# Electronic Supplementary Material (ESI) for ChemComm.
# 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. 
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data_ueno
_database_code_depnum_ccdc_archive 'CCDC 2129375'
loop_
_audit_author_name
_audit_author_address
'Masayoshi Takase'
;Ehime University
Japan
;
_audit_update_record             
;
2021-12-17 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_audit_creation_date             2019-11-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C55 H60 N6 O0.17 S0.83'
_chemical_formula_sum            'C55 H60 N6 O0.17 S0.83'
_chemical_formula_weight         834.42
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.8389(5)
_cell_length_b                   12.9075(5)
_cell_length_c                   15.5565(7)
_cell_angle_alpha                111.925(4)
_cell_angle_beta                 93.798(4)
_cell_angle_gamma                96.861(3)
_cell_volume                     2173.56(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15589
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.3710
_cell_measurement_theta_min      1.6940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             893
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0896
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40881
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.240
_diffrn_reflns_theta_min         1.722
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8125
_reflns_number_total             12970
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         12970
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0649
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0832P)²+0.0940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1716
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C31
 1.23 with sigma of 0.005
3. Rigid bond restraints
 O1, S1, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(S1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(S1) = Uanis(O1)
5. Others
 Sof(O1)=1-FVAR(1)
 Sof(S1)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C32(H32a,H32b), C34(H34a,H34b), C36(H36a,H36b), C38(H38a,H38b), C40(H40a,
 H40b), C46(H46a,H46b), C48(H48a,H48b), C50(H50a,H50b), C52(H52a,H52b),
 C54(H54a,H54b)
6.b Secondary CH2 refined with riding coordinates and stretchable bonds:
 C42(H42a,H42b), C44(H44a,H44b)
6.c Idealised Me refined as rotating group:
 C33(H33a,H33b,H33c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C39(H39a,H39b,
 H39c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c), C45(H45a,H45b,H45c), C47(H47a,
 H47b,H47c), C49(H49a,H49b,H49c), C51(H51a,H51b,H51c), C53(H53a,H53b,H53c),
 C55(H55a,H55b,H55c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.64285(6) -0.05598(6) 0.26895(5) 0.0236(2) Uani 0.829(4) 1 d . U P A 1
O1 O 0.6196(10) -0.0285(4) 0.2621(8) 0.0236(2) Uani 0.171(4) 1 d D U P A 2
C1 C 0.73093(15) 0.32236(14) 0.32305(12) 0.0167(4) Uani 1 1 d . . . . .
C2 C 0.81127(15) 0.41169(14) 0.32332(12) 0.0167(4) Uani 1 1 d . . . . .
C3 C 0.85638(15) 0.50126(14) 0.40477(12) 0.0163(4) Uani 1 1 d . . . . .
C4 C 0.82009(15) 0.50667(14) 0.48771(12) 0.0162(4) Uani 1 1 d . . . . .
C5 C 0.73518(15) 0.42411(14) 0.48909(12) 0.0158(4) Uani 1 1 d . . . . .
C6 C 0.69079(15) 0.32950(14) 0.40826(12) 0.0163(4) Uani 1 1 d . . . . .
C7 C 0.65424(15) 0.12029(14) 0.21530(12) 0.0181(4) Uani 1 1 d . . . . .
C8 C 0.64983(16) 0.06162(15) 0.11911(13) 0.0197(4) Uani 1 1 d . . . . .
C9 C 0.69034(16) 0.13897(15) 0.07949(13) 0.0208(4) Uani 1 1 d . . . . .
C10 C 0.71905(15) 0.24530(15) 0.15107(12) 0.0182(4) Uani 1 1 d . . . . .
C11 C 0.77985(16) 0.35159(15) 0.15482(12) 0.0190(4) Uani 1 1 d . . . . .
C12 C 0.80184(17) 0.40580(16) 0.09444(13) 0.0218(4) Uani 1 1 d . . . . .
C13 C 0.88136(17) 0.50698(15) 0.14449(13) 0.0219(4) Uani 1 1 d . . . . .
C14 C 0.90357(16) 0.51612(15) 0.23639(13) 0.0197(4) Uani 1 1 d . . . . .
C15 C 0.96786(16) 0.59834(15) 0.32283(13) 0.0196(4) Uani 1 1 d . . . . .
C16 C 1.05566(16) 0.68967(15) 0.35150(13) 0.0217(4) Uani 1 1 d . . . . .
C17 C 1.07370(16) 0.73580(15) 0.45159(13) 0.0203(4) Uani 1 1 d . . . . .
C18 C 0.99564(16) 0.67457(14) 0.48433(12) 0.0180(4) Uani 1 1 d . . . . .
C19 C 0.95572(15) 0.68164(14) 0.57345(13) 0.0179(4) Uani 1 1 d . . . . .
C20 C 0.97455(16) 0.75389(15) 0.66720(13) 0.0194(4) Uani 1 1 d . . . . .
C21 C 0.89477(16) 0.71342(15) 0.71697(13) 0.0201(4) Uani 1 1 d . . . . .
C22 C 0.82391(16) 0.61796(15) 0.65320(12) 0.0190(4) Uani 1 1 d . . . . .
C23 C 0.71969(16) 0.54505(14) 0.65112(12) 0.0184(4) Uani 1 1 d . . . . .
C24 C 0.62972(16) 0.55345(15) 0.70450(12) 0.0191(4) Uani 1 1 d . . . . .
C25 C 0.54233(16) 0.45790(15) 0.65787(13) 0.0197(4) Uani 1 1 d . . . . .
C26 C 0.58021(15) 0.39043(15) 0.57529(12) 0.0178(4) Uani 1 1 d . . . . .
C27 C 0.54190(15) 0.28299(15) 0.49799(12) 0.0176(4) Uani 1 1 d . . . . .
C28 C 0.46169(16) 0.18875(15) 0.48596(13) 0.0199(4) Uani 1 1 d . . . . .
C29 C 0.47864(17) 0.09939(15) 0.40352(13) 0.0216(4) Uani 1 1 d . . . . .
C30 C 0.56749(16) 0.13892(14) 0.36433(13) 0.0190(4) Uani 1 1 d . . . . .
C31 C 0.62201(16) 0.07499(15) 0.28411(13) 0.0207(4) Uani 1 1 d D U . . .
C32 C 0.60664(17) -0.06170(15) 0.06353(14) 0.0247(4) Uani 1 1 d . . . . .
H32A H 0.560909 -0.069760 0.005128 0.030 Uiso 1 1 calc R . . . .
H32B H 0.555304 -0.090975 0.099793 0.030 Uiso 1 1 calc R . . . .
C33 C 0.7025(2) -0.13311(18) 0.03899(16) 0.0354(5) Uani 1 1 d . . . . .
H33A H 0.750332 -0.108486 -0.001042 0.053 Uiso 1 1 calc GR . . . .
H33B H 0.669237 -0.212851 0.005883 0.053 Uiso 1 1 calc GR . . . .
H33C H 0.749647 -0.123838 0.096367 0.053 Uiso 1 1 calc GR . . . .
C34 C 0.71138(18) 0.10590(17) -0.02056(13) 0.0255(4) Uani 1 1 d . . . . .
H34A H 0.678477 0.157077 -0.045955 0.031 Uiso 1 1 calc R . . . .
H34B H 0.671288 0.028105 -0.056950 0.031 Uiso 1 1 calc R . . . .
C35 C 0.83855(19) 0.11076(19) -0.03303(14) 0.0337(5) Uani 1 1 d . . . . .
H35A H 0.847535 0.090528 -0.099226 0.050 Uiso 1 1 calc GR . . . .
H35B H 0.870810 0.057400 -0.010951 0.050 Uiso 1 1 calc GR . . . .
H35C H 0.878879 0.187488 0.003104 0.050 Uiso 1 1 calc GR . . . .
C36 C 0.74694(18) 0.37266(17) -0.00400(13) 0.0283(5) Uani 1 1 d . . . . .
H36A H 0.770289 0.300700 -0.044149 0.034 Uiso 1 1 calc R . . . .
H36B H 0.775197 0.431296 -0.027468 0.034 Uiso 1 1 calc R . . . .
C37 C 0.6156(2) 0.3583(2) -0.01159(15) 0.0382(6) Uani 1 1 d . . . . .
H37A H 0.583876 0.329528 -0.077447 0.057 Uiso 1 1 calc GR . . . .
H37B H 0.591738 0.431508 0.021861 0.057 Uiso 1 1 calc GR . . . .
H37C H 0.587451 0.304613 0.015966 0.057 Uiso 1 1 calc GR . . . .
C38 C 0.92674(19) 0.59170(16) 0.10516(14) 0.0273(4) Uani 1 1 d . . . . .
H38A H 0.914736 0.555713 0.036149 0.033 Uiso 1 1 calc R . . . .
H38B H 1.010262 0.614153 0.124707 0.033 Uiso 1 1 calc R . . . .
C39 C 0.8693(2) 0.69711(18) 0.13684(16) 0.0360(5) Uani 1 1 d . . . . .
H39A H 0.788231 0.676767 0.111122 0.054 Uiso 1 1 calc GR . . . .
H39B H 0.907093 0.752536 0.114609 0.054 Uiso 1 1 calc GR . . . .
H39C H 0.875593 0.729840 0.205164 0.054 Uiso 1 1 calc GR . . . .
C40 C 1.12803(17) 0.73497(16) 0.29363(14) 0.0241(4) Uani 1 1 d . . . . .
H40A H 1.166572 0.812450 0.333025 0.029 Uiso 1 1 calc R . . . .
H40B H 1.077649 0.739784 0.242295 0.029 Uiso 1 1 calc R . . . .
C41 C 1.21856(19) 0.66211(18) 0.25215(15) 0.0317(5) Uani 1 1 d . . . . .
H41A H 1.180987 0.585414 0.212556 0.048 Uiso 1 1 calc GR . . . .
H41B H 1.270530 0.659257 0.302661 0.048 Uiso 1 1 calc GR . . . .
H41C H 1.262285 0.694873 0.214595 0.048 Uiso 1 1 calc GR . . . .
C42 C 1.16548(17) 0.83377(15) 0.50627(14) 0.0244(4) Uani 1 1 d . . . . .
H42A H 1.2303(10) 0.82894(17) 0.4727(5) 0.029 Uiso 1 1 calc GR . . . .
H42B H 1.1886(4) 0.82873(17) 0.5642(8) 0.029 Uiso 1 1 calc GR . . . .
C43 C 1.12742(19) 0.94718(17) 0.52528(16) 0.0332(5) Uani 1 1 d . . . . .
H43A H 1.116305 0.958597 0.466635 0.050 Uiso 1 1 calc GR . . . .
H43B H 1.186132 1.007301 0.568822 0.050 Uiso 1 1 calc GR . . . .
H43C H 1.055133 0.949167 0.552703 0.050 Uiso 1 1 calc GR . . . .
C44 C 1.05716(17) 0.86194(15) 0.71458(14) 0.0249(4) Uani 1 1 d . . . . .
H44A H 1.1122(8) 0.86585(16) 0.6756(5) 0.030 Uiso 1 1 calc GR . . . .
H44B H 1.0943(6) 0.86139(15) 0.7689(8) 0.030 Uiso 1 1 calc GR . . . .
