# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1b
_database_code_depnum_ccdc_archive 'CCDC 2133054'
loop_
_audit_author_name
_audit_author_address
'Tadashi Hyodo'
;Tokushima Bunri University
Japan
;
_audit_update_record             
;
2022-01-07 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H48 Br4 N4 O8'
_chemical_formula_weight         1128.54

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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   14.5014(16)
_cell_length_b                   13.1843(15)
_cell_length_c                   24.596(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.374(4)
_cell_angle_gamma                90
_cell_volume                     4639.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9742
_cell_measurement_theta_min      3.61
_cell_measurement_theta_max      78.44

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_F_000             2272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.713
_shelx_estimated_absorpt_T_min   0.602
_shelx_estimated_absorpt_T_max   0.798
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6889
_exptl_absorpt_correction_T_max  0.8416
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            62659
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.089
_diffrn_reflns_theta_max         79.793
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9721
_reflns_number_gt                8711
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (Hübschle et al., 2011)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0772P)²+8.4719P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9721
_refine_ls_number_parameters     614
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.1421
_refine_ls_wR_factor_gt          0.1389
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1B C 0.8324(5) 0.7920(6) 0.5251(3) 0.0338(15) Uani 0.752(11) 1 d . . P A -1
H1BA H 0.768648 0.793933 0.534635 0.041 Uiso 0.752(11) 1 calc R U P A -1
H1BB H 0.838089 0.848550 0.499427 0.041 Uiso 0.752(11) 1 calc R U P A -1
C2B C 0.8466(3) 0.6931(3) 0.4974(2) 0.0328(13) Uani 0.752(11) 1 d . . P A -1
H2BA H 0.845364 0.636319 0.523624 0.039 Uiso 0.752(11) 1 calc R U P A -1
H2BB H 0.907936 0.692906 0.484695 0.039 Uiso 0.752(11) 1 calc R U P A -1
Br1B Br 0.74622(19) 0.6776(3) 0.43489(11) 0.0427(4) Uani 0.752(11) 1 d . . P A
-1
Br2B Br 0.92510(14) 0.8098(2) 0.59272(11) 0.0380(4) Uani 0.752(11) 1 d . . P A
-1
C1C C 0.8845(11) 0.7188(11) 0.5330(7) 0.039(4) Uani 0.248(11) 1 d . . P A -2
H1CA H 0.934156 0.707580 0.510372 0.046 Uiso 0.248(11) 1 calc R U P A -2
H1CB H 0.859119 0.652011 0.541509 0.046 Uiso 0.248(11) 1 calc R U P A -2
C2C C 0.8106(17) 0.7811(19) 0.5029(10) 0.045(6) Uani 0.248(11) 1 d . . P A -2
H2CA H 0.837903 0.844760 0.491205 0.054 Uiso 0.248(11) 1 calc R U P A -2
H2CB H 0.765554 0.799282 0.527552 0.054 Uiso 0.248(11) 1 calc R U P A -2
Br1C Br 0.7425(5) 0.7079(6) 0.4358(3) 0.0345(10) Uani 0.248(11) 1 d . . P A -2
Br2C Br 0.9322(6) 0.7844(7) 0.5964(3) 0.0430(12) Uani 0.248(11) 1 d . . P A -2
C1 C 0.97996(17) 0.2464(2) 0.67189(10) 0.0195(5) Uani 1 1 d . . . . .
C2 C 1.0340(2) 0.2626(2) 0.73055(12) 0.0271(6) Uani 1 1 d . . . . .
H2A H 1.002623 0.225442 0.757368 0.032 Uiso 1 1 calc R U . . .
H2AB H 1.098235 0.235693 0.732975 0.032 Uiso 1 1 calc R U . . .
C3 C 1.0379(2) 0.3762(3) 0.74464(13) 0.0298(6) Uani 1 1 d . . . . .
H3 H 1.073041 0.386098 0.782746 0.036 Uiso 1 1 calc R U . . .
C4 C 1.0872(2) 0.4337(3) 0.70348(14) 0.0322(7) Uani 1 1 d . . . . .
H4A H 1.151960 0.408411 0.705617 0.039 Uiso 1 1 calc R U . . .
H4AB H 1.089983 0.506915 0.712598 0.039 Uiso 1 1 calc R U . . .
C5 C 1.03332(19) 0.4181(2) 0.64508(12) 0.0254(6) Uani 1 1 d . . . . .
H5 H 1.065594 0.455338 0.618130 0.031 Uiso 1 1 calc R U . . .
C6 C 0.93332(19) 0.4593(2) 0.64196(12) 0.0232(5) Uani 1 1 d . . . . .
H6A H 0.935505 0.532604 0.650760 0.028 Uiso 1 1 calc R U . . .
H6AB H 0.898569 0.450549 0.604138 0.028 Uiso 1 1 calc R U . . .
C7 C 0.88312(18) 0.4022(2) 0.68294(11) 0.0205(5) Uani 1 1 d . . . . .
C8 C 0.88084(17) 0.2884(2) 0.66932(10) 0.0181(5) Uani 1 1 d . . . . .
H8A H 0.848771 0.251436 0.695875 0.022 Uiso 1 1 calc R U . . .
H8AB H 0.845020 0.277593 0.631935 0.022 Uiso 1 1 calc R U . . .
C9 C 1.02931(18) 0.3048(2) 0.63100(12) 0.0223(6) Uani 1 1 d . . . . .
H9A H 1.093528 0.278278 0.632452 0.027 Uiso 1 1 calc R U . . .
H9AB H 0.995135 0.294948 0.593122 0.027 Uiso 1 1 calc R U . . .
C10 C 0.9381(2) 0.4173(3) 0.74154(12) 0.0283(6) Uani 1 1 d . . . . .
H10A H 0.940345 0.490396 0.750966 0.034 Uiso 1 1 calc R U . . .
H10B H 0.906146 0.381261 0.768495 0.034 Uiso 1 1 calc R U . . .
C11 C 0.78377(19) 0.4439(2) 0.68213(11) 0.0250(6) Uani 1 1 d . . . . .
H11A H 0.758106 0.415489 0.713799 0.030 Uiso 1 1 calc R U . . .
H11B H 0.787015 0.518503 0.686601 0.030 Uiso 1 1 calc R U . . .
C12 C 0.70505(17) 0.4795(2) 0.58414(11) 0.0207(5) Uani 1 1 d . . . . .
C13 C 0.63585(17) 0.4236(2) 0.54302(11) 0.0178(5) Uani 1 1 d . . . . .
C14 C 0.59924(18) 0.4491(2) 0.48891(11) 0.0186(5) Uani 1 1 d . . . . .
H14 H 0.618087 0.507868 0.471226 0.022 Uiso 1 1 calc R U . . .
C15 C 0.53283(17) 0.38151(19) 0.46286(10) 0.0162(5) Uani 1 1 d . . . . .
C16 C 0.47619(18) 0.38532(19) 0.40629(10) 0.0171(5) Uani 1 1 d . . . . .
C17 C 0.43134(17) 0.24320(19) 0.45020(10) 0.0154(5) Uani 1 1 d . . . . .
C18 C 0.50562(17) 0.2955(2) 0.48930(10) 0.0163(5) Uani 1 1 d . . . . .
C19 C 0.54269(17) 0.2692(2) 0.54314(10) 0.0179(5) Uani 1 1 d . . . . .
H19 H 0.524228 0.210234 0.560771 0.022 Uiso 1 1 calc R U . . .
C20 C 0.60916(17) 0.3370(2) 0.56880(10) 0.0181(5) Uani 1 1 d . . . . .
C21 C 0.66262(17) 0.3333(2) 0.62576(11) 0.0203(5) Uani 1 1 d . . . . .
C22 C 0.35500(17) 0.2678(2) 0.35234(10) 0.0175(5) Uani 1 1 d . . . . .
H22A H 0.327951 0.329420 0.332957 0.021 Uiso 1 1 calc R U . . .
H22B H 0.303317 0.229290 0.364406 0.021 Uiso 1 1 calc R U . . .
C23 C 0.39957(17) 0.20258(19) 0.31211(10) 0.0145(5) Uani 1 1 d . . . . .
C24 C 0.32124(18) 0.1614(2) 0.26774(10) 0.0196(5) Uani 1 1 d . . . . .
H24A H 0.277874 0.119217 0.285287 0.024 Uiso 1 1 calc R U . . .
H24B H 0.285326 0.218685 0.248734 0.024 Uiso 1 1 calc R U . . .
C25 C 0.36340(19) 0.0976(2) 0.22571(11) 0.0220(5) Uani 1 1 d . . . . .
H25 H 0.312015 0.070988 0.197210 0.026 Uiso 1 1 calc R U . . .
C26 C 0.41817(18) 0.0081(2) 0.25548(11) 0.0200(5) Uani 1 1 d . . . . .
H26A H 0.375552 -0.034894 0.273172 0.024 Uiso 1 1 calc R U . . .
H26B H 0.444637 -0.034029 0.228460 0.024 Uiso 1 1 calc R U . . .
C27 C 0.49753(17) 0.04825(19) 0.29942(10) 0.0153(5) Uani 1 1 d . . . . .
C28 C 0.56222(18) 0.1153(2) 0.27082(11) 0.0191(5) Uani 1 1 d . . . . .
H28A H 0.614057 0.141248 0.298536 0.023 Uiso 1 1 calc R U . . .
H28B H 0.589514 0.074273 0.243696 0.023 Uiso 1 1 calc R U . . .
C29 C 0.5078(2) 0.2042(2) 0.24159(11) 0.0208(5) Uani 1 1 d . . . . .
H29 H 0.550805 0.247569 0.223638 0.025 Uiso 1 1 calc R U . . .
C30 C 0.46680(18) 0.2669(2) 0.28442(10) 0.0175(5) Uani 1 1 d . . . . .
H30A H 0.433010 0.326247 0.266234 0.021 Uiso 1 1 calc R U . . .
H30B H 0.518073 0.292316 0.312697 0.021 Uiso 1 1 calc R U . . .
C31 C 0.4289(2) 0.1640(2) 0.19778(11) 0.0247(6) Uani 1 1 d . . . . .
H31A H 0.455498 0.123656 0.170125 0.030 Uiso 1 1 calc R U . . .
H31B H 0.393566 0.221493 0.178604 0.030 Uiso 1 1 calc R U . . .
C32 C 0.45356(17) 0.11235(18) 0.34092(10) 0.0141(4) Uani 1 1 d . . . . .
H32A H 0.410615 0.069541 0.358465 0.017 Uiso 1 1 calc R U . . .
H32B H 0.503366 0.137475 0.370189 0.017 Uiso 1 1 calc R U . . .
C33 C 0.55148(19) -0.0426(2) 0.32789(11) 0.0208(5) Uani 1 1 d . . . . .
H33A H 0.506109 -0.091776 0.338627 0.025 Uiso 1 1 calc R U . . .
H33B H 0.585330 -0.076597 0.301153 0.025 Uiso 1 1 calc R U . . .
C34 C 0.59416(18) -0.01480(19) 0.42972(10) 0.0174(5) Uani 1 1 d . . . . .
C35 C 0.67963(17) 0.01694(19) 0.46806(11) 0.0168(5) Uani 1 1 d . . . . .
C36 C 0.69180(17) 0.0305(2) 0.52482(11) 0.0175(5) Uani 1 1 d . . . . .
H36 H 0.642624 0.022166 0.545662 0.021 Uiso 1 1 calc R U . . .
C37 C 0.78251(17) 0.05725(19) 0.54851(10) 0.0170(5) Uani 1 1 d . . . . .
C38 C 0.82153(18) 0.0744(2) 0.60779(11) 0.0193(5) Uani 1 1 d . . . . .
C39 C 0.94023(17) 0.0998(2) 0.55648(11) 0.0186(5) Uani 1 1 d . . . . .
C40 C 0.85399(17) 0.07071(19) 0.51764(11) 0.0170(5) Uani 1 1 d . . . . .
C41 C 0.84159(17) 0.0569(2) 0.46108(11) 0.0184(5) Uani 1 1 d . . . . .
H41 H 0.890766 0.065507 0.440262 0.022 Uiso 1 1 calc R U . . .
C42 C 0.75145(17) 0.0295(2) 0.43716(10) 0.0179(5) Uani 1 1 d . . . . .
C43 C 0.71308(18) 0.0058(2) 0.37829(11) 0.0208(5) Uani 1 1 d . . . . .
C44 C 0.97734(19) 0.1320(2) 0.65942(11) 0.0217(5) Uani 1 1 d . . . . .
H44A H 1.041370 0.108882 0.656639 0.026 Uiso 1 1 calc R U . . .
H44B H 0.957167 0.095510 0.690658 0.026 Uiso 1 1 calc R U . . .
N1 N 0.72028(15) 0.41939(19) 0.63111(9) 0.0207(5) Uani 1 1 d . . . . .
N2 N 0.42151(15) 0.29820(16) 0.40098(9) 0.0159(4) Uani 1 1 d . . . . .
N3 N 0.61861(15) -0.01564(17) 0.37686(9) 0.0180(4) Uani 1 1 d . . . . .
N4 N 0.91479(15) 0.10441(18) 0.60857(9) 0.0191(4) Uani 1 1 d . . . . .
O1 O 0.65923(13) 0.27046(18) 0.66102(8) 0.0262(4) Uani 1 1 d . . . . .
O2 O 0.74014(14) 0.56167(15) 0.57892(9) 0.0259(4) Uani 1 1 d . . . . .
O3 O 0.47489(14) 0.45149(14) 0.37200(8) 0.0227(4) Uani 1 1 d . . . . .
O4 O 0.38574(13) 0.16980(15) 0.45833(8) 0.0209(4) Uani 1 1 d . . . . .
O5 O 0.51804(13) -0.03692(15) 0.44001(8) 0.0218(4) Uani 1 1 d . . . . .
O6 O 0.75417(14) 0.00457(19) 0.33926(8) 0.0303(5) Uani 1 1 d . . . . .
O7 O 1.01766(13) 0.11591(16) 0.54602(8) 0.0251(4) Uani 1 1 d . . . . .
O8 O 0.78424(14) 0.06324(17) 0.64754(8) 0.0265(4) Uani 1 1 d . . . . .
C1A C 0.7833(5) 0.3603(7) 0.4121(3) 0.096(2) Uani 1 1 d . . . . .
H1AA H 0.724751 0.321818 0.412269 0.115 Uiso 1 1 calc R U . . .
H1AB H 0.766345 0.430209 0.399652 0.115 Uiso 1 1 calc R U . . .
C2A C 0.8330(4) 0.3160(4) 0.3760(2) 0.0667(13) Uani 1 1 d . . . . .
H2AA H 0.849902 0.246045 0.388402 0.080 Uiso 1 1 calc R U . . .
H2AC H 0.891646 0.354410 0.375868 0.080 Uiso 1 1 calc R U . . .
Br1A Br 0.85383(4) 0.36453(5) 0.48656(2) 0.07197(19) Uani 1 1 d . . . . .
Br2A Br 0.76119(3) 0.31195(3) 0.30011(2) 0.04370(12) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1B C2B 1.500(9) . ?
C1B Br2B 1.974(7) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C2B Br1B 1.949(6) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C1C C2C 1.45(3) . ?
C1C Br2C 1.820(19) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C2C Br1C 2.03(3) . ?
C2C H2CA 0.9900 . ?
C2C H2CB 0.9900 . ?
C1 C8 1.532(3) . ?
C1 C9 1.533(4) . ?
C1 C44 1.540(4) . ?
C1 C2 1.540(4) . ?
C2 C3 1.536(5) . ?
C2 H2A 0.9900 . ?
C2 H2AB 0.9900 . ?
C3 C4 1.532(5) . ?
C3 C10 1.536(4) . ?
C3 H3 1.0000 . ?
C4 C5 1.533(4) . ?
C4 H4A 0.9900 . ?
C4 H4AB 0.9900 . ?
C5 C9 1.532(4) . ?
C5 C6 1.538(4) . ?
C5 H5 1.0000 . ?
C6 C7 1.533(4) . ?
C6 H6A 0.9900 . ?
C6 H6AB 0.9900 . ?
C7 C8 1.536(4) . ?
C7 C11 1.539(4) . ?
C7 C10 1.542(4) . ?
C8 H8A 0.9900 . ?
C8 H8AB 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9AB 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N1 1.466(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O2 1.213(4) . ?
C12 N1 1.388(4) . ?
C12 C13 1.497(3) . ?
C13 C14 1.391(4) . ?
C13 C20 1.392(4) . ?
C14 C15 1.390(4) . ?
C14 H14 0.9500 . ?
C15 C18 1.395(4) . ?
C15 C16 1.497(4) . ?
C16 O3 1.211(3) . ?
C16 N2 1.390(3) . ?
C17 O4 1.207(3) . ?
C17 N2 1.398(3) . ?
C17 C18 1.491(3) . ?
C18 C19 1.390(4) . ?
C19 C20 1.388(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.487(4) . ?
C21 O1 1.206(4) . ?
C21 N1 1.403(4) . ?
C22 N2 1.465(3) . ?
C22 C23 1.531(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C32 1.533(3) . ?
C23 C30 1.533(3) . ?
C23 C24 1.540(3) . ?
C24 C25 1.535(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C31 1.534(4) . ?
C25 C26 1.540(4) . ?
C25 H25 1.0000 . ?
C26 C27 1.539(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C33 1.535(4) . ?
C27 C28 1.540(3) . ?
C27 C32 1.541(3) . ?
C28 C29 1.527(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C31 1.533(4) . ?
C29 C30 1.533(3) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 N3 1.464(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 O5 1.208(3) . ?
C34 N3 1.402(3) . ?
C34 C35 1.490(3) . ?
C35 C36 1.390(4) . ?
C35 C42 1.396(4) . ?
C36 C37 1.395(4) . ?
C36 H36 0.9500 . ?
C37 C40 1.392(3) . ?
C37 C38 1.493(4) . ?
C38 O8 1.201(3) . ?
C38 N4 1.406(3) . ?
C39 O7 1.211(3) . ?
C39 N4 1.391(3) . ?
C39 C40 1.495(3) . ?
C40 C41 1.386(4) . ?
C41 C42 1.391(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.497(4) . ?
C43 O6 1.210(3) . ?
C43 N3 1.394(3) . ?
C44 N4 1.466(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C1A C2A 1.361(9) . ?
C1A Br1A 1.948(7) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C2A Br2A 1.985(5) . ?
C2A H2AA 0.9900 . ?
C2A H2AC 0.9900 . ?

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
C2B C1B Br2B 111.1(5) . . ?
C2B C1B H1BA 109.4 . . ?
Br2B C1B H1BA 109.4 . . ?
C2B C1B H1BB 109.4 . . ?
Br2B C1B H1BB 109.4 . . ?
H1BA C1B H1BB 108.0 . . ?
C1B C2B Br1B 108.0(4) . . ?
C1B C2B H2BA 110.1 . . ?
Br1B C2B H2BA 110.1 . . ?
C1B C2B H2BB 110.1 . . ?
Br1B C2B H2BB 110.1 . . ?
H2BA C2B H2BB 108.4 . . ?
C2C C1C Br2C 108.3(15) . . ?
C2C C1C H1CA 110.0 . . ?
Br2C C1C H1CA 110.0 . . ?
C2C C1C H1CB 110.0 . . ?
Br2C C1C H1CB 110.0 . . ?
H1CA C1C H1CB 108.4 . . ?
C1C C2C Br1C 111.5(16) . . ?
C1C C2C H2CA 109.3 . . ?
Br1C C2C H2CA 109.3 . . ?
C1C C2C H2CB 109.3 . . ?
Br1C C2C H2CB 109.3 . . ?
H2CA C2C H2CB 108.0 . . ?
C8 C1 C9 109.1(2) . . ?
C8 C1 C44 110.7(2) . . ?
C9 C1 C44 111.1(2) . . ?
C8 C1 C2 108.6(2) . . ?
C9 C1 C2 108.9(2) . . ?
C44 C1 C2 108.4(2) . . ?
C3 C2 C1 109.9(2) . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2AB 109.7 . . ?
C1 C2 H2AB 109.7 . . ?
H2A C2 H2AB 108.2 . . ?
C4 C3 C10 109.3(3) . . ?
C4 C3 C2 109.7(3) . . ?
C10 C3 C2 109.5(2) . . ?
C4 C3 H3 109.5 . . ?
C10 C3 H3 109.5 . . ?
C2 C3 H3 109.5 . . ?
C3 C4 C5 109.3(2) . . ?
C3 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
C3 C4 H4AB 109.8 . . ?
C5 C4 H4AB 109.8 . . ?
H4A C4 H4AB 108.3 . . ?
C9 C5 C4 109.7(2) . . ?
C9 C5 C6 109.4(2) . . ?
C4 C5 C6 109.4(2) . . ?
C9 C5 H5 109.5 . . ?
C4 C5 H5 109.5 . . ?
C6 C5 H5 109.5 . . ?
C7 C6 C5 109.8(2) . . ?
C7 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C7 C6 H6AB 109.7 . . ?
C5 C6 H6AB 109.7 . . ?
H6A C6 H6AB 108.2 . . ?
C6 C7 C8 109.4(2) . . ?
C6 C7 C11 111.1(2) . . ?
C8 C7 C11 111.0(2) . . ?
C6 C7 C10 108.8(2) . . ?
C8 C7 C10 108.6(2) . . ?
C11 C7 C10 107.8(2) . . ?
C1 C8 C7 110.9(2) . . ?
C1 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C1 C8 H8AB 109.5 . . ?
C7 C8 H8AB 109.5 . . ?
H8A C8 H8AB 108.0 . . ?
C5 C9 C1 110.2(2) . . ?
C5 C9 H9A 109.6 . . ?
C1 C9 H9A 109.6 . . ?
C5 C9 H9AB 109.6 . . ?
C1 C9 H9AB 109.6 . . ?
H9A C9 H9AB 108.1 . . ?
C3 C10 C7 109.9(2) . . ?
C3 C10 H10A 109.7 . . ?
C7 C10 H10A 109.7 . . ?
C3 C10 H10B 109.7 . . ?
C7 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
N1 C11 C7 112.9(2) . . ?
N1 C11 H11A 109.0 . . ?
C7 C11 H11A 109.0 . . ?
N1 C11 H11B 109.0 . . ?
C7 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
O2 C12 N1 125.8(3) . . ?
O2 C12 C13 127.9(3) . . ?
N1 C12 C13 106.3(2) . . ?
C14 C13 C20 122.9(2) . . ?
C14 C13 C12 129.6(3) . . ?
C20 C13 C12 107.5(2) . . ?
C15 C14 C13 114.5(2) . . ?
C15 C14 H14 122.8 . . ?
C13 C14 H14 122.8 . . ?
C14 C15 C18 122.2(2) . . ?
C14 C15 C16 129.9(2) . . ?
C18 C15 C16 107.8(2) . . ?
O3 C16 N2 125.9(2) . . ?
O3 C16 C15 128.0(2) . . ?
N2 C16 C15 106.1(2) . . ?
O4 C17 N2 125.3(2) . . ?
O4 C17 C18 128.5(2) . . ?
N2 C17 C18 106.2(2) . . ?
C19 C18 C15 123.5(2) . . ?
C19 C18 C17 128.7(2) . . ?
C15 C18 C17 107.7(2) . . ?
C20 C19 C18 113.9(2) . . ?
C20 C19 H19 123.1 . . ?
C18 C19 H19 123.1 . . ?
C19 C20 C13 123.0(2) . . ?
C19 C20 C21 128.6(3) . . ?
C13 C20 C21 108.4(2) . . ?
O1 C21 N1 125.6(2) . . ?
O1 C21 C20 128.6(3) . . ?
N1 C21 C20 105.8(2) . . ?
N2 C22 C23 113.0(2) . . ?
N2 C22 H22A 109.0 . . ?
C23 C22 H22A 109.0 . . ?
N2 C22 H22B 109.0 . . ?
C23 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C22 C23 C32 112.0(2) . . ?
C22 C23 C30 110.0(2) . . ?
C32 C23 C30 108.7(2) . . ?
C22 C23 C24 108.4(2) . . ?
C32 C23 C24 108.5(2) . . ?
C30 C23 C24 109.2(2) . . ?
C25 C24 C23 110.0(2) . . ?
C25 C24 H24A 109.7 . . ?
C23 C24 H24A 109.7 . . ?
C25 C24 H24B 109.7 . . ?
C23 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
C31 C25 C24 109.4(2) . . ?
C31 C25 C26 110.0(2) . . ?
C24 C25 C26 109.3(2) . . ?
C31 C25 H25 109.4 . . ?
C24 C25 H25 109.4 . . ?
C26 C25 H25 109.4 . . ?
C27 C26 C25 109.8(2) . . ?
C27 C26 H26A 109.7 . . ?
C25 C26 H26A 109.7 . . ?
C27 C26 H26B 109.7 . . ?
C25 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C33 C27 C26 108.6(2) . . ?
C33 C27 C28 110.7(2) . . ?
C26 C27 C28 108.6(2) . . ?
C33 C27 C32 111.1(2) . . ?
C26 C27 C32 108.1(2) . . ?
C28 C27 C32 109.7(2) . . ?
C29 C28 C27 110.5(2) . . ?
C29 C28 H28A 109.6 . . ?
C27 C28 H28A 109.6 . . ?
C29 C28 H28B 109.6 . . ?
C27 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
C28 C29 C31 109.6(2) . . ?
C28 C29 C30 108.6(2) . . ?
C31 C29 C30 109.9(2) . . ?
C28 C29 H29 109.6 . . ?
C31 C29 H29 109.6 . . ?
C30 C29 H29 109.6 . . ?
C29 C30 C23 110.6(2) . . ?
C29 C30 H30A 109.5 . . ?
C23 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C23 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C29 C31 C25 109.2(2) . . ?
C29 C31 H31A 109.8 . . ?
C25 C31 H31A 109.8 . . ?
C29 C31 H31B 109.8 . . ?
C25 C31 H31B 109.8 . . ?
H31A C31 H31B 108.3 . . ?
C23 C32 C27 110.77(19) . . ?
C23 C32 H32A 109.5 . . ?
C27 C32 H32A 109.5 . . ?
C23 C32 H32B 109.5 . . ?
C27 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
N3 C33 C27 114.0(2) . . ?
N3 C33 H33A 108.7 . . ?
C27 C33 H33A 108.7 . . ?
N3 C33 H33B 108.7 . . ?
C27 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
O5 C34 N3 124.8(2) . . ?
O5 C34 C35 129.0(2) . . ?
N3 C34 C35 106.2(2) . . ?
C36 C35 C42 123.2(2) . . ?
C36 C35 C34 128.9(2) . . ?
C42 C35 C34 107.8(2) . . ?
C35 C36 C37 114.1(2) . . ?
C35 C36 H36 122.9 . . ?
C37 C36 H36 122.9 . . ?
C40 C37 C36 122.7(2) . . ?
C40 C37 C38 108.4(2) . . ?
C36 C37 C38 128.9(2) . . ?
O8 C38 N4 125.6(2) . . ?
O8 C38 C37 128.9(2) . . ?
N4 C38 C37 105.5(2) . . ?
O7 C39 N4 125.6(2) . . ?
O7 C39 C40 128.1(2) . . ?
N4 C39 C40 106.3(2) . . ?
C41 C40 C37 123.0(2) . . ?
C41 C40 C39 129.3(2) . . ?
C37 C40 C39 107.7(2) . . ?
C40 C41 C42 114.7(2) . . ?
C40 C41 H41 122.6 . . ?
C42 C41 H41 122.6 . . ?
C41 C42 C35 122.3(2) . . ?
C41 C42 C43 129.7(2) . . ?
C35 C42 C43 108.0(2) . . ?
O6 C43 N3 125.9(3) . . ?
O6 C43 C42 128.1(3) . . ?
N3 C43 C42 106.0(2) . . ?
N4 C44 C1 113.9(2) . . ?
N4 C44 H44A 108.8 . . ?
C1 C44 H44A 108.8 . . ?
N4 C44 H44B 108.8 . . ?
C1 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?
C12 N1 C21 111.8(2) . . ?
C12 N1 C11 125.4(2) . . ?
C21 N1 C11 122.7(2) . . ?
C16 N2 C17 111.8(2) . . ?
C16 N2 C22 126.3(2) . . ?
C17 N2 C22 121.7(2) . . ?
C43 N3 C34 111.8(2) . . ?
C43 N3 C33 126.1(2) . . ?
C34 N3 C33 122.0(2) . . ?
C39 N4 C38 111.9(2) . . ?
C39 N4 C44 125.2(2) . . ?
C38 N4 C44 122.8(2) . . ?
C2A C1A Br1A 111.9(5) . . ?
C2A C1A H1AA 109.2 . . ?
Br1A C1A H1AA 109.2 . . ?
C2A C1A H1AB 109.2 . . ?
Br1A C1A H1AB 109.2 . . ?
H1AA C1A H1AB 107.9 . . ?
C1A C2A Br2A 111.9(4) . . ?
C1A C2A H2AA 109.2 . . ?
Br2A C2A H2AA 109.2 . . ?
C1A C2A H2AC 109.2 . . ?
Br2A C2A H2AC 109.2 . . ?
H2AA C2A H2AC 107.9 . . ?

