_restraints     572
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.1157
_refine_ls_restrained_S_all      1.024
_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)+(0.1962P)²+63.6865P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2923
_refine_ls_wR_factor_ref         0.3040
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C21-C30 = C27-C28 = C28-C29 = C30-C29 = C27-C26
 1.39 with sigma of 0.01
 C15-C20 \\sim C19-C20 \\sim C17-C18 \\sim C18-C19 \\sim C17-C16 \\sim C15-C16
 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within -2.5A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within -2.5A
4.a Ternary CH refined with riding coordinates:
 C20(H20), C15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H18A,H18B), C16(H16A,H16B), C17(H17A,H17B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C1(H1), C2(H2), C6(H6), C29(H29), C28(H28), C27(H27), C25(H25),
 C24(H24), C23(H23)
4.d Fitted hexagon refined as free rotating group:
 N1(C11,C10,C9,C8,C12), N2(C13,C5,C4,C3,C14), C26(C25,C24,C23,C22,C21)
;
_atom_sites_solution_hydrogens   geom
_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
O2 O 0.4862(3) 0.0903(3) 0.6050(2) 0.0434(14) Uani 1 1 d . U . . .
O1 O 0.4783(3) 0.1001(2) 0.7802(2) 0.0368(12) Uani 1 1 d . U . . .
O4 O 0.4812(3) 0.3921(3) 0.7608(2) 0.0374(12) Uani 1 1 d . U . . .
N1 N 0.4886(2) 0.09777(19) 0.69246(17) 0.0360(14) Uani 1 1 d G U . . .
C11 C 0.4930(3) 0.1251(2) 0.64440(14) 0.0403(17) Uani 1 1 d G U . . .
C10 C 0.4940(3) 0.1833(2) 0.64052(13) 0.0373(16) Uani 1 1 d G U . . .
C9 C 0.4905(3) 0.21402(19) 0.68471(17) 0.0340(15) Uani 1 1 d G U . . .
C8 C 0.4861(3) 0.1867(2) 0.73278(14) 0.0338(15) Uani 1 1 d G U . . .
C12 C 0.4852(2) 0.1285(2) 0.73665(14) 0.0325(15) Uani 1 1 d G U . . .
O3 O 0.4933(3) 0.3866(3) 0.5875(2) 0.0501(16) Uani 1 1 d . U . . .
C7 C 0.4771(4) 0.2167(3) 0.7764(3) 0.0309(15) Uani 1 1 d . U . . .
H7 H 0.470787 0.196897 0.809153 0.037 Uiso 1 1 calc R U . . .
N2 N 0.4887(3) 0.3902(2) 0.67317(17) 0.0386(14) Uani 1 1 d G U . . .
C13 C 0.4839(3) 0.3623(2) 0.72105(14) 0.0396(17) Uani 1 1 d G U . . .
C5 C 0.4848(3) 0.3051(2) 0.72467(14) 0.0371(16) Uani 1 1 d G U . . .
C4 C 0.4905(3) 0.2758(2) 0.68041(18) 0.0350(15) Uani 1 1 d G U . . .
C3 C 0.4953(3) 0.3037(2) 0.63253(15) 0.0393(17) Uani 1 1 d G U . . .
C14 C 0.4944(3) 0.3609(2) 0.62891(14) 0.0412(18) Uani 1 1 d G U . . .
C1 C 0.5008(4) 0.2136(4) 0.5922(3) 0.0391(17) Uani 1 1 d . U . . .
H1 H 0.505430 0.194082 0.561931 0.047 Uiso 1 1 calc R U . . .
C2 C 0.5009(4) 0.2711(4) 0.5883(3) 0.0408(18) Uani 1 1 d . U . . .
H2 H 0.504896 0.289532 0.555152 0.049 Uiso 1 1 calc R U . . .
C20 C 0.5454(3) 0.5082(3) 0.6980(3) 0.0376(17) Uani 1 1 d D U . . .
H20 H 0.533488 0.498729 0.735209 0.045 Uiso 1 1 calc R U . . .
C6 C 0.4772(4) 0.2752(4) 0.7725(3) 0.0349(16) Uani 1 1 d . U . . .