C45 C 0.9980(2) 0.96710(17) 0.73912(17) 0.0374(6) Uani 1 1 d . . . . .
H45A H 0.957556 0.967485 0.682217 0.056 Uiso 1 1 calc GR . . . .
H45B H 1.055611 1.035223 0.767558 0.056 Uiso 1 1 calc GR . . . .
H45C H 0.943021 0.965759 0.783242 0.056 Uiso 1 1 calc GR . . . .
C46 C 0.89409(17) 0.76452(16) 0.82125(13) 0.0229(4) Uani 1 1 d . . . . .
H46A H 0.821303 0.794483 0.834974 0.027 Uiso 1 1 calc R . . . .
H46B H 0.957524 0.828923 0.848467 0.027 Uiso 1 1 calc R . . . .
C47 C 0.90682(19) 0.68102(18) 0.86814(14) 0.0286(5) Uani 1 1 d . . . . .
H47A H 0.846757 0.615006 0.839311 0.043 Uiso 1 1 calc GR . . . .
H47B H 0.899691 0.717560 0.934781 0.043 Uiso 1 1 calc GR . . . .
H47C H 0.982183 0.656862 0.860432 0.043 Uiso 1 1 calc GR . . . .
C48 C 0.61569(17) 0.65301(16) 0.79071(13) 0.0234(4) Uani 1 1 d . . . . .
H48A H 0.685213 0.673495 0.836250 0.028 Uiso 1 1 calc R . . . .
H48B H 0.549709 0.631762 0.819884 0.028 Uiso 1 1 calc R . . . .
C49 C 0.59637(19) 0.75432(17) 0.76771(15) 0.0316(5) Uani 1 1 d . . . . .
H49A H 0.527513 0.734226 0.722701 0.047 Uiso 1 1 calc GR . . . .
H49B H 0.662757 0.777040 0.740737 0.047 Uiso 1 1 calc GR . . . .
H49C H 0.586355 0.817153 0.824847 0.047 Uiso 1 1 calc GR . . . .
C50 C 0.43121(17) 0.44470(17) 0.69669(14) 0.0263(4) Uani 1 1 d . . . . .
H50A H 0.373342 0.391333 0.645709 0.032 Uiso 1 1 calc R . . . .
H50B H 0.403844 0.518712 0.720212 0.032 Uiso 1 1 calc R . . . .
C51 C 0.4403(2) 0.4017(2) 0.77544(15) 0.0391(6) Uani 1 1 d . . . . .
H51A H 0.463017 0.326428 0.751839 0.059 Uiso 1 1 calc GR . . . .
H51B H 0.365923 0.397415 0.799040 0.059 Uiso 1 1 calc GR . . . .
H51C H 0.497943 0.453708 0.826064 0.059 Uiso 1 1 calc GR . . . .
C52 C 0.37090(17) 0.17962(16) 0.54613(14) 0.0235(4) Uani 1 1 d . . . . .
H52A H 0.397310 0.232068 0.611358 0.028 Uiso 1 1 calc R . . . .
H52B H 0.358344 0.101811 0.544839 0.028 Uiso 1 1 calc R . . . .
C53 C 0.25736(17) 0.20754(18) 0.51391(16) 0.0309(5) Uani 1 1 d . . . . .
H53A H 0.225287 0.149318 0.452933 0.046 Uiso 1 1 calc GR . . . .
H53B H 0.270896 0.281294 0.508778 0.046 Uiso 1 1 calc GR . . . .
H53C H 0.203295 0.209842 0.559408 0.046 Uiso 1 1 calc GR . . . .
C54 C 0.40398(18) -0.01451(16) 0.36260(14) 0.0259(4) Uani 1 1 d . . . . .
H54A H 0.351247 -0.021307 0.407680 0.031 Uiso 1 1 calc R . . . .
H54B H 0.452586 -0.074506 0.351325 0.031 Uiso 1 1 calc R . . . .
C55 C 0.33411(19) -0.03116(18) 0.27072(15) 0.0331(5) Uani 1 1 d . . . . .
H55A H 0.386238 -0.026424 0.225483 0.050 Uiso 1 1 calc GR . . . .
H55B H 0.285527 0.027857 0.281867 0.050 Uiso 1 1 calc GR . . . .
H55C H 0.285865 -0.105553 0.246010 0.050 Uiso 1 1 calc GR . . . .
N1 N 0.69389(13) 0.23429(12) 0.23455(10) 0.0177(3) Uani 1 1 d . . . . .
N2 N 0.84022(13) 0.42000(12) 0.24104(10) 0.0180(3) Uani 1 1 d . . . . .
N3 N 0.93437(13) 0.58917(12) 0.40396(10) 0.0178(3) Uani 1 1 d . . . . .
N4 N 0.86465(13) 0.59849(12) 0.56789(10) 0.0169(3) Uani 1 1 d . . . . .
N5 N 0.68799(13) 0.44436(12) 0.57220(10) 0.0182(3) Uani 1 1 d . . . . .
N6 N 0.60317(13) 0.25359(12) 0.41997(10) 0.0169(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
S1 C31 1.668(2) . ?
O1 C31 1.246(5) . ?
C1 C2 1.403(2) . ?
C1 C6 1.412(2) . ?
C1 N1 1.418(2) . ?
C2 C3 1.377(2) . ?
C2 N2 1.385(2) . ?
C3 C4 1.366(2) . ?
C3 N3 1.379(2) . ?
C4 C5 1.382(2) . ?
C4 N4 1.378(2) . ?
C5 C6 1.400(2) . ?
C5 N5 1.389(2) . ?
C6 N6 1.409(2) . ?
C7 C8 1.396(2) . ?
C7 C31 1.450(3) . ?
C7 N1 1.401(2) . ?
C8 C9 1.411(3) . ?
C8 C32 1.504(2) . ?
C9 C10 1.392(2) . ?
C9 C34 1.499(3) . ?
C10 C11 1.450(3) . ?
C10 N1 1.405(2) . ?
C11 C12 1.385(3) . ?
C11 N2 1.388(2) . ?
C12 C13 1.431(3) . ?
C12 C36 1.504(3) . ?
C13 C14 1.394(3) . ?
C13 C38 1.504(3) . ?
C14 C15 1.456(3) . ?
C14 N2 1.400(2) . ?
C15 C16 1.386(3) . ?
C15 N3 1.390(2) . ?
C16 C17 1.434(3) . ?
C16 C40 1.504(3) . ?
C17 C18 1.388(3) . ?
C17 C42 1.500(3) . ?
C18 C19 1.469(3) . ?
C18 N3 1.401(2) . ?
C19 C20 1.392(2) . ?
C19 N4 1.401(2) . ?
C20 C21 1.430(3) . ?
C20 C44 1.502(3) . ?
C21 C22 1.391(2) . ?
C21 C46 1.507(3) . ?
C22 C23 1.450(3) . ?
C22 N4 1.386(2) . ?
C23 C24 1.383(3) . ?
C23 N5 1.403(2) . ?
C24 C25 1.430(3) . ?
C24 C48 1.507(2) . ?
C25 C26 1.394(2) . ?
C25 C50 1.501(3) . ?
C26 C27 1.452(2) . ?
C26 N5 1.391(2) . ?
C27 C28 1.395(2) . ?
C27 N6 1.408(2) . ?
C28 C29 1.414(3) . ?
C28 C52 1.494(3) . ?
C29 C30 1.388(3) . ?
C29 C54 1.505(2) . ?
C30 C31 1.456(3) . ?
C30 N6 1.401(2) . ?
C32 C33 1.526(3) . ?
C34 C35 1.527(3) . ?
C36 C37 1.535(3) . ?
C38 C39 1.524(3) . ?
C40 C41 1.526(3) . ?
C42 C43 1.512(3) . ?
C44 C45 1.534(3) . ?
C46 C47 1.526(3) . ?
C48 C49 1.517(3) . ?
C50 C51 1.525(3) . ?
C52 C53 1.533(3) . ?
C54 C55 1.531(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 118.31(15) . . ?
C2 C1 N1 115.69(16) . . ?
C6 C1 N1 125.94(16) . . ?
C3 C2 C1 121.66(16) . . ?
C3 C2 N2 116.48(16) . . ?
N2 C2 C1 121.54(15) . . ?
C2 C3 N3 121.09(16) . . ?
C4 C3 C2 120.02(17) . . ?
C4 C3 N3 118.83(15) . . ?
C3 C4 C5 119.78(16) . . ?
C3 C4 N4 118.87(16) . . ?
N4 C4 C5 121.25(16) . . ?
C4 C5 C6 121.65(16) . . ?
C4 C5 N5 116.95(15) . . ?
N5 C5 C6 121.12(16) . . ?
C5 C6 C1 118.34(16) . . ?
C5 C6 N6 115.30(16) . . ?
N6 C6 C1 126.21(15) . . ?
C8 C7 C31 127.61(16) . . ?
C8 C7 N1 107.28(16) . . ?
N1 C7 C31 125.09(15) . . ?
C7 C8 C9 108.33(16) . . ?
C7 C8 C32 127.64(17) . . ?
C9 C8 C32 124.00(17) . . ?
C8 C9 C34 124.20(16) . . ?
C10 C9 C8 108.01(16) . . ?
C10 C9 C34 127.36(18) . . ?
C9 C10 C11 132.54(17) . . ?
C9 C10 N1 107.58(16) . . ?
N1 C10 C11 119.26(15) . . ?
C12 C11 C10 138.29(17) . . ?
C12 C11 N2 107.01(15) . . ?
N2 C11 C10 114.60(16) . . ?
C11 C12 C13 107.86(16) . . ?
C11 C12 C36 127.67(17) . . ?
C13 C12 C36 124.30(17) . . ?
C12 C13 C38 125.23(17) . . ?
C14 C13 C12 108.30(16) . . ?
C14 C13 C38 126.37(17) . . ?
C13 C14 C15 136.92(17) . . ?
C13 C14 N2 106.01(16) . . ?
N2 C14 C15 117.00(16) . . ?
C16 C15 C14 138.83(17) . . ?
C16 C15 N3 105.94(15) . . ?
N3 C15 C14 115.21(16) . . ?
C15 C16 C17 108.06(16) . . ?
C15 C16 C40 129.29(17) . . ?
C17 C16 C40 122.58(16) . . ?
C16 C17 C42 122.36(17) . . ?
C18 C17 C16 108.91(16) . . ?
C18 C17 C42 128.73(17) . . ?
C17 C18 C19 138.60(16) . . ?
C17 C18 N3 104.99(16) . . ?
N3 C18 C19 116.08(15) . . ?
C20 C19 C18 139.08(16) . . ?
C20 C19 N4 104.81(15) . . ?
N4 C19 C18 115.86(15) . . ?
C19 C20 C21 108.91(15) . . ?
C19 C20 C44 129.36(17) . . ?
C21 C20 C44 121.63(16) . . ?
C20 C21 C46 124.49(16) . . ?
C22 C21 C20 108.16(16) . . ?
C22 C21 C46 127.29(17) . . ?
C21 C22 C23 138.20(17) . . ?
N4 C22 C21 105.70(16) . . ?
N4 C22 C23 115.80(15) . . ?
C24 C23 C22 135.88(16) . . ?
C24 C23 N5 105.99(15) . . ?
N5 C23 C22 117.64(16) . . ?
C23 C24 C25 108.87(15) . . ?
C23 C24 C48 126.73(16) . . ?
C25 C24 C48 123.90(17) . . ?
C24 C25 C50 121.71(16) . . ?
C26 C25 C24 107.70(16) . . ?
C26 C25 C50 130.54(17) . . ?
C25 C26 C27 138.55(17) . . ?
N5 C26 C25 106.51(15) . . ?
N5 C26 C27 114.88(15) . . ?
C28 C27 C26 133.55(17) . . ?
C28 C27 N6 107.26(15) . . ?
N6 C27 C26 118.61(16) . . ?
C27 C28 C29 107.99(16) . . ?
C27 C28 C52 127.95(16) . . ?
C29 C28 C52 124.05(16) . . ?
C28 C29 C54 124.43(17) . . ?
C30 C29 C28 108.30(16) . . ?
C30 C29 C54 127.03(17) . . ?
C29 C30 C31 128.06(16) . . ?
C29 C30 N6 107.62(16) . . ?
N6 C30 C31 124.20(16) . . ?
O1 C31 C7 116.9(5) . . ?
O1 C31 C30 119.6(5) . . ?
C7 C31 S1 119.27(14) . . ?
C7 C31 C30 121.80(16) . . ?
C30 C31 S1 118.88(14) . . ?
C8 C32 C33 113.19(17) . . ?
C9 C34 C35 112.84(17) . . ?
C12 C36 C37 112.65(17) . . ?
C13 C38 C39 112.77(17) . . ?
C16 C40 C41 112.97(16) . . ?
C17 C42 C43 113.13(17) . . ?
C20 C44 C45 112.57(17) . . ?
C21 C46 C47 113.47(15) . . ?
C24 C48 C49 111.37(16) . . ?
C25 C50 C51 113.50(18) . . ?
C28 C52 C53 112.07(16) . . ?
C29 C54 C55 111.24(16) . . ?
C7 N1 C1 127.69(15) . . ?
C7 N1 C10 108.72(14) . . ?
C10 N1 C1 121.95(15) . . ?
C2 N2 C11 122.17(15) . . ?
C2 N2 C14 123.97(15) . . ?
C11 N2 C14 110.76(15) . . ?
C3 N3 C15 123.66(15) . . ?
C3 N3 C18 124.13(15) . . ?
C15 N3 C18 112.03(15) . . ?
C4 N4 C19 124.66(15) . . ?
C4 N4 C22 123.01(15) . . ?
C22 N4 C19 112.32(14) . . ?
C5 N5 C23 122.88(15) . . ?
C5 N5 C26 122.15(15) . . ?
C26 N5 C23 110.92(15) . . ?
C27 N6 C6 122.79(14) . . ?
C30 N6 C6 128.45(15) . . ?
C30 N6 C27 108.59(14) . . ?