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
Br2B C1B C2B Br1B 175.5(3) . . . . ?
Br2C C1C C2C Br1C -173.4(9) . . . . ?
C8 C1 C2 C3 -59.5(3) . . . . ?
C9 C1 C2 C3 59.2(3) . . . . ?
C44 C1 C2 C3 -179.8(2) . . . . ?
C1 C2 C3 C4 -59.9(3) . . . . ?
C1 C2 C3 C10 60.1(3) . . . . ?
C10 C3 C4 C5 -60.3(3) . . . . ?
C2 C3 C4 C5 59.7(3) . . . . ?
C3 C4 C5 C9 -59.6(3) . . . . ?
C3 C4 C5 C6 60.4(3) . . . . ?
C9 C5 C6 C7 59.8(3) . . . . ?
C4 C5 C6 C7 -60.4(3) . . . . ?
C5 C6 C7 C8 -58.8(3) . . . . ?
C5 C6 C7 C11 178.2(2) . . . . ?
C5 C6 C7 C10 59.7(3) . . . . ?
C9 C1 C8 C7 -58.6(3) . . . . ?
C44 C1 C8 C7 178.8(2) . . . . ?
C2 C1 C8 C7 59.9(3) . . . . ?
C6 C7 C8 C1 58.8(3) . . . . ?
C11 C7 C8 C1 -178.3(2) . . . . ?
C10 C7 C8 C1 -59.8(3) . . . . ?
C4 C5 C9 C1 59.9(3) . . . . ?
C6 C5 C9 C1 -60.0(3) . . . . ?
C8 C1 C9 C5 59.1(3) . . . . ?
C44 C1 C9 C5 -178.6(2) . . . . ?
C2 C1 C9 C5 -59.3(3) . . . . ?
C4 C3 C10 C7 60.3(3) . . . . ?
C2 C3 C10 C7 -59.9(3) . . . . ?
C6 C7 C10 C3 -59.8(3) . . . . ?
C8 C7 C10 C3 59.2(3) . . . . ?
C11 C7 C10 C3 179.6(3) . . . . ?
C6 C7 C11 N1 69.9(3) . . . . ?
C8 C7 C11 N1 -52.0(3) . . . . ?
C10 C7 C11 N1 -170.9(3) . . . . ?
O2 C12 C13 C14 3.7(4) . . . . ?
N1 C12 C13 C14 -177.8(2) . . . . ?
O2 C12 C13 C20 -174.7(3) . . . . ?
N1 C12 C13 C20 3.8(3) . . . . ?
C20 C13 C14 C15 0.8(4) . . . . ?
C12 C13 C14 C15 -177.4(2) . . . . ?
C13 C14 C15 C18 0.1(4) . . . . ?
C13 C14 C15 C16 177.5(2) . . . . ?
C14 C15 C16 O3 -2.8(4) . . . . ?
C18 C15 C16 O3 174.9(3) . . . . ?
C14 C15 C16 N2 179.3(2) . . . . ?
C18 C15 C16 N2 -3.1(3) . . . . ?
C14 C15 C18 C19 -0.8(4) . . . . ?
C16 C15 C18 C19 -178.7(2) . . . . ?
C14 C15 C18 C17 177.9(2) . . . . ?
C16 C15 C18 C17 0.0(3) . . . . ?
O4 C17 C18 C19 3.5(4) . . . . ?
N2 C17 C18 C19 -178.3(2) . . . . ?
O4 C17 C18 C15 -175.1(2) . . . . ?
N2 C17 C18 C15 3.1(3) . . . . ?
C15 C18 C19 C20 0.6(4) . . . . ?
C17 C18 C19 C20 -177.8(2) . . . . ?
C18 C19 C20 C13 0.3(4) . . . . ?
C18 C19 C20 C21 179.8(2) . . . . ?
C14 C13 C20 C19 -1.0(4) . . . . ?
C12 C13 C20 C19 177.5(2) . . . . ?
C14 C13 C20 C21 179.4(2) . . . . ?
C12 C13 C20 C21 -2.0(3) . . . . ?
C19 C20 C21 O1 0.3(5) . . . . ?
C13 C20 C21 O1 179.8(3) . . . . ?
C19 C20 C21 N1 -179.9(2) . . . . ?
C13 C20 C21 N1 -0.4(3) . . . . ?
N2 C22 C23 C32 51.6(3) . . . . ?
N2 C22 C23 C30 -69.4(3) . . . . ?
N2 C22 C23 C24 171.2(2) . . . . ?
C22 C23 C24 C25 178.6(2) . . . . ?
C32 C23 C24 C25 -59.6(3) . . . . ?
C30 C23 C24 C25 58.8(3) . . . . ?
C23 C24 C25 C31 -60.5(3) . . . . ?
C23 C24 C25 C26 60.0(3) . . . . ?
C31 C25 C26 C27 59.8(3) . . . . ?
C24 C25 C26 C27 -60.3(3) . . . . ?
C25 C26 C27 C33 -179.4(2) . . . . ?
C25 C26 C27 C28 -59.0(3) . . . . ?
C25 C26 C27 C32 59.9(3) . . . . ?
C33 C27 C28 C29 178.8(2) . . . . ?
C26 C27 C28 C29 59.7(3) . . . . ?
C32 C27 C28 C29 -58.2(3) . . . . ?
C27 C28 C29 C31 -60.5(3) . . . . ?
C27 C28 C29 C30 59.6(3) . . . . ?
C28 C29 C30 C23 -61.0(3) . . . . ?
C31 C29 C30 C23 58.8(3) . . . . ?
C22 C23 C30 C29 -176.8(2) . . . . ?
C32 C23 C30 C29 60.2(3) . . . . ?
C24 C23 C30 C29 -57.9(3) . . . . ?
C28 C29 C31 C25 59.7(3) . . . . ?
C30 C29 C31 C25 -59.6(3) . . . . ?
C24 C25 C31 C29 60.5(3) . . . . ?
C26 C25 C31 C29 -59.6(3) . . . . ?
C22 C23 C32 C27 180.0(2) . . . . ?
C30 C23 C32 C27 -58.2(3) . . . . ?
C24 C23 C32 C27 60.4(3) . . . . ?
C33 C27 C32 C23 -179.8(2) . . . . ?
C26 C27 C32 C23 -60.7(3) . . . . ?
C28 C27 C32 C23 57.5(3) . . . . ?
C26 C27 C33 N3 -170.1(2) . . . . ?
C28 C27 C33 N3 70.9(3) . . . . ?
C32 C27 C33 N3 -51.2(3) . . . . ?
O5 C34 C35 C36 -1.3(5) . . . . ?
N3 C34 C35 C36 179.3(3) . . . . ?
O5 C34 C35 C42 177.1(3) . . . . ?
N3 C34 C35 C42 -2.4(3) . . . . ?
C42 C35 C36 C37 -0.3(4) . . . . ?
C34 C35 C36 C37 177.8(2) . . . . ?
C35 C36 C37 C40 0.9(4) . . . . ?
C35 C36 C37 C38 -177.8(2) . . . . ?
C40 C37 C38 O8 -174.4(3) . . . . ?
C36 C37 C38 O8 4.5(5) . . . . ?
C40 C37 C38 N4 3.9(3) . . . . ?
C36 C37 C38 N4 -177.2(3) . . . . ?
C36 C37 C40 C41 -1.2(4) . . . . ?
C38 C37 C40 C41 177.8(2) . . . . ?
C36 C37 C40 C39 179.4(2) . . . . ?
C38 C37 C40 C39 -1.6(3) . . . . ?
O7 C39 C40 C41 -1.1(5) . . . . ?
N4 C39 C40 C41 179.3(3) . . . . ?
O7 C39 C40 C37 178.2(3) . . . . ?
N4 C39 C40 C37 -1.3(3) . . . . ?
C37 C40 C41 C42 0.7(4) . . . . ?
C39 C40 C41 C42 179.9(3) . . . . ?
C40 C41 C42 C35 0.0(4) . . . . ?
C40 C41 C42 C43 -178.2(3) . . . . ?
C36 C35 C42 C41 -0.1(4) . . . . ?
C34 C35 C42 C41 -178.6(2) . . . . ?
C36 C35 C42 C43 178.4(2) . . . . ?
C34 C35 C42 C43 0.0(3) . . . . ?
C41 C42 C43 O6 1.1(5) . . . . ?
C35 C42 C43 O6 -177.3(3) . . . . ?
C41 C42 C43 N3 -179.2(3) . . . . ?
C35 C42 C43 N3 2.4(3) . . . . ?
C8 C1 C44 N4 51.3(3) . . . . ?
C9 C1 C44 N4 -70.0(3) . . . . ?
C2 C1 C44 N4 170.3(2) . . . . ?
O2 C12 N1 C21 174.3(2) . . . . ?
C13 C12 N1 C21 -4.2(3) . . . . ?
O2 C12 N1 C11 -1.9(4) . . . . ?
C13 C12 N1 C11 179.6(2) . . . . ?
O1 C21 N1 C12 -177.3(3) . . . . ?
C20 C21 N1 C12 3.0(3) . . . . ?
O1 C21 N1 C11 -1.0(4) . . . . ?
C20 C21 N1 C11 179.3(2) . . . . ?
C7 C11 N1 C12 -90.9(3) . . . . ?
C7 C11 N1 C21 93.3(3) . . . . ?
O3 C16 N2 C17 -172.8(2) . . . . ?
C15 C16 N2 C17 5.2(3) . . . . ?
O3 C16 N2 C22 2.7(4) . . . . ?
C15 C16 N2 C22 -179.3(2) . . . . ?
O4 C17 N2 C16 173.0(2) . . . . ?
C18 C17 N2 C16 -5.3(3) . . . . ?
O4 C17 N2 C22 -2.7(4) . . . . ?
C18 C17 N2 C22 179.1(2) . . . . ?
C23 C22 N2 C16 89.9(3) . . . . ?
C23 C22 N2 C17 -95.0(3) . . . . ?
O6 C43 N3 C34 175.6(3) . . . . ?
C42 C43 N3 C34 -4.1(3) . . . . ?
O6 C43 N3 C33 -0.7(4) . . . . ?
C42 C43 N3 C33 179.6(2) . . . . ?
O5 C34 N3 C43 -175.4(3) . . . . ?
C35 C34 N3 C43 4.1(3) . . . . ?
O5 C34 N3 C33 1.1(4) . . . . ?
C35 C34 N3 C33 -179.5(2) . . . . ?
C27 C33 N3 C43 -93.0(3) . . . . ?
C27 C33 N3 C34 91.0(3) . . . . ?
O7 C39 N4 C38 -175.5(3) . . . . ?
C40 C39 N4 C38 4.0(3) . . . . ?
O7 C39 N4 C44 1.5(4) . . . . ?
C40 C39 N4 C44 -178.9(2) . . . . ?
O8 C38 N4 C39 173.5(3) . . . . ?
C37 C38 N4 C39 -4.9(3) . . . . ?
O8 C38 N4 C44 -3.7(4) . . . . ?
C37 C38 N4 C44 177.9(2) . . . . ?
C1 C44 N4 C39 89.3(3) . . . . ?
C1 C44 N4 C38 -93.9(3) . . . . ?
Br1A C1A C2A Br2A -179.9(3) . . . . ?

_refine_diff_density_max         1.208
_refine_diff_density_min         -1.665
_refine_diff_density_rms         0.098



####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 2133053'
loop_
_audit_author_name
_audit_author_address
'Tadashi Hyodo'
;Tokushima Bunri University
Japan
;
_audit_update_record             
;
2022-01-07 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT431_2a                  
;
PROBLEM: Short Inter HL..A Contact  Br3..O2 3.04 Ang.
2-x,1-y,1-z  = 2_766

RESPONSE: This is attributed to the Br...O halogen bond
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C55 H47 Br9 N4 O8'
_chemical_formula_weight         1611.15

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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8012(3)
_cell_length_b                   15.8268(4)
_cell_length_c                   18.8202(4)
_cell_angle_alpha                87.366(2)
_cell_angle_beta                 80.576(2)
_cell_angle_gamma                72.004(2)
_cell_volume                     2739.09(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    28738
_cell_measurement_theta_min      2.4840
_cell_measurement_theta_max      78.6810

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_F_000             1568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    8.346
_shelx_estimated_absorpt_T_min   0.434
_shelx_estimated_absorpt_T_max   0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.41659
_exptl_absorpt_correction_T_max  1.00000
_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   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            32381
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.380
_diffrn_reflns_theta_max         79.440
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             10830
_reflns_number_gt                10016
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (Hübschle et al., 2011)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1083P)²+22.5575P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10830
_refine_ls_number_parameters     759
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0859
_refine_ls_wR_factor_ref         0.2232
_refine_ls_wR_factor_gt          0.2184
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6561(7) 0.1581(4) 0.1869(3) 0.0237(11) Uani 1 1 d . . . . .
C2 C 0.6827(6) 0.2202(4) 0.1238(3) 0.0224(11) Uani 1 1 d . . . . .
H2A H 0.599225 0.236716 0.097099 0.027 Uiso 1 1 calc R U . . .
H2B H 0.690955 0.275328 0.142965 0.027 Uiso 1 1 calc R U . . .
C3 C 0.8218(7) 0.1743(4) 0.0726(3) 0.0261(12) Uani 1 1 d . . . . .
C4 C 0.9512(7) 0.1489(4) 0.1150(3) 0.0293(12) Uani 1 1 d . . . . .
H4A H 1.041958 0.118707 0.082484 0.035 Uiso 1 1 calc R U . . .
H4B H 0.962189 0.203229 0.134197 0.035 Uiso 1 1 calc R U . . .
C5 C 0.9250(7) 0.0871(4) 0.1772(4) 0.0330(14) Uani 1 1 d . . . . .
H5 H 1.008778 0.071361 0.204521 0.040 Uiso 1 1 calc R U . . .
C6 C 0.7861(7) 0.1327(4) 0.2278(3) 0.0271(12) Uani 1 1 d . . . . .
H6A H 0.795023 0.186696 0.248535 0.033 Uiso 1 1 calc R U . . .
H6B H 0.770344 0.092227 0.267813 0.033 Uiso 1 1 calc R U . . .
C7 C 0.6437(9) 0.0730(4) 0.1550(4) 0.0379(15) Uani 1 1 d . . . . .
H7A H 0.625137 0.032482 0.194458 0.045 Uiso 1 1 calc R U . . .
H7B H 0.561122 0.088639 0.127748 0.045 Uiso 1 1 calc R U . . .
C8 C 0.8062(10) 0.0891(4) 0.0437(4) 0.0386(16) Uani 1 1 d . . . . .
H8A H 0.722351 0.104534 0.017300 0.046 Uiso 1 1 calc R U . . .
H8B H 0.894658 0.059226 0.009508 0.046 Uiso 1 1 calc R U . . .
C9 C 0.7841(10) 0.0262(4) 0.1050(4) 0.0427(17) Uani 1 1 d . . . . .
H9 H 0.775877 -0.029282 0.085105 0.051 Uiso 1 1 calc R U . . .
C10 C 0.9121(9) 0.0028(4) 0.1471(4) 0.0437(18) Uani 1 1 d . . . . .
H10A H 0.896788 -0.037861 0.187065 0.052 Uiso 1 1 calc R U . . .
H10B H 1.003129 -0.027838 0.114957 0.052 Uiso 1 1 calc R U . . .
C11 C 0.5117(7) 0.2019(4) 0.2358(3) 0.0270(12) Uani 1 1 d . . . . .
H11A H 0.432865 0.219709 0.206115 0.032 Uiso 1 1 calc R U . . .
H11B H 0.490304 0.157721 0.271285 0.032 Uiso 1 1 calc R U . . .
C12 C 0.5621(6) 0.2660(4) 0.3414(3) 0.0252(11) Uani 1 1 d . . . . .
C13 C 0.5896(6) 0.3414(4) 0.3741(3) 0.0224(11) Uani 1 1 d . . . . .
C14 C 0.6629(7) 0.3279(4) 0.4317(3) 0.0276(12) Uani 1 1 d . . . . .
H14 H 0.695830 0.270033 0.451247 0.033 Uiso 1 1 calc R U . . .
C15 C 0.6892(7) 0.3999(4) 0.4619(3) 0.0274(12) Uani 1 1 d . . . . .
H15 H 0.741323 0.390213 0.501403 0.033 Uiso 1 1 calc R U . . .
C16 C 0.6409(6) 0.4836(4) 0.4351(3) 0.0238(11) Uani 1 1 d . . . . .
C17 C 0.6708(6) 0.5588(4) 0.4671(3) 0.0261(12) Uani 1 1 d . . . . .
C18 C 0.5333(6) 0.6616(4) 0.3824(3) 0.0246(11) Uani 1 1 d . . . . .
C19 C 0.5139(6) 0.5850(4) 0.3477(3) 0.0246(11) Uani 1 1 d . . . . .
C20 C 0.4437(6) 0.5982(4) 0.2877(3) 0.0241(11) Uani 1 1 d . . . . .
H20 H 0.409637 0.656240 0.268677 0.029 Uiso 1 1 calc R U . . .
C21 C 0.4234(6) 0.5256(4) 0.2554(3) 0.0263(12) Uani 1 1 d . . . . .
H21 H 0.376278 0.534806 0.214107 0.032 Uiso 1 1 calc R U . . .
C22 C 0.4710(6) 0.4415(4) 0.2829(3) 0.0216(11) Uani 1 1 d . . . . .
C23 C 0.4526(6) 0.3657(4) 0.2464(3) 0.0238(11) Uani 1 1 d . . . . .
C24 C 0.5415(6) 0.4269(4) 0.3443(3) 0.0206(10) Uani 1 1 d . . . . .
C25 C 0.5648(6) 0.4992(4) 0.3759(3) 0.0227(11) Uani 1 1 d . . . . .
C26 C 0.6607(7) 0.7162(4) 0.4634(4) 0.0285(12) Uani 1 1 d . . . . .
H26A H 0.672612 0.704781 0.514525 0.034 Uiso 1 1 calc R U . . .
H26B H 0.578037 0.770888 0.461558 0.034 Uiso 1 1 calc R U . . .
C27 C 0.7988(6) 0.7319(4) 0.4219(3) 0.0211(10) Uani 1 1 d . . . . .
C28 C 0.7927(6) 0.7440(3) 0.3404(3) 0.0204(10) Uani 1 1 d . . . . .
H28A H 0.783469 0.689514 0.320579 0.025 Uiso 1 1 calc R U . . .
H28B H 0.705970 0.793955 0.333036 0.025 Uiso 1 1 calc R U . . .
C29 C 0.9290(6) 0.7627(4) 0.3000(3) 0.0218(11) Uani 1 1 d . . . . .
C30 C 1.0642(6) 0.6857(4) 0.3127(3) 0.0219(11) Uani 1 1 d . . . . .
H30A H 1.059966 0.630140 0.292431 0.026 Uiso 1 1 calc R U . . .
H30B H 1.152695 0.698310 0.287529 0.026 Uiso 1 1 calc R U . . .
C31 C 1.0725(6) 0.6736(4) 0.3933(3) 0.0253(11) Uani 1 1 d . . . . .
H31 H 1.159759 0.622769 0.400449 0.030 Uiso 1 1 calc R U . . .
C32 C 0.9348(6) 0.6544(4) 0.4318(3) 0.0236(11) Uani 1 1 d . . . . .
H32A H 0.940229 0.645438 0.483822 0.028 Uiso 1 1 calc R U . . .
H32B H 0.927941 0.599220 0.412126 0.028 Uiso 1 1 calc R U . . .
C33 C 0.8118(7) 0.8172(4) 0.4527(4) 0.0295(13) Uani 1 1 d . . . . .
H33A H 0.817709 0.809499 0.504765 0.035 Uiso 1 1 calc R U . . .
H33B H 0.724780 0.867720 0.447030 0.035 Uiso 1 1 calc R U . . .
C34 C 1.0841(7) 0.7596(4) 0.4238(4) 0.0308(13) Uani 1 1 d . . . . .
H34A H 1.090873 0.752430 0.475757 0.037 Uiso 1 1 calc R U . . .
H34B H 1.172675 0.772224 0.398716 0.037 Uiso 1 1 calc R U . . .
C35 C 0.9406(7) 0.8485(4) 0.3314(4) 0.0308(13) Uani 1 1 d . . . . .
H35A H 1.028441 0.861601 0.305963 0.037 Uiso 1 1 calc R U . . .
H35B H 0.854721 0.899101 0.324090 0.037 Uiso 1 1 calc R U . . .
C36 C 0.9491(7) 0.8367(4) 0.4127(4) 0.0319(13) Uani 1 1 d . . . . .
H36 H 0.956006 0.892601 0.432441 0.038 Uiso 1 1 calc R U . . .
C37 C 0.9236(7) 0.7781(4) 0.2196(3) 0.0293(13) Uani 1 1 d . . . . .
H37A H 0.837695 0.829380 0.213702 0.035 Uiso 1 1 calc R U . . .
H37B H 1.011107 0.793766 0.197078 0.035 Uiso 1 1 calc R U . . .
C38 C 1.0460(6) 0.6387(4) 0.1517(3) 0.0244(11) Uani 1 1 d . . . . .
C39 C 1.0343(7) 0.5553(4) 0.1211(3) 0.0242(11) Uani 1 1 d . . . . .
C40 C 1.1576(7) 0.4846(4) 0.1028(3) 0.0295(13) Uani 1 1 d . . . . .
H40 H 1.249715 0.488356 0.109224 0.035 Uiso 1 1 calc R U . . .
C41 C 1.1461(7) 0.4068(4) 0.0745(3) 0.0290(12) Uani 1 1 d . . . . .
H41 H 1.230489 0.357125 0.063442 0.035 Uiso 1 1 calc R U . . .
C42 C 1.0142(7) 0.4018(4) 0.0628(3) 0.0255(12) Uani 1 1 d . . . . .
C43 C 1.0022(7) 0.3210(4) 0.0317(3) 0.0298(13) Uani 1 1 d . . . . .
C44 C 0.7373(7) 0.3908(4) 0.0373(3) 0.0261(12) Uani 1 1 d . . . . .
C45 C 0.7505(7) 0.4715(4) 0.0680(3) 0.0248(11) Uani 1 1 d . . . . .
C46 C 0.6276(7) 0.5442(4) 0.0853(3) 0.0266(12) Uani 1 1 d . . . . .
H46 H 0.536445 0.543199 0.074879 0.032 Uiso 1 1 calc R U . . .
C47 C 0.6387(7) 0.6187(4) 0.1181(3) 0.0256(11) Uani 1 1 d . . . . .
H47 H 0.553969 0.667707 0.130782 0.031 Uiso 1 1 calc R U . . .
C48 C 0.7695(7) 0.6224(4) 0.1323(3) 0.0254(11) Uani 1 1 d . . . . .
C49 C 0.7780(7) 0.6995(4) 0.1711(3) 0.0275(12) Uani 1 1 d . . . . .
C50 C 0.8985(7) 0.5514(4) 0.1116(3) 0.0243(11) Uani 1 1 d . . . . .
C51 C 0.8863(6) 0.4745(4) 0.0812(3) 0.0240(11) Uani 1 1 d . . . . .
C52 C 0.8476(8) 0.2325(4) 0.0068(3) 0.0307(13) Uani 1 1 d . . . . .
H52A H 0.936521 0.199353 -0.025603 0.037 Uiso 1 1 calc R U . . .
H52B H 0.764894 0.245061 -0.020156 0.037 Uiso 1 1 calc R U . . .
N1 N 0.5124(5) 0.2805(3) 0.2746(3) 0.0240(10) Uani 1 1 d . . . . .
N2 N 0.6252(5) 0.6415(3) 0.4355(3) 0.0249(10) Uani 1 1 d . . . . .
N3 N 0.9161(6) 0.7008(3) 0.1811(3) 0.0253(10) Uani 1 1 d . . . . .
N4 N 0.8634(6) 0.3171(3) 0.0278(3) 0.0271(10) Uani 1 1 d . . . . .
O1 O 0.5845(5) 0.1935(3) 0.3700(2) 0.0321(10) Uani 1 1 d . . . . .
O2 O 0.7338(5) 0.5484(3) 0.5195(2) 0.0341(10) Uani 1 1 d . . . . .
O3 O 0.4751(5) 0.7373(3) 0.3666(3) 0.0325(10) Uani 1 1 d . . . . .
O4 O 0.3924(5) 0.3740(3) 0.1942(2) 0.0293(9) Uani 1 1 d . . . . .
O5 O 1.1631(5) 0.6503(3) 0.1518(2) 0.0329(10) Uani 1 1 d . . . . .
O6 O 1.1099(6) 0.2588(3) 0.0112(3) 0.0417(12) Uani 1 1 d . . . . .
O7 O 0.6236(5) 0.3867(3) 0.0226(3) 0.0330(10) Uani 1 1 d . . . . .
O8 O 0.6698(5) 0.7585(3) 0.1959(3) 0.0366(11) Uani 1 1 d . . . . .
C53 C 1.0853(7) 0.3509(5) 0.2801(3) 0.0297(13) Uani 1 1 d . . . . .
H53 H 1.154391 0.356216 0.235929 0.036 Uiso 1 1 calc R U . . .
Br1 Br 0.89177(8) 0.40994(7) 0.26290(4) 0.0552(3) Uani 1 1 d . . . . .
Br2 Br 1.11048(11) 0.22625(6) 0.29862(7) 0.0607(3) Uani 1 1 d . . . . .
Br3 Br 1.13153(8) 0.40293(5) 0.36013(4) 0.0375(2) Uani 1 1 d . . . . .
C54 C 0.4242(13) 0.8943(9) 0.1299(9) 0.038(4) Uani 0.622(8) 1 d D . P A 1
H54 H 0.476238 0.893342 0.171567 0.046 Uiso 0.622(8) 1 calc R U P A 1
Br4 Br 0.5682(3) 0.84961(16) 0.04738(16) 0.0469(6) Uani 0.622(8) 1 d D . P A 1
Br5 Br 0.2990(3) 0.8203(3) 0.1547(2) 0.0282(5) Uani 0.622(8) 1 d D . P A 1
Br6 Br 0.31464(17) 1.01413(14) 0.11570(14) 0.0508(8) Uani 0.622(8) 1 d D . P A
1
C54B C 0.425(2) 0.9020(11) 0.1538(14) 0.046(9) Uani 0.378(8) 1 d D . P A 2
H54B H 0.491383 0.886855 0.190684 0.055 Uiso 0.378(8) 1 calc R U P A 2
Br4B Br 0.5386(11) 0.8862(8) 0.0602(4) 0.107(3) Uani 0.378(8) 1 d D . P A 2
Br5B Br 0.3043(10) 0.8253(7) 0.1662(6) 0.073(3) Uani 0.378(8) 1 d D . P A 2
Br6B Br 0.3100(5) 1.0237(4) 0.1654(9) 0.164(5) Uani 0.378(8) 1 d D . P A 2
C55 C 0.3036(19) 0.9548(10) 0.3999(9) 0.048(5) Uani 0.580(6) 1 d D U P B 1
H55 H 0.335131 0.899269 0.370174 0.058 Uiso 0.580(6) 1 calc R U P B 1
Br7 Br 0.1161(3) 1.02372(19) 0.3792(3) 0.0973(16) Uani 0.580(6) 1 d D . P B 1
Br8 Br 0.4507(6) 1.0148(4) 0.3741(3) 0.1093(18) Uani 0.580(6) 1 d D . P B 1
Br9 Br 0.2987(5) 0.9201(3) 0.4977(3) 0.0564(12) Uani 0.580(6) 1 d D . P B 1
C55B C 0.355(2) 0.9417(10) 0.3901(7) 0.032(4) Uani 0.420(6) 1 d D U P B 2
H55B H 0.424970 0.882532 0.373626 0.038 Uiso 0.420(6) 1 calc R U P B 2
Br7B Br 0.2169(6) 0.9828(2) 0.3251(2) 0.089(2) Uani 0.420(6) 1 d D . P B 2
Br8B Br 0.4582(5) 1.0270(2) 0.38905(19) 0.0359(7) Uani 0.420(6) 1 d D . P B 2
Br9B Br 0.2590(7) 0.9323(4) 0.4867(3) 0.0547(15) Uani 0.420(6) 1 d D . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.534(8) . ?
C1 C11 1.535(9) . ?
C1 C7 1.546(8) . ?
C1 C2 1.548(7) . ?
C2 C3 1.528(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C8 1.536(8) . ?
C3 C52 1.544(8) . ?
C3 C4 1.548(9) . ?
C4 C5 1.531(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.520(9) . ?
C5 C10 1.521(10) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C9 1.529(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.522(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.534(12) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N1 1.474(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O1 1.217(8) . ?
C12 N1 1.405(8) . ?
C12 C13 1.482(8) . ?
C13 C14 1.370(8) . ?
C13 C24 1.412(8) . ?
C14 C15 1.407(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.364(9) . ?
C15 H15 0.9500 . ?
C16 C25 1.411(8) . ?
C16 C17 1.484(8) . ?
C17 O2 1.225(8) . ?
C17 N2 1.386(8) . ?
C18 O3 1.203(8) . ?
C18 N2 1.415(8) . ?
C18 C19 1.479(8) . ?
C19 C20 1.390(8) . ?
C19 C25 1.407(8) . ?
C20 C21 1.406(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.375(8) . ?
C21 H21 0.9500 . ?
C22 C24 1.416(8) . ?
C22 C23 1.481(8) . ?
C23 O4 1.209(7) . ?
C23 N1 1.411(8) . ?
C24 C25 1.408(8) . ?
C26 N2 1.471(7) . ?
C26 C27 1.533(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C32 1.539(7) . ?
C27 C33 1.541(7) . ?
C27 C28 1.545(8) . ?
C28 C29 1.530(7) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C37 1.529(8) . ?
C29 C30 1.541(7) . ?
C29 C35 1.547(8) . ?
C30 C31 1.532(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.533(8) . ?
C31 C34 1.545(8) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C36 1.542(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C36 1.534(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.546(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36 1.0000 . ?
C37 N3 1.476(8) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 O5 1.217(8) . ?
C38 N3 1.394(8) . ?
C38 C39 1.508(8) . ?
C39 C40 1.376(9) . ?
C39 C50 1.392(8) . ?
C40 C41 1.407(10) . ?
C40 H40 0.9500 . ?
C41 C42 1.372(9) . ?
C41 H41 0.9500 . ?
C42 C51 1.421(8) . ?
C42 C43 1.475(9) . ?
C43 O6 1.222(8) . ?
C43 N4 1.394(9) . ?
C44 O7 1.211(8) . ?
C44 N4 1.406(8) . ?
C44 C45 1.476(8) . ?
C45 C46 1.389(9) . ?
C45 C51 1.409(9) . ?
C46 C47 1.397(8) . ?
C46 H46 0.9500 . ?
C47 C48 1.371(9) . ?
C47 H47 0.9500 . ?
C48 C50 1.419(9) . ?
C48 C49 1.481(8) . ?
C49 O8 1.216(8) . ?
C49 N3 1.404(8) . ?
C50 C51 1.414(9) . ?
C52 N4 1.473(8) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 Br1 1.911(6) . ?
C53 Br3 1.929(6) . ?
C53 Br2 1.934(7) . ?
C53 H53 1.0000 . ?
C54 Br6 1.901(12) . ?
C54 Br4 1.916(16) . ?
C54 Br5 1.935(13) . ?
C54 H54 1.0000 . ?
C54B Br4B 1.91(2) . ?
C54B Br6B 1.909(16) . ?
C54B Br5B 1.923(18) . ?
C54B H54B 1.0000 . ?
C55 Br9 1.895(14) . ?
C55 Br7 1.917(16) . ?
C55 Br8 1.947(15) . ?
C55 H55 1.0000 . ?
C55B Br8B 1.916(16) . ?
C55B Br7B 1.920(17) . ?
C55B Br9B 1.928(15) . ?
C55B H55B 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
C6 C1 C11 112.6(5) . . ?
C6 C1 C7 108.9(5) . . ?
C11 C1 C7 107.3(5) . . ?
C6 C1 C2 109.2(5) . . ?
C11 C1 C2 110.6(5) . . ?
C7 C1 C2 108.1(5) . . ?
C3 C2 C1 110.5(5) . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C8 108.5(5) . . ?
C2 C3 C52 112.0(5) . . ?
C8 C3 C52 107.0(5) . . ?
C2 C3 C4 108.9(5) . . ?
C8 C3 C4 108.9(5) . . ?
C52 C3 C4 111.5(5) . . ?
C5 C4 C3 109.8(5) . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C6 C5 C10 109.3(6) . . ?
C6 C5 C4 110.3(5) . . ?
C10 C5 C4 109.3(6) . . ?
C6 C5 H5 109.3 . . ?
C10 C5 H5 109.3 . . ?
C4 C5 H5 109.3 . . ?
C5 C6 C1 110.2(5) . . ?
C5 C6 H6A 109.6 . . ?
C1 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
C1 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C9 C7 C1 110.1(6) . . ?
C9 C7 H7A 109.6 . . ?
C1 C7 H7A 109.6 . . ?
C9 C7 H7B 109.6 . . ?
C1 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C3 110.8(5) . . ?
C9 C8 H8A 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C8 C9 C7 108.1(6) . . ?
C8 C9 C10 110.1(7) . . ?
C7 C9 C10 109.5(6) . . ?
C8 C9 H9 109.7 . . ?
C7 C9 H9 109.7 . . ?
C10 C9 H9 109.7 . . ?
C5 C10 C9 109.8(5) . . ?
C5 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C5 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
N1 C11 C1 113.2(5) . . ?
N1 C11 H11A 108.9 . . ?
C1 C11 H11A 108.9 . . ?
N1 C11 H11B 108.9 . . ?
C1 C11 H11B 108.9 . . ?
H11A C11 H11B 107.8 . . ?
O1 C12 N1 120.8(5) . . ?
O1 C12 C13 121.7(5) . . ?
N1 C12 C13 117.5(5) . . ?
C14 C13 C24 120.5(5) . . ?
C14 C13 C12 120.4(5) . . ?
C24 C13 C12 119.1(5) . . ?
C13 C14 C15 119.8(6) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 120.8(6) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C25 120.4(5) . . ?
C15 C16 C17 120.2(5) . . ?
C25 C16 C17 119.5(5) . . ?
O2 C17 N2 120.9(5) . . ?
O2 C17 C16 121.5(6) . . ?
N2 C17 C16 117.6(5) . . ?
O3 C18 N2 121.1(6) . . ?
O3 C18 C19 122.5(6) . . ?
N2 C18 C19 116.4(5) . . ?
C20 C19 C25 120.2(5) . . ?
C20 C19 C18 119.9(5) . . ?
C25 C19 C18 120.0(5) . . ?
C19 C20 C21 119.9(5) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.6(5) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C24 120.3(5) . . ?
C21 C22 C23 119.6(5) . . ?
C24 C22 C23 120.1(5) . . ?
O4 C23 N1 120.1(5) . . ?
O4 C23 C22 123.2(5) . . ?
N1 C23 C22 116.7(5) . . ?
C25 C24 C13 119.4(5) . . ?
C25 C24 C22 119.2(5) . . ?
C13 C24 C22 121.3(5) . . ?
C19 C25 C24 119.8(5) . . ?
C19 C25 C16 121.2(5) . . ?
C24 C25 C16 119.0(5) . . ?
N2 C26 C27 113.9(5) . . ?
N2 C26 H26A 108.8 . . ?
C27 C26 H26A 108.8 . . ?
N2 C26 H26B 108.8 . . ?
C27 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
C26 C27 C32 111.4(5) . . ?
C26 C27 C33 107.3(5) . . ?
C32 C27 C33 108.7(5) . . ?
C26 C27 C28 111.9(5) . . ?
C32 C27 C28 108.3(4) . . ?
C33 C27 C28 109.3(5) . . ?
C29 C28 C27 111.3(4) . . ?
C29 C28 H28A 109.4 . . ?
C27 C28 H28A 109.4 . . ?
C29 C28 H28B 109.4 . . ?
C27 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
C37 C29 C28 112.4(5) . . ?
C37 C29 C30 111.2(5) . . ?
C28 C29 C30 109.3(4) . . ?
C37 C29 C35 107.3(5) . . ?
C28 C29 C35 108.5(5) . . ?
C30 C29 C35 108.0(5) . . ?
C31 C30 C29 110.8(5) . . ?
C31 C30 H30A 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C30 C31 C32 109.1(4) . . ?
C30 C31 C34 109.0(5) . . ?
C32 C31 C34 109.9(5) . . ?
C30 C31 H31 109.6 . . ?
C32 C31 H31 109.6 . . ?
C34 C31 H31 109.6 . . ?
C31 C32 C27 110.6(5) . . ?
C31 C32 H32A 109.5 . . ?
C27 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C27 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
C27 C33 C36 109.6(5) . . ?
C27 C33 H33A 109.7 . . ?
C36 C33 H33A 109.7 . . ?
C27 C33 H33B 109.7 . . ?
C36 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
C36 C34 C31 108.9(5) . . ?
C36 C34 H34A 109.9 . . ?
C31 C34 H34A 109.9 . . ?
C36 C34 H34B 109.9 . . ?
C31 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
C36 C35 C29 109.9(5) . . ?
C36 C35 H35A 109.7 . . ?
C29 C35 H35A 109.7 . . ?
C36 C35 H35B 109.7 . . ?
C29 C35 H35B 109.7 . . ?
H35A C35 H35B 108.2 . . ?
C34 C36 C33 109.6(5) . . ?
C34 C36 C35 109.6(5) . . ?
C33 C36 C35 109.9(5) . . ?
C34 C36 H36 109.2 . . ?
C33 C36 H36 109.2 . . ?
C35 C36 H36 109.2 . . ?
N3 C37 C29 114.0(5) . . ?
N3 C37 H37A 108.8 . . ?
C29 C37 H37A 108.8 . . ?
N3 C37 H37B 108.8 . . ?
C29 C37 H37B 108.8 . . ?
H37A C37 H37B 107.6 . . ?
O5 C38 N3 121.8(6) . . ?
O5 C38 C39 121.7(6) . . ?
N3 C38 C39 116.5(5) . . ?
C40 C39 C50 121.2(6) . . ?
C40 C39 C38 119.6(6) . . ?
C50 C39 C38 119.2(5) . . ?
C39 C40 C41 119.4(6) . . ?
C39 C40 H40 120.3 . . ?
C41 C40 H40 120.3 . . ?
C42 C41 C40 120.7(6) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C41 C42 C51 120.3(6) . . ?
C41 C42 C43 120.9(6) . . ?
C51 C42 C43 118.8(6) . . ?
O6 C43 N4 120.9(6) . . ?
O6 C43 C42 121.2(6) . . ?
N4 C43 C42 117.8(5) . . ?
O7 C44 N4 121.3(5) . . ?
O7 C44 C45 122.4(6) . . ?
N4 C44 C45 116.3(5) . . ?
C46 C45 C51 120.0(6) . . ?
C46 C45 C44 119.7(5) . . ?
C51 C45 C44 120.4(5) . . ?
C45 C46 C47 119.6(6) . . ?
C45 C46 H46 120.2 . . ?
C47 C46 H46 120.2 . . ?
C48 C47 C46 121.3(6) . . ?
C48 C47 H47 119.4 . . ?
C46 C47 H47 119.4 . . ?
C47 C48 C50 120.5(5) . . ?
C47 C48 C49 120.6(6) . . ?
C50 C48 C49 118.9(5) . . ?
O8 C49 N3 120.4(6) . . ?
O8 C49 C48 121.9(6) . . ?
N3 C49 C48 117.6(5) . . ?
C39 C50 C51 119.8(6) . . ?
C39 C50 C48 122.1(6) . . ?
C51 C50 C48 118.2(5) . . ?
C45 C51 C50 120.3(5) . . ?
C45 C51 C42 121.2(6) . . ?
C50 C51 C42 118.5(5) . . ?
N4 C52 C3 112.2(5) . . ?
N4 C52 H52A 109.2 . . ?
C3 C52 H52A 109.2 . . ?
N4 C52 H52B 109.2 . . ?
C3 C52 H52B 109.2 . . ?
H52A C52 H52B 107.9 . . ?
C12 N1 C23 123.5(5) . . ?
C12 N1 C11 117.2(5) . . ?
C23 N1 C11 119.0(5) . . ?
C17 N2 C18 124.1(5) . . ?
C17 N2 C26 118.9(5) . . ?
C18 N2 C26 116.8(5) . . ?
C38 N3 C49 124.3(5) . . ?
C38 N3 C37 118.2(5) . . ?
C49 N3 C37 117.2(5) . . ?
C43 N4 C44 124.2(5) . . ?
C43 N4 C52 118.6(5) . . ?
C44 N4 C52 117.0(5) . . ?
Br1 C53 Br3 111.8(3) . . ?
Br1 C53 Br2 110.2(3) . . ?
Br3 C53 Br2 109.4(3) . . ?
Br1 C53 H53 108.5 . . ?
Br3 C53 H53 108.5 . . ?
Br2 C53 H53 108.5 . . ?
Br6 C54 Br4 110.8(7) . . ?
Br6 C54 Br5 111.2(6) . . ?
Br4 C54 Br5 111.9(8) . . ?
Br6 C54 H54 107.6 . . ?
Br4 C54 H54 107.6 . . ?
Br5 C54 H54 107.6 . . ?
Br4B C54B Br6B 108.7(10) . . ?
Br4B C54B Br5B 110.3(12) . . ?
Br6B C54B Br5B 111.0(10) . . ?
Br4B C54B H54B 108.9 . . ?
Br6B C54B H54B 108.9 . . ?
Br5B C54B H54B 108.9 . . ?
Br9 C55 Br7 112.3(10) . . ?
Br9 C55 Br8 109.2(8) . . ?
Br7 C55 Br8 113.1(6) . . ?
Br9 C55 H55 107.3 . . ?
Br7 C55 H55 107.3 . . ?
Br8 C55 H55 107.3 . . ?
Br8B C55B Br7B 107.4(7) . . ?
Br8B C55B Br9B 109.1(7) . . ?
Br7B C55B Br9B 110.9(11) . . ?
Br8B C55B H55B 109.8 . . ?
Br7B C55B H55B 109.8 . . ?
Br9B C55B H55B 109.8 . . ?