H6 H 0.471953 0.294584 0.802615 0.042 Uiso 1 1 calc R U . . .
C29 C 0.3274(4) 0.2669(5) 0.7222(3) 0.056(2) Uani 1 1 d D U . . .
H29 H 0.330276 0.302834 0.704460 0.067 Uiso 1 1 calc R U . . .
C28 C 0.3199(5) 0.2610(5) 0.7761(4) 0.071(3) Uani 1 1 d D U . . .
H28 H 0.314442 0.292016 0.794622 0.085 Uiso 1 1 calc R U . . .
C27 C 0.3201(5) 0.2110(5) 0.8029(4) 0.068(3) Uani 1 1 d D U . . .
H27 H 0.318992 0.209829 0.839506 0.082 Uiso 1 1 calc R U . . .
C26 C 0.3221(3) 0.1623(3) 0.7745(2) 0.059(2) Uani 1 1 d DG U . . .
C25 C 0.3192(3) 0.1112(4) 0.80181(18) 0.076(3) Uani 1 1 d G U . . .
H25 H 0.315786 0.109988 0.838285 0.091 Uiso 1 1 calc R U . . .
C24 C 0.3214(4) 0.0618(3) 0.7757(3) 0.072(3) Uani 1 1 d G U . . .
H24 H 0.319413 0.026869 0.794401 0.086 Uiso 1 1 calc R U . . .
C23 C 0.3265(3) 0.0635(3) 0.7224(3) 0.068(3) Uani 1 1 d G U . . .
H23 H 0.327927 0.029784 0.704551 0.082 Uiso 1 1 calc R U . . .
C22 C 0.3294(3) 0.1146(3) 0.69506(18) 0.056(2) Uani 1 1 d G U . . .
C21 C 0.3272(3) 0.1640(3) 0.7211(2) 0.057(2) Uani 1 1 d DG U . . .
C30 C 0.3304(4) 0.2178(4) 0.6958(3) 0.0464(19) Uani 1 1 d D U . . .
C19 C 0.5496(4) 0.5732(4) 0.6872(4) 0.048(2) Uani 1 1 d D U . . .
H19A H 0.585933 0.607792 0.706554 0.057 Uiso 1 1 calc R U . . .
H19B H 0.556969 0.583404 0.649993 0.057 Uiso 1 1 calc R U . . .
C18 C 0.4865(3) 0.5689(4) 0.7039(4) 0.051(2) Uani 1 1 d D U . . .
H18A H 0.488052 0.609947 0.696187 0.061 Uiso 1 1 calc R U . . .
H18B H 0.480995 0.561643 0.741530 0.061 Uiso 1 1 calc R U . . .
C16 C 0.4264(4) 0.4490(4) 0.6828(4) 0.050(2) Uani 1 1 d D U . . .
H16A H 0.416404 0.435155 0.719202 0.060 Uiso 1 1 calc R U . . .
H16B H 0.391549 0.416194 0.661138 0.060 Uiso 1 1 calc R U . . .
C17 C 0.4292(4) 0.5140(4) 0.6759(4) 0.054(2) Uani 1 1 d D U . . .
H17A H 0.432127 0.524181 0.638732 0.065 Uiso 1 1 calc R U . . .
H17B H 0.389005 0.510460 0.689220 0.065 Uiso 1 1 calc R U . . .
C15 C 0.4905(3) 0.4535(4) 0.6678(3) 0.0417(18) Uani 1 1 d D U . . .
H15 H 0.497924 0.465611 0.630596 0.050 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C11 1.280(6) . ?
O1 C12 1.289(6) . ?
O4 C13 1.277(7) . ?
N1 C11 1.3900 . ?
N1 C12 1.3900 . ?
N1 C20 1.504(8) 2_655 ?
C11 C10 1.3900 . ?
C10 C9 1.3900 . ?
C10 C1 1.419(8) . ?
C9 C8 1.3900 . ?
C9 C4 1.491(4) . ?
C8 C12 1.3900 . ?
C8 C7 1.418(8) . ?
O3 C14 1.245(6) . ?
C7 H7 0.9500 . ?
C7 C6 1.410(11) . ?
N2 C13 1.3900 . ?
N2 C14 1.3900 . ?