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

data_xcalibur
_database_code_depnum_ccdc_archive 'CCDC 2129376'
loop_
_audit_author_name
_audit_author_address
'Masayoshi Takase'
;Ehime University
Japan
;
_audit_update_record             
;
2021-12-17 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C56 H61 Cl3 N6 O'
_chemical_formula_moiety         'C55 H60 N6 O, C H Cl3'
_chemical_formula_weight         940.50
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   10.7101(2)
_cell_length_b                   14.4283(3)
_cell_length_c                   16.8559(5)
_cell_angle_alpha                67.980(2)
_cell_angle_beta                 82.080(2)
_cell_angle_gamma                77.4040(19)
_cell_volume                     2352.07(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26462
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      31.29
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             996.00
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  0.988

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

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            38961
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.548
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             10786
_reflns_number_gt                8827
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1163
_refine_ls_wR_factor_gt          0.1089
_refine_ls_number_restraints     124
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         10786
_refine_ls_number_parameters     635
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0535P)²+1.2721P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

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

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C56 C 0.84419(17) 0.64657(14) 0.13609(12) 0.0277(4) Uani 1 1 d D U . . .
H56 H 0.939830 0.630962 0.136445 0.033 Uiso 1 1 calc R U . A 1
Cl1 Cl 0.7883(3) 0.5334(2) 0.1611(2) 0.0545(11) Uani 0.633(17) 1 d D U P B 1
Cl2 Cl 0.8002(4) 0.7334(3) 0.0329(2) 0.0498(6) Uani 0.633(17) 1 d D U P B 1
Cl3 Cl 0.7821(2) 0.70159(17) 0.21443(13) 0.0286(7) Uani 0.633(17) 1 d D U P B 1
Cl10 Cl 0.7865(3) 0.5318(2) 0.16005(18) 0.0117(9) Uani 0.367(17) 1 d D U P B 2
Cl20 Cl 0.8246(13) 0.7192(8) 0.0289(5) 0.080(2) Uani 0.367(17) 1 d D U P B 2
Cl30 Cl 0.7681(9) 0.7130(7) 0.1996(8) 0.094(2) Uani 0.367(17) 1 d D U P B 2
O4 O 0.14126(11) 0.64017(9) 0.13266(8) 0.0227(3) Uani 1 1 d . . . . .
N1 N 0.61752(12) 0.35887(9) 0.32215(8) 0.0164(3) Uani 1 1 d . . . . .
N2 N 0.45165(12) 0.49694(9) 0.20490(8) 0.0148(3) Uani 1 1 d . . . . .
N3 N 0.39042(12) 0.71318(9) 0.20778(8) 0.0145(3) Uani 1 1 d . . . . .
N4 N 0.51174(12) 0.74667(9) 0.32592(8) 0.0156(3) Uani 1 1 d . . . . .
N5 N 0.65024(12) 0.59197(10) 0.44956(8) 0.0159(3) Uani 1 1 d . . . . .
N6 N 0.70003(12) 0.40204(10) 0.44813(8) 0.0166(3) Uani 1 1 d . . . . .
C1 C 0.56892(14) 0.45369(11) 0.32832(10) 0.0148(3) Uani 1 1 d . . . . .
C2 C 0.48966(14) 0.52835(11) 0.26689(9) 0.0140(3) Uani 1 1 d . . . . .
C3 C 0.46164(13) 0.62806(11) 0.26827(9) 0.0136(3) Uani 1 1 d . . . . .
C4 C 0.51534(14) 0.64771(11) 0.33052(9) 0.0141(3) Uani 1 1 d . . . . .
C5 C 0.59106(14) 0.57144(11) 0.39158(9) 0.0145(3) Uani 1 1 d . . . . .
C6 C 0.61766(14) 0.47495(11) 0.39038(9) 0.0147(3) Uani 1 1 d . . . . .
C7 C 0.71227(15) 0.28773(11) 0.37298(10) 0.0181(3) Uani 1 1 d . . . . .
C8 C 0.77024(15) 0.22465(12) 0.32862(11) 0.0197(3) Uani 1 1 d . . . . .
C9 C 0.70932(15) 0.25749(12) 0.24969(11) 0.0193(3) Uani 1 1 d . . . . .
C10 C 0.61349(15) 0.34026(11) 0.24725(10) 0.0174(3) Uani 1 1 d . . . . .
C11 C 0.50908(14) 0.40436(11) 0.19448(10) 0.0159(3) Uani 1 1 d . . . . .
C12 C 0.43475(15) 0.38692(11) 0.14209(10) 0.0170(3) Uani 1 1 d . . . . .
C13 C 0.32871(15) 0.46749(11) 0.12163(10) 0.0174(3) Uani 1 1 d . . . . .
C14 C 0.33903(14) 0.53389(11) 0.16141(10) 0.0157(3) Uani 1 1 d . . . . .
C15 C 0.25208(14) 0.62925(11) 0.15309(10) 0.0163(3) Uani 1 1 d . . . . .
C16 C 0.29323(14) 0.71622(11) 0.15923(9) 0.0154(3) Uani 1 1 d . . . . .
C17 C 0.24067(15) 0.81733(12) 0.11727(10) 0.0173(3) Uani 1 1 d . . . . .
C18 C 0.30333(15) 0.87824(11) 0.14186(10) 0.0169(3) Uani 1 1 d . . . . .
C19 C 0.39436(14) 0.81308(11) 0.19899(10) 0.0159(3) Uani 1 1 d . . . . .
C20 C 0.47598(14) 0.82924(11) 0.25218(10) 0.0159(3) Uani 1 1 d . . . . .
C21 C 0.53425(15) 0.90690(12) 0.25030(10) 0.0183(3) Uani 1 1 d . . . . .
C22 C 0.60657(15) 0.87020(12) 0.32462(10) 0.0189(3) Uani 1 1 d . . . . .
C23 C 0.59183(14) 0.77097(12) 0.37180(10) 0.0173(3) Uani 1 1 d . . . . .
C24 C 0.64689(15) 0.68968(12) 0.44731(10) 0.0175(3) Uani 1 1 d . . . . .
C25 C 0.70981(15) 0.67857(12) 0.51769(10) 0.0199(3) Uani 1 1 d . . . . .
C26 C 0.75602(15) 0.57216(12) 0.56102(10) 0.0186(3) Uani 1 1 d . . . . .
C27 C 0.71903(14) 0.51828(12) 0.51749(10) 0.0164(3) Uani 1 1 d . . . . .
C28 C 0.74137(14) 0.41323(12) 0.51896(10) 0.0169(3) Uani 1 1 d . . . . .
C29 C 0.80137(14) 0.31623(12) 0.56801(10) 0.0184(3) Uani 1 1 d . . . . .
C30 C 0.79654(15) 0.24789(12) 0.52504(10) 0.0199(3) Uani 1 1 d . . . . .
C31 C 0.73689(15) 0.30327(12) 0.44960(10) 0.0184(3) Uani 1 1 d . . . . .
C32 C 0.88688(16) 0.14208(13) 0.35360(12) 0.0257(4) Uani 1 1 d . . . . .
H32A H 0.903638 0.105400 0.312884 0.031 Uiso 1 1 calc R U . . .
H32B H 0.869532 0.092715 0.411466 0.031 Uiso 1 1 calc R U . . .
C33 C 1.00567(17) 0.18420(16) 0.35380(14) 0.0348(4) Uani 1 1 d . . . . .
H33A H 0.989372 0.220928 0.393775 0.042 Uiso 1 1 calc R U . . .
H33B H 1.025589 0.230711 0.295976 0.042 Uiso 1 1 calc R U . . .
H33C H 1.078350 0.128019 0.371766 0.042 Uiso 1 1 calc R U . . .
C34 C 0.75959(16) 0.21614(13) 0.17908(12) 0.0252(4) Uani 1 1 d . . . . .
H34A H 0.692948 0.236905 0.137392 0.030 Uiso 1 1 calc R U . . .
H34B H 0.777387 0.140939 0.203918 0.030 Uiso 1 1 calc R U . . .
C35 C 0.88119(19) 0.25358(16) 0.13244(13) 0.0334(4) Uani 1 1 d . . . . .
H35A H 0.947742 0.232708 0.173350 0.040 Uiso 1 1 calc R U . . .
H35B H 0.863377 0.327899 0.106109 0.040 Uiso 1 1 calc R U . . .
H35C H 0.910830 0.224265 0.087787 0.040 Uiso 1 1 calc R U . . .
C36 C 0.45110(15) 0.29661(12) 0.11507(11) 0.0205(3) Uani 1 1 d . . . . .
H36A H 0.365825 0.279480 0.117064 0.025 Uiso 1 1 calc R U . . .
H36B H 0.503235 0.237650 0.156637 0.025 Uiso 1 1 calc R U . . .
C37 C 0.51557(19) 0.31397(15) 0.02466(12) 0.0309(4) Uani 1 1 d . . . . .
H37A H 0.601307 0.328717 0.022582 0.037 Uiso 1 1 calc R U . . .
H37B H 0.463857 0.371512 -0.017106 0.037 Uiso 1 1 calc R U . . .
H37C H 0.522676 0.252739 0.010852 0.037 Uiso 1 1 calc R U . . .
C38 C 0.22316(17) 0.47528(13) 0.06825(11) 0.0246(4) Uani 1 1 d . . . . .
H38A H 0.258819 0.444908 0.024267 0.030 Uiso 1 1 calc R U . . .
H38B H 0.187566 0.547877 0.038207 0.030 Uiso 1 1 calc R U . . .
C39 C 0.11594(18) 0.42156(15) 0.12213(15) 0.0368(5) Uani 1 1 d . . . . .
H39A H 0.081862 0.450196 0.166723 0.044 Uiso 1 1 calc R U . . .
H39B H 0.149597 0.348802 0.148991 0.044 Uiso 1 1 calc R U . . .
H39C H 0.047324 0.431084 0.085371 0.044 Uiso 1 1 calc R U . . .
C40 C 0.13591(16) 0.85670(12) 0.05597(11) 0.0223(3) Uani 1 1 d . . . . .
H40A H 0.134177 0.805338 0.030522 0.027 Uiso 1 1 calc R U . . .
H40B H 0.154693 0.919091 0.008882 0.027 Uiso 1 1 calc R U . . .
C41 C 0.00483(16) 0.88061(14) 0.09922(13) 0.0297(4) Uani 1 1 d . . . . .
H41A H -0.061199 0.900486 0.058096 0.036 Uiso 1 1 calc R U . . .
H41B H 0.003211 0.936503 0.119219 0.036 Uiso 1 1 calc R U . . .
H41C H -0.011919 0.820242 0.148188 0.036 Uiso 1 1 calc R U . . .
C42 C 0.26391(16) 0.99168(12) 0.11550(10) 0.0205(3) Uani 1 1 d . . . . .
H42A H 0.204143 1.016256 0.069023 0.025 Uiso 1 1 calc R U . . .
H42B H 0.340717 1.023368 0.092284 0.025 Uiso 1 1 calc R U . . .
C43 C 0.19899(18) 1.02617(13) 0.18938(12) 0.0277(4) Uani 1 1 d . . . . .
H43A H 0.177793 1.100568 0.168722 0.033 Uiso 1 1 calc R U . . .
H43B H 0.257405 1.001924 0.235811 0.033 Uiso 1 1 calc R U . . .
H43C H 0.120330 0.998017 0.210782 0.033 Uiso 1 1 calc R U . . .
C44 C 0.53925(17) 1.00789(12) 0.17918(11) 0.0241(4) Uani 1 1 d . . . . .
H44A H 0.587323 1.047338 0.197109 0.029 Uiso 1 1 calc R U . . .
H44B H 0.450983 1.046771 0.168664 0.029 Uiso 1 1 calc R U . . .
C45 C 0.60355(19) 0.99522(15) 0.09590(13) 0.0365(5) Uani 1 1 d . . . . .
H45A H 0.557451 0.954776 0.078694 0.044 Uiso 1 1 calc R U . . .
H45B H 0.692697 0.960519 0.105112 0.044 Uiso 1 1 calc R U . . .
H45C H 0.601624 1.062264 0.050640 0.044 Uiso 1 1 calc R U . . .
C46 C 0.68651(16) 0.93314(12) 0.34225(11) 0.0234(3) Uani 1 1 d . . . . .
H46A H 0.729534 0.972141 0.287823 0.028 Uiso 1 1 calc R U . . .
H46B H 0.753742 0.887579 0.381092 0.028 Uiso 1 1 calc R U . . .
C47 C 0.60555(19) 1.00698(15) 0.38317(14) 0.0340(4) Uani 1 1 d . . . . .
H47A H 0.565789 0.968470 0.438292 0.041 Uiso 1 1 calc R U . . .
H47B H 0.538587 1.051978 0.345020 0.041 Uiso 1 1 calc R U . . .
H47C H 0.660483 1.047726 0.392383 0.041 Uiso 1 1 calc R U . . .
C48 C 0.72706(17) 0.75845(13) 0.55084(11) 0.0249(4) Uani 1 1 d . . . . .
H48A H 0.815742 0.742692 0.568898 0.030 Uiso 1 1 calc R U . . .
H48B H 0.716533 0.825158 0.503323 0.030 Uiso 1 1 calc R U . . .
C49 C 0.6358(2) 0.76709(17) 0.62463(14) 0.0388(5) Uani 1 1 d . . . . .
H49A H 0.645848 0.701669 0.672390 0.047 Uiso 1 1 calc R U . . .
H49B H 0.547633 0.785838 0.606765 0.047 Uiso 1 1 calc R U . . .
H49C H 0.654074 0.819407 0.642978 0.047 Uiso 1 1 calc R U . . .
C50 C 0.83623(17) 0.53574(13) 0.63698(11) 0.0249(4) Uani 1 1 d . . . . .
H50A H 0.820993 0.467269 0.674996 0.030 Uiso 1 1 calc R U . . .
H50B H 0.808127 0.581910 0.669671 0.030 Uiso 1 1 calc R U . . .
C51 C 0.97960(18) 0.53060(17) 0.61317(13) 0.0373(5) Uani 1 1 d . . . . .
H51A H 0.996130 0.598614 0.577441 0.045 Uiso 1 1 calc R U . . .
H51B H 1.008602 0.484459 0.581294 0.045 Uiso 1 1 calc R U . . .
H51C H 1.026168 0.505408 0.665493 0.045 Uiso 1 1 calc R U . . .
C52 C 0.86813(16) 0.27932(13) 0.64987(10) 0.0241(4) Uani 1 1 d . . . . .
H52A H 0.836257 0.218111 0.690610 0.029 Uiso 1 1 calc R U . . .
H52B H 0.846425 0.332471 0.675855 0.029 Uiso 1 1 calc R U . . .
C53 C 1.01312(17) 0.25353(16) 0.63652(12) 0.0329(4) Uani 1 1 d . . . . .
H53A H 1.046099 0.315110 0.599942 0.040 Uiso 1 1 calc R U . . .
H53B H 1.035195 0.202694 0.608917 0.040 Uiso 1 1 calc R U . . .
H53C H 1.051459 0.226178 0.692113 0.040 Uiso 1 1 calc R U . . .
C54 C 0.83570(16) 0.13385(12) 0.56212(11) 0.0242(4) Uani 1 1 d . . . . .
H54A H 0.866903 0.113807 0.619900 0.029 Uiso 1 1 calc R U . . .
H54B H 0.906920 0.111591 0.525409 0.029 Uiso 1 1 calc R U . . .
C55 C 0.72342(17) 0.08077(13) 0.56854(12) 0.0272(4) Uani 1 1 d . . . . .
H55A H 0.692106 0.100809 0.511439 0.033 Uiso 1 1 calc R U . . .
H55B H 0.654135 0.100628 0.606701 0.033 Uiso 1 1 calc R U . . .
H55C H 0.752208 0.006933 0.591579 0.033 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2'

