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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_Ph
_audit_block_doi                 10.5517/ccdc.csd.cc2m1483
_database_code_depnum_ccdc_archive 'CCDC 2414164'
loop_
_audit_author_name
_audit_author_address
'Tianshu Yang'
;FUJIAN NORMAL UNIVERSITY
China
;
_audit_update_record             
;
2025-02-12 deposited with the CCDC.	2025-02-27 downloaded from the CCDC.
;
_audit_creation_date             2025-02-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C59 H55 N15 O3, 3(C3 H3), C H Cl3, H2 O, 1.2[CHCl3]'
_chemical_formula_sum            'C70.20 H68.20 Cl6.60 N15 O4'
_chemical_formula_weight         1419.96
_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 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.2295(3)
_cell_length_b                   15.4768(3)
_cell_length_c                   17.3417(4)
_cell_angle_alpha                70.136(2)
_cell_angle_beta                 79.294(2)
_cell_angle_gamma                85.330(2)
_cell_volume                     3528.67(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    19965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.9950
_cell_measurement_theta_min      2.3890
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1477
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.6
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46596
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.017
_diffrn_reflns_theta_min         2.389
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9502
_reflns_number_total             13676
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         13676
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0881
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1711P)²+3.1247P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2705
_refine_ls_wR_factor_ref         0.2954
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4A \\sim O4-H4B
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C23(H23), C40(H40), C57(H57), C63(H63)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C15(H15), C19(H19), C20(H20), C21(H21),
 C27(H27), C29(H29), C30(H30), C32(H32), C36(H36), C37(H37), C38(H38), C44(H44),
  C46(H46), C47(H47), C49(H49), C53(H53), C54(H54), C55(H55), N9(H9), C60(H60),
 C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.9928(3) 0.5540(4) 0.2791(2) 0.0599(11) Uani 1 1 d . . . . .
H1A H 1.016719 0.509808 0.250423 0.090 Uiso 1 1 calc R U . . .
H1B H 1.034562 0.552286 0.318593 0.090 Uiso 1 1 calc R U . . .
H1C H 0.992198 0.615922 0.238162 0.090 Uiso 1 1 calc R U . . .
C2 C 0.8907(2) 0.5289(3) 0.3261(2) 0.0471(9) Uani 1 1 d . . . . .
C3 C 0.8204(2) 0.5263(3) 0.2652(2) 0.0463(9) Uani 1 1 d . . . . .
C4 C 0.8859(2) 0.4309(3) 0.3960(2) 0.0482(9) Uani 1 1 d . . . . .
C5 C 0.8452(2) 0.5993(3) 0.3708(2) 0.0463(8) Uani 1 1 d . . . . .
C6 C 0.8623(3) 0.5561(3) 0.1722(2) 0.0520(10) Uani 1 1 d . . . . .
H6A H 0.812520 0.554379 0.140616 0.078 Uiso 1 1 calc R U . . .
H6B H 0.915103 0.514135 0.162580 0.078 Uiso 1 1 calc R U . . .
H6C H 0.886180 0.618693 0.154020 0.078 Uiso 1 1 calc R U . . .
C7 C 0.9808(3) 0.3776(3) 0.4066(3) 0.0580(10) Uani 1 1 d . . . . .
H7A H 1.008682 0.366159 0.354806 0.087 Uiso 1 1 calc R U . . .
H7B H 0.969354 0.318880 0.451858 0.087 Uiso 1 1 calc R U . . .
H7C H 1.024981 0.413705 0.419940 0.087 Uiso 1 1 calc R U . . .
C8 C 0.9053(3) 0.6834(3) 0.3563(2) 0.0562(10) Uani 1 1 d . . . . .
H8A H 0.916411 0.719484 0.296945 0.084 Uiso 1 1 calc R U . . .
H8B H 0.966822 0.662764 0.374829 0.084 Uiso 1 1 calc R U . . .
H8C H 0.870945 0.721433 0.387972 0.084 Uiso 1 1 calc R U . . .
C9 C 0.7870(2) 0.4297(3) 0.2970(2) 0.0481(9) Uani 1 1 d . . . . .
C10 C 0.7282(3) 0.3891(3) 0.2630(2) 0.0517(10) Uani 1 1 d . . . . .
H10 H 0.705005 0.424892 0.213559 0.062 Uiso 1 1 calc R U . . .
C11 C 0.7038(3) 0.2997(3) 0.2994(2) 0.0515(9) Uani 1 1 d . . . . .
H11 H 0.665073 0.272759 0.274947 0.062 Uiso 1 1 calc R U . . .
C12 C 0.7359(3) 0.2475(3) 0.3729(2) 0.0492(9) Uani 1 1 d . . . . .
C13 C 0.7929(3) 0.2864(3) 0.4095(2) 0.0510(9) Uani 1 1 d . . . . .
H13 H 0.813622 0.250811 0.460183 0.061 Uiso 1 1 calc R U . . .
C14 C 0.8186(2) 0.3767(3) 0.3714(2) 0.0462(9) Uani 1 1 d . . . . .
C15 C 0.6412(3) 0.1084(3) 0.3958(2) 0.0508(9) Uani 1 1 d . . . . .
H15 H 0.593396 0.133326 0.362216 0.061 Uiso 1 1 calc R U . . .
C16 C 0.6535(3) 0.0189(3) 0.4427(2) 0.0536(9) Uani 1 1 d . . . . .
C17 C 0.5947(3) -0.0600(3) 0.4547(2) 0.0532(9) Uani 1 1 d . . . . .
C18 C 0.4703(3) -0.1134(3) 0.4183(2) 0.0530(9) Uani 1 1 d . . . . .
C19 C 0.4807(3) -0.2021(3) 0.4719(3) 0.0577(10) Uani 1 1 d . . . . .
H19 H 0.440420 -0.250006 0.475905 0.069 Uiso 1 1 calc R U . . .
C20 C 0.5529(3) -0.2181(3) 0.5198(3) 0.0592(10) Uani 1 1 d . . . . .
H20 H 0.562485 -0.277559 0.557923 0.071 Uiso 1 1 calc R U . . .
C21 C 0.6105(3) -0.1467(3) 0.5115(3) 0.0579(10) Uani 1 1 d . . . . .
H21 H 0.659918 -0.156344 0.543743 0.069 Uiso 1 1 calc R U . . .
C22 C 0.3911(3) -0.0914(3) 0.3667(3) 0.0560(10) Uani 1 1 d . . . . .
C23 C 0.2991(4) 0.0284(3) 0.2771(3) 0.0710(13) Uani 1 1 d . . . . .
H23 H 0.255606 -0.024011 0.289786 0.085 Uiso 1 1 calc R U . . .
C24 C 0.3380(5) 0.0587(6) 0.1854(4) 0.119(3) Uani 1 1 d . . . . .
H24A H 0.284972 0.078378 0.154027 0.178 Uiso 1 1 calc R U . . .
H24B H 0.373160 0.007473 0.171362 0.178 Uiso 1 1 calc R U . . .
H24C H 0.381178 0.110136 0.171048 0.178 Uiso 1 1 calc R U . . .
C25 C 0.2413(4) 0.1029(4) 0.3045(4) 0.0915(18) Uani 1 1 d . . . . .
H25A H 0.276940 0.160230 0.281442 0.137 Uiso 1 1 calc R U . . .
H25B H 0.229660 0.084058 0.365401 0.137 Uiso 1 1 calc R U . . .
H25C H 0.180034 0.112572 0.284443 0.137 Uiso 1 1 calc R U . . .
C26 C 0.8259(2) 0.5426(3) 0.4617(2) 0.0443(8) Uani 1 1 d . . . . .
C27 C 0.7910(2) 0.5757(3) 0.5270(2) 0.0432(8) Uani 1 1 d . . . . .
H27 H 0.777069 0.639275 0.517136 0.052 Uiso 1 1 calc R U . . .
C28 C 0.7773(2) 0.5125(3) 0.6071(2) 0.0438(8) Uani 1 1 d . . . . .
C29 C 0.7979(3) 0.4199(3) 0.6222(2) 0.0495(9) Uani 1 1 d . . . . .
H29 H 0.788735 0.378103 0.677559 0.059 Uiso 1 1 calc R U . . .
C30 C 0.8322(3) 0.3883(3) 0.5558(2) 0.0497(9) Uani 1 1 d . . . . .
H30 H 0.846336 0.324798 0.565503 0.060 Uiso 1 1 calc R U . . .
C31 C 0.8454(2) 0.4499(3) 0.4760(2) 0.0464(8) Uani 1 1 d . . . . .
C32 C 0.7261(2) 0.4983(3) 0.7578(2) 0.0445(8) Uani 1 1 d . . . . .
H32 H 0.739087 0.435040 0.784833 0.053 Uiso 1 1 calc R U . . .
C33 C 0.6881(3) 0.5619(3) 0.7941(2) 0.0470(8) Uani 1 1 d . . . . .
C34 C 0.6567(2) 0.5481(3) 0.8831(2) 0.0473(9) Uani 1 1 d . . . . .
C35 C 0.6201(2) 0.4463(3) 1.0151(2) 0.0483(9) Uani 1 1 d . . . . .
C36 C 0.5975(3) 0.5169(3) 1.0486(2) 0.0524(10) Uani 1 1 d . . . . .
H36 H 0.576553 0.503736 1.106667 0.063 Uiso 1 1 calc R U . . .
C37 C 0.6064(3) 0.6061(3) 0.9957(2) 0.0569(11) Uani 1 1 d . . . . .
H37 H 0.592219 0.655455 1.017180 0.068 Uiso 1 1 calc R U . . .
C38 C 0.6359(3) 0.6241(3) 0.9111(2) 0.0530(9) Uani 1 1 d . . . . .
H38 H 0.641918 0.685322 0.873425 0.064 Uiso 1 1 calc R U . . .
C39 C 0.6086(2) 0.3485(3) 1.0713(2) 0.0518(9) Uani 1 1 d . . . . .
C40 C 0.6078(4) 0.1872(4) 1.0824(3) 0.0728(13) Uani 1 1 d . . . . .
H40 H 0.554731 0.181138 1.130505 0.087 Uiso 1 1 calc R U . . .
C41 C 0.5799(5) 0.1348(4) 1.0315(4) 0.0919(17) Uani 1 1 d . . . . .
H41A H 0.517411 0.157335 1.015849 0.138 Uiso 1 1 calc R U . . .
H41B H 0.576186 0.069229 1.064270 0.138 Uiso 1 1 calc R U . . .
H41C H 0.627899 0.143561 0.981102 0.138 Uiso 1 1 calc R U . . .
C42 C 0.6998(5) 0.1500(5) 1.1183(5) 0.109(2) Uani 1 1 d . . . . .
H42A H 0.688816 0.088170 1.158809 0.164 Uiso 1 1 calc R U . . .
H42B H 0.717369 0.190685 1.145809 0.164 Uiso 1 1 calc R U . . .
H42C H 0.751670 0.147495 1.073200 0.164 Uiso 1 1 calc R U . . .
C43 C 0.7393(2) 0.5907(3) 0.2804(2) 0.0470(9) Uani 1 1 d . . . . .
C44 C 0.6572(2) 0.6107(3) 0.2433(2) 0.0495(9) Uani 1 1 d . . . . .
H44 H 0.648700 0.584194 0.203111 0.059 Uiso 1 1 calc R U . . .
C45 C 0.5898(3) 0.6691(3) 0.2662(2) 0.0533(10) Uani 1 1 d . . . . .
C46 C 0.6011(3) 0.7104(3) 0.3234(2) 0.0594(11) Uani 1 1 d . . . . .
H46 H 0.553356 0.751503 0.337777 0.071 Uiso 1 1 calc R U . . .
C47 C 0.6834(3) 0.6907(3) 0.3593(2) 0.0558(10) Uani 1 1 d . . . . .
H47 H 0.692523 0.718467 0.398462 0.067 Uiso 1 1 calc R U . . .
C48 C 0.7519(3) 0.6304(3) 0.3378(2) 0.0481(9) Uani 1 1 d . . . . .
C49 C 0.4214(3) 0.7278(3) 0.2530(2) 0.0507(9) Uani 1 1 d . . . . .
H49 H 0.405180 0.750063 0.298615 0.061 Uiso 1 1 calc R U . . .
C50 C 0.3653(3) 0.7289(3) 0.1964(2) 0.0508(9) Uani 1 1 d . . . . .
C51 C 0.2668(3) 0.7638(3) 0.1899(2) 0.0486(9) Uani 1 1 d . . . . .
C52 C 0.1314(3) 0.7650(3) 0.1350(3) 0.0503(9) Uani 1 1 d . . . . .
C53 C 0.0844(3) 0.8259(3) 0.1728(3) 0.0581(10) Uani 1 1 d . . . . .
H53 H 0.021506 0.847685 0.164454 0.070 Uiso 1 1 calc R U . . .
C54 C 0.1311(3) 0.8539(3) 0.2226(3) 0.0614(11) Uani 1 1 d . . . . .
H54 H 0.100203 0.894617 0.250201 0.074 Uiso 1 1 calc R U . . .
C55 C 0.2238(3) 0.8223(3) 0.2322(3) 0.0562(10) Uani 1 1 d . . . . .
H55 H 0.257048 0.840231 0.266814 0.067 Uiso 1 1 calc R U . . .
C56 C 0.0811(3) 0.7286(3) 0.0832(2) 0.0497(9) Uani 1 1 d . . . . .
C57 C 0.0912(3) 0.6191(3) 0.0069(2) 0.0525(9) Uani 1 1 d . . . . .
H57 H 0.020308 0.629476 0.013668 0.063 Uiso 1 1 calc R U . . .
C58 C 0.1327(3) 0.6596(4) -0.0853(3) 0.0691(12) Uani 1 1 d . . . . .
H58A H 0.101524 0.632515 -0.117277 0.104 Uiso 1 1 calc R U . . .
H58B H 0.201633 0.646103 -0.093821 0.104 Uiso 1 1 calc R U . . .
H58C H 0.121750 0.726344 -0.104129 0.104 Uiso 1 1 calc R U . . .
C59 C 0.1111(3) 0.5174(3) 0.0396(3) 0.0590(11) Uani 1 1 d . . . . .
H59A H 0.081409 0.486735 0.009457 0.089 Uiso 1 1 calc R U . . .
H59B H 0.084454 0.493554 0.098993 0.089 Uiso 1 1 calc R U . . .
H59C H 0.180332 0.505700 0.031651 0.089 Uiso 1 1 calc R U . . .
N1 N 0.7121(2) 0.1543(3) 0.40752(19) 0.0527(8) Uani 1 1 d . . . . .
N2 N 0.7656(2) 0.0936(3) 0.4607(2) 0.0595(9) Uani 1 1 d . . . . .
N3 N 0.7288(2) 0.0121(3) 0.4814(2) 0.0590(9) Uani 1 1 d . . . . .
N4 N 0.3774(3) -0.0058(3) 0.3251(2) 0.0616(9) Uani 1 1 d . . . . .
N5 N 0.7411(2) 0.5447(2) 0.67535(17) 0.0441(7) Uani 1 1 d . . . . .
N6 N 0.7124(3) 0.6340(3) 0.6605(2) 0.0596(9) Uani 1 1 d . . . . .
N7 N 0.6805(3) 0.6442(2) 0.7326(2) 0.0573(8) Uani 1 1 d . . . . .
N8 N 0.6509(2) 0.4616(2) 0.93330(18) 0.0470(7) Uani 1 1 d . . . . .
N9 N 0.6169(2) 0.2850(3) 1.0346(2) 0.0587(9) Uani 1 1 d . . . . .
H9 H 0.628234 0.302335 0.979899 0.070 Uiso 1 1 calc R U . . .
N10 N 0.5040(2) 0.6885(3) 0.22986(19) 0.0537(8) Uani 1 1 d . . . . .
N11 N 0.5012(2) 0.6660(3) 0.1617(2) 0.0600(9) Uani 1 1 d . . . . .
N12 N 0.4157(2) 0.6909(3) 0.1415(2) 0.0567(9) Uani 1 1 d . . . . .
N13 N 0.2215(2) 0.7341(2) 0.1426(2) 0.0491(7) Uani 1 1 d . . . . .
N14 N 0.1295(2) 0.6649(2) 0.05591(19) 0.0494(7) Uani 1 1 d . . . . .
N15 N 0.5253(2) -0.0432(2) 0.4093(2) 0.0532(8) Uani 1 1 d . . . . .
O1 O 0.3432(2) -0.1561(2) 0.36779(19) 0.0632(8) Uani 1 1 d . . . . .
O2 O 0.5924(2) 0.3308(2) 1.14778(16) 0.0618(8) Uani 1 1 d . . . . .
O3 O -0.00094(19) 0.7560(2) 0.0720(2) 0.0617(8) Uani 1 1 d . . . . .
C60 C 0.5839(3) 0.4508(3) 0.5194(3) 0.0616(11) Uani 1 1 d . . . . .
H60 H 0.640060 0.416218 0.533865 0.074 Uiso 1 1 calc R U . . .
C61 C 0.5523(3) 0.4533(4) 0.4509(3) 0.0699(12) Uani 1 1 d . . . . .
H61 H 0.588396 0.422774 0.415647 0.084 Uiso 1 1 calc R U . . .
C62 C 0.4666(3) 0.5002(4) 0.4295(3) 0.0734(13) Uani 1 1 d . . . . .
H62 H 0.443390 0.498939 0.381941 0.088 Uiso 1 1 calc R U . . .
C63 C 1.0788(4) 0.0968(4) 0.5435(4) 0.0842(16) Uani 1 1 d . . . . .
H63 H 1.107332 0.043040 0.527174 0.101 Uiso 1 1 calc R U . . .
Cl1 Cl 1.10178(12) 0.08011(11) 0.64297(10) 0.0972(5) Uani 1 1 d . . . . .
Cl2 Cl 0.95551(11) 0.10014(12) 0.54113(17) 0.1264(8) Uani 1 1 d . . . . .
Cl3 Cl 1.13462(9) 0.19556(9) 0.47081(9) 0.0781(4) Uani 1 1 d . . . . .
C64 C 0.9703(6) 0.1580(5) 0.2609(5) 0.112(2) Uani 1 1 d . . . . .
H64 H 0.922538 0.121373 0.302280 0.134 Uiso 1 1 calc R U . . .
C65 C 1.0086(8) 0.1351(6) 0.1884(6) 0.128(3) Uani 1 1 d . . . . .
H65 H 0.987823 0.081518 0.181953 0.154 Uiso 1 1 calc R U . . .
C66 C 1.0737(6) 0.1884(7) 0.1291(5) 0.116(3) Uani 1 1 d . . . . .
H66 H 1.095191 0.172793 0.080170 0.139 Uiso 1 1 calc R U . . .
C67 C 1.1112(6) 0.2645(6) 0.1349(7) 0.130(3) Uani 1 1 d . . . . .
H67 H 1.157495 0.301272 0.092067 0.156 Uiso 1 1 calc R U . . .
C68 C 1.0754(6) 0.2852(5) 0.2109(4) 0.0973(19) Uani 1 1 d . . . . .
H68 H 1.100123 0.334514 0.221380 0.117 Uiso 1 1 calc R U . . .
C69 C 1.0015(6) 0.2288(5) 0.2693(4) 0.105(2) Uani 1 1 d . . . . .
H69 H 0.974170 0.244878 0.317035 0.126 Uiso 1 1 calc R U . . .
O4 O 0.4721(2) 0.2049(2) 0.2769(2) 0.0702(8) Uani 1 1 d D . . . .
H4A H 0.524(4) 0.242(4) 0.227(3) 0.099(18) Uiso 1 1 d D . . . .
H4B H 0.426(6) 0.262(5) 0.276(6) 0.18(4) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.537(5) . ?
C2 C3 1.596(4) . ?
C2 C4 1.585(6) . ?
C2 C5 1.574(5) . ?
C3 C6 1.533(5) . ?
C3 C9 1.490(6) . ?
C3 C43 1.508(5) . ?
C4 C7 1.531(5) . ?
C4 C14 1.526(5) . ?
C4 C31 1.515(5) . ?
C5 C8 1.539(6) . ?
C5 C26 1.507(5) . ?
C5 C48 1.521(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.401(5) . ?
C9 C14 1.406(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.356(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.394(5) . ?
C12 C13 1.397(5) . ?
C12 N1 1.404(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.376(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.363(6) . ?
C15 N1 1.363(5) . ?
C16 C17 1.470(6) . ?
C16 N3 1.345(5) . ?
C17 C21 1.399(6) . ?
C17 N15 1.331(5) . ?
C18 C19 1.387(6) . ?
C18 C22 1.512(5) . ?
C18 N15 1.340(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.394(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.380(7) . ?
C21 H21 0.9500 . ?
C22 N4 1.294(6) . ?
C22 O1 1.250(5) . ?
C23 H23 1.0000 . ?
C23 C24 1.505(8) . ?
C23 C25 1.519(7) . ?
C23 N4 1.471(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.391(5) . ?
C26 C31 1.384(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.391(5) . ?
C28 C29 1.383(6) . ?
C28 N5 1.430(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.392(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.377(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.366(5) . ?
C32 N5 1.349(4) . ?
C33 C34 1.471(5) . ?
C33 N7 1.367(5) . ?
C34 C38 1.410(5) . ?
C34 N8 1.325(5) . ?
C35 C36 1.393(5) . ?
C35 C39 1.500(6) . ?
C35 N8 1.348(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.374(6) . ?
C37 H37 0.9500 . ?
C37 C38 1.386(5) . ?
C38 H38 0.9500 . ?
C39 N9 1.328(5) . ?
C39 O2 1.239(4) . ?
C40 H40 1.0000 . ?
C40 C41 1.506(7) . ?
C40 C42 1.539(7) . ?
C40 N9 1.461(6) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.400(4) . ?
C43 C48 1.378(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.362(5) . ?
C45 C46 1.387(5) . ?
C45 N10 1.441(4) . ?
C46 H46 0.9500 . ?
C46 C47 1.392(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.383(5) . ?
C49 H49 0.9500 . ?
C49 C50 1.370(5) . ?
C49 N10 1.337(5) . ?
C50 C51 1.471(5) . ?
C50 N12 1.352(5) . ?
C51 C55 1.387(5) . ?
C51 N13 1.341(4) . ?
C52 C53 1.384(6) . ?
C52 C56 1.514(5) . ?
C52 N13 1.345(4) . ?
C53 H53 0.9500 . ?
C53 C54 1.375(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.389(5) . ?
C55 H55 0.9500 . ?
C56 N14 1.325(5) . ?
C56 O3 1.236(4) . ?
C57 H57 1.0000 . ?
C57 C58 1.526(6) . ?
C57 C59 1.503(6) . ?
C57 N14 1.472(4) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
N1 N2 1.367(4) . ?
N2 N3 1.313(5) . ?
N5 N6 1.360(5) . ?
N6 N7 1.306(4) . ?
N9 H9 0.8800 . ?
N10 N11 1.350(4) . ?
N11 N12 1.319(4) . ?
C60 H60 0.9500 . ?
C60 C61 1.333(7) . ?
C60 C62 1.418(7) 2_666 ?
C61 H61 0.9500 . ?
C61 C62 1.411(7) . ?
C62 H62 0.9500 . ?
C63 H63 1.0000 . ?
C63 Cl1 1.744(6) . ?
C63 Cl2 1.759(5) . ?
C63 Cl3 1.752(7) . ?
C64 H64 0.9500 . ?
C64 C65 1.422(11) . ?
C64 C69 1.277(10) . ?
C65 H65 0.9500 . ?
C65 C66 1.338(12) . ?
C66 H66 0.9500 . ?
C66 C67 1.373(11) . ?
C67 H67 0.9500 . ?
C67 C68 1.451(12) . ?
C68 H68 0.9500 . ?
C68 C69 1.431(11) . ?
C69 H69 0.9500 . ?
O4 H4A 1.06(5) . ?
O4 H4B 1.05(5) . ?

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
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C3 111.7(3) . . ?
C1 C2 C4 112.7(3) . . ?
C1 C2 C5 112.7(3) . . ?
C4 C2 C3 106.3(3) . . ?
C5 C2 C3 106.7(3) . . ?
C5 C2 C4 106.3(3) . . ?
C6 C3 C2 116.4(3) . . ?
C9 C3 C2 104.6(3) . . ?
C9 C3 C6 111.6(3) . . ?
C9 C3 C43 110.4(3) . . ?
C43 C3 C2 103.8(3) . . ?
C43 C3 C6 109.7(3) . . ?
C7 C4 C2 116.6(3) . . ?
C14 C4 C2 104.5(3) . . ?
C14 C4 C7 109.5(3) . . ?
C31 C4 C2 104.6(3) . . ?
C31 C4 C7 108.5(3) . . ?
C31 C4 C14 113.2(3) . . ?
C8 C5 C2 116.5(3) . . ?
C26 C5 C2 104.4(3) . . ?
C26 C5 C8 110.9(3) . . ?
C26 C5 C48 110.6(3) . . ?
C48 C5 C2 104.3(3) . . ?
C48 C5 C8 109.9(3) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C3 128.0(3) . . ?
C10 C9 C14 118.8(4) . . ?
C14 C9 C3 113.1(3) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10 119.4 . . ?
C10 C11 H11 120.2 . . ?
C10 C11 C12 119.7(3) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 120.7(4) . . ?
C11 C12 N1 118.2(3) . . ?
C13 C12 N1 121.0(3) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.2(3) . . ?
C14 C13 H13 120.4 . . ?
C9 C14 C4 111.2(4) . . ?
C13 C14 C4 128.2(3) . . ?
C13 C14 C9 120.5(3) . . ?
C16 C15 H15 127.4 . . ?
N1 C15 H15 127.4 . . ?
N1 C15 C16 105.2(3) . . ?
C15 C16 C17 128.0(3) . . ?
N3 C16 C15 109.0(4) . . ?
N3 C16 C17 123.0(4) . . ?
C21 C17 C16 121.5(3) . . ?
N15 C17 C16 116.0(4) . . ?
N15 C17 C21 122.5(4) . . ?
C19 C18 C22 119.5(4) . . ?
N15 C18 C19 124.3(4) . . ?
N15 C18 C22 116.2(4) . . ?
C18 C19 H19 121.4 . . ?
C18 C19 C20 117.1(4) . . ?
C20 C19 H19 121.4 . . ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.5(4) . . ?
C21 C20 H20 120.2 . . ?
C17 C21 H21 120.6 . . ?
C20 C21 C17 118.8(4) . . ?
C20 C21 H21 120.6 . . ?
N4 C22 C18 116.9(4) . . ?
O1 C22 C18 118.4(4) . . ?
O1 C22 N4 124.7(4) . . ?
C24 C23 H23 107.6 . . ?
C24 C23 C25 113.3(5) . . ?
C25 C23 H23 107.6 . . ?
N4 C23 H23 107.6 . . ?
N4 C23 C24 110.1(5) . . ?
N4 C23 C25 110.5(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C5 125.9(4) . . ?
C31 C26 C5 112.9(3) . . ?
C31 C26 C27 121.2(3) . . ?
C26 C27 H27 121.2 . . ?
C28 C27 C26 117.6(4) . . ?
C28 C27 H27 121.2 . . ?
C27 C28 N5 118.8(3) . . ?
C29 C28 C27 121.7(3) . . ?
C29 C28 N5 119.6(3) . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.7(3) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 H30 120.3 . . ?
C31 C30 C29 119.4(4) . . ?
C31 C30 H30 120.3 . . ?
C26 C31 C4 111.6(3) . . ?
C30 C31 C4 127.9(4) . . ?
C30 C31 C26 120.5(3) . . ?
C33 C32 H32 127.5 . . ?
N5 C32 H32 127.5 . . ?
N5 C32 C33 105.0(3) . . ?
C32 C33 C34 128.0(4) . . ?
C32 C33 N7 108.4(3) . . ?
N7 C33 C34 123.6(3) . . ?
C38 C34 C33 120.4(4) . . ?
N8 C34 C33 116.1(3) . . ?
N8 C34 C38 123.6(3) . . ?
C36 C35 C39 119.3(3) . . ?
N8 C35 C36 123.0(4) . . ?
N8 C35 C39 117.7(3) . . ?
C35 C36 H36 120.8 . . ?
C37 C36 C35 118.4(3) . . ?
C37 C36 H36 120.8 . . ?
C36 C37 H37 120.0 . . ?
C36 C37 C38 120.1(4) . . ?
C38 C37 H37 120.0 . . ?
C34 C38 H38 121.3 . . ?
C37 C38 C34 117.3(4) . . ?
C37 C38 H38 121.3 . . ?
N9 C39 C35 116.5(3) . . ?
O2 C39 C35 119.8(4) . . ?
O2 C39 N9 123.8(4) . . ?
C41 C40 H40 107.3 . . ?
C41 C40 C42 113.7(5) . . ?
C42 C40 H40 107.3 . . ?
N9 C40 H40 107.3 . . ?
N9 C40 C41 111.1(4) . . ?
N9 C40 C42 110.0(4) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C3 126.4(3) . . ?
C48 C43 C3 113.0(3) . . ?
C48 C43 C44 120.6(3) . . ?
C43 C44 H44 120.8 . . ?
C45 C44 C43 118.4(3) . . ?
C45 C44 H44 120.8 . . ?
C44 C45 C46 122.2(3) . . ?
C44 C45 N10 118.9(3) . . ?
C46 C45 N10 118.9(3) . . ?
C45 C46 H46 120.5 . . ?
C45 C46 C47 118.9(4) . . ?
C47 C46 H46 120.5 . . ?
C46 C47 H47 120.2 . . ?
C48 C47 C46 119.7(3) . . ?
C48 C47 H47 120.2 . . ?
C43 C48 C5 112.2(3) . . ?
C43 C48 C47 120.3(3) . . ?
C47 C48 C5 127.5(3) . . ?
C50 C49 H49 127.6 . . ?
N10 C49 H49 127.6 . . ?
N10 C49 C50 104.9(3) . . ?
C49 C50 C51 130.0(3) . . ?
N12 C50 C49 108.6(3) . . ?
N12 C50 C51 121.4(3) . . ?
C55 C51 C50 121.1(3) . . ?
N13 C51 C50 116.1(3) . . ?
N13 C51 C55 122.8(3) . . ?
C53 C52 C56 120.2(3) . . ?
N13 C52 C53 123.3(3) . . ?
N13 C52 C56 116.5(3) . . ?
C52 C53 H53 120.8 . . ?
C54 C53 C52 118.3(3) . . ?
C54 C53 H53 120.8 . . ?
C53 C54 H54 120.2 . . ?
C53 C54 C55 119.5(4) . . ?
C55 C54 H54 120.2 . . ?
C51 C55 C54 118.4(3) . . ?
C51 C55 H55 120.8 . . ?
C54 C55 H55 120.8 . . ?
N14 C56 C52 115.1(3) . . ?
O3 C56 C52 119.8(3) . . ?
O3 C56 N14 125.0(3) . . ?
C58 C57 H57 108.2 . . ?
C59 C57 H57 108.2 . . ?
C59 C57 C58 111.3(4) . . ?
N14 C57 H57 108.2 . . ?
N14 C57 C58 111.0(3) . . ?
N14 C57 C59 109.8(3) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C15 N1 C12 130.4(3) . . ?
C15 N1 N2 109.2(4) . . ?
N2 N1 C12 120.4(3) . . ?
N3 N2 N1 107.2(3) . . ?
N2 N3 C16 109.4(3) . . ?
C22 N4 C23 124.1(4) . . ?
C32 N5 C28 129.8(3) . . ?
C32 N5 N6 110.3(3) . . ?
N6 N5 C28 119.8(3) . . ?
N7 N6 N5 107.3(3) . . ?
N6 N7 C33 109.0(3) . . ?
C34 N8 C35 117.6(3) . . ?
C39 N9 C40 121.8(4) . . ?
C39 N9 H9 119.1 . . ?
C40 N9 H9 119.1 . . ?
C49 N10 C45 129.8(3) . . ?
C49 N10 N11 110.9(3) . . ?
N11 N10 C45 119.3(3) . . ?
N12 N11 N10 106.9(3) . . ?
N11 N12 C50 108.7(3) . . ?
C51 N13 C52 117.6(3) . . ?
C56 N14 C57 123.1(3) . . ?
C17 N15 C18 117.7(4) . . ?
C61 C60 H60 120.1 . . ?
C61 C60 C62 119.8(4) . 2_666 ?
C62 C60 H60 120.1 2_666 . ?
C60 C61 H61 119.1 . . ?
C60 C61 C62 121.8(5) . . ?
C62 C61 H61 119.1 . . ?
C60 C62 H62 120.8 2_666 . ?
C61 C62 C60 118.3(4) . 2_666 ?
C61 C62 H62 120.8 . . ?
Cl1 C63 H63 107.4 . . ?
Cl1 C63 Cl2 112.0(4) . . ?
Cl1 C63 Cl3 111.1(3) . . ?
Cl2 C63 H63 107.4 . . ?
Cl3 C63 H63 107.4 . . ?
Cl3 C63 Cl2 111.2(3) . . ?
C65 C64 H64 120.7 . . ?
C69 C64 H64 120.7 . . ?
C69 C64 C65 118.6(9) . . ?
C64 C65 H65 119.7 . . ?
C66 C65 C64 120.5(8) . . ?
C66 C65 H65 119.7 . . ?
C65 C66 H66 118.2 . . ?
C65 C66 C67 123.7(8) . . ?
C67 C66 H66 118.2 . . ?
C66 C67 H67 122.2 . . ?
C66 C67 C68 115.7(9) . . ?
C68 C67 H67 122.2 . . ?
C67 C68 H68 121.1 . . ?
C69 C68 C67 117.7(7) . . ?
C69 C68 H68 121.1 . . ?
C64 C69 C68 123.6(7) . . ?
C64 C69 H69 118.2 . . ?
C68 C69 H69 118.2 . . ?
H4A O4 H4B 95(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C6 -4.9(5) . . . . ?
C1 C2 C3 C9 118.8(4) . . . . ?
C1 C2 C3 C43 -125.5(4) . . . . ?
C1 C2 C4 C7 0.5(4) . . . . ?
C1 C2 C4 C14 -120.5(3) . . . . ?
C1 C2 C4 C31 120.3(3) . . . . ?
C1 C2 C5 C8 3.8(4) . . . . ?
C1 C2 C5 C26 -118.8(3) . . . . ?
C1 C2 C5 C48 125.0(3) . . . . ?
C2 C3 C9 C10 -176.0(3) . . . . ?
C2 C3 C9 C14 5.7(4) . . . . ?
C2 C3 C43 C44 -178.3(4) . . . . ?