N2 C15 1.507(9) . ?
C13 C5 1.3900 . ?
C5 C4 1.3900 . ?
C5 C6 1.400(9) . ?
C4 C3 1.3900 . ?
C3 C14 1.3900 . ?
C3 C2 1.437(9) . ?
C1 H1 0.9500 . ?
C1 C2 1.384(12) . ?
C2 H2 0.9500 . ?
C20 H20 1.0000 . ?
C20 C19 1.542(7) . ?
C20 C15 1.533(7) . ?
C6 H6 0.9500 . ?
C29 H29 0.9500 . ?
C29 C28 1.409(11) . ?
C29 C30 1.398(10) . ?
C28 H28 0.9500 . ?
C28 C27 1.393(11) . ?
C27 H27 0.9500 . ?
C27 C26 1.406(10) . ?
C26 C25 1.3900 . ?
C26 C21 1.3900 . ?
C25 H25 0.9500 . ?
C25 C24 1.3900 . ?
C24 H24 0.9500 . ?
C24 C23 1.3900 . ?
C23 H23 0.9500 . ?
C23 C22 1.3900 . ?
C22 C22 1.484(10) 12_556 ?
C22 C21 1.3900 . ?
C21 C30 1.418(8) . ?
C30 C30 1.518(17) 12_556 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C18 1.531(8) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C17 1.533(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.541(7) . ?
C16 C15 1.539(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C15 H15 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
C11 N1 C12 120.0 . . ?
C11 N1 C20 121.1(4) . 2_655 ?
C12 N1 C20 118.8(4) . 2_655 ?
O2 C11 N1 117.0(4) . . ?
O2 C11 C10 122.2(4) . . ?
C10 C11 N1 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 C1 121.4(5) . . ?
C9 C10 C1 118.6(5) . . ?
C10 C9 C4 119.9(3) . . ?
C8 C9 C10 120.0 . . ?
C8 C9 C4 120.1(3) . . ?
C9 C8 C7 118.1(4) . . ?
C12 C8 C9 120.0 . . ?
C12 C8 C7 121.7(4) . . ?
O1 C12 N1 117.9(4) . . ?
O1 C12 C8 122.0(4) . . ?
C8 C12 N1 120.0 . . ?
C8 C7 H7 119.1 . . ?
C6 C7 C8 121.9(7) . . ?
C6 C7 H7 119.1 . . ?
C13 N2 C14 120.0 . . ?
C13 N2 C15 121.6(4) . . ?
C14 N2 C15 118.4(4) . . ?
O4 C13 N2 117.9(4) . . ?
O4 C13 C5 122.0(4) . . ?
N2 C13 C5 120.0 . . ?
C13 C5 C4 120.0 . . ?
C13 C5 C6 120.3(4) . . ?
C4 C5 C6 119.6(4) . . ?
C5 C4 C9 119.5(4) . . ?
C3 C4 C9 120.5(4) . . ?
C3 C4 C5 120.0 . . ?
C4 C3 C14 120.0 . . ?
C4 C3 C2 117.3(5) . . ?
C14 C3 C2 122.7(5) . . ?
O3 C14 N2 115.6(5) . . ?
O3 C14 C3 124.2(5) . . ?
C3 C14 N2 120.0 . . ?
C10 C1 H1 119.3 . . ?
C2 C1 C10 121.4(7) . . ?
C2 C1 H1 119.3 . . ?
C3 C2 H2 118.9 . . ?
C1 C2 C3 122.2(7) . . ?
C1 C2 H2 118.9 . . ?
N1 C20 H20 105.8 3_665 . ?
N1 C20 C19 112.5(5) 3_665 . ?
N1 C20 C15 114.5(6) 3_665 . ?
C19 C20 H20 105.8 . . ?
C15 C20 H20 105.8 . . ?
C15 C20 C19 111.6(6) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 C7 120.7(7) . . ?
C5 C6 H6 119.7 . . ?
C28 C29 H29 121.3 . . ?
C30 C29 H29 121.3 . . ?
C30 C29 C28 117.3(10) . . ?
C29 C28 H28 119.0 . . ?
C27 C28 C29 121.9(11) . . ?