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

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C56 Cl30 1.708(6) . ?
C56 Cl20 1.731(7) . ?
C56 Cl1 1.745(3) . ?
C56 Cl3 1.769(3) . ?
C56 Cl2 1.774(4) . ?
C56 Cl10 1.778(3) . ?
C56 H56 1.0000 . ?
O4 C15 1.2420(19) . ?
N1 C1 1.3910(19) . ?
N1 C10 1.394(2) . ?
N1 C7 1.3941(19) . ?
N2 C14 1.3953(19) . ?
N2 C11 1.4075(19) . ?
N2 C2 1.4197(19) . ?
N3 C16 1.3939(19) . ?
N3 C19 1.4021(19) . ?
N3 C3 1.4131(18) . ?
N4 C20 1.3902(19) . ?
N4 C4 1.3929(19) . ?
N4 C23 1.405(2) . ?
N5 C5 1.3836(19) . ?
N5 C24 1.3887(19) . ?
N5 C27 1.4007(19) . ?
N6 C6 1.3772(19) . ?
N6 C31 1.385(2) . ?
N6 C28 1.403(2) . ?
C1 C6 1.386(2) . ?
C1 C2 1.400(2) . ?
C2 C3 1.413(2) . ?
C3 C4 1.404(2) . ?
C4 C5 1.385(2) . ?
C5 C6 1.366(2) . ?
C7 C8 1.381(2) . ?
C7 C31 1.458(2) . ?
C8 C9 1.432(2) . ?
C8 C32 1.509(2) . ?
C9 C10 1.386(2) . ?
C9 C34 1.509(2) . ?
C10 C11 1.450(2) . ?
C11 C12 1.387(2) . ?
C12 C13 1.411(2) . ?
C12 C36 1.503(2) . ?
C13 C14 1.389(2) . ?
C13 C38 1.500(2) . ?
C14 C15 1.453(2) . ?
C15 C16 1.460(2) . ?
C16 C17 1.387(2) . ?
C17 C18 1.415(2) . ?
C17 C40 1.500(2) . ?
C18 C19 1.394(2) . ?
C18 C42 1.503(2) . ?
C19 C20 1.444(2) . ?
C20 C21 1.385(2) . ?
C21 C22 1.429(2) . ?
C21 C44 1.507(2) . ?
C22 C23 1.385(2) . ?
C22 C46 1.503(2) . ?
C23 C24 1.459(2) . ?
C24 C25 1.385(2) . ?
C25 C26 1.436(2) . ?
C25 C48 1.510(2) . ?
C26 C27 1.394(2) . ?
C26 C50 1.502(2) . ?
C27 C28 1.473(2) . ?
C28 C29 1.393(2) . ?
C29 C30 1.438(2) . ?
C29 C52 1.501(2) . ?
C30 C31 1.379(2) . ?
C30 C54 1.508(2) . ?
C32 C33 1.526(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.521(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.537(2) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.522(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.522(2) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.535(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.533(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.532(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.499(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.525(3) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.522(2) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.532(2) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 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
Cl30 C56 Cl20 110.7(4) . . ?
Cl1 C56 Cl3 109.67(16) . . ?
Cl1 C56 Cl2 111.1(2) . . ?
Cl3 C56 Cl2 110.03(18) . . ?
Cl30 C56 Cl10 112.1(2) . . ?
Cl20 C56 Cl10 108.5(3) . . ?
Cl1 C56 H56 108.7 . . ?
Cl3 C56 H56 108.7 . . ?
Cl2 C56 H56 108.7 . . ?
C1 N1 C10 121.99(13) . . ?
C1 N1 C7 123.54(13) . . ?
C10 N1 C7 110.54(13) . . ?
C14 N2 C11 107.90(12) . . ?
C14 N2 C2 127.93(13) . . ?
C11 N2 C2 122.40(12) . . ?
C16 N3 C19 108.32(12) . . ?
C16 N3 C3 128.83(12) . . ?
C19 N3 C3 122.03(12) . . ?
C20 N4 C4 120.88(13) . . ?
C20 N4 C23 110.50(12) . . ?
C4 N4 C23 122.88(13) . . ?
C5 N5 C24 123.29(13) . . ?
C5 N5 C27 124.88(13) . . ?
C24 N5 C27 111.82(12) . . ?
C6 N6 C31 122.79(13) . . ?
C6 N6 C28 124.88(13) . . ?
C31 N6 C28 111.73(13) . . ?
C6 C1 N1 116.45(13) . . ?
C6 C1 C2 121.83(14) . . ?
N1 C1 C2 121.07(13) . . ?
C1 C2 C3 118.19(13) . . ?
C1 C2 N2 115.70(13) . . ?
C3 C2 N2 125.97(13) . . ?
C4 C3 C2 118.56(13) . . ?
C4 C3 N3 116.00(13) . . ?
C2 C3 N3 125.27(13) . . ?
C5 C4 N4 116.19(13) . . ?
C5 C4 C3 121.68(13) . . ?
N4 C4 C3 121.41(13) . . ?
C6 C5 N5 118.48(13) . . ?
C6 C5 C4 119.67(14) . . ?
N5 C5 C4 121.60(13) . . ?
C5 C6 N6 118.53(14) . . ?
C5 C6 C1 120.03(14) . . ?
N6 C6 C1 121.30(14) . . ?
C8 C7 N1 106.51(14) . . ?
C8 C7 C31 135.99(14) . . ?
N1 C7 C31 116.96(13) . . ?
C7 C8 C9 108.46(14) . . ?
C7 C8 C32 126.28(15) . . ?
C9 C8 C32 124.97(15) . . ?
C10 C9 C8 107.68(14) . . ?
C10 C9 C34 128.44(15) . . ?
C8 C9 C34 123.22(14) . . ?
C9 C10 N1 106.79(13) . . ?
C9 C10 C11 138.71(15) . . ?
N1 C10 C11 114.28(13) . . ?
C12 C11 N2 107.98(13) . . ?
C12 C11 C10 132.34(14) . . ?
N2 C11 C10 118.73(13) . . ?
C11 C12 C13 107.85(13) . . ?
C11 C12 C36 128.93(14) . . ?
C13 C12 C36 123.04(14) . . ?
C14 C13 C12 108.01(14) . . ?
C14 C13 C38 127.48(14) . . ?
C12 C13 C38 124.48(14) . . ?
C13 C14 N2 108.20(13) . . ?
C13 C14 C15 125.34(14) . . ?
N2 C14 C15 126.30(13) . . ?
O4 C15 C14 118.57(14) . . ?
O4 C15 C16 118.48(14) . . ?
C14 C15 C16 122.65(13) . . ?
C17 C16 N3 108.02(13) . . ?
C17 C16 C15 125.25(14) . . ?
N3 C16 C15 126.73(13) . . ?
C16 C17 C18 108.20(13) . . ?
C16 C17 C40 126.53(14) . . ?
C18 C17 C40 125.27(14) . . ?
C19 C18 C17 107.48(13) . . ?
C19 C18 C42 128.78(14) . . ?
C17 C18 C42 123.46(14) . . ?
C18 C19 N3 107.90(13) . . ?
C18 C19 C20 132.97(14) . . ?
N3 C19 C20 118.83(13) . . ?
C21 C20 N4 106.98(13) . . ?
C21 C20 C19 137.35(14) . . ?
N4 C20 C19 115.65(13) . . ?
C20 C21 C22 107.79(14) . . ?
C20 C21 C44 128.22(15) . . ?
C22 C21 C44 123.51(14) . . ?
C23 C22 C21 108.75(14) . . ?
C23 C22 C46 128.64(15) . . ?
C21 C22 C46 122.59(14) . . ?
C22 C23 N4 105.99(13) . . ?
C22 C23 C24 136.21(15) . . ?
N4 C23 C24 117.45(13) . . ?
C25 C24 N5 106.10(13) . . ?
C25 C24 C23 138.73(15) . . ?
N5 C24 C23 114.88(13) . . ?
C24 C25 C26 108.32(14) . . ?
C24 C25 C48 129.39(15) . . ?
C26 C25 C48 122.24(14) . . ?
C27 C26 C25 108.34(14) . . ?
C27 C26 C50 130.43(15) . . ?
C25 C26 C50 121.15(14) . . ?
C26 C27 N5 105.35(13) . . ?
C26 C27 C28 138.59(14) . . ?
N5 C27 C28 115.76(13) . . ?
C29 C28 N6 105.21(13) . . ?
C29 C28 C27 139.31(14) . . ?
N6 C28 C27 115.29(13) . . ?
C28 C29 C30 108.32(14) . . ?
C28 C29 C52 130.82(15) . . ?
C30 C29 C52 120.81(14) . . ?
C31 C30 C29 108.23(14) . . ?
C31 C30 C54 126.31(15) . . ?
C29 C30 C54 125.07(14) . . ?
C30 C31 N6 106.41(14) . . ?
C30 C31 C7 138.10(15) . . ?
N6 C31 C7 115.31(13) . . ?
C8 C32 C33 112.21(14) . . ?
C8 C32 H32A 109.2 . . ?
C33 C32 H32A 109.2 . . ?
C8 C32 H32B 109.2 . . ?
C33 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C9 C34 C35 112.32(14) . . ?
C9 C34 H34A 109.1 . . ?
C35 C34 H34A 109.1 . . ?
C9 C34 H34B 109.1 . . ?
C35 C34 H34B 109.1 . . ?
H34A C34 H34B 107.9 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C12 C36 C37 113.57(14) . . ?
C12 C36 H36A 108.9 . . ?
C37 C36 H36A 108.9 . . ?
C12 C36 H36B 108.9 . . ?
C37 C36 H36B 108.9 . . ?
H36A C36 H36B 107.7 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C13 C38 C39 112.05(15) . . ?
C13 C38 H38A 109.2 . . ?
C39 C38 H38A 109.2 . . ?
C13 C38 H38B 109.2 . . ?
C39 C38 H38B 109.2 . . ?
H38A C38 H38B 107.9 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C17 C40 C41 112.36(14) . . ?
C17 C40 H40A 109.1 . . ?
C41 C40 H40A 109.1 . . ?
C17 C40 H40B 109.1 . . ?
C41 C40 H40B 109.1 . . ?
H40A C40 H40B 107.9 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C18 C42 C43 113.28(13) . . ?
C18 C42 H42A 108.9 . . ?
C43 C42 H42A 108.9 . . ?
C18 C42 H42B 108.9 . . ?
C43 C42 H42B 108.9 . . ?
H42A C42 H42B 107.7 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C21 C44 C45 111.90(14) . . ?
C21 C44 H44A 109.2 . . ?
C45 C44 H44A 109.2 . . ?
C21 C44 H44B 109.2 . . ?
C45 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C22 C46 C47 111.86(14) . . ?
C22 C46 H46A 109.2 . . ?
C47 C46 H46A 109.2 . . ?
C22 C46 H46B 109.2 . . ?
C47 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 C25 114.47(15) . . ?
C49 C48 H48A 108.6 . . ?
C25 C48 H48A 108.6 . . ?
C49 C48 H48B 108.6 . . ?
C25 C48 H48B 108.6 . . ?
H48A C48 H48B 107.6 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C26 C50 C51 113.72(14) . . ?
C26 C50 H50A 108.8 . . ?
C51 C50 H50A 108.8 . . ?
C26 C50 H50B 108.8 . . ?
C51 C50 H50B 108.8 . . ?
H50A C50 H50B 107.7 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C29 C52 C53 112.80(14) . . ?
C29 C52 H52A 109.0 . . ?
C53 C52 H52A 109.0 . . ?
C29 C52 H52B 109.0 . . ?
C53 C52 H52B 109.0 . . ?
H52A C52 H52B 107.8 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C30 C54 C55 111.35(14) . . ?