C2 C3 C43 C48 1.0(4) . . . . ?
C2 C4 C14 C9 1.3(4) . . . . ?
C2 C4 C14 C13 177.2(3) . . . . ?
C2 C4 C31 C26 0.7(4) . . . . ?
C2 C4 C31 C30 -175.8(3) . . . . ?
C2 C5 C26 C27 175.8(3) . . . . ?
C2 C5 C26 C31 -5.0(4) . . . . ?
C2 C5 C48 C43 -1.6(4) . . . . ?
C2 C5 C48 C47 178.2(4) . . . . ?
C3 C2 C4 C7 123.2(3) . . . . ?
C3 C2 C4 C14 2.1(3) . . . . ?
C3 C2 C4 C31 -117.1(3) . . . . ?
C3 C2 C5 C8 -119.1(3) . . . . ?
C3 C2 C5 C26 118.3(3) . . . . ?
C3 C2 C5 C48 2.1(4) . . . . ?
C3 C9 C10 C11 -180.0(3) . . . . ?
C3 C9 C14 C4 -4.6(4) . . . . ?
C3 C9 C14 C13 179.1(3) . . . . ?
C3 C43 C44 C45 178.3(4) . . . . ?
C3 C43 C48 C5 0.3(5) . . . . ?
C3 C43 C48 C47 -179.4(4) . . . . ?
C4 C2 C3 C6 -128.2(3) . . . . ?
C4 C2 C3 C9 -4.6(3) . . . . ?
C4 C2 C3 C43 111.2(3) . . . . ?
C4 C2 C5 C8 127.8(3) . . . . ?
C4 C2 C5 C26 5.1(3) . . . . ?
C4 C2 C5 C48 -111.0(3) . . . . ?
C5 C2 C3 C6 118.7(4) . . . . ?
C5 C2 C3 C9 -117.7(3) . . . . ?
C5 C2 C3 C43 -1.9(4) . . . . ?
C5 C2 C4 C7 -123.5(3) . . . . ?
C5 C2 C4 C14 115.5(3) . . . . ?
C5 C2 C4 C31 -3.7(3) . . . . ?
C5 C26 C27 C28 179.7(3) . . . . ?
C5 C26 C31 C4 2.8(4) . . . . ?
C5 C26 C31 C30 179.6(3) . . . . ?
C6 C3 C9 C10 -49.3(5) . . . . ?
C6 C3 C9 C14 132.4(3) . . . . ?
C6 C3 C43 C44 56.7(5) . . . . ?
C6 C3 C43 C48 -124.0(4) . . . . ?
C7 C4 C14 C9 -124.3(3) . . . . ?
C7 C4 C14 C13 51.6(5) . . . . ?
C7 C4 C31 C26 125.8(4) . . . . ?
C7 C4 C31 C30 -50.8(5) . . . . ?
C8 C5 C26 C27 49.6(4) . . . . ?
C8 C5 C26 C31 -131.2(3) . . . . ?
C8 C5 C48 C43 123.9(4) . . . . ?
C8 C5 C48 C47 -56.3(5) . . . . ?
C9 C3 C43 C44 -66.7(5) . . . . ?
C9 C3 C43 C48 112.6(4) . . . . ?
C9 C10 C11 C12 1.4(6) . . . . ?
C10 C9 C14 C4 176.9(3) . . . . ?
C10 C9 C14 C13 0.6(5) . . . . ?
C10 C11 C12 C13 0.0(6) . . . . ?
C10 C11 C12 N1 -177.9(3) . . . . ?
C11 C12 C13 C14 -1.1(5) . . . . ?
C11 C12 N1 C15 -20.4(6) . . . . ?
C11 C12 N1 N2 157.7(3) . . . . ?
C12 C13 C14 C4 -174.8(3) . . . . ?
C12 C13 C14 C9 0.8(5) . . . . ?
C12 N1 N2 N3 -178.4(3) . . . . ?
C13 C12 N1 C15 161.7(4) . . . . ?
C13 C12 N1 N2 -20.2(5) . . . . ?
C14 C4 C31 C26 -112.4(4) . . . . ?
C14 C4 C31 C30 71.0(4) . . . . ?
C14 C9 C10 C11 -1.8(5) . . . . ?
C15 C16 C17 C21 -173.5(4) . . . . ?
C15 C16 C17 N15 5.6(6) . . . . ?
C15 C16 N3 N2 -0.4(5) . . . . ?
C15 N1 N2 N3 0.0(4) . . . . ?
C16 C15 N1 C12 178.0(4) . . . . ?
C16 C15 N1 N2 -0.3(4) . . . . ?
C16 C17 C21 C20 -179.9(4) . . . . ?
C16 C17 N15 C18 179.8(3) . . . . ?
C17 C16 N3 N2 -178.2(3) . . . . ?
C18 C19 C20 C21 -0.6(6) . . . . ?
C18 C22 N4 C23 -175.1(4) . . . . ?
C19 C18 C22 N4 172.2(4) . . . . ?
C19 C18 C22 O1 -7.1(5) . . . . ?
C19 C18 N15 C17 0.2(5) . . . . ?
C19 C20 C21 C17 -0.2(6) . . . . ?
C21 C17 N15 C18 -1.1(5) . . . . ?
C22 C18 C19 C20 -178.1(3) . . . . ?
C22 C18 N15 C17 179.0(3) . . . . ?
C24 C23 N4 C22 -109.0(6) . . . . ?
C25 C23 N4 C22 125.1(5) . . . . ?
C26 C5 C48 C43 -113.3(4) . . . . ?
C26 C5 C48 C47 66.5(5) . . . . ?
C26 C27 C28 C29 0.4(5) . . . . ?
C26 C27 C28 N5 -179.7(3) . . . . ?
C27 C26 C31 C4 -178.0(3) . . . . ?
C27 C26 C31 C30 -1.1(5) . . . . ?
C27 C28 C29 C30 -0.8(5) . . . . ?
C27 C28 N5 C32 -176.6(3) . . . . ?
C27 C28 N5 N6 6.1(5) . . . . ?
C28 C29 C30 C31 0.2(5) . . . . ?
C28 N5 N6 N7 178.3(3) . . . . ?
C29 C28 N5 C32 3.3(5) . . . . ?
C29 C28 N5 N6 -173.9(3) . . . . ?
C29 C30 C31 C4 177.0(3) . . . . ?
C29 C30 C31 C26 0.7(5) . . . . ?
C31 C4 C14 C9 114.5(3) . . . . ?
C31 C4 C14 C13 -69.6(5) . . . . ?
C31 C26 C27 C28 0.6(5) . . . . ?
C32 C33 C34 C38 168.0(4) . . . . ?
C32 C33 C34 N8 -11.2(5) . . . . ?
C32 C33 N7 N6 -0.3(4) . . . . ?
C32 N5 N6 N7 0.6(4) . . . . ?
C33 C32 N5 C28 -178.2(3) . . . . ?
C33 C32 N5 N6 -0.7(4) . . . . ?
C33 C34 C38 C37 179.7(3) . . . . ?
C33 C34 N8 C35 -178.4(3) . . . . ?
C34 C33 N7 N6 -178.7(3) . . . . ?
C35 C36 C37 C38 0.8(5) . . . . ?
C35 C39 N9 C40 179.6(3) . . . . ?
C36 C35 C39 N9 170.0(3) . . . . ?
C36 C35 C39 O2 -10.1(5) . . . . ?
C36 C35 N8 C34 -2.1(5) . . . . ?
C36 C37 C38 C34 -0.6(5) . . . . ?
C38 C34 N8 C35 2.4(5) . . . . ?
C39 C35 C36 C37 -178.5(3) . . . . ?
C39 C35 N8 C34 176.9(3) . . . . ?
C41 C40 N9 C39 156.7(4) . . . . ?
C42 C40 N9 C39 -76.6(6) . . . . ?
C43 C3 C9 C10 72.9(4) . . . . ?
C43 C3 C9 C14 -105.3(3) . . . . ?
C43 C44 C45 C46 1.4(7) . . . . ?
C43 C44 C45 N10 -178.6(4) . . . . ?
C44 C43 C48 C5 179.7(4) . . . . ?
C44 C43 C48 C47 -0.1(6) . . . . ?
C44 C45 C46 C47 -0.8(7) . . . . ?
C44 C45 N10 C49 165.6(4) . . . . ?
C44 C45 N10 N11 -14.7(6) . . . . ?
C45 C46 C47 C48 -0.2(7) . . . . ?
C45 N10 N11 N12 180.0(4) . . . . ?
C46 C45 N10 C49 -14.4(7) . . . . ?
C46 C45 N10 N11 165.3(4) . . . . ?
C46 C47 C48 C5 -179.1(4) . . . . ?
C46 C47 C48 C43 0.6(7) . . . . ?
C48 C5 C26 C27 -72.6(4) . . . . ?
C48 C5 C26 C31 106.6(4) . . . . ?
C48 C43 C44 C45 -1.0(6) . . . . ?
C49 C50 C51 C55 15.9(7) . . . . ?
C49 C50 C51 N13 -162.8(4) . . . . ?
C49 C50 N12 N11 0.0(5) . . . . ?
C49 N10 N11 N12 -0.3(5) . . . . ?
C50 C49 N10 C45 -180.0(4) . . . . ?
C50 C49 N10 N11 0.3(5) . . . . ?
C50 C51 C55 C54 179.1(4) . . . . ?
C50 C51 N13 C52 -179.7(4) . . . . ?
C51 C50 N12 N11 179.8(4) . . . . ?
C52 C53 C54 C55 1.3(7) . . . . ?
C52 C56 N14 C57 178.0(4) . . . . ?
C53 C52 C56 N14 -174.4(4) . . . . ?
C53 C52 C56 O3 2.8(6) . . . . ?
C53 C52 N13 C51 0.5(6) . . . . ?
C53 C54 C55 C51 0.8(7) . . . . ?
C55 C51 N13 C52 1.7(6) . . . . ?
C56 C52 C53 C54 176.9(4) . . . . ?
C56 C52 N13 C51 -178.5(4) . . . . ?
C58 C57 N14 C56 101.5(4) . . . . ?
C59 C57 N14 C56 -135.0(4) . . . . ?
N1 C12 C13 C14 176.7(3) . . . . ?
N1 C15 C16 C17 178.0(4) . . . . ?
N1 C15 C16 N3 0.4(4) . . . . ?
N1 N2 N3 C16 0.2(4) . . . . ?
N3 C16 C17 C21 3.9(6) . . . . ?
N3 C16 C17 N15 -177.1(4) . . . . ?
N5 C28 C29 C30 179.3(3) . . . . ?
N5 C32 C33 C34 178.9(3) . . . . ?
N5 C32 C33 N7 0.6(4) . . . . ?
N5 N6 N7 C33 -0.2(4) . . . . ?
N7 C33 C34 C38 -13.9(5) . . . . ?
N7 C33 C34 N8 166.9(3) . . . . ?
N8 C34 C38 C37 -1.1(5) . . . . ?
N8 C35 C36 C37 0.6(5) . . . . ?
N8 C35 C39 N9 -9.1(4) . . . . ?
N8 C35 C39 O2 170.8(3) . . . . ?
N10 C45 C46 C47 179.2(4) . . . . ?
N10 C49 C50 C51 -180.0(4) . . . . ?
N10 C49 C50 N12 -0.2(5) . . . . ?
N10 N11 N12 C50 0.1(5) . . . . ?
N12 C50 C51 C55 -163.9(4) . . . . ?
N12 C50 C51 N13 17.5(6) . . . . ?
N13 C51 C55 C54 -2.4(7) . . . . ?
N13 C52 C53 C54 -2.0(7) . . . . ?
N13 C52 C56 N14 4.6(6) . . . . ?
N13 C52 C56 O3 -178.2(4) . . . . ?
N15 C17 C21 C20 1.1(6) . . . . ?
N15 C18 C19 C20 0.6(6) . . . . ?
N15 C18 C22 N4 -6.6(5) . . . . ?
N15 C18 C22 O1 174.0(3) . . . . ?
O1 C22 N4 C23 4.2(7) . . . . ?
O2 C39 N9 C40 -0.3(6) . . . . ?
O3 C56 N14 C57 1.0(7) . . . . ?
C60 C61 C62 C60 3.1(8) . . . 2_666 ?
C62 C60 C61 C62 -3.1(8) 2_666 . . . ?
C64 C65 C66 C67 3.2(12) . . . . ?
C65 C64 C69 C68 -2.0(11) . . . . ?
C65 C66 C67 C68 -0.2(10) . . . . ?
C66 C67 C68 C69 -3.6(9) . . . . ?
C67 C68 C69 C64 4.9(10) . . . . ?
C69 C64 C65 C66 -2.1(12) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 135 electrons were 
found in a volume of 515Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
1.2[CHCl3] per formula unit 
which account for 139 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.115 0.000 0.000 475.0 134.8 '2.4 CHCl3'
2 0.493 0.572 0.724 19.8 0.0 ?
3 0.507 0.428 0.276 19.8 0.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_CYH
_audit_block_doi                 10.5517/ccdc.csd.cc2mbpvj
_database_code_depnum_ccdc_archive 'CCDC 2423358'
loop_
_audit_author_name
_audit_author_address
'Tianshu Yang'
;FUJIAN NORMAL UNIVERSITY
China
;
_audit_update_record             
;
2025-02-12 deposited with the CCDC.	2025-02-27 downloaded from the CCDC.
;
_audit_creation_date             2025-02-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C59 H57 N15 O3), 3.5(C6 H12), 3(C1 H1 Cl3), 2.1[CHCl3], 2.1[CHCl3]'
_chemical_formula_sum            'C146.20 H163.20 Cl21.60 N30 O6'
_chemical_formula_weight         3202.38
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   22.8874(11)
_cell_length_b                   22.8874(11)
_cell_length_c                   57.200(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     25949(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    6314
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      66.3210
_cell_measurement_theta_min      2.4190
_shelx_estimated_absorpt_T_max   0.716
_shelx_estimated_absorpt_T_min   0.653
_exptl_absorpt_coefficient_mu    3.585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             9994
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            29664
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        66.564
_diffrn_reflns_theta_max         66.564
_diffrn_reflns_theta_min         2.359
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00 -27.00   0.50    3.50    --  -97.00  54.00-179.00   52
  2  ω    -53.00 -24.00   0.50    3.50    --  -97.00  45.00 -90.00   58
  3  ω    -69.00 -27.00   0.50    3.50    --  -97.00  61.00 -60.00   84
  4  ω    -54.00 -29.00   0.50    3.50    --  -97.00  45.00 -60.00   50
  5  ω    -54.00 -27.00   0.50    3.50    --  -97.00  45.00 120.00   54
  6  ω    -98.00 -39.00   0.50    3.50    --  -97.00 117.00 154.00  118
  7  ω     66.00 114.00   0.50    0.88    --   46.22 141.00  50.00   96
  8  ω    112.00 163.00   0.50    3.50    --  107.47  54.00-179.00  102
  9  ω    -24.00  21.00   0.50    0.88    --   46.22 -19.00 -30.00   90
 10  ω   -118.00 -93.00   0.50    0.88    --  -46.22-141.00  -7.00   50
 11  ω    -28.00  11.00   0.50    0.88    --   46.22 -19.00  60.00   78
 12  ω     40.00  68.00   0.50    3.50    --  107.47-113.00-114.00   56
 13  ω     76.00 108.00   0.50    3.50    --  107.47-113.00-114.00   64
 14  ω     61.00  92.00   0.50    3.50    --  107.47 -95.00 -90.00   62
 15  ω     50.00  79.00   0.50    3.50    --  107.47 -81.00  48.00   58
 16  ω    106.00 133.00   0.50    3.50    --  107.47 -81.00  48.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0159408000
_diffrn_orient_matrix_UB_12      0.0280516000
_diffrn_orient_matrix_UB_13      0.0251292000
_diffrn_orient_matrix_UB_21      -0.0479422667
_diffrn_orient_matrix_UB_22      -0.0711899333
_diffrn_orient_matrix_UB_23      0.0096397667
_diffrn_orient_matrix_UB_31      0.0589909333
_diffrn_orient_matrix_UB_32      -0.0140533333
_diffrn_orient_matrix_UB_33      0.0010913667
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5921
_reflns_number_total             9828
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.456
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         9828
_refine_ls_number_restraints     390
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.1446
_refine_ls_restrained_S_all      1.515
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3752
_refine_ls_wR_factor_ref         0.4041
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C45-C44 \\sim C44-C43 \\sim C48-C43 \\sim C48-C47 \\sim C47-C46 \\sim C46-C45
 with sigma of 0.02
 C43-C45 \\sim C44-C46 \\sim C45-C47 \\sim C46-C48 \\sim C47-C43 \\sim C48-C44
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C43A \\sim C44A
\\sim C45A \\sim C46A \\sim C47A \\sim C48A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
C40 \\sim C41 \\sim C42 \\sim C41A \\sim C42A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C50 \\sim C50A \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim Cl1A \\sim Cl2A \\sim Cl3A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C19 \\sim C20 \\sim C21 \\sim C20A \\sim C21A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Same fragment restrains
{C19, C20A, C21A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C19, C20, C21}
{C40, C41A, C42A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C40, C41, C42}
{C43A, C44A, C45A, C46A, C47A, C48A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C43, C44, C45, C46, C47, C48}
{C50A, Cl1A, Cl2A, Cl3A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C50, Cl1, Cl2, Cl3}
5. Others
 Sof(H19A)=Sof(H40A)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44C)=
 Sof(H44D)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=
 Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=
 Sof(H49C)=Sof(H49D)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21A)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=
 Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=Sof(H40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=
 Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=FVAR(1)
 Sof(C50A)=Sof(H50A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=1-FVAR(2)
 Sof(C50)=Sof(H50)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(2)
 Fixed Sof: H1A(0.33333) H1B(0.33333) H1C(0.33333) H22A(0.33333) H22B(0.33333)
 H22C(0.33333)
6.a Ternary CH refined with riding coordinates:
 C19(H19), C19(H19A), C40(H40), C40(H40A), C50(H50), C50A(H50A)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C49(H49A,H49B), C43A(H43C,H43D), C44A(H44C,H44D),
 C45A(H45C,H45D), C46A(H46C,H46D), C47A(H47C,H47D), C48A(H48C,H48D), C49A(H49C,
 H49D)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C11(H11), C15(H15), C16(H16), C17(H17), N5(H5),
 C27(H27), C28(H28), C30(H30), C32(H32), C36(H36), C37(H37), C38(H38), N10(H10)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C20A(H20D,H20E,H20F), C21A(H21D,H21E,H21F), C41A(H41D,H41E,H41F),
 C42A(H42D,H42E,H42F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.666667 0.333333 0.20994(13) 0.101(2) Uani 1 3 d S T P . .
H1A H 0.661617 0.370940 0.204228 0.151 Uiso 0.3333 1 calc R U P A -1
H1B H 0.629060 0.290676 0.204228 0.151 Uiso 0.3333 1 calc R U P A -1
H1C H 0.709324 0.338383 0.204228 0.151 Uiso 0.3333 1 calc R U P A -1
C2 C 0.666667 0.333333 0.23677(12) 0.0877(17) Uani 1 3 d S T P . .
C3 C 0.7184(2) 0.4050(2) 0.24728(7) 0.0850(10) Uani 1 1 d . . . . .
C4 C 0.7631(2) 0.4614(2) 0.22969(8) 0.0957(11) Uani 1 1 d . . . . .
H4A H 0.791185 0.447909 0.220912 0.144 Uiso 1 1 calc R U . . .
H4B H 0.792073 0.503291 0.238217 0.144 Uiso 1 1 calc R U . . .
H4C H 0.734231 0.468719 0.218829 0.144 Uiso 1 1 calc R U . . .
C5 C 0.67502(19) 0.42412(18) 0.26184(6) 0.0782(9) Uani 1 1 d . . . . .
C6 C 0.6955(2) 0.48420(19) 0.27383(7) 0.0836(10) Uani 1 1 d . . . . .
H6 H 0.739923 0.521169 0.271780 0.100 Uiso 1 1 calc R U . . .
C7 C 0.65125(19) 0.48992(18) 0.28870(7) 0.0821(9) Uani 1 1 d . . . . .
H7 H 0.664330 0.530860 0.296814 0.099 Uiso 1 1 calc R U . . .
C8 C 0.58617(19) 0.43371(19) 0.29159(6) 0.0802(9) Uani 1 1 d . . . . .
C9 C 0.56329(19) 0.37579(19) 0.27857(6) 0.0810(9) Uani 1 1 d . . . . .
H9 H 0.518217 0.339582 0.279969 0.097 Uiso 1 1 calc R U . . .
C10 C 0.60881(19) 0.37223(19) 0.26323(6) 0.0788(9) Uani 1 1 d . . . . .
C11 C 0.56180(19) 0.47878(18) 0.32795(7) 0.0783(9) Uani 1 1 d . . . . .
H11 H 0.604376 0.517700 0.330837 0.094 Uiso 1 1 calc R U . . .
C12 C 0.5052(2) 0.45372(19) 0.34141(7) 0.0831(10) Uani 1 1 d . . . . .
C13 C 0.4953(2) 0.47785(19) 0.36386(7) 0.0800(9) Uani 1 1 d . . . . .
C14 C 0.5411(2) 0.5500(2) 0.39454(7) 0.0891(11) Uani 1 1 d . . . . .
C15 C 0.4832(3) 0.5231(3) 0.40607(9) 0.1088(14) Uani 1 1 d . . . . .
H15 H 0.480662 0.540470 0.420882 0.131 Uiso 1 1 calc R U . . .
C16 C 0.4260(3) 0.4690(3) 0.39616(10) 0.1174(15) Uani 1 1 d . . . . .
H16 H 0.384034 0.448941 0.404186 0.141 Uiso 1 1 calc R U . . .
C17 C 0.4309(3) 0.4452(2) 0.37486(9) 0.0996(12) Uani 1 1 d . . . . .
H17 H 0.392977 0.408378 0.367652 0.120 Uiso 1 1 calc R U . . .
C18 C 0.6027(3) 0.6110(2) 0.40421(8) 0.0997(13) Uani 1 1 d . . . . .
C19 C 0.7234(3) 0.6918(3) 0.40058(11) 0.1246(17) Uani 1 1 d D U . . .
H19 H 0.723362 0.700082 0.417735 0.149 Uiso 0.576(8) 1 calc R U P B 1
H19A H 0.713561 0.709710 0.415067 0.149 Uiso 0.424(8) 1 calc R U P B 2
C20 C 0.7843(7) 0.6853(8) 0.3942(3) 0.146(5) Uani 0.576(8) 1 d D U P B 1
H20A H 0.786874 0.682576 0.377144 0.219 Uiso 0.576(8) 1 calc R U P B 1
H20B H 0.779864 0.644278 0.401290 0.219 Uiso 0.576(8) 1 calc R U P B 1
H20C H 0.825374 0.724695 0.399970 0.219 Uiso 0.576(8) 1 calc R U P B 1
C21 C 0.7283(8) 0.7502(8) 0.3870(3) 0.121(4) Uani 0.576(8) 1 d D U P B 1
H21A H 0.769196 0.791786 0.391645 0.181 Uiso 0.576(8) 1 calc R U P B 1
H21B H 0.688644 0.754606 0.390199 0.181 Uiso 0.576(8) 1 calc R U P B 1
H21C H 0.730402 0.742472 0.370226 0.181 Uiso 0.576(8) 1 calc R U P B 1
N1 N 0.54411(15) 0.43629(15) 0.30967(5) 0.0785(8) Uani 1 1 d . . . . .
N2 N 0.47889(17) 0.38721(18) 0.31152(6) 0.0926(9) Uani 1 1 d . . . . .
N3 N 0.45522(17) 0.39725(17) 0.33081(6) 0.0909(9) Uani 1 1 d . . . . .
N4 N 0.54880(18) 0.52845(16) 0.37314(6) 0.0847(8) Uani 1 1 d . . . . .
N5 N 0.6609(2) 0.63139(18) 0.39386(7) 0.1028(11) Uani 1 1 d . . . . .
H5 H 0.662314 0.607185 0.382145 0.123 Uiso 1 1 calc R U . . .
O1 O 0.5960(2) 0.63827(19) 0.42211(7) 0.1245(11) Uani 1 1 d . . . . .
C22 C 0.333333 0.666667 0.28995(19) 0.139(4) Uani 1 3 d S T P . .
H22A H 0.311822 0.691725 0.284234 0.209 Uiso 0.3333 1 calc R U P C -1
H22B H 0.308275 0.620097 0.284234 0.209 Uiso 0.3333 1 calc R U P C -1
H22C H 0.379903 0.688178 0.284234 0.209 Uiso 0.3333 1 calc R U P C -1
C23 C 0.333333 0.666667 0.31775(18) 0.117(3) Uani 1 3 d S T P . .
C24 C 0.3491(3) 0.6123(3) 0.32782(10) 0.1124(14) Uani 1 1 d . . . . .
C25 C 0.3602(3) 0.5681(3) 0.31016(12) 0.1346(19) Uani 1 1 d . . . . .
H25A H 0.317136 0.536251 0.302858 0.202 Uiso 1 1 calc R U . . .
H25B H 0.378609 0.543116 0.318277 0.202 Uiso 1 1 calc R U . . .
H25C H 0.392080 0.596854 0.298096 0.202 Uiso 1 1 calc R U . . .
C26 C 0.4117(3) 0.6540(3) 0.34274(10) 0.1091(13) Uani 1 1 d . . . . .
C27 C 0.4480(3) 0.6301(3) 0.35570(11) 0.1175(15) Uani 1 1 d . . . . .
H27 H 0.437512 0.584467 0.354382 0.141 Uiso 1 1 calc R U . . .
C28 C 0.4982(3) 0.6737(3) 0.37011(13) 0.1298(18) Uani 1 1 d . . . . .
H28 H 0.522758 0.658348 0.379127 0.156 Uiso 1 1 calc R U . . .
C29 C 0.5136(3) 0.7401(3) 0.37170(12) 0.1208(16) Uani 1 1 d . . . . .
C30 C 0.4827(3) 0.7650(3) 0.35784(11) 0.1141(15) Uani 1 1 d . . . . .
H30 H 0.496896 0.811771 0.357981 0.137 Uiso 1 1 calc R U . . .
C31 C 0.4306(3) 0.7212(3) 0.34365(10) 0.1086(13) Uani 1 1 d . . . . .
C32 C 0.5837(3) 0.7686(3) 0.40800(12) 0.1216(16) Uani 1 1 d . . . . .
H32 H 0.572806 0.724853 0.413139 0.146 Uiso 1 1 calc R U . . .
C33 C 0.6237(4) 0.8273(3) 0.41837(16) 0.149(3) Uani 1 1 d . . . . .
C34 C 0.6559(4) 0.8392(3) 0.44184(15) 0.144(2) Uani 1 1 d . . . . .
C35 C 0.6756(3) 0.7915(3) 0.47375(12) 0.1242(18) Uani 1 1 d . . . . .
C36 C 0.7063(4) 0.8517(5) 0.48512(16) 0.164(3) Uani 1 1 d . . . . .
H36 H 0.723868 0.855332 0.500424 0.196 Uiso 1 1 calc R U . . .
C37 C 0.7114(6) 0.9090(5) 0.4737(3) 0.204(5) Uani 1 1 d . . . . .
H37 H 0.732664 0.951675 0.481223 0.245 Uiso 1 1 calc R U . . .
C38 C 0.6867(5) 0.9028(4) 0.4525(2) 0.181(4) Uani 1 1 d . . . . .
H38 H 0.689585 0.940673 0.444635 0.217 Uiso 1 1 calc R U . . .
C39 C 0.6698(3) 0.7306(3) 0.48452(11) 0.1196(17) Uani 1 1 d . . . . .
C40 C 0.6423(5) 0.6137(4) 0.47903(14) 0.155(2) Uani 1 1 d D U . . .
H40 H 0.655547 0.619112 0.495893 0.186 Uiso 0.576(8) 1 calc R U P B 1
H40A H 0.642475 0.611214 0.496482 0.186 Uiso 0.424(8) 1 calc R U P B 2
C41 C 0.6878(8) 0.5939(10) 0.4662(4) 0.160(5) Uani 0.576(8) 1 d D U P B 1
H41A H 0.696353 0.564049 0.476062 0.240 Uiso 0.576(8) 1 calc R U P B 1
H41B H 0.730688 0.634562 0.462438 0.240 Uiso 0.576(8) 1 calc R U P B 1
H41C H 0.665801 0.570416 0.451655 0.240 Uiso 0.576(8) 1 calc R U P B 1
C42 C 0.5682(7) 0.5570(12) 0.4776(4) 0.198(8) Uani 0.576(8) 1 d D U P B 1
H42A H 0.556503 0.543021 0.461239 0.297 Uiso 0.576(8) 1 calc R U P B 1
H42B H 0.538990 0.573521 0.483582 0.297 Uiso 0.576(8) 1 calc R U P B 1
H42C H 0.561881 0.518438 0.486933 0.297 Uiso 0.576(8) 1 calc R U P B 1
N6 N 0.5625(3) 0.7847(2) 0.38905(11) 0.1352(17) Uani 1 1 d . . . . .
N7 N 0.5866(4) 0.8499(3) 0.38715(15) 0.179(3) Uani 1 1 d . . . . .
N8 N 0.6232(4) 0.8758(3) 0.40573(18) 0.192(3) Uani 1 1 d . . . . .
N9 N 0.6512(2) 0.7845(2) 0.45209(10) 0.1224(15) Uani 1 1 d . . . . .
N10 N 0.6449(3) 0.6753(2) 0.47173(8) 0.1189(13) Uani 1 1 d . . . . .
H10 H 0.628803 0.676074 0.457835 0.143 Uiso 1 1 calc R U . . .
O2 O 0.6908(2) 0.7336(3) 0.50540(8) 0.1423(14) Uani 1 1 d . . . . .
C43 C 0.6330(7) 0.7354(6) 0.3218(2) 0.205(6) Uani 0.576(8) 1 d D U P B 1
H43A H 0.673863 0.758926 0.311885 0.246 Uiso 0.576(8) 1 calc R U P B 1
H43B H 0.645351 0.754929 0.337652 0.246 Uiso 0.576(8) 1 calc R U P B 1
C44 C 0.6132(4) 0.6631(4) 0.32311(16) 0.115(3) Uani 0.576(8) 1 d D U P B 1
H44A H 0.588634 0.644333 0.337947 0.138 Uiso 0.576(8) 1 calc R U P B 1
H44B H 0.654690 0.659737 0.323585 0.138 Uiso 0.576(8) 1 calc R U P B 1
C45 C 0.5698(9) 0.6206(6) 0.3032(2) 0.130(4) Uani 0.576(8) 1 d D U P B 1
H45A H 0.591838 0.597243 0.295985 0.156 Uiso 0.576(8) 1 calc R U P B 1
H45B H 0.526051 0.585534 0.309680 0.156 Uiso 0.576(8) 1 calc R U P B 1
C46 C 0.5565(8) 0.6578(7) 0.2847(2) 0.174(4) Uani 0.576(8) 1 d D U P B 1
H46A H 0.589692 0.666946 0.272103 0.209 Uiso 0.576(8) 1 calc R U P B 1
H46B H 0.511568 0.626087 0.278150 0.209 Uiso 0.576(8) 1 calc R U P B 1
C47 C 0.5574(8) 0.7200(6) 0.2890(3) 0.147(4) Uani 0.576(8) 1 d D U P B 1
H47A H 0.511219 0.712145 0.286587 0.177 Uiso 0.576(8) 1 calc R U P B 1
H47B H 0.586861 0.753262 0.277160 0.177 Uiso 0.576(8) 1 calc R U P B 1
C48 C 0.5804(7) 0.7500(5) 0.31215(19) 0.125(3) Uani 0.576(8) 1 d D U P B 1
H48A H 0.541395 0.731858 0.322965 0.150 Uiso 0.576(8) 1 calc R U P B 1
H48B H 0.599464 0.799474 0.311095 0.150 Uiso 0.576(8) 1 calc R U P B 1
C49 C 0.6475(6) 0.3961(6) 0.33557(16) 0.061(3) Uani 0.576(8) 1 d . . P B 1
H49A H 0.643704 0.408340 0.351871 0.073 Uiso 0.576(8) 1 calc R U P B 1
H49B H 0.638504 0.425326 0.325201 0.073 Uiso 0.576(8) 1 calc R U P B 1
C50 C 0.5919(7) 0.6984(6) 0.5440(3) 0.160(4) Uani 0.488(6) 1 d D U P D 1
H50 H 0.636139 0.717705 0.535725 0.192 Uiso 0.488(6) 1 calc R U P D 1
Cl1 Cl 0.5653(8) 0.6150(4) 0.5505(2) 0.203(4) Uani 0.488(6) 1 d D U P D 1
Cl2 Cl 0.5326(3) 0.6999(3) 0.52458(11) 0.193(2) Uani 0.488(6) 1 d D U P D 1
Cl3 Cl 0.6013(4) 0.7478(4) 0.56651(11) 0.231(4) Uani 0.488(6) 1 d D U P D 1
C43A C 0.5977(7) 0.6953(7) 0.3064(3) 0.166(4) Uani 0.424(8) 1 d D U P B 2
H43C H 0.633309 0.709658 0.294336 0.199 Uiso 0.424(8) 1 calc R U P B 2
H43D H 0.619694 0.716265 0.321414 0.199 Uiso 0.424(8) 1 calc R U P B 2
C44A C 0.5615(10) 0.6192(7) 0.3088(3) 0.132(5) Uani 0.424(8) 1 d D U P B 2
H44C H 0.595080 0.604654 0.311444 0.158 Uiso 0.424(8) 1 calc R U P B 2
H44D H 0.531332 0.605528 0.322586 0.158 Uiso 0.424(8) 1 calc R U P B 2
C45A C 0.5210(7) 0.5850(6) 0.2875(2) 0.142(4) Uani 0.424(8) 1 d D U P B 2
H45C H 0.473982 0.553266 0.292383 0.171 Uiso 0.424(8) 1 calc R U P B 2
H45D H 0.539251 0.558049 0.280378 0.171 Uiso 0.424(8) 1 calc R U P B 2
C46A C 0.5200(12) 0.6315(9) 0.2694(3) 0.209(7) Uani 0.424(8) 1 d D U P B 2
H46C H 0.554758 0.638391 0.257722 0.250 Uiso 0.424(8) 1 calc R U P B 2
H46D H 0.475882 0.606469 0.261368 0.250 Uiso 0.424(8) 1 calc R U P B 2
C47A C 0.5296(6) 0.6959(7) 0.2746(2) 0.125(4) Uani 0.424(8) 1 d D U P B 2
H47C H 0.487602 0.696059 0.270520 0.150 Uiso 0.424(8) 1 calc R U P B 2
H47D H 0.565702 0.729085 0.264315 0.150 Uiso 0.424(8) 1 calc R U P B 2
C48A C 0.5475(7) 0.7202(7) 0.2994(2) 0.104(3) Uani 0.424(8) 1 d D U P B 2
H48C H 0.507110 0.699923 0.309568 0.125 Uiso 0.424(8) 1 calc R U P B 2
H48D H 0.569526 0.769981 0.300292 0.125 Uiso 0.424(8) 1 calc R U P B 2
C49A C 0.6272(10) 0.3732(8) 0.3392(2) 0.063(4) Uani 0.424(8) 1 d . . P B 2
H49C H 0.603071 0.397513 0.334970 0.076 Uiso 0.424(8) 1 calc R U P B 2
H49D H 0.629228 0.371117 0.356416 0.076 Uiso 0.424(8) 1 calc R U P B 2
C50A C 0.6029(7) 0.6967(6) 0.5508(2) 0.152(3) Uani 0.512(6) 1 d D U P D 2
H50A H 0.637608 0.712867 0.538164 0.183 Uiso 0.512(6) 1 calc R U P D 2
Cl1A Cl 0.5476(6) 0.6111(4) 0.5469(2) 0.182(3) Uani 0.512(6) 1 d D U P D 2
Cl2A Cl 0.5551(2) 0.7375(2) 0.54783(11) 0.170(2) Uani 0.512(6) 1 d D U P D 2
Cl3A Cl 0.64225(19) 0.7185(2) 0.57658(6) 0.1488(15) Uani 0.512(6) 1 d D U P D 2
C20A C 0.7730(9) 0.6713(9) 0.4070(3) 0.123(5) Uani 0.424(8) 1 d D U P B 2
H20D H 0.781278 0.649915 0.393564 0.185 Uiso 0.424(8) 1 calc R U P B 2
H20E H 0.755331 0.639196 0.420043 0.185 Uiso 0.424(8) 1 calc R U P B 2
H20F H 0.815356 0.711133 0.411753 0.185 Uiso 0.424(8) 1 calc R U P B 2
C21A C 0.7454(10) 0.7444(9) 0.3829(3) 0.115(4) Uani 0.424(8) 1 d D U P B 2
H21D H 0.781902 0.786868 0.389212 0.173 Uiso 0.424(8) 1 calc R U P B 2
H21E H 0.707419 0.750459 0.378418 0.173 Uiso 0.424(8) 1 calc R U P B 2
H21F H 0.761738 0.731428 0.369098 0.173 Uiso 0.424(8) 1 calc R U P B 2
C41A C 0.7057(8) 0.6163(12) 0.4691(6) 0.144(5) Uani 0.424(8) 1 d D U P B 2
H41D H 0.704431 0.573690 0.472382 0.216 Uiso 0.424(8) 1 calc R U P B 2
H41E H 0.745797 0.653610 0.476319 0.216 Uiso 0.424(8) 1 calc R U P B 2
H41F H 0.707336 0.623299 0.452122 0.216 Uiso 0.424(8) 1 calc R U P B 2
C42A C 0.5795(8) 0.5504(11) 0.4690(5) 0.156(6) Uani 0.424(8) 1 d D U P B 2
H42D H 0.575245 0.557019 0.452294 0.234 Uiso 0.424(8) 1 calc R U P B 2
H42E H 0.538949 0.543597 0.477214 0.234 Uiso 0.424(8) 1 calc R U P B 2
H42F H 0.584571 0.510725 0.471178 0.234 Uiso 0.424(8) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.535(11) . ?