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
C6 C1 C2 C3 59.1(6) . . . . ?
C11 C1 C2 C3 -176.5(5) . . . . ?
C7 C1 C2 C3 -59.2(6) . . . . ?
C1 C2 C3 C8 59.2(6) . . . . ?
C1 C2 C3 C52 177.0(5) . . . . ?
C1 C2 C3 C4 -59.2(6) . . . . ?
C2 C3 C4 C5 59.0(6) . . . . ?
C8 C3 C4 C5 -59.1(7) . . . . ?
C52 C3 C4 C5 -176.9(5) . . . . ?
C3 C4 C5 C6 -59.5(7) . . . . ?
C3 C4 C5 C10 60.8(7) . . . . ?
C10 C5 C6 C1 -60.8(6) . . . . ?
C4 C5 C6 C1 59.4(7) . . . . ?
C11 C1 C6 C5 178.2(5) . . . . ?
C7 C1 C6 C5 59.4(6) . . . . ?
C2 C1 C6 C5 -58.5(6) . . . . ?
C6 C1 C7 C9 -58.4(7) . . . . ?
C11 C1 C7 C9 179.5(5) . . . . ?
C2 C1 C7 C9 60.2(7) . . . . ?
C2 C3 C8 C9 -60.4(8) . . . . ?
C52 C3 C8 C9 178.6(6) . . . . ?
C4 C3 C8 C9 58.0(8) . . . . ?
C3 C8 C9 C7 61.4(8) . . . . ?
C3 C8 C9 C10 -58.2(8) . . . . ?
C1 C7 C9 C8 -61.3(7) . . . . ?
C1 C7 C9 C10 58.7(7) . . . . ?
C6 C5 C10 C9 60.6(7) . . . . ?
C4 C5 C10 C9 -60.3(8) . . . . ?
C8 C9 C10 C5 59.0(8) . . . . ?
C7 C9 C10 C5 -59.7(8) . . . . ?
C6 C1 C11 N1 55.6(6) . . . . ?
C7 C1 C11 N1 175.4(5) . . . . ?
C2 C1 C11 N1 -66.9(6) . . . . ?
O1 C12 C13 C14 10.5(9) . . . . ?
N1 C12 C13 C14 -167.8(5) . . . . ?
O1 C12 C13 C24 -170.6(6) . . . . ?
N1 C12 C13 C24 11.0(8) . . . . ?
C24 C13 C14 C15 0.7(9) . . . . ?
C12 C13 C14 C15 179.5(5) . . . . ?
C13 C14 C15 C16 0.9(9) . . . . ?
C14 C15 C16 C25 -0.7(9) . . . . ?
C14 C15 C16 C17 -179.4(5) . . . . ?
C15 C16 C17 O2 -2.9(9) . . . . ?
C25 C16 C17 O2 178.4(5) . . . . ?
C15 C16 C17 N2 177.0(5) . . . . ?
C25 C16 C17 N2 -1.8(8) . . . . ?
O3 C18 C19 C20 9.5(8) . . . . ?
N2 C18 C19 C20 -170.2(5) . . . . ?
O3 C18 C19 C25 -169.7(5) . . . . ?
N2 C18 C19 C25 10.5(7) . . . . ?
C25 C19 C20 C21 0.2(8) . . . . ?
C18 C19 C20 C21 -179.1(5) . . . . ?
C19 C20 C21 C22 0.6(9) . . . . ?
C20 C21 C22 C24 0.0(9) . . . . ?
C20 C21 C22 C23 -178.0(5) . . . . ?
C21 C22 C23 O4 -2.7(9) . . . . ?
C24 C22 C23 O4 179.3(5) . . . . ?
C21 C22 C23 N1 176.0(5) . . . . ?
C24 C22 C23 N1 -2.0(8) . . . . ?
C14 C13 C24 C25 -2.3(8) . . . . ?
C12 C13 C24 C25 178.8(5) . . . . ?
C14 C13 C24 C22 177.3(5) . . . . ?
C12 C13 C24 C22 -1.6(8) . . . . ?
C21 C22 C24 C25 -1.3(8) . . . . ?
C23 C22 C24 C25 176.7(5) . . . . ?
C21 C22 C24 C13 179.1(5) . . . . ?
C23 C22 C24 C13 -2.9(8) . . . . ?
C20 C19 C25 C24 -1.5(8) . . . . ?
C18 C19 C25 C24 177.7(5) . . . . ?
C20 C19 C25 C16 177.7(5) . . . . ?
C18 C19 C25 C16 -3.1(8) . . . . ?
C13 C24 C25 C19 -178.3(5) . . . . ?
C22 C24 C25 C19 2.1(8) . . . . ?
C13 C24 C25 C16 2.5(8) . . . . ?
C22 C24 C25 C16 -177.1(5) . . . . ?
C15 C16 C25 C19 179.8(5) . . . . ?
C17 C16 C25 C19 -1.4(8) . . . . ?
C15 C16 C25 C24 -1.0(8) . . . . ?
C17 C16 C25 C24 177.8(5) . . . . ?
N2 C26 C27 C32 -66.7(7) . . . . ?
N2 C26 C27 C33 174.5(5) . . . . ?
N2 C26 C27 C28 54.7(7) . . . . ?
C26 C27 C28 C29 178.2(4) . . . . ?
C32 C27 C28 C29 -58.7(6) . . . . ?
C33 C27 C28 C29 59.5(6) . . . . ?
C27 C28 C29 C37 -178.0(4) . . . . ?
C27 C28 C29 C30 58.0(6) . . . . ?
C27 C28 C29 C35 -59.5(6) . . . . ?
C37 C29 C30 C31 177.4(5) . . . . ?
C28 C29 C30 C31 -57.9(6) . . . . ?
C35 C29 C30 C31 60.0(6) . . . . ?
C29 C30 C31 C32 59.0(6) . . . . ?
C29 C30 C31 C34 -61.0(6) . . . . ?
C30 C31 C32 C27 -60.2(6) . . . . ?
C34 C31 C32 C27 59.3(6) . . . . ?
C26 C27 C32 C31 -177.0(5) . . . . ?
C33 C27 C32 C31 -59.1(6) . . . . ?
C28 C27 C32 C31 59.5(6) . . . . ?
C26 C27 C33 C36 -179.8(5) . . . . ?
C32 C27 C33 C36 59.7(6) . . . . ?
C28 C27 C33 C36 -58.3(6) . . . . ?
C30 C31 C34 C36 60.3(6) . . . . ?
C32 C31 C34 C36 -59.2(7) . . . . ?
C37 C29 C35 C36 -179.1(5) . . . . ?
C28 C29 C35 C36 59.2(6) . . . . ?
C30 C29 C35 C36 -59.2(6) . . . . ?
C31 C34 C36 C33 60.3(7) . . . . ?
C31 C34 C36 C35 -60.4(7) . . . . ?
C27 C33 C36 C34 -61.3(7) . . . . ?
C27 C33 C36 C35 59.2(7) . . . . ?
C29 C35 C36 C34 60.6(6) . . . . ?
C29 C35 C36 C33 -59.9(7) . . . . ?
C28 C29 C37 N3 -62.2(7) . . . . ?
C30 C29 C37 N3 60.7(7) . . . . ?
C35 C29 C37 N3 178.6(5) . . . . ?
O5 C38 C39 C40 10.1(8) . . . . ?
N3 C38 C39 C40 -168.6(5) . . . . ?
O5 C38 C39 C50 -169.7(5) . . . . ?
N3 C38 C39 C50 11.7(7) . . . . ?
C50 C39 C40 C41 -0.5(8) . . . . ?
C38 C39 C40 C41 179.7(5) . . . . ?
C39 C40 C41 C42 2.2(8) . . . . ?
C40 C41 C42 C51 -2.0(8) . . . . ?
C40 C41 C42 C43 178.6(5) . . . . ?
C41 C42 C43 O6 -4.8(9) . . . . ?
C51 C42 C43 O6 175.8(5) . . . . ?
C41 C42 C43 N4 173.9(5) . . . . ?
C51 C42 C43 N4 -5.5(7) . . . . ?
O7 C44 C45 C46 4.2(9) . . . . ?
N4 C44 C45 C46 -174.0(5) . . . . ?
O7 C44 C45 C51 -177.1(6) . . . . ?
N4 C44 C45 C51 4.7(8) . . . . ?
C51 C45 C46 C47 -2.3(8) . . . . ?
C44 C45 C46 C47 176.5(5) . . . . ?
C45 C46 C47 C48 1.4(9) . . . . ?
C46 C47 C48 C50 2.2(9) . . . . ?
C46 C47 C48 C49 -176.2(5) . . . . ?
C47 C48 C49 O8 5.2(9) . . . . ?
C50 C48 C49 O8 -173.3(6) . . . . ?
C47 C48 C49 N3 -177.3(5) . . . . ?
C50 C48 C49 N3 4.2(8) . . . . ?
C40 C39 C50 C51 -1.3(8) . . . . ?
C38 C39 C50 C51 178.4(5) . . . . ?
C40 C39 C50 C48 177.8(5) . . . . ?
C38 C39 C50 C48 -2.4(8) . . . . ?
C47 C48 C50 C39 175.9(5) . . . . ?
C49 C48 C50 C39 -5.6(8) . . . . ?
C47 C48 C50 C51 -4.9(8) . . . . ?
C49 C48 C50 C51 173.6(5) . . . . ?
C46 C45 C51 C50 -0.5(8) . . . . ?
C44 C45 C51 C50 -179.2(5) . . . . ?
C46 C45 C51 C42 -178.8(5) . . . . ?
C44 C45 C51 C42 2.5(8) . . . . ?
C39 C50 C51 C45 -176.8(5) . . . . ?
C48 C50 C51 C45 4.0(8) . . . . ?
C39 C50 C51 C42 1.5(7) . . . . ?
C48 C50 C51 C42 -177.7(5) . . . . ?
C41 C42 C51 C45 178.4(5) . . . . ?
C43 C42 C51 C45 -2.2(8) . . . . ?
C41 C42 C51 C50 0.1(8) . . . . ?
C43 C42 C51 C50 179.5(5) . . . . ?
C2 C3 C52 N4 60.9(7) . . . . ?
C8 C3 C52 N4 179.6(6) . . . . ?
C4 C3 C52 N4 -61.4(7) . . . . ?
O1 C12 N1 C23 164.8(6) . . . . ?
C13 C12 N1 C23 -16.8(8) . . . . ?
O1 C12 N1 C11 -9.7(8) . . . . ?
C13 C12 N1 C11 168.7(5) . . . . ?
O4 C23 N1 C12 -169.0(5) . . . . ?
C22 C23 N1 C12 12.4(8) . . . . ?
O4 C23 N1 C11 5.4(8) . . . . ?
C22 C23 N1 C11 -173.3(5) . . . . ?
C1 C11 N1 C12 -88.0(6) . . . . ?
C1 C11 N1 C23 97.3(6) . . . . ?
O2 C17 N2 C18 -170.0(5) . . . . ?
C16 C17 N2 C18 10.2(8) . . . . ?
O2 C17 N2 C26 3.3(8) . . . . ?
C16 C17 N2 C26 -176.5(5) . . . . ?
O3 C18 N2 C17 165.8(5) . . . . ?
C19 C18 N2 C17 -14.4(8) . . . . ?
O3 C18 N2 C26 -7.6(8) . . . . ?
C19 C18 N2 C26 172.2(5) . . . . ?
C27 C26 N2 C17 95.3(6) . . . . ?
C27 C26 N2 C18 -91.0(6) . . . . ?
O5 C38 N3 C49 167.8(5) . . . . ?
C39 C38 N3 C49 -13.6(7) . . . . ?
O5 C38 N3 C37 -6.1(8) . . . . ?
C39 C38 N3 C37 172.6(4) . . . . ?
O8 C49 N3 C38 -176.6(6) . . . . ?
C48 C49 N3 C38 5.9(8) . . . . ?
O8 C49 N3 C37 -2.7(8) . . . . ?
C48 C49 N3 C37 179.7(5) . . . . ?
C29 C37 N3 C38 -89.5(6) . . . . ?
C29 C37 N3 C49 96.2(6) . . . . ?
O6 C43 N4 C44 -167.6(6) . . . . ?
C42 C43 N4 C44 13.7(8) . . . . ?
O6 C43 N4 C52 7.5(8) . . . . ?
C42 C43 N4 C52 -171.2(5) . . . . ?
O7 C44 N4 C43 168.6(6) . . . . ?
C45 C44 N4 C43 -13.2(8) . . . . ?
O7 C44 N4 C52 -6.5(8) . . . . ?
C45 C44 N4 C52 171.7(5) . . . . ?
C3 C52 N4 C43 91.2(7) . . . . ?
C3 C52 N4 C44 -93.3(6) . . . . ?