C30 C54 H54A 109.4 . . ?
C55 C54 H54A 109.4 . . ?
C30 C54 H54B 109.4 . . ?
C55 C54 H54B 109.4 . . ?
H54A C54 H54B 108.0 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 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
C10 N1 C1 C6 -157.02(14) . . . . ?
C7 N1 C1 C6 -1.5(2) . . . . ?
C10 N1 C1 C2 13.9(2) . . . . ?
C7 N1 C1 C2 169.45(14) . . . . ?
C6 C1 C2 C3 1.2(2) . . . . ?
N1 C1 C2 C3 -169.23(13) . . . . ?
C6 C1 C2 N2 177.19(13) . . . . ?
N1 C1 C2 N2 6.8(2) . . . . ?
C14 N2 C2 C1 150.59(14) . . . . ?
C11 N2 C2 C1 -12.3(2) . . . . ?
C14 N2 C2 C3 -33.8(2) . . . . ?
C11 N2 C2 C3 163.31(14) . . . . ?
C1 C2 C3 C4 0.5(2) . . . . ?
N2 C2 C3 C4 -175.01(13) . . . . ?
C1 C2 C3 N3 175.72(13) . . . . ?
N2 C2 C3 N3 0.2(2) . . . . ?
C16 N3 C3 C4 -155.84(14) . . . . ?
C19 N3 C3 C4 12.6(2) . . . . ?
C16 N3 C3 C2 28.9(2) . . . . ?
C19 N3 C3 C2 -162.71(14) . . . . ?
C20 N4 C4 C5 158.76(14) . . . . ?
C23 N4 C4 C5 8.0(2) . . . . ?
C20 N4 C4 C3 -11.7(2) . . . . ?
C23 N4 C4 C3 -162.41(14) . . . . ?
C2 C3 C4 C5 -2.0(2) . . . . ?
N3 C3 C4 C5 -177.67(13) . . . . ?
C2 C3 C4 N4 167.88(13) . . . . ?
N3 C3 C4 N4 -7.7(2) . . . . ?
C24 N5 C5 C6 169.25(14) . . . . ?
C27 N5 C5 C6 -11.4(2) . . . . ?
C24 N5 C5 C4 -5.0(2) . . . . ?
C27 N5 C5 C4 174.31(14) . . . . ?
N4 C4 C5 C6 -168.62(13) . . . . ?
C3 C4 C5 C6 1.8(2) . . . . ?
N4 C4 C5 N5 5.6(2) . . . . ?
C3 C4 C5 N5 176.01(13) . . . . ?
N5 C5 C6 N6 1.3(2) . . . . ?
C4 C5 C6 N6 175.73(13) . . . . ?
N5 C5 C6 C1 -174.42(13) . . . . ?
C4 C5 C6 C1 0.0(2) . . . . ?
C31 N6 C6 C5 -177.31(14) . . . . ?
C28 N6 C6 C5 12.4(2) . . . . ?
C31 N6 C6 C1 -1.6(2) . . . . ?
C28 N6 C6 C1 -171.92(14) . . . . ?
N1 C1 C6 C5 169.36(13) . . . . ?
C2 C1 C6 C5 -1.5(2) . . . . ?
N1 C1 C6 N6 -6.3(2) . . . . ?
C2 C1 C6 N6 -177.12(14) . . . . ?
C1 N1 C7 C8 -156.88(14) . . . . ?
C10 N1 C7 C8 1.11(17) . . . . ?
C1 N1 C7 C31 16.0(2) . . . . ?
C10 N1 C7 C31 174.03(13) . . . . ?
N1 C7 C8 C9 -0.35(18) . . . . ?
C31 C7 C8 C9 -171.25(17) . . . . ?
N1 C7 C8 C32 173.67(15) . . . . ?
C31 C7 C8 C32 2.8(3) . . . . ?
C7 C8 C9 C10 -0.52(18) . . . . ?
C32 C8 C9 C10 -174.64(15) . . . . ?
C7 C8 C9 C34 170.89(15) . . . . ?
C32 C8 C9 C34 -3.2(2) . . . . ?
C8 C9 C10 N1 1.17(17) . . . . ?
C34 C9 C10 N1 -169.65(15) . . . . ?
C8 C9 C10 C11 -172.66(18) . . . . ?
C34 C9 C10 C11 16.5(3) . . . . ?
C1 N1 C10 C9 156.96(14) . . . . ?
C7 N1 C10 C9 -1.44(17) . . . . ?
C1 N1 C10 C11 -27.5(2) . . . . ?
C7 N1 C10 C11 174.10(13) . . . . ?
C14 N2 C11 C12 2.36(16) . . . . ?
C2 N2 C11 C12 168.27(13) . . . . ?
C14 N2 C11 C10 -167.84(13) . . . . ?
C2 N2 C11 C10 -1.9(2) . . . . ?
C9 C10 C11 C12 27.3(3) . . . . ?
N1 C10 C11 C12 -146.17(16) . . . . ?
C9 C10 C11 N2 -165.30(18) . . . . ?
N1 C10 C11 N2 21.2(2) . . . . ?
N2 C11 C12 C13 -1.57(17) . . . . ?
C10 C11 C12 C13 166.78(16) . . . . ?
N2 C11 C12 C36 -176.75(15) . . . . ?
C10 C11 C12 C36 -8.4(3) . . . . ?
C11 C12 C13 C14 0.20(17) . . . . ?
C36 C12 C13 C14 175.72(14) . . . . ?
C11 C12 C13 C38 -178.05(15) . . . . ?
C36 C12 C13 C38 -2.5(2) . . . . ?
C12 C13 C14 N2 1.27(17) . . . . ?
C38 C13 C14 N2 179.45(15) . . . . ?
C12 C13 C14 C15 176.90(14) . . . . ?
C38 C13 C14 C15 -4.9(3) . . . . ?
C11 N2 C14 C13 -2.24(16) . . . . ?
C2 N2 C14 C13 -167.14(14) . . . . ?
C11 N2 C14 C15 -177.82(14) . . . . ?
C2 N2 C14 C15 17.3(2) . . . . ?
C13 C14 C15 O4 23.7(2) . . . . ?
N2 C14 C15 O4 -161.48(15) . . . . ?
C13 C14 C15 C16 -149.96(15) . . . . ?
N2 C14 C15 C16 24.9(2) . . . . ?
C19 N3 C16 C17 2.69(16) . . . . ?
C3 N3 C16 C17 172.36(14) . . . . ?
C19 N3 C16 C15 -177.02(14) . . . . ?
C3 N3 C16 C15 -7.3(2) . . . . ?
O4 C15 C16 C17 -23.8(2) . . . . ?
C14 C15 C16 C17 149.80(15) . . . . ?
O4 C15 C16 N3 155.82(15) . . . . ?
C14 C15 C16 N3 -30.5(2) . . . . ?
N3 C16 C17 C18 -1.70(17) . . . . ?
C15 C16 C17 C18 178.01(14) . . . . ?
N3 C16 C17 C40 178.08(15) . . . . ?
C15 C16 C17 C40 -2.2(3) . . . . ?
C16 C17 C18 C19 0.07(18) . . . . ?
C40 C17 C18 C19 -179.72(15) . . . . ?
C16 C17 C18 C42 -174.28(14) . . . . ?
C40 C17 C18 C42 5.9(2) . . . . ?
C17 C18 C19 N3 1.58(17) . . . . ?
C42 C18 C19 N3 175.53(15) . . . . ?
C17 C18 C19 C20 -171.90(16) . . . . ?
C42 C18 C19 C20 2.0(3) . . . . ?
C16 N3 C19 C18 -2.64(16) . . . . ?
C3 N3 C19 C18 -173.17(13) . . . . ?
C16 N3 C19 C20 171.92(13) . . . . ?
C3 N3 C19 C20 1.4(2) . . . . ?
C4 N4 C20 C21 -153.55(13) . . . . ?
C23 N4 C20 C21 0.45(17) . . . . ?
C4 N4 C20 C19 25.4(2) . . . . ?
C23 N4 C20 C19 179.35(13) . . . . ?
C18 C19 C20 C21 -28.7(3) . . . . ?
N3 C19 C20 C21 158.34(18) . . . . ?
C18 C19 C20 N4 152.80(16) . . . . ?
N3 C19 C20 N4 -20.1(2) . . . . ?
N4 C20 C21 C22 -0.05(17) . . . . ?
C19 C20 C21 C22 -178.59(17) . . . . ?
N4 C20 C21 C44 172.14(15) . . . . ?
C19 C20 C21 C44 -6.4(3) . . . . ?
C20 C21 C22 C23 -0.36(18) . . . . ?
C44 C21 C22 C23 -173.00(15) . . . . ?
C20 C21 C22 C46 177.85(14) . . . . ?
C44 C21 C22 C46 5.2(2) . . . . ?
C21 C22 C23 N4 0.62(17) . . . . ?
C46 C22 C23 N4 -177.46(15) . . . . ?
C21 C22 C23 C24 173.26(17) . . . . ?
C46 C22 C23 C24 -4.8(3) . . . . ?
C20 N4 C23 C22 -0.67(17) . . . . ?
C4 N4 C23 C22 152.71(14) . . . . ?
C20 N4 C23 C24 -174.93(13) . . . . ?
C4 N4 C23 C24 -21.6(2) . . . . ?
C5 N5 C24 C25 176.65(14) . . . . ?
C27 N5 C24 C25 -2.76(17) . . . . ?
C5 N5 C24 C23 -8.4(2) . . . . ?
C27 N5 C24 C23 172.17(13) . . . . ?
C22 C23 C24 C25 21.3(3) . . . . ?
N4 C23 C24 C25 -166.66(18) . . . . ?
C22 C23 C24 N5 -151.28(18) . . . . ?
N4 C23 C24 N5 20.7(2) . . . . ?
N5 C24 C25 C26 2.23(17) . . . . ?
C23 C24 C25 C26 -170.79(18) . . . . ?
N5 C24 C25 C48 -175.18(15) . . . . ?
C23 C24 C25 C48 11.8(3) . . . . ?
C24 C25 C26 C27 -0.99(18) . . . . ?
C48 C25 C26 C27 176.65(14) . . . . ?
C24 C25 C26 C50 175.92(14) . . . . ?
C48 C25 C26 C50 -6.4(2) . . . . ?
C25 C26 C27 N5 -0.67(17) . . . . ?
C50 C26 C27 N5 -177.19(16) . . . . ?
C25 C26 C27 C28 172.46(18) . . . . ?
C50 C26 C27 C28 -4.1(3) . . . . ?
C5 N5 C27 C26 -177.26(14) . . . . ?
C24 N5 C27 C26 2.14(17) . . . . ?
C5 N5 C27 C28 7.8(2) . . . . ?
C24 N5 C27 C28 -172.81(13) . . . . ?
C6 N6 C28 C29 168.62(14) . . . . ?
C31 N6 C28 C29 -2.62(17) . . . . ?
C6 N6 C28 C27 -15.4(2) . . . . ?
C31 N6 C28 C27 173.38(13) . . . . ?
C26 C27 C28 C29 6.5(3) . . . . ?
N5 C27 C28 C29 179.16(18) . . . . ?
C26 C27 C28 N6 -167.55(17) . . . . ?
N5 C27 C28 N6 5.08(19) . . . . ?
N6 C28 C29 C30 0.71(17) . . . . ?
C27 C28 C29 C30 -173.74(18) . . . . ?
N6 C28 C29 C52 178.11(15) . . . . ?
C27 C28 C29 C52 3.7(3) . . . . ?
C28 C29 C30 C31 1.39(18) . . . . ?
C52 C29 C30 C31 -176.32(14) . . . . ?
C28 C29 C30 C54 -171.82(15) . . . . ?
C52 C29 C30 C54 10.5(2) . . . . ?
C29 C30 C31 N6 -2.92(17) . . . . ?
C54 C30 C31 N6 170.19(15) . . . . ?
C29 C30 C31 C7 171.65(18) . . . . ?
C54 C30 C31 C7 -15.2(3) . . . . ?
C6 N6 C31 C30 -167.95(14) . . . . ?
C28 N6 C31 C30 3.50(17) . . . . ?
C6 N6 C31 C7 16.1(2) . . . . ?
C28 N6 C31 C7 -172.49(13) . . . . ?
C8 C7 C31 C30 -26.5(3) . . . . ?
N1 C7 C31 C30 163.31(18) . . . . ?
C8 C7 C31 N6 147.75(18) . . . . ?
N1 C7 C31 N6 -22.5(2) . . . . ?
C7 C8 C32 C33 -63.2(2) . . . . ?
C9 C8 C32 C33 109.90(19) . . . . ?
C10 C9 C34 C35 97.5(2) . . . . ?
C8 C9 C34 C35 -72.0(2) . . . . ?
C11 C12 C36 C37 -99.9(2) . . . . ?
C13 C12 C36 C37 85.63(19) . . . . ?
C14 C13 C38 C39 -89.9(2) . . . . ?
C12 C13 C38 C39 88.0(2) . . . . ?
C16 C17 C40 C41 97.28(19) . . . . ?
C18 C17 C40 C41 -83.0(2) . . . . ?
C19 C18 C42 C43 -65.0(2) . . . . ?
C17 C18 C42 C43 108.07(18) . . . . ?
C20 C21 C44 C45 -59.4(2) . . . . ?
C22 C21 C44 C45 111.69(18) . . . . ?
C23 C22 C46 C47 -100.3(2) . . . . ?
C21 C22 C46 C47 81.8(2) . . . . ?
C24 C25 C48 C49 99.4(2) . . . . ?
C26 C25 C48 C49 -77.7(2) . . . . ?
C27 C26 C50 C51 88.1(2) . . . . ?
C25 C26 C50 C51 -88.0(2) . . . . ?
C28 C29 C52 C53 -106.9(2) . . . . ?
C30 C29 C52 C53 70.3(2) . . . . ?
C31 C30 C54 C55 -52.3(2) . . . . ?
C29 C30 C54 C55 119.71(18) . . . . ?