C2 C3 1.585(5) 3_665 ?
C2 C3 1.585(5) . ?
C2 C3 1.585(5) 2_655 ?
C3 C4 1.550(6) . ?
C3 C5 1.518(6) . ?
C3 C10 1.523(5) 3_665 ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.391(6) . ?
C5 C10 1.383(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.378(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.409(6) . ?
C8 C9 1.376(5) . ?
C8 N1 1.434(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.395(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.362(6) . ?
C11 N1 1.345(5) . ?
C12 C13 1.460(6) . ?
C12 N3 1.367(5) . ?
C13 C17 1.423(6) . ?
C13 N4 1.306(5) . ?
C14 C15 1.324(7) . ?
C14 C18 1.508(7) . ?
C14 N4 1.363(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.396(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.362(7) . ?
C17 H17 0.9500 . ?
C18 N5 1.313(7) . ?
C18 O1 1.248(6) . ?
C19 H19 1.0000 . ?
C19 H19A 1.0000 . ?
C19 C20 1.517(12) . ?
C19 C21 1.503(11) . ?
C19 N5 1.459(7) . ?
C19 C20A 1.474(12) . ?
C19 C21A 1.458(12) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N1 N2 1.351(5) . ?
N2 N3 1.299(5) . ?
N5 H5 0.8800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 C23 1.590(15) . ?
C23 C24 1.568(7) . ?
C23 C24 1.568(7) 2_665 ?
C23 C24 1.568(7) 3_565 ?
C24 C25 1.538(8) . ?
C24 C26 1.525(8) . ?
C24 C31 1.504(7) 3_565 ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.413(8) . ?
C26 C31 1.374(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.359(9) . ?
C28 H28 0.9500 . ?
C28 C29 1.381(8) . ?
C29 C30 1.363(8) . ?
C29 N6 1.462(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.375(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.328(8) . ?
C32 N6 1.313(8) . ?
C33 C34 1.489(11) . ?
C33 N8 1.330(9) . ?
C34 C38 1.400(10) . ?
C34 N9 1.339(8) . ?
C35 C36 1.360(9) . ?
C35 C39 1.467(9) . ?
C35 N9 1.336(8) . ?
C36 H36 0.9500 . ?
C36 C37 1.418(15) . ?
C37 H37 0.9500 . ?
C37 C38 1.311(14) . ?
C38 H38 0.9500 . ?
C39 N10 1.318(7) . ?
C39 O2 1.276(7) . ?
C40 H40 1.0000 . ?
C40 H40A 1.0000 . ?
C40 C41 1.517(15) . ?
C40 C42 1.538(14) . ?
C40 N10 1.444(9) . ?
C40 C41A 1.531(15) . ?
C40 C42A 1.553(15) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N6 N7 1.311(7) . ?
N7 N8 1.299(10) . ?
N10 H10 0.8800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.483(11) . ?
C43 C48 1.506(11) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.503(12) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.483(11) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.435(11) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.463(11) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C49 1.718(9) 18_545 ?
C49 C49 1.718(9) 17 ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50 1.0000 . ?
C50 Cl1 1.728(11) . ?
C50 Cl2 1.767(14) . ?
C50 Cl3 1.655(14) . ?
C43A H43C 0.9900 . ?
C43A H43D 0.9900 . ?
C43A C44A 1.514(13) . ?
C43A C48A 1.569(13) . ?
C44A H44C 0.9900 . ?
C44A H44D 0.9900 . ?
C44A C45A 1.493(15) . ?
C45A H45C 0.9900 . ?
C45A H45D 0.9900 . ?
C45A C46A 1.495(13) . ?
C46A H46C 0.9900 . ?
C46A H46D 0.9900 . ?
C46A C47A 1.410(13) . ?
C47A H47C 0.9900 . ?
C47A H47D 0.9900 . ?
C47A C48A 1.503(14) . ?
C48A H48C 0.9900 . ?
C48A H48D 0.9900 . ?
C49A C49A 1.708(12) 18_545 ?
C49A C49A 1.708(12) 17 ?
C49A H49C 0.9900 . ?
C49A H49D 0.9900 . ?
C50A H50A 1.0000 . ?
C50A Cl1A 1.736(11) . ?
C50A Cl2A 1.767(14) . ?
C50A Cl3A 1.666(14) . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C41A H41D 0.9800 . ?
C41A H41E 0.9800 . ?
C41A H41F 0.9800 . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 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
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C3 112.3(3) . . ?
C1 C2 C3 112.3(3) . 2_655 ?
C1 C2 C3 112.3(3) . 3_665 ?
C3 C2 C3 106.5(3) 3_665 2_655 ?
C3 C2 C3 106.5(3) 3_665 . ?
C3 C2 C3 106.5(3) . 2_655 ?
C4 C3 C2 117.1(4) . . ?
C5 C3 C2 104.4(3) . . ?
C5 C3 C4 111.7(3) . . ?
C5 C3 C10 109.8(3) . 3_665 ?
C10 C3 C2 104.2(3) 3_665 . ?
C10 C3 C4 109.2(3) 3_665 . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C3 127.5(4) . . ?
C10 C5 C3 112.2(3) . . ?
C10 C5 C6 120.2(4) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 C5 119.8(4) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 H7 120.7 . . ?
C6 C7 C8 118.5(3) . . ?
C8 C7 H7 120.7 . . ?
C7 C8 N1 118.2(3) . . ?
C9 C8 C7 122.4(4) . . ?
C9 C8 N1 119.4(4) . . ?
C8 C9 H9 121.3 . . ?
C8 C9 C10 117.5(4) . . ?
C10 C9 H9 121.3 . . ?
C5 C10 C3 112.3(3) . 2_655 ?
C5 C10 C9 121.0(3) . . ?
C9 C10 C3 126.7(4) . 2_655 ?
C12 C11 H11 127.6 . . ?
N1 C11 H11 127.6 . . ?
N1 C11 C12 104.8(3) . . ?
C11 C12 C13 129.3(4) . . ?
C11 C12 N3 108.5(4) . . ?
N3 C12 C13 122.2(4) . . ?
C17 C13 C12 120.5(4) . . ?
N4 C13 C12 116.0(3) . . ?
N4 C13 C17 123.5(4) . . ?
C15 C14 C18 120.1(4) . . ?
C15 C14 N4 124.0(4) . . ?
N4 C14 C18 115.8(4) . . ?
C14 C15 H15 120.4 . . ?
C14 C15 C16 119.1(5) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.3(5) . . ?
C17 C16 H16 120.4 . . ?
C13 C17 H17 121.4 . . ?
C16 C17 C13 117.2(5) . . ?
C16 C17 H17 121.4 . . ?
N5 C18 C14 118.5(4) . . ?
O1 C18 C14 118.3(5) . . ?
O1 C18 N5 123.2(5) . . ?
C20 C19 H19 110.2 . . ?
C21 C19 H19 110.2 . . ?
C21 C19 C20 107.4(9) . . ?
N5 C19 H19 110.2 . . ?
N5 C19 H19A 106.9 . . ?
N5 C19 C20 110.9(7) . . ?
N5 C19 C21 108.0(9) . . ?
N5 C19 C20A 108.1(8) . . ?
C20A C19 H19A 106.9 . . ?
C21A C19 H19A 106.9 . . ?
C21A C19 N5 111.7(11) . . ?
C21A C19 C20A 115.7(11) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C11 N1 C8 128.7(3) . . ?
C11 N1 N2 110.4(3) . . ?
N2 N1 C8 120.5(3) . . ?
N3 N2 N1 107.7(3) . . ?
N2 N3 C12 108.5(3) . . ?
C13 N4 C14 116.9(4) . . ?
C18 N5 C19 124.0(4) . . ?
C18 N5 H5 118.0 . . ?
C19 N5 H5 118.0 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
C24 C23 C22 111.5(4) 3_565 . ?
C24 C23 C22 111.5(4) 2_665 . ?
C24 C23 C22 111.5(4) . . ?
C24 C23 C24 107.3(4) 3_565 . ?
C24 C23 C24 107.3(4) 2_665 . ?
C24 C23 C24 107.3(4) 3_565 2_665 ?
C25 C24 C23 117.4(6) . . ?
C26 C24 C23 103.0(4) . . ?
C26 C24 C25 111.5(5) . . ?
C31 C24 C23 104.8(4) 3_565 . ?
C31 C24 C25 110.6(5) 3_565 . ?
C31 C24 C26 108.8(4) 3_565 . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C24 126.9(5) . . ?
C31 C26 C24 113.2(5) . . ?
C31 C26 C27 119.8(5) . . ?
C26 C27 H27 120.7 . . ?
C28 C27 C26 118.6(5) . . ?
C28 C27 H27 120.7 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.3(5) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 N6 119.9(5) . . ?
C30 C29 C28 121.5(6) . . ?
C30 C29 N6 118.6(5) . . ?
C29 C30 H30 120.7 . . ?
C29 C30 C31 118.7(5) . . ?
C31 C30 H30 120.7 . . ?
C26 C31 C24 111.4(5) . 2_665 ?
C26 C31 C30 120.8(5) . . ?
C30 C31 C24 127.8(5) . 2_665 ?
C33 C32 H32 127.7 . . ?
N6 C32 H32 127.7 . . ?
N6 C32 C33 104.5(5) . . ?
C32 C33 C34 128.1(6) . . ?
C32 C33 N8 108.1(6) . . ?
N8 C33 C34 123.1(6) . . ?
C38 C34 C33 122.1(7) . . ?
N9 C34 C33 114.9(5) . . ?
N9 C34 C38 122.9(7) . . ?
C36 C35 C39 121.2(7) . . ?
N9 C35 C36 122.5(7) . . ?
N9 C35 C39 116.2(5) . . ?
C35 C36 H36 120.7 . . ?
C35 C36 C37 118.6(8) . . ?
C37 C36 H36 120.7 . . ?
C36 C37 H37 120.2 . . ?
C38 C37 C36 119.6(7) . . ?
C38 C37 H37 120.2 . . ?
C34 C38 H38 120.6 . . ?
C37 C38 C34 118.8(8) . . ?
C37 C38 H38 120.6 . . ?
N10 C39 C35 117.9(5) . . ?
O2 C39 C35 119.3(5) . . ?
O2 C39 N10 122.8(6) . . ?
C41 C40 H40 107.2 . . ?
C41 C40 C42 110.8(12) . . ?
C42 C40 H40 107.2 . . ?
N10 C40 H40 107.2 . . ?
N10 C40 H40A 110.1 . . ?
N10 C40 C41 116.9(12) . . ?
N10 C40 C42 107.3(13) . . ?
N10 C40 C41A 106.2(13) . . ?
N10 C40 C42A 111.8(12) . . ?
C41A C40 H40A 110.1 . . ?
C41A C40 C42A 108.5(11) . . ?
C42A C40 H40A 110.1 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C32 N6 C29 128.7(5) . . ?
N7 N6 C29 118.6(5) . . ?
N7 N6 C32 112.5(6) . . ?
N8 N7 N6 105.1(6) . . ?
N7 N8 C33 109.7(6) . . ?
C35 N9 C34 117.5(5) . . ?
C39 N10 C40 124.3(5) . . ?
C39 N10 H10 117.8 . . ?
C40 N10 H10 117.8 . . ?
H43A C43 H43B 107.4 . . ?
C44 C43 H43A 108.3 . . ?
C44 C43 H43B 108.3 . . ?
C44 C43 C48 115.8(8) . . ?
C48 C43 H43A 108.3 . . ?
C48 C43 H43B 108.3 . . ?
C43 C44 H44A 108.6 . . ?
C43 C44 H44B 108.6 . . ?
C43 C44 C45 114.6(7) . . ?
H44A C44 H44B 107.6 . . ?
C45 C44 H44A 108.6 . . ?
C45 C44 H44B 108.6 . . ?
C44 C45 H45A 108.4 . . ?
C44 C45 H45B 108.4 . . ?
H45A C45 H45B 107.5 . . ?
C46 C45 C44 115.3(8) . . ?
C46 C45 H45A 108.4 . . ?
C46 C45 H45B 108.4 . . ?
C45 C46 H46A 106.6 . . ?
C45 C46 H46B 106.6 . . ?
H46A C46 H46B 106.6 . . ?
C47 C46 C45 122.8(9) . . ?
C47 C46 H46A 106.6 . . ?
C47 C46 H46B 106.6 . . ?
C46 C47 H47A 108.2 . . ?
C46 C47 H47B 108.2 . . ?
C46 C47 C48 116.5(7) . . ?
H47A C47 H47B 107.3 . . ?
C48 C47 H47A 108.2 . . ?
C48 C47 H47B 108.2 . . ?
C43 C48 H48A 109.4 . . ?
C43 C48 H48B 109.4 . . ?
C47 C48 C43 111.4(7) . . ?
C47 C48 H48A 109.4 . . ?
C47 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C49 C49 C49 117.8(3) 18_545 17 ?
C49 C49 H49A 107.9 18_545 . ?
C49 C49 H49A 107.9 17 . ?
C49 C49 H49B 107.9 17 . ?
C49 C49 H49B 107.9 18_545 . ?
H49A C49 H49B 107.2 . . ?
Cl1 C50 H50 108.0 . . ?
Cl1 C50 Cl2 107.8(8) . . ?
Cl2 C50 H50 108.0 . . ?
Cl3 C50 H50 108.0 . . ?
Cl3 C50 Cl1 116.3(10) . . ?
Cl3 C50 Cl2 108.3(7) . . ?
H43C C43A H43D 108.0 . . ?
C44A C43A H43C 109.4 . . ?
C44A C43A H43D 109.4 . . ?
C44A C43A C48A 111.2(10) . . ?
C48A C43A H43C 109.4 . . ?
C48A C43A H43D 109.4 . . ?
C43A C44A H44C 109.3 . . ?
C43A C44A H44D 109.3 . . ?
H44C C44A H44D 108.0 . . ?
C45A C44A C43A 111.6(9) . . ?
C45A C44A H44C 109.3 . . ?
C45A C44A H44D 109.3 . . ?
C44A C45A H45C 108.6 . . ?
C44A C45A H45D 108.6 . . ?
C44A C45A C46A 114.7(10) . . ?
H45C C45A H45D 107.6 . . ?
C46A C45A H45C 108.6 . . ?
C46A C45A H45D 108.6 . . ?
C45A C46A H46C 106.5 . . ?
C45A C46A H46D 106.5 . . ?
H46C C46A H46D 106.5 . . ?
C47A C46A C45A 123.3(11) . . ?
C47A C46A H46C 106.5 . . ?
C47A C46A H46D 106.5 . . ?
C46A C47A H47C 108.0 . . ?
C46A C47A H47D 108.0 . . ?
C46A C47A C48A 117.2(9) . . ?
H47C C47A H47D 107.2 . . ?
C48A C47A H47C 108.0 . . ?
C48A C47A H47D 108.0 . . ?
C43A C48A H48C 111.2 . . ?
C43A C48A H48D 111.2 . . ?
C47A C48A C43A 102.8(8) . . ?
C47A C48A H48C 111.2 . . ?
C47A C48A H48D 111.2 . . ?
H48C C48A H48D 109.1 . . ?
C49A C49A C49A 105.7(8) 17 18_545 ?
C49A C49A H49C 110.6 17 . ?
C49A C49A H49C 110.6 18_545 . ?
C49A C49A H49D 110.6 18_545 . ?
C49A C49A H49D 110.6 17 . ?
H49C C49A H49D 108.7 . . ?
Cl1A C50A H50A 108.7 . . ?
Cl1A C50A Cl2A 106.8(8) . . ?
Cl2A C50A H50A 108.7 . . ?
Cl3A C50A H50A 108.7 . . ?
Cl3A C50A Cl1A 115.6(9) . . ?
Cl3A C50A Cl2A 108.3(6) . . ?
C19 C20A H20D 109.5 . . ?
C19 C20A H20E 109.5 . . ?
C19 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C21A H21E 109.5 . . ?
C19 C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C40 C41A H41D 109.5 . . ?
C40 C41A H41E 109.5 . . ?
C40 C41A H41F 109.5 . . ?
H41D C41A H41E 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
C40 C42A H42D 109.5 . . ?
C40 C42A H42E 109.5 . . ?
C40 C42A H42F 109.5 . . ?
H42D C42A H42E 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 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
C1 C2 C3 C4 -3.6(4) . . . . ?
C1 C2 C3 C5 120.5(2) . . . . ?
C1 C2 C3 C10 -124.3(2) . . . 3_665 ?
C2 C3 C5 C6 -176.4(4) . . . . ?
C2 C3 C5 C10 6.3(4) . . . . ?
C3 C2 C3 C4 119.7(5) 3_665 . . . ?
C3 C2 C3 C4 -126.9(5) 2_655 . . . ?
C3 C2 C3 C5 -116.2(2) 3_665 . . . ?
C3 C2 C3 C5 -2.8(5) 2_655 . . . ?
C3 C2 C3 C10 -1.1(4) 3_665 . . 3_665 ?
C3 C2 C3 C10 112.4(3) 2_655 . . 3_665 ?
C3 C5 C6 C7 -171.6(4) . . . . ?
C3 C5 C10 C3 -7.5(4) . . . 2_655 ?
C3 C5 C10 C9 170.3(3) . . . . ?
C4 C3 C5 C6 -48.9(5) . . . . ?
C4 C3 C5 C10 133.8(3) . . . . ?
C5 C6 C7 C8 1.0(5) . . . . ?
C6 C5 C10 C3 175.0(3) . . . 2_655 ?
C6 C5 C10 C9 -7.2(5) . . . . ?
C6 C7 C8 C9 -6.1(5) . . . . ?
C6 C7 C8 N1 170.5(3) . . . . ?
C7 C8 C9 C10 4.5(5) . . . . ?
C7 C8 N1 C11 -15.8(5) . . . . ?
C7 C8 N1 N2 172.6(3) . . . . ?
C8 C9 C10 C3 179.6(3) . . . 2_655 ?
C8 C9 C10 C5 2.2(5) . . . . ?
C8 N1 N2 N3 172.1(3) . . . . ?
C9 C8 N1 C11 161.0(3) . . . . ?
C9 C8 N1 N2 -10.7(5) . . . . ?
C10 C3 C5 C6 72.4(5) 3_665 . . . ?
C10 C3 C5 C10 -104.8(4) 3_665 . . . ?
C10 C5 C6 C7 5.5(5) . . . . ?
C11 C12 C13 C17 178.2(4) . . . . ?
C11 C12 C13 N4 -4.1(6) . . . . ?
C11 C12 N3 N2 -0.3(4) . . . . ?
C11 N1 N2 N3 -0.9(4) . . . . ?
C12 C11 N1 C8 -171.6(3) . . . . ?
C12 C11 N1 N2 0.7(4) . . . . ?
C12 C13 C17 C16 177.7(4) . . . . ?
C12 C13 N4 C14 -177.5(3) . . . . ?
C13 C12 N3 N2 -178.5(3) . . . . ?
C14 C15 C16 C17 -0.2(8) . . . . ?
C14 C18 N5 C19 176.3(4) . . . . ?
C15 C14 C18 N5 172.0(4) . . . . ?
C15 C14 C18 O1 -5.9(6) . . . . ?
C15 C14 N4 C13 -0.6(6) . . . . ?
C15 C16 C17 C13 -0.2(8) . . . . ?
C17 C13 N4 C14 0.1(5) . . . . ?
C18 C14 C15 C16 176.5(4) . . . . ?
C18 C14 N4 C13 -176.6(3) . . . . ?
C20 C19 N5 C18 153.4(9) . . . . ?
C21 C19 N5 C18 -89.2(8) . . . . ?
N1 C8 C9 C10 -172.1(3) . . . . ?
N1 C11 C12 C13 177.7(3) . . . . ?
N1 C11 C12 N3 -0.3(4) . . . . ?
N1 N2 N3 C12 0.7(4) . . . . ?
N3 C12 C13 C17 -4.0(6) . . . . ?
N3 C12 C13 N4 173.7(3) . . . . ?
N4 C13 C17 C16 0.2(6) . . . . ?
N4 C14 C15 C16 0.6(7) . . . . ?
N4 C14 C18 N5 -11.8(6) . . . . ?
N4 C14 C18 O1 170.3(4) . . . . ?
O1 C18 N5 C19 -6.0(7) . . . . ?
C22 C23 C24 C25 -1.2(5) . . . . ?
C22 C23 C24 C26 121.8(3) . . . . ?
C22 C23 C24 C31 -124.4(3) . . . 3_565 ?
C23 C24 C26 C27 -179.2(6) . . . . ?
C23 C24 C26 C31 3.5(6) . . . . ?
C24 C23 C24 C25 121.3(7) 3_565 . . . ?
C24 C23 C24 C25 -123.7(7) 2_665 . . . ?
C24 C23 C24 C26 -0.7(7) 2_665 . . . ?
C24 C23 C24 C26 -115.8(4) 3_565 . . . ?
C24 C23 C24 C31 113.1(4) 2_665 . . 3_565 ?
C24 C23 C24 C31 -2.0(7) 3_565 . . 3_565 ?
C24 C26 C27 C28 -172.7(6) . . . . ?
C24 C26 C31 C24 -5.1(6) . . . 2_665 ?
C24 C26 C31 C30 174.7(5) . . . . ?
C25 C24 C26 C27 -52.4(7) . . . . ?
C25 C24 C26 C31 130.3(5) . . . . ?
C26 C27 C28 C29 -0.8(10) . . . . ?
C27 C26 C31 C24 177.4(5) . . . 2_665 ?
C27 C26 C31 C30 -2.8(8) . . . . ?
C27 C28 C29 C30 -4.7(11) . . . . ?
C27 C28 C29 N6 173.4(6) . . . . ?
C28 C29 C30 C31 6.4(9) . . . . ?
C28 C29 N6 C32 -19.1(10) . . . . ?
C28 C29 N6 N7 166.2(7) . . . . ?
C29 C30 C31 C24 177.2(6) . . . 2_665 ?
C29 C30 C31 C26 -2.5(8) . . . . ?
C29 N6 N7 N8 174.4(7) . . . . ?
C30 C29 N6 C32 159.1(6) . . . . ?
C30 C29 N6 N7 -15.7(10) . . . . ?
C31 C24 C26 C27 70.0(7) 3_565 . . . ?
C31 C24 C26 C31 -107.4(5) 3_565 . . . ?
C31 C26 C27 C28 4.5(8) . . . . ?
C32 C33 C34 C38 -167.9(9) . . . . ?
C32 C33 C34 N9 10.3(12) . . . . ?
C32 C33 N8 N7 -2.9(12) . . . . ?
C32 N6 N7 N8 -1.2(10) . . . . ?
C33 C32 N6 C29 -175.6(7) . . . . ?
C33 C32 N6 N7 -0.6(9) . . . . ?
C33 C34 C38 C37 177.1(10) . . . . ?
C33 C34 N9 C35 -176.1(6) . . . . ?
C34 C33 N8 N7 -174.2(8) . . . . ?
C35 C36 C37 C38 0.1(16) . . . . ?
C35 C39 N10 C40 173.5(7) . . . . ?
C36 C35 C39 N10 -174.1(6) . . . . ?
C36 C35 C39 O2 3.7(9) . . . . ?
C36 C35 N9 C34 -2.1(10) . . . . ?
C36 C37 C38 C34 -0.2(17) . . . . ?
C38 C34 N9 C35 2.0(11) . . . . ?
C39 C35 C36 C37 178.9(8) . . . . ?
C39 C35 N9 C34 180.0(6) . . . . ?
C41 C40 N10 C39 -111.4(11) . . . . ?
C42 C40 N10 C39 123.6(11) . . . . ?
N6 C29 C30 C31 -171.8(5) . . . . ?
N6 C32 C33 C34 172.7(8) . . . . ?
N6 C32 C33 N8 2.1(9) . . . . ?
N6 N7 N8 C33 2.5(11) . . . . ?
N8 C33 C34 C38 1.6(14) . . . . ?
N8 C33 C34 N9 179.7(8) . . . . ?
N9 C34 C38 C37 -0.9(15) . . . . ?
N9 C35 C36 C37 1.1(12) . . . . ?
N9 C35 C39 N10 3.8(8) . . . . ?
N9 C35 C39 O2 -178.4(5) . . . . ?
O2 C39 N10 C40 -4.2(10) . . . . ?
C43 C44 C45 C46 3.2(18) . . . . ?
C44 C43 C48 C47 -55.6(13) . . . . ?
C44 C45 C46 C47 -26(2) . . . . ?
C45 C46 C47 C48 7(2) . . . . ?
C46 C47 C48 C43 32.3(16) . . . . ?
C48 C43 C44 C45 36.6(16) . . . . ?
C43A C44A C45A C46A -5(2) . . . . ?
C44A C43A C48A C47A -70.0(12) . . . . ?
C44A C45A C46A C47A -26(3) . . . . ?
C45A C46A C47A C48A 5(3) . . . . ?
C46A C47A C48A C43A 39.6(16) . . . . ?
C48A C43A C44A C45A 52.6(17) . . . . ?
C20A C19 N5 C18 121.0(10) . . . . ?
C21A C19 N5 C18 -110.5(9) . . . . ?
C41A C40 N10 C39 -94.7(13) . . . . ?
C42A C40 N10 C39 147.2(13) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 1440 electrons were 
found in a volume of 6405Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
2.1[CHCl3], 2.1[CHCl3] per Asymmetric Unit 
which account for 1462 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.209 589.6 120.3 '2.1 CHCl3'
2 0.000 0.000 0.500 955.2 239.7 '4.2 CHCl3'
3 0.000 0.000 0.791 589.6 113.3 '2.1 CHCl3'
4 -0.333 0.333 0.833 955.2 239.7 '4.2 CHCl3'
5 0.333 0.667 0.167 955.2 239.7 '4.2 CHCl3'
6 0.333 0.667 0.458 589.6 113.3 '2.1 CHCl3'
7 0.333 0.667 0.875 589.6 120.3 '2.1 CHCl3'
8 0.667 0.333 0.125 589.6 113.3 '2.1 CHCl3'
9 0.667 0.333 0.542 589.6 120.3 '2.1 CHCl3'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.338
_oxdiff_exptl_absorpt_empirical_full_min 0.336
# start Validation Reply Form
_vrf_PLAT084_CYH                 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.40 Report
RESPONSE: We made numerous attempts to obtain higher-quality data 
for this structure. However, due to solvent disorder, the R2 value remains 
high. Nonetheless, we are confident that the data quality is consistent 
with its intrinsic characteristics, as indicated by the favorable Rint value.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_PhMe
_audit_block_doi                 10.5517/ccdc.csd.cc2mbq4v
_database_code_depnum_ccdc_archive 'CCDC 2423367'
loop_
_audit_author_name
_audit_author_address
'Tianshu Yang'
;FUJIAN NORMAL UNIVERSITY
China
;
_audit_update_record             
;
2025-02-14 deposited with the CCDC.	2025-02-27 downloaded from the CCDC.