C27 C28 H28 119.0 . . ?
C28 C27 H27 120.9 . . ?
C28 C27 C26 118.2(9) . . ?
C26 C27 H27 120.9 . . ?
C25 C26 C27 117.5(6) . . ?
C25 C26 C21 120.0 . . ?
C21 C26 C27 122.5(6) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C24 H24 120.0 . . ?
C25 C24 C23 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C22 C22 120.8 . 12_556 ?
C23 C22 C21 120.0 . . ?
C21 C22 C22 119.2 . 12_556 ?
C26 C21 C30 117.0(5) . . ?
C22 C21 C26 120.0 . . ?
C22 C21 C30 123.0(5) . . ?
C29 C30 C21 122.8(8) . . ?
C29 C30 C30 119.5(5) . 12_556 ?
C21 C30 C30 117.8(4) . 12_556 ?
C20 C19 H19A 110.0 . . ?
C20 C19 H19B 110.0 . . ?
H19A C19 H19B 108.4 . . ?
C18 C19 C20 108.5(6) . . ?
C18 C19 H19A 110.0 . . ?
C18 C19 H19B 110.0 . . ?
C19 C18 H18A 109.4 . . ?
C19 C18 H18B 109.4 . . ?
C19 C18 C17 111.0(8) . . ?
H18A C18 H18B 108.0 . . ?
C17 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C15 C16 C17 111.3(7) . . ?
C18 C17 C16 112.5(7) . . ?
C18 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C16 C17 H17A 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
N2 C15 C20 113.3(5) . . ?
N2 C15 C16 112.5(6) . . ?
N2 C15 H15 107.0 . . ?
C20 C15 C16 109.5(7) . . ?
C20 C15 H15 107.0 . . ?
C16 C15 H15 107.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C11 C10 C9 169.1(6) . . . . ?
O2 C11 C10 C1 -13.3(6) . . . . ?
O4 C13 C5 C4 -177.3(6) . . . . ?
O4 C13 C5 C6 5.5(6) . . . . ?
N1 C11 C10 C9 0.0 . . . . ?
N1 C11 C10 C1 177.6(6) . . . . ?
N1 C20 C19 C18 -169.0(7) 3_665 . . . ?
N1 C20 C15 N2 45.1(8) 3_665 . . . ?
N1 C20 C15 C16 171.6(6) 3_665 . . . ?
C11 N1 C12 O1 177.0(5) . . . . ?
C11 N1 C12 C8 0.0 . . . . ?
C11 C10 C9 C8 0.0 . . . . ?
C11 C10 C9 C4 -179.0(5) . . . . ?
C11 C10 C1 C2 179.1(6) . . . . ?
C10 C9 C8 C12 0.0 . . . . ?
C10 C9 C8 C7 -174.6(5) . . . . ?
C10 C9 C4 C5 177.8(3) . . . . ?
C10 C9 C4 C3 -1.4(6) . . . . ?
C10 C1 C2 C3 1.1(13) . . . . ?
C9 C10 C1 C2 -3.2(10) . . . . ?
C9 C8 C12 O1 -176.8(5) . . . . ?
C9 C8 C12 N1 0.0 . . . . ?
C9 C8 C7 C6 -4.6(9) . . . . ?
C9 C4 C3 C14 179.2(5) . . . . ?
C9 C4 C3 C2 -0.7(6) . . . . ?
C8 C9 C4 C5 -1.2(6) . . . . ?
C8 C9 C4 C3 179.6(3) . . . . ?
C8 C7 C6 C5 1.5(12) . . . . ?
C12 N1 C11 O2 -169.7(5) . . . . ?
C12 N1 C11 C10 0.0 . . . . ?
C12 C8 C7 C6 -179.1(6) . . . . ?
C7 C8 C12 O1 -2.5(6) . . . . ?
C7 C8 C12 N1 174.4(6) . . . . ?
N2 C13 C5 C4 0.0 . . . . ?
N2 C13 C5 C6 -177.1(6) . . . . ?
C13 N2 C14 O3 174.6(6) . . . . ?
C13 N2 C14 C3 0.0 . . . . ?
C13 N2 C15 C20 57.3(7) . . . . ?