#==============================================================================

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


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

data_xcalibur_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2129377'
loop_
_audit_author_name
_audit_author_address
'Masayoshi Takase'
;Ehime University
Japan
;
_audit_update_record             
;
2021-12-17 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C55 H60 I8 N6 O'
_chemical_formula_moiety         'C55 H60 I8 N6 O'
_chemical_formula_weight         1836.35
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   9.05536(18)
_cell_length_b                   26.9319(6)
_cell_length_c                   24.0347(5)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.1939(19)
_cell_angle_gamma                90.0000
_cell_volume                     5861.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    39426
_cell_measurement_theta_min      1.73
_cell_measurement_theta_max      31.24
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3456.00
_exptl_absorpt_coefficient_mu    4.278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_T_max  0.958

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

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            96557
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.512
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             13462
_reflns_number_gt                10540
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0896
_refine_ls_number_restraints     218
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         13462
_refine_ls_number_parameters     736
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0325P)²+23.7057P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.47
_refine_diff_density_min         -1.58
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
I I -0.4742 1.8119
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

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

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C48 C 0.0861(14) 0.4753(4) 0.0977(5) 0.033(3) Uani 0.580(13) 1 d D U P A 1
H48A H 0.021899 0.452302 0.076527 0.039 Uiso 0.580(13) 1 calc R U P A 1
H48B H 0.032559 0.485232 0.131812 0.039 Uiso 0.580(13) 1 calc R U P A 1
C49 C 0.1155(14) 0.5218(4) 0.0622(5) 0.051(4) Uani 0.580(13) 1 d D U P A 1
H49A H 0.174182 0.545579 0.083784 0.077 Uiso 0.580(13) 1 calc R U P A 1
H49B H 0.021303 0.537030 0.051588 0.077 Uiso 0.580(13) 1 calc R U P A 1
H49C H 0.169795 0.512287 0.028651 0.077 Uiso 0.580(13) 1 calc R U P A 1
C148 C 0.1464(16) 0.4823(6) 0.0807(6) 0.031(4) Uani 0.420(13) 1 d D U P A 2
H14A H 0.172176 0.479494 0.040848 0.037 Uiso 0.420(13) 1 calc R U P A 2
H14B H 0.161084 0.517012 0.093084 0.037 Uiso 0.420(13) 1 calc R U P A 2
C149 C -0.0130(16) 0.4645(7) 0.0917(7) 0.048(5) Uani 0.420(13) 1 d D U P A 2
H14C H -0.023173 0.429845 0.080013 0.072 Uiso 0.420(13) 1 calc R U P A 2
H14D H -0.082371 0.485212 0.070614 0.072 Uiso 0.420(13) 1 calc R U P A 2
H14E H -0.034526 0.467271 0.131538 0.072 Uiso 0.420(13) 1 calc R U P A 2
I1 I 0.4596(2) 0.23503(9) 0.41671(8) 0.0413(3) Uani 0.766(6) 1 d . U P B 3
I2 I 0.3737(4) 0.23547(12) 0.30183(15) 0.0249(3) Uani 0.766(6) 1 d . U P B 3
I3 I 0.2685(3) 0.23995(9) 0.18333(8) 0.0287(3) Uani 0.766(6) 1 d . U P B 3
I4 I 0.08010(14) 0.33924(4) 0.21931(5) 0.0229(3) Uani 0.766(6) 1 d . U P B 3
I5 I -0.07236(11) 0.41878(3) 0.26371(4) 0.0240(3) Uani 0.766(6) 1 d . U P B 3
I6 I -0.27937(16) 0.51451(5) 0.31242(6) 0.0318(3) Uani 0.766(6) 1 d . U P B 3
I7 I -0.34807(10) 0.51880(3) 0.19027(3) 0.0327(3) Uani 0.766(6) 1 d . U P B 3
I8 I -0.4052(3) 0.51393(11) 0.07383(13) 0.0808(7) Uani 0.766(6) 1 d . U P B 3
I11 I 0.4427(10) 0.2236(4) 0.4094(4) 0.076(3) Uani 0.234(6) 1 d . U P B 4
I12 I 0.3641(16) 0.2308(5) 0.2940(6) 0.042(3) Uani 0.234(6) 1 d . U P B 4
I13 I 0.2737(10) 0.2365(3) 0.1789(3) 0.052(2) Uani 0.234(6) 1 d . U P B 4
I14 I 0.0651(7) 0.3439(3) 0.2188(3) 0.079(2) Uani 0.234(6) 1 d . U P B 4
I15 I -0.0924(7) 0.4251(3) 0.2624(3) 0.108(3) Uani 0.234(6) 1 d . U P B 4
I16 I -0.2878(8) 0.5159(2) 0.3026(4) 0.099(2) Uani 0.234(6) 1 d . U P B 4
I17 I -0.3415(9) 0.5163(3) 0.1889(4) 0.145(3) Uani 0.234(6) 1 d . U P B 4
I18 I -0.4408(7) 0.5160(3) 0.0748(3) 0.0381(9) Uani 0.234(6) 1 d . U P B 4
O1 O 0.5985(5) 0.38165(19) 0.50044(16) 0.0554(14) Uani 1 1 d . . . . .
N1 N 0.7090(4) 0.29861(14) 0.26054(16) 0.0178(8) Uani 1 1 d . . . . .
N2 N 0.6824(4) 0.34270(14) 0.36240(16) 0.0184(8) Uani 1 1 d . . . . .
N3 N 0.4474(4) 0.42734(14) 0.36985(16) 0.0188(8) Uani 1 1 d . . . . .
N4 N 0.3303(4) 0.45653(14) 0.26942(16) 0.0198(8) Uani 1 1 d . . . . .
N5 N 0.3890(4) 0.41033(14) 0.17333(16) 0.0213(9) Uani 1 1 d . . . . .
N6 N 0.5693(4) 0.33054(15) 0.16943(16) 0.0208(9) Uani 1 1 d . . . . .
C1 C 0.6149(5) 0.33822(16) 0.26707(19) 0.0162(9) Uani 1 1 d . . . . .
C2 C 0.5919(5) 0.36066(16) 0.31896(19) 0.0168(9) Uani 1 1 d . . . . .
C3 C 0.4909(5) 0.40079(16) 0.32167(19) 0.0158(9) Uani 1 1 d . . . . .
C4 C 0.4248(5) 0.41630(16) 0.27183(19) 0.0179(10) Uani 1 1 d . . . . .
C5 C 0.4538(5) 0.39392(17) 0.22139(19) 0.0182(10) Uani 1 1 d . . . . .
C6 C 0.5444(5) 0.35413(17) 0.2193(2) 0.0195(10) Uani 1 1 d . . . . .
C7 C 0.7174(5) 0.26882(17) 0.2124(2) 0.0216(10) Uani 1 1 d . . . . .
C8 C 0.8014(5) 0.22657(18) 0.2289(2) 0.0241(11) Uani 1 1 d . . . . .
C9 C 0.8496(5) 0.23307(18) 0.2833(2) 0.0237(11) Uani 1 1 d . . . . .
C10 C 0.7947(5) 0.27999(19) 0.3023(2) 0.0240(11) Uani 1 1 d . . . . .
C11 C 0.8008(5) 0.30929(17) 0.3521(2) 0.0202(10) Uani 1 1 d . . . . .
C12 C 0.8987(5) 0.31073(18) 0.3967(2) 0.0228(11) Uani 1 1 d . . . . .
C13 C 0.8320(5) 0.34054(19) 0.4376(2) 0.0233(10) Uani 1 1 d . . . . .
C14 C 0.7004(6) 0.35949(19) 0.4165(2) 0.0239(11) Uani 1 1 d . . . . .
C15 C 0.5904(6) 0.3857(2) 0.4492(2) 0.0283(12) Uani 1 1 d . . . . .
C16 C 0.4758(5) 0.41732(17) 0.42596(19) 0.0200(10) Uani 1 1 d . . . . .
C17 C 0.3853(5) 0.44816(18) 0.4577(2) 0.0213(10) Uani 1 1 d . . . . .
C18 C 0.3024(5) 0.47761(18) 0.4218(2) 0.0221(10) Uani 1 1 d . . . . .
C19 C 0.3442(5) 0.46651(17) 0.3674(2) 0.0188(10) Uani 1 1 d . . . . .
C20 C 0.2990(5) 0.48531(18) 0.3144(2) 0.0223(10) Uani 1 1 d . . . . .
C21 C 0.2239(5) 0.52817(18) 0.2938(2) 0.0235(11) Uani 1 1 d . . . . .
C22 C 0.2012(6) 0.52143(19) 0.2368(2) 0.0264(11) Uani 1 1 d . . . . .
C23 C 0.2683(6) 0.47630(18) 0.2202(2) 0.0236(11) Uani 1 1 d . . . . .
C24 C 0.2886(6) 0.44880(18) 0.1705(2) 0.0270(11) Uani 1 1 d . . . . .
C25 C 0.2317(7) 0.4477(2) 0.1146(2) 0.0416(16) Uani 1 1 d D . . . .
C26 C 0.3004(7) 0.4096(2) 0.0859(2) 0.0370(14) Uani 1 1 d . . . . .
C27 C 0.4043(6) 0.38538(19) 0.1221(2) 0.0276(12) Uani 1 1 d . . . . .
C28 C 0.5046(6) 0.34574(18) 0.1197(2) 0.0254(11) Uani 1 1 d . . . . .
C29 C 0.5655(6) 0.31267(19) 0.0782(2) 0.0283(12) Uani 1 1 d . . . . .
C30 C 0.6495(6) 0.27697(19) 0.1046(2) 0.0265(12) Uani 1 1 d . . . . .
C31 C 0.6522(5) 0.28792(18) 0.1636(2) 0.0233(11) Uani 1 1 d . . . . .
C32 C 0.8138(6) 0.1785(2) 0.1962(2) 0.0336(13) Uani 1 1 d . . . . .
H32A H 0.883121 0.155721 0.215290 0.040 Uiso 1 1 calc R U . . .
H32B H 0.853345 0.185595 0.158653 0.040 Uiso 1 1 calc R U . . .
C33 C 0.6608(7) 0.1536(2) 0.1909(3) 0.0402(15) Uani 1 1 d . . . . .
H33A H 0.590883 0.176933 0.173919 0.048 Uiso 1 1 calc R U . . .
H33B H 0.625550 0.144099 0.227900 0.048 Uiso 1 1 calc R U . . .
H33C H 0.668816 0.123921 0.167486 0.048 Uiso 1 1 calc R U . . .
C34 C 0.9315(6) 0.1951(2) 0.3171(2) 0.0330(13) Uani 1 1 d . . . . .
H34A H 0.952806 0.166140 0.293135 0.040 Uiso 1 1 calc R U . . .
H34B H 1.027345 0.209521 0.328788 0.040 Uiso 1 1 calc R U . . .
C35 C 0.8527(9) 0.1776(3) 0.3674(3) 0.068(2) Uani 1 1 d . . . . .
H35A H 0.764177 0.159094 0.356201 0.082 Uiso 1 1 calc R U . . .
H35B H 0.823887 0.206148 0.390150 0.082 Uiso 1 1 calc R U . . .
H35C H 0.917814 0.155825 0.389100 0.082 Uiso 1 1 calc R U . . .
C36 C 1.0561(5) 0.29386(19) 0.3987(2) 0.0268(11) Uani 1 1 d . . . . .
H36A H 1.072074 0.267792 0.370269 0.032 Uiso 1 1 calc R U . . .
H36B H 1.077888 0.279382 0.435649 0.032 Uiso 1 1 calc R U . . .
C37 C 1.1611(6) 0.3376(2) 0.3877(2) 0.0337(13) Uani 1 1 d . . . . .
H37A H 1.145531 0.363376 0.415922 0.040 Uiso 1 1 calc R U . . .
H37B H 1.141198 0.351420 0.350715 0.040 Uiso 1 1 calc R U . . .
H37C H 1.263601 0.326024 0.389562 0.040 Uiso 1 1 calc R U . . .
C38 C 0.8955(6) 0.3486(2) 0.4952(2) 0.0326(13) Uani 1 1 d . . . . .
H38A H 0.860208 0.380887 0.509801 0.039 Uiso 1 1 calc R U . . .
H38B H 1.004538 0.350193 0.492800 0.039 Uiso 1 1 calc R U . . .
C39 C 0.8521(7) 0.3077(3) 0.5353(2) 0.0449(16) Uani 1 1 d . . . . .
H39A H 0.883644 0.275531 0.520355 0.054 Uiso 1 1 calc R U . . .
H39B H 0.744672 0.307675 0.540044 0.054 Uiso 1 1 calc R U . . .
H39C H 0.899998 0.313352 0.571361 0.054 Uiso 1 1 calc R U . . .
C40 C 0.3754(6) 0.44888(19) 0.5207(2) 0.0256(11) Uani 1 1 d . . . . .
H40A H 0.327998 0.480222 0.532624 0.031 Uiso 1 1 calc R U . . .
H40B H 0.476411 0.448139 0.536571 0.031 Uiso 1 1 calc R U . . .
C41 C 0.2880(7) 0.4053(2) 0.5435(2) 0.0387(14) Uani 1 1 d . . . . .
H41A H 0.335415 0.374134 0.532341 0.046 Uiso 1 1 calc R U . . .
H41B H 0.187090 0.406286 0.528609 0.046 Uiso 1 1 calc R U . . .
H41C H 0.284952 0.407280 0.584166 0.046 Uiso 1 1 calc R U . . .
C42 C 0.1790(6) 0.5110(2) 0.4403(2) 0.0340(13) Uani 1 1 d . . . . .
H42A H 0.194377 0.544662 0.424737 0.041 Uiso 1 1 calc R U . . .
H42B H 0.180652 0.513712 0.481372 0.041 Uiso 1 1 calc R U . . .
C43 C 0.0299(6) 0.4917(3) 0.4217(3) 0.0462(17) Uani 1 1 d . . . . .
H43A H 0.010719 0.459617 0.439588 0.055 Uiso 1 1 calc R U . . .
H43B H 0.029611 0.487410 0.381193 0.055 Uiso 1 1 calc R U . . .
H43C H -0.047065 0.515396 0.432237 0.055 Uiso 1 1 calc R U . . .
C44 C 0.1930(6) 0.5756(2) 0.3243(2) 0.0326(13) Uani 1 1 d . . . . .
H44A H 0.120755 0.569056 0.354299 0.039 Uiso 1 1 calc R U . . .
H44B H 0.148414 0.599851 0.298304 0.039 Uiso 1 1 calc R U . . .
C45 C 0.3338(6) 0.59777(19) 0.3497(2) 0.0338(13) Uani 1 1 d . . . . .
H45A H 0.403579 0.605802 0.319952 0.041 Uiso 1 1 calc R U . . .
H45B H 0.378859 0.573642 0.375130 0.041 Uiso 1 1 calc R U . . .
H45C H 0.309012 0.628058 0.370251 0.041 Uiso 1 1 calc R U . . .
C46 C 0.1313(7) 0.5600(2) 0.1991(2) 0.0399(15) Uani 1 1 d . . . . .
H46A H 0.079333 0.543039 0.168174 0.048 Uiso 1 1 calc R U . . .
H46B H 0.057427 0.579192 0.220401 0.048 Uiso 1 1 calc R U . . .
C47 C 0.2456(9) 0.5951(3) 0.1755(3) 0.066(2) Uani 1 1 d . . . . .
H47A H 0.320869 0.576034 0.155588 0.079 Uiso 1 1 calc R U . . .
H47B H 0.292241 0.613659 0.205946 0.079 Uiso 1 1 calc R U . . .
H47C H 0.197643 0.618333 0.149828 0.079 Uiso 1 1 calc R U . . .
C50 C 0.2560(9) 0.3926(2) 0.0281(2) 0.0504(19) Uani 1 1 d . . . . .
H50A H 0.345308 0.387285 0.005177 0.061 Uiso 1 1 calc R U . . .
H50B H 0.194776 0.418379 0.009861 0.061 Uiso 1 1 calc R U . . .
C51 C 0.1674(10) 0.3436(3) 0.0322(3) 0.067(2) Uani 1 1 d . . . . .
H51A H 0.077741 0.349200 0.054016 0.081 Uiso 1 1 calc R U . . .
H51B H 0.228186 0.318201 0.050451 0.081 Uiso 1 1 calc R U . . .
H51C H 0.140314 0.332306 -0.005228 0.081 Uiso 1 1 calc R U . . .
C52 C 0.5568(8) 0.3198(2) 0.0158(2) 0.0420(16) Uani 1 1 d . . . . .
H52A H 0.452283 0.324057 0.004595 0.050 Uiso 1 1 calc R U . . .
H52B H 0.595343 0.289752 -0.002951 0.050 Uiso 1 1 calc R U . . .
C53 C 0.6460(8) 0.3651(2) -0.0026(3) 0.0505(18) Uani 1 1 d . . . . .
H53A H 0.749964 0.360489 0.007562 0.061 Uiso 1 1 calc R U . . .
H53B H 0.607626 0.394883 0.015878 0.061 Uiso 1 1 calc R U . . .
H53C H 0.637412 0.369083 -0.043005 0.061 Uiso 1 1 calc R U . . .
C54 C 0.7353(6) 0.2366(2) 0.0762(2) 0.0332(13) Uani 1 1 d . . . . .
H54A H 0.698168 0.232580 0.037679 0.040 Uiso 1 1 calc R U . . .
H54B H 0.718938 0.204830 0.096076 0.040 Uiso 1 1 calc R U . . .
C55 C 0.9018(7) 0.2477(3) 0.0747(3) 0.0458(17) Uani 1 1 d . . . . .
H55A H 0.937038 0.254995 0.112425 0.055 Uiso 1 1 calc R U . . .
H55B H 0.919731 0.276503 0.050677 0.055 Uiso 1 1 calc R U . . .
H55C H 0.954670 0.218848 0.060019 0.055 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2'