;
_audit_creation_date             2025-02-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C59 H57 N15 O3), 5(C7 H8), 2(C H Cl3), 2(H2 O)'
_chemical_formula_sum            'C155 H160 Cl6 N30 O8'
_chemical_formula_weight         2783.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0150 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0410 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.3812(3)
_cell_length_b                   15.4937(3)
_cell_length_c                   17.2333(4)
_cell_angle_alpha                71.658(2)
_cell_angle_beta                 79.5378(19)
_cell_angle_gamma                82.7903(17)
_cell_volume                     3574.59(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    17720
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      55.0310
_cell_measurement_theta_min      2.3970
_shelx_estimated_absorpt_T_max   0.899
_shelx_estimated_absorpt_T_min   0.872
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.116a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1466
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40828
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         55.126
_diffrn_reflns_theta_min         2.376
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     21.00 110.00   0.50    1.40    --   65.46-125.00 -30.00  178
  2  ω     76.00 102.00   0.50    1.40    --   65.46-125.00  60.00   52
  3  ω     -5.00  76.00   0.50    1.40    --   65.46 -96.00  68.00  162
  4  ω     -6.00  19.00   0.50    1.40    --   65.46 -38.00 120.00   50
  5  ω     44.00 139.00   0.50    1.40    --   65.46  57.00 150.00  190
  6  ω     88.00 113.00   0.50    1.40    --   65.46  96.00 176.00   50
  7  ω     -5.00  87.00   0.50    1.40    --   65.46 -57.00 -30.00  184
  8  ω    -12.00  27.00   0.50    1.40    --   65.46 -38.00-180.00   78
  9  ω     38.00  64.00   0.50    1.40    --   65.46 -38.00-180.00   52
 10  ω     -6.00  37.00   0.50    0.35    --   -1.17 -99.00-120.00   86
 11  ω     -3.00  35.00   0.50    0.35    --   -1.17 -96.00  68.00   76
 12  ω    -75.00 -10.00   0.50    0.35    --   -1.17 -77.00  30.00  130
 13  ω   -140.00 -62.00   0.50    1.40    --  -67.80 -57.00 -30.00  156
 14  ω   -141.00 -85.00   0.50    1.40    --  -67.80 -96.00  68.00  112
 15  ω   -140.00 -90.00   0.50    1.40    --  -67.80 -99.00  90.00  100
 16  ω   -135.00 -92.00   0.50    1.40    --  -67.80 -99.00 150.00   86
 17  ω   -138.00 -80.00   0.50    1.40    --  -67.80-125.00 -30.00  116
 18  ω   -132.00 -89.00   0.50    1.40    --  -67.80 -99.00 -60.00   86
 19  ω    -57.00 -10.00   0.50    1.40    --  -67.80  57.00   0.00   94
 20  ω     35.00  72.00   0.50    0.35    --   -1.17  57.00 -90.00   74
 21  ω    -96.00 -14.00   0.50    1.40    --  -67.80  77.00  30.00  164
 22  ω    -96.00 -13.00   0.50    1.40    --  -67.80  77.00-180.00  166
 23  ω   -109.00 -39.00   0.50    1.40    --  -67.80 125.00-150.00  140
 24  ω    -90.00 -30.00   0.50    1.40    --  -67.80  96.00 176.00  120
 25  ω    -35.00  23.00   0.50    0.35    --   -1.17  96.00 176.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0183075000
_diffrn_orient_matrix_UB_12      0.0876229000
_diffrn_orient_matrix_UB_13      -0.0416694000
_diffrn_orient_matrix_UB_21      0.0108575000
_diffrn_orient_matrix_UB_22      0.0245233000
_diffrn_orient_matrix_UB_23      0.0655393000
_diffrn_orient_matrix_UB_31      0.0925344000
_diffrn_orient_matrix_UB_32      0.0075969000
_diffrn_orient_matrix_UB_33      -0.0287569000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_source                   'micro-focus metaljet'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9413
_reflns_number_total             13351
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.116a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.116a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.116a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         13351
_refine_ls_number_restraints     790
_refine_ls_R_factor_all          0.1928
_refine_ls_R_factor_gt           0.1378
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0849P)²+25.3942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3414
_refine_ls_wR_factor_ref         0.3586
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C61-C60 \\sim C65-C60 \\sim C65-C64 \\sim C64-C63 \\sim C62-C61 \\sim C63-C62
 with sigma of 0.02
 C67-C69 \\sim C68-C70 \\sim C69-C71 \\sim C70-C72 \\sim C71-C67 \\sim C72-C68
 with sigma of 0.02
 C68-C67 \\sim C69-C68 \\sim C70-C69 \\sim C71-C70 \\sim C72-C71 \\sim C72-C67
 with sigma of 0.02
 C66-C60 \\sim C73-C67
 with sigma of 0.02
 C73-C72 \\sim C73-C68
 with sigma of 0.02
 C60-C62 \\sim C61-C63 \\sim C62-C64 \\sim C63-C65 \\sim C64-C60 \\sim C65-C61
 with sigma of 0.02
 C66-C65 \\sim C66-C61
 with sigma of 0.02
3. Restrained planarity
 C67, C68, C69, C70, C71, C72, C73
 with sigma of 0.01
 C60, C61, C62, C63, C64, C65, C66
 with sigma of 0.01
 C60A, C61A, C62A, C63A, C64A, C65A, C66A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C40 \\sim C41 \\sim C41A \\sim C42 \\sim C42A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C67 \\sim C67A \\sim C68 \\sim C68A \\sim C69 \\sim C69A \\sim C70 \\sim C70A
\\sim C71 \\sim C71A \\sim C72 \\sim C72A \\sim C73 \\sim C73A \\sim C78A \\sim
C78B \\sim Cl1A \\sim Cl1B \\sim Cl2A \\sim Cl2B \\sim Cl3A \\sim Cl3B \\sim
C78 \\sim Cl1 \\sim Cl2 \\sim Cl3: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C23 \\sim C24 \\sim C24A \\sim C25 \\sim C25A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C60A
\\sim C61A \\sim C62A \\sim C63A \\sim C64A \\sim C65A \\sim C66A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C72A) \\sim Ueq, Uanis(C67A) \\sim Ueq, Uanis(C68A) \\sim Ueq,
Uanis(C73A) \\sim Ueq, Uanis(C69A) \\sim Ueq, Uanis(C71A) \\sim Ueq,
Uanis(C70A) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C72)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C71) \\sim Ueq,
Uanis(C70) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Same fragment restrains
{C23, C24, C25} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C23, C24A, C25A}
{C60A, C61A, C62A, C63A, C64A, C65A, C66A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C60, C61, C62, C63, C64, C65, C66}
{C78A, Cl1A, Cl2A, Cl3A} sigma for 1-2: 0.01, 1-3: 0.01
{C78B, Cl1B, Cl2B, Cl3B} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C78, Cl1, Cl2, Cl3}
{C40, C41A, C42A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C40, C41, C42}
{C67A, C68A, C69A, C70A, C71A, C72A, C73A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C67, C68, C69, C70, C71, C72, C73}
6. Others
 1*[Sof(C78)+Sof(H78)+Sof(Cl1)+Sof(Cl2)+Sof(Cl3)]+1*[Sof(C78A)+Sof(H78A)+
 Sof(Cl1A)+Sof(Cl2A)+Sof(Cl3A)]+1*[Sof(C78B)+Sof(H78B)+Sof(Cl1B)+Sof(Cl2B)+
 Sof(Cl3B)]=1 with esd of 0
 Sof(C78)=Sof(H78)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(1)
 Sof(C60A)=Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63A)=
 Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66D)=Sof(H66E)=
 Sof(H66F)=1-FVAR(2)
 Sof(C60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=
 Sof(H64)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=FVAR(2)
 Sof(H23A)=Sof(C24)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=1-FVAR(3)
 Sof(H23)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25A)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=FVAR(3)
 Sof(H40A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42D)=
 Sof(H42E)=Sof(H42F)=1-FVAR(4)
 Sof(H40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=FVAR(4)
 Sof(C67A)=Sof(C68A)=Sof(H68A)=Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(H70A)=
 Sof(C71A)=Sof(H71A)=Sof(C72A)=Sof(H72A)=Sof(C73A)=Sof(H73D)=Sof(H73E)=
 Sof(H73F)=1-FVAR(5)
 Sof(C67)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70)=Sof(C71)=
 Sof(H71)=Sof(C72)=Sof(H72)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=FVAR(5)
 Sof(C78A)=Sof(H78A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(6)
 Sof(C78B)=Sof(H78B)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=FVAR(7)
 Fixed Sof: C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5) H75(0.5)
7.a Riding coordinates:
 C73(H73A,H73B,H73C), C73A(H73D,H73E,H73F)
7.b Ternary CH refined with riding coordinates:
 C23(H23), C23(H23A), C40(H40), C40(H40A), C57(H57), C78A(H78A), C78B(H78B),
 C78(H78)
7.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C15(H15), C19(H19), C20(H20), C21(H21),
 C27(H27), C29(H29), C30(H30), C32(H32), C36(H36), C37(H37), C38(H38), C43(H43),
  C45(H45), C46(H46), C49(H49), C53(H53), C54(H54), C55(H55), N5(H5), N10(H10A),
  N15(H15A), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C61A(H61A),
 C62A(H62A), C63A(H63A), C64A(H64A), C65A(H65A), C68(H68), C69(H69), C70(H70),
 C71(H71), C72(H72), C68A(H68A), C69A(H69A), C70A(H70A), C71A(H71A), C72A(H72A),
  C75(H75), C76(H76), C77(H77)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C24A(H24A,
 H24B,H24C), C25A(H25A,H25B,H25C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C66(H66A,H66B,H66C), C66A(H66D,H66E,
 H66F), C74(H74A,H74B,H74C), C24(H24D,H24E,H24F), C25(H25D,H25E,H25F),
 C41A(H41D,H41E,H41F), C42A(H42D,H42E,H42F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.9910(5) 0.5392(6) 0.2839(4) 0.057(2) Uani 1 1 d . . . . .
H1A H 1.031956 0.536196 0.324413 0.086 Uiso 1 1 calc R U . . .
H1B H 0.989607 0.600446 0.244180 0.086 Uiso 1 1 calc R U . . .
H1C H 1.015710 0.494338 0.254456 0.086 Uiso 1 1 calc R U . . .
C2 C 0.8906(4) 0.5183(5) 0.3284(4) 0.0459(18) Uani 1 1 d . . . . .
C3 C 0.8197(4) 0.5168(5) 0.2674(4) 0.0452(17) Uani 1 1 d . . . . .
C4 C 0.8893(4) 0.4212(5) 0.3966(4) 0.0453(17) Uani 1 1 d . . . . .
C5 C 0.8439(5) 0.5903(5) 0.3739(4) 0.0429(16) Uani 1 1 d . . . . .
C6 C 0.8607(5) 0.5444(6) 0.1746(4) 0.0514(19) Uani 1 1 d . . . . .
H6A H 0.878037 0.607646 0.156758 0.077 Uiso 1 1 calc R U . . .
H6B H 0.813044 0.538922 0.142678 0.077 Uiso 1 1 calc R U . . .
H6C H 0.917156 0.504224 0.165313 0.077 Uiso 1 1 calc R U . . .
C7 C 0.9853(5) 0.3660(6) 0.4049(4) 0.057(2) Uani 1 1 d . . . . .
H7A H 1.013294 0.356583 0.351609 0.085 Uiso 1 1 calc R U . . .
H7B H 0.976040 0.306716 0.446777 0.085 Uiso 1 1 calc R U . . .
H7C H 1.027876 0.399317 0.421490 0.085 Uiso 1 1 calc R U . . .
C8 C 0.8993(5) 0.6746(5) 0.3597(4) 0.0529(19) Uani 1 1 d . . . . .
H8A H 0.960619 0.654800 0.379224 0.079 Uiso 1 1 calc R U . . .
H8B H 0.862719 0.714487 0.390363 0.079 Uiso 1 1 calc R U . . .
H8C H 0.909567 0.707945 0.300582 0.079 Uiso 1 1 calc R U . . .
C9 C 0.7910(4) 0.4192(5) 0.2973(4) 0.0455(17) Uani 1 1 d . . . . .
C10 C 0.7342(5) 0.3806(6) 0.2615(4) 0.0500(19) Uani 1 1 d . . . . .
H10 H 0.711662 0.415339 0.211562 0.060 Uiso 1 1 calc R U . . .
C11 C 0.7110(5) 0.2924(6) 0.2988(4) 0.0519(19) Uani 1 1 d . . . . .
H11 H 0.673597 0.265276 0.273953 0.062 Uiso 1 1 calc R U . . .
C12 C 0.7423(5) 0.2426(6) 0.3728(4) 0.0498(18) Uani 1 1 d . . . . .
C13 C 0.7989(5) 0.2799(6) 0.4103(4) 0.0501(18) Uani 1 1 d . . . . .
H13 H 0.820243 0.245572 0.460917 0.060 Uiso 1 1 calc R U . . .
C14 C 0.8227(4) 0.3693(5) 0.3707(4) 0.0452(17) Uani 1 1 d . . . . .
C15 C 0.6503(5) 0.1079(6) 0.3944(4) 0.0535(19) Uani 1 1 d . . . . .
H15 H 0.605125 0.133343 0.357806 0.064 Uiso 1 1 calc R U . . .
C16 C 0.6603(5) 0.0201(6) 0.4444(5) 0.057(2) Uani 1 1 d . . . . .
C17 C 0.6031(5) -0.0568(6) 0.4568(5) 0.0555(19) Uani 1 1 d . . . . .
C18 C 0.4793(5) -0.1068(5) 0.4199(5) 0.0536(18) Uani 1 1 d . . . . .
C19 C 0.4897(6) -0.1925(6) 0.4753(5) 0.060(2) Uani 1 1 d . . . . .
H19 H 0.449233 -0.238532 0.480115 0.072 Uiso 1 1 calc R U . . .
C20 C 0.5613(7) -0.2096(6) 0.5238(5) 0.067(2) Uani 1 1 d . . . . .
H20 H 0.570623 -0.267708 0.562829 0.080 Uiso 1 1 calc R U . . .
C21 C 0.6187(6) -0.1407(6) 0.5144(5) 0.062(2) Uani 1 1 d . . . . .
H21 H 0.668019 -0.150648 0.546940 0.074 Uiso 1 1 calc R U . . .
C22 C 0.4028(6) -0.0854(6) 0.3662(5) 0.057(2) Uani 1 1 d . . . . .
C23 C 0.3192(8) 0.0301(7) 0.2657(8) 0.093(3) Uani 1 1 d D U . . .
H23 H 0.278969 -0.018136 0.265877 0.111 Uiso 0.532(16) 1 calc R U P A 1
H23A H 0.257518 0.002621 0.291757 0.111 Uiso 0.468(16) 1 calc R U P A 2
C24A C 0.3581(18) 0.0884(17) 0.1826(13) 0.129(7) Uani 0.532(16) 1 d D U P A 1
H24A H 0.305912 0.118305 0.151956 0.193 Uiso 0.532(16) 1 calc R U P A 1
H24B H 0.399657 0.050618 0.152465 0.193 Uiso 0.532(16) 1 calc R U P A 1
H24C H 0.394510 0.134743 0.188573 0.193 Uiso 0.532(16) 1 calc R U P A 1
C25A C 0.2603(15) 0.1180(14) 0.2949(16) 0.104(6) Uani 0.532(16) 1 d D U P A 1
H25A H 0.304535 0.163928 0.288409 0.156 Uiso 0.532(16) 1 calc R U P A 1
H25B H 0.231288 0.096344 0.352926 0.156 Uiso 0.532(16) 1 calc R U P A 1
H25C H 0.210771 0.145159 0.260325 0.156 Uiso 0.532(16) 1 calc R U P A 1
C26 C 0.8290(4) 0.5362(5) 0.4647(3) 0.0389(15) Uani 1 1 d . . . . .
C27 C 0.7952(4) 0.5710(5) 0.5306(3) 0.0388(15) Uani 1 1 d . . . . .
H27 H 0.779093 0.634365 0.521624 0.047 Uiso 1 1 calc R U . . .
C28 C 0.7857(4) 0.5101(5) 0.6099(4) 0.0358(14) Uani 1 1 d . . . . .
C29 C 0.8084(4) 0.4184(5) 0.6232(4) 0.0404(15) Uani 1 1 d . . . . .
H29 H 0.801396 0.378027 0.677998 0.049 Uiso 1 1 calc R U . . .
C30 C 0.8419(4) 0.3841(5) 0.5565(4) 0.0423(15) Uani 1 1 d . . . . .
H30 H 0.858254 0.320750 0.565467 0.051 Uiso 1 1 calc R U . . .
C31 C 0.8508(4) 0.4439(5) 0.4773(4) 0.0395(15) Uani 1 1 d . . . . .
C32 C 0.7321(4) 0.4976(5) 0.7600(3) 0.0366(14) Uani 1 1 d . . . . .
H32 H 0.745884 0.434473 0.785544 0.044 Uiso 1 1 calc R U . . .
C33 C 0.6912(5) 0.5618(5) 0.7970(4) 0.0396(15) Uani 1 1 d . . . . .
C34 C 0.6564(4) 0.5491(5) 0.8857(4) 0.0374(14) Uani 1 1 d . . . . .
C35 C 0.6228(4) 0.4471(5) 1.0144(4) 0.0403(15) Uani 1 1 d . . . . .
C36 C 0.5940(4) 0.5172(5) 1.0500(4) 0.0440(17) Uani 1 1 d . . . . .
H36 H 0.571937 0.503653 1.107603 0.053 Uiso 1 1 calc R U . . .
C37 C 0.5978(5) 0.6066(5) 1.0004(4) 0.0467(17) Uani 1 1 d . . . . .
H37 H 0.579490 0.655573 1.023351 0.056 Uiso 1 1 calc R U . . .
C38 C 0.6289(5) 0.6232(5) 0.9164(4) 0.0446(16) Uani 1 1 d . . . . .
H38 H 0.631446 0.683841 0.880429 0.054 Uiso 1 1 calc R U . . .
C39 C 0.6174(5) 0.3497(5) 1.0665(4) 0.0482(18) Uani 1 1 d . . . . .
C40 C 0.6273(6) 0.1895(5) 1.0682(5) 0.060(2) Uani 1 1 d D U . . .
H40 H 0.576156 0.182321 1.117100 0.072 Uiso 0.755(17) 1 calc R U P B 1
H40A H 0.615317 0.180085 1.129175 0.072 Uiso 0.245(17) 1 calc R U P B 2
C41 C 0.7189(10) 0.1563(9) 1.1027(10) 0.084(4) Uani 0.755(17) 1 d D U P B 1
H41A H 0.714285 0.093760 1.139552 0.126 Uiso 0.755(17) 1 calc R U P B 1
H41B H 0.730716 0.195994 1.133787 0.126 Uiso 0.755(17) 1 calc R U P B 1
H41C H 0.771184 0.157658 1.057202 0.126 Uiso 0.755(17) 1 calc R U P B 1
C42 C 0.5982(10) 0.1418(7) 1.0158(6) 0.060(3) Uani 0.755(17) 1 d D U P B 1
H42A H 0.648863 0.141576 0.969379 0.091 Uiso 0.755(17) 1 calc R U P B 1
H42B H 0.540315 0.173141 0.994635 0.091 Uiso 0.755(17) 1 calc R U P B 1
H42C H 0.586154 0.078827 1.048637 0.091 Uiso 0.755(17) 1 calc R U P B 1
C43 C 0.6548(4) 0.6010(5) 0.2485(4) 0.0455(17) Uani 1 1 d . . . . .
H43 H 0.646700 0.574050 0.207935 0.055 Uiso 1 1 calc R U . . .
C44 C 0.5854(5) 0.6604(5) 0.2731(4) 0.0438(16) Uani 1 1 d . . . . .
C45 C 0.5952(5) 0.7013(5) 0.3318(4) 0.0451(16) Uani 1 1 d . . . . .
H45 H 0.546357 0.742476 0.347722 0.054 Uiso 1 1 calc R U . . .
C46 C 0.6780(5) 0.6808(5) 0.3669(4) 0.0458(17) Uani 1 1 d . . . . .
H46 H 0.686186 0.707643 0.407485 0.055 Uiso 1 1 calc R U . . .
C47 C 0.7485(5) 0.6209(5) 0.3425(4) 0.0419(16) Uani 1 1 d . . . . .
C48 C 0.7375(5) 0.5809(5) 0.2847(4) 0.0442(17) Uani 1 1 d . . . . .
C49 C 0.4168(5) 0.7232(5) 0.2613(4) 0.0417(15) Uani 1 1 d . . . . .
H49 H 0.401982 0.747173 0.306832 0.050 Uiso 1 1 calc R U . . .
C50 C 0.3581(5) 0.7246(5) 0.2061(4) 0.0402(15) Uani 1 1 d . . . . .
C51 C 0.2600(4) 0.7604(4) 0.2010(4) 0.0377(14) Uani 1 1 d . . . . .
C52 C 0.1235(5) 0.7595(4) 0.1498(4) 0.0401(15) Uani 1 1 d . . . . .
C53 C 0.0746(5) 0.8209(5) 0.1885(4) 0.0486(17) Uani 1 1 d . . . . .
H53 H 0.010348 0.841117 0.182727 0.058 Uiso 1 1 calc R U . . .
C54 C 0.1228(5) 0.8523(5) 0.2364(5) 0.0524(18) Uani 1 1 d . . . . .
H54 H 0.091920 0.894695 0.264094 0.063 Uiso 1 1 calc R U . . .
C55 C 0.2152(5) 0.8212(5) 0.2429(4) 0.0477(17) Uani 1 1 d . . . . .
H55 H 0.248763 0.841145 0.275990 0.057 Uiso 1 1 calc R U . . .
C56 C 0.0719(5) 0.7207(5) 0.0996(4) 0.0407(15) Uani 1 1 d . . . . .
C57 C 0.0857(5) 0.6152(5) 0.0164(4) 0.0468(17) Uani 1 1 d . . . . .
H57 H 0.014974 0.624661 0.025882 0.056 Uiso 1 1 calc R U . . .
C58 C 0.1202(7) 0.6603(7) -0.0745(5) 0.075(3) Uani 1 1 d . . . . .
H58A H 0.189450 0.650899 -0.085470 0.112 Uiso 1 1 calc R U . . .
H58B H 0.101666 0.725799 -0.088571 0.112 Uiso 1 1 calc R U . . .
H58C H 0.091865 0.633342 -0.108263 0.112 Uiso 1 1 calc R U . . .
C59 C 0.1121(5) 0.5142(5) 0.0424(5) 0.0513(18) Uani 1 1 d . . . . .
H59A H 0.080187 0.484847 0.012793 0.077 Uiso 1 1 calc R U . . .
H59B H 0.092326 0.488785 0.102079 0.077 Uiso 1 1 calc R U . . .
H59C H 0.180889 0.503124 0.029271 0.077 Uiso 1 1 calc R U . . .
N1 N 0.7195(4) 0.1505(5) 0.4087(4) 0.0559(16) Uani 1 1 d . . . . .
N2 N 0.7703(5) 0.0918(6) 0.4645(5) 0.071(2) Uani 1 1 d . . . . .
N3 N 0.7340(5) 0.0123(6) 0.4869(5) 0.073(2) Uani 1 1 d . . . . .
N4 N 0.5345(4) -0.0385(4) 0.4096(4) 0.0539(15) Uani 1 1 d . . . . .
N5 N 0.3902(5) -0.0001(5) 0.3204(5) 0.069(2) Uani 1 1 d . . . . .
H5 H 0.426353 0.040331 0.323150 0.083 Uiso 1 1 calc R U . . .
N6 N 0.7487(4) 0.5442(4) 0.6787(3) 0.0395(13) Uani 1 1 d . . . . .
N7 N 0.7199(5) 0.6334(4) 0.6659(3) 0.0568(17) Uani 1 1 d . . . . .
N8 N 0.6849(5) 0.6438(4) 0.7381(3) 0.0564(17) Uani 1 1 d . . . . .
N9 N 0.6554(3) 0.4623(4) 0.9334(3) 0.0365(12) Uani 1 1 d . . . . .
N10 N 0.6290(4) 0.2877(4) 1.0265(3) 0.0462(14) Uani 1 1 d . . . . .
H10A H 0.638289 0.306607 0.972115 0.055 Uiso 1 1 calc R U . . .
N11 N 0.4988(4) 0.6813(4) 0.2376(3) 0.0422(13) Uani 1 1 d . . . . .
N12 N 0.4939(4) 0.6562(4) 0.1695(3) 0.0447(14) Uani 1 1 d . . . . .
N13 N 0.4088(4) 0.6827(4) 0.1509(3) 0.0442(14) Uani 1 1 d . . . . .
N14 N 0.2140(4) 0.7291(4) 0.1551(3) 0.0389(12) Uani 1 1 d . . . . .
N15 N 0.1238(4) 0.6596(4) 0.0675(3) 0.0431(13) Uani 1 1 d . . . . .
H15A H 0.182724 0.644925 0.076866 0.052 Uiso 1 1 calc R U . . .
O1 O 0.3558(4) -0.1469(4) 0.3668(4) 0.0654(15) Uani 1 1 d . . . . .
O2 O 0.6018(4) 0.3313(4) 1.1430(3) 0.0592(15) Uani 1 1 d . . . . .
O3 O -0.0109(3) 0.7465(3) 0.0921(3) 0.0539(13) Uani 1 1 d . . . . .
C60 C 0.2954(12) 0.1232(11) 0.8051(9) 0.077(3) Uani 0.334(8) 1 d D U P C 1
C61 C 0.3856(11) 0.0943(13) 0.8278(11) 0.077(3) Uani 0.334(8) 1 d D U P C 1
H61 H 0.427702 0.055849 0.801743 0.092 Uiso 0.334(8) 1 calc R U P C 1
C62 C 0.4125(12) 0.1222(14) 0.8887(12) 0.076(4) Uani 0.334(8) 1 d D U P C 1
H62 H 0.473791 0.102371 0.903741 0.091 Uiso 0.334(8) 1 calc R U P C 1
C63 C 0.3545(15) 0.1769(14) 0.9276(11) 0.078(4) Uani 0.334(8) 1 d D U P C 1
H63 H 0.374725 0.195025 0.969320 0.093 Uiso 0.334(8) 1 calc R U P C 1
C64 C 0.2655(14) 0.2059(14) 0.9055(12) 0.079(4) Uani 0.334(8) 1 d D U P C 1
H64 H 0.223731 0.244335 0.931842 0.095 Uiso 0.334(8) 1 calc R U P C 1
C65 C 0.2381(11) 0.1789(13) 0.8455(12) 0.076(4) Uani 0.334(8) 1 d D U P C 1
H65 H 0.176739 0.199342 0.830935 0.091 Uiso 0.334(8) 1 calc R U P C 1
C66 C 0.2616(18) 0.0954(17) 0.7396(13) 0.086(6) Uani 0.334(8) 1 d D U P C 1
H66A H 0.308138 0.109696 0.689026 0.129 Uiso 0.334(8) 1 calc R U P C 1
H66B H 0.200570 0.128583 0.727911 0.129 Uiso 0.334(8) 1 calc R U P C 1
H66C H 0.253886 0.029677 0.759041 0.129 Uiso 0.334(8) 1 calc R U P C 1
C60A C 0.3037(8) 0.1558(6) 0.8752(6) 0.076(3) Uani 0.666(8) 1 d D U P C 2
C61A C 0.3871(8) 0.1095(7) 0.8481(6) 0.082(3) Uani 0.666(8) 1 d D U P C 2
H61A H 0.443627 0.107522 0.870070 0.099 Uiso 0.666(8) 1 calc R U P C 2
C62A C 0.3860(9) 0.0665(8) 0.7889(7) 0.082(3) Uani 0.666(8) 1 d D U P C 2
H62A H 0.442811 0.035222 0.770764 0.098 Uiso 0.666(8) 1 calc R U P C 2
C63A C 0.3075(9) 0.0672(8) 0.7558(7) 0.084(3) Uani 0.666(8) 1 d D U P C 2
H63A H 0.309058 0.037081 0.715279 0.101 Uiso 0.666(8) 1 calc R U P C 2
C64A C 0.2248(9) 0.1128(8) 0.7822(7) 0.081(3) Uani 0.666(8) 1 d D U P C 2
H64A H 0.168505 0.114310 0.760096 0.097 Uiso 0.666(8) 1 calc R U P C 2
C65A C 0.2251(7) 0.1553(7) 0.8401(7) 0.070(3) Uani 0.666(8) 1 d D U P C 2
H65A H 0.167754 0.186439 0.857319 0.084 Uiso 0.666(8) 1 calc R U P C 2
C66A C 0.2981(10) 0.2045(9) 0.9394(7) 0.082(4) Uani 0.666(8) 1 d D U P C 2
H66D H 0.334480 0.168006 0.983036 0.123 Uiso 0.666(8) 1 calc R U P C 2
H66E H 0.231699 0.213206 0.963504 0.123 Uiso 0.666(8) 1 calc R U P C 2
H66F H 0.324399 0.264058 0.913395 0.123 Uiso 0.666(8) 1 calc R U P C 2
C67 C 0.9938(15) 0.0052(14) 0.6141(13) 0.131(5) Uani 0.340(7) 1 d D U P D -1
C68 C 1.0553(17) -0.0406(16) 0.6733(14) 0.135(5) Uani 0.340(7) 1 d D U P D -1
H68 H 1.050444 -0.102948 0.704405 0.161 Uiso 0.340(7) 1 calc R U P D -1
C69 C 1.1246(18) 0.0124(19) 0.6833(15) 0.135(5) Uani 0.340(7) 1 d D U P D -1
H69 H 1.167220 -0.014824 0.721899 0.163 Uiso 0.340(7) 1 calc R U P D -1
C70 C 1.1298(17) 0.1039(19) 0.6365(16) 0.119(5) Uani 0.340(7) 1 d D U P D -1
H70 H 1.176323 0.137844 0.644043 0.142 Uiso 0.340(7) 1 calc R U P D -1
C71 C 1.0675(17) 0.1482(15) 0.5776(15) 0.090(4) Uani 0.340(7) 1 d D U P D -1
H71 H 1.072187 0.210441 0.546209 0.108 Uiso 0.340(7) 1 calc R U P D -1
C72 C 0.9980(16) 0.0964(14) 0.5672(13) 0.087(4) Uani 0.340(7) 1 d D U P D -1
H72 H 0.955194 0.123784 0.528783 0.104 Uiso 0.340(7) 1 calc R U P D -1
C73 C 0.925(2) -0.045(2) 0.603(2) 0.160(8) Uani 0.340(7) 1 d D U P D -1
H73A H 0.863197 -0.030635 0.632629 0.241 Uiso 0.340(7) 1 d R U P D -1
H73B H 0.942237 -0.110925 0.624039 0.241 Uiso 0.340(7) 1 d R U P D -1
H73C H 0.921377 -0.029085 0.543779 0.241 Uiso 0.340(7) 1 d R U P D -1
C67A C 0.9567(14) -0.2144(14) 0.8037(11) 0.146(5) Uani 0.660(7) 1 d D U P D -2
C68A C 0.9269(14) -0.1877(13) 0.8775(11) 0.134(5) Uani 0.660(7) 1 d D U P D -2
H68A H 0.877106 -0.215004 0.919023 0.161 Uiso 0.660(7) 1 calc R U P D -2
C69A C 0.9780(15) -0.1164(14) 0.8843(12) 0.140(4) Uani 0.660(7) 1 d D U P D -2
H69A H 0.961640 -0.095502 0.931598 0.168 Uiso 0.660(7) 1 calc R U P D -2
C70A C 1.0504(15) -0.0781(14) 0.8229(13) 0.150(5) Uani 0.660(7) 1 d D U P D -2
H70A H 1.082173 -0.031028 0.829174 0.180 Uiso 0.660(7) 1 calc R U P D -2
C71A C 1.0793(14) -0.1071(14) 0.7497(12) 0.142(4) Uani 0.660(7) 1 d D U P D -2
H71A H 1.131136 -0.082250 0.709379 0.171 Uiso 0.660(7) 1 calc R U P D -2
C72A C 1.0269(13) -0.1743(13) 0.7406(11) 0.139(5) Uani 0.660(7) 1 d D U P D -2
H72A H 1.040045 -0.191709 0.691359 0.167 Uiso 0.660(7) 1 calc R U P D -2
C73A C 0.9090(15) -0.2835(13) 0.7941(13) 0.132(7) Uani 0.660(7) 1 d D U P D -2
H73D H 0.954868 -0.334342 0.788432 0.198 Uiso 0.660(7) 1 d R U P D -2
H73E H 0.878268 -0.259472 0.744552 0.198 Uiso 0.660(7) 1 d R U P D -2
H73F H 0.861038 -0.304862 0.842742 0.198 Uiso 0.660(7) 1 d R U P D -2
C78A C 1.0845(13) 0.1066(14) 0.5201(12) 0.080(4) Uani 0.416(3) 1 d D U P E -2
H78A H 1.114544 0.050926 0.505391 0.096 Uiso 0.416(3) 1 calc R U P E -2
Cl1A Cl 0.9666(3) 0.1153(3) 0.5095(5) 0.092(2) Uani 0.416(3) 1 d D U P E -2
Cl2A Cl 1.1446(3) 0.2004(3) 0.4516(3) 0.0665(14) Uani 0.416(3) 1 d D U P E -2
Cl3A Cl 1.0981(5) 0.0917(5) 0.6195(4) 0.0896(19) Uani 0.416(3) 1 d D U P E -2
C78B C 0.8929(19) -0.0359(19) 0.6246(19) 0.146(6) Uani 0.166(3) 1 d D U P F -3
H78B H 0.878735 -0.055286 0.578056 0.175 Uiso 0.166(3) 1 calc R U P F -3
Cl1B Cl 0.7864(13) -0.0278(18) 0.6866(16) 0.169(9) Uani 0.166(3) 1 d D U P F -3
Cl2B Cl 0.9423(13) 0.0700(12) 0.5788(11) 0.114(5) Uani 0.166(3) 1 d D U P F -3
Cl3B Cl 0.9710(17) -0.1180(14) 0.6725(17) 0.171(6) Uani 0.166(3) 1 d D U P F -3
C74 C 0.4696(11) 0.4650(12) 0.3519(10) 0.061(4) Uani 0.5 1 d . . P G 1
H74A H 0.529934 0.442944 0.325244 0.091 Uiso 0.5 1 calc R U P G 1
H74B H 0.445395 0.521447 0.314007 0.091 Uiso 0.5 1 calc R U P G 1
H74C H 0.423618 0.418718 0.366100 0.091 Uiso 0.5 1 calc R U P G 1
C75 C 0.4846(5) 0.4829(5) 0.4287(4) 0.0506(18) Uani 1 1 d . . . . .
H75 H 0.474020 0.471274 0.380180 0.061 Uiso 0.5 1 calc R U P G 2
C76 C 0.5659(5) 0.4467(5) 0.4634(5) 0.0506(18) Uani 1 1 d . . . . .
H76 H 0.611610 0.409866 0.438305 0.061 Uiso 1 1 calc R U . . .
C77 C 0.5813(5) 0.4634(5) 0.5335(4) 0.0490(17) Uani 1 1 d . . . . .
H77 H 0.637556 0.437981 0.556367 0.059 Uiso 1 1 calc R U . . .
C78 C 0.9211(13) -0.0673(15) 0.9676(14) 0.110(5) Uani 0.419(3) 1 d D U P H -1
H78 H 0.918415 -0.123013 1.016747 0.132 Uiso 0.419(3) 1 calc R U P H -1
Cl1 Cl 0.8311(4) 0.0089(4) 0.9905(4) 0.099(2) Uani 0.419(3) 1 d D U P H -1
Cl2 Cl 0.9018(6) -0.1014(6) 0.8837(5) 0.113(2) Uani 0.419(3) 1 d D U P H -1
Cl3 Cl 1.0311(4) -0.0298(5) 0.9523(5) 0.108(2) Uani 0.419(3) 1 d D U P H -1
O4 O 0.4862(5) 0.2112(4) 0.2697(3) 0.0640(15) Uani 1 1 d . . . . .
H4A H 0.520(7) 0.253(7) 0.229(7) 0.096 Uiso 1 1 d . U . . .
H4B H 0.431(8) 0.249(7) 0.276(6) 0.096 Uiso 1 1 d . U . . .
C24 C 0.3544(16) 0.0150(18) 0.1840(13) 0.105(7) Uani 0.468(16) 1 d D U P A 2
H24D H 0.307294 0.041719 0.146879 0.158 Uiso 0.468(16) 1 calc R U P A 2
H24E H 0.364905 -0.050604 0.191225 0.158 Uiso 0.468(16) 1 calc R U P A 2
H24F H 0.414136 0.043898 0.160220 0.158 Uiso 0.468(16) 1 calc R U P A 2
C25 C 0.305(2) 0.1434(12) 0.225(2) 0.131(7) Uani 0.468(16) 1 d D U P A 2
H25D H 0.365039 0.166413 0.192606 0.196 Uiso 0.468(16) 1 calc R U P A 2
H25E H 0.286292 0.171453 0.269968 0.196 Uiso 0.468(16) 1 calc R U P A 2
H25F H 0.255883 0.158769 0.189598 0.196 Uiso 0.468(16) 1 calc R U P A 2
C41A C 0.7227(15) 0.140(2) 1.048(2) 0.070(7) Uani 0.245(17) 1 d D U P B 2
H41D H 0.727966 0.079957 1.089559 0.105 Uiso 0.245(17) 1 calc R U P B 2
H41E H 0.774132 0.175669 1.047518 0.105 Uiso 0.245(17) 1 calc R U P B 2
H41F H 0.727337 0.131030 0.993188 0.105 Uiso 0.245(17) 1 calc R U P B 2
C42A C 0.545(2) 0.159(2) 1.046(3) 0.078(8) Uani 0.245(17) 1 d D U P B 2
H42D H 0.565925 0.133803 0.999381 0.117 Uiso 0.245(17) 1 calc R U P B 2
H42E H 0.498416 0.211032 1.029541 0.117 Uiso 0.245(17) 1 calc R U P B 2
H42F H 0.514940 0.112014 1.093354 0.117 Uiso 0.245(17) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.529(9) . ?
C2 C3 1.598(8) . ?
C2 C4 1.591(10) . ?
C2 C5 1.575(10) . ?
C3 C6 1.542(8) . ?
C3 C9 1.520(10) . ?
C3 C48 1.495(10) . ?
C4 C7 1.535(10) . ?
C4 C14 1.529(8) . ?
C4 C31 1.531(8) . ?