C13 N2 C15 C16 -67.7(7) . . . . ?
C13 C5 C4 C9 -179.2(5) . . . . ?
C13 C5 C4 C3 0.0 . . . . ?
C13 C5 C6 C7 179.1(6) . . . . ?
C5 C4 C3 C14 0.0 . . . . ?
C5 C4 C3 C2 -179.9(6) . . . . ?
C4 C9 C8 C12 179.0(5) . . . . ?
C4 C9 C8 C7 4.4(6) . . . . ?
C4 C5 C6 C7 1.9(10) . . . . ?
C4 C3 C14 O3 -174.1(6) . . . . ?
C4 C3 C14 N2 0.0 . . . . ?
C4 C3 C2 C1 0.9(10) . . . . ?
C14 N2 C13 O4 177.4(5) . . . . ?
C14 N2 C13 C5 0.0 . . . . ?
C14 N2 C15 C20 -120.3(6) . . . . ?
C14 N2 C15 C16 114.7(6) . . . . ?
C14 C3 C2 C1 -179.0(6) . . . . ?
C1 C10 C9 C8 -177.7(6) . . . . ?
C1 C10 C9 C4 3.3(6) . . . . ?
C2 C3 C14 O3 5.7(7) . . . . ?
C2 C3 C14 N2 179.9(6) . . . . ?
C20 N1 C11 O2 14.4(6) 2_655 . . . ?
C20 N1 C11 C10 -176.0(5) 2_655 . . . ?
C20 N1 C12 O1 -7.0(6) 2_655 . . . ?
C20 N1 C12 C8 176.1(5) 2_655 . . . ?
C20 C19 C18 C17 -57.4(10) . . . . ?
C6 C5 C4 C9 -2.0(6) . . . . ?
C6 C5 C4 C3 177.2(6) . . . . ?
C29 C28 C27 C26 -5.9(15) . . . . ?
C28 C29 C30 C21 -0.9(13) . . . . ?
C28 C29 C30 C30 177.9(9) . . . 12_556 ?
C28 C27 C26 C25 -177.0(8) . . . . ?
C28 C27 C26 C21 3.4(12) . . . . ?
C27 C26 C25 C24 -179.6(7) . . . . ?
C27 C26 C21 C22 179.6(8) . . . . ?
C27 C26 C21 C30 0.1(8) . . . . ?
C26 C25 C24 C23 0.0 . . . . ?
C26 C21 C30 C29 -1.4(10) . . . . ?
C26 C21 C30 C30 179.8(7) . . . 12_556 ?
C25 C26 C21 C22 0.0 . . . . ?
C25 C26 C21 C30 -179.5(6) . . . . ?
C25 C24 C23 C22 0.0 . . . . ?
C24 C23 C22 C22 177.6(10) . . . 12_556 ?
C24 C23 C22 C21 0.0 . . . . ?
C23 C22 C21 C26 0.0 . . . . ?
C23 C22 C21 C30 179.5(7) . . . . ?
C22 C22 C21 C26 -177.6(10) 12_556 . . . ?
C22 C22 C21 C30 1.8(9) 12_556 . . . ?
C22 C21 C30 C29 179.1(6) . . . . ?
C22 C21 C30 C30 0.3(12) . . . 12_556 ?
C21 C26 C25 C24 0.0 . . . . ?
C30 C29 C28 C27 4.6(15) . . . . ?
C19 C20 C15 N2 174.2(7) . . . . ?
C19 C20 C15 C16 -59.2(9) . . . . ?
C19 C18 C17 C16 54.9(11) . . . . ?
C17 C16 C15 N2 -178.8(7) . . . . ?
C17 C16 C15 C20 54.2(9) . . . . ?
C15 N2 C13 O4 -0.2(6) . . . . ?
C15 N2 C13 C5 -177.6(5) . . . . ?
C15 N2 C14 O3 -7.7(6) . . . . ?
C15 N2 C14 C3 177.7(5) . . . . ?
C15 C20 C19 C18 60.8(10) . . . . ?
C15 C16 C17 C18 -53.0(11) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.272 -0.608 -0.465 4623.6 1612.5 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_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 2.568
_oxdiff_exptl_absorpt_empirical_full_min 0.432