_refine_diff_density_max         3.507
_refine_diff_density_min         -2.037
_refine_diff_density_rms         0.177



####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 2133055'
loop_
_audit_author_name
_audit_author_address
'Tadashi Hyodo'
;Tokushima Bunri University
Japan
;
_audit_update_record             
;
2022-01-07 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H80 Br8 O4'
_chemical_formula_weight         1720.70

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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3961(12)
_cell_length_b                   11.9472(13)
_cell_length_c                   14.8227(16)
_cell_angle_alpha                101.231(3)
_cell_angle_beta                 104.003(3)
_cell_angle_gamma                93.302(3)
_cell_volume                     1741.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9742
_cell_measurement_theta_min      3.61
_cell_measurement_theta_max      78.44

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_F_000             860
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.896
_shelx_estimated_absorpt_T_min   0.563
_shelx_estimated_absorpt_T_max   0.590
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8968
_exptl_absorpt_correction_T_max  0.9403
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            23618
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.147
_diffrn_reflns_theta_max         79.935
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             7009
_reflns_number_gt                6695
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (Hübschle et al., 2011)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0409P)²+5.7451P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7009
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1220
_refine_ls_wR_factor_gt          0.1210
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8760(3) 0.6442(3) 0.7574(2) 0.0166(6) Uani 1 1 d . . . . .
C2 C 0.9464(4) 0.5643(3) 0.8193(2) 0.0215(7) Uani 1 1 d . . . . .
H2A H 0.882722 0.497647 0.815724 0.026 Uiso 1 1 calc R U . . .
H2AB H 1.021383 0.535144 0.794839 0.026 Uiso 1 1 calc R U . . .
C3 C 0.9991(4) 0.6295(3) 0.9233(2) 0.0280(8) Uani 1 1 d . . . . .
H3 H 1.045003 0.576897 0.962308 0.034 Uiso 1 1 calc R U . . .
C4 C 1.0988(3) 0.7331(3) 0.9297(2) 0.0214(7) Uani 1 1 d . . . . .
H4A H 1.132747 0.774479 0.996957 0.026 Uiso 1 1 calc R U . . .
H4AB H 1.175524 0.705889 0.906512 0.026 Uiso 1 1 calc R U . . .
C5 C 1.0311(3) 0.8154(3) 0.8696(2) 0.0176(6) Uani 1 1 d . . . . .
C6 C 0.9784(3) 0.7463(3) 0.7659(2) 0.0157(6) Uani 1 1 d . . . . .
H6A H 0.936535 0.797799 0.725232 0.019 Uiso 1 1 calc R U . . .
H6AB H 1.054346 0.717605 0.742394 0.019 Uiso 1 1 calc R U . . .
C7 C 0.7610(3) 0.6902(3) 0.7978(3) 0.0273(8) Uani 1 1 d . . . . .
H7A H 0.717266 0.743892 0.760107 0.033 Uiso 1 1 calc R U . . .
H7AB H 0.693702 0.625574 0.792438 0.033 Uiso 1 1 calc R U . . .
C8 C 0.8137(4) 0.7524(4) 0.9024(3) 0.0345(9) Uani 1 1 d . . . . .
H8 H 0.737465 0.780031 0.927547 0.041 Uiso 1 1 calc R U . . .
C9 C 0.8836(4) 0.6720(4) 0.9619(3) 0.0375(10) Uani 1 1 d . . . . .
H9A H 0.917336 0.713251 1.029214 0.045 Uiso 1 1 calc R U . . .
H9AB H 0.819639 0.605960 0.959143 0.045 Uiso 1 1 calc R U . . .
C10 C 0.9132(4) 0.8561(3) 0.9089(3) 0.0291(8) Uani 1 1 d . . . . .
H10A H 0.946879 0.897801 0.976046 0.035 Uiso 1 1 calc R U . . .
H10B H 0.867592 0.909521 0.871729 0.035 Uiso 1 1 calc R U . . .
C11 C 0.8228(3) 0.5791(3) 0.6539(2) 0.0162(6) Uani 1 1 d . . . . .
C12 C 0.7062(3) 0.5029(3) 0.6253(2) 0.0221(7) Uani 1 1 d . . . . .
H12 H 0.659477 0.491946 0.671169 0.027 Uiso 1 1 calc R U . . .
C13 C 0.6565(3) 0.4425(3) 0.5315(2) 0.0218(7) Uani 1 1 d . . . . .
H13 H 0.576594 0.391772 0.514717 0.026 Uiso 1 1 calc R U . . .
C14 C 0.7220(3) 0.4553(3) 0.4617(2) 0.0166(6) Uani 1 1 d . . . . .
C15 C 0.8373(3) 0.5314(3) 0.4894(2) 0.0241(7) Uani 1 1 d . . . . .
H15 H 0.883263 0.543017 0.443278 0.029 Uiso 1 1 calc R U . . .
C16 C 0.8872(3) 0.5912(3) 0.5834(2) 0.0245(7) Uani 1 1 d . . . . .
H16 H 0.967261 0.641699 0.600010 0.029 Uiso 1 1 calc R U . . .
C17 C 0.6717(3) 0.3936(3) 0.3603(2) 0.0163(6) Uani 1 1 d . . . . .
C18 C 0.6382(3) 0.2742(3) 0.3339(2) 0.0188(6) Uani 1 1 d . . . . .
C19 C 0.5953(3) 0.2195(3) 0.2384(2) 0.0203(6) Uani 1 1 d . . . . .
H19 H 0.571565 0.138759 0.220805 0.024 Uiso 1 1 calc R U . . .
C20 C 0.5872(3) 0.2835(3) 0.1688(2) 0.0186(6) Uani 1 1 d . . . . .
H20 H 0.556969 0.245588 0.103646 0.022 Uiso 1 1 calc R U . . .
C21 C 0.6221(3) 0.4010(3) 0.1920(2) 0.0174(6) Uani 1 1 d . . . . .
C22 C 0.6635(3) 0.4544(3) 0.2881(2) 0.0178(6) Uani 1 1 d . . . . .
H22 H 0.687001 0.535165 0.305095 0.021 Uiso 1 1 calc R U . . .
C23 C 0.6454(5) 0.0944(3) 0.3823(3) 0.0405(10) Uani 1 1 d . . . . .
H23A H 0.555433 0.062711 0.343885 0.061 Uiso 1 1 calc R U . . .
H23B H 0.665898 0.064019 0.440435 0.061 Uiso 1 1 calc R U . . .
H23C H 0.710226 0.072477 0.345622 0.061 Uiso 1 1 calc R U . . .
C24 C 0.6242(4) 0.4665(3) 0.1144(2) 0.0229(7) Uani 1 1 d . . . . .
H24A H 0.716675 0.475051 0.108000 0.027 Uiso 1 1 calc R U . . .
H24B H 0.568055 0.419799 0.053414 0.027 Uiso 1 1 calc R U . . .
C25 C 0.5765(3) 0.5844(3) 0.1294(2) 0.0186(6) Uani 1 1 d . . . . .
C26 C 0.6558(3) 0.6799(3) 0.1255(2) 0.0183(6) Uani 1 1 d . . . . .
H26 H 0.743099 0.670832 0.118196 0.022 Uiso 1 1 calc R U . . .
C27 C 0.6122(3) 0.7887(3) 0.1320(2) 0.0168(6) Uani 1 1 d . . . . .
C28 C 0.4840(3) 0.8015(3) 0.1446(2) 0.0196(6) Uani 1 1 d . . . . .
C29 C 0.4035(3) 0.7067(3) 0.1500(2) 0.0227(7) Uani 1 1 d . . . . .
H29 H 0.316881 0.715497 0.158851 0.027 Uiso 1 1 calc R U . . .
C30 C 0.4501(4) 0.5998(3) 0.1423(2) 0.0216(7) Uani 1 1 d . . . . .
H30 H 0.394596 0.535781 0.146011 0.026 Uiso 1 1 calc R U . . .
C31 C 0.3360(4) 0.9331(3) 0.1912(3) 0.0268(7) Uani 1 1 d . . . . .
H31A H 0.328967 1.015802 0.203845 0.040 Uiso 1 1 calc R U . . .
H31B H 0.348556 0.906109 0.250808 0.040 Uiso 1 1 calc R U . . .
H31C H 0.254117 0.892702 0.145707 0.040 Uiso 1 1 calc R U . . .
C32 C 0.7019(3) 0.8888(3) 0.1294(2) 0.0185(6) Uani 1 1 d . . . . .
C33 C 0.8289(4) 0.9140(3) 0.1909(3) 0.0267(8) Uani 1 1 d . . . . .
H33 H 0.858270 0.866389 0.234560 0.032 Uiso 1 1 calc R U . . .
C34 C 0.9134(4) 1.0072(3) 0.1897(3) 0.0279(8) Uani 1 1 d . . . . .
H34 H 1.000295 1.021411 0.231766 0.033 Uiso 1 1 calc R U . . .
C35 C 0.8741(3) 1.0809(3) 0.1281(2) 0.0178(6) Uani 1 1 d . . . . .
C36 C 0.7482(3) 1.0536(3) 0.0651(2) 0.0170(6) Uani 1 1 d . . . . .
H36 H 0.719243 1.100565 0.020874 0.020 Uiso 1 1 calc R U . . .
C37 C 0.6637(3) 0.9594(3) 0.0653(2) 0.0170(6) Uani 1 1 d . . . . .
H37 H 0.578585 0.942778 0.020948 0.020 Uiso 1 1 calc R U . . .
C38 C 0.3597(4) 0.2153(3) 0.4780(3) 0.0316(8) Uani 1 1 d . . . . .
H38A H 0.434122 0.225273 0.448349 0.038 Uiso 1 1 calc R U . . .
H38B H 0.304413 0.279148 0.469569 0.038 Uiso 1 1 calc R U . . .
C39 C 0.9073(7) 0.2756(5) 0.6033(4) 0.0615(16) Uani 1 1 d . . . . .
H39A H 0.953206 0.354644 0.621209 0.074 Uiso 1 1 calc R U . . .
H39B H 0.820308 0.275909 0.557697 0.074 Uiso 1 1 calc R U . . .
O1 O 0.6523(3) 0.2168(2) 0.40720(17) 0.0278(6) Uani 1 1 d . . . . .
O2 O 0.4470(2) 0.9106(2) 0.15247(18) 0.0250(5) Uani 1 1 d . . . . .
Br1 Br 0.25304(4) 0.07256(3) 0.41324(3) 0.03181(12) Uani 1 1 d . . . . .
Br2 Br 0.43155(5) 0.22434(4) 0.61158(3) 0.03890(13) Uani 1 1 d . . . . .
Br3 Br 1.01153(6) 0.17610(5) 0.54179(4) 0.05252(16) Uani 1 1 d . . . . .
Br4 Br 0.87649(7) 0.23392(5) 0.71298(5) 0.0663(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C11 1.529(4) . ?
C1 C6 1.538(4) . ?
C1 C7 1.544(4) . ?
C1 C2 1.545(5) . ?
C2 C3 1.535(5) . ?
C2 H2A 0.9900 . ?
C2 H2AB 0.9900 . ?
C3 C9 1.523(6) . ?
C3 C4 1.540(5) . ?
C3 H3 1.0000 . ?
C4 C5 1.540(5) . ?
C4 H4A 0.9900 . ?
C4 H4AB 0.9900 . ?
C5 C35 1.527(4) 2_776 ?
C5 C10 1.543(5) . ?
C5 C6 1.546(4) . ?
C6 H6A 0.9900 . ?
C6 H6AB 0.9900 . ?
C7 C8 1.533(5) . ?
C7 H7A 0.9900 . ?
C7 H7AB 0.9900 . ?
C8 C9 1.526(7) . ?
C8 C10 1.541(5) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9900 . ?
C9 H9AB 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C16 1.395(5) . ?
C11 C12 1.397(4) . ?
C12 C13 1.392(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.396(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(5) . ?
C14 C17 1.490(4) . ?
C15 C16 1.393(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.395(4) . ?
C17 C18 1.404(4) . ?
C18 O1 1.377(4) . ?
C18 C19 1.389(5) . ?
C19 C20 1.389(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.384(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.393(4) . ?
C21 C24 1.515(4) . ?
C22 H22 0.9500 . ?
C23 O1 1.430(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.514(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.388(5) . ?
C25 C30 1.390(5) . ?
C26 C27 1.394(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.403(5) . ?
C27 C32 1.485(4) . ?
C28 O2 1.372(4) . ?
C28 C29 1.395(5) . ?
C29 C30 1.386(5) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 O2 1.425(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.389(5) . ?
C32 C37 1.394(4) . ?
C33 C34 1.384(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.396(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(4) . ?
C36 C37 1.388(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 Br2 1.919(4) . ?
C38 Br1 1.921(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 Br4 1.882(5) . ?
C39 Br3 1.904(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?

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 C1 C6 111.2(3) . . ?
C11 C1 C7 110.6(3) . . ?
C6 C1 C7 108.4(3) . . ?
C11 C1 C2 110.3(3) . . ?
C6 C1 C2 107.5(2) . . ?
C7 C1 C2 108.7(3) . . ?
C3 C2 C1 110.3(3) . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2AB 109.6 . . ?
C1 C2 H2AB 109.6 . . ?
H2A C2 H2AB 108.1 . . ?
C9 C3 C2 109.7(3) . . ?
C9 C3 C4 109.1(3) . . ?
C2 C3 C4 110.0(3) . . ?
C9 C3 H3 109.3 . . ?
C2 C3 H3 109.3 . . ?
C4 C3 H3 109.3 . . ?
C5 C4 C3 110.5(3) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4AB 109.5 . . ?
C3 C4 H4AB 109.5 . . ?
H4A C4 H4AB 108.1 . . ?
C35 C5 C4 112.9(3) 2_776 . ?
C35 C5 C10 109.8(3) 2_776 . ?
C4 C5 C10 107.6(3) . . ?
C35 C5 C6 109.3(3) 2_776 . ?
C4 C5 C6 107.4(3) . . ?
C10 C5 C6 109.8(3) . . ?
C1 C6 C5 112.2(3) . . ?
C1 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
C1 C6 H6AB 109.2 . . ?
C5 C6 H6AB 109.2 . . ?
H6A C6 H6AB 107.9 . . ?
C8 C7 C1 110.6(3) . . ?
C8 C7 H7A 109.5 . . ?
C1 C7 H7A 109.5 . . ?
C8 C7 H7AB 109.5 . . ?
C1 C7 H7AB 109.5 . . ?
H7A C7 H7AB 108.1 . . ?
C9 C8 C7 110.6(3) . . ?
C9 C8 C10 109.4(3) . . ?
C7 C8 C10 108.8(3) . . ?
C9 C8 H8 109.3 . . ?
C7 C8 H8 109.3 . . ?
C10 C8 H8 109.3 . . ?
C3 C9 C8 109.3(3) . . ?
C3 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
C3 C9 H9AB 109.8 . . ?
C8 C9 H9AB 109.8 . . ?
H9A C9 H9AB 108.3 . . ?
C8 C10 C5 110.1(3) . . ?
C8 C10 H10A 109.6 . . ?
C5 C10 H10A 109.6 . . ?
C8 C10 H10B 109.6 . . ?
C5 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C16 C11 C12 116.4(3) . . ?
C16 C11 C1 122.6(3) . . ?
C12 C11 C1 121.0(3) . . ?
C13 C12 C11 121.9(3) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C14 121.1(3) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 117.3(3) . . ?
C15 C14 C17 119.7(3) . . ?
C13 C14 C17 123.0(3) . . ?
C14 C15 C16 121.4(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C15 C16 C11 121.8(3) . . ?
C15 C16 H16 119.1 . . ?
C11 C16 H16 119.1 . . ?
C22 C17 C18 118.0(3) . . ?
C22 C17 C14 119.7(3) . . ?
C18 C17 C14 122.2(3) . . ?
O1 C18 C19 123.3(3) . . ?
O1 C18 C17 116.2(3) . . ?
C19 C18 C17 120.4(3) . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C21 C20 C19 121.6(3) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C20 C21 C22 117.8(3) . . ?
C20 C21 C24 120.2(3) . . ?
C22 C21 C24 121.8(3) . . ?
C21 C22 C17 122.4(3) . . ?
C21 C22 H22 118.8 . . ?
C17 C22 H22 118.8 . . ?
O1 C23 H23A 109.5 . . ?
O1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C21 115.8(3) . . ?
C25 C24 H24A 108.3 . . ?
C21 C24 H24A 108.3 . . ?
C25 C24 H24B 108.3 . . ?
C21 C24 H24B 108.3 . . ?
H24A C24 H24B 107.4 . . ?
C26 C25 C30 117.9(3) . . ?
C26 C25 C24 120.5(3) . . ?
C30 C25 C24 121.5(3) . . ?
C25 C26 C27 122.5(3) . . ?
C25 C26 H26 118.7 . . ?
C27 C26 H26 118.7 . . ?
C26 C27 C28 118.2(3) . . ?
C26 C27 C32 120.5(3) . . ?
C28 C27 C32 121.2(3) . . ?
O2 C28 C29 124.0(3) . . ?
O2 C28 C27 115.9(3) . . ?
C29 C28 C27 120.0(3) . . ?
C30 C29 C28 119.9(3) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 121.3(3) . . ?
C29 C30 H30 119.3 . . ?
C25 C30 H30 119.3 . . ?
O2 C31 H31A 109.5 . . ?
O2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C37 117.6(3) . . ?
C33 C32 C27 120.5(3) . . ?
C37 C32 C27 122.0(3) . . ?
C34 C33 C32 121.1(3) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C34 C35 121.6(3) . . ?
C33 C34 H34 119.2 . . ?
C35 C34 H34 119.2 . . ?
C36 C35 C34 116.9(3) . . ?
C36 C35 C5 122.9(3) . 2_776 ?
C34 C35 C5 120.2(3) . 2_776 ?
C37 C36 C35 121.6(3) . . ?
C37 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
C36 C37 C32 121.1(3) . . ?
C36 C37 H37 119.5 . . ?
C32 C37 H37 119.5 . . ?
Br2 C38 Br1 113.2(2) . . ?
Br2 C38 H38A 108.9 . . ?
Br1 C38 H38A 108.9 . . ?
Br2 C38 H38B 108.9 . . ?
Br1 C38 H38B 108.9 . . ?
H38A C38 H38B 107.8 . . ?
Br4 C39 Br3 113.7(2) . . ?
Br4 C39 H39A 108.8 . . ?
Br3 C39 H39A 108.8 . . ?
Br4 C39 H39B 108.8 . . ?
Br3 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
C18 O1 C23 117.0(3) . . ?
C28 O2 C31 117.0(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
C11 C1 C2 C3 -179.7(3) . . . . ?
C6 C1 C2 C3 58.9(3) . . . . ?
C7 C1 C2 C3 -58.3(3) . . . . ?
C1 C2 C3 C9 60.6(4) . . . . ?
C1 C2 C3 C4 -59.5(4) . . . . ?
C9 C3 C4 C5 -60.9(4) . . . . ?
C2 C3 C4 C5 59.5(4) . . . . ?
C3 C4 C5 C35 -179.0(3) . . . 2_776 ?
C3 C4 C5 C10 59.7(3) . . . . ?
C3 C4 C5 C6 -58.5(3) . . . . ?
C11 C1 C6 C5 178.6(3) . . . . ?
C7 C1 C6 C5 56.8(3) . . . . ?
C2 C1 C6 C5 -60.6(3) . . . . ?
C35 C5 C6 C1 -176.8(3) 2_776 . . . ?
C4 C5 C6 C1 60.4(3) . . . . ?
C10 C5 C6 C1 -56.3(4) . . . . ?
C11 C1 C7 C8 178.3(3) . . . . ?
C6 C1 C7 C8 -59.6(4) . . . . ?
C2 C1 C7 C8 57.1(4) . . . . ?
C1 C7 C8 C9 -58.3(4) . . . . ?
C1 C7 C8 C10 61.9(4) . . . . ?
C2 C3 C9 C8 -60.2(4) . . . . ?
C4 C3 C9 C8 60.4(4) . . . . ?
C7 C8 C9 C3 59.3(4) . . . . ?
C10 C8 C9 C3 -60.6(4) . . . . ?
C9 C8 C10 C5 60.8(4) . . . . ?
C7 C8 C10 C5 -60.2(4) . . . . ?
C35 C5 C10 C8 177.3(3) 2_776 . . . ?
C4 C5 C10 C8 -59.4(4) . . . . ?
C6 C5 C10 C8 57.2(4) . . . . ?
C6 C1 C11 C16 17.1(4) . . . . ?
C7 C1 C11 C16 137.5(3) . . . . ?
C2 C1 C11 C16 -102.2(4) . . . . ?
C6 C1 C11 C12 -163.4(3) . . . . ?
C7 C1 C11 C12 -43.0(4) . . . . ?
C2 C1 C11 C12 77.4(4) . . . . ?
C16 C11 C12 C13 -0.2(5) . . . . ?
C1 C11 C12 C13 -179.7(3) . . . . ?
C11 C12 C13 C14 0.3(5) . . . . ?
C12 C13 C14 C15 -0.8(5) . . . . ?
C12 C13 C14 C17 -179.3(3) . . . . ?
C13 C14 C15 C16 1.1(5) . . . . ?
C17 C14 C15 C16 179.7(3) . . . . ?
C14 C15 C16 C11 -1.1(6) . . . . ?
C12 C11 C16 C15 0.6(5) . . . . ?
C1 C11 C16 C15 -179.9(3) . . . . ?
C15 C14 C17 C22 -46.9(4) . . . . ?
C13 C14 C17 C22 131.5(3) . . . . ?
C15 C14 C17 C18 129.7(4) . . . . ?
C13 C14 C17 C18 -51.9(5) . . . . ?
C22 C17 C18 O1 177.7(3) . . . . ?
C14 C17 C18 O1 1.0(5) . . . . ?
C22 C17 C18 C19 -1.5(5) . . . . ?
C14 C17 C18 C19 -178.1(3) . . . . ?
O1 C18 C19 C20 -178.3(3) . . . . ?
C17 C18 C19 C20 0.8(5) . . . . ?
C18 C19 C20 C21 0.6(5) . . . . ?
C19 C20 C21 C22 -1.3(5) . . . . ?
C19 C20 C21 C24 174.4(3) . . . . ?
C20 C21 C22 C17 0.6(5) . . . . ?
C24 C21 C22 C17 -175.0(3) . . . . ?
C18 C17 C22 C21 0.8(5) . . . . ?
C14 C17 C22 C21 177.5(3) . . . . ?
C20 C21 C24 C25 142.5(3) . . . . ?
C22 C21 C24 C25 -42.0(5) . . . . ?
C21 C24 C25 C26 126.4(3) . . . . ?
C21 C24 C25 C30 -57.1(4) . . . . ?
C30 C25 C26 C27 -1.4(5) . . . . ?
C24 C25 C26 C27 175.2(3) . . . . ?
C25 C26 C27 C28 1.2(5) . . . . ?
C25 C26 C27 C32 178.7(3) . . . . ?
C26 C27 C28 O2 178.7(3) . . . . ?
C32 C27 C28 O2 1.1(4) . . . . ?
C26 C27 C28 C29 -0.2(4) . . . . ?
C32 C27 C28 C29 -177.8(3) . . . . ?
O2 C28 C29 C30 -179.2(3) . . . . ?
C27 C28 C29 C30 -0.4(5) . . . . ?
C28 C29 C30 C25 0.1(5) . . . . ?
C26 C25 C30 C29 0.8(5) . . . . ?
C24 C25 C30 C29 -175.8(3) . . . . ?
C26 C27 C32 C33 -52.5(4) . . . . ?
C28 C27 C32 C33 125.0(4) . . . . ?
C26 C27 C32 C37 126.5(3) . . . . ?
C28 C27 C32 C37 -56.0(4) . . . . ?
C37 C32 C33 C34 1.3(5) . . . . ?
C27 C32 C33 C34 -179.7(3) . . . . ?
C32 C33 C34 C35 1.2(6) . . . . ?
C33 C34 C35 C36 -2.7(6) . . . . ?
C33 C34 C35 C5 178.6(3) . . . 2_776 ?
C34 C35 C36 C37 1.9(5) . . . . ?
C5 C35 C36 C37 -179.4(3) 2_776 . . . ?
C35 C36 C37 C32 0.5(5) . . . . ?
C33 C32 C37 C36 -2.1(5) . . . . ?
C27 C32 C37 C36 178.9(3) . . . . ?
C19 C18 O1 C23 11.6(5) . . . . ?
C17 C18 O1 C23 -167.5(3) . . . . ?
C29 C28 O2 C31 16.0(5) . . . . ?
C27 C28 O2 C31 -162.9(3) . . . . ?

_refine_diff_density_max         1.570
_refine_diff_density_min         -2.026
_refine_diff_density_rms         0.116



####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 2133056'
loop_
_audit_author_name
_audit_author_address
'Tadashi Hyodo'
;Tokushima Bunri University
Japan
;
_audit_update_record             
;
2022-01-07 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57.50 H49.50 Cl4.50 N4 O10'
_chemical_formula_weight         1116.03

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   24.0138(10)
_cell_length_b                   7.9580(3)
_cell_length_c                   27.4313(12)
_cell_angle_alpha                90
_cell_angle_beta                 98.369(2)
_cell_angle_gamma                90
_cell_volume                     5186.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9742
_cell_measurement_theta_min      3.61
_cell_measurement_theta_max      78.44