C5 C8 1.546(9) . ?
C5 C26 1.516(8) . ?
C5 C47 1.532(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.394(8) . ?
C9 C14 1.381(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.370(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.388(10) . ?
C12 C13 1.399(9) . ?
C12 N1 1.420(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.393(11) . ?
C15 H15 0.9500 . ?
C15 C16 1.369(11) . ?
C15 N1 1.357(9) . ?
C16 C17 1.472(11) . ?
C16 N3 1.365(10) . ?
C17 C21 1.387(12) . ?
C17 N4 1.338(10) . ?
C18 C19 1.379(11) . ?
C18 C22 1.503(11) . ?
C18 N4 1.350(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.391(12) . ?
C20 H20 0.9500 . ?
C20 C21 1.382(12) . ?
C21 H21 0.9500 . ?
C22 N5 1.319(10) . ?
C22 O1 1.233(9) . ?
C23 H23 1.0000 . ?
C23 H23A 1.0000 . ?
C23 C24A 1.48(2) . ?
C23 C25A 1.677(19) . ?
C23 N5 1.450(11) . ?
C23 C24 1.49(2) . ?
C23 C25 1.673(19) . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
C26 C27 1.391(9) . ?
C26 C31 1.381(10) . ?
C27 H27 0.9500 . ?
C27 C28 1.389(8) . ?
C28 C29 1.373(9) . ?
C28 N6 1.437(8) . ?
C29 H29 0.9500 . ?
C29 C30 1.398(9) . ?
C30 H30 0.9500 . ?
C30 C31 1.381(9) . ?
C32 H32 0.9500 . ?
C32 C33 1.363(9) . ?
C32 N6 1.351(7) . ?
C33 C34 1.479(8) . ?
C33 N8 1.358(9) . ?
C34 C38 1.394(9) . ?
C34 N9 1.338(8) . ?
C35 C36 1.392(10) . ?
C35 C39 1.497(10) . ?
C35 N9 1.346(7) . ?
C36 H36 0.9500 . ?
C36 C37 1.382(10) . ?
C37 H37 0.9500 . ?
C37 C38 1.386(9) . ?
C38 H38 0.9500 . ?
C39 N10 1.326(9) . ?
C39 O2 1.242(7) . ?
C40 H40 1.0000 . ?
C40 H40A 1.0000 . ?
C40 C41 1.509(13) . ?
C40 C42 1.473(12) . ?
C40 N10 1.466(9) . ?
C40 C41A 1.528(16) . ?
C40 C42A 1.487(15) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43 0.9500 . ?
C43 C44 1.372(10) . ?
C43 C48 1.398(9) . ?
C44 C45 1.387(9) . ?
C44 N11 1.442(8) . ?
C45 H45 0.9500 . ?
C45 C46 1.389(9) . ?
C46 H46 0.9500 . ?
C46 C47 1.386(10) . ?
C47 C48 1.369(9) . ?
C49 H49 0.9500 . ?
C49 C50 1.375(8) . ?
C49 N11 1.334(9) . ?
C50 C51 1.458(9) . ?
C50 N13 1.370(8) . ?
C51 C55 1.389(9) . ?
C51 N14 1.347(8) . ?
C52 C53 1.381(10) . ?
C52 C56 1.526(9) . ?
C52 N14 1.337(8) . ?
C53 H53 0.9500 . ?
C53 C54 1.394(10) . ?
C54 H54 0.9500 . ?
C54 C55 1.368(10) . ?
C55 H55 0.9500 . ?
C56 N15 1.328(9) . ?
C56 O3 1.224(8) . ?
C57 H57 1.0000 . ?
C57 C58 1.519(10) . ?
C57 C59 1.505(11) . ?
C57 N15 1.483(8) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
N1 N2 1.351(9) . ?
N2 N3 1.315(10) . ?
N5 H5 0.8800 . ?
N6 N7 1.352(8) . ?
N7 N8 1.307(8) . ?
N10 H10A 0.8800 . ?
N11 N12 1.362(7) . ?
N12 N13 1.305(7) . ?
N15 H15A 0.8800 . ?
C60 C61 1.401(11) . ?
C60 C65 1.379(11) . ?
C60 C66 1.502(16) . ?
C61 H61 0.9500 . ?
C61 C62 1.383(12) . ?
C62 H62 0.9500 . ?
C62 C63 1.358(12) . ?
C63 H63 0.9500 . ?
C63 C64 1.382(12) . ?
C64 H64 0.9500 . ?
C64 C65 1.364(12) . ?
C65 H65 0.9500 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C60A C61A 1.402(12) . ?
C60A C65A 1.378(12) . ?
C60A C66A 1.509(16) . ?
C61A H61A 0.9500 . ?
C61A C62A 1.387(13) . ?
C62A H62A 0.9500 . ?
C62A C63A 1.351(13) . ?
C63A H63A 0.9500 . ?
C63A C64A 1.384(13) . ?
C64A H64A 0.9500 . ?
C64A C65A 1.358(13) . ?
C65A H65A 0.9500 . ?
C66A H66D 0.9800 . ?
C66A H66E 0.9800 . ?
C66A H66F 0.9800 . ?
C67 C68 1.428(14) . ?
C67 C72 1.393(14) . ?
C67 C73 1.410(18) . ?
C68 H68 0.9500 . ?
C68 C69 1.434(14) . ?
C69 H69 0.9500 . ?
C69 C70 1.397(14) . ?
C70 H70 0.9500 . ?
C70 C71 1.430(14) . ?
C71 H71 0.9500 . ?
C71 C72 1.424(14) . ?
C72 H72 0.9500 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9801 . ?
C73 H73C 0.9804 . ?
C67A C68A 1.437(15) . ?
C67A C72A 1.385(15) . ?
C67A C73A 1.407(19) . ?
C68A H68A 0.9500 . ?
C68A C69A 1.446(16) . ?
C69A H69A 0.9500 . ?
C69A C70A 1.383(15) . ?
C70A H70A 0.9500 . ?
C70A C71A 1.444(15) . ?
C71A H71A 0.9500 . ?
C71A C72A 1.421(15) . ?
C72A H72A 0.9500 . ?
C73A H73D 0.9798 . ?
C73A H73E 0.9801 . ?
C73A H73F 0.9802 . ?
C78A H78A 1.0000 . ?
C78A Cl1A 1.722(18) . ?
C78A Cl2A 1.77(2) . ?
C78A Cl3A 1.70(2) . ?
C78B H78B 1.0000 . ?
C78B Cl1B 1.72(2) . ?
C78B Cl2B 1.76(2) . ?
C78B Cl3B 1.70(2) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C74 C75 1.491(16) . ?
C75 H75 0.9500 . ?
C75 C76 1.385(10) . ?
C75 C77 1.391(11) 2_666 ?
C76 H76 0.9500 . ?
C76 C77 1.372(10) . ?
C77 H77 0.9500 . ?
C78 H78 1.0000 . ?
C78 Cl1 1.719(19) . ?
C78 Cl2 1.76(2) . ?
C78 Cl3 1.70(2) . ?
O4 H4A 0.90(11) . ?
O4 H4B 0.93(11) . ?
C24 H24D 0.9800 . ?
C24 H24E 0.9800 . ?
C24 H24F 0.9800 . ?
C25 H25D 0.9800 . ?
C25 H25E 0.9800 . ?
C25 H25F 0.9800 . ?
C41A H41D 0.9800 . ?
C41A H41E 0.9800 . ?
C41A H41F 0.9800 . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 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
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C3 113.0(5) . . ?
C1 C2 C4 111.6(6) . . ?
C1 C2 C5 112.6(6) . . ?
C4 C2 C3 106.3(5) . . ?
C5 C2 C3 106.1(5) . . ?
C5 C2 C4 106.8(5) . . ?
C6 C3 C2 115.6(5) . . ?
C9 C3 C2 104.0(6) . . ?
C9 C3 C6 111.1(6) . . ?
C48 C3 C2 104.1(5) . . ?
C48 C3 C6 110.9(6) . . ?
C48 C3 C9 110.6(5) . . ?
C7 C4 C2 116.3(6) . . ?
C14 C4 C2 104.2(5) . . ?
C14 C4 C7 109.6(6) . . ?
C14 C4 C31 114.2(5) . . ?
C31 C4 C2 103.5(6) . . ?
C31 C4 C7 109.2(5) . . ?
C8 C5 C2 117.2(5) . . ?
C26 C5 C2 104.5(6) . . ?
C26 C5 C8 110.6(5) . . ?
C26 C5 C47 110.5(5) . . ?
C47 C5 C2 104.2(5) . . ?
C47 C5 C8 109.6(6) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C3 127.0(6) . . ?
C14 C9 C3 112.7(5) . . ?
C14 C9 C10 120.3(7) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.7(7) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 119.9(6) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 121.5(7) . . ?
C11 C12 N1 118.6(6) . . ?
C13 C12 N1 119.8(7) . . ?
C12 C13 H13 121.2 . . ?
C14 C13 C12 117.5(7) . . ?
C14 C13 H13 121.2 . . ?
C9 C14 C4 112.3(6) . . ?
C9 C14 C13 121.1(6) . . ?
C13 C14 C4 126.5(6) . . ?
C16 C15 H15 127.8 . . ?
N1 C15 H15 127.8 . . ?
N1 C15 C16 104.4(7) . . ?
C15 C16 C17 128.9(7) . . ?
N3 C16 C15 108.9(7) . . ?
N3 C16 C17 122.2(8) . . ?
C21 C17 C16 121.8(7) . . ?
N4 C17 C16 114.8(7) . . ?
N4 C17 C21 123.3(7) . . ?
C19 C18 C22 119.7(7) . . ?
N4 C18 C19 124.1(8) . . ?
N4 C18 C22 116.2(7) . . ?
C18 C19 H19 121.0 . . ?
C18 C19 C20 117.9(8) . . ?
C20 C19 H19 121.0 . . ?
C19 C20 H20 120.5 . . ?
C21 C20 C19 119.0(8) . . ?
C21 C20 H20 120.5 . . ?
C17 C21 H21 120.6 . . ?
C20 C21 C17 118.8(8) . . ?
C20 C21 H21 120.6 . . ?
N5 C22 C18 117.0(7) . . ?
O1 C22 C18 119.4(8) . . ?
O1 C22 N5 123.5(8) . . ?
C24A C23 H23 115.3 . . ?
C24A C23 C25A 93.8(13) . . ?
C25A C23 H23 115.3 . . ?
N5 C23 H23 115.3 . . ?
N5 C23 H23A 112.1 . . ?
N5 C23 C24A 112.1(13) . . ?
N5 C23 C25A 102.4(10) . . ?
N5 C23 C24 111.7(13) . . ?
N5 C23 C25 114.0(12) . . ?
C24 C23 H23A 112.1 . . ?
C24 C23 C25 93.6(13) . . ?
C25 C23 H23A 112.1 . . ?
C23 C24A H24A 109.5 . . ?
C23 C24A H24B 109.5 . . ?
C23 C24A H24C 109.5 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C23 C25A H25A 109.5 . . ?
C23 C25A H25B 109.5 . . ?
C23 C25A H25C 109.5 . . ?
H25A C25A H25B 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C27 C26 C5 126.4(7) . . ?
C31 C26 C5 112.3(6) . . ?
C31 C26 C27 121.3(6) . . ?
C26 C27 H27 121.1 . . ?
C28 C27 C26 117.9(6) . . ?
C28 C27 H27 121.1 . . ?
C27 C28 N6 118.8(6) . . ?
C29 C28 C27 121.4(6) . . ?
C29 C28 N6 119.8(5) . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.3(6) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 120.6 . . ?
C31 C30 C29 118.9(7) . . ?
C31 C30 H30 120.6 . . ?
C26 C31 C4 112.4(6) . . ?
C26 C31 C30 120.3(6) . . ?
C30 C31 C4 127.2(7) . . ?
C33 C32 H32 127.8 . . ?
N6 C32 H32 127.8 . . ?
N6 C32 C33 104.3(6) . . ?
C32 C33 C34 128.1(6) . . ?
N8 C33 C32 109.0(5) . . ?
N8 C33 C34 122.9(6) . . ?
C38 C34 C33 121.6(6) . . ?
N9 C34 C33 115.0(6) . . ?
N9 C34 C38 123.4(6) . . ?
C36 C35 C39 120.2(6) . . ?
N9 C35 C36 122.9(6) . . ?
N9 C35 C39 116.9(6) . . ?
C35 C36 H36 120.4 . . ?
C37 C36 C35 119.2(6) . . ?
C37 C36 H36 120.4 . . ?
C36 C37 H37 120.8 . . ?
C36 C37 C38 118.5(7) . . ?
C38 C37 H37 120.8 . . ?
C34 C38 H38 120.6 . . ?
C37 C38 C34 118.7(7) . . ?
C37 C38 H38 120.6 . . ?
N10 C39 C35 116.6(5) . . ?
O2 C39 C35 119.5(7) . . ?
O2 C39 N10 124.0(7) . . ?
C41 C40 H40 106.0 . . ?
C42 C40 H40 106.0 . . ?
C42 C40 C41 118.4(10) . . ?
N10 C40 H40 106.0 . . ?
N10 C40 H40A 107.9 . . ?
N10 C40 C41 108.3(7) . . ?
N10 C40 C42 111.3(7) . . ?
N10 C40 C41A 111.0(13) . . ?
N10 C40 C42A 106.7(15) . . ?
C41A C40 H40A 107.9 . . ?
C42A C40 H40A 107.9 . . ?
C42A C40 C41A 115.3(14) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 H43 120.7 . . ?
C44 C43 C48 118.5(6) . . ?
C48 C43 H43 120.7 . . ?
C43 C44 C45 122.2(6) . . ?
C43 C44 N11 119.6(6) . . ?
C45 C44 N11 118.2(6) . . ?
C44 C45 H45 120.7 . . ?
C44 C45 C46 118.5(7) . . ?
C46 C45 H45 120.7 . . ?
C45 C46 H46 120.1 . . ?
C47 C46 C45 119.8(6) . . ?
C47 C46 H46 120.1 . . ?
C46 C47 C5 127.2(6) . . ?
C48 C47 C5 111.8(6) . . ?
C48 C47 C46 120.9(6) . . ?
C43 C48 C3 126.4(6) . . ?
C47 C48 C3 113.6(6) . . ?
C47 C48 C43 120.1(7) . . ?
C50 C49 H49 127.1 . . ?
N11 C49 H49 127.1 . . ?
N11 C49 C50 105.8(6) . . ?
C49 C50 C51 131.0(6) . . ?
N13 C50 C49 107.1(6) . . ?
N13 C50 C51 121.9(5) . . ?
C55 C51 C50 122.3(6) . . ?
N14 C51 C50 116.0(6) . . ?
N14 C51 C55 121.7(6) . . ?
C53 C52 C56 119.2(6) . . ?
N14 C52 C53 124.0(6) . . ?
N14 C52 C56 116.8(6) . . ?
C52 C53 H53 121.2 . . ?
C52 C53 C54 117.7(7) . . ?
C54 C53 H53 121.2 . . ?
C53 C54 H54 120.5 . . ?
C55 C54 C53 119.0(7) . . ?
C55 C54 H54 120.5 . . ?
C51 C55 H55 120.0 . . ?
C54 C55 C51 120.0(6) . . ?
C54 C55 H55 120.0 . . ?
N15 C56 C52 114.6(6) . . ?
O3 C56 C52 119.8(6) . . ?
O3 C56 N15 125.5(6) . . ?
C58 C57 H57 108.1 . . ?
C59 C57 H57 108.1 . . ?
C59 C57 C58 112.4(7) . . ?
N15 C57 H57 108.1 . . ?
N15 C57 C58 109.7(6) . . ?
N15 C57 C59 110.5(6) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C15 N1 C12 128.8(7) . . ?
N2 N1 C12 120.6(6) . . ?
N2 N1 C15 110.6(7) . . ?
N3 N2 N1 107.5(6) . . ?
N2 N3 C16 108.6(7) . . ?
C17 N4 C18 116.8(7) . . ?
C22 N5 C23 122.9(7) . . ?
C22 N5 H5 118.6 . . ?
C23 N5 H5 118.6 . . ?
C32 N6 C28 128.8(6) . . ?
C32 N6 N7 110.8(5) . . ?
N7 N6 C28 120.3(5) . . ?
N8 N7 N6 107.1(5) . . ?
N7 N8 C33 108.9(6) . . ?
C34 N9 C35 117.2(6) . . ?
C39 N10 C40 123.5(6) . . ?
C39 N10 H10A 118.3 . . ?
C40 N10 H10A 118.3 . . ?
C49 N11 C44 129.9(5) . . ?
C49 N11 N12 110.6(5) . . ?
N12 N11 C44 119.5(5) . . ?
N13 N12 N11 106.8(5) . . ?
N12 N13 C50 109.7(5) . . ?
C52 N14 C51 117.7(6) . . ?
C56 N15 C57 122.2(5) . . ?
C56 N15 H15A 118.9 . . ?
C57 N15 H15A 118.9 . . ?
C61 C60 C66 122.1(9) . . ?
C65 C60 C61 117.2(8) . . ?
C65 C60 C66 120.7(9) . . ?
C60 C61 H61 120.3 . . ?
C62 C61 C60 119.3(8) . . ?
C62 C61 H61 120.3 . . ?
C61 C62 H62 118.9 . . ?
C63 C62 C61 122.3(9) . . ?
C63 C62 H62 118.9 . . ?
C62 C63 H63 120.6 . . ?
C62 C63 C64 118.8(9) . . ?
C64 C63 H63 120.6 . . ?
C63 C64 H64 120.3 . . ?
C65 C64 C63 119.5(9) . . ?
C65 C64 H64 120.3 . . ?
C60 C65 H65 118.5 . . ?
C64 C65 C60 123.0(9) . . ?
C64 C65 H65 118.5 . . ?
C60 C66 H66A 109.5 . . ?
C60 C66 H66B 109.5 . . ?
C60 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C61A C60A C66A 122.8(10) . . ?
C65A C60A C61A 116.6(9) . . ?
C65A C60A C66A 120.6(10) . . ?
C60A C61A H61A 120.5 . . ?
C62A C61A C60A 119.1(9) . . ?
C62A C61A H61A 120.5 . . ?
C61A C62A H62A 118.6 . . ?
C63A C62A C61A 122.8(10) . . ?
C63A C62A H62A 118.6 . . ?
C62A C63A H63A 120.7 . . ?
C62A C63A C64A 118.6(10) . . ?
C64A C63A H63A 120.7 . . ?
C63A C64A H64A 120.4 . . ?
C65A C64A C63A 119.2(10) . . ?
C65A C64A H64A 120.4 . . ?
C60A C65A H65A 118.1 . . ?
C64A C65A C60A 123.8(9) . . ?
C64A C65A H65A 118.1 . . ?
C60A C66A H66D 109.5 . . ?
C60A C66A H66E 109.5 . . ?
C60A C66A H66F 109.5 . . ?
H66D C66A H66E 109.5 . . ?
H66D C66A H66F 109.5 . . ?
H66E C66A H66F 109.5 . . ?
C72 C67 C68 123.8(10) . . ?
C72 C67 C73 118.5(11) . . ?
C73 C67 C68 117.7(11) . . ?
C67 C68 H68 121.7 . . ?
C67 C68 C69 116.5(9) . . ?
C69 C68 H68 121.7 . . ?
C68 C69 H69 119.9 . . ?
C70 C69 C68 120.3(10) . . ?
C70 C69 H69 119.9 . . ?
C69 C70 H70 119.0 . . ?
C69 C70 C71 122.1(10) . . ?
C71 C70 H70 119.0 . . ?
C70 C71 H71 120.9 . . ?
C72 C71 C70 118.3(9) . . ?
C72 C71 H71 120.9 . . ?
C67 C72 C71 119.1(9) . . ?
C67 C72 H72 120.5 . . ?
C71 C72 H72 120.5 . . ?
C67 C73 H73A 109.4 . . ?
C67 C73 H73B 110.3 . . ?
C67 C73 H73C 108.7 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C72A C67A C68A 124.1(11) . . ?
C72A C67A C73A 118.5(13) . . ?
C73A C67A C68A 117.4(12) . . ?
C67A C68A H68A 122.4 . . ?
C67A C68A C69A 115.2(11) . . ?
C69A C68A H68A 122.4 . . ?
C68A C69A H69A 119.5 . . ?
C70A C69A C68A 121.1(11) . . ?
C70A C69A H69A 119.5 . . ?
C69A C70A H70A 118.9 . . ?
C69A C70A C71A 122.3(12) . . ?
C71A C70A H70A 118.9 . . ?
C70A C71A H71A 121.4 . . ?
C72A C71A C70A 117.2(11) . . ?
C72A C71A H71A 121.4 . . ?
C67A C72A C71A 119.9(11) . . ?
C67A C72A H72A 120.0 . . ?
C71A C72A H72A 120.0 . . ?
C67A C73A H73D 109.2 . . ?
C67A C73A H73E 109.6 . . ?
C67A C73A H73F 109.6 . . ?
H73D C73A H73E 109.5 . . ?
H73D C73A H73F 109.5 . . ?
H73E C73A H73F 109.5 . . ?
Cl1A C78A H78A 107.3 . . ?
Cl1A C78A Cl2A 112.2(11) . . ?
Cl2A C78A H78A 107.3 . . ?
Cl3A C78A H78A 107.3 . . ?
Cl3A C78A Cl1A 111.5(12) . . ?
Cl3A C78A Cl2A 111.1(11) . . ?
Cl1B C78B H78B 106.1 . . ?
Cl1B C78B Cl2B 112.4(13) . . ?
Cl2B C78B H78B 106.1 . . ?
Cl3B C78B H78B 106.1 . . ?
Cl3B C78B Cl1B 113.1(14) . . ?
Cl3B C78B Cl2B 112.4(13) . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C75 C74 H74A 109.5 . . ?
C75 C74 H74B 109.5 . . ?
C75 C74 H74C 109.5 . . ?
C76 C75 C74 120.1(9) . . ?
C76 C75 H75 120.7 . . ?
C76 C75 C77 118.5(7) . 2_666 ?
C77 C75 C74 121.4(9) 2_666 . ?
C77 C75 H75 120.7 2_666 . ?
C75 C76 H76 119.6 . . ?
C77 C76 C75 120.9(7) . . ?
C77 C76 H76 119.6 . . ?
C75 C77 H77 119.7 2_666 . ?
C76 C77 C75 120.6(7) . 2_666 ?
C76 C77 H77 119.7 . . ?
Cl1 C78 H78 106.7 . . ?
Cl1 C78 Cl2 110.8(11) . . ?
Cl2 C78 H78 106.7 . . ?
Cl3 C78 H78 106.7 . . ?
Cl3 C78 Cl1 113.7(12) . . ?
Cl3 C78 Cl2 111.9(12) . . ?
H4A O4 H4B 97(9) . . ?
C23 C24 H24D 109.5 . . ?
C23 C24 H24E 109.5 . . ?
C23 C24 H24F 109.5 . . ?
H24D C24 H24E 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
C23 C25 H25D 109.5 . . ?
C23 C25 H25E 109.5 . . ?
C23 C25 H25F 109.5 . . ?
H25D C25 H25E 109.5 . . ?
H25D C25 H25F 109.5 . . ?
H25E C25 H25F 109.5 . . ?
C40 C41A H41D 109.5 . . ?
C40 C41A H41E 109.5 . . ?
C40 C41A H41F 109.5 . . ?
H41D C41A H41E 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
C40 C42A H42D 109.5 . . ?
C40 C42A H42E 109.5 . . ?
C40 C42A H42F 109.5 . . ?
H42D C42A H42E 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C11 H11 O2 0.95 2.52 3.211(8) 130.0 1_554 yes
C15 H15 O4 0.95 2.44 3.387(10) 174.3 . yes
C32 H32 N14 0.95 2.45 3.402(9) 177.1 2_666 yes
C37 H37 N12 0.95 2.60 3.296(8) 130.6 1_556 yes
C49 H49 O1 0.95 2.18 3.067(8) 155.2 1_565 yes
C55 H55 O1 0.95 2.45 3.373(9) 165.2 1_565 yes
N10 H10A N13 0.88 2.29 3.084(7) 149.9 2_666 yes
N15 H15A N9 0.88 2.70 3.485(8) 149.7 2_666 yes
C65 H65 O3 0.95 2.68 3.424(16) 135.3 2_566 yes
C63A H63A N4 0.95 2.81 3.417(13) 122.3 2_656 yes
C65A H65A O3 0.95 2.49 3.436(12) 174.5 2_566 yes
C78A H78A N2 1.00 2.56 3.46(2) 148.8 2_756 yes
C78A H78A N3 1.00 2.28 3.01(2) 128.4 2_756 yes
C74 H74B N11 0.98 2.55 3.345(18) 137.9 . yes
C74 H74C N7 0.98 2.52 3.389(15) 148.3 2_666 yes
C78 H78 O3 1.00 2.26 3.17(2) 150.0 1_646 yes
O4 H4A O2 0.90(11) 1.91(11) 2.810(7) 174(10) 1_554 yes
O4 H4B N8 0.93(11) 2.19(11) 3.108(10) 167(9) 2_666 yes
C25 H25D O4 0.98 2.65 3.22(3) 117.8 . yes
C42A H42E N13 0.98 3.16 3.51(4) 102.7 2_666 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C6 -5.1(10) . . . . ?
C1 C2 C3 C9 117.0(7) . . . . ?
C1 C2 C3 C48 -127.1(7) . . . . ?
C1 C2 C4 C7 -1.1(8) . . . . ?
C1 C2 C4 C14 -121.8(5) . . . . ?
C1 C2 C4 C31 118.6(5) . . . . ?
C1 C2 C5 C8 6.5(8) . . . . ?
C1 C2 C5 C26 -116.3(6) . . . . ?
C1 C2 C5 C47 127.7(6) . . . . ?
C2 C3 C9 C10 -175.7(6) . . . . ?
C2 C3 C9 C14 8.3(7) . . . . ?
C2 C3 C48 C43 -177.8(6) . . . . ?
C2 C3 C48 C47 1.6(7) . . . . ?
C2 C4 C14 C9 3.4(7) . . . . ?
C2 C4 C14 C13 179.1(6) . . . . ?
C2 C4 C31 C26 1.3(6) . . . . ?
C2 C4 C31 C30 -174.9(6) . . . . ?
C2 C5 C26 C27 175.5(5) . . . . ?
C2 C5 C26 C31 -6.1(6) . . . . ?
C2 C5 C47 C46 176.6(6) . . . . ?
C2 C5 C47 C48 -2.9(7) . . . . ?
C3 C2 C4 C7 122.5(6) . . . . ?
C3 C2 C4 C14 1.8(6) . . . . ?
C3 C2 C4 C31 -117.8(5) . . . . ?
C3 C2 C5 C8 -117.6(6) . . . . ?
C3 C2 C5 C26 119.6(5) . . . . ?
C3 C2 C5 C47 3.7(6) . . . . ?
C3 C9 C10 C11 -176.7(6) . . . . ?
C3 C9 C14 C4 -7.6(8) . . . . ?
C3 C9 C14 C13 176.3(6) . . . . ?
C4 C2 C3 C6 -127.8(7) . . . . ?
C4 C2 C3 C9 -5.7(6) . . . . ?
C4 C2 C3 C48 110.2(6) . . . . ?
C4 C2 C5 C8 129.3(6) . . . . ?
C4 C2 C5 C26 6.5(6) . . . . ?
C4 C2 C5 C47 -109.5(5) . . . . ?
C5 C2 C3 C6 118.7(7) . . . . ?
C5 C2 C3 C9 -119.2(5) . . . . ?
C5 C2 C3 C48 -3.2(7) . . . . ?
C5 C2 C4 C7 -124.5(6) . . . . ?
C5 C2 C4 C14 114.8(5) . . . . ?
C5 C2 C4 C31 -4.8(6) . . . . ?
C5 C26 C27 C28 179.6(5) . . . . ?
C5 C26 C31 C4 3.1(7) . . . . ?
C5 C26 C31 C30 179.6(5) . . . . ?
C5 C47 C48 C3 0.8(8) . . . . ?
C5 C47 C48 C43 -179.7(6) . . . . ?
C6 C3 C9 C10 -50.7(9) . . . . ?
C6 C3 C9 C14 133.3(6) . . . . ?
C6 C3 C48 C43 57.2(9) . . . . ?
C6 C3 C48 C47 -123.4(6) . . . . ?
C7 C4 C14 C9 -121.7(7) . . . . ?
C7 C4 C14 C13 54.1(8) . . . . ?
C7 C4 C31 C26 125.7(6) . . . . ?
C7 C4 C31 C30 -50.5(8) . . . . ?
C8 C5 C26 C27 48.5(8) . . . . ?
C8 C5 C26 C31 -133.0(6) . . . . ?
C8 C5 C47 C46 -57.2(8) . . . . ?
C8 C5 C47 C48 123.3(6) . . . . ?
C9 C3 C48 C43 -66.7(8) . . . . ?
C9 C3 C48 C47 112.7(6) . . . . ?
C9 C10 C11 C12 1.5(11) . . . . ?
C10 C9 C14 C4 176.1(6) . . . . ?
C10 C9 C14 C13 0.0(10) . . . . ?
C10 C11 C12 C13 -1.1(11) . . . . ?
C10 C11 C12 N1 -178.2(7) . . . . ?
C11 C12 C13 C14 0.2(10) . . . . ?
C11 C12 N1 C15 -19.5(11) . . . . ?
C11 C12 N1 N2 159.5(7) . . . . ?
C12 C13 C14 C4 -175.1(6) . . . . ?
C12 C13 C14 C9 0.4(10) . . . . ?
C12 N1 N2 N3 -179.9(7) . . . . ?
C13 C12 N1 C15 163.4(7) . . . . ?
C13 C12 N1 N2 -17.6(10) . . . . ?
C14 C4 C31 C26 -111.3(7) . . . . ?
C14 C4 C31 C30 72.5(8) . . . . ?
C14 C9 C10 C11 -1.0(10) . . . . ?
C15 C16 C17 C21 -175.5(8) . . . . ?
C15 C16 C17 N4 3.1(12) . . . . ?
C15 C16 N3 N2 -0.5(9) . . . . ?
C15 N1 N2 N3 -0.7(9) . . . . ?
C16 C15 N1 C12 179.5(7) . . . . ?
C16 C15 N1 N2 0.4(8) . . . . ?
C16 C17 C21 C20 179.0(7) . . . . ?
C16 C17 N4 C18 -179.0(6) . . . . ?
C17 C16 N3 N2 -178.7(7) . . . . ?
C18 C19 C20 C21 -0.2(11) . . . . ?
C18 C22 N5 C23 179.9(9) . . . . ?
C19 C18 C22 N5 173.5(7) . . . . ?
C19 C18 C22 O1 -6.5(11) . . . . ?
C19 C18 N4 C17 0.0(11) . . . . ?
C19 C20 C21 C17 -0.1(12) . . . . ?
C21 C17 N4 C18 -0.3(11) . . . . ?
C22 C18 C19 C20 180.0(7) . . . . ?
C22 C18 N4 C17 -179.7(6) . . . . ?
C24A C23 N5 C22 -133.2(15) . . . . ?
C25A C23 N5 C22 127.5(12) . . . . ?
C26 C5 C47 C46 64.8(9) . . . . ?
C26 C5 C47 C48 -114.6(6) . . . . ?
C26 C27 C28 C29 -0.3(9) . . . . ?
C26 C27 C28 N6 -178.5(5) . . . . ?
C27 C26 C31 C4 -178.4(5) . . . . ?
C27 C26 C31 C30 -1.9(9) . . . . ?
C27 C28 C29 C30 0.0(9) . . . . ?
C27 C28 N6 C32 178.7(6) . . . . ?
C27 C28 N6 N7 2.8(8) . . . . ?
C28 C29 C30 C31 -0.6(9) . . . . ?
C28 N6 N7 N8 176.4(6) . . . . ?
C29 C28 N6 C32 0.5(9) . . . . ?
C29 C28 N6 N7 -175.3(6) . . . . ?
C29 C30 C31 C4 177.5(6) . . . . ?
C29 C30 C31 C26 1.5(9) . . . . ?
C31 C4 C14 C9 115.5(7) . . . . ?
C31 C4 C14 C13 -68.7(9) . . . . ?
C31 C26 C27 C28 1.3(8) . . . . ?
C32 C33 C34 C38 170.3(6) . . . . ?
C32 C33 C34 N9 -8.4(9) . . . . ?
C32 C33 N8 N7 0.2(8) . . . . ?
C32 N6 N7 N8 -0.2(8) . . . . ?
C33 C32 N6 C28 -175.9(6) . . . . ?
C33 C32 N6 N7 0.3(7) . . . . ?
C33 C34 C38 C37 -179.4(6) . . . . ?
C33 C34 N9 C35 -178.9(5) . . . . ?
C34 C33 N8 N7 -179.0(6) . . . . ?
C35 C36 C37 C38 1.1(9) . . . . ?
C35 C39 N10 C40 179.1(6) . . . . ?
C36 C35 C39 N10 167.8(6) . . . . ?
C36 C35 C39 O2 -11.4(9) . . . . ?
C36 C35 N9 C34 -2.3(9) . . . . ?
C36 C37 C38 C34 -1.0(10) . . . . ?
C38 C34 N9 C35 2.4(9) . . . . ?
C39 C35 C36 C37 -178.7(6) . . . . ?
C39 C35 N9 C34 177.1(5) . . . . ?
C41 C40 N10 C39 -74.3(11) . . . . ?
C42 C40 N10 C39 153.9(9) . . . . ?
C43 C44 C45 C46 -0.2(10) . . . . ?
C43 C44 N11 C49 167.0(7) . . . . ?
C43 C44 N11 N12 -12.5(9) . . . . ?
C44 C43 C48 C3 178.7(6) . . . . ?
C44 C43 C48 C47 -0.7(10) . . . . ?
C44 C45 C46 C47 0.3(10) . . . . ?
C44 N11 N12 N13 179.7(5) . . . . ?
C45 C44 N11 C49 -12.6(10) . . . . ?
C45 C44 N11 N12 167.9(6) . . . . ?
C45 C46 C47 C5 180.0(6) . . . . ?
C45 C46 C47 C48 -0.6(10) . . . . ?
C46 C47 C48 C3 -178.7(6) . . . . ?
C46 C47 C48 C43 0.8(10) . . . . ?
C47 C5 C26 C27 -73.0(7) . . . . ?
C47 C5 C26 C31 105.5(6) . . . . ?
C48 C3 C9 C10 73.0(8) . . . . ?