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

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C48 C49 1.537(12) . ?
C48 C25 1.567(12) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C148 C25 1.458(13) . ?
C148 C149 1.544(15) . ?
C148 H14A 0.9900 . ?
C148 H14B 0.9900 . ?
C149 H14C 0.9800 . ?
C149 H14D 0.9800 . ?
C149 H14E 0.9800 . ?
I1 I2 2.866(4) . ?
I2 I3 3.002(4) . ?
I4 I5 2.7648(16) . ?
I6 I7 3.0011(15) . ?
I7 I8 2.847(3) . ?
I11 I12 2.867(16) . ?
I12 I13 2.885(15) . ?
I14 I15 2.813(8) . ?
I16 I17 2.773(12) . ?
I17 I18 2.884(11) . ?
O1 C15 1.238(6) . ?
N1 C10 1.362(6) . ?
N1 C1 1.375(6) . ?
N1 C7 1.410(6) . ?
N2 C14 1.386(6) . ?
N2 C2 1.411(6) . ?
N2 C11 1.422(6) . ?
N3 C16 1.398(6) . ?
N3 C19 1.411(6) . ?
N3 C3 1.418(6) . ?
N4 C20 1.362(6) . ?
N4 C4 1.381(6) . ?
N4 C23 1.412(6) . ?
N5 C5 1.367(6) . ?
N5 C24 1.380(7) . ?
N5 C27 1.410(6) . ?
N6 C6 1.377(6) . ?
N6 C31 1.379(6) . ?
N6 C28 1.392(6) . ?
C1 C6 1.379(7) . ?
C1 C2 1.402(6) . ?
C2 C3 1.418(6) . ?
C3 C4 1.401(6) . ?
C4 C5 1.380(6) . ?
C5 C6 1.351(7) . ?
C7 C31 1.408(7) . ?
C7 C8 1.425(7) . ?
C8 C9 1.387(7) . ?
C8 C32 1.519(7) . ?
C9 C10 1.433(7) . ?
C9 C34 1.501(7) . ?
C10 C11 1.435(7) . ?
C11 C12 1.389(7) . ?
C12 C13 1.407(7) . ?
C12 C36 1.497(7) . ?
C13 C14 1.390(7) . ?
C13 C38 1.514(7) . ?
C14 C15 1.453(7) . ?
C15 C16 1.452(7) . ?
C16 C17 1.396(7) . ?
C17 C18 1.391(7) . ?
C17 C40 1.516(7) . ?
C18 C19 1.395(7) . ?
C18 C42 1.504(7) . ?
C19 C20 1.428(7) . ?
C20 C21 1.427(7) . ?
C21 C22 1.396(7) . ?
C21 C44 1.499(7) . ?
C22 C23 1.417(7) . ?
C22 C46 1.515(7) . ?
C23 C24 1.418(7) . ?
C24 C25 1.437(7) . ?
C25 C26 1.384(9) . ?
C26 C27 1.437(8) . ?
C26 C50 1.517(8) . ?
C27 C28 1.403(8) . ?
C28 C29 1.446(7) . ?
C29 C30 1.379(8) . ?
C29 C52 1.513(7) . ?
C30 C31 1.450(7) . ?
C30 C54 1.502(7) . ?
C32 C33 1.545(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.483(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.538(7) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.517(8) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.520(7) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.513(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.533(8) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.513(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C50 C51 1.547(9) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.531(8) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.538(8) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 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
C49 C48 C25 112.5(10) . . ?
C49 C48 H48A 109.1 . . ?
C25 C48 H48A 109.1 . . ?
C49 C48 H48B 109.1 . . ?
C25 C48 H48B 109.1 . . ?
H48A C48 H48B 107.8 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C25 C148 C149 101.5(10) . . ?
C25 C148 H14A 111.5 . . ?
C149 C148 H14A 111.5 . . ?
C25 C148 H14B 111.5 . . ?
C149 C148 H14B 111.5 . . ?
H14A C148 H14B 109.3 . . ?
C148 C149 H14C 109.5 . . ?
C148 C149 H14D 109.5 . . ?
H14C C149 H14D 109.5 . . ?
C148 C149 H14E 109.5 . . ?
H14C C149 H14E 109.5 . . ?
H14D C149 H14E 109.5 . . ?
I1 I2 I3 176.54(17) . . ?
I8 I7 I6 174.92(8) . . ?
I11 I12 I13 177.8(6) . . ?
I16 I17 I18 171.9(4) . . ?
C10 N1 C1 123.6(4) . . ?
C10 N1 C7 111.3(4) . . ?
C1 N1 C7 124.8(4) . . ?
C14 N2 C2 130.4(4) . . ?
C14 N2 C11 106.5(4) . . ?
C2 N2 C11 121.6(4) . . ?
C16 N3 C19 107.7(4) . . ?
C16 N3 C3 129.8(4) . . ?
C19 N3 C3 121.9(4) . . ?
C20 N4 C4 122.9(4) . . ?
C20 N4 C23 111.6(4) . . ?
C4 N4 C23 125.1(4) . . ?
C5 N5 C24 124.4(4) . . ?
C5 N5 C27 122.7(4) . . ?
C24 N5 C27 112.4(4) . . ?
C6 N6 C31 124.3(4) . . ?
C6 N6 C28 122.9(4) . . ?
C31 N6 C28 112.7(4) . . ?
N1 C1 C6 115.6(4) . . ?
N1 C1 C2 122.0(4) . . ?
C6 C1 C2 122.4(4) . . ?
C1 C2 N2 115.0(4) . . ?
C1 C2 C3 117.9(4) . . ?
N2 C2 C3 126.9(4) . . ?
C4 C3 C2 117.5(4) . . ?
C4 C3 N3 115.4(4) . . ?
C2 C3 N3 127.1(4) . . ?
C5 C4 N4 115.2(4) . . ?
C5 C4 C3 122.6(4) . . ?
N4 C4 C3 122.2(4) . . ?
C6 C5 N5 119.0(4) . . ?
C6 C5 C4 119.7(4) . . ?
N5 C5 C4 121.2(4) . . ?
C5 C6 N6 119.9(4) . . ?
C5 C6 C1 119.7(4) . . ?
N6 C6 C1 120.3(4) . . ?
C31 C7 N1 116.8(4) . . ?
C31 C7 C8 138.3(5) . . ?
N1 C7 C8 104.8(4) . . ?
C9 C8 C7 109.1(4) . . ?
C9 C8 C32 124.9(5) . . ?
C7 C8 C32 125.2(5) . . ?
C8 C9 C10 107.6(4) . . ?
C8 C9 C34 125.3(5) . . ?
C10 C9 C34 126.8(5) . . ?
N1 C10 C9 106.7(4) . . ?
N1 C10 C11 115.6(4) . . ?
C9 C10 C11 137.6(5) . . ?
C12 C11 N2 109.1(4) . . ?
C12 C11 C10 133.0(5) . . ?
N2 C11 C10 117.8(4) . . ?
C11 C12 C13 106.3(4) . . ?
C11 C12 C36 128.4(5) . . ?
C13 C12 C36 124.2(5) . . ?
C14 C13 C12 109.0(4) . . ?
C14 C13 C38 127.1(5) . . ?
C12 C13 C38 124.0(4) . . ?
N2 C14 C13 108.6(4) . . ?
N2 C14 C15 126.0(4) . . ?
C13 C14 C15 124.7(5) . . ?
O1 C15 C16 118.3(5) . . ?
O1 C15 C14 117.1(5) . . ?
C16 C15 C14 124.6(5) . . ?
C17 C16 N3 107.8(4) . . ?
C17 C16 C15 123.9(4) . . ?
N3 C16 C15 127.8(4) . . ?
C18 C17 C16 108.4(4) . . ?
C18 C17 C40 125.4(4) . . ?
C16 C17 C40 126.2(4) . . ?
C17 C18 C19 108.3(4) . . ?
C17 C18 C42 123.9(4) . . ?
C19 C18 C42 127.6(5) . . ?
C18 C19 N3 107.6(4) . . ?
C18 C19 C20 133.0(4) . . ?
N3 C19 C20 119.4(4) . . ?
N4 C20 C21 106.6(4) . . ?
N4 C20 C19 116.5(4) . . ?
C21 C20 C19 136.9(5) . . ?
C22 C21 C20 107.7(4) . . ?
C22 C21 C44 124.3(4) . . ?
C20 C21 C44 127.5(5) . . ?
C21 C22 C23 109.1(4) . . ?
C21 C22 C46 123.9(5) . . ?
C23 C22 C46 126.7(5) . . ?
N4 C23 C22 104.8(4) . . ?
N4 C23 C24 117.2(4) . . ?
C22 C23 C24 138.0(5) . . ?
N5 C24 C23 115.9(4) . . ?
N5 C24 C25 105.4(5) . . ?
C23 C24 C25 138.7(5) . . ?
C26 C25 C24 108.8(5) . . ?
C26 C25 C148 115.6(8) . . ?
C24 C25 C148 134.1(9) . . ?
C26 C25 C48 127.0(6) . . ?
C24 C25 C48 122.1(7) . . ?
C25 C26 C27 109.2(5) . . ?
C25 C26 C50 124.3(6) . . ?
C27 C26 C50 126.0(6) . . ?
C28 C27 N5 117.7(4) . . ?
C28 C27 C26 138.0(5) . . ?
N5 C27 C26 104.2(5) . . ?
N6 C28 C27 117.3(4) . . ?
N6 C28 C29 104.5(5) . . ?
C27 C28 C29 138.2(5) . . ?
C30 C29 C28 108.9(4) . . ?
C30 C29 C52 124.7(5) . . ?
C28 C29 C52 125.9(5) . . ?
C29 C30 C31 108.4(5) . . ?
C29 C30 C54 125.6(5) . . ?
C31 C30 C54 125.8(5) . . ?
N6 C31 C7 116.6(4) . . ?
N6 C31 C30 105.1(4) . . ?
C7 C31 C30 138.3(5) . . ?
C8 C32 C33 110.2(4) . . ?
C8 C32 H32A 109.6 . . ?
C33 C32 H32A 109.6 . . ?
C8 C32 H32B 109.6 . . ?
C33 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C9 114.8(5) . . ?
C35 C34 H34A 108.6 . . ?
C9 C34 H34A 108.6 . . ?
C35 C34 H34B 108.6 . . ?
C9 C34 H34B 108.6 . . ?
H34A C34 H34B 107.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C12 C36 C37 110.6(4) . . ?
C12 C36 H36A 109.5 . . ?
C37 C36 H36A 109.5 . . ?
C12 C36 H36B 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C13 C38 C39 112.2(5) . . ?
C13 C38 H38A 109.2 . . ?
C39 C38 H38A 109.2 . . ?
C13 C38 H38B 109.2 . . ?
C39 C38 H38B 109.2 . . ?
H38A C38 H38B 107.9 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C17 C40 C41 112.5(4) . . ?
C17 C40 H40A 109.1 . . ?
C41 C40 H40A 109.1 . . ?
C17 C40 H40B 109.1 . . ?
C41 C40 H40B 109.1 . . ?
H40A C40 H40B 107.8 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C18 C42 C43 111.7(5) . . ?
C18 C42 H42A 109.3 . . ?
C43 C42 H42A 109.3 . . ?
C18 C42 H42B 109.3 . . ?
C43 C42 H42B 109.3 . . ?
H42A C42 H42B 107.9 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C21 C44 C45 111.7(4) . . ?
C21 C44 H44A 109.3 . . ?
C45 C44 H44A 109.3 . . ?
C21 C44 H44B 109.3 . . ?
C45 C44 H44B 109.3 . . ?
H44A C44 H44B 107.9 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 C22 111.6(5) . . ?
C47 C46 H46A 109.3 . . ?
C22 C46 H46A 109.3 . . ?
C47 C46 H46B 109.3 . . ?
C22 C46 H46B 109.3 . . ?
H46A C46 H46B 108.0 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C26 C50 C51 109.6(5) . . ?
C26 C50 H50A 109.8 . . ?
C51 C50 H50A 109.8 . . ?
C26 C50 H50B 109.8 . . ?
C51 C50 H50B 109.8 . . ?
H50A C50 H50B 108.2 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C29 C52 C53 111.2(5) . . ?
C29 C52 H52A 109.4 . . ?
C53 C52 H52A 109.4 . . ?
C29 C52 H52B 109.4 . . ?
C53 C52 H52B 109.4 . . ?