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_F_000             2316
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.855
_shelx_estimated_absorpt_T_min   0.804
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8274
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            60354
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_av_R_equivalents  0.1001
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.644
_diffrn_reflns_theta_max         79.444
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10894
_reflns_number_gt                7759
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (Hübschle et al., 2011)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0877P)²+4.6133P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10894
_refine_ls_number_parameters     703
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.1796
_refine_ls_wR_factor_gt          0.1633
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C58 C 0.7252(6) 0.165(2) 0.2683(5) 0.121(6) Uani 0.5 1 d . . P A -1
H58 H 0.683851 0.162768 0.256055 0.145 Uiso 0.5 1 calc R U P A -1
Cl4 Cl 0.7423(2) 0.3464(10) 0.2448(3) 0.177(3) Uani 0.5 1 d . . P A -1
Cl5 Cl 0.72472(10) 0.1146(5) 0.32171(10) 0.0900(9) Uani 0.5 1 d . . P A -1
Cl6 Cl 0.7501(2) 0.0361(18) 0.22297(17) 0.277(6) Uani 0.5 1 d . . P A -1
C1 C 0.23875(11) 0.4599(3) 0.52886(9) 0.0228(5) Uani 1 1 d . . . . .
C2 C 0.17901(12) 0.3910(4) 0.51440(10) 0.0285(6) Uani 1 1 d . . . . .
H2A H 0.152307 0.455543 0.531411 0.034 Uiso 1 1 calc R U . . .
H2AB H 0.167486 0.403096 0.478430 0.034 Uiso 1 1 calc R U . . .
C3 C 0.17758(13) 0.2056(4) 0.52883(11) 0.0330(6) Uani 1 1 d . . . . .
H3 H 0.138812 0.160074 0.518653 0.040 Uiso 1 1 calc R U . . .
C4 C 0.19368(14) 0.1864(4) 0.58463(12) 0.0377(7) Uani 1 1 d . . . . .
H4A H 0.192271 0.066415 0.593957 0.045 Uiso 1 1 calc R U . . .
H4AB H 0.166846 0.249282 0.601929 0.045 Uiso 1 1 calc R U . . .
C5 C 0.25343(13) 0.2552(4) 0.59943(11) 0.0330(7) Uani 1 1 d . . . . .
H5 H 0.264336 0.243804 0.635874 0.040 Uiso 1 1 calc R U . . .
C6 C 0.29511(13) 0.1573(4) 0.57315(11) 0.0318(6) Uani 1 1 d . . . . .
H6A H 0.294595 0.037222 0.582559 0.038 Uiso 1 1 calc R U . . .
H6AB H 0.333625 0.200929 0.583456 0.038 Uiso 1 1 calc R U . . .
C7 C 0.27967(12) 0.1740(4) 0.51707(10) 0.0276(6) Uani 1 1 d . . . . .
C8 C 0.28019(12) 0.3605(3) 0.50271(10) 0.0251(6) Uani 1 1 d . . . . .
H8A H 0.318581 0.406576 0.511864 0.030 Uiso 1 1 calc R U . . .
H8AB H 0.269754 0.371869 0.466592 0.030 Uiso 1 1 calc R U . . .
C9 C 0.25514(12) 0.4413(4) 0.58506(10) 0.0292(6) Uani 1 1 d . . . . .
H9A H 0.293473 0.486604 0.595200 0.035 Uiso 1 1 calc R U . . .
H9AB H 0.228641 0.506146 0.602233 0.035 Uiso 1 1 calc R U . . .
C10 C 0.21944(13) 0.1074(4) 0.50260(11) 0.0328(6) Uani 1 1 d . . . . .
H10A H 0.208535 0.117467 0.466503 0.039 Uiso 1 1 calc R U . . .
H10B H 0.218145 -0.012977 0.511427 0.039 Uiso 1 1 calc R U . . .
C11 C 0.31891(13) 0.0699(4) 0.48928(11) 0.0332(6) Uani 1 1 d . . . . .
H11A H 0.323329 -0.042754 0.504648 0.040 Uiso 1 1 calc R U . . .
H11B H 0.300204 0.054498 0.454959 0.040 Uiso 1 1 calc R U . . .
C12 C 0.39083(12) 0.2134(4) 0.44559(10) 0.0300(6) Uani 1 1 d . . . . .
C13 C 0.42105(13) 0.1232(4) 0.52514(10) 0.0302(6) Uani 1 1 d . . . . .
C14 C 0.46905(13) 0.2037(4) 0.50627(10) 0.0298(6) Uani 1 1 d . . . . .
C15 C 0.45145(12) 0.2556(4) 0.45836(10) 0.0279(6) Uani 1 1 d . . . . .
C16 C 0.48721(13) 0.3352(4) 0.43051(10) 0.0316(6) Uani 1 1 d . . . . .
H16 H 0.475055 0.369952 0.397548 0.038 Uiso 1 1 calc R U . . .
C17 C 0.54213(13) 0.3613(4) 0.45365(11) 0.0332(7) Uani 1 1 d . . . . .
C18 C 0.56043(13) 0.3105(4) 0.50175(11) 0.0354(7) Uani 1 1 d . . . . .
H18 H 0.598189 0.331210 0.516251 0.042 Uiso 1 1 calc R U . . .
C19 C 0.52384(13) 0.2298(4) 0.52868(10) 0.0339(7) Uani 1 1 d . . . . .
H19 H 0.535962 0.193449 0.561498 0.041 Uiso 1 1 calc R U . . .
C20 C 0.58139(12) 0.4281(5) 0.38083(11) 0.0357(7) Uani 1 1 d . . . . .
C21 C 0.57937(13) 0.2688(5) 0.35957(12) 0.0386(7) Uani 1 1 d . . . . .
H21 H 0.575025 0.172430 0.379109 0.046 Uiso 1 1 calc R U . . .
C22 C 0.58370(14) 0.2503(4) 0.30979(12) 0.0385(7) Uani 1 1 d . . . . .
H22 H 0.581509 0.142828 0.294558 0.046 Uiso 1 1 calc R U . . .
C23 C 0.59133(12) 0.3947(4) 0.28330(11) 0.0338(7) Uani 1 1 d . . . . .
C24 C 0.59337(12) 0.5531(4) 0.30561(11) 0.0327(7) Uani 1 1 d . . . . .
C25 C 0.58820(12) 0.5738(4) 0.35460(11) 0.0355(7) Uani 1 1 d . . . . .
H25 H 0.589239 0.681682 0.369549 0.043 Uiso 1 1 calc R U . . .
C26 C 0.59864(13) 0.4174(4) 0.23096(12) 0.0373(7) Uani 1 1 d . . . . .
C27 C 0.60154(12) 0.6808(4) 0.26760(11) 0.0346(7) Uani 1 1 d . . . . .
C28 C 0.61884(13) 0.6669(5) 0.17954(11) 0.0361(7) Uani 1 1 d . . . . .
H28A H 0.642771 0.585172 0.164970 0.043 Uiso 1 1 calc R U . . .
H28B H 0.642264 0.767006 0.189430 0.043 Uiso 1 1 calc R U . . .
C29 C 0.57082(12) 0.7198(4) 0.13967(10) 0.0303(6) Uani 1 1 d . . . . .
C30 C 0.59837(12) 0.7862(4) 0.09624(10) 0.0314(6) Uani 1 1 d . . . . .
H30A H 0.623120 0.882448 0.107341 0.038 Uiso 1 1 calc R U . . .
H30B H 0.621876 0.696822 0.084542 0.038 Uiso 1 1 calc R U . . .
C31 C 0.55352(12) 0.8418(4) 0.05397(10) 0.0307(6) Uani 1 1 d . . . . .
H31 H 0.572215 0.884321 0.026099 0.037 Uiso 1 1 calc R U . . .
C32 C 0.51874(12) 0.9826(4) 0.07235(10) 0.0290(6) Uani 1 1 d . . . . .
H32A H 0.489987 1.021448 0.045118 0.035 Uiso 1 1 calc R U . . .
H32B H 0.543531 1.078882 0.083347 0.035 Uiso 1 1 calc R U . . .
C33 C 0.48956(11) 0.9204(4) 0.11553(9) 0.0264(6) Uani 1 1 d . . . . .
C34 C 0.53516(11) 0.8627(4) 0.15761(10) 0.0276(6) Uani 1 1 d . . . . .
H34A H 0.517121 0.822464 0.185686 0.033 Uiso 1 1 calc R U . . .
H34B H 0.559828 0.958700 0.169098 0.033 Uiso 1 1 calc R U . . .
C35 C 0.45210(11) 0.7693(4) 0.09727(10) 0.0294(6) Uani 1 1 d . . . . .
H35A H 0.432871 0.727123 0.124409 0.035 Uiso 1 1 calc R U . . .
H35B H 0.422935 0.805437 0.070008 0.035 Uiso 1 1 calc R U . . .
C36 C 0.48724(12) 0.6288(4) 0.07940(11) 0.0315(6) Uani 1 1 d . . . . .
H36 H 0.462283 0.531654 0.068034 0.038 Uiso 1 1 calc R U . . .
C37 C 0.53228(13) 0.5721(4) 0.12160(11) 0.0333(7) Uani 1 1 d . . . . .
H37A H 0.554918 0.480267 0.110058 0.040 Uiso 1 1 calc R U . . .
H37B H 0.513961 0.528632 0.149122 0.040 Uiso 1 1 calc R U . . .
C38 C 0.51576(13) 0.6933(4) 0.03638(11) 0.0344(7) Uani 1 1 d . . . . .
H38A H 0.538490 0.602439 0.024423 0.041 Uiso 1 1 calc R U . . .
H38B H 0.486843 0.728630 0.008824 0.041 Uiso 1 1 calc R U . . .
C39 C 0.45539(12) 1.0697(4) 0.12993(10) 0.0281(6) Uani 1 1 d . . . . .
H39A H 0.481936 1.161751 0.141111 0.034 Uiso 1 1 calc R U . . .
H39B H 0.430987 1.109586 0.099952 0.034 Uiso 1 1 calc R U . . .
C40 C 0.43089(12) 1.1165(4) 0.21491(10) 0.0311(6) Uani 1 1 d . . . . .
C41 C 0.36381(12) 0.9863(4) 0.15845(10) 0.0271(6) Uani 1 1 d . . . . .
C42 C 0.33939(12) 1.0139(4) 0.20514(10) 0.0268(6) Uani 1 1 d . . . . .
C43 C 0.37952(12) 1.0933(4) 0.23874(10) 0.0295(6) Uani 1 1 d . . . . .
C44 C 0.36731(13) 1.1439(4) 0.28419(10) 0.0318(6) Uani 1 1 d . . . . .
H44 H 0.394792 1.198100 0.307333 0.038 Uiso 1 1 calc R U . . .
C45 C 0.31333(13) 1.1128(4) 0.29491(10) 0.0313(6) Uani 1 1 d . . . . .
H45 H 0.303478 1.146443 0.325762 0.038 Uiso 1 1 calc R U . . .
C46 C 0.27379(12) 1.0325(4) 0.26063(10) 0.0290(6) Uani 1 1 d . . . . .
C47 C 0.28577(12) 0.9813(4) 0.21486(10) 0.0287(6) Uani 1 1 d . . . . .
H47 H 0.258505 0.926896 0.191577 0.034 Uiso 1 1 calc R U . . .
C48 C 0.20764(12) 0.9497(4) 0.31373(10) 0.0275(6) Uani 1 1 d . . . . .
C49 C 0.15341(12) 0.9802(4) 0.32396(10) 0.0292(6) Uani 1 1 d . . . . .
H49 H 0.127834 1.042858 0.301254 0.035 Uiso 1 1 calc R U . . .
C50 C 0.13631(11) 0.9204(4) 0.36675(10) 0.0275(6) Uani 1 1 d . . . . .
H50 H 0.099182 0.939301 0.373636 0.033 Uiso 1 1 calc R U . . .
C51 C 0.17525(11) 0.8319(3) 0.39923(9) 0.0233(5) Uani 1 1 d . . . . .
C52 C 0.22882(11) 0.8025(3) 0.38852(9) 0.0228(5) Uani 1 1 d . . . . .
C53 C 0.24676(11) 0.8579(4) 0.34601(10) 0.0259(6) Uani 1 1 d . . . . .
H53 H 0.283593 0.835272 0.338935 0.031 Uiso 1 1 calc R U . . .
C54 C 0.17110(11) 0.7637(3) 0.44862(9) 0.0236(5) Uani 1 1 d . . . . .
C55 C 0.26116(11) 0.7142(3) 0.43180(9) 0.0228(5) Uani 1 1 d . . . . .
C56 C 0.24155(12) 0.6468(3) 0.51770(9) 0.0243(6) Uani 1 1 d . . . . .
H56A H 0.217418 0.707326 0.538223 0.029 Uiso 1 1 calc R U . . .
H56B H 0.280709 0.685374 0.527858 0.029 Uiso 1 1 calc R U . . .
C57 C 0.42254(14) 0.7108(5) 0.30673(12) 0.0465(9) Uani 1 1 d . . . . .
H57 H 0.396060 0.763894 0.279565 0.056 Uiso 1 1 calc R U . . .
N1 N 0.37498(10) 0.1394(3) 0.48778(8) 0.0283(5) Uani 1 1 d . . . . .
N2 N 0.60215(11) 0.5924(3) 0.22366(9) 0.0338(6) Uani 1 1 d . . . . .
N3 N 0.41980(10) 1.0410(3) 0.16826(8) 0.0275(5) Uani 1 1 d . . . . .
N4 N 0.22419(9) 0.6951(3) 0.46591(8) 0.0225(5) Uani 1 1 d . . . . .
O1 O 0.35980(9) 0.2338(3) 0.40683(7) 0.0391(5) Uani 1 1 d . . . . .
O2 O 0.42011(10) 0.0544(3) 0.56440(8) 0.0403(5) Uani 1 1 d . . . . .
O3 O 0.58088(9) 0.4490(3) 0.43122(8) 0.0437(6) Uani 1 1 d . . . . .
O4 O 0.60711(10) 0.8316(3) 0.27268(8) 0.0426(5) Uani 1 1 d . . . . .
O5 O 0.60260(11) 0.3124(3) 0.19967(8) 0.0449(6) Uani 1 1 d . . . . .
O6 O 0.47369(9) 1.1915(3) 0.23082(8) 0.0404(5) Uani 1 1 d . . . . .
O7 O 0.34041(8) 0.9346(3) 0.11950(7) 0.0314(5) Uani 1 1 d . . . . .
O8 O 0.21865(8) 1.0108(3) 0.26897(7) 0.0343(5) Uani 1 1 d . . . . .
O9 O 0.13215(8) 0.7702(3) 0.47199(7) 0.0291(4) Uani 1 1 d . . . . .
O10 O 0.31034(8) 0.6735(3) 0.43766(7) 0.0282(4) Uani 1 1 d . . . . .
Cl1 Cl 0.38421(4) 0.65221(15) 0.35386(3) 0.0565(3) Uani 1 1 d . . . . .
Cl2 Cl 0.45209(4) 0.53008(14) 0.28312(3) 0.0557(3) Uani 1 1 d . . . . .
Cl3 Cl 0.47485(4) 0.85783(13) 0.32832(4) 0.0597(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C58 Cl5 1.520(11) . ?
C58 Cl4 1.659(16) . ?
C58 Cl6 1.781(17) . ?
C58 H58 1.0000 . ?
C1 C56 1.522(4) . ?
C1 C8 1.529(4) . ?
C1 C2 1.533(4) . ?
C1 C9 1.542(4) . ?
C2 C3 1.529(4) . ?
C2 H2A 0.9900 . ?
C2 H2AB 0.9900 . ?
C3 C4 1.531(4) . ?
C3 C10 1.532(4) . ?
C3 H3 1.0000 . ?
C4 C5 1.534(4) . ?
C4 H4A 0.9900 . ?
C4 H4AB 0.9900 . ?
C5 C6 1.529(4) . ?
C5 C9 1.535(4) . ?
C5 H5 1.0000 . ?
C6 C7 1.535(4) . ?
C6 H6A 0.9900 . ?
C6 H6AB 0.9900 . ?
C7 C8 1.536(4) . ?
C7 C10 1.537(4) . ?
C7 C11 1.538(4) . ?
C8 H8A 0.9900 . ?
C8 H8AB 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9AB 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N1 1.462(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O1 1.217(3) . ?
C12 N1 1.400(4) . ?
C12 C15 1.485(4) . ?
C13 O2 1.211(4) . ?
C13 N1 1.400(4) . ?
C13 C14 1.477(4) . ?
C14 C15 1.384(4) . ?
C14 C19 1.384(4) . ?
C15 C16 1.383(4) . ?
C16 C17 1.393(4) . ?
C16 H16 0.9500 . ?
C17 O3 1.378(4) . ?
C17 C18 1.389(4) . ?
C18 C19 1.385(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C25 1.387(5) . ?
C20 C21 1.394(5) . ?
C20 O3 1.394(4) . ?
C21 C22 1.392(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.399(5) . ?
C23 C26 1.483(4) . ?
C24 C25 1.377(4) . ?
C24 C27 1.489(4) . ?
C25 H25 0.9500 . ?
C26 O5 1.211(4) . ?
C26 N2 1.411(4) . ?
C27 O4 1.213(4) . ?
C27 N2 1.398(4) . ?
C28 N2 1.456(4) . ?
C28 C29 1.528(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C37 1.533(5) . ?
C29 C30 1.538(4) . ?
C29 C34 1.546(4) . ?
C30 C31 1.529(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C38 1.525(4) . ?
C31 C32 1.526(4) . ?
C31 H31 1.0000 . ?
C32 C33 1.543(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C39 1.529(4) . ?
C33 C35 1.541(4) . ?
C33 C34 1.541(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.524(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.533(4) . ?
C36 C38 1.536(4) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 N3 1.466(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 O6 1.213(4) . ?
C40 N3 1.404(4) . ?
C40 C43 1.489(4) . ?
C41 O7 1.205(3) . ?
C41 N3 1.401(4) . ?
C41 C42 1.500(4) . ?
C42 C47 1.377(4) . ?
C42 C43 1.385(4) . ?
C43 C44 1.382(4) . ?
C44 C45 1.393(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.390(4) . ?
C45 H45 0.9500 . ?
C46 O8 1.387(3) . ?
C46 C47 1.390(4) . ?
C47 H47 0.9500 . ?
C48 O8 1.381(3) . ?
C48 C49 1.393(4) . ?
C48 C53 1.399(4) . ?
C49 C50 1.383(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.386(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.381(4) . ?
C51 C54 1.476(4) . ?
C52 C53 1.373(4) . ?
C52 C55 1.496(4) . ?
C53 H53 0.9500 . ?
C54 O9 1.210(3) . ?
C54 N4 1.404(3) . ?
C55 O10 1.213(3) . ?
C55 N4 1.389(3) . ?
C56 N4 1.472(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 Cl3 1.755(4) . ?
C57 Cl1 1.756(4) . ?
C57 Cl2 1.768(4) . ?
C57 H57 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
Cl5 C58 Cl4 129.9(13) . . ?
Cl5 C58 Cl6 124.9(10) . . ?
Cl4 C58 Cl6 95.8(7) . . ?
Cl5 C58 H58 100.0 . . ?
Cl4 C58 H58 100.0 . . ?
Cl6 C58 H58 100.0 . . ?
C56 C1 C8 111.1(2) . . ?
C56 C1 C2 111.4(2) . . ?
C8 C1 C2 110.0(2) . . ?
C56 C1 C9 106.4(2) . . ?
C8 C1 C9 109.3(2) . . ?
C2 C1 C9 108.5(2) . . ?
C3 C2 C1 109.5(2) . . ?
C3 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C3 C2 H2AB 109.8 . . ?
C1 C2 H2AB 109.8 . . ?
H2A C2 H2AB 108.2 . . ?
C2 C3 C4 110.1(3) . . ?
C2 C3 C10 109.2(2) . . ?
C4 C3 C10 109.3(3) . . ?
C2 C3 H3 109.4 . . ?
C4 C3 H3 109.4 . . ?
C10 C3 H3 109.4 . . ?
C3 C4 C5 108.6(2) . . ?
C3 C4 H4A 110.0 . . ?
C5 C4 H4A 110.0 . . ?
C3 C4 H4AB 110.0 . . ?
C5 C4 H4AB 110.0 . . ?
H4A C4 H4AB 108.3 . . ?
C6 C5 C4 110.2(3) . . ?
C6 C5 C9 109.1(2) . . ?
C4 C5 C9 109.6(3) . . ?
C6 C5 H5 109.3 . . ?
C4 C5 H5 109.3 . . ?
C9 C5 H5 109.3 . . ?
C5 C6 C7 110.4(2) . . ?
C5 C6 H6A 109.6 . . ?
C7 C6 H6A 109.6 . . ?
C5 C6 H6AB 109.6 . . ?
C7 C6 H6AB 109.6 . . ?
H6A C6 H6AB 108.1 . . ?
C6 C7 C8 109.4(2) . . ?
C6 C7 C10 108.0(2) . . ?
C8 C7 C10 108.0(2) . . ?
C6 C7 C11 112.0(2) . . ?
C8 C7 C11 111.4(2) . . ?
C10 C7 C11 107.9(2) . . ?
C1 C8 C7 110.4(2) . . ?
C1 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
C1 C8 H8AB 109.6 . . ?
C7 C8 H8AB 109.6 . . ?
H8A C8 H8AB 108.1 . . ?
C5 C9 C1 109.7(2) . . ?
C5 C9 H9A 109.7 . . ?
C1 C9 H9A 109.7 . . ?
C5 C9 H9AB 109.7 . . ?
C1 C9 H9AB 109.7 . . ?
H9A C9 H9AB 108.2 . . ?
C3 C10 C7 111.1(2) . . ?
C3 C10 H10A 109.4 . . ?
C7 C10 H10A 109.4 . . ?
C3 C10 H10B 109.4 . . ?
C7 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N1 C11 C7 116.3(2) . . ?
N1 C11 H11A 108.2 . . ?
C7 C11 H11A 108.2 . . ?
N1 C11 H11B 108.2 . . ?
C7 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
O1 C12 N1 124.9(3) . . ?
O1 C12 C15 129.1(3) . . ?
N1 C12 C15 106.0(2) . . ?
O2 C13 N1 125.3(3) . . ?
O2 C13 C14 128.6(3) . . ?
N1 C13 C14 106.1(2) . . ?
C15 C14 C19 121.1(3) . . ?
C15 C14 C13 108.4(3) . . ?
C19 C14 C13 130.5(3) . . ?
C16 C15 C14 122.2(3) . . ?
C16 C15 C12 129.7(2) . . ?
C14 C15 C12 108.0(3) . . ?
C15 C16 C17 116.1(3) . . ?
C15 C16 H16 122.0 . . ?
C17 C16 H16 122.0 . . ?
O3 C17 C18 115.5(3) . . ?
O3 C17 C16 121.9(3) . . ?
C18 C17 C16 122.5(3) . . ?
C19 C18 C17 120.3(3) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C14 C19 C18 117.9(3) . . ?
C14 C19 H19 121.0 . . ?
C18 C19 H19 121.0 . . ?
C25 C20 C21 122.9(3) . . ?
C25 C20 O3 115.7(3) . . ?
C21 C20 O3 121.2(3) . . ?
C22 C21 C20 120.2(3) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C21 117.5(3) . . ?
C23 C22 H22 121.3 . . ?
C21 C22 H22 121.3 . . ?
C22 C23 C24 121.1(3) . . ?
C22 C23 C26 130.7(3) . . ?
C24 C23 C26 108.2(3) . . ?
C25 C24 C23 122.2(3) . . ?
C25 C24 C27 129.9(3) . . ?
C23 C24 C27 108.0(3) . . ?
C24 C25 C20 116.1(3) . . ?
C24 C25 H25 121.9 . . ?
C20 C25 H25 121.9 . . ?
O5 C26 N2 124.6(3) . . ?
O5 C26 C23 129.4(3) . . ?
N2 C26 C23 106.0(3) . . ?
O4 C27 N2 125.6(3) . . ?
O4 C27 C24 128.2(3) . . ?
N2 C27 C24 106.2(3) . . ?
N2 C28 C29 115.9(2) . . ?
N2 C28 H28A 108.3 . . ?
C29 C28 H28A 108.3 . . ?
N2 C28 H28B 108.3 . . ?
C29 C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
C28 C29 C37 112.2(3) . . ?
C28 C29 C30 106.5(2) . . ?
C37 C29 C30 108.7(2) . . ?
C28 C29 C34 111.7(2) . . ?
C37 C29 C34 109.3(2) . . ?
C30 C29 C34 108.3(2) . . ?
C31 C30 C29 110.6(2) . . ?
C31 C30 H30A 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C38 C31 C32 110.2(2) . . ?
C38 C31 C30 109.6(3) . . ?
C32 C31 C30 108.7(2) . . ?
C38 C31 H31 109.4 . . ?
C32 C31 H31 109.4 . . ?
C30 C31 H31 109.4 . . ?
C31 C32 C33 110.5(2) . . ?
C31 C32 H32A 109.6 . . ?
C33 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
C33 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
C39 C33 C35 112.4(2) . . ?
C39 C33 C34 112.8(2) . . ?
C35 C33 C34 109.2(2) . . ?
C39 C33 C32 105.6(2) . . ?
C35 C33 C32 108.1(2) . . ?
C34 C33 C32 108.6(2) . . ?
C33 C34 C29 110.3(2) . . ?
C33 C34 H34A 109.6 . . ?
C29 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
C29 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C36 C35 C33 110.6(2) . . ?
C36 C35 H35A 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 108.1 . . ?
C35 C36 C37 109.6(2) . . ?
C35 C36 C38 109.4(3) . . ?
C37 C36 C38 109.5(2) . . ?
C35 C36 H36 109.4 . . ?
C37 C36 H36 109.4 . . ?
C38 C36 H36 109.4 . . ?
C36 C37 C29 110.2(3) . . ?
C36 C37 H37A 109.6 . . ?
C29 C37 H37A 109.6 . . ?
C36 C37 H37B 109.6 . . ?
C29 C37 H37B 109.6 . . ?
H37A C37 H37B 108.1 . . ?
C31 C38 C36 109.1(2) . . ?
C31 C38 H38A 109.9 . . ?
C36 C38 H38A 109.9 . . ?
C31 C38 H38B 109.9 . . ?
C36 C38 H38B 109.9 . . ?
H38A C38 H38B 108.3 . . ?
N3 C39 C33 117.1(2) . . ?
N3 C39 H39A 108.0 . . ?
C33 C39 H39A 108.0 . . ?
N3 C39 H39B 108.0 . . ?
C33 C39 H39B 108.0 . . ?
H39A C39 H39B 107.3 . . ?
O6 C40 N3 125.2(3) . . ?
O6 C40 C43 128.0(3) . . ?
N3 C40 C43 106.7(2) . . ?
O7 C41 N3 126.0(2) . . ?
O7 C41 C42 128.1(3) . . ?
N3 C41 C42 105.9(2) . . ?
C47 C42 C43 122.5(3) . . ?
C47 C42 C41 129.1(3) . . ?
C43 C42 C41 108.3(2) . . ?
C44 C43 C42 121.0(3) . . ?
C44 C43 C40 131.2(3) . . ?
C42 C43 C40 107.8(2) . . ?
C43 C44 C45 117.7(3) . . ?
C43 C44 H44 121.1 . . ?
C45 C44 H44 121.1 . . ?
C46 C45 C44 120.3(3) . . ?
C46 C45 H45 119.9 . . ?
C44 C45 H45 119.9 . . ?
O8 C46 C47 116.1(3) . . ?
O8 C46 C45 121.4(3) . . ?
C47 C46 C45 122.3(3) . . ?
C42 C47 C46 116.2(3) . . ?
C42 C47 H47 121.9 . . ?
C46 C47 H47 121.9 . . ?
O8 C48 C49 115.0(2) . . ?
O8 C48 C53 123.3(2) . . ?
C49 C48 C53 121.6(2) . . ?
C50 C49 C48 120.9(3) . . ?
C50 C49 H49 119.6 . . ?
C48 C49 H49 119.6 . . ?
C49 C50 C51 117.7(3) . . ?
C49 C50 H50 121.2 . . ?
C51 C50 H50 121.2 . . ?
C52 C51 C50 120.8(2) . . ?
C52 C51 C54 108.8(2) . . ?
C50 C51 C54 130.3(2) . . ?
C53 C52 C51 122.9(2) . . ?
C53 C52 C55 129.3(2) . . ?
C51 C52 C55 107.6(2) . . ?
C52 C53 C48 116.1(2) . . ?
C52 C53 H53 121.9 . . ?
C48 C53 H53 121.9 . . ?
O9 C54 N4 124.9(2) . . ?
O9 C54 C51 129.2(3) . . ?
N4 C54 C51 105.9(2) . . ?
O10 C55 N4 126.0(2) . . ?
O10 C55 C52 127.9(2) . . ?
N4 C55 C52 106.1(2) . . ?
N4 C56 C1 115.8(2) . . ?
N4 C56 H56A 108.3 . . ?
C1 C56 H56A 108.3 . . ?
N4 C56 H56B 108.3 . . ?
C1 C56 H56B 108.3 . . ?
H56A C56 H56B 107.4 . . ?
Cl3 C57 Cl1 110.8(2) . . ?
Cl3 C57 Cl2 111.11(19) . . ?
Cl1 C57 Cl2 109.6(2) . . ?
Cl3 C57 H57 108.4 . . ?
Cl1 C57 H57 108.4 . . ?
Cl2 C57 H57 108.4 . . ?
C12 N1 C13 111.3(2) . . ?
C12 N1 C11 123.0(2) . . ?
C13 N1 C11 125.3(2) . . ?
C27 N2 C26 111.5(3) . . ?
C27 N2 C28 123.4(3) . . ?
C26 N2 C28 123.3(3) . . ?
C41 N3 C40 110.9(2) . . ?
C41 N3 C39 123.6(2) . . ?
C40 N3 C39 122.3(2) . . ?
C55 N4 C54 111.6(2) . . ?
C55 N4 C56 124.0(2) . . ?
C54 N4 C56 122.9(2) . . ?
C17 O3 C20 119.1(2) . . ?
C48 O8 C46 120.1(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
C56 C1 C2 C3 -177.0(2) . . . . ?
C8 C1 C2 C3 59.4(3) . . . . ?
C9 C1 C2 C3 -60.1(3) . . . . ?
C1 C2 C3 C4 61.1(3) . . . . ?
C1 C2 C3 C10 -58.9(3) . . . . ?
C2 C3 C4 C5 -60.3(3) . . . . ?
C10 C3 C4 C5 59.7(3) . . . . ?
C3 C4 C5 C6 -60.1(3) . . . . ?
C3 C4 C5 C9 59.9(3) . . . . ?
C4 C5 C6 C7 60.4(3) . . . . ?
C9 C5 C6 C7 -59.9(3) . . . . ?
C5 C6 C7 C8 58.9(3) . . . . ?
C5 C6 C7 C10 -58.4(3) . . . . ?
C5 C6 C7 C11 -177.1(2) . . . . ?
C56 C1 C8 C7 176.2(2) . . . . ?
C2 C1 C8 C7 -60.0(3) . . . . ?
C9 C1 C8 C7 59.1(3) . . . . ?
C6 C7 C8 C1 -58.5(3) . . . . ?
C10 C7 C8 C1 58.9(3) . . . . ?
C11 C7 C8 C1 177.2(2) . . . . ?
C6 C5 C9 C1 60.1(3) . . . . ?
C4 C5 C9 C1 -60.6(3) . . . . ?
C56 C1 C9 C5 -179.9(2) . . . . ?
C8 C1 C9 C5 -59.8(3) . . . . ?
C2 C1 C9 C5 60.1(3) . . . . ?
C2 C3 C10 C7 60.0(3) . . . . ?
C4 C3 C10 C7 -60.5(3) . . . . ?
C6 C7 C10 C3 58.9(3) . . . . ?
C8 C7 C10 C3 -59.3(3) . . . . ?
C11 C7 C10 C3 -179.9(2) . . . . ?
C6 C7 C11 N1 -76.5(3) . . . . ?
C8 C7 C11 N1 46.3(3) . . . . ?
C10 C7 C11 N1 164.7(2) . . . . ?
O2 C13 C14 C15 176.0(3) . . . . ?
N1 C13 C14 C15 -3.4(3) . . . . ?
O2 C13 C14 C19 -3.8(6) . . . . ?
N1 C13 C14 C19 176.9(3) . . . . ?
C19 C14 C15 C16 0.1(5) . . . . ?
C13 C14 C15 C16 -179.7(3) . . . . ?
C19 C14 C15 C12 -178.8(3) . . . . ?
C13 C14 C15 C12 1.5(3) . . . . ?
O1 C12 C15 C16 3.3(6) . . . . ?
N1 C12 C15 C16 -177.8(3) . . . . ?
O1 C12 C15 C14 -178.0(3) . . . . ?
N1 C12 C15 C14 1.0(3) . . . . ?
C14 C15 C16 C17 -0.4(5) . . . . ?
C12 C15 C16 C17 178.2(3) . . . . ?
C15 C16 C17 O3 -175.6(3) . . . . ?
C15 C16 C17 C18 0.2(5) . . . . ?
O3 C17 C18 C19 176.4(3) . . . . ?
C16 C17 C18 C19 0.3(5) . . . . ?
C15 C14 C19 C18 0.4(5) . . . . ?
C13 C14 C19 C18 -179.8(3) . . . . ?
C17 C18 C19 C14 -0.6(5) . . . . ?
C25 C20 C21 C22 -0.6(5) . . . . ?
O3 C20 C21 C22 -175.7(3) . . . . ?
C20 C21 C22 C23 1.5(5) . . . . ?
C21 C22 C23 C24 -1.3(5) . . . . ?
C21 C22 C23 C26 178.5(3) . . . . ?
C22 C23 C24 C25 0.3(5) . . . . ?
C26 C23 C24 C25 -179.6(3) . . . . ?
C22 C23 C24 C27 -179.6(3) . . . . ?
C26 C23 C24 C27 0.5(3) . . . . ?
C23 C24 C25 C20 0.6(4) . . . . ?
C27 C24 C25 C20 -179.5(3) . . . . ?
C21 C20 C25 C24 -0.4(4) . . . . ?
O3 C20 C25 C24 174.9(3) . . . . ?
C22 C23 C26 O5 -4.4(6) . . . . ?
C24 C23 C26 O5 175.4(3) . . . . ?
C22 C23 C26 N2 177.5(3) . . . . ?
C24 C23 C26 N2 -2.7(3) . . . . ?
C25 C24 C27 O4 2.5(5) . . . . ?
C23 C24 C27 O4 -177.6(3) . . . . ?
C25 C24 C27 N2 -178.0(3) . . . . ?
C23 C24 C27 N2 1.9(3) . . . . ?
N2 C28 C29 C37 -58.5(4) . . . . ?
N2 C28 C29 C30 -177.3(3) . . . . ?
N2 C28 C29 C34 64.6(4) . . . . ?
C28 C29 C30 C31 179.7(3) . . . . ?
C37 C29 C30 C31 58.6(3) . . . . ?
C34 C29 C30 C31 -60.0(3) . . . . ?
C29 C30 C31 C38 -59.9(3) . . . . ?
C29 C30 C31 C32 60.6(3) . . . . ?
C38 C31 C32 C33 59.8(3) . . . . ?
C30 C31 C32 C33 -60.3(3) . . . . ?
C31 C32 C33 C39 -178.9(2) . . . . ?
C31 C32 C33 C35 -58.4(3) . . . . ?
C31 C32 C33 C34 59.9(3) . . . . ?
C39 C33 C34 C29 -176.1(2) . . . . ?
C35 C33 C34 C29 58.2(3) . . . . ?
C32 C33 C34 C29 -59.4(3) . . . . ?
C28 C29 C34 C33 176.4(2) . . . . ?
C37 C29 C34 C33 -58.8(3) . . . . ?
C30 C29 C34 C33 59.4(3) . . . . ?
C39 C33 C35 C36 175.4(2) . . . . ?
C34 C33 C35 C36 -58.7(3) . . . . ?
C32 C33 C35 C36 59.2(3) . . . . ?
C33 C35 C36 C37 59.4(3) . . . . ?
C33 C35 C36 C38 -60.7(3) . . . . ?
C35 C36 C37 C29 -59.7(3) . . . . ?
C38 C36 C37 C29 60.3(3) . . . . ?
C28 C29 C37 C36 -176.3(2) . . . . ?
C30 C29 C37 C36 -58.8(3) . . . . ?
C34 C29 C37 C36 59.3(3) . . . . ?
C32 C31 C38 C36 -59.7(3) . . . . ?
C30 C31 C38 C36 60.0(3) . . . . ?
C35 C36 C38 C31 59.9(3) . . . . ?
C37 C36 C38 C31 -60.3(3) . . . . ?
C35 C33 C39 N3 58.1(3) . . . . ?
C34 C33 C39 N3 -65.9(3) . . . . ?
C32 C33 C39 N3 175.7(2) . . . . ?
O7 C41 C42 C47 2.6(5) . . . . ?
N3 C41 C42 C47 179.8(3) . . . . ?
O7 C41 C42 C43 -172.9(3) . . . . ?
N3 C41 C42 C43 4.3(3) . . . . ?
C47 C42 C43 C44 0.1(5) . . . . ?
C41 C42 C43 C44 175.9(3) . . . . ?
C47 C42 C43 C40 -176.7(3) . . . . ?
C41 C42 C43 C40 -0.8(3) . . . . ?
O6 C40 C43 C44 -2.1(6) . . . . ?
N3 C40 C43 C44 -179.3(3) . . . . ?
O6 C40 C43 C42 174.2(3) . . . . ?
N3 C40 C43 C42 -2.9(3) . . . . ?
C42 C43 C44 C45 -0.2(5) . . . . ?
C40 C43 C44 C45 175.7(3) . . . . ?
C43 C44 C45 C46 0.3(4) . . . . ?
C44 C45 C46 O8 -175.4(3) . . . . ?
C44 C45 C46 C47 -0.3(5) . . . . ?
C43 C42 C47 C46 -0.1(4) . . . . ?
C41 C42 C47 C46 -175.0(3) . . . . ?
O8 C46 C47 C42 175.5(3) . . . . ?
C45 C46 C47 C42 0.2(4) . . . . ?
O8 C48 C49 C50 177.6(3) . . . . ?
C53 C48 C49 C50 0.1(5) . . . . ?
C48 C49 C50 C51 1.0(4) . . . . ?
C49 C50 C51 C52 -1.1(4) . . . . ?
C49 C50 C51 C54 175.2(3) . . . . ?
C50 C51 C52 C53 0.1(4) . . . . ?
C54 C51 C52 C53 -176.9(3) . . . . ?
C50 C51 C52 C55 176.6(2) . . . . ?
C54 C51 C52 C55 -0.5(3) . . . . ?
C51 C52 C53 C48 0.9(4) . . . . ?
C55 C52 C53 C48 -174.7(3) . . . . ?
O8 C48 C53 C52 -178.4(3) . . . . ?
C49 C48 C53 C52 -1.0(4) . . . . ?
C52 C51 C54 O9 176.7(3) . . . . ?
C50 C51 C54 O9 0.0(5) . . . . ?
C52 C51 C54 N4 0.3(3) . . . . ?
C50 C51 C54 N4 -176.4(3) . . . . ?
C53 C52 C55 O10 -0.3(5) . . . . ?
C51 C52 C55 O10 -176.5(3) . . . . ?
C53 C52 C55 N4 176.6(3) . . . . ?
C51 C52 C55 N4 0.5(3) . . . . ?
C8 C1 C56 N4 64.5(3) . . . . ?
C2 C1 C56 N4 -58.5(3) . . . . ?
C9 C1 C56 N4 -176.6(2) . . . . ?
O1 C12 N1 C13 175.8(3) . . . . ?
C15 C12 N1 C13 -3.2(3) . . . . ?
O1 C12 N1 C11 3.0(5) . . . . ?
C15 C12 N1 C11 -176.0(3) . . . . ?
O2 C13 N1 C12 -175.3(3) . . . . ?
C14 C13 N1 C12 4.1(3) . . . . ?
O2 C13 N1 C11 -2.7(5) . . . . ?
C14 C13 N1 C11 176.6(3) . . . . ?
C7 C11 N1 C12 -105.6(3) . . . . ?
C7 C11 N1 C13 82.7(4) . . . . ?
O4 C27 N2 C26 175.7(3) . . . . ?
C24 C27 N2 C26 -3.7(3) . . . . ?
O4 C27 N2 C28 10.5(5) . . . . ?
C24 C27 N2 C28 -169.0(2) . . . . ?
O5 C26 N2 C27 -174.2(3) . . . . ?
C23 C26 N2 C27 4.1(3) . . . . ?
O5 C26 N2 C28 -8.9(5) . . . . ?
C23 C26 N2 C28 169.3(3) . . . . ?
C29 C28 N2 C27 -100.5(4) . . . . ?
C29 C28 N2 C26 96.0(4) . . . . ?
O7 C41 N3 C40 171.0(3) . . . . ?
C42 C41 N3 C40 -6.3(3) . . . . ?
O7 C41 N3 C39 10.8(5) . . . . ?
C42 C41 N3 C39 -166.5(2) . . . . ?
O6 C40 N3 C41 -171.4(3) . . . . ?
C43 C40 N3 C41 5.8(3) . . . . ?
O6 C40 N3 C39 -10.9(5) . . . . ?
C43 C40 N3 C39 166.4(2) . . . . ?
C33 C39 N3 C41 -89.5(3) . . . . ?
C33 C39 N3 C40 112.5(3) . . . . ?
O10 C55 N4 C54 176.7(3) . . . . ?
C52 C55 N4 C54 -0.3(3) . . . . ?
O10 C55 N4 C56 10.3(4) . . . . ?
C52 C55 N4 C56 -166.7(2) . . . . ?
O9 C54 N4 C55 -176.6(3) . . . . ?
C51 C54 N4 C55 0.0(3) . . . . ?
O9 C54 N4 C56 -10.0(4) . . . . ?
C51 C54 N4 C56 166.6(2) . . . . ?
C1 C56 N4 C55 -93.9(3) . . . . ?
C1 C56 N4 C54 101.2(3) . . . . ?
C18 C17 O3 C20 145.6(3) . . . . ?
C16 C17 O3 C20 -38.3(5) . . . . ?
C25 C20 O3 C17 137.7(3) . . . . ?
C21 C20 O3 C17 -46.8(4) . . . . ?
C49 C48 O8 C46 161.2(3) . . . . ?
C53 C48 O8 C46 -21.2(4) . . . . ?
C47 C46 O8 C48 137.3(3) . . . . ?
C45 C46 O8 C48 -47.4(4) . . . . ?