C48 C3 C9 C14 -103.0(6) . . . . ?
C48 C43 C44 C45 0.4(10) . . . . ?
C48 C43 C44 N11 -179.2(6) . . . . ?
C49 C50 C51 C55 16.3(11) . . . . ?
C49 C50 C51 N14 -161.8(7) . . . . ?
C49 C50 N13 N12 0.2(7) . . . . ?
C49 N11 N12 N13 0.1(7) . . . . ?
C50 C49 N11 C44 -179.6(6) . . . . ?
C50 C49 N11 N12 0.0(7) . . . . ?
C50 C51 C55 C54 -179.6(6) . . . . ?
C50 C51 N14 C52 179.1(5) . . . . ?
C51 C50 N13 N12 -179.4(6) . . . . ?
C52 C53 C54 C55 0.0(11) . . . . ?
C52 C56 N15 C57 -179.5(5) . . . . ?
C53 C52 C56 N15 -177.5(6) . . . . ?
C53 C52 C56 O3 2.2(9) . . . . ?
C53 C52 N14 C51 0.1(9) . . . . ?
C53 C54 C55 C51 1.0(11) . . . . ?
C55 C51 N14 C52 1.0(9) . . . . ?
C56 C52 C53 C54 177.6(6) . . . . ?
C56 C52 N14 C51 -178.1(5) . . . . ?
C58 C57 N15 C56 100.9(8) . . . . ?
C59 C57 N15 C56 -134.7(6) . . . . ?
N1 C12 C13 C14 177.2(6) . . . . ?
N1 C15 C16 C17 178.1(7) . . . . ?
N1 C15 C16 N3 0.0(8) . . . . ?
N1 N2 N3 C16 0.7(9) . . . . ?
N3 C16 C17 C21 2.3(12) . . . . ?
N3 C16 C17 N4 -179.0(7) . . . . ?
N4 C17 C21 C20 0.4(12) . . . . ?
N4 C18 C19 C20 0.3(11) . . . . ?
N4 C18 C22 N5 -6.8(10) . . . . ?
N4 C18 C22 O1 173.2(7) . . . . ?
N6 C28 C29 C30 178.1(5) . . . . ?
N6 C32 C33 C34 178.8(6) . . . . ?
N6 C32 C33 N8 -0.4(7) . . . . ?
N6 N7 N8 C33 0.0(8) . . . . ?
N8 C33 C34 C38 -10.7(10) . . . . ?
N8 C33 C34 N9 170.6(6) . . . . ?
N9 C34 C38 C37 -0.8(10) . . . . ?
N9 C35 C36 C37 0.6(9) . . . . ?
N9 C35 C39 N10 -11.6(8) . . . . ?
N9 C35 C39 O2 169.2(6) . . . . ?
N11 C44 C45 C46 179.3(6) . . . . ?
N11 C49 C50 C51 179.4(6) . . . . ?
N11 C49 C50 N13 -0.1(7) . . . . ?
N11 N12 N13 C50 -0.2(7) . . . . ?
N13 C50 C51 C55 -164.3(6) . . . . ?
N13 C50 C51 N14 17.6(9) . . . . ?
N14 C51 C55 C54 -1.6(10) . . . . ?
N14 C52 C53 C54 -0.5(10) . . . . ?
N14 C52 C56 N15 0.8(8) . . . . ?
N14 C52 C56 O3 -179.5(6) . . . . ?
O1 C22 N5 C23 -0.1(14) . . . . ?
O2 C39 N10 C40 -1.7(11) . . . . ?
O3 C56 N15 C57 0.8(10) . . . . ?
C60 C61 C62 C63 0.1(3) . . . . ?
C61 C60 C65 C64 -0.1(7) . . . . ?
C61 C62 C63 C64 -0.2(7) . . . . ?
C62 C63 C64 C65 0.1(9) . . . . ?
C63 C64 C65 C60 0.0(9) . . . . ?
C65 C60 C61 C62 0.1(3) . . . . ?
C66 C60 C61 C62 -180.0(3) . . . . ?
C66 C60 C65 C64 179.9(5) . . . . ?
C60A C61A C62A C63A 0.0(3) . . . . ?
C61A C60A C65A C64A 0.2(6) . . . . ?
C61A C62A C63A C64A 0.0(6) . . . . ?
C62A C63A C64A C65A 0.1(8) . . . . ?
C63A C64A C65A C60A -0.3(9) . . . . ?
C65A C60A C61A C62A -0.1(3) . . . . ?
C66A C60A C61A C62A 180.0(3) . . . . ?
C66A C60A C65A C64A -179.9(5) . . . . ?
C67 C68 C69 C70 0.0(3) . . . . ?
C68 C67 C72 C71 0.3(6) . . . . ?
C68 C69 C70 C71 0.0(6) . . . . ?
C69 C70 C71 C72 0.2(8) . . . . ?
C70 C71 C72 C67 -0.3(8) . . . . ?
C72 C67 C68 C69 -0.1(3) . . . . ?
C73 C67 C68 C69 179.9(3) . . . . ?
C73 C67 C72 C71 -179.7(5) . . . . ?
C67A C68A C69A C70A 0(3) . . . . ?
C68A C67A C72A C71A 5(4) . . . . ?
C68A C69A C70A C71A 0(4) . . . . ?
C69A C70A C71A C72A 3(3) . . . . ?
C70A C71A C72A C67A -5(3) . . . . ?
C72A C67A C68A C69A -2(3) . . . . ?
C73A C67A C68A C69A -180(2) . . . . ?
C73A C67A C72A C71A -177(2) . . . . ?
C74 C75 C76 C77 179.2(9) . . . . ?
C75 C76 C77 C75 0.0(11) . . . 2_666 ?
C77 C75 C76 C77 0.0(11) 2_666 . . . ?
C24 C23 N5 C22 -84.4(15) . . . . ?
C25 C23 N5 C22 171.1(15) . . . . ?
C41A C40 N10 C39 -117.2(19) . . . . ?
C42A C40 N10 C39 116(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.794
_oxdiff_exptl_absorpt_empirical_full_min 0.344
# start Validation Reply Form
_vrf_PLAT084_PhMe                
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.36 Report
RESPONSE: Small and poor crystal, combined with highly disorder in
 the crystal structure, leading to a bad and weak diffraction.
;
_vrf_PLAT340_PhMe                
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01051 Ang.
RESPONSE: The small crystal size and absence of heavy atoms in 
the structure resulted in weak diffraction intensity. 
;
# end Validation Reply Form

####################################################################### 
# 
# 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_o-xylene
_audit_block_doi                 10.5517/ccdc.csd.cc2m123w
_database_code_depnum_ccdc_archive 'CCDC 2414097'
loop_
_audit_author_name
_audit_author_address
'Tianshu Yang'
;FUJIAN NORMAL UNIVERSITY
China
;
_audit_update_record             
;
2025-02-12 deposited with the CCDC.	2025-02-27 downloaded from the CCDC.
;
_audit_creation_date             2025-02-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C59 H57 N15 O3), 3(C8 H10), 3(C H Cl3), 2(H2 O)'
_chemical_formula_sum            'C145 H151 Cl9 N30 O8'
_chemical_formula_weight         2761.00
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHONCl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.8347(8)
_cell_length_b                   15.5615(9)
_cell_length_c                   16.9145(9)
_cell_angle_alpha                72.925(5)
_cell_angle_beta                 81.228(4)
_cell_angle_gamma                82.651(4)
_cell_volume                     3674.6(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6257
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.4390
_cell_measurement_theta_min      2.7540
_shelx_estimated_absorpt_T_max   0.818
_shelx_estimated_absorpt_T_min   0.773
_exptl_absorpt_coefficient_mu    2.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.127a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1406
_diffrn_reflns_av_unetI/netI     0.1261
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40218
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.465
_diffrn_reflns_theta_min         2.753
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00 -28.00   0.50    1.10    --    0.00 -72.00  -7.00   52
  2  ω    -39.00  76.00   0.50    1.10    --    0.00  72.00 122.00  230
  3  ω   -111.00 -17.00   0.50    4.38    --  -55.91 -72.00  -7.00  188
  4  ω    -82.00 -28.00   0.50    4.38    --  -55.91  72.00 122.00  108
  5  ω    -16.00  10.00   0.50    4.38    --  -55.91  72.00 122.00   52
  6  ω     13.00 122.00   0.50    4.38    --   55.91  72.00 122.00  218
  7  ω   -115.00 -59.00   0.50    4.38    --  -97.00 -72.00  -7.00  112
  8  ω    -78.00 -53.00   0.50    4.38    --  -97.00  72.00 122.00   50
  9  ω     89.00 170.00   0.50    4.38    --  111.81  72.00 122.00  162
 10  ω     50.00  80.00   0.50    4.38    --  111.81 -72.00  -7.00   60
 11  ω    -92.00 -48.00   0.50    1.10    --    0.00 179.00-150.00   88
 12  ω    -13.00  12.00   0.50    1.10    --    0.00 -72.00  -7.00   50
 13  ω    -18.00  27.00   0.50    4.38    --  -55.91  19.00-120.00   90
 14  ω    -28.00  21.00   0.50    4.38    --  -55.91  19.00  90.00   98
 15  ω    -18.00  25.00   0.50    4.38    --  -55.91  19.00 -60.00   86
 16  ω   -107.00 -26.00   0.50    4.38    --  -55.91 125.00 -90.00  162
 17  ω   -145.00-100.00   0.50    4.38    --  -55.91 -99.00-180.00   90
 18  ω   -111.00 -31.00   0.50    4.38    --  -55.91 125.00 120.00  160
 19  ω   -131.00 -82.00   0.50    4.38    --  -55.91-125.00  30.00   98
 20  ω   -131.00 -83.00   0.50    4.38    --  -55.91-125.00  90.00   96
 21  ω    -36.00  22.00   0.50    4.38    --   55.91 -19.00  60.00  116
 22  ω     -2.00  23.00   0.50    4.38    --   55.91 -72.00  -7.00   50
 23  ω     76.00 130.00   0.50    4.38    --   55.91 125.00  30.00  108
 24  ω    -20.00  11.00   0.50    4.38    --   55.91 -19.00-180.00   62
 25  ω    -46.00 -15.00   0.50    4.38    --  -97.00  38.00 120.00   62
 26  ω    -44.00 -15.00   0.50    4.38    --  -97.00  38.00 -60.00   58
 27  ω    -45.00 -15.00   0.50    4.38    --  -97.00  38.00  60.00   60
 28  ω   -150.00 -86.00   0.50    4.38    --  -97.00 -92.00  90.00  128
 29  ω   -151.00 -49.00   0.50    4.38    --  -97.00 179.00  90.00  204
 30  ω     50.00 123.00   0.50    4.38    --  111.81 179.00 -60.00  146
 31  ω    110.00 173.00   0.50    4.38    --  111.81  38.00  90.00  126
 32  ω     43.00  69.00   0.50    4.38    --  111.81-111.00 -30.00   52
 33  ω     29.00  54.00   0.50    4.38    --  111.81 -50.00-120.00   50
 34  ω     51.00 100.00   0.50    4.38    --  111.81  38.00  90.00   98
 35  ω     69.00 146.00   0.50    4.38    --  111.81  50.00 -60.00  154
 36  ω     89.00 175.00   0.50    4.38    --  111.81 111.00-120.00  172
 37  ω     82.00 144.00   0.50    4.38    --  111.81  64.00   0.00  124
 38  ω     30.00  63.00   0.50    4.38    --  111.81 -64.00 -60.00   66
 39  ω     78.00 108.00   0.50    4.38    --  111.81-111.00   0.00   60
 40  ω     51.00 101.00   0.50    4.38    --  111.81-111.00-150.00  100
 41  ω     37.00  99.00   0.50    4.38    --  111.81 -77.00  90.00  124
 42  ω    146.00 172.00   0.50    4.38    --  111.81 111.00   0.00   52
 43  ω    106.00 132.00   0.50    4.38    --  111.81 111.00   0.00   52
 44  ω     42.00 146.00   0.50    4.38    --  111.81 179.00 150.00  208
 45  ω     98.00 124.00   0.50    4.38    --  111.81 179.00 -90.00   52
 46  ω     28.00  54.00   0.50    4.38    --  111.81 -50.00-150.00   52
 47  ω     57.00  89.00   0.50    4.38    --  111.81 179.00 -90.00   64
 48  ω     28.00  53.00   0.50    4.38    --  111.81 -50.00 120.00   50
 49  ω     68.00 108.00   0.50    4.38    --  111.81-111.00  90.00   80
 50  ω     58.00 116.00   0.50    4.38    --  111.81  38.00 150.00  116
 51  ω    135.00 172.00   0.50    4.38    --  111.81  38.00 150.00   74
 52  ω     31.00 107.00   0.50    4.38    --  111.81-111.00 -90.00  152
 53  ω     31.00 108.00   0.50    4.38    --  111.81-111.00-180.00  154
 54  ω     25.00  98.00   0.50    4.38    --  111.81-111.00 120.00  146
 55  ω     79.00 139.00   0.50    4.38    --  111.81 179.00  30.00  120
 56  ω     62.00  95.00   0.50    4.38    --  111.81 -77.00 -60.00   66
 57  ω     28.00  53.00   0.50    4.38    --  111.81 -50.00   0.00   50
 58  ω     29.00  54.00   0.50    4.38    --  111.81 -50.00 -60.00   50
 59  ω     25.00 161.00   0.50    4.38    --  111.81  25.00-120.00  272
 60  ω     80.00 107.00   0.50    4.38    --  111.81-111.00 -30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0542963000
_diffrn_orient_matrix_UB_12      0.0489780000
_diffrn_orient_matrix_UB_13      0.0417035000
_diffrn_orient_matrix_UB_21      0.0234684000
_diffrn_orient_matrix_UB_22      -0.0900609000
_diffrn_orient_matrix_UB_23      0.0646843000
_diffrn_orient_matrix_UB_31      0.0873422000
_diffrn_orient_matrix_UB_32      -0.0172965000
_diffrn_orient_matrix_UB_33      -0.0573608000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4608
_reflns_number_total             14035
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.127a 64-bit (release 16-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         14035
_refine_ls_number_restraints     1488
_refine_ls_R_factor_all          0.2876
_refine_ls_R_factor_gt           0.1353
_refine_ls_restrained_S_all      1.141
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3432
_refine_ls_wR_factor_ref         0.4357
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Cl1-Cl2 \\sim Cl1-Cl3 \\sim Cl2-Cl3
 with sigma of 0.02
 C67-C61 \\sim C66-C60
 with sigma of 0.02
 Cl2-C76 \\sim Cl3-C76 \\sim Cl1-C76
 with sigma of 0.02
 C67-C62 \\sim C67-C60
 with sigma of 0.02
 C60-C62 \\sim C61-C63 \\sim C62-C64 \\sim C63-C65 \\sim C64-C60 \\sim C65-C61
 with sigma of 0.02
 C61-C60 \\sim C62-C61 \\sim C63-C62 \\sim C64-C63 \\sim C65-C64 \\sim C65-C60
 with sigma of 0.02
 C66-C61 \\sim C66-C65
 with sigma of 0.02
 C75-C68 \\sim C75-C70
 with sigma of 0.02
 C69-C68 \\sim C70-C69 \\sim C71-C70 \\sim C72-C71 \\sim C73-C72 \\sim C73-C68
 with sigma of 0.02
 C68-C70 \\sim C69-C71 \\sim C70-C72 \\sim C71-C73 \\sim C72-C68 \\sim C73-C69
 with sigma of 0.02
 C74-C73 \\sim C74-C69
 with sigma of 0.02
3. Restrained planarity
 C60, C61, C62, C63, C64, C65, C66, C67
 with sigma of 0.01
 C68, C69, C70, C71, C72, C73, C74, C75
 with sigma of 0.01
 C68A, C69A, C70A, C71A, C72A, C73A, C74A, C75A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C76 \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim C76A \\sim Cl1A \\sim Cl2A \\sim Cl3A
\\sim C76B \\sim Cl1B \\sim Cl2B \\sim Cl3B \\sim C76C \\sim Cl1C \\sim Cl2C
\\sim Cl3C \\sim C76D \\sim Cl1D \\sim Cl2D \\sim Cl3D \\sim C76E \\sim Cl1E
\\sim Cl2E \\sim Cl3E \\sim C76F \\sim Cl1F \\sim Cl2F \\sim Cl3F: within 2.5A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
N5 \\sim C23 \\sim C24 \\sim C25 \\sim C23A \\sim C24A \\sim C25A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N15 \\sim C57 \\sim C58 \\sim C59 \\sim C57A \\sim C58A \\sim C59A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C40 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim
C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim N1 \\sim
N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N9 \\sim N10
\\sim N11 \\sim N12 \\sim N13 \\sim N14 \\sim N15 \\sim O3 \\sim O2 \\sim O1
\\sim C23 \\sim C24 \\sim C25 \\sim C41 \\sim C42 \\sim C41A \\sim C42A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim
C68A \\sim C69A \\sim C70A \\sim C71A \\sim C72A \\sim C73A \\sim C74A \\sim
C75A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
C63 \\sim C62 \\sim C61 \\sim C67 \\sim C60 \\sim C65 \\sim C64 \\sim C66:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Same fragment restrains
{C40, C41A, C42A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C40, C41, C42}
{N15, C57A, C58A, C59A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{N15, C57, C58, C59}
{C76D, Cl1D, Cl2D, Cl3D} sigma for 1-2: 0.01, 1-3: 0.01
{C76E, Cl1E, Cl2E, Cl3E} sigma for 1-2: 0.01, 1-3: 0.01
{C76F, Cl1F, Cl2F, Cl3F} sigma for 1-2: 0.01, 1-3: 0.01
{C76A, Cl1A, Cl2A, Cl3A} sigma for 1-2: 0.01, 1-3: 0.01
{C76B, Cl1B, Cl2B, Cl3B} sigma for 1-2: 0.01, 1-3: 0.01
{C76C, Cl1C, Cl2C, Cl3C} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C76, Cl1, Cl2, Cl3}
{N5, C23A, C24A, C25A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{N5, C23, C24, C25}
{C68A, C69A, C70A, C71A, C72A, C73A, C74A, C75A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C68, C69, C70, C71, C72, C73, C74, C75}
6. Others
 1*[Sof(C76)+Sof(H76)+Sof(Cl1)+Sof(Cl2)+Sof(Cl3)]+1*[Sof(C76A)+Sof(H76A)+
 Sof(Cl1A)+Sof(Cl2A)+Sof(Cl3A)]+1*[Sof(C76B)+Sof(H76B)+Sof(Cl1B)+Sof(Cl2B)+
 Sof(Cl3B)]+1*[Sof(C76C)+Sof(H76C)+Sof(Cl1C)+Sof(Cl2C)+Sof(Cl3C)]+1*[Sof(C76D)+
 Sof(H76D)+Sof(Cl1D)+Sof(Cl2D)+Sof(Cl3D)]+1*[Sof(C76E)+Sof(H76E)+Sof(Cl1E)+
 Sof(Cl2E)+Sof(Cl3E)]+1*[Sof(C76F)+Sof(H76F)+Sof(Cl1F)+Sof(Cl2F)+Sof(Cl3F)]=1.5
 with esd of 0
 Sof(H5B)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(H5A)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(H40A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42D)=
 Sof(H42E)=Sof(H42F)=1-FVAR(2)
 Sof(H40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=FVAR(2)
 Sof(C68A)=Sof(C69A)=Sof(C70A)=Sof(H70A)=Sof(C71A)=Sof(H71A)=Sof(C72A)=
 Sof(H72A)=Sof(C73A)=Sof(H73A)=Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=
 Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=1-FVAR(3)
 Sof(C68)=Sof(C69)=Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72)=
 Sof(C73)=Sof(H73)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C75)=Sof(H75A)=
 Sof(H75B)=Sof(H75C)=FVAR(3)
 Sof(H15B)=Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=
 Sof(C59A)=Sof(H59D)=Sof(H59E)=Sof(H59F)=1-FVAR(4)
 Sof(H15A)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=
 Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(4)
 Sof(C76)=Sof(H76)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(5)
 Sof(C76A)=Sof(H76A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(6)
 Sof(C76B)=Sof(H76B)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=FVAR(7)
 Sof(C76C)=Sof(H76C)=Sof(Cl1C)=Sof(Cl2C)=Sof(Cl3C)=FVAR(8)
 Sof(C76D)=Sof(H76D)=Sof(Cl1D)=Sof(Cl2D)=Sof(Cl3D)=FVAR(9)
 Sof(C76E)=Sof(H76E)=Sof(Cl1E)=Sof(Cl2E)=Sof(Cl3E)=FVAR(10)
 Sof(C76F)=Sof(H76F)=Sof(Cl1F)=Sof(Cl2F)=Sof(Cl3F)=FVAR(11)
 Fixed Sof: C60(0.5) C61(0.5) C62(0.5) H62(0.5) C63(0.5) H63(0.5) C64(0.5)
 H64(0.5) C65(0.5) H65(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) C67(0.5)
 H67A(0.5) H67B(0.5) H67C(0.5)
7.a Riding coordinates:
 O4(H4A,H4B)
7.b Ternary CH refined with riding coordinates:
 C40(H40), C40(H40A), C23(H23), C57(H57), C76(H76), C76A(H76A), C76B(H76B),
 C76C(H76C), C76D(H76D), C76E(H76E), C76F(H76F), C23A(H23A), C57A(H57A)
7.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C15(H15), C19(H19), C20(H20), C21(H21),
 C27(H27), C28(H28), C30(H30), C32(H32), C36(H36), C37(H37), C38(H38), C44(H44),
  C46(H46), C47(H47), C49(H49), C53(H53), C54(H54), C55(H55), N5(H5A), N5(H5B),
 N10(H10A), N15(H15A), N15(H15B), C70(H70), C71(H71), C72(H72), C73(H73),
 C70A(H70A), C71A(H71A), C72A(H72A), C73A(H73A), C62(H62), C63(H63), C64(H64),
 C65(H65)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C), C74A(H74D,H74E,H74F), C75A(H75D,H75E,H75F), C66(H66A,H66B,H66C),
 C67(H67A,H67B,H67C), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C41A(H41D,
 H41E,H41F), C42A(H42D,H42E,H42F), C58A(H58D,H58E,H58F), C59A(H59D,H59E,H59F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.0178(4) 0.4455(6) 0.7237(4) 0.110(3) Uani 1 1 d . . . . .
H1A H 0.024351 0.385832 0.763897 0.165 Uiso 1 1 calc R U . . .
H1B H -0.023870 0.444355 0.684293 0.165 Uiso 1 1 calc R U . . .
H1C H -0.007151 0.490475 0.753222 0.165 Uiso 1 1 calc R U . . .
C2 C 0.1132(4) 0.4705(5) 0.6753(4) 0.0825(19) Uani 1 1 d . . . . .
C3 C 0.1831(4) 0.4754(5) 0.7351(4) 0.086(2) Uani 1 1 d . . . . .
C4 C 0.1063(4) 0.5667(5) 0.6074(4) 0.0819(19) Uani 1 1 d . . . . .
C5 C 0.1576(4) 0.4002(5) 0.6269(4) 0.0765(18) Uani 1 1 d . . . . .
C6 C 0.1497(5) 0.4451(6) 0.8291(4) 0.104(2) Uani 1 1 d . . . . .
H6A H 0.091733 0.479728 0.840722 0.156 Uiso 1 1 calc R U . . .
H6B H 0.195600 0.455603 0.860409 0.156 Uiso 1 1 calc R U . . .
H6C H 0.140457 0.380661 0.845970 0.156 Uiso 1 1 calc R U . . .
C7 C 0.0107(5) 0.6184(6) 0.6002(5) 0.103(2) Uani 1 1 d . . . . .
H7A H -0.027855 0.585917 0.578738 0.154 Uiso 1 1 calc R U . . .
H7B H 0.016642 0.679010 0.561972 0.154 Uiso 1 1 calc R U . . .
H7C H -0.017313 0.623212 0.655229 0.154 Uiso 1 1 calc R U . . .
C8 C 0.1040(5) 0.3193(5) 0.6360(4) 0.102(2) Uani 1 1 d . . . . .
H8A H 0.099456 0.281828 0.694026 0.153 Uiso 1 1 calc R U . . .
H8B H 0.135845 0.283482 0.599569 0.153 Uiso 1 1 calc R U . . .
H8C H 0.042413 0.340833 0.620404 0.153 Uiso 1 1 calc R U . . .
C9 C 0.2067(4) 0.5713(5) 0.7056(4) 0.0814(19) Uani 1 1 d . . . . .
C10 C 0.2639(5) 0.6110(6) 0.7426(5) 0.098(2) Uani 1 1 d . . . . .
H10 H 0.289741 0.577297 0.791699 0.118 Uiso 1 1 calc R U . . .
C11 C 0.2805(5) 0.6984(6) 0.7059(5) 0.102(2) Uani 1 1 d . . . . .
H11 H 0.317210 0.726700 0.730595 0.123 Uiso 1 1 calc R U . . .
C12 C 0.2446(5) 0.7475(6) 0.6326(5) 0.096(2) Uani 1 1 d . . . . .
C13 C 0.1889(4) 0.7084(5) 0.5964(4) 0.090(2) Uani 1 1 d . . . . .
H13 H 0.164885 0.742011 0.546266 0.107 Uiso 1 1 calc R U . . .
C14 C 0.1687(4) 0.6208(5) 0.6336(4) 0.0826(19) Uani 1 1 d . . . . .
C15 C 0.3380(6) 0.8779(7) 0.6086(5) 0.109(2) Uani 1 1 d . . . . .
H15 H 0.384086 0.852461 0.644155 0.131 Uiso 1 1 calc R U . . .
C16 C 0.3291(6) 0.9638(8) 0.5585(6) 0.121(3) Uani 1 1 d . . . . .
C17 C 0.3815(6) 1.0400(7) 0.5441(6) 0.108(2) Uani 1 1 d . . . . .
C18 C 0.5045(6) 1.0929(7) 0.5774(6) 0.106(2) Uani 1 1 d . . . . .
C19 C 0.4900(6) 1.1753(7) 0.5209(6) 0.115(3) Uani 1 1 d . . . . .
H19 H 0.527968 1.222187 0.514637 0.138 Uiso 1 1 calc R U . . .
C20 C 0.4197(7) 1.1886(7) 0.4738(6) 0.118(3) Uani 1 1 d . . . . .
H20 H 0.409318 1.244830 0.433401 0.141 Uiso 1 1 calc R U . . .
C21 C 0.3650(7) 1.1220(7) 0.4845(6) 0.123(3) Uani 1 1 d . . . . .
H21 H 0.316011 1.130864 0.451855 0.148 Uiso 1 1 calc R U . . .
C22 C 0.5803(7) 1.0772(7) 0.6303(6) 0.113(3) Uani 1 1 d . . . . .
C26 C 0.1434(4) 0.5474(5) 0.5256(4) 0.0737(17) Uani 1 1 d . . . . .
C27 C 0.1503(4) 0.6064(5) 0.4463(5) 0.0830(19) Uani 1 1 d . . . . .
H27 H 0.131209 0.668662 0.438748 0.100 Uiso 1 1 calc R U . . .
C28 C 0.1851(4) 0.5753(5) 0.3775(4) 0.0759(17) Uani 1 1 d . . . . .
H28 H 0.189174 0.615839 0.323017 0.091 Uiso 1 1 calc R U . . .
C29 C 0.2137(4) 0.4843(5) 0.3894(4) 0.0750(18) Uani 1 1 d . . . . .
C30 C 0.2063(4) 0.4234(5) 0.4682(4) 0.0773(18) Uani 1 1 d . . . . .
H30 H 0.224920 0.361057 0.475968 0.093 Uiso 1 1 calc R U . . .
C31 C 0.1707(4) 0.4565(6) 0.5353(4) 0.0770(19) Uani 1 1 d . . . . .
C32 C 0.2713(4) 0.4987(5) 0.2387(4) 0.0765(18) Uani 1 1 d . . . . .
H32 H 0.258812 0.561660 0.214691 0.092 Uiso 1 1 calc R U . . .
C33 C 0.3112(5) 0.4373(5) 0.1994(5) 0.0834(19) Uani 1 1 d . . . . .
C34 C 0.3468(4) 0.4494(5) 0.1104(4) 0.0791(18) Uani 1 1 d . . . . .
C35 C 0.3778(4) 0.5530(6) -0.0160(5) 0.0830(19) Uani 1 1 d . . . . .
C36 C 0.4095(4) 0.4857(7) -0.0538(5) 0.087(2) Uani 1 1 d . . . . .
H36 H 0.432681 0.500496 -0.111262 0.105 Uiso 1 1 calc R U . . .
C37 C 0.4072(5) 0.3974(7) -0.0077(5) 0.095(2) Uani 1 1 d . . . . .
H37 H 0.426038 0.349910 -0.032953 0.114 Uiso 1 1 calc R U . . .
C38 C 0.3770(4) 0.3791(5) 0.0759(5) 0.0842(19) Uani 1 1 d . . . . .
H38 H 0.376906 0.318392 0.109837 0.101 Uiso 1 1 calc R U . . .
C39 C 0.3790(5) 0.6484(6) -0.0636(5) 0.090(2) Uani 1 1 d . . . . .
C40 C 0.3638(6) 0.8068(6) -0.0597(6) 0.128(2) Uani 1 1 d D U . . .
H40 H 0.410320 0.816982 -0.110145 0.153 Uiso 0.678(10) 1 calc R U P A 1
H40A H 0.356193 0.818689 -0.119788 0.153 Uiso 0.322(10) 1 calc R U P A 2
C41 C 0.2679(9) 0.8442(10) -0.0907(10) 0.148(4) Uani 0.678(10) 1 d D U P A 1
H41A H 0.219860 0.832665 -0.043065 0.222 Uiso 0.678(10) 1 calc R U P A 1
H41B H 0.256509 0.813804 -0.130963 0.222 Uiso 0.678(10) 1 calc R U P A 1
H41C H 0.267457 0.909250 -0.117279 0.222 Uiso 0.678(10) 1 calc R U P A 1
C42 C 0.3888(11) 0.8547(8) -0.0062(9) 0.129(3) Uani 0.678(10) 1 d D U P A 1
H42A H 0.386744 0.919380 -0.035085 0.194 Uiso 0.678(10) 1 calc R U P A 1
H42B H 0.450842 0.832572 0.007771 0.194 Uiso 0.678(10) 1 calc R U P A 1
H42C H 0.345672 0.844715 0.044992 0.194 Uiso 0.678(10) 1 calc R U P A 1
C43 C 0.2664(4) 0.4122(4) 0.7156(4) 0.0763(16) Uani 1 1 d . U . . .
C44 C 0.3490(4) 0.3957(5) 0.7477(4) 0.0769(16) Uani 1 1 d . U . . .
H44 H 0.359569 0.424829 0.787120 0.092 Uiso 1 1 calc R U . . .
C45 C 0.4154(5) 0.3372(5) 0.7220(4) 0.0768(16) Uani 1 1 d . U . . .
C46 C 0.4015(5) 0.2931(4) 0.6655(4) 0.0821(17) Uani 1 1 d . U . . .
H46 H 0.448170 0.251855 0.648972 0.099 Uiso 1 1 calc R U . . .
C47 C 0.3181(5) 0.3101(5) 0.6331(4) 0.0838(18) Uani 1 1 d . U . . .
H47 H 0.307659 0.280129 0.594227 0.101 Uiso 1 1 calc R U . . .
C48 C 0.2502(5) 0.3704(5) 0.6573(4) 0.0765(16) Uani 1 1 d . U . . .
C49 C 0.5803(4) 0.2787(4) 0.7295(4) 0.0783(16) Uani 1 1 d . U . . .
H49 H 0.592193 0.252996 0.684062 0.094 Uiso 1 1 calc R U . . .
C50 C 0.6410(4) 0.2797(4) 0.7827(4) 0.0780(16) Uani 1 1 d . U . . .
C51 C 0.7353(5) 0.2444(5) 0.7863(4) 0.0844(17) Uani 1 1 d . U . . .
C52 C 0.8702(5) 0.2428(5) 0.8386(4) 0.0827(17) Uani 1 1 d . U . . .
C53 C 0.9173(5) 0.1829(5) 0.7952(5) 0.100(2) Uani 1 1 d . U . . .
H53 H 0.979869 0.162480 0.800102 0.120 Uiso 1 1 calc R U . . .
C54 C 0.8681(5) 0.1544(5) 0.7446(6) 0.111(2) Uani 1 1 d . U . . .
H54 H 0.897409 0.114859 0.713259 0.133 Uiso 1 1 calc R U . . .
C55 C 0.7777(5) 0.1838(5) 0.7404(5) 0.098(2) Uani 1 1 d . U . . .
H55 H 0.743493 0.163821 0.707056 0.118 Uiso 1 1 calc R U . . .
C56 C 0.9205(5) 0.2784(5) 0.8937(5) 0.0915(18) Uani 1 1 d . U . . .
N1 N 0.2677(5) 0.8351(5) 0.5978(4) 0.117(2) Uani 1 1 d . U . . .
N2 N 0.2176(5) 0.8931(5) 0.5429(5) 0.130(2) Uani 1 1 d . U . . .
N3 N 0.2529(6) 0.9709(5) 0.5187(5) 0.144(3) Uani 1 1 d . U . . .
N4 N 0.4520(5) 1.0236(5) 0.5903(4) 0.111(2) Uani 1 1 d . . . . .
N5 N 0.5949(5) 0.9928(5) 0.6792(5) 0.131(2) Uani 1 1 d D U . . .
H5A H 0.561404 0.951224 0.676565 0.158 Uiso 0.600(10) 1 calc R U P B 1
H5B H 0.557574 0.951985 0.682410 0.158 Uiso 0.400(10) 1 calc R U P B 2
C23 C 0.6656(10) 0.9667(12) 0.7378(9) 0.142(3) Uani 0.600(10) 1 d D U P B 1
H23 H 0.661862 1.016160 0.765217 0.171 Uiso 0.600(10) 1 calc R U P B 1
C24 C 0.6494(11) 0.8792(10) 0.8079(11) 0.151(4) Uani 0.600(10) 1 d D U P B 1
H24A H 0.593117 0.888477 0.844179 0.227 Uiso 0.600(10) 1 calc R U P B 1
H24B H 0.701325 0.862717 0.840592 0.227 Uiso 0.600(10) 1 calc R U P B 1
H24C H 0.643581 0.830555 0.783538 0.227 Uiso 0.600(10) 1 calc R U P B 1
C25 C 0.7619(10) 0.9619(11) 0.6912(11) 0.142(4) Uani 0.600(10) 1 d D U P B 1
H25A H 0.770471 0.910443 0.667705 0.212 Uiso 0.600(10) 1 calc R U P B 1
H25B H 0.807181 0.954428 0.729819 0.212 Uiso 0.600(10) 1 calc R U P B 1
H25C H 0.769964 1.017746 0.646094 0.212 Uiso 0.600(10) 1 calc R U P B 1
N6 N 0.2528(4) 0.4520(4) 0.3189(3) 0.0811(15) Uani 1 1 d . U . . .