H52A C52 H52B 108.0 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C30 C54 C55 112.2(5) . . ?
C30 C54 H54A 109.2 . . ?
C55 C54 H54A 109.2 . . ?
C30 C54 H54B 109.2 . . ?
C55 C54 H54B 109.2 . . ?
H54A C54 H54B 107.9 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 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
C10 N1 C1 C6 175.7(4) . . . . ?
C7 N1 C1 C6 -11.7(6) . . . . ?
C10 N1 C1 C2 -4.6(7) . . . . ?
C7 N1 C1 C2 168.0(4) . . . . ?
N1 C1 C2 N2 5.7(6) . . . . ?
C6 C1 C2 N2 -174.6(4) . . . . ?
N1 C1 C2 C3 -179.0(4) . . . . ?
C6 C1 C2 C3 0.7(7) . . . . ?
C14 N2 C2 C1 172.5(5) . . . . ?
C11 N2 C2 C1 8.1(6) . . . . ?
C14 N2 C2 C3 -2.3(8) . . . . ?
C11 N2 C2 C3 -166.7(4) . . . . ?
C1 C2 C3 C4 -2.1(6) . . . . ?
N2 C2 C3 C4 172.6(4) . . . . ?
C1 C2 C3 N3 177.4(4) . . . . ?
N2 C2 C3 N3 -7.9(7) . . . . ?
C16 N3 C3 C4 170.3(4) . . . . ?
C19 N3 C3 C4 0.2(6) . . . . ?
C16 N3 C3 C2 -9.2(7) . . . . ?
C19 N3 C3 C2 -179.3(4) . . . . ?
C20 N4 C4 C5 -174.7(4) . . . . ?
C23 N4 C4 C5 -2.2(7) . . . . ?
C20 N4 C4 C3 2.8(7) . . . . ?
C23 N4 C4 C3 175.3(4) . . . . ?
C2 C3 C4 C5 0.4(7) . . . . ?
N3 C3 C4 C5 -179.2(4) . . . . ?
C2 C3 C4 N4 -176.8(4) . . . . ?
N3 C3 C4 N4 3.6(6) . . . . ?
C24 N5 C5 C6 176.4(4) . . . . ?
C27 N5 C5 C6 4.6(7) . . . . ?
C24 N5 C5 C4 -1.6(7) . . . . ?
C27 N5 C5 C4 -173.4(4) . . . . ?
N4 C4 C5 C6 -179.7(4) . . . . ?
C3 C4 C5 C6 2.8(7) . . . . ?
N4 C4 C5 N5 -1.7(6) . . . . ?
C3 C4 C5 N5 -179.1(4) . . . . ?
N5 C5 C6 N6 -0.6(7) . . . . ?
C4 C5 C6 N6 177.6(4) . . . . ?
N5 C5 C6 C1 177.6(4) . . . . ?
C4 C5 C6 C1 -4.3(7) . . . . ?
C31 N6 C6 C5 -175.7(4) . . . . ?
C28 N6 C6 C5 0.0(7) . . . . ?
C31 N6 C6 C1 6.1(7) . . . . ?
C28 N6 C6 C1 -178.2(4) . . . . ?
N1 C1 C6 C5 -177.7(4) . . . . ?
C2 C1 C6 C5 2.6(7) . . . . ?
N1 C1 C6 N6 0.4(6) . . . . ?
C2 C1 C6 N6 -179.3(4) . . . . ?
C10 N1 C7 C31 -170.6(4) . . . . ?
C1 N1 C7 C31 16.0(6) . . . . ?
C10 N1 C7 C8 6.7(5) . . . . ?
C1 N1 C7 C8 -166.7(4) . . . . ?
C31 C7 C8 C9 172.1(6) . . . . ?
N1 C7 C8 C9 -4.2(5) . . . . ?
C31 C7 C8 C32 -17.7(9) . . . . ?
N1 C7 C8 C32 166.0(4) . . . . ?
C7 C8 C9 C10 0.5(5) . . . . ?
C32 C8 C9 C10 -169.8(5) . . . . ?
C7 C8 C9 C34 175.1(5) . . . . ?
C32 C8 C9 C34 4.8(8) . . . . ?
C1 N1 C10 C9 167.0(4) . . . . ?
C7 N1 C10 C9 -6.4(5) . . . . ?
C1 N1 C10 C11 -10.1(7) . . . . ?
C7 N1 C10 C11 176.4(4) . . . . ?
C8 C9 C10 N1 3.6(5) . . . . ?
C34 C9 C10 N1 -170.9(5) . . . . ?
C8 C9 C10 C11 179.8(6) . . . . ?
C34 C9 C10 C11 5.3(10) . . . . ?
C14 N2 C11 C12 -7.4(5) . . . . ?
C2 N2 C11 C12 160.3(4) . . . . ?
C14 N2 C11 C10 169.6(4) . . . . ?
C2 N2 C11 C10 -22.8(6) . . . . ?
N1 C10 C11 C12 -161.0(5) . . . . ?
C9 C10 C11 C12 23.0(10) . . . . ?
N1 C10 C11 N2 23.0(6) . . . . ?
C9 C10 C11 N2 -153.0(6) . . . . ?
N2 C11 C12 C13 6.9(5) . . . . ?
C10 C11 C12 C13 -169.4(5) . . . . ?
N2 C11 C12 C36 -161.4(5) . . . . ?
C10 C11 C12 C36 22.4(9) . . . . ?
C11 C12 C13 C14 -3.9(6) . . . . ?
C36 C12 C13 C14 165.0(5) . . . . ?
C11 C12 C13 C38 174.8(5) . . . . ?
C36 C12 C13 C38 -16.3(8) . . . . ?
C2 N2 C14 C13 -161.3(5) . . . . ?
C11 N2 C14 C13 4.8(5) . . . . ?
C2 N2 C14 C15 27.8(8) . . . . ?
C11 N2 C14 C15 -166.1(5) . . . . ?
C12 C13 C14 N2 -0.7(6) . . . . ?
C38 C13 C14 N2 -179.3(5) . . . . ?
C12 C13 C14 C15 170.4(5) . . . . ?
C38 C13 C14 C15 -8.2(9) . . . . ?
N2 C14 C15 O1 153.2(5) . . . . ?
C13 C14 C15 O1 -16.3(9) . . . . ?
N2 C14 C15 C16 -28.8(8) . . . . ?
C13 C14 C15 C16 161.7(5) . . . . ?
C19 N3 C16 C17 3.1(5) . . . . ?
C3 N3 C16 C17 -168.1(4) . . . . ?
C19 N3 C16 C15 -169.6(5) . . . . ?
C3 N3 C16 C15 19.2(8) . . . . ?
O1 C15 C16 C17 8.1(8) . . . . ?
C14 C15 C16 C17 -169.9(5) . . . . ?
O1 C15 C16 N3 179.7(5) . . . . ?
C14 C15 C16 N3 1.7(8) . . . . ?
N3 C16 C17 C18 -0.7(5) . . . . ?
C15 C16 C17 C18 172.3(5) . . . . ?
N3 C16 C17 C40 177.9(4) . . . . ?
C15 C16 C17 C40 -9.1(8) . . . . ?
C16 C17 C18 C19 -1.9(6) . . . . ?
C40 C17 C18 C19 179.4(4) . . . . ?
C16 C17 C18 C42 172.2(5) . . . . ?
C40 C17 C18 C42 -6.5(8) . . . . ?
C17 C18 C19 N3 3.8(5) . . . . ?
C42 C18 C19 N3 -170.0(5) . . . . ?
C17 C18 C19 C20 -178.9(5) . . . . ?
C42 C18 C19 C20 7.3(9) . . . . ?
C16 N3 C19 C18 -4.2(5) . . . . ?
C3 N3 C19 C18 167.8(4) . . . . ?
C16 N3 C19 C20 178.0(4) . . . . ?
C3 N3 C19 C20 -10.0(6) . . . . ?
C4 N4 C20 C21 168.4(4) . . . . ?
C23 N4 C20 C21 -5.0(5) . . . . ?
C4 N4 C20 C19 -12.4(7) . . . . ?
C23 N4 C20 C19 174.2(4) . . . . ?
C18 C19 C20 N4 -161.4(5) . . . . ?
N3 C19 C20 N4 15.6(7) . . . . ?
C18 C19 C20 C21 17.6(10) . . . . ?
N3 C19 C20 C21 -165.4(5) . . . . ?
N4 C20 C21 C22 5.1(5) . . . . ?
C19 C20 C21 C22 -173.9(6) . . . . ?
N4 C20 C21 C44 -166.6(5) . . . . ?
C19 C20 C21 C44 14.4(10) . . . . ?
C20 C21 C22 C23 -3.4(6) . . . . ?
C44 C21 C22 C23 168.6(5) . . . . ?
C20 C21 C22 C46 -176.9(5) . . . . ?
C44 C21 C22 C46 -4.8(8) . . . . ?
C20 N4 C23 C22 2.9(5) . . . . ?
C4 N4 C23 C22 -170.3(4) . . . . ?
C20 N4 C23 C24 -177.9(4) . . . . ?
C4 N4 C23 C24 8.9(7) . . . . ?
C21 C22 C23 N4 0.4(5) . . . . ?
C46 C22 C23 N4 173.7(5) . . . . ?
C21 C22 C23 C24 -178.5(6) . . . . ?
C46 C22 C23 C24 -5.2(10) . . . . ?
C5 N5 C24 C23 8.3(7) . . . . ?
C27 N5 C24 C23 -179.1(4) . . . . ?
C5 N5 C24 C25 -170.5(5) . . . . ?
C27 N5 C24 C25 2.0(6) . . . . ?
N4 C23 C24 N5 -11.3(7) . . . . ?
C22 C23 C24 N5 167.6(6) . . . . ?
N4 C23 C24 C25 167.0(6) . . . . ?
C22 C23 C24 C25 -14.2(12) . . . . ?
N5 C24 C25 C26 -0.9(6) . . . . ?
C23 C24 C25 C26 -179.3(6) . . . . ?
N5 C24 C25 C148 -165.9(10) . . . . ?
C23 C24 C25 C148 15.7(15) . . . . ?
N5 C24 C25 C48 163.4(7) . . . . ?
C23 C24 C25 C48 -15.0(11) . . . . ?
C149 C148 C25 C26 102.5(11) . . . . ?
C149 C148 C25 C24 -93.3(14) . . . . ?
C49 C48 C25 C26 -91.2(10) . . . . ?
C49 C48 C25 C24 107.5(9) . . . . ?
C24 C25 C26 C27 -0.5(7) . . . . ?
C148 C25 C26 C27 167.7(8) . . . . ?
C48 C25 C26 C27 -163.8(7) . . . . ?
C24 C25 C26 C50 171.9(5) . . . . ?
C148 C25 C26 C50 -20.0(11) . . . . ?
C48 C25 C26 C50 8.6(11) . . . . ?
C5 N5 C27 C28 -7.9(7) . . . . ?
C24 N5 C27 C28 179.4(4) . . . . ?
C5 N5 C27 C26 170.4(4) . . . . ?
C24 N5 C27 C26 -2.3(6) . . . . ?
C25 C26 C27 C28 179.4(6) . . . . ?
C50 C26 C27 C28 7.2(11) . . . . ?
C25 C26 C27 N5 1.6(6) . . . . ?
C50 C26 C27 N5 -170.6(6) . . . . ?
C6 N6 C28 C27 -3.3(7) . . . . ?
C31 N6 C28 C27 172.9(4) . . . . ?
C6 N6 C28 C29 177.4(4) . . . . ?
C31 N6 C28 C29 -6.5(5) . . . . ?
N5 C27 C28 N6 6.9(7) . . . . ?
C26 C27 C28 N6 -170.6(6) . . . . ?
N5 C27 C28 C29 -174.1(5) . . . . ?
C26 C27 C28 C29 8.4(11) . . . . ?
N6 C28 C29 C30 5.9(5) . . . . ?
C27 C28 C29 C30 -173.2(6) . . . . ?
N6 C28 C29 C52 -166.3(5) . . . . ?
C27 C28 C29 C52 14.6(10) . . . . ?
C28 C29 C30 C31 -3.4(6) . . . . ?
C52 C29 C30 C31 168.9(5) . . . . ?
C28 C29 C30 C54 -178.0(5) . . . . ?
C52 C29 C30 C54 -5.7(8) . . . . ?
C6 N6 C31 C7 -1.7(7) . . . . ?
C28 N6 C31 C7 -177.8(4) . . . . ?
C6 N6 C31 C30 -179.4(4) . . . . ?
C28 N6 C31 C30 4.5(5) . . . . ?
N1 C7 C31 N6 -8.6(6) . . . . ?
C8 C7 C31 N6 175.4(5) . . . . ?
N1 C7 C31 C30 168.2(5) . . . . ?
C8 C7 C31 C30 -7.8(11) . . . . ?
C29 C30 C31 N6 -0.5(5) . . . . ?
C54 C30 C31 N6 174.1(5) . . . . ?
C29 C30 C31 C7 -177.5(5) . . . . ?
C54 C30 C31 C7 -2.9(9) . . . . ?
C9 C8 C32 C33 106.1(6) . . . . ?
C7 C8 C32 C33 -62.6(7) . . . . ?
C8 C9 C34 C35 -116.8(7) . . . . ?
C10 C9 C34 C35 56.7(8) . . . . ?
C11 C12 C36 C37 95.1(6) . . . . ?
C13 C12 C36 C37 -71.3(6) . . . . ?
C14 C13 C38 C39 93.6(6) . . . . ?
C12 C13 C38 C39 -84.8(6) . . . . ?
C18 C17 C40 C41 102.5(6) . . . . ?
C16 C17 C40 C41 -76.0(6) . . . . ?
C17 C18 C42 C43 -109.7(6) . . . . ?
C19 C18 C42 C43 63.2(7) . . . . ?
C22 C21 C44 C45 -117.3(6) . . . . ?
C20 C21 C44 C45 53.1(7) . . . . ?
C21 C22 C46 C47 88.7(7) . . . . ?
C23 C22 C46 C47 -83.6(7) . . . . ?
C25 C26 C50 C51 -103.1(7) . . . . ?
C27 C26 C50 C51 68.0(9) . . . . ?
C30 C29 C52 C53 -104.6(6) . . . . ?
C28 C29 C52 C53 66.5(8) . . . . ?
C29 C30 C54 C55 103.2(6) . . . . ?
C31 C30 C54 C55 -70.5(7) . . . . ?

#==============================================================================

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