_refine_diff_density_max         0.861
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.072



####################################################################### 
# 
# 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_1a_without_SQUEEZE
_database_code_depnum_ccdc_archive 'CCDC 2133052'
loop_
_audit_author_name
_audit_author_address
'Tadashi Hyodo'
;Tokushima Bunri University
Japan
;
_audit_update_record             
;
2022-01-11 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT057_data1_p21c_a        
;
PROBLEM: Correction for Absorption Required RT(exp) 
... 1.40
RESPONSE: This refinement is the model structure of overlapped 
and violently disordered solvent molecules across the unit cells.
The overlapped and violently disordered solvent molecules were 
isotropically refined with DFIX, DANG, EADP, EQIV, FLAT, SADI, 
SAME and PART and the structure was converged.
After checking the solvent volume and electron counts by 
PLATON/SQUEEZE, PLATON/SQUEEZEd data was refined to give the 
final structure.
;
_vrf_PLAT075_data1_p21c_a        
;
PROBLEM: Occupancy      1.050 Greater Than 1.0 for 
... C52, H52A, H52B, H52C, C53, H53A, H53B, C54, H54A and H54B
RESPONSE: This refinement is the model structure of overlapped 
and violently disordered solvent molecules across the unit cells.
The overlapped and violently disordered solvent molecules were 
isotropically refined with DFIX, DANG, EADP, EQIV, FLAT, SADI, 
SAME and PART and the structure was converged.
After checking the solvent volume and electron counts by 
PLATON/SQUEEZE, PLATON/SQUEEZEd data was refined to give the 
final structure.
;
_vrf_PLAT097_data1_p21c_a        
;
PROBLEM: Large Reported Max.(Positive) Residual Density 11.40 eA-3 
RESPONSE: This refinement is the model structure of overlapped 
and violently disordered solvent molecules across the unit cells.
The overlapped and violently disordered solvent molecules were 
isotropically refined with DFIX, DANG, EADP, EQIV, FLAT, SADI, 
SAME and PART and the structure was converged.
After checking the solvent volume and electron counts by 
PLATON/SQUEEZE, PLATON/SQUEEZEd data was refined to give the 
final structure.
;
_vrf_PLAT084_data1_p21c_a        
;
PROBLEM: High wR2 Value (i.e. > 0.25) .. 0.41
RESPONSE: This refinement is the model structure of overlapped 
and violently disordered solvent molecules across the unit cells.
The overlapped and violently disordered solvent molecules were 
isotropically refined with DFIX, DANG, EADP, EQIV, FLAT, SADI, 
SAME and PART and the structure was converged.
After checking the solvent volume and electron counts by 
PLATON/SQUEEZE, PLATON/SQUEEZEd data was refined to give the 
final structure.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C51 H56.67 I N4 O8.33'
_chemical_formula_weight         985.84

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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   18.087(3)
_cell_length_b                   16.027(3)
_cell_length_c                   16.477(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.124(4)
_cell_angle_gamma                90
_cell_volume                     4588.6(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9742
_cell_measurement_theta_min      3.61
_cell_measurement_theta_max      78.44

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             2041
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.975
_shelx_estimated_absorpt_T_min   0.381
_shelx_estimated_absorpt_T_max   0.586
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            67015
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.543
_diffrn_reflns_theta_max         80.219
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9739
_reflns_number_gt                9518
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (Hübschle et al., 2011)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9739
_refine_ls_number_parameters     564
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.1070
_refine_ls_wR_factor_ref         0.4062
_refine_ls_wR_factor_gt          0.4024
_refine_ls_goodness_of_fit_ref   2.153
_refine_ls_restrained_S_all      2.184
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8236(2) 0.6826(3) 0.2960(3) 0.0217(9) Uani 1 1 d . . . . .
C2 C 0.7752(3) 0.6030(3) 0.2696(3) 0.0201(9) Uani 1 1 d . . . . .
H2A H 0.799304 0.556264 0.306969 0.024 Uiso 1 1 calc R U . . .
H2B H 0.723026 0.611942 0.276254 0.024 Uiso 1 1 calc R U . . .
C3 C 0.7691(3) 0.5804(3) 0.1779(3) 0.0242(10) Uani 1 1 d . . . . .
C4 C 0.7335(3) 0.6536(3) 0.1203(3) 0.0232(9) Uani 1 1 d . . . . .
H4A H 0.730600 0.639462 0.061051 0.028 Uiso 1 1 calc R U . . .
H4B H 0.680538 0.663624 0.123993 0.028 Uiso 1 1 calc R U . . .
C5 C 0.7810(4) 0.7323(3) 0.1456(4) 0.0276(12) Uani 1 1 d . . . . .
H5 H 0.756256 0.779157 0.107645 0.033 Uiso 1 1 calc R U . . .
C6 C 0.7853(3) 0.7548(4) 0.2374(4) 0.0233(10) Uani 1 1 d . . . . .
H6A H 0.732797 0.764668 0.242832 0.028 Uiso 1 1 calc R U . . .
H6B H 0.815568 0.806588 0.253895 0.028 Uiso 1 1 calc R U . . .
C7 C 0.9048(3) 0.6666(4) 0.2863(4) 0.0289(11) Uani 1 1 d . . . . .
H7A H 0.936912 0.717106 0.303405 0.035 Uiso 1 1 calc R U . . .
H7B H 0.929345 0.620141 0.323707 0.035 Uiso 1 1 calc R U . . .
C8 C 0.8507(3) 0.5646(4) 0.1694(4) 0.0314(11) Uani 1 1 d . . . . .
H8A H 0.847783 0.548901 0.110487 0.038 Uiso 1 1 calc R U . . .
H8B H 0.875088 0.518099 0.206860 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8621(4) 0.7177(5) 0.1370(4) 0.0390(14) Uani 1 1 d . . . . .
H9A H 0.893482 0.768723 0.153518 0.047 Uiso 1 1 calc R U . . .
H9B H 0.859352 0.704739 0.077456 0.047 Uiso 1 1 calc R U . . .
C10 C 0.8997(3) 0.6447(4) 0.1940(4) 0.0333(12) Uani 1 1 d . . . . .
H10 H 0.952537 0.634779 0.188105 0.040 Uiso 1 1 calc R U . . .
C11 C 0.8309(3) 0.7041(3) 0.3889(3) 0.0249(10) Uani 1 1 d . . . . .
H11A H 0.864465 0.662047 0.425294 0.030 Uiso 1 1 calc R U . . .
H11B H 0.856650 0.758976 0.401827 0.030 Uiso 1 1 calc R U . . .
C12 C 0.7231(3) 0.4998(3) 0.1524(4) 0.0278(10) Uani 1 1 d . . . . .
H12A H 0.716992 0.489247 0.091740 0.033 Uiso 1 1 calc R U . . .
H12B H 0.752873 0.452873 0.184674 0.033 Uiso 1 1 calc R U . . .
C13 C 0.7109(3) 0.7779(3) 0.4022(3) 0.0208(10) Uani 1 1 d . . . . .
C14 C 0.6400(3) 0.7506(4) 0.4254(3) 0.0186(9) Uani 1 1 d . . . . .
C15 C 0.5755(3) 0.7979(3) 0.4251(3) 0.0187(9) Uani 1 1 d . . . . .
H15 H 0.570836 0.855373 0.410592 0.022 Uiso 1 1 calc R U . . .
C16 C 0.5179(3) 0.7526(4) 0.4482(3) 0.0190(9) Uani 1 1 d . . . . .
C17 C 0.4404(3) 0.7805(4) 0.4531(4) 0.0207(10) Uani 1 1 d . . . . .
C18 C 0.4547(3) 0.6414(3) 0.4917(3) 0.0198(9) Uani 1 1 d . . . . .
C19 C 0.5266(3) 0.6685(3) 0.4698(3) 0.0181(9) Uani 1 1 d . . . . .
C20 C 0.5928(3) 0.6214(3) 0.4717(3) 0.0208(9) Uani 1 1 d . . . . .
H20 H 0.598563 0.564159 0.487279 0.025 Uiso 1 1 calc R U . . .
C21 C 0.6486(3) 0.6672(3) 0.4484(3) 0.0181(9) Uani 1 1 d . . . . .
C22 C 0.7255(3) 0.6392(3) 0.4416(3) 0.0217(9) Uani 1 1 d . . . . .
C23 C 0.2631(3) 0.6917(3) 0.4130(3) 0.0243(10) Uani 1 1 d . . . . .
C24 C 0.2772(3) 0.6096(3) 0.3706(3) 0.0251(10) Uani 1 1 d . . . . .
H24A H 0.283542 0.563119 0.411475 0.030 Uiso 1 1 calc R U . . .
H24B H 0.325101 0.614342 0.352990 0.030 Uiso 1 1 calc R U . . .
C25 C 0.2086(3) 0.5909(3) 0.2924(3) 0.0270(10) Uani 1 1 d . . . . .
C26 C 0.1996(3) 0.6654(4) 0.2311(4) 0.0293(11) Uani 1 1 d . . . . .
H26A H 0.156630 0.654267 0.180036 0.035 Uiso 1 1 calc R U . . .
H26B H 0.247224 0.671897 0.213319 0.035 Uiso 1 1 calc R U . . .
C27 C 0.1834(4) 0.7473(4) 0.2732(4) 0.0319(12) Uani 1 1 d . . . . .
H27 H 0.176719 0.794591 0.232265 0.038 Uiso 1 1 calc R U . . .
C28 C 0.2523(3) 0.7639(3) 0.3498(4) 0.0262(12) Uani 1 1 d . . . . .
H28A H 0.243867 0.816435 0.377590 0.031 Uiso 1 1 calc R U . . .
H28B H 0.299378 0.770508 0.330940 0.031 Uiso 1 1 calc R U . . .
C29 C 0.1897(3) 0.6814(4) 0.4424(4) 0.0329(11) Uani 1 1 d . . . . .
H29A H 0.180283 0.732899 0.471071 0.039 Uiso 1 1 calc R U . . .
H29B H 0.196479 0.634625 0.483064 0.039 Uiso 1 1 calc R U . . .
C30 C 0.1350(3) 0.5831(4) 0.3216(4) 0.0335(12) Uani 1 1 d . . . . .
H30A H 0.090510 0.571655 0.272193 0.040 Uiso 1 1 calc R U . . .
H30B H 0.140417 0.535752 0.361370 0.040 Uiso 1 1 calc R U . . .
C31 C 0.1104(4) 0.7366(4) 0.3021(6) 0.0413(17) Uani 1 1 d . . . . .
H31A H 0.065907 0.725549 0.252576 0.050 Uiso 1 1 calc R U . . .
H31B H 0.099924 0.788682 0.329365 0.050 Uiso 1 1 calc R U . . .
C32 C 0.1204(3) 0.6637(4) 0.3651(5) 0.0374(13) Uani 1 1 d . . . . .
H32 H 0.072670 0.657362 0.383944 0.045 Uiso 1 1 calc R U . . .
C33 C 0.3294(3) 0.7094(3) 0.4919(3) 0.0244(10) Uani 1 1 d . . . . .
H33A H 0.320239 0.764080 0.515378 0.029 Uiso 1 1 calc R U . . .
H33B H 0.329132 0.666367 0.534909 0.029 Uiso 1 1 calc R U . . .
C34 C 0.2197(3) 0.5083(4) 0.2496(4) 0.0291(11) Uani 1 1 d . . . . .
H34A H 0.216044 0.461404 0.287398 0.035 Uiso 1 1 calc R U . . .
H34B H 0.177711 0.501954 0.196737 0.035 Uiso 1 1 calc R U . . .
C35 C 0.3082(3) 0.5298(3) 0.1548(3) 0.0268(10) Uani 1 1 d . . . . .
C36 C 0.3924(3) 0.5133(3) 0.1663(3) 0.0232(9) Uani 1 1 d . . . . .
C37 C 0.4379(3) 0.5340(3) 0.1134(3) 0.0218(9) Uani 1 1 d . . . . .
H37 H 0.417837 0.560530 0.060278 0.026 Uiso 1 1 calc R U . . .
C38 C 0.5145(3) 0.5128(3) 0.1448(3) 0.0227(9) Uani 1 1 d . . . . .
C39 C 0.5803(3) 0.5277(3) 0.1073(3) 0.0229(9) Uani 1 1 d . . . . .
C40 C 0.6288(3) 0.4616(3) 0.2364(3) 0.0264(10) Uani 1 1 d . . . . .
C41 C 0.5447(3) 0.4743(3) 0.2237(3) 0.0233(10) Uani 1 1 d . . . . .
C42 C 0.4999(3) 0.4534(3) 0.2758(3) 0.0265(10) Uani 1 1 d . . . . .
H42 H 0.520200 0.426745 0.328770 0.032 Uiso 1 1 calc R U . . .
C43 C 0.4225(3) 0.4743(3) 0.2449(3) 0.0254(10) Uani 1 1 d . . . . .
C44 C 0.3581(3) 0.4643(3) 0.2836(3) 0.0255(10) Uani 1 1 d . . . . .
N1 N 0.7578(2) 0.7072(3) 0.4103(3) 0.0222(8) Uani 1 1 d . . . . .
N2 N 0.4058(2) 0.7106(3) 0.4770(3) 0.0226(8) Uani 1 1 d . . . . .
N3 N 0.2941(3) 0.5037(3) 0.2299(3) 0.0256(9) Uani 1 1 d . . . . .
N4 N 0.6464(2) 0.5011(3) 0.1669(3) 0.0239(9) Uani 1 1 d . . . . .
O1 O 0.7267(2) 0.8470(2) 0.3824(3) 0.0272(8) Uani 1 1 d . . . . .
O2 O 0.4123(2) 0.8497(2) 0.4408(3) 0.0263(8) Uani 1 1 d . . . . .
O3 O 0.4400(2) 0.5748(2) 0.5172(2) 0.0264(8) Uani 1 1 d . . . . .
O4 O 0.7567(2) 0.5718(2) 0.4603(3) 0.0277(8) Uani 1 1 d . . . . .
O5 O 0.2622(2) 0.5604(3) 0.0962(3) 0.0345(9) Uani 1 1 d . . . . .
O6 O 0.5778(2) 0.5592(2) 0.0403(2) 0.0254(7) Uani 1 1 d . . . . .
O7 O 0.6742(2) 0.4253(3) 0.2920(3) 0.0345(9) Uani 1 1 d . . . . .
O8 O 0.3575(3) 0.4276(3) 0.3481(3) 0.0324(9) Uani 1 1 d . . . . .
C45 C 0.4314(4) 0.7291(3) 0.2237(5) 0.0322(13) Uani 1 1 d . . . . .
H45A H 0.423638 0.781074 0.251601 0.048 Uiso 1 1 calc R U . . .
H45B H 0.431693 0.681903 0.261537 0.048 Uiso 1 1 calc R U . . .
H45C H 0.389565 0.722007 0.171637 0.048 Uiso 1 1 calc R U . . .
I1 I 0.53967(2) 0.73443(2) 0.19346(2) 0.0330(3) Uani 1 1 d . . . . .
C46 C 1.0247(8) 0.8075(8) 0.5111(9) 0.053(2) Uiso 0.62(2) 1 d D . P A 1
H46A H 0.994689 0.757960 0.487409 0.080 Uiso 0.62(2) 1 calc R U P A 1
H46B H 1.027445 0.812386 0.571132 0.080 Uiso 0.62(2) 1 calc R U P A 1
H46C H 1.076860 0.802371 0.504817 0.080 Uiso 0.62(2) 1 calc R U P A 1
C47 C 0.9860(8) 0.8853(7) 0.4641(8) 0.053(2) Uiso 0.62(2) 1 d D . P A 1
H47A H 0.999152 0.892850 0.410068 0.064 Uiso 0.62(2) 1 calc R U P A 1
H47B H 0.929350 0.882550 0.452626 0.064 Uiso 0.62(2) 1 calc R U P A 1
C48 C 1.0197(8) 0.9544(8) 0.5258(9) 0.053(2) Uiso 0.62(2) 1 d D . P A 1
H48A H 1.076491 0.955071 0.538925 0.064 Uiso 0.62(2) 1 calc R U P A 1
H48B H 1.005067 0.947265 0.579003 0.064 Uiso 0.62(2) 1 calc R U P A 1
C49 C 1.0263(10) 0.8659(12) 0.4392(10) 0.041(3) Uiso 0.330(16) 1 d D . P B 2
C50 C 1.0144(14) 0.7681(11) 0.4563(16) 0.041(3) Uiso 0.330(16) 1 d D . P B 2
H50A H 1.036005 0.756017 0.516588 0.062 Uiso 0.330(16) 1 calc R U P B 2
H50B H 1.040722 0.734149 0.423391 0.062 Uiso 0.330(16) 1 calc R U P B 2
H50C H 0.959357 0.754893 0.439380 0.062 Uiso 0.330(16) 1 calc R U P B 2
C51 C 1.0917(11) 0.9146(14) 0.4853(13) 0.041(3) Uiso 0.330(16) 1 d D . P B 2
H51A H 1.139085 0.883037 0.489920 0.062 Uiso 0.330(16) 1 calc R U P B 2
H51B H 1.087011 0.926669 0.541990 0.062 Uiso 0.330(16) 1 calc R U P B 2
H51C H 1.093327 0.967058 0.455342 0.062 Uiso 0.330(16) 1 calc R U P B 2
O9 O 0.9834(8) 0.9135(9) 0.3894(9) 0.041(3) Uiso 0.330(16) 1 d D . P B 2
C52 C 1.0603(5) 0.6376(6) 0.6291(6) 0.0614(16) Uiso 1.05(2) 1 d D . P C 3
H52A H 1.110486 0.614331 0.629166 0.092 Uiso 1.05(2) 1 calc R U P C 3
H52B H 1.064574 0.665507 0.683075 0.092 Uiso 1.05(2) 1 calc R U P C 3
H52C H 1.043886 0.677927 0.582900 0.092 Uiso 1.05(2) 1 calc R U P C 3
C53 C 1.0028(5) 0.5692(5) 0.6171(6) 0.0614(16) Uiso 1.05(2) 1 d D . P C 3
H53A H 0.949313 0.590092 0.603876 0.074 Uiso 1.05(2) 1 calc R U P C 3
H53B H 1.013247 0.530542 0.665839 0.074 Uiso 1.05(2) 1 calc R U P C 3
C54 C 1.0229(5) 0.5286(6) 0.5358(5) 0.0614(16) Uiso 1.05(2) 1 d D . P C 3
H54A H 1.036906 0.577150 0.505939 0.074 Uiso 1.05(2) 1 calc R U P C 3
H54B H 1.071647 0.498118 0.560087 0.074 Uiso 1.05(2) 1 calc R U P C 3


_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 C11 1.538(7) . ?
C1 C2 1.540(6) . ?
C1 C7 1.541(6) . ?
C1 C6 1.543(7) . ?
C2 C3 1.529(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C12 1.530(7) . ?
C3 C4 1.534(7) . ?
C3 C8 1.542(7) . ?
C4 C5 1.517(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C9 1.530(8) . ?
C5 C6 1.536(9) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C10 1.540(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C10 1.548(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.535(11) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10 1.0000 . ?
C11 N1 1.463(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N4 1.472(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 O1 1.211(7) . ?
C13 N1 1.399(7) . ?
C13 C14 1.502(7) . ?
C14 C21 1.386(7) . ?
C14 C15 1.389(7) . ?
C15 C16 1.408(7) . ?
C15 H15 0.9500 . ?
C16 C19 1.391(7) . ?
C16 C17 1.495(7) . ?
C17 O2 1.213(8) . ?
C17 N2 1.392(7) . ?
C18 O3 1.203(6) . ?
C18 N2 1.399(6) . ?
C18 C19 1.506(6) . ?
C19 C20 1.409(6) . ?
C20 C21 1.386(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.495(6) . ?
C22 O4 1.218(6) . ?
C22 N1 1.401(7) . ?
C23 C33 1.530(7) . ?
C23 C28 1.534(7) . ?
C23 C29 1.543(7) . ?
C23 C24 1.543(7) . ?
C24 C25 1.549(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C34 1.539(8) . ?
C25 C30 1.541(7) . ?
C25 C26 1.543(8) . ?
C26 C27 1.550(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.531(9) . ?
C27 C31 1.533(9) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C32 1.545(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C32 1.535(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.540(11) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32 1.0000 . ?
C33 N2 1.469(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 N3 1.471(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O5 1.189(7) . ?
C35 N3 1.396(7) . ?
C35 C36 1.506(7) . ?
C36 C37 1.394(7) . ?
C36 C43 1.405(7) . ?
C37 C38 1.380(7) . ?
C37 H37 0.9500 . ?
C38 C41 1.406(7) . ?
C38 C39 1.505(7) . ?
C39 O6 1.203(7) . ?
C39 N4 1.386(6) . ?
C40 O7 1.198(7) . ?
C40 N4 1.419(7) . ?
C40 C41 1.490(8) . ?
C41 C42 1.376(7) . ?
C42 C43 1.390(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.484(7) . ?
C44 O8 1.217(7) . ?
C44 N3 1.397(7) . ?
C45 I1 2.152(7) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.532(13) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.511(13) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C48 1.74(3) 3_776 ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 O9 1.227(16) . ?
C49 C51 1.44(3) . ?
C49 C50 1.62(3) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.486(10) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.617(10) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C54 1.543(12) 3_766 ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?