N7 N 0.2816(5) 0.3640(5) 0.3320(4) 0.1044(18) Uani 1 1 d . U . . .
N8 N 0.3190(5) 0.3555(5) 0.2571(5) 0.114(2) Uani 1 1 d . U . . .
N9 N 0.3449(3) 0.5359(4) 0.0662(3) 0.0766(14) Uani 1 1 d . . . . .
N10 N 0.3646(4) 0.7099(4) -0.0227(4) 0.0980(18) Uani 1 1 d . U . . .
H10A H 0.354678 0.690603 0.032001 0.118 Uiso 1 1 calc R U . . .
N11 N 0.5015(4) 0.3206(4) 0.7537(3) 0.0776(13) Uani 1 1 d . U . . .
N12 N 0.5115(4) 0.3473(4) 0.8216(3) 0.0869(15) Uani 1 1 d . U . . .
N13 N 0.5961(4) 0.3217(4) 0.8381(3) 0.0883(15) Uani 1 1 d . U . . .
N14 N 0.7828(3) 0.2735(3) 0.8346(3) 0.0780(14) Uani 1 1 d . U . . .
N15 N 0.8748(4) 0.3389(4) 0.9273(3) 0.0859(15) Uani 1 1 d D U . . .
H15A H 0.815981 0.350557 0.922248 0.103 Uiso 0.54(6) 1 calc R U P C 1
H15B H 0.819723 0.360423 0.913686 0.103 Uiso 0.46(6) 1 calc R U P C 2
C57 C 0.9146(12) 0.3892(14) 0.9730(13) 0.087(3) Uani 0.54(6) 1 d D U P C 1
H57 H 0.982802 0.380447 0.961220 0.105 Uiso 0.54(6) 1 calc R U P C 1
C58 C 0.886(2) 0.4884(12) 0.942(2) 0.094(5) Uani 0.54(6) 1 d D U P C 1
H58A H 0.905364 0.509625 0.882108 0.142 Uiso 0.54(6) 1 calc R U P C 1
H58B H 0.915918 0.521417 0.971019 0.142 Uiso 0.54(6) 1 calc R U P C 1
H58C H 0.819823 0.498991 0.953383 0.142 Uiso 0.54(6) 1 calc R U P C 1
C59 C 0.889(2) 0.352(2) 1.0660(11) 0.113(6) Uani 0.54(6) 1 d D U P C 1
H59A H 0.824145 0.341123 1.077443 0.170 Uiso 0.54(6) 1 calc R U P C 1
H59B H 0.900008 0.396042 1.094127 0.170 Uiso 0.54(6) 1 calc R U P C 1
H59C H 0.926418 0.295528 1.086607 0.170 Uiso 0.54(6) 1 calc R U P C 1
O3 O 0.6242(4) 1.1383(4) 0.6294(4) 0.1278(19) Uani 1 1 d . . . . .
O2 O 0.3974(3) 0.6681(4) -0.1426(3) 0.1125(17) Uani 1 1 d . . . . .
O1 O 1.0031(3) 0.2517(3) 0.8979(3) 0.1075(15) Uani 1 1 d . U . . .
O4 O 0.5067(4) 0.7829(4) 0.7300(3) 0.1273(18) Uani 1 1 d . . . . .
H4A H 0.467034 0.753438 0.768435 0.191 Uiso 1 1 d R U . . .
H4B H 0.554874 0.744638 0.729605 0.191 Uiso 1 1 d R U . . .
C68 C 0.3763(8) 0.1032(5) 0.8436(6) 0.157(3) Uani 0.800(8) 1 d D U P D 1
C69 C 0.3000(7) 0.1545(6) 0.8708(6) 0.161(3) Uani 0.800(8) 1 d D U P D 1
C70 C 0.2168(7) 0.1613(6) 0.8406(6) 0.157(3) Uani 0.800(8) 1 d D U P D 1
H70 H 0.165683 0.196508 0.859595 0.188 Uiso 0.800(8) 1 calc R U P D 1
C71 C 0.2084(8) 0.1175(7) 0.7836(7) 0.161(3) Uani 0.800(8) 1 d D U P D 1
H71 H 0.151428 0.121588 0.763045 0.194 Uiso 0.800(8) 1 calc R U P D 1
C72 C 0.2841(8) 0.0666(7) 0.7558(7) 0.162(3) Uani 0.800(8) 1 d D U P D 1
H72 H 0.278695 0.036269 0.715706 0.195 Uiso 0.800(8) 1 calc R U P D 1
C73 C 0.3638(8) 0.0601(6) 0.7849(6) 0.155(3) Uani 0.800(8) 1 d D U P D 1
H73 H 0.414214 0.024785 0.764923 0.185 Uiso 0.800(8) 1 calc R U P D 1
C74 C 0.4629(9) 0.0946(8) 0.8740(8) 0.174(5) Uani 0.800(8) 1 d D U P D 1
H74A H 0.473834 0.152231 0.881731 0.261 Uiso 0.800(8) 1 calc R U P D 1
H74B H 0.511615 0.077816 0.833746 0.261 Uiso 0.800(8) 1 calc R U P D 1
H74C H 0.462567 0.047756 0.927467 0.261 Uiso 0.800(8) 1 calc R U P D 1
C75 C 0.3105(11) 0.2063(9) 0.9381(9) 0.190(6) Uani 0.800(8) 1 d D U P D 1
H75A H 0.353406 0.170066 0.976358 0.285 Uiso 0.800(8) 1 calc R U P D 1
H75B H 0.250699 0.215299 0.969691 0.285 Uiso 0.800(8) 1 calc R U P D 1
H75C H 0.333875 0.264991 0.909232 0.285 Uiso 0.800(8) 1 calc R U P D 1
C76 C 0.9177(8) 0.8848(10) 0.4820(8) 0.151(4) Uani 0.585(3) 1 d D U P E 1
H76 H 0.888286 0.939886 0.497901 0.181 Uiso 0.585(3) 1 calc R U P E 1
Cl1 Cl 0.8980(3) 0.9074(3) 0.3799(3) 0.1556(18) Uani 0.585(3) 1 d D U P E 1
Cl2 Cl 0.8600(2) 0.8000(2) 0.5510(3) 0.1352(16) Uani 0.585(3) 1 d D U P E 1
Cl3 Cl 1.0296(3) 0.8846(3) 0.4939(4) 0.1530(19) Uani 0.585(3) 1 d D U P E 1
C68A C 0.350(2) 0.0488(16) 0.8059(17) 0.159(4) Uani 0.200(8) 1 d D U P D 2
C69A C 0.306(2) 0.1037(16) 0.8557(15) 0.160(4) Uani 0.200(8) 1 d D U P D 2
C70A C 0.212(2) 0.122(2) 0.865(2) 0.160(4) Uani 0.200(8) 1 d D U P D 2
H70A H 0.183688 0.158918 0.898402 0.191 Uiso 0.200(8) 1 calc R U P D 2
C71A C 0.1601(18) 0.086(2) 0.825(2) 0.163(4) Uani 0.200(8) 1 d D U P D 2
H71A H 0.095391 0.097816 0.830849 0.195 Uiso 0.200(8) 1 calc R U P D 2
C72A C 0.202(2) 0.031(2) 0.775(2) 0.167(4) Uani 0.200(8) 1 d D U P D 2
H72A H 0.166257 0.006032 0.747115 0.200 Uiso 0.200(8) 1 calc R U P D 2
C73A C 0.293(2) 0.0138(19) 0.7667(19) 0.161(4) Uani 0.200(8) 1 d D U P D 2
H73A H 0.320391 -0.023850 0.732730 0.194 Uiso 0.200(8) 1 calc R U P D 2
C74A C 0.447(2) 0.030(3) 0.797(3) 0.172(7) Uani 0.200(8) 1 d D U P D 2
H74D H 0.475445 0.074728 0.813089 0.258 Uiso 0.200(8) 1 calc R U P D 2
H74E H 0.469239 0.033179 0.738235 0.258 Uiso 0.200(8) 1 calc R U P D 2
H74F H 0.463676 -0.030465 0.831988 0.258 Uiso 0.200(8) 1 calc R U P D 2
C75A C 0.370(3) 0.145(3) 0.902(2) 0.151(6) Uani 0.200(8) 1 d D U P D 2
H75D H 0.376695 0.103927 0.957559 0.227 Uiso 0.200(8) 1 calc R U P D 2
H75E H 0.341361 0.203799 0.907512 0.227 Uiso 0.200(8) 1 calc R U P D 2
H75F H 0.430305 0.152745 0.869392 0.227 Uiso 0.200(8) 1 calc R U P D 2
C76A C 1.039(3) 0.9508(19) 0.6032(19) 0.254(6) Uani 0.129(3) 1 d D U P F -7
H76A H 1.098229 0.926109 0.577521 0.304 Uiso 0.129(3) 1 calc R U P F -7
Cl1A Cl 1.058(3) 0.922(2) 0.7056(19) 0.277(6) Uani 0.129(3) 1 d D U P F -7
Cl2A Cl 1.039(3) 1.0619(17) 0.551(2) 0.279(12) Uani 0.129(3) 1 d D U P F -7
Cl3A Cl 0.9636(18) 0.8911(15) 0.581(2) 0.202(6) Uani 0.129(3) 1 d D U P F -7
C76B C 0.974(2) 0.7951(19) 0.8128(16) 0.281(6) Uani 0.217(3) 1 d D U P G 3
H76B H 1.021546 0.750762 0.841698 0.337 Uiso 0.217(3) 1 calc R U P G 3
Cl1B Cl 0.8998(16) 0.7248(13) 0.8017(16) 0.271(6) Uani 0.217(3) 1 d D U P G 3
Cl2B Cl 0.9363(18) 0.8544(17) 0.8830(14) 0.283(6) Uani 0.217(3) 1 d D U P G 3
Cl3B Cl 1.0363(15) 0.8495(17) 0.7237(14) 0.281(6) Uani 0.217(3) 1 d D U P G 3
C76C C 0.985(2) 0.8117(19) 0.8286(17) 0.280(5) Uani 0.176(3) 1 d D U P H 4
H76C H 1.035130 0.769674 0.855755 0.336 Uiso 0.176(3) 1 calc R U P H 4
Cl1C Cl 0.8929(19) 0.783(2) 0.9025(17) 0.276(6) Uani 0.176(3) 1 d D U P H 4
Cl2C Cl 1.023(2) 0.9136(16) 0.816(2) 0.286(6) Uani 0.176(3) 1 d D U P H 4
Cl3C Cl 0.986(2) 0.7788(19) 0.7414(16) 0.260(7) Uani 0.176(3) 1 d D U P H 4
C76D C 1.030(3) 0.899(3) 0.847(3) 0.281(5) Uani 0.083(3) 1 d D U P I 5
H76D H 1.047461 0.837172 0.882913 0.337 Uiso 0.083(3) 1 calc R U P I 5
Cl1D Cl 0.917(3) 0.894(4) 0.843(4) 0.281(6) Uani 0.083(3) 1 d D U P I 5
Cl2D Cl 1.055(4) 0.965(4) 0.904(4) 0.286(9) Uani 0.083(3) 1 d D U P I 5
Cl3D Cl 1.100(4) 0.901(4) 0.757(3) 0.278(7) Uani 0.083(3) 1 d D U P I 5
C76E C 0.9262(19) 1.001(2) 0.953(2) 0.289(9) Uani 0.159(3) 1 d D U P J -6
H76E H 0.935461 1.057582 0.906572 0.346 Uiso 0.159(3) 1 calc R U P J -6
Cl1E Cl 0.994(2) 0.923(2) 0.912(2) 0.285(7) Uani 0.159(3) 1 d D U P J -6
Cl2E Cl 0.8115(16) 0.9971(18) 0.960(2) 0.287(10) Uani 0.159(3) 1 d D U P J -6
Cl3E Cl 0.966(2) 1.027(2) 1.031(2) 0.294(13) Uani 0.159(3) 1 d D U P J -6
C76F C 0.923(3) 0.8196(19) 0.889(2) 0.280(6) Uani 0.151(3) 1 d D U P F 7
H76F H 0.979067 0.792942 0.916093 0.336 Uiso 0.151(3) 1 calc R U P F 7
Cl1F Cl 0.851(2) 0.7352(16) 0.932(2) 0.273(8) Uani 0.151(3) 1 d D U P F 7
Cl2F Cl 0.896(3) 0.9143(17) 0.921(2) 0.285(6) Uani 0.151(3) 1 d D U P F 7
Cl3F Cl 0.963(2) 0.834(2) 0.7871(18) 0.281(5) Uani 0.151(3) 1 d D U P F 7
C60 C 0.5466(11) 0.4682(9) 0.5146(10) 0.112(5) Uani 0.5 1 d D U P K -1
C61 C 0.4743(10) 0.4973(9) 0.4668(10) 0.110(5) Uani 0.5 1 d D U P K -1
C62 C 0.4075(10) 0.5624(8) 0.4856(10) 0.111(5) Uani 0.5 1 d D U P K -1
H62 H 0.357638 0.583074 0.453617 0.133 Uiso 0.5 1 calc R U P K -1
C63 C 0.4142(10) 0.5967(9) 0.5514(10) 0.121(4) Uani 0.5 1 d D U P K -1
H63 H 0.368371 0.640929 0.563773 0.145 Uiso 0.5 1 calc R U P K -1
C64 C 0.4855(10) 0.5684(9) 0.5990(10) 0.115(4) Uani 0.5 1 d D U P K -1
H64 H 0.489081 0.592733 0.643702 0.138 Uiso 0.5 1 calc R U P K -1
C65 C 0.5528(11) 0.5030(9) 0.5803(10) 0.115(5) Uani 0.5 1 d D U P K -1
H65 H 0.602583 0.482436 0.612461 0.139 Uiso 0.5 1 calc R U P K -1
C66 C 0.6199(13) 0.3978(12) 0.4959(12) 0.120(6) Uani 0.5 1 d D U P K -1
H66A H 0.593107 0.340501 0.506393 0.180 Uiso 0.5 1 calc R U P K -1
H66B H 0.668252 0.389488 0.531679 0.180 Uiso 0.5 1 calc R U P K -1
H66C H 0.646082 0.417619 0.437301 0.180 Uiso 0.5 1 calc R U P K -1
C67 C 0.4677(13) 0.4585(12) 0.3943(14) 0.132(7) Uani 0.5 1 d D U P K -1
H67A H 0.525617 0.463351 0.357369 0.199 Uiso 0.5 1 calc R U P K -1
H67B H 0.417932 0.492585 0.363014 0.199 Uiso 0.5 1 calc R U P K -1
H67C H 0.455254 0.394982 0.416414 0.199 Uiso 0.5 1 calc R U P K -1
C23A C 0.6744(11) 0.9684(16) 0.7281(11) 0.141(4) Uani 0.400(10) 1 d D U P B 2
H23A H 0.722247 1.009659 0.696621 0.169 Uiso 0.400(10) 1 calc R U P B 2
C24A C 0.6535(18) 0.9830(16) 0.8153(13) 0.163(6) Uani 0.400(10) 1 d D U P B 2
H24D H 0.603223 1.030519 0.815290 0.244 Uiso 0.400(10) 1 calc R U P B 2
H24E H 0.708100 1.001163 0.830032 0.244 Uiso 0.400(10) 1 calc R U P B 2
H24F H 0.635691 0.926809 0.856061 0.244 Uiso 0.400(10) 1 calc R U P B 2
C25A C 0.7161(17) 0.8727(14) 0.7317(16) 0.156(6) Uani 0.400(10) 1 d D U P B 2
H25D H 0.673716 0.829290 0.766523 0.234 Uiso 0.400(10) 1 calc R U P B 2
H25E H 0.774111 0.861753 0.755581 0.234 Uiso 0.400(10) 1 calc R U P B 2
H25F H 0.727329 0.865450 0.675283 0.234 Uiso 0.400(10) 1 calc R U P B 2
C41A C 0.2846(16) 0.8672(16) -0.0218(19) 0.139(4) Uani 0.322(10) 1 d D U P A 2
H41D H 0.278580 0.927633 -0.060940 0.208 Uiso 0.322(10) 1 calc R U P A 2
H41E H 0.299669 0.871879 0.031119 0.208 Uiso 0.322(10) 1 calc R U P A 2
H41F H 0.226772 0.839539 -0.012313 0.208 Uiso 0.322(10) 1 calc R U P A 2
C42A C 0.4526(12) 0.8360(17) -0.057(2) 0.135(5) Uani 0.322(10) 1 d D U P A 2
H42D H 0.499888 0.809009 -0.091789 0.202 Uiso 0.322(10) 1 calc R U P A 2
H42E H 0.467098 0.816762 0.000677 0.202 Uiso 0.322(10) 1 calc R U P A 2
H42F H 0.450596 0.901957 -0.077765 0.202 Uiso 0.322(10) 1 calc R U P A 2
C57A C 0.9125(15) 0.3723(17) 0.9872(13) 0.092(3) Uani 0.46(6) 1 d D U P C 2
H57A H 0.980264 0.356740 0.981827 0.111 Uiso 0.46(6) 1 calc R U P C 2
C58A C 0.895(3) 0.4735(16) 0.966(2) 0.088(5) Uani 0.46(6) 1 d D U P C 2
H58D H 0.919798 0.500387 0.908296 0.132 Uiso 0.46(6) 1 calc R U P C 2
H58E H 0.925326 0.495734 1.003235 0.132 Uiso 0.46(6) 1 calc R U P C 2
H58F H 0.829136 0.490313 0.973890 0.132 Uiso 0.46(6) 1 calc R U P C 2
C59A C 0.873(3) 0.327(2) 1.0756(9) 0.104(5) Uani 0.46(6) 1 d D U P C 2
H59D H 0.863981 0.263947 1.080271 0.155 Uiso 0.46(6) 1 calc R U P C 2
H59E H 0.814802 0.358748 1.089680 0.155 Uiso 0.46(6) 1 calc R U P C 2
H59F H 0.916307 0.327191 1.114128 0.155 Uiso 0.46(6) 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.557(9) . ?
C2 C3 1.579(8) . ?
C2 C4 1.599(9) . ?
C2 C5 1.574(9) . ?
C3 C6 1.541(9) . ?
C3 C9 1.498(9) . ?
C3 C43 1.536(9) . ?
C4 C7 1.541(9) . ?
C4 C14 1.518(9) . ?
C4 C26 1.509(9) . ?
C5 C8 1.531(9) . ?
C5 C31 1.537(9) . ?
C5 C48 1.510(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.419(9) . ?
C9 C14 1.393(9) . ?
C10 H10 0.9500 . ?
C10 C11 1.356(10) . ?
C11 H11 0.9500 . ?
C11 C12 1.395(10) . ?
C12 C13 1.390(9) . ?
C12 N1 1.382(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.374(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.358(11) . ?
C15 N1 1.368(9) . ?
C16 C17 1.443(12) . ?
C16 N3 1.378(10) . ?
C17 C21 1.394(12) . ?
C17 N4 1.353(10) . ?
C18 C19 1.370(11) . ?
C18 C22 1.494(12) . ?
C18 N4 1.358(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.366(11) . ?
C20 H20 0.9500 . ?
C20 C21 1.352(11) . ?
C21 H21 0.9500 . ?
C22 N5 1.342(10) . ?
C22 O3 1.213(9) . ?
C26 C27 1.382(9) . ?
C26 C31 1.390(9) . ?
C27 H27 0.9500 . ?
C27 C28 1.393(9) . ?
C28 H28 0.9500 . ?
C28 C29 1.390(9) . ?
C29 C30 1.388(8) . ?
C29 N6 1.441(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.385(9) . ?
C32 H32 0.9500 . ?
C32 C33 1.345(9) . ?
C32 N6 1.343(8) . ?
C33 C34 1.482(10) . ?
C33 N8 1.362(9) . ?
C34 C38 1.381(9) . ?
C34 N9 1.334(8) . ?
C35 C36 1.379(10) . ?
C35 C39 1.468(10) . ?
C35 N9 1.360(8) . ?
C36 H36 0.9500 . ?
C36 C37 1.368(10) . ?
C37 H37 0.9500 . ?
C37 C38 1.373(9) . ?
C38 H38 0.9500 . ?
C39 N10 1.316(9) . ?
C39 O2 1.273(8) . ?
C40 H40 1.0000 . ?
C40 H40A 1.0000 . ?
C40 C41 1.573(13) . ?
C40 C42 1.442(12) . ?
C40 N10 1.452(10) . ?
C40 C41A 1.585(15) . ?
C40 C42A 1.460(15) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.379(8) . ?
C43 C48 1.394(8) . ?
C44 H44 0.9500 . ?
C44 C45 1.364(9) . ?
C45 C46 1.381(8) . ?
C45 N11 1.424(8) . ?
C46 H46 0.9500 . ?
C46 C47 1.393(8) . ?
C47 H47 0.9500 . ?
C47 C48 1.385(9) . ?
C49 H49 0.9500 . ?
C49 C50 1.371(8) . ?
C49 N11 1.333(8) . ?
C50 C51 1.439(9) . ?
C50 N13 1.344(8) . ?
C51 C55 1.421(10) . ?
C51 N14 1.358(8) . ?
C52 C53 1.405(9) . ?
C52 C56 1.534(10) . ?
C52 N14 1.327(8) . ?
C53 H53 0.9500 . ?
C53 C54 1.399(10) . ?
C54 H54 0.9500 . ?
C54 C55 1.365(10) . ?
C55 H55 0.9500 . ?
C56 N15 1.304(9) . ?
C56 O1 1.249(8) . ?
N1 N2 1.332(9) . ?
N2 N3 1.308(9) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C23 1.489(12) . ?
N5 C23A 1.489(13) . ?
C23 H23 1.0000 . ?
C23 C24 1.54(2) . ?
C23 C25 1.528(18) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
N6 N7 1.345(7) . ?
N7 N8 1.340(8) . ?
N10 H10A 0.8800 . ?
N11 N12 1.363(7) . ?
N12 N13 1.314(7) . ?
N15 H15A 0.8800 . ?
N15 H15B 0.8800 . ?
N15 C57 1.475(9) . ?
N15 C57A 1.472(10) . ?
C57 H57 1.0000 . ?
C57 C58 1.503(12) . ?
C57 C59 1.513(12) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
O4 H4A 0.8701 . ?
O4 H4B 0.8702 . ?
C68 C69 1.398(11) . ?
C68 C73 1.396(12) . ?
C68 C74 1.432(16) . ?
C69 C70 1.388(11) . ?
C69 C75 1.610(17) . ?
C70 H70 0.9500 . ?
C70 C71 1.361(11) . ?
C71 H71 0.9500 . ?
C71 C72 1.392(11) . ?
C72 H72 0.9500 . ?
C72 C73 1.330(11) . ?
C73 H73 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76 1.0000 . ?
C76 Cl1 1.721(11) . ?
C76 Cl2 1.707(10) . ?
C76 Cl3 1.703(11) . ?
C68A C69A 1.403(14) . ?
C68A C73A 1.391(14) . ?
C68A C74A 1.433(17) . ?
C69A C70A 1.384(13) . ?
C69A C75A 1.612(19) . ?
C70A H70A 0.9500 . ?
C70A C71A 1.358(13) . ?
C71A H71A 0.9500 . ?
C71A C72A 1.395(14) . ?
C72A H72A 0.9500 . ?
C72A C73A 1.335(14) . ?
C73A H73A 0.9500 . ?
C74A H74D 0.9800 . ?
C74A H74E 0.9800 . ?
C74A H74F 0.9800 . ?
C75A H75D 0.9800 . ?
C75A H75E 0.9800 . ?
C75A H75F 0.9800 . ?
C76A H76A 1.0000 . ?
C76A Cl1A 1.713(15) . ?
C76A Cl2A 1.697(14) . ?
C76A Cl3A 1.694(14) . ?
Cl1A Cl3F 2.13(5) . ?
C76B H76B 1.0000 . ?
C76B Cl1B 1.709(15) . ?
C76B Cl2B 1.698(14) . ?
C76B Cl3B 1.694(14) . ?
C76C H76C 1.0000 . ?
C76C Cl1C 1.711(15) . ?
C76C Cl2C 1.697(14) . ?
C76C Cl3C 1.696(14) . ?
C76D H76D 1.0000 . ?
C76D Cl1D 1.714(15) . ?
C76D Cl2D 1.699(14) . ?
C76D Cl3D 1.697(14) . ?
C76E H76E 1.0000 . ?
C76E Cl1E 1.710(15) . ?
C76E Cl2E 1.695(14) . ?
C76E Cl3E 1.693(14) . ?
C76F H76F 1.0000 . ?
C76F Cl1F 1.712(15) . ?
C76F Cl2F 1.700(14) . ?
C76F Cl3F 1.694(14) . ?
C60 C61 1.391(14) . ?
C60 C65 1.391(15) . ?
C60 C66 1.51(2) . ?
C61 C62 1.395(14) . ?
C61 C67 1.54(2) . ?
C62 H62 0.9500 . ?
C62 C63 1.389(15) . ?
C63 H63 0.9500 . ?
C63 C64 1.377(14) . ?
C64 H64 0.9500 . ?
C64 C65 1.402(15) . ?
C65 H65 0.9500 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C23A H23A 1.0000 . ?
C23A C24A 1.54(2) . ?
C23A C25A 1.53(2) . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C41A H41D 0.9800 . ?
C41A H41E 0.9800 . ?
C41A H41F 0.9800 . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 0.9800 . ?
C57A H57A 1.0000 . ?
C57A C58A 1.506(13) . ?
C57A C59A 1.516(13) . ?
C58A H58D 0.9800 . ?
C58A H58E 0.9800 . ?
C58A H58F 0.9800 . ?
C59A H59D 0.9800 . ?
C59A H59E 0.9800 . ?
C59A H59F 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
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C3 112.0(5) . . ?
C1 C2 C4 111.6(6) . . ?
C1 C2 C5 112.1(6) . . ?
C3 C2 C4 106.9(5) . . ?
C5 C2 C3 107.2(5) . . ?
C5 C2 C4 106.6(5) . . ?
C6 C3 C2 115.9(5) . . ?
C9 C3 C2 104.2(5) . . ?
C9 C3 C6 112.9(6) . . ?
C9 C3 C43 110.1(5) . . ?
C43 C3 C2 104.2(5) . . ?
C43 C3 C6 109.1(6) . . ?
C7 C4 C2 117.4(5) . . ?
C14 C4 C2 103.5(5) . . ?
C14 C4 C7 109.6(6) . . ?
C26 C4 C2 104.6(6) . . ?
C26 C4 C7 109.3(5) . . ?
C26 C4 C14 112.3(5) . . ?
C8 C5 C2 117.1(5) . . ?
C8 C5 C31 110.2(5) . . ?
C31 C5 C2 104.2(6) . . ?
C48 C5 C2 104.3(5) . . ?
C48 C5 C8 111.4(6) . . ?
C48 C5 C31 109.1(5) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C3 126.0(7) . . ?
C14 C9 C3 113.1(6) . . ?
C14 C9 C10 120.9(7) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 C9 118.2(7) . . ?
C11 C10 H10 120.9 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 121.1(7) . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 120.6(8) . . ?
N1 C12 C11 117.3(7) . . ?
N1 C12 C13 122.1(8) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.5(7) . . ?
C14 C13 H13 120.3 . . ?
C9 C14 C4 112.1(6) . . ?
C13 C14 C4 128.3(6) . . ?
C13 C14 C9 119.7(6) . . ?
C16 C15 H15 126.7 . . ?
C16 C15 N1 106.6(8) . . ?
N1 C15 H15 126.7 . . ?
C15 C16 C17 132.2(9) . . ?
C15 C16 N3 106.8(8) . . ?
N3 C16 C17 121.0(10) . . ?
C21 C17 C16 123.3(9) . . ?
N4 C17 C16 114.1(9) . . ?
N4 C17 C21 122.5(8) . . ?
C19 C18 C22 119.5(9) . . ?
N4 C18 C19 123.6(9) . . ?
N4 C18 C22 116.9(9) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 C18 118.6(9) . . ?
C20 C19 H19 120.7 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.2(9) . . ?
C21 C20 H20 119.9 . . ?
C17 C21 H21 120.5 . . ?
C20 C21 C17 118.9(9) . . ?
C20 C21 H21 120.5 . . ?
N5 C22 C18 115.9(8) . . ?
O3 C22 C18 121.2(9) . . ?
O3 C22 N5 122.9(9) . . ?
C27 C26 C4 128.8(7) . . ?
C27 C26 C31 118.8(6) . . ?
C31 C26 C4 112.3(6) . . ?
C26 C27 H27 119.8 . . ?
C26 C27 C28 120.5(7) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 120.4 . . ?
C29 C28 C27 119.3(6) . . ?
C29 C28 H28 120.4 . . ?
C28 C29 N6 119.7(6) . . ?
C30 C29 C28 121.4(6) . . ?
C30 C29 N6 118.9(7) . . ?
C29 C30 H30 121.1 . . ?
C31 C30 C29 117.8(7) . . ?
C31 C30 H30 121.1 . . ?
C26 C31 C5 112.2(6) . . ?
C30 C31 C5 125.6(7) . . ?
C30 C31 C26 122.2(6) . . ?
C33 C32 H32 127.3 . . ?
N6 C32 H32 127.3 . . ?
N6 C32 C33 105.4(6) . . ?
C32 C33 C34 129.9(7) . . ?
C32 C33 N8 108.4(7) . . ?
N8 C33 C34 121.7(7) . . ?
C38 C34 C33 124.1(7) . . ?
N9 C34 C33 112.7(7) . . ?
N9 C34 C38 123.1(6) . . ?
C36 C35 C39 120.8(8) . . ?
N9 C35 C36 123.0(7) . . ?
N9 C35 C39 116.2(7) . . ?
C35 C36 H36 120.3 . . ?
C37 C36 C35 119.3(7) . . ?
C37 C36 H36 120.3 . . ?
C36 C37 H37 120.8 . . ?
C36 C37 C38 118.4(7) . . ?
C38 C37 H37 120.8 . . ?
C34 C38 H38 120.2 . . ?
C37 C38 C34 119.6(7) . . ?
C37 C38 H38 120.2 . . ?
N10 C39 C35 118.7(7) . . ?
O2 C39 C35 118.6(8) . . ?
O2 C39 N10 122.6(8) . . ?
C41 C40 H40 107.0 . . ?
C42 C40 H40 107.0 . . ?
C42 C40 C41 112.4(11) . . ?
C42 C40 N10 113.9(8) . . ?
N10 C40 H40 107.0 . . ?
N10 C40 H40A 106.9 . . ?
N10 C40 C41 109.0(8) . . ?
N10 C40 C41A 116.5(12) . . ?
N10 C40 C42A 109.4(12) . . ?
C41A C40 H40A 106.9 . . ?
C42A C40 H40A 106.9 . . ?
C42A C40 C41A 109.7(13) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C3 127.9(6) . . ?
C44 C43 C48 121.0(7) . . ?
C48 C43 C3 111.1(5) . . ?
C43 C44 H44 120.4 . . ?
C45 C44 C43 119.2(6) . . ?
C45 C44 H44 120.4 . . ?
C44 C45 C46 121.6(6) . . ?
C44 C45 N11 119.7(6) . . ?
C46 C45 N11 118.7(7) . . ?
C45 C46 H46 120.5 . . ?
C45 C46 C47 119.0(7) . . ?
C47 C46 H46 120.5 . . ?
C46 C47 H47 119.8 . . ?
C48 C47 C46 120.3(6) . . ?
C48 C47 H47 119.8 . . ?
C43 C48 C5 113.1(6) . . ?
C47 C48 C5 128.1(6) . . ?
C47 C48 C43 118.8(6) . . ?
C50 C49 H49 126.6 . . ?
N11 C49 H49 126.6 . . ?
N11 C49 C50 106.9(6) . . ?
C49 C50 C51 131.2(7) . . ?
N13 C50 C49 107.1(6) . . ?
N13 C50 C51 121.7(6) . . ?
C55 C51 C50 122.1(6) . . ?
N14 C51 C50 116.6(6) . . ?
N14 C51 C55 121.2(6) . . ?
C53 C52 C56 120.0(6) . . ?
N14 C52 C53 124.3(6) . . ?
N14 C52 C56 115.7(7) . . ?
C52 C53 H53 121.4 . . ?
C54 C53 C52 117.2(7) . . ?
C54 C53 H53 121.4 . . ?
C53 C54 H54 120.1 . . ?
C55 C54 C53 119.8(8) . . ?
C55 C54 H54 120.1 . . ?
C51 C55 H55 120.3 . . ?
C54 C55 C51 119.4(7) . . ?
C54 C55 H55 120.3 . . ?
N15 C56 C52 116.9(6) . . ?
O1 C56 C52 117.2(8) . . ?
O1 C56 N15 125.7(7) . . ?
C15 N1 C12 131.1(8) . . ?
N2 N1 C12 120.1(7) . . ?
N2 N1 C15 108.8(8) . . ?
N3 N2 N1 108.9(7) . . ?
N2 N3 C16 109.0(8) . . ?
C17 N4 C18 116.1(8) . . ?
C22 N5 H5A 118.7 . . ?
C22 N5 H5B 120.1 . . ?
C22 N5 C23 122.6(10) . . ?
C22 N5 C23A 119.9(11) . . ?
C23 N5 H5A 118.7 . . ?
C23A N5 H5B 120.1 . . ?
N5 C23 H23 106.8 . . ?
N5 C23 C24 113.7(13) . . ?
N5 C23 C25 111.2(11) . . ?
C24 C23 H23 106.8 . . ?
C25 C23 H23 106.8 . . ?
C25 C23 C24 111.1(12) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C32 N6 C29 129.3(6) . . ?
C32 N6 N7 111.8(6) . . ?
N7 N6 C29 118.8(6) . . ?
N8 N7 N6 105.2(6) . . ?
N7 N8 C33 109.2(7) . . ?
C34 N9 C35 116.5(6) . . ?
C39 N10 C40 125.9(7) . . ?
C39 N10 H10A 117.1 . . ?
C40 N10 H10A 117.1 . . ?
C49 N11 C45 130.8(6) . . ?