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 C1 C2 110.6(4) . . ?
C11 C1 C7 108.6(4) . . ?
C2 C1 C7 108.5(4) . . ?
C11 C1 C6 110.7(4) . . ?
C2 C1 C6 108.9(4) . . ?
C7 C1 C6 109.6(4) . . ?
C3 C2 C1 110.8(4) . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C12 110.8(4) . . ?
C2 C3 C4 109.4(4) . . ?
C12 C3 C4 112.0(4) . . ?
C2 C3 C8 108.7(4) . . ?
C12 C3 C8 107.4(4) . . ?
C4 C3 C8 108.5(4) . . ?
C5 C4 C3 111.0(4) . . ?
C5 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
C5 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
C4 C5 C9 109.3(5) . . ?
C4 C5 C6 109.6(4) . . ?
C9 C5 C6 109.9(5) . . ?
C4 C5 H5 109.3 . . ?
C9 C5 H5 109.3 . . ?
C6 C5 H5 109.3 . . ?
C5 C6 C1 109.3(5) . . ?
C5 C6 H6A 109.8 . . ?
C1 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
C1 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
C10 C7 C1 110.0(4) . . ?
C10 C7 H7A 109.7 . . ?
C1 C7 H7A 109.7 . . ?
C10 C7 H7B 109.7 . . ?
C1 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C3 C8 C10 109.5(4) . . ?
C3 C8 H8A 109.8 . . ?
C10 C8 H8A 109.8 . . ?
C3 C8 H8B 109.8 . . ?
C10 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C5 C9 C10 109.4(5) . . ?
C5 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
C5 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
C9 C10 C7 109.0(5) . . ?
C9 C10 C8 110.4(5) . . ?
C7 C10 C8 108.7(5) . . ?
C9 C10 H10 109.6 . . ?
C7 C10 H10 109.6 . . ?
C8 C10 H10 109.6 . . ?
N1 C11 C1 114.5(4) . . ?
N1 C11 H11A 108.6 . . ?
C1 C11 H11A 108.6 . . ?
N1 C11 H11B 108.6 . . ?
C1 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
N4 C12 C3 114.1(4) . . ?
N4 C12 H12A 108.7 . . ?
C3 C12 H12A 108.7 . . ?
N4 C12 H12B 108.7 . . ?
C3 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O1 C13 N1 125.7(5) . . ?
O1 C13 C14 128.1(5) . . ?
N1 C13 C14 106.1(5) . . ?
C21 C14 C15 123.9(5) . . ?
C21 C14 C13 108.1(5) . . ?
C15 C14 C13 128.0(5) . . ?
C14 C15 C16 113.7(4) . . ?
C14 C15 H15 123.2 . . ?
C16 C15 H15 123.2 . . ?
C19 C16 C15 121.9(5) . . ?
C19 C16 C17 108.6(5) . . ?
C15 C16 C17 129.5(5) . . ?
O2 C17 N2 125.6(5) . . ?
O2 C17 C16 128.3(5) . . ?
N2 C17 C16 106.0(5) . . ?
O3 C18 N2 125.0(4) . . ?
O3 C18 C19 129.0(4) . . ?
N2 C18 C19 106.0(4) . . ?
C16 C19 C20 124.1(4) . . ?
C16 C19 C18 107.3(4) . . ?
C20 C19 C18 128.6(4) . . ?
C21 C20 C19 112.9(4) . . ?
C21 C20 H20 123.5 . . ?
C19 C20 H20 123.5 . . ?
C20 C21 C14 123.5(5) . . ?
C20 C21 C22 128.7(4) . . ?
C14 C21 C22 107.8(4) . . ?
O4 C22 N1 124.9(4) . . ?
O4 C22 C21 128.5(5) . . ?
N1 C22 C21 106.6(4) . . ?
C33 C23 C28 111.0(4) . . ?
C33 C23 C29 107.0(4) . . ?
C28 C23 C29 109.6(5) . . ?
C33 C23 C24 110.8(4) . . ?
C28 C23 C24 110.0(4) . . ?
C29 C23 C24 108.4(4) . . ?
C23 C24 C25 110.3(4) . . ?
C23 C24 H24A 109.6 . . ?
C25 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
C25 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
C34 C25 C30 107.9(4) . . ?
C34 C25 C26 111.7(5) . . ?
C30 C25 C26 108.9(5) . . ?
C34 C25 C24 111.8(4) . . ?
C30 C25 C24 108.5(4) . . ?
C26 C25 C24 108.0(4) . . ?
C25 C26 C27 111.2(5) . . ?
C25 C26 H26A 109.4 . . ?
C27 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
C27 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C31 109.8(6) . . ?
C28 C27 C26 107.7(5) . . ?
C31 C27 C26 109.3(5) . . ?
C28 C27 H27 110.0 . . ?
C31 C27 H27 110.0 . . ?
C26 C27 H27 110.0 . . ?
C27 C28 C23 110.5(4) . . ?
C27 C28 H28A 109.6 . . ?
C23 C28 H28A 109.6 . . ?
C27 C28 H28B 109.6 . . ?
C23 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
C23 C29 C32 109.5(5) . . ?
C23 C29 H29A 109.8 . . ?
C32 C29 H29A 109.8 . . ?
C23 C29 H29B 109.8 . . ?
C32 C29 H29B 109.8 . . ?
H29A C29 H29B 108.2 . . ?
C32 C30 C25 110.7(5) . . ?
C32 C30 H30A 109.5 . . ?
C25 C30 H30A 109.5 . . ?
C32 C30 H30B 109.5 . . ?
C25 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C27 C31 C32 110.1(5) . . ?
C27 C31 H31A 109.6 . . ?
C32 C31 H31A 109.6 . . ?
C27 C31 H31B 109.6 . . ?
C32 C31 H31B 109.6 . . ?
H31A C31 H31B 108.2 . . ?
C30 C32 C31 109.1(6) . . ?
C30 C32 C29 109.5(5) . . ?
C31 C32 C29 109.4(5) . . ?
C30 C32 H32 109.6 . . ?
C31 C32 H32 109.6 . . ?
C29 C32 H32 109.6 . . ?
N2 C33 C23 114.3(4) . . ?
N2 C33 H33A 108.7 . . ?
C23 C33 H33A 108.7 . . ?
N2 C33 H33B 108.7 . . ?
C23 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
N3 C34 C25 112.8(4) . . ?
N3 C34 H34A 109.0 . . ?
C25 C34 H34A 109.0 . . ?
N3 C34 H34B 109.0 . . ?
C25 C34 H34B 109.0 . . ?
H34A C34 H34B 107.8 . . ?
O5 C35 N3 125.8(5) . . ?
O5 C35 C36 129.0(5) . . ?
N3 C35 C36 105.2(4) . . ?
C37 C36 C43 122.5(5) . . ?
C37 C36 C35 129.1(5) . . ?
C43 C36 C35 108.3(5) . . ?
C38 C37 C36 114.4(5) . . ?
C38 C37 H37 122.8 . . ?
C36 C37 H37 122.8 . . ?
C37 C38 C41 123.1(5) . . ?
C37 C38 C39 129.3(5) . . ?
C41 C38 C39 107.5(4) . . ?
O6 C39 N4 125.8(5) . . ?
O6 C39 C38 127.6(5) . . ?
N4 C39 C38 106.5(4) . . ?
O7 C40 N4 125.0(5) . . ?
O7 C40 C41 129.0(5) . . ?
N4 C40 C41 105.9(4) . . ?
C42 C41 C38 122.6(5) . . ?
C42 C41 C40 129.4(5) . . ?
C38 C41 C40 108.0(5) . . ?
C41 C42 C43 114.9(5) . . ?
C41 C42 H42 122.5 . . ?
C43 C42 H42 122.5 . . ?
C42 C43 C36 122.5(5) . . ?
C42 C43 C44 130.4(5) . . ?
C36 C43 C44 107.1(5) . . ?
O8 C44 N3 124.4(5) . . ?
O8 C44 C43 128.7(5) . . ?
N3 C44 C43 106.9(4) . . ?
C13 N1 C22 111.2(4) . . ?
C13 N1 C11 124.7(4) . . ?
C22 N1 C11 124.1(4) . . ?
C17 N2 C18 112.0(4) . . ?
C17 N2 C33 125.1(5) . . ?
C18 N2 C33 122.7(4) . . ?
C35 N3 C44 112.0(4) . . ?
C35 N3 C34 125.7(5) . . ?
C44 N3 C34 122.0(4) . . ?
C39 N4 C40 111.5(4) . . ?
C39 N4 C12 123.7(4) . . ?
C40 N4 C12 123.8(4) . . ?
I1 C45 H45A 109.5 . . ?
I1 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
I1 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C46 102.3(10) . . ?
C48 C47 H47A 111.3 . . ?
C46 C47 H47A 111.3 . . ?
C48 C47 H47B 111.3 . . ?
C46 C47 H47B 111.3 . . ?
H47A C47 H47B 109.2 . . ?
C47 C48 C48 104.7(12) . 3_776 ?
C47 C48 H48A 110.8 . . ?
C48 C48 H48A 110.8 3_776 . ?
C47 C48 H48B 110.8 . . ?
C48 C48 H48B 110.8 3_776 . ?
H48A C48 H48B 108.9 . . ?
O9 C49 C51 106.9(18) . . ?
O9 C49 C50 129.0(19) . . ?
C51 C49 C50 124.1(16) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C52 C53 C54 95.5(7) . . ?
C52 C53 H53A 112.6 . . ?
C54 C53 H53A 112.6 . . ?
C52 C53 H53B 112.6 . . ?
C54 C53 H53B 112.6 . . ?
H53A C53 H53B 110.1 . . ?
C54 C54 C53 132.5(10) 3_766 . ?
C54 C54 H54A 104.1 3_766 . ?
C53 C54 H54A 104.1 . . ?
C54 C54 H54B 104.1 3_766 . ?
C53 C54 H54B 104.1 . . ?
H54A C54 H54B 105.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 C1 C2 C3 -178.9(4) . . . . ?
C7 C1 C2 C3 -59.9(5) . . . . ?
C6 C1 C2 C3 59.3(5) . . . . ?
C1 C2 C3 C12 178.3(4) . . . . ?
C1 C2 C3 C4 -57.8(5) . . . . ?
C1 C2 C3 C8 60.5(5) . . . . ?
C2 C3 C4 C5 57.9(5) . . . . ?
C12 C3 C4 C5 -178.8(4) . . . . ?
C8 C3 C4 C5 -60.5(6) . . . . ?
C3 C4 C5 C9 61.1(6) . . . . ?
C3 C4 C5 C6 -59.5(6) . . . . ?
C4 C5 C6 C1 60.3(6) . . . . ?
C9 C5 C6 C1 -59.9(6) . . . . ?
C11 C1 C6 C5 178.3(4) . . . . ?
C2 C1 C6 C5 -59.9(5) . . . . ?
C7 C1 C6 C5 58.6(5) . . . . ?
C11 C1 C7 C10 179.9(5) . . . . ?
C2 C1 C7 C10 59.7(6) . . . . ?
C6 C1 C7 C10 -59.1(6) . . . . ?
C2 C3 C8 C10 -60.4(6) . . . . ?
C12 C3 C8 C10 179.6(5) . . . . ?
C4 C3 C8 C10 58.5(6) . . . . ?
C4 C5 C9 C10 -59.3(7) . . . . ?
C6 C5 C9 C10 61.0(7) . . . . ?
C5 C9 C10 C7 -60.5(6) . . . . ?
C5 C9 C10 C8 58.8(7) . . . . ?
C1 C7 C10 C9 59.8(6) . . . . ?
C1 C7 C10 C8 -60.6(6) . . . . ?
C3 C8 C10 C9 -58.8(6) . . . . ?
C3 C8 C10 C7 60.7(6) . . . . ?
C2 C1 C11 N1 -51.4(5) . . . . ?
C7 C1 C11 N1 -170.4(4) . . . . ?
C6 C1 C11 N1 69.3(5) . . . . ?
C2 C3 C12 N4 54.4(6) . . . . ?
C4 C3 C12 N4 -68.1(6) . . . . ?
C8 C3 C12 N4 172.9(4) . . . . ?
O1 C13 C14 C21 -176.4(6) . . . . ?
N1 C13 C14 C21 1.8(6) . . . . ?
O1 C13 C14 C15 3.6(10) . . . . ?
N1 C13 C14 C15 -178.3(5) . . . . ?
C21 C14 C15 C16 -1.7(8) . . . . ?
C13 C14 C15 C16 178.4(5) . . . . ?
C14 C15 C16 C19 0.6(7) . . . . ?
C14 C15 C16 C17 -178.2(5) . . . . ?
C19 C16 C17 O2 178.1(6) . . . . ?
C15 C16 C17 O2 -2.9(10) . . . . ?
C19 C16 C17 N2 -0.6(6) . . . . ?
C15 C16 C17 N2 178.3(5) . . . . ?
C15 C16 C19 C20 0.7(8) . . . . ?
C17 C16 C19 C20 179.8(5) . . . . ?
C15 C16 C19 C18 179.3(4) . . . . ?
C17 C16 C19 C18 -1.6(6) . . . . ?
O3 C18 C19 C16 -176.5(5) . . . . ?
N2 C18 C19 C16 3.2(5) . . . . ?
O3 C18 C19 C20 2.0(8) . . . . ?
N2 C18 C19 C20 -178.2(5) . . . . ?
C16 C19 C20 C21 -0.9(7) . . . . ?
C18 C19 C20 C21 -179.2(4) . . . . ?
C19 C20 C21 C14 -0.2(7) . . . . ?
C19 C20 C21 C22 -179.2(5) . . . . ?
C15 C14 C21 C20 1.6(9) . . . . ?
C13 C14 C21 C20 -178.4(5) . . . . ?
C15 C14 C21 C22 -179.3(5) . . . . ?
C13 C14 C21 C22 0.7(6) . . . . ?
C20 C21 C22 O4 -5.2(9) . . . . ?
C14 C21 C22 O4 175.7(5) . . . . ?
C20 C21 C22 N1 176.2(5) . . . . ?
C14 C21 C22 N1 -2.9(6) . . . . ?
C33 C23 C24 C25 178.3(4) . . . . ?
C28 C23 C24 C25 -58.6(5) . . . . ?
C29 C23 C24 C25 61.1(6) . . . . ?
C23 C24 C25 C34 -178.6(4) . . . . ?
C23 C24 C25 C30 -59.7(5) . . . . ?
C23 C24 C25 C26 58.1(5) . . . . ?
C34 C25 C26 C27 176.5(4) . . . . ?
C30 C25 C26 C27 57.4(6) . . . . ?
C24 C25 C26 C27 -60.2(6) . . . . ?
C25 C26 C27 C28 61.2(6) . . . . ?
C25 C26 C27 C31 -58.1(7) . . . . ?
C31 C27 C28 C23 59.0(6) . . . . ?
C26 C27 C28 C23 -60.0(6) . . . . ?
C33 C23 C28 C27 -177.2(5) . . . . ?
C29 C23 C28 C27 -59.2(6) . . . . ?
C24 C23 C28 C27 59.8(6) . . . . ?
C33 C23 C29 C32 179.7(5) . . . . ?
C28 C23 C29 C32 59.2(6) . . . . ?
C24 C23 C29 C32 -60.8(6) . . . . ?
C34 C25 C30 C32 179.9(5) . . . . ?
C26 C25 C30 C32 -58.7(6) . . . . ?
C24 C25 C30 C32 58.7(6) . . . . ?
C28 C27 C31 C32 -59.0(7) . . . . ?
C26 C27 C31 C32 59.0(8) . . . . ?
C25 C30 C32 C31 60.3(6) . . . . ?
C25 C30 C32 C29 -59.4(7) . . . . ?
C27 C31 C32 C30 -60.3(7) . . . . ?
C27 C31 C32 C29 59.4(7) . . . . ?
C23 C29 C32 C30 60.1(6) . . . . ?
C23 C29 C32 C31 -59.4(6) . . . . ?
C28 C23 C33 N2 -67.7(6) . . . . ?
C29 C23 C33 N2 172.7(4) . . . . ?
C24 C23 C33 N2 54.8(6) . . . . ?
C30 C25 C34 N3 -171.7(5) . . . . ?
C26 C25 C34 N3 68.6(6) . . . . ?
C24 C25 C34 N3 -52.5(6) . . . . ?
O5 C35 C36 C37 4.1(9) . . . . ?
N3 C35 C36 C37 -174.1(5) . . . . ?
O5 C35 C36 C43 -178.5(5) . . . . ?
N3 C35 C36 C43 3.3(5) . . . . ?
C43 C36 C37 C38 0.2(7) . . . . ?
C35 C36 C37 C38 177.3(4) . . . . ?
C36 C37 C38 C41 -0.6(7) . . . . ?
C36 C37 C38 C39 -177.8(4) . . . . ?
C37 C38 C39 O6 -2.7(8) . . . . ?
C41 C38 C39 O6 179.8(5) . . . . ?
C37 C38 C39 N4 174.8(5) . . . . ?
C41 C38 C39 N4 -2.7(5) . . . . ?
C37 C38 C41 C42 1.0(8) . . . . ?
C39 C38 C41 C42 178.7(4) . . . . ?
C37 C38 C41 C40 -179.5(4) . . . . ?
C39 C38 C41 C40 -1.9(5) . . . . ?
O7 C40 C41 C42 5.7(9) . . . . ?
N4 C40 C41 C42 -175.0(5) . . . . ?
O7 C40 C41 C38 -173.7(6) . . . . ?
N4 C40 C41 C38 5.7(5) . . . . ?
C38 C41 C42 C43 -0.8(7) . . . . ?
C40 C41 C42 C43 179.9(5) . . . . ?
C41 C42 C43 C36 0.3(7) . . . . ?
C41 C42 C43 C44 -177.9(5) . . . . ?
C37 C36 C43 C42 0.0(8) . . . . ?
C35 C36 C43 C42 -177.7(5) . . . . ?
C37 C36 C43 C44 178.5(4) . . . . ?
C35 C36 C43 C44 0.9(5) . . . . ?
C42 C43 C44 O8 -8.1(9) . . . . ?
C36 C43 C44 O8 173.4(5) . . . . ?
C42 C43 C44 N3 173.6(5) . . . . ?
C36 C43 C44 N3 -4.8(5) . . . . ?
O1 C13 N1 C22 174.5(5) . . . . ?
C14 C13 N1 C22 -3.7(6) . . . . ?
O1 C13 N1 C11 -5.8(8) . . . . ?
C14 C13 N1 C11 176.0(4) . . . . ?
O4 C22 N1 C13 -174.6(5) . . . . ?
C21 C22 N1 C13 4.1(5) . . . . ?
O4 C22 N1 C11 5.7(8) . . . . ?
C21 C22 N1 C11 -175.6(4) . . . . ?
C1 C11 N1 C13 -87.5(6) . . . . ?
C1 C11 N1 C22 92.2(6) . . . . ?
O2 C17 N2 C18 -176.0(5) . . . . ?
C16 C17 N2 C18 2.8(6) . . . . ?
O2 C17 N2 C33 -0.5(9) . . . . ?
C16 C17 N2 C33 178.2(5) . . . . ?
O3 C18 N2 C17 176.0(5) . . . . ?
C19 C18 N2 C17 -3.8(6) . . . . ?
O3 C18 N2 C33 0.4(8) . . . . ?
C19 C18 N2 C33 -179.3(4) . . . . ?
C23 C33 N2 C17 88.5(6) . . . . ?
C23 C33 N2 C18 -96.5(6) . . . . ?
O5 C35 N3 C44 175.1(5) . . . . ?
C36 C35 N3 C44 -6.6(5) . . . . ?
O5 C35 N3 C34 0.9(8) . . . . ?
C36 C35 N3 C34 179.2(4) . . . . ?
O8 C44 N3 C35 -171.1(5) . . . . ?
C43 C44 N3 C35 7.3(6) . . . . ?
O8 C44 N3 C34 3.4(8) . . . . ?
C43 C44 N3 C34 -178.3(4) . . . . ?
C25 C34 N3 C35 -90.1(6) . . . . ?
C25 C34 N3 C44 96.2(6) . . . . ?
O6 C39 N4 C40 -175.9(5) . . . . ?
C38 C39 N4 C40 6.5(5) . . . . ?
O6 C39 N4 C12 -6.7(8) . . . . ?
C38 C39 N4 C12 175.7(4) . . . . ?
O7 C40 N4 C39 171.8(5) . . . . ?
C41 C40 N4 C39 -7.6(6) . . . . ?
O7 C40 N4 C12 2.6(8) . . . . ?
C41 C40 N4 C12 -176.8(4) . . . . ?
C3 C12 N4 C39 90.3(6) . . . . ?
C3 C12 N4 C40 -101.8(6) . . . . ?
C46 C47 C48 C48 177.9(13) . . . 3_776 ?
C52 C53 C54 C54 -158.6(14) . . . 3_766 ?

_refine_diff_density_max         11.400
_refine_diff_density_min         -4.862
_refine_diff_density_rms         0.361



####################################################################### 
# 
# 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_1a_with_SQUEEZE
_database_code_depnum_ccdc_archive 'CCDC 2133051'
loop_
_audit_author_name
_audit_author_address
'Tadashi Hyodo'
;Tokushima Bunri University
Japan
;
_audit_update_record             
;
2022-01-11 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H43 I N4 O8'
_chemical_formula_weight         894.73

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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   18.087(3)
_cell_length_b                   16.027(3)
_cell_length_c                   16.477(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.124(4)
_cell_angle_gamma                90
_cell_volume                     4588.6(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9742
_cell_measurement_theta_min      3.61
_cell_measurement_theta_max      78.44

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_F_000             1832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.919
_shelx_estimated_absorpt_T_min   0.384
_shelx_estimated_absorpt_T_max   0.589
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3516
_exptl_absorpt_correction_T_max  0.5600
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            67015
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.543
_diffrn_reflns_theta_max         80.219
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9739
_reflns_number_gt                9518
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (Hübschle et al., 2011)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1039P)²+7.0032P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9739
_refine_ls_number_parameters     527
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1586
_refine_ls_wR_factor_gt          0.1505
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.82323(15) 0.68260(19) 0.29627(18) 0.0208(5) Uani 1 1 d . . . . .
C2 C 0.77493(16) 0.60302(18) 0.26990(18) 0.0202(5) Uani 1 1 d . . . . .
H2A H 0.798916 0.556380 0.307410 0.024 Uiso 1 1 calc R U . . .
H2B H 0.722659 0.612015 0.276216 0.024 Uiso 1 1 calc R U . . .
C3 C 0.76914(17) 0.58007(19) 0.17794(19) 0.0226(6) Uani 1 1 d . . . . .
C4 C 0.73275(17) 0.65354(19) 0.12038(18) 0.0233(6) Uani 1 1 d . . . . .
H4A H 0.729028 0.639449 0.060878 0.028 Uiso 1 1 calc R U . . .
H4B H 0.680081 0.663779 0.124963 0.028 Uiso 1 1 calc R U . . .
C5 C 0.7817(2) 0.73270(19) 0.1460(2) 0.0269(7) Uani 1 1 d . . . . .
H5 H 0.757428 0.779917 0.108288 0.032 Uiso 1 1 calc R U . . .
C6 C 0.78603(18) 0.7545(2) 0.2378(2) 0.0229(6) Uani 1 1 d . . . . .
H6A H 0.816723 0.805948 0.254579 0.027 Uiso 1 1 calc R U . . .
H6B H 0.733581 0.764891 0.242976 0.027 Uiso 1 1 calc R U . . .
C7 C 0.90436(17) 0.6671(2) 0.2864(2) 0.0292(7) Uani 1 1 d . . . . .
H7A H 0.936091 0.717938 0.303026 0.035 Uiso 1 1 calc R U . . .
H7B H 0.929318 0.621116 0.324257 0.035 Uiso 1 1 calc R U . . .
C8 C 0.85115(19) 0.5658(2) 0.1694(2) 0.0319(7) Uani 1 1 d . . . . .
H8A H 0.875616 0.518729 0.206041 0.038 Uiso 1 1 calc R U . . .
H8B H 0.848272 0.551068 0.110267 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8629(2) 0.7169(3) 0.1373(2) 0.0370(8) Uani 1 1 d . . . . .
H9A H 0.859983 0.703215 0.077957 0.044 Uiso 1 1 calc R U . . .
H9B H 0.894621 0.767826 0.153297 0.044 Uiso 1 1 calc R U . . .
C10 C 0.89986(18) 0.6446(3) 0.1949(2) 0.0343(8) Uani 1 1 d . . . . .
H10 H 0.952876 0.634403 0.189624 0.041 Uiso 1 1 calc R U . . .
C11 C 0.83092(16) 0.70369(19) 0.38929(19) 0.0231(6) Uani 1 1 d . . . . .
H11A H 0.863980 0.661142 0.425481 0.028 Uiso 1 1 calc R U . . .
H11B H 0.857096 0.758270 0.402659 0.028 Uiso 1 1 calc R U . . .
C12 C 0.72307(18) 0.49922(19) 0.1527(2) 0.0258(6) Uani 1 1 d . . . . .
H12A H 0.716955 0.488437 0.092017 0.031 Uiso 1 1 calc R U . . .
H12B H 0.752883 0.452344 0.185068 0.031 Uiso 1 1 calc R U . . .
C13 C 0.71126(17) 0.77817(19) 0.40290(19) 0.0202(5) Uani 1 1 d . . . . .
C14 C 0.64036(17) 0.75111(19) 0.42551(18) 0.0185(5) Uani 1 1 d . . . . .
C15 C 0.57523(16) 0.79734(16) 0.42502(17) 0.0184(5) Uani 1 1 d . . . . .
H15 H 0.569979 0.854756 0.410215 0.022 Uiso 1 1 calc R U . . .
C16 C 0.51813(18) 0.75224(18) 0.44813(18) 0.0181(5) Uani 1 1 d . . . . .
C17 C 0.44111(17) 0.78071(19) 0.45337(18) 0.0202(5) Uani 1 1 d . . . . .
C18 C 0.45485(17) 0.64164(18) 0.49175(18) 0.0206(5) Uani 1 1 d . . . . .
C19 C 0.52640(16) 0.66796(17) 0.47017(17) 0.0184(5) Uani 1 1 d . . . . .
C20 C 0.59207(16) 0.62197(17) 0.47145(17) 0.0203(5) Uani 1 1 d . . . . .
H20 H 0.597713 0.564714 0.486843 0.024 Uiso 1 1 calc R U . . .
C21 C 0.64861(16) 0.66706(18) 0.44826(17) 0.0185(5) Uani 1 1 d . . . . .
C22 C 0.72574(16) 0.63881(18) 0.44176(18) 0.0208(5) Uani 1 1 d . . . . .
C23 C 0.26336(17) 0.69125(19) 0.4133(2) 0.0231(6) Uani 1 1 d . . . . .
C24 C 0.27682(17) 0.60953(18) 0.37018(19) 0.0224(6) Uani 1 1 d . . . . .
H24A H 0.282952 0.562726 0.410721 0.027 Uiso 1 1 calc R U . . .
H24B H 0.324747 0.614135 0.352606 0.027 Uiso 1 1 calc R U . . .
C25 C 0.20840(17) 0.5916(2) 0.2921(2) 0.0253(6) Uani 1 1 d . . . . .
C26 C 0.19856(18) 0.6653(2) 0.2306(2) 0.0284(6) Uani 1 1 d . . . . .
H26A H 0.154799 0.654310 0.180300 0.034 Uiso 1 1 calc R U . . .
H26B H 0.245597 0.671580 0.211580 0.034 Uiso 1 1 calc R U . . .
C27 C 0.1837(2) 0.7465(2) 0.2734(2) 0.0307(7) Uani 1 1 d . . . . .
H27 H 0.177338 0.793764 0.232503 0.037 Uiso 1 1 calc R U . . .
C28 C 0.25207(19) 0.76379(18) 0.3497(2) 0.0261(7) Uani 1 1 d . . . . .
H28A H 0.243126 0.816211 0.377334 0.031 Uiso 1 1 calc R U . . .
H28B H 0.299194 0.770843 0.331004 0.031 Uiso 1 1 calc R U . . .
C29 C 0.18900(19) 0.6813(2) 0.4414(2) 0.0316(7) Uani 1 1 d . . . . .
H29A H 0.195272 0.634657 0.482189 0.038 Uiso 1 1 calc R U . . .
H29B H 0.179541 0.732924 0.470001 0.038 Uiso 1 1 calc R U . . .
C30 C 0.13461(19) 0.5834(2) 0.3218(3) 0.0337(7) Uani 1 1 d . . . . .
H30A H 0.089914 0.572151 0.272570 0.040 Uiso 1 1 calc R U . . .
H30B H 0.140149 0.536021 0.361556 0.040 Uiso 1 1 calc R U . . .
C31 C 0.1103(2) 0.7371(2) 0.3022(3) 0.0387(9) Uani 1 1 d . . . . .
H31A H 0.065769 0.726071 0.252690 0.046 Uiso 1 1 calc R U . . .
H31B H 0.100272 0.789394 0.329289 0.046 Uiso 1 1 calc R U . . .
C32 C 0.12077(19) 0.6641(2) 0.3655(3) 0.0363(8) Uani 1 1 d . . . . .
H32 H 0.073170 0.657964 0.384577 0.044 Uiso 1 1 calc R U . . .
C33 C 0.32949(18) 0.7095(2) 0.4924(2) 0.0247(6) Uani 1 1 d . . . . .
H33A H 0.320301 0.764275 0.515640 0.030 Uiso 1 1 calc R U . . .
H33B H 0.329523 0.666597 0.535603 0.030 Uiso 1 1 calc R U . . .
C34 C 0.21962(18) 0.5093(2) 0.2493(2) 0.0293(6) Uani 1 1 d . . . . .
H34A H 0.215144 0.462361 0.286656 0.035 Uiso 1 1 calc R U . . .
H34B H 0.177877 0.503462 0.196088 0.035 Uiso 1 1 calc R U . . .
C35 C 0.30875(19) 0.52973(19) 0.1554(2) 0.0257(6) Uani 1 1 d . . . . .
C36 C 0.39228(17) 0.51313(17) 0.16660(18) 0.0220(6) Uani 1 1 d . . . . .
C37 C 0.43794(17) 0.53378(17) 0.11405(18) 0.0214(5) Uani 1 1 d . . . . .
H37 H 0.417805 0.560375 0.060960 0.026 Uiso 1 1 calc R U . . .
C38 C 0.51501(18) 0.51261(17) 0.14500(18) 0.0218(6) Uani 1 1 d . . . . .
C39 C 0.58012(17) 0.52806(17) 0.10783(18) 0.0218(6) Uani 1 1 d . . . . .
C40 C 0.62948(18) 0.46202(19) 0.23591(19) 0.0247(6) Uani 1 1 d . . . . .
C41 C 0.54504(18) 0.47378(17) 0.22305(19) 0.0223(6) Uani 1 1 d . . . . .
C42 C 0.49945(18) 0.45391(18) 0.27596(19) 0.0239(6) Uani 1 1 d . . . . .
H42 H 0.519704 0.428341 0.329562 0.029 Uiso 1 1 calc R U . . .
C43 C 0.42226(18) 0.47428(18) 0.24443(19) 0.0233(6) Uani 1 1 d . . . . .
C44 C 0.35753(19) 0.46389(19) 0.2837(2) 0.0256(6) Uani 1 1 d . . . . .
N1 N 0.75758(14) 0.70735(16) 0.41028(15) 0.0205(5) Uani 1 1 d . . . . .
N2 N 0.40559(14) 0.71071(16) 0.47653(16) 0.0212(5) Uani 1 1 d . . . . .
N3 N 0.29386(15) 0.50360(16) 0.23027(17) 0.0255(5) Uani 1 1 d . . . . .
N4 N 0.64667(15) 0.50069(16) 0.16719(16) 0.0223(5) Uani 1 1 d . . . . .
O1 O 0.72709(13) 0.84702(13) 0.38226(14) 0.0260(4) Uani 1 1 d . . . . .
O2 O 0.41262(12) 0.84964(13) 0.44042(14) 0.0240(4) Uani 1 1 d . . . . .
O3 O 0.44011(13) 0.57508(14) 0.51771(14) 0.0264(4) Uani 1 1 d . . . . .
O4 O 0.75671(13) 0.57210(14) 0.46007(15) 0.0276(5) Uani 1 1 d . . . . .
O5 O 0.26263(14) 0.56093(16) 0.09548(15) 0.0327(5) Uani 1 1 d . . . . .
O6 O 0.57826(13) 0.55881(14) 0.04053(13) 0.0249(4) Uani 1 1 d . . . . .
O7 O 0.67482(14) 0.42558(15) 0.29224(15) 0.0328(5) Uani 1 1 d . . . . .
O8 O 0.35763(15) 0.42813(15) 0.34836(15) 0.0321(5) Uani 1 1 d . . . . .
C45 C 0.4316(2) 0.72925(19) 0.2237(2) 0.0279(7) Uani 1 1 d . . . . .
H45A H 0.420352 0.783929 0.244126 0.042 Uiso 1 1 calc R U . . .
H45B H 0.434473 0.687275 0.267736 0.042 Uiso 1 1 calc R U . . .
H45C H 0.390623 0.714157 0.173060 0.042 Uiso 1 1 calc R U . . .
I1 I 0.53966(2) 0.73447(2) 0.19348(2) 0.03255(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.532(4) . ?
C1 C11 1.538(4) . ?
C1 C2 1.539(4) . ?
C1 C7 1.540(4) . ?
C2 C3 1.534(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C12 1.534(4) . ?
C3 C4 1.540(4) . ?
C3 C8 1.545(4) . ?
C4 C5 1.538(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.533(5) . ?
C5 C9 1.535(5) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C10 1.531(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C10 1.531(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.529(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10 1.0000 . ?
C11 N1 1.462(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N4 1.466(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 O1 1.212(4) . ?
C13 N1 1.396(4) . ?
C13 C14 1.496(4) . ?
C14 C15 1.390(4) . ?
C14 C21 1.395(4) . ?
C15 C16 1.397(4) . ?
C15 H15 0.9500 . ?
C16 C19 1.396(4) . ?
C16 C17 1.491(4) . ?
C17 O2 1.213(4) . ?
C17 N2 1.397(4) . ?
C18 O3 1.206(4) . ?
C18 N2 1.399(4) . ?
C18 C19 1.495(4) . ?
C19 C20 1.393(4) . ?
C20 C21 1.390(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.499(4) . ?
C22 O4 1.206(4) . ?
C22 N1 1.405(4) . ?
C23 C33 1.532(4) . ?
C23 C28 1.541(4) . ?
C23 C24 1.542(4) . ?
C23 C29 1.547(4) . ?
C24 C25 1.544(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.535(4) . ?
C25 C34 1.535(4) . ?
C25 C30 1.549(4) . ?
C26 C27 1.538(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.524(5) . ?
C27 C31 1.536(5) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C32 1.519(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C32 1.533(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.545(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32 1.0000 . ?
C33 N2 1.471(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 N3 1.464(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O5 1.210(4) . ?
C35 N3 1.398(4) . ?
C35 C36 1.494(4) . ?
C36 C37 1.392(4) . ?
C36 C43 1.393(4) . ?
C37 C38 1.387(4) . ?
C37 H37 0.9500 . ?
C38 C41 1.396(4) . ?
C38 C39 1.491(4) . ?
C39 O6 1.205(4) . ?
C39 N4 1.394(4) . ?
C40 O7 1.205(4) . ?
C40 N4 1.400(4) . ?
C40 C41 1.494(4) . ?
C41 C42 1.393(4) . ?
C42 C43 1.387(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.496(4) . ?
C44 O8 1.210(4) . ?
C44 N3 1.394(4) . ?
C45 I1 2.149(3) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C11 111.3(2) . . ?
C6 C1 C2 109.3(2) . . ?
C11 C1 C2 110.5(2) . . ?
C6 C1 C7 108.6(3) . . ?
C11 C1 C7 108.4(2) . . ?
C2 C1 C7 108.6(2) . . ?
C3 C2 C1 110.8(2) . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C12 110.7(2) . . ?
C2 C3 C4 109.0(2) . . ?
C12 C3 C4 111.8(2) . . ?
C2 C3 C8 108.7(2) . . ?
C12 C3 C8 108.2(3) . . ?
C4 C3 C8 108.3(3) . . ?
C5 C4 C3 110.3(2) . . ?
C5 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
C5 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 C9 110.0(3) . . ?
C6 C5 C4 109.0(2) . . ?
C9 C5 C4 109.4(3) . . ?
C6 C5 H5 109.5 . . ?
C9 C5 H5 109.5 . . ?
C4 C5 H5 109.5 . . ?
C1 C6 C5 110.0(3) . . ?
C1 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C1 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C10 C7 C1 110.5(2) . . ?
C10 C7 H7A 109.6 . . ?
C1 C7 H7A 109.6 . . ?
C10 C7 H7B 109.6 . . ?
C1 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C10 C8 C3 110.3(3) . . ?
C10 C8 H8A 109.6 . . ?
C3 C8 H8A 109.6 . . ?
C10 C8 H8B 109.6 . . ?
C3 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C5 109.4(3) . . ?
C10 C9 H9A 109.8 . . ?
C5 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
C5 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
C9 C10 C8 109.7(3) . . ?
C9 C10 C7 109.0(3) . . ?
C8 C10 C7 109.5(3) . . ?
C9 C10 H10 109.5 . . ?
C8 C10 H10 109.5 . . ?
C7 C10 H10 109.5 . . ?
N1 C11 C1 114.1(2) . . ?
N1 C11 H11A 108.7 . . ?
C1 C11 H11A 108.7 . . ?
N1 C11 H11B 108.7 . . ?
C1 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N4 C12 C3 114.1(2) . . ?
N4 C12 H12A 108.7 . . ?
C3 C12 H12A 108.7 . . ?
N4 C12 H12B 108.7 . . ?
C3 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O1 C13 N1 125.6(3) . . ?
O1 C13 C14 128.3(3) . . ?
N1 C13 C14 106.1(2) . . ?
C15 C14 C21 122.9(3) . . ?
C15 C14 C13 128.9(3) . . ?
C21 C14 C13 108.2(3) . . ?
C14 C15 C16 114.3(3) . . ?
C14 C15 H15 122.8 . . ?
C16 C15 H15 122.8 . . ?
C19 C16 C15 122.5(3) . . ?
C19 C16 C17 108.4(3) . . ?
C15 C16 C17 129.1(3) . . ?
O2 C17 N2 125.1(3) . . ?
O2 C17 C16 128.8(3) . . ?
N2 C17 C16 106.1(2) . . ?
O3 C18 N2 124.8(3) . . ?
O3 C18 C19 128.7(3) . . ?
N2 C18 C19 106.5(2) . . ?
C20 C19 C16 123.0(3) . . ?
C20 C19 C18 129.6(3) . . ?
C16 C19 C18 107.3(2) . . ?
C21 C20 C19 114.2(3) . . ?
C21 C20 H20 122.9 . . ?
C19 C20 H20 122.9 . . ?
C20 C21 C14 123.0(3) . . ?
C20 C21 C22 129.3(3) . . ?
C14 C21 C22 107.7(2) . . ?
O4 C22 N1 125.2(3) . . ?
O4 C22 C21 128.8(3) . . ?
N1 C22 C21 106.0(2) . . ?
C33 C23 C28 111.0(3) . . ?
C33 C23 C24 111.6(2) . . ?
C28 C23 C24 109.6(3) . . ?
C33 C23 C29 107.7(3) . . ?
C28 C23 C29 108.6(3) . . ?
C24 C23 C29 108.2(2) . . ?
C23 C24 C25 110.5(2) . . ?
C23 C24 H24A 109.6 . . ?
C25 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
C25 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
C26 C25 C34 111.3(3) . . ?
C26 C25 C24 109.0(2) . . ?
C34 C25 C24 111.4(3) . . ?
C26 C25 C30 108.8(3) . . ?
C34 C25 C30 107.9(3) . . ?
C24 C25 C30 108.3(3) . . ?
C25 C26 C27 110.5(3) . . ?
C25 C26 H26A 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
C28 C27 C31 109.7(3) . . ?
C28 C27 C26 109.1(3) . . ?
C31 C27 C26 109.6(3) . . ?
C28 C27 H27 109.5 . . ?
C31 C27 H27 109.5 . . ?
C26 C27 H27 109.5 . . ?
C27 C28 C23 110.3(3) . . ?
C27 C28 H28A 109.6 . . ?
C23 C28 H28A 109.6 . . ?
C27 C28 H28B 109.6 . . ?
C23 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
C32 C29 C23 110.3(3) . . ?
C32 C29 H29A 109.6 . . ?
C23 C29 H29A 109.6 . . ?
C32 C29 H29B 109.6 . . ?
C23 C29 H29B 109.6 . . ?
H29A C29 H29B 108.1 . . ?
C32 C30 C25 110.1(3) . . ?
C32 C30 H30A 109.6 . . ?
C25 C30 H30A 109.6 . . ?
C32 C30 H30B 109.6 . . ?
C25 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
C27 C31 C32 109.1(3) . . ?
C27 C31 H31A 109.9 . . ?
C32 C31 H31A 109.9 . . ?
C27 C31 H31B 109.9 . . ?
C32 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
C29 C32 C30 109.8(3) . . ?
C29 C32 C31 109.7(3) . . ?
C30 C32 C31 109.1(3) . . ?
C29 C32 H32 109.4 . . ?
C30 C32 H32 109.4 . . ?
C31 C32 H32 109.4 . . ?
N2 C33 C23 113.6(2) . . ?
N2 C33 H33A 108.9 . . ?
C23 C33 H33A 108.9 . . ?
N2 C33 H33B 108.9 . . ?
C23 C33 H33B 108.9 . . ?
H33A C33 H33B 107.7 . . ?
N3 C34 C25 113.5(3) . . ?
N3 C34 H34A 108.9 . . ?
C25 C34 H34A 108.9 . . ?
N3 C34 H34B 108.9 . . ?
C25 C34 H34B 108.9 . . ?
H34A C34 H34B 107.7 . . ?
O5 C35 N3 125.9(3) . . ?
O5 C35 C36 128.2(3) . . ?
N3 C35 C36 105.9(3) . . ?
C37 C36 C43 122.2(3) . . ?
C37 C36 C35 129.4(3) . . ?
C43 C36 C35 108.4(3) . . ?
C38 C37 C36 115.0(3) . . ?
C38 C37 H37 122.5 . . ?
C36 C37 H37 122.5 . . ?
C37 C38 C41 122.8(3) . . ?
C37 C38 C39 129.5(3) . . ?
C41 C38 C39 107.6(3) . . ?
O6 C39 N4 124.9(3) . . ?
O6 C39 C38 128.5(3) . . ?
N4 C39 C38 106.6(2) . . ?
O7 C40 N4 125.5(3) . . ?
O7 C40 C41 128.3(3) . . ?
N4 C40 C41 106.1(3) . . ?
C42 C41 C38 122.1(3) . . ?
C42 C41 C40 129.9(3) . . ?
C38 C41 C40 107.9(3) . . ?
C43 C42 C41 114.9(3) . . ?
C43 C42 H42 122.5 . . ?
C41 C42 H42 122.5 . . ?
C42 C43 C36 123.0(3) . . ?
C42 C43 C44 129.7(3) . . ?
C36 C43 C44 107.2(3) . . ?
O8 C44 N3 124.8(3) . . ?
O8 C44 C43 128.6(3) . . ?
N3 C44 C43 106.6(3) . . ?
C13 N1 C22 111.7(2) . . ?
C13 N1 C11 125.0(2) . . ?
C22 N1 C11 123.2(2) . . ?
C17 N2 C18 111.5(2) . . ?
C17 N2 C33 125.6(3) . . ?
C18 N2 C33 122.6(2) . . ?
C44 N3 C35 111.5(3) . . ?
C44 N3 C34 122.7(3) . . ?
C35 N3 C34 125.7(3) . . ?
C39 N4 C40 111.4(3) . . ?
C39 N4 C12 124.0(3) . . ?
C40 N4 C12 123.8(3) . . ?
I1 C45 H45A 109.5 . . ?
I1 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
I1 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 58.9(3) . . . . ?
C11 C1 C2 C3 -178.2(2) . . . . ?
C7 C1 C2 C3 -59.4(3) . . . . ?
C1 C2 C3 C12 178.2(2) . . . . ?
C1 C2 C3 C4 -58.4(3) . . . . ?
C1 C2 C3 C8 59.5(3) . . . . ?
C2 C3 C4 C5 58.9(3) . . . . ?
C12 C3 C4 C5 -178.4(2) . . . . ?
C8 C3 C4 C5 -59.2(3) . . . . ?
C3 C4 C5 C6 -60.1(3) . . . . ?
C3 C4 C5 C9 60.2(3) . . . . ?
C11 C1 C6 C5 178.1(2) . . . . ?
C2 C1 C6 C5 -59.6(3) . . . . ?
C7 C1 C6 C5 58.8(3) . . . . ?
C9 C5 C6 C1 -59.6(3) . . . . ?
C4 C5 C6 C1 60.3(3) . . . . ?
C6 C1 C7 C10 -59.7(4) . . . . ?
C11 C1 C7 C10 179.2(3) . . . . ?
C2 C1 C7 C10 59.0(3) . . . . ?
C2 C3 C8 C10 -59.1(4) . . . . ?
C12 C3 C8 C10 -179.4(3) . . . . ?
C4 C3 C8 C10 59.2(3) . . . . ?
C6 C5 C9 C10 59.8(4) . . . . ?
C4 C5 C9 C10 -59.9(4) . . . . ?
C5 C9 C10 C8 60.1(4) . . . . ?
C5 C9 C10 C7 -59.8(4) . . . . ?
C3 C8 C10 C9 -60.3(4) . . . . ?
C3 C8 C10 C7 59.4(4) . . . . ?
C1 C7 C10 C9 60.5(4) . . . . ?
C1 C7 C10 C8 -59.5(4) . . . . ?
C6 C1 C11 N1 69.4(3) . . . . ?
C2 C1 C11 N1 -52.2(3) . . . . ?
C7 C1 C11 N1 -171.1(3) . . . . ?
C2 C3 C12 N4 54.2(3) . . . . ?
C4 C3 C12 N4 -67.5(3) . . . . ?
C8 C3 C12 N4 173.3(3) . . . . ?
O1 C13 C14 C15 2.8(5) . . . . ?
N1 C13 C14 C15 -177.4(3) . . . . ?
O1 C13 C14 C21 -177.7(3) . . . . ?
N1 C13 C14 C21 2.2(3) . . . . ?
C21 C14 C15 C16 -0.8(4) . . . . ?
C13 C14 C15 C16 178.7(3) . . . . ?
C14 C15 C16 C19 0.3(4) . . . . ?
C14 C15 C16 C17 -179.0(3) . . . . ?
C19 C16 C17 O2 178.8(3) . . . . ?
C15 C16 C17 O2 -1.8(5) . . . . ?
C19 C16 C17 N2 -1.5(3) . . . . ?
C15 C16 C17 N2 177.9(3) . . . . ?
C15 C16 C19 C20 0.4(4) . . . . ?
C17 C16 C19 C20 179.8(3) . . . . ?
C15 C16 C19 C18 179.4(3) . . . . ?
C17 C16 C19 C18 -1.2(3) . . . . ?
O3 C18 C19 C20 2.7(5) . . . . ?
N2 C18 C19 C20 -177.6(3) . . . . ?
O3 C18 C19 C16 -176.2(3) . . . . ?
N2 C18 C19 C16 3.4(3) . . . . ?
C16 C19 C20 C21 -0.4(4) . . . . ?
C18 C19 C20 C21 -179.2(3) . . . . ?
C19 C20 C21 C14 -0.1(4) . . . . ?
C19 C20 C21 C22 -179.6(3) . . . . ?
C15 C14 C21 C20 0.8(5) . . . . ?
C13 C14 C21 C20 -178.8(3) . . . . ?
C15 C14 C21 C22 -179.7(3) . . . . ?
C13 C14 C21 C22 0.7(3) . . . . ?
C20 C21 C22 O4 -4.8(5) . . . . ?
C14 C21 C22 O4 175.7(3) . . . . ?
C20 C21 C22 N1 176.1(3) . . . . ?
C14 C21 C22 N1 -3.4(3) . . . . ?
C33 C23 C24 C25 178.6(2) . . . . ?
C28 C23 C24 C25 -58.0(3) . . . . ?
C29 C23 C24 C25 60.3(3) . . . . ?
C23 C24 C25 C26 58.1(3) . . . . ?
C23 C24 C25 C34 -178.6(2) . . . . ?
C23 C24 C25 C30 -60.1(3) . . . . ?
C34 C25 C26 C27 177.4(3) . . . . ?
C24 C25 C26 C27 -59.3(3) . . . . ?
C30 C25 C26 C27 58.7(3) . . . . ?
C25 C26 C27 C28 60.3(4) . . . . ?
C25 C26 C27 C31 -59.8(4) . . . . ?
C31 C27 C28 C23 60.3(4) . . . . ?
C26 C27 C28 C23 -59.7(4) . . . . ?
C33 C23 C28 C27 -177.3(3) . . . . ?
C24 C23 C28 C27 58.9(3) . . . . ?
C29 C23 C28 C27 -59.1(3) . . . . ?
C33 C23 C29 C32 179.3(3) . . . . ?
C28 C23 C29 C32 59.0(4) . . . . ?
C24 C23 C29 C32 -59.9(4) . . . . ?
C26 C25 C30 C32 -59.3(4) . . . . ?
C34 C25 C30 C32 179.8(3) . . . . ?
C24 C25 C30 C32 59.0(4) . . . . ?
C28 C27 C31 C32 -59.7(4) . . . . ?
C26 C27 C31 C32 60.0(4) . . . . ?
C23 C29 C32 C30 60.1(4) . . . . ?
C23 C29 C32 C31 -59.8(4) . . . . ?
C25 C30 C32 C29 -59.7(4) . . . . ?
C25 C30 C32 C31 60.6(4) . . . . ?
C27 C31 C32 C29 59.7(4) . . . . ?
C27 C31 C32 C30 -60.7(4) . . . . ?
C28 C23 C33 N2 -68.0(3) . . . . ?
C24 C23 C33 N2 54.6(3) . . . . ?
C29 C23 C33 N2 173.2(3) . . . . ?
C26 C25 C34 N3 70.0(3) . . . . ?
C24 C25 C34 N3 -52.0(4) . . . . ?
C30 C25 C34 N3 -170.8(3) . . . . ?
O5 C35 C36 C37 4.4(5) . . . . ?
N3 C35 C36 C37 -174.1(3) . . . . ?
O5 C35 C36 C43 -178.3(3) . . . . ?
N3 C35 C36 C43 3.2(3) . . . . ?
C43 C36 C37 C38 0.1(4) . . . . ?
C35 C36 C37 C38 177.1(3) . . . . ?
C36 C37 C38 C41 -0.2(4) . . . . ?
C36 C37 C38 C39 -177.4(3) . . . . ?
C37 C38 C39 O6 -4.1(5) . . . . ?
C41 C38 C39 O6 178.4(3) . . . . ?
C37 C38 C39 N4 175.1(3) . . . . ?
C41 C38 C39 N4 -2.4(3) . . . . ?
C37 C38 C41 C42 -0.4(5) . . . . ?
C39 C38 C41 C42 177.3(3) . . . . ?
C37 C38 C41 C40 -179.0(3) . . . . ?
C39 C38 C41 C40 -1.3(3) . . . . ?
O7 C40 C41 C42 7.5(5) . . . . ?
N4 C40 C41 C42 -173.9(3) . . . . ?
O7 C40 C41 C38 -174.1(3) . . . . ?
N4 C40 C41 C38 4.5(3) . . . . ?
C38 C41 C42 C43 1.1(4) . . . . ?
C40 C41 C42 C43 179.4(3) . . . . ?
C41 C42 C43 C36 -1.2(4) . . . . ?
C41 C42 C43 C44 -178.7(3) . . . . ?
C37 C36 C43 C42 0.6(4) . . . . ?
C35 C36 C43 C42 -176.9(3) . . . . ?
C37 C36 C43 C44 178.6(3) . . . . ?
C35 C36 C43 C44 1.1(3) . . . . ?
C42 C43 C44 O8 -7.7(6) . . . . ?
C36 C43 C44 O8 174.5(3) . . . . ?
C42 C43 C44 N3 172.8(3) . . . . ?
C36 C43 C44 N3 -5.0(3) . . . . ?
O1 C13 N1 C22 175.3(3) . . . . ?
C14 C13 N1 C22 -4.6(3) . . . . ?
O1 C13 N1 C11 -3.9(5) . . . . ?
C14 C13 N1 C11 176.2(2) . . . . ?
O4 C22 N1 C13 -174.1(3) . . . . ?
C21 C22 N1 C13 5.0(3) . . . . ?
O4 C22 N1 C11 5.1(5) . . . . ?
C21 C22 N1 C11 -175.7(2) . . . . ?
C1 C11 N1 C13 -87.8(3) . . . . ?
C1 C11 N1 C22 93.0(3) . . . . ?
O2 C17 N2 C18 -176.5(3) . . . . ?
C16 C17 N2 C18 3.8(3) . . . . ?
O2 C17 N2 C33 -2.6(5) . . . . ?
C16 C17 N2 C33 177.6(3) . . . . ?
O3 C18 N2 C17 175.1(3) . . . . ?
C19 C18 N2 C17 -4.5(3) . . . . ?
O3 C18 N2 C33 1.1(5) . . . . ?
C19 C18 N2 C33 -178.6(2) . . . . ?
C23 C33 N2 C17 89.8(3) . . . . ?
C23 C33 N2 C18 -97.0(3) . . . . ?
O8 C44 N3 C35 -172.3(3) . . . . ?
C43 C44 N3 C35 7.2(3) . . . . ?
O8 C44 N3 C34 2.8(5) . . . . ?
C43 C44 N3 C34 -177.7(3) . . . . ?
O5 C35 N3 C44 174.9(3) . . . . ?
C36 C35 N3 C44 -6.5(3) . . . . ?
O5 C35 N3 C34 0.1(5) . . . . ?
C36 C35 N3 C34 178.6(3) . . . . ?
C25 C34 N3 C44 95.8(4) . . . . ?
C25 C34 N3 C35 -89.9(4) . . . . ?
O6 C39 N4 C40 -175.3(3) . . . . ?
C38 C39 N4 C40 5.4(3) . . . . ?
O6 C39 N4 C12 -5.4(4) . . . . ?
C38 C39 N4 C12 175.4(2) . . . . ?
O7 C40 N4 C39 172.4(3) . . . . ?
C41 C40 N4 C39 -6.2(3) . . . . ?
O7 C40 N4 C12 2.5(5) . . . . ?
C41 C40 N4 C12 -176.2(3) . . . . ?
C3 C12 N4 C39 89.6(3) . . . . ?
C3 C12 N4 C40 -101.7(3) . . . . ?

_refine_diff_density_max         1.120
_refine_diff_density_min         -1.946
_refine_diff_density_rms         0.253