C49 N11 N12 109.0(5) . . ?
N12 N11 C45 120.1(6) . . ?
N13 N12 N11 107.1(5) . . ?
N12 N13 C50 109.9(5) . . ?
C52 N14 C51 118.1(6) . . ?
C56 N15 H15A 117.7 . . ?
C56 N15 H15B 119.0 . . ?
C56 N15 C57 124.7(9) . . ?
C56 N15 C57A 122.0(11) . . ?
C57 N15 H15A 117.7 . . ?
C57A N15 H15B 119.0 . . ?
N15 C57 H57 107.8 . . ?
N15 C57 C58 110.3(8) . . ?
N15 C57 C59 110.7(8) . . ?
C58 C57 H57 107.8 . . ?
C58 C57 C59 112.3(9) . . ?
C59 C57 H57 107.8 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
H4A O4 H4B 104.5 . . ?
C69 C68 C74 122.2(9) . . ?
C73 C68 C69 116.5(9) . . ?
C73 C68 C74 121.3(9) . . ?
C68 C69 C75 118.7(8) . . ?
C70 C69 C68 121.0(9) . . ?
C70 C69 C75 120.3(9) . . ?
C69 C70 H70 120.0 . . ?
C71 C70 C69 120.1(9) . . ?
C71 C70 H70 120.0 . . ?
C70 C71 H71 120.3 . . ?
C70 C71 C72 119.4(9) . . ?
C72 C71 H71 120.3 . . ?
C71 C72 H72 119.7 . . ?
C73 C72 C71 120.5(9) . . ?
C73 C72 H72 119.7 . . ?
C68 C73 H73 118.7 . . ?
C72 C73 C68 122.6(9) . . ?
C72 C73 H73 118.7 . . ?
C68 C74 H74A 109.5 . . ?
C68 C74 H74B 109.5 . . ?
C68 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C69 C75 H75A 109.5 . . ?
C69 C75 H75B 109.5 . . ?
C69 C75 H75C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
Cl1 C76 H76 103.1 . . ?
Cl2 C76 H76 103.1 . . ?
Cl2 C76 Cl1 115.2(7) . . ?
Cl3 C76 H76 103.1 . . ?
Cl3 C76 Cl1 113.8(7) . . ?
Cl3 C76 Cl2 116.0(7) . . ?
C69A C68A C74A 121.2(12) . . ?
C73A C68A C69A 116.6(11) . . ?
C73A C68A C74A 122.2(13) . . ?
C68A C69A C75A 117.8(11) . . ?
C70A C69A C68A 121.0(11) . . ?
C70A C69A C75A 121.3(12) . . ?
C69A C70A H70A 120.0 . . ?
C71A C70A C69A 120.0(11) . . ?
C71A C70A H70A 120.0 . . ?
C70A C71A H71A 120.2 . . ?
C70A C71A C72A 119.6(12) . . ?
C72A C71A H71A 120.2 . . ?
C71A C72A H72A 119.8 . . ?
C73A C72A C71A 120.4(12) . . ?
C73A C72A H72A 119.8 . . ?
C68A C73A H73A 118.8 . . ?
C72A C73A C68A 122.4(12) . . ?
C72A C73A H73A 118.8 . . ?
C68A C74A H74D 109.5 . . ?
C68A C74A H74E 109.5 . . ?
C68A C74A H74F 109.5 . . ?
H74D C74A H74E 109.5 . . ?
H74D C74A H74F 109.5 . . ?
H74E C74A H74F 109.5 . . ?
C69A C75A H75D 109.5 . . ?
C69A C75A H75E 109.5 . . ?
C69A C75A H75F 109.5 . . ?
H75D C75A H75E 109.5 . . ?
H75D C75A H75F 109.5 . . ?
H75E C75A H75F 109.5 . . ?
Cl1A C76A H76A 101.0 . . ?
Cl2A C76A H76A 101.0 . . ?
Cl2A C76A Cl1A 116.4(12) . . ?
Cl3A C76A H76A 101.0 . . ?
Cl3A C76A Cl1A 115.6(12) . . ?
Cl3A C76A Cl2A 117.2(12) . . ?
C76A Cl1A Cl3F 113.4(19) . . ?
Cl1B C76B H76B 101.4 . . ?
Cl2B C76B H76B 101.4 . . ?
Cl2B C76B Cl1B 116.4(11) . . ?
Cl3B C76B H76B 101.4 . . ?
Cl3B C76B Cl1B 115.5(12) . . ?
Cl3B C76B Cl2B 116.6(12) . . ?
Cl1C C76C H76C 101.3 . . ?
Cl2C C76C H76C 101.3 . . ?
Cl2C C76C Cl1C 116.5(12) . . ?
Cl3C C76C H76C 101.3 . . ?
Cl3C C76C Cl1C 115.2(12) . . ?
Cl3C C76C Cl2C 117.0(12) . . ?
Cl1D C76D H76D 101.6 . . ?
Cl2D C76D H76D 101.6 . . ?
Cl2D C76D Cl1D 116.0(12) . . ?
Cl3D C76D H76D 101.6 . . ?
Cl3D C76D Cl1D 115.2(12) . . ?
Cl3D C76D Cl2D 116.8(12) . . ?
Cl1E C76E H76E 100.9 . . ?
Cl2E C76E H76E 100.9 . . ?
Cl2E C76E Cl1E 116.5(12) . . ?
Cl3E C76E H76E 100.9 . . ?
Cl3E C76E Cl1E 115.8(12) . . ?
Cl3E C76E Cl2E 117.3(12) . . ?
Cl1F C76F H76F 101.2 . . ?
Cl2F C76F H76F 101.2 . . ?
Cl2F C76F Cl1F 116.2(12) . . ?
Cl3F C76F H76F 101.2 . . ?
Cl3F C76F Cl1F 115.6(12) . . ?
Cl3F C76F Cl2F 117.1(12) . . ?
C76F Cl3F Cl1A 131(2) . . ?
C61 C60 C66 120.3(10) . . ?
C65 C60 C61 120.9(9) . . ?
C65 C60 C66 118.8(9) . . ?
C60 C61 C62 119.0(9) . . ?
C60 C61 C67 120.7(10) . . ?
C62 C61 C67 120.2(9) . . ?
C61 C62 H62 120.2 . . ?
C63 C62 C61 119.6(9) . . ?
C63 C62 H62 120.2 . . ?
C62 C63 H63 119.1 . . ?
C64 C63 C62 121.8(9) . . ?
C64 C63 H63 119.1 . . ?
C63 C64 H64 120.7 . . ?
C63 C64 C65 118.7(9) . . ?
C65 C64 H64 120.7 . . ?
C60 C65 C64 119.9(9) . . ?
C60 C65 H65 120.1 . . ?
C64 C65 H65 120.1 . . ?
C60 C66 H66A 109.5 . . ?
C60 C66 H66B 109.5 . . ?
C60 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C61 C67 H67A 109.5 . . ?
C61 C67 H67B 109.5 . . ?
C61 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N5 C23A H23A 106.5 . . ?
N5 C23A C24A 114.0(13) . . ?
N5 C23A C25A 110.9(14) . . ?
C24A C23A H23A 106.5 . . ?
C25A C23A H23A 106.5 . . ?
C25A C23A C24A 111.8(13) . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C23A C25A H25D 109.5 . . ?
C23A C25A H25E 109.5 . . ?
C23A C25A H25F 109.5 . . ?
H25D C25A H25E 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
C40 C41A H41D 109.5 . . ?
C40 C41A H41E 109.5 . . ?
C40 C41A H41F 109.5 . . ?
H41D C41A H41E 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
C40 C42A H42D 109.5 . . ?
C40 C42A H42E 109.5 . . ?
C40 C42A H42F 109.5 . . ?
H42D C42A H42E 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?
N15 C57A H57A 108.0 . . ?
N15 C57A C58A 110.0(9) . . ?
N15 C57A C59A 110.6(9) . . ?
C58A C57A H57A 108.0 . . ?
C58A C57A C59A 112.1(10) . . ?
C59A C57A H57A 108.0 . . ?
C57A C58A H58D 109.5 . . ?
C57A C58A H58E 109.5 . . ?
C57A C58A H58F 109.5 . . ?
H58D C58A H58E 109.5 . . ?
H58D C58A H58F 109.5 . . ?
H58E C58A H58F 109.5 . . ?
C57A C59A H59D 109.5 . . ?
C57A C59A H59E 109.5 . . ?
C57A C59A H59F 109.5 . . ?
H59D C59A H59E 109.5 . . ?
H59D C59A H59F 109.5 . . ?
H59E C59A H59F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C11 H11 O2 0.95 2.49 3.199(9) 131.4 1_556 yes
C15 H15 O4 0.95 2.44 3.392(11) 176.9 . yes
C21 H21 Cl2 0.95 2.69 3.480(11) 140.4 2_676 yes
C32 H32 N13 0.95 2.86 3.446(8) 120.7 2_666 yes
C32 H32 N14 0.95 2.48 3.427(9) 174.3 2_666 yes
C37 H37 N12 0.95 2.60 3.315(9) 132.4 1_554 yes
C49 H49 O3 0.95 2.21 3.089(9) 153.2 1_545 yes
C55 H55 O3 0.95 2.49 3.423(10) 166.1 1_545 yes
C24 H24C O4 0.98 2.61 3.358(16) 132.9 . yes
N10 H10A N13 0.88 2.37 3.147(8) 147.9 2_666 yes
C58 H58C N9 0.98 2.66 3.53(3) 148.3 2_666 yes
O4 H4A O2 0.87 1.95 2.808(7) 168.7 1_556 yes
O4 H4B N8 0.87 2.27 3.137(9) 173.8 2_666 yes
C70 H70 O1 0.95 2.51 3.419(12) 160.6 1_455 yes
C76 H76 N3 1.00 2.37 3.160(17) 135.7 2_676 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C6 6.4(9) . . . . ?
C1 C2 C3 C9 -118.2(7) . . . . ?
C1 C2 C3 C43 126.3(6) . . . . ?
C1 C2 C4 C7 0.1(8) . . . . ?
C1 C2 C4 C14 121.0(6) . . . . ?
C1 C2 C4 C26 -121.2(6) . . . . ?
C1 C2 C5 C8 -1.6(8) . . . . ?
C1 C2 C5 C31 120.4(5) . . . . ?
C1 C2 C5 C48 -125.2(5) . . . . ?
C2 C3 C9 C10 176.3(6) . . . . ?
C2 C3 C9 C14 -5.7(7) . . . . ?
C2 C3 C43 C44 176.3(6) . . . . ?
C2 C3 C43 C48 -3.1(7) . . . . ?
C2 C4 C14 C9 -1.7(7) . . . . ?
C2 C4 C14 C13 179.4(7) . . . . ?
C2 C4 C26 C27 177.7(5) . . . . ?
C2 C4 C26 C31 -0.3(6) . . . . ?
C2 C5 C31 C26 2.0(6) . . . . ?
C2 C5 C31 C30 -178.6(5) . . . . ?
C2 C5 C48 C43 0.0(7) . . . . ?
C2 C5 C48 C47 -178.6(6) . . . . ?
C3 C2 C4 C7 -122.7(6) . . . . ?
C3 C2 C4 C14 -1.8(6) . . . . ?
C3 C2 C4 C26 116.0(5) . . . . ?
C3 C2 C5 C8 121.7(6) . . . . ?
C3 C2 C5 C31 -116.3(5) . . . . ?
C3 C2 C5 C48 -1.9(6) . . . . ?
C3 C9 C10 C11 177.8(7) . . . . ?
C3 C9 C14 C4 4.8(8) . . . . ?
C3 C9 C14 C13 -176.2(6) . . . . ?
C3 C43 C44 C45 -179.6(6) . . . . ?
C3 C43 C48 C5 2.0(7) . . . . ?
C3 C43 C48 C47 -179.3(6) . . . . ?
C4 C2 C3 C6 129.0(7) . . . . ?
C4 C2 C3 C9 4.4(7) . . . . ?
C4 C2 C3 C43 -111.1(6) . . . . ?
C4 C2 C5 C8 -124.0(6) . . . . ?
C4 C2 C5 C31 -2.1(5) . . . . ?
C4 C2 C5 C48 112.3(5) . . . . ?
C4 C26 C27 C28 -178.6(5) . . . . ?
C4 C26 C31 C5 -1.1(6) . . . . ?
C4 C26 C31 C30 179.5(5) . . . . ?
C5 C2 C3 C6 -116.9(7) . . . . ?
C5 C2 C3 C9 118.4(6) . . . . ?
C5 C2 C3 C43 3.0(6) . . . . ?
C5 C2 C4 C7 122.8(6) . . . . ?
C5 C2 C4 C14 -116.3(5) . . . . ?
C5 C2 C4 C26 1.5(5) . . . . ?
C6 C3 C9 C10 49.8(9) . . . . ?
C6 C3 C9 C14 -132.3(6) . . . . ?
C6 C3 C43 C44 -59.4(8) . . . . ?
C6 C3 C43 C48 121.3(6) . . . . ?
C7 C4 C14 C9 124.3(6) . . . . ?
C7 C4 C14 C13 -54.6(9) . . . . ?
C7 C4 C26 C27 51.2(8) . . . . ?
C7 C4 C26 C31 -126.8(6) . . . . ?
C8 C5 C31 C26 128.5(6) . . . . ?
C8 C5 C31 C30 -52.2(8) . . . . ?
C8 C5 C48 C43 -127.2(6) . . . . ?
C8 C5 C48 C47 54.1(8) . . . . ?
C9 C3 C43 C44 65.1(8) . . . . ?
C9 C3 C43 C48 -114.3(6) . . . . ?
C9 C10 C11 C12 -1.7(11) . . . . ?
C10 C9 C14 C4 -177.1(6) . . . . ?
C10 C9 C14 C13 1.9(10) . . . . ?
C10 C11 C12 C13 1.6(12) . . . . ?
C10 C11 C12 N1 -177.7(7) . . . . ?
C11 C12 C13 C14 0.3(11) . . . . ?
C11 C12 N1 C15 19.4(13) . . . . ?
C11 C12 N1 N2 -161.3(7) . . . . ?
C12 C13 C14 C4 176.8(7) . . . . ?
C12 C13 C14 C9 -2.0(10) . . . . ?
C12 N1 N2 N3 -179.7(7) . . . . ?
C13 C12 N1 C15 -159.9(8) . . . . ?
C13 C12 N1 N2 19.4(12) . . . . ?
C14 C4 C26 C27 -70.7(8) . . . . ?
C14 C4 C26 C31 111.3(6) . . . . ?
C14 C9 C10 C11 0.0(10) . . . . ?
C15 C16 C17 C21 174.9(10) . . . . ?
C15 C16 C17 N4 -1.5(15) . . . . ?
C15 C16 N3 N2 -0.4(11) . . . . ?
C15 N1 N2 N3 -0.2(10) . . . . ?
C16 C15 N1 C12 179.4(8) . . . . ?
C16 C15 N1 N2 0.0(10) . . . . ?
C16 C17 C21 C20 -177.9(8) . . . . ?
C16 C17 N4 C18 178.6(7) . . . . ?
C17 C16 N3 N2 -179.5(8) . . . . ?
C18 C19 C20 C21 1.4(13) . . . . ?
C18 C22 N5 C23 -177.8(10) . . . . ?
C18 C22 N5 C23A 174.2(11) . . . . ?
C19 C18 C22 N5 -174.8(8) . . . . ?
C19 C18 C22 O3 6.4(13) . . . . ?
C19 C18 N4 C17 -0.7(12) . . . . ?
C19 C20 C21 C17 0.0(14) . . . . ?
C21 C17 N4 C18 2.2(12) . . . . ?
C22 C18 C19 C20 -179.3(8) . . . . ?
C22 C18 N4 C17 177.5(7) . . . . ?
C22 N5 C23 C24 159.8(11) . . . . ?
C22 N5 C23 C25 -73.9(15) . . . . ?
C22 N5 C23A C24A 89.6(17) . . . . ?
C22 N5 C23A C25A -143.1(15) . . . . ?
C26 C4 C14 C9 -113.9(7) . . . . ?
C26 C4 C14 C13 67.2(9) . . . . ?
C26 C27 C28 C29 -0.7(9) . . . . ?
C27 C26 C31 C5 -179.4(5) . . . . ?
C27 C26 C31 C30 1.3(8) . . . . ?
C27 C28 C29 C30 1.7(8) . . . . ?
C27 C28 C29 N6 -177.9(5) . . . . ?
C28 C29 C30 C31 -1.1(8) . . . . ?
C28 C29 N6 C32 3.6(9) . . . . ?
C28 C29 N6 N7 178.8(6) . . . . ?
C29 C30 C31 C5 -179.6(5) . . . . ?
C29 C30 C31 C26 -0.3(8) . . . . ?
C29 N6 N7 N8 -176.3(5) . . . . ?
C30 C29 N6 C32 -175.9(5) . . . . ?
C30 C29 N6 N7 -0.8(8) . . . . ?
C31 C5 C48 C43 110.9(6) . . . . ?
C31 C5 C48 C47 -67.7(8) . . . . ?
C31 C26 C27 C28 -0.7(8) . . . . ?
C32 C33 C34 C38 -172.2(7) . . . . ?
C32 C33 C34 N9 6.4(9) . . . . ?
C32 C33 N8 N7 2.1(8) . . . . ?
C32 N6 N7 N8 -0.3(7) . . . . ?
C33 C32 N6 C29 177.0(5) . . . . ?
C33 C32 N6 N7 1.6(7) . . . . ?
C33 C34 C38 C37 178.8(6) . . . . ?
C33 C34 N9 C35 179.0(5) . . . . ?
C34 C33 N8 N7 179.8(6) . . . . ?
C35 C36 C37 C38 -2.9(9) . . . . ?
C35 C39 N10 C40 179.8(6) . . . . ?
C36 C35 C39 N10 -167.4(6) . . . . ?
C36 C35 C39 O2 9.9(9) . . . . ?
C36 C35 N9 C34 1.8(8) . . . . ?
C36 C37 C38 C34 2.4(9) . . . . ?
C38 C34 N9 C35 -2.4(8) . . . . ?
C39 C35 C36 C37 -179.8(6) . . . . ?
C39 C35 N9 C34 -177.6(5) . . . . ?
C41 C40 N10 C39 80.8(11) . . . . ?
C42 C40 N10 C39 -152.7(10) . . . . ?
C43 C3 C9 C10 -72.5(8) . . . . ?
C43 C3 C9 C14 105.5(6) . . . . ?
C43 C44 C45 C46 -0.8(9) . . . . ?
C43 C44 C45 N11 179.1(5) . . . . ?
C44 C43 C48 C5 -177.4(5) . . . . ?
C44 C43 C48 C47 1.4(9) . . . . ?
C44 C45 C46 C47 1.0(9) . . . . ?
C44 C45 N11 C49 -168.2(6) . . . . ?
C44 C45 N11 N12 13.9(8) . . . . ?
C45 C46 C47 C48 0.1(9) . . . . ?
C45 N11 N12 N13 178.4(5) . . . . ?
C46 C45 N11 C49 11.6(10) . . . . ?
C46 C45 N11 N12 -166.3(5) . . . . ?
C46 C47 C48 C5 177.4(6) . . . . ?
C46 C47 C48 C43 -1.2(9) . . . . ?
C48 C5 C31 C26 -108.9(6) . . . . ?
C48 C5 C31 C30 70.4(7) . . . . ?
C48 C43 C44 C45 -0.4(9) . . . . ?
C49 C50 C51 C55 -12.9(11) . . . . ?
C49 C50 C51 N14 165.7(6) . . . . ?
C49 C50 N13 N12 -0.6(7) . . . . ?
C49 N11 N12 N13 0.1(7) . . . . ?
C50 C49 N11 C45 -178.5(6) . . . . ?
C50 C49 N11 N12 -0.5(7) . . . . ?
C50 C51 C55 C54 178.3(7) . . . . ?
C50 C51 N14 C52 -179.4(6) . . . . ?
C51 C50 N13 N12 -179.9(5) . . . . ?
C52 C53 C54 C55 -1.3(11) . . . . ?
C52 C56 N15 C57 -171.9(12) . . . . ?
C52 C56 N15 C57A 174.5(13) . . . . ?
C53 C52 C56 N15 175.0(6) . . . . ?
C53 C52 C56 O1 -0.2(10) . . . . ?
C53 C52 N14 C51 0.8(9) . . . . ?
C53 C54 C55 C51 1.3(11) . . . . ?
C55 C51 N14 C52 -0.8(9) . . . . ?
C56 C52 C53 C54 -178.6(6) . . . . ?
C56 C52 N14 C51 179.7(5) . . . . ?
C56 N15 C57 C58 131.5(13) . . . . ?
C56 N15 C57 C59 -103.7(13) . . . . ?
C56 N15 C57A C58A 135.3(14) . . . . ?
C56 N15 C57A C59A -100.4(15) . . . . ?
N1 C12 C13 C14 179.6(7) . . . . ?
N1 C15 C16 C17 179.2(9) . . . . ?
N1 C15 C16 N3 0.2(10) . . . . ?
N1 N2 N3 C16 0.4(11) . . . . ?
N3 C16 C17 C21 -6.3(14) . . . . ?
N3 C16 C17 N4 177.4(8) . . . . ?
N4 C17 C21 C20 -1.9(13) . . . . ?
N4 C18 C19 C20 -1.0(13) . . . . ?
N4 C18 C22 N5 6.8(11) . . . . ?
N4 C18 C22 O3 -172.0(8) . . . . ?
N6 C29 C30 C31 178.4(5) . . . . ?
N6 C32 C33 C34 -179.6(6) . . . . ?
N6 C32 C33 N8 -2.2(7) . . . . ?
N6 N7 N8 C33 -1.1(8) . . . . ?
N8 C33 C34 C38 10.6(10) . . . . ?
N8 C33 C34 N9 -170.8(6) . . . . ?
N9 C34 C38 C37 0.3(9) . . . . ?
N9 C35 C36 C37 0.8(9) . . . . ?
N9 C35 C39 N10 12.1(8) . . . . ?
N9 C35 C39 O2 -170.7(5) . . . . ?
N11 C45 C46 C47 -178.9(5) . . . . ?
N11 C49 C50 C51 179.9(6) . . . . ?
N11 C49 C50 N13 0.7(7) . . . . ?
N11 N12 N13 C50 0.3(7) . . . . ?
N13 C50 C51 C55 166.2(6) . . . . ?
N13 C50 C51 N14 -15.2(9) . . . . ?
N14 C51 C55 C54 -0.3(10) . . . . ?
N14 C52 C53 C54 0.2(11) . . . . ?
N14 C52 C56 N15 -3.8(9) . . . . ?
N14 C52 C56 O1 -179.1(6) . . . . ?
O3 C22 N5 C23 0.9(15) . . . . ?
O3 C22 N5 C23A -7.1(16) . . . . ?
O2 C39 N10 C40 2.6(11) . . . . ?
O1 C56 N15 C57 2.9(16) . . . . ?
O1 C56 N15 C57A -10.8(16) . . . . ?
C68 C69 C70 C71 0.1(3) . . . . ?
C69 C68 C73 C72 -0.1(6) . . . . ?
C69 C70 C71 C72 -0.5(6) . . . . ?
C70 C71 C72 C73 0.5(8) . . . . ?
C71 C72 C73 C68 -0.2(9) . . . . ?
C73 C68 C69 C70 0.2(3) . . . . ?
C73 C68 C69 C75 -179.6(4) . . . . ?
C74 C68 C69 C70 -179.6(3) . . . . ?
C74 C68 C69 C75 0.6(4) . . . . ?
C74 C68 C73 C72 179.7(5) . . . . ?
C75 C69 C70 C71 179.9(4) . . . . ?
C68A C69A C70A C71A 0.0(3) . . . . ?
C69A C68A C73A C72A 0.2(7) . . . . ?
C69A C70A C71A C72A -0.1(7) . . . . ?
C70A C71A C72A C73A 0.2(9) . . . . ?
C71A C72A C73A C68A -0.3(9) . . . . ?
C73A C68A C69A C70A -0.1(3) . . . . ?
C73A C68A C69A C75A 179.9(4) . . . . ?
C74A C68A C69A C70A 180.0(3) . . . . ?
C74A C68A C69A C75A 0.0(4) . . . . ?
C74A C68A C73A C72A -179.9(5) . . . . ?
C75A C69A C70A C71A -179.9(4) . . . . ?
Cl2A C76A Cl1A Cl3F 133(3) . . . . ?
Cl3A C76A Cl1A Cl3F -11(3) . . . . ?
Cl1F C76F Cl3F Cl1A -176(2) . . . . ?
Cl2F C76F Cl3F Cl1A 41(4) . . . . ?
C60 C61 C62 C63 0.0(3) . . . . ?
C61 C60 C65 C64 0.0(6) . . . . ?
C61 C62 C63 C64 0.1(7) . . . . ?
C62 C63 C64 C65 -0.1(8) . . . . ?
C63 C64 C65 C60 0.1(8) . . . . ?
C65 C60 C61 C62 0.0(3) . . . . ?
C65 C60 C61 C67 -179.9(4) . . . . ?
C66 C60 C61 C62 179.9(3) . . . . ?
C66 C60 C61 C67 0.0(4) . . . . ?
C66 C60 C65 C64 -180.0(5) . . . . ?
C67 C61 C62 C63 179.9(4) . . . . ?
C41A C40 N10 C39 136.9(16) . . . . ?
C42A C40 N10 C39 -98.0(16) . . . . ?

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.260
_oxdiff_exptl_absorpt_empirical_full_min 0.363
# start Validation Reply Form
_vrf_PLAT026_o-xylene            
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        33% Check
RESPONSE: Small and poor crystal, combined with highly disorder in the crystal
 structure, leading to a bad and weak diffraction.
;
_vrf_PLAT084_o-xylene            
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.44 Report
RESPONSE: The small crystal size and absence of heavy atoms in the structure 
resulted in weak diffraction intensity. Despite our best efforts to resolve the 
disorder of the o-xylene molecules, we were unable to completely reduce the 
R2 value. 
;
_vrf_PLAT340_o-xylene            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01112 Ang.
RESPONSE: The small crystal size and absence of heavy atoms in the structure 
resulted in weak diffraction intensity. 
;
# end Validation Reply Form
####################################################################### 
# 
# 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_p-xylene
_audit_block_doi                 10.5517/ccdc.csd.cc2m121t
_database_code_depnum_ccdc_archive 'CCDC 2414095'
loop_
_audit_author_name
_audit_author_address
'Tianshu Yang'
;FUJIAN NORMAL UNIVERSITY
China
;
_audit_update_record             
;
2025-02-14 deposited with the CCDC.	2025-02-27 downloaded from the CCDC.
;
_audit_creation_date             2025-02-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C59 H57 N15 O3, 3(C8 H10), H2 O'
_chemical_formula_sum            'C83 H89 N15 O4'
_chemical_formula_weight         1360.69
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.6409(5)
_cell_length_b                   15.4829(5)
_cell_length_c                   17.0956(5)
_cell_angle_alpha                71.798(3)
_cell_angle_beta                 80.271(3)
_cell_angle_gamma                79.849(3)
_cell_volume                     3596.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    21813
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.8950
_cell_measurement_theta_min      2.7470
_shelx_estimated_absorpt_T_max   0.884
_shelx_estimated_absorpt_T_min   0.787
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.127a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48157
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.085
_diffrn_reflns_theta_min         2.741
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00   0.00   0.50    0.06    --   45.97 -19.00-180.00   54
  2  ω    -23.00  17.00   0.50    0.06    --   45.97 -19.00-150.00   80
  3  ω    -28.00  30.00   0.50    0.06    --   45.97 -38.00  30.00  116
  4  ω    -26.00  23.00   0.50    0.06    --   45.97 -19.00  60.00   98
  5  ω    -28.00  18.00   0.50    0.06    --   45.97 -19.00 120.00   92
  6  ω    -24.00  23.00   0.50    0.06    --   45.97 -19.00 150.00   94
  7  ω     38.00  89.00   0.50    0.22    --  107.47 -86.00 121.00  102
  8  ω     48.00  86.00   0.50    0.22    --  107.47 -95.00  90.00   76
  9  ω     40.00 111.00   0.50    0.22    --  107.47-125.00 150.00  142
 10  ω     47.00 106.00   0.50    0.22    --  107.47-125.00  60.00  118
 11  ω     56.00 109.00   0.50    0.22    --  107.47-125.00  30.00  106
 12  ω     35.00  97.00   0.50    0.22    --  107.47 -95.00 -60.00  124
 13  ω     75.00 108.00   0.50    0.22    --  107.47-125.00 -60.00   66
 14  ω     48.00 105.00   0.50    0.22    --  107.47 -95.00-150.00  114
 15  ω     36.00  67.00   0.50    0.22    --  107.47 -61.00-150.00   62
 16  ω     44.00  90.00   0.50    0.06    --   45.97-125.00 -60.00   92
 17  ω    -26.00  72.00   0.50    0.06    --   45.97 -86.00 121.00  196
 18  ω     45.00  89.00   0.50    0.22    --  107.47 -77.00 -60.00   88
 19  ω    103.00 174.00   0.50    0.22    --  107.47  45.00 150.00  142
 20  ω     94.00 167.00   0.50    0.22    --  107.47  45.00  30.00  146
 21  ω     96.00 131.00   0.50    0.22    --  107.47  45.00-180.00   70
 22  ω    134.00 174.00   0.50    0.22    --  107.47  45.00-180.00   80
 23  ω     83.00 149.00   0.50    0.22    --  107.47  86.00-120.00  132
 24  ω    -99.00 -74.00   0.50    0.22    --  -97.00  86.00-120.00   50
 25  ω    -63.00 -29.00   0.50    0.22    --  -97.00 137.00-108.61   68
 26  ω   -120.00 -94.00   0.50    0.22    --  -97.00 137.00-108.61   52
 27  ω    -67.00 -31.00   0.50    0.22    --  -97.00 125.00  30.00   72
 28  ω   -108.00 -73.00   0.50    0.22    --  -97.00 125.00  30.00   70
 29  ω   -108.00 -69.00   0.50    0.22    --  -97.00 109.00  42.25   78
 30  ω    -68.00 -34.00   0.50    0.22    --  -97.00 142.00 121.03   68
 31  ω   -124.00 -73.00   0.50    0.22    --  -97.00 142.00 121.03  102
 32  ω   -106.00 -79.00   0.50    0.22    --  -97.00 108.00  83.18   54
 33  ω    -55.00  24.00   0.50    0.06    --  -45.97  86.00-120.00  158
 34  ω   -106.00 -81.00   0.50    0.22    --  -97.00 107.00-114.48   50
 35  ω    -76.00 -30.00   0.50    0.22    --  -97.00 107.00-114.48   92
 36  ω    -53.00 -25.00   0.50    0.22    --  -97.00  45.00-180.00   56
 37  ω    -54.00 -29.00   0.50    0.22    --  -97.00  45.00-150.00   50
 38  ω    -50.00 -24.00   0.50    0.22    --  -97.00  45.00-120.00   52
 39  ω    -74.00 -25.00   0.50    0.22    --  -97.00  61.00-120.00   98
 40  ω    -53.00 -28.00   0.50    0.22    --  -97.00  45.00   0.00   50
 41  ω    -50.00 -25.00   0.50    0.22    --  -97.00  45.00 -90.00   50
 42  ω    -53.00 -24.00   0.50    0.22    --  -97.00  45.00  30.00   58
 43  ω    -54.00 -29.00   0.50    0.22    --  -97.00  45.00  60.00   50
 44  ω    -72.00 -36.00   0.50    0.22    --  -97.00  61.00  90.00   72
 45  ω    -53.00 -25.00   0.50    0.22    --  -97.00  45.00 150.00   56
 46  ω    -50.00 -24.00   0.50    0.22    --  -97.00  45.00  90.00   52
 47  ω   -143.00-101.00   0.50    0.22    --  -97.00 -30.00 -30.00   84
 48  ω   -142.00 -89.00   0.50    0.22    --  -97.00 -95.00-180.00  106
 49  ω   -162.00 -90.00   0.50    0.22    --  -97.00 -86.00 121.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0146927000
_diffrn_orient_matrix_UB_12      -0.0718828000
_diffrn_orient_matrix_UB_13      0.0852311000
_diffrn_orient_matrix_UB_21      0.1066918000
_diffrn_orient_matrix_UB_22      -0.0238875000
_diffrn_orient_matrix_UB_23      0.0000252000
_diffrn_orient_matrix_UB_31      -0.0001083000
_diffrn_orient_matrix_UB_32      0.0736704000
_diffrn_orient_matrix_UB_33      0.0432435000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11859
_reflns_number_total             14306
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.127a 64-bit (release 16-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         14306
_refine_ls_number_restraints     593
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0739
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1034P)²+3.4300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1878
_refine_ls_wR_factor_ref         0.1980
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C86-C81 = C82-C81 = C83-C82 = C84-C83 = C85-C84 = C86-C85
 1.39 with sigma of 0.01
 C87-C81 = C88-C84
 1.5 with sigma of 0.01
 C30-C29 = C30-C31 = C30-H30
 1.5 with sigma of 0.01
 C81-C83 \\sim C82-C84 \\sim C83-C85 \\sim C84-C86 \\sim C85-C81 \\sim C86-C82
 with sigma of 0.02
3. Restrained planarity
 C64A, C65A, C66A, C67A, C68A, C69A, C70A, C71A
 with sigma of 0.01
 C81A, C82A, C83A, C84A, C85A, C86A, C87A, C88A
 with sigma of 0.01
 C81, C82, C83, C84, C85, C86, C87, C88
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C64 \\sim C64A \\sim C65 \\sim C65A \\sim C66 \\sim C66A \\sim C67 \\sim C67A
\\sim C68 \\sim C68A \\sim C69 \\sim C69A \\sim C70 \\sim C70A \\sim C71 \\sim
C71A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
C81 \\sim C81A \\sim C82 \\sim C82A \\sim C83 \\sim C83A \\sim C84 \\sim C84A
\\sim C85 \\sim C85A \\sim C86 \\sim C86A \\sim C87 \\sim C87A \\sim C88 \\sim
C88A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
Uanis(C70A) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq: with sigma
of 0.003 and sigma for terminal atoms of 0.006
5. Same fragment restrains
{C81A, C82A, C83A, C84A, C85A, C86A, C87A, C88A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C81, C82, C83, C84, C85, C86, C87, C88}
{C64A, C65A, C66A, C67A, C68A, C69A, C70A, C71A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C64, C65, C66, C67, C68, C69, C70, C71}
6. Others
 Sof(C64A)=Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=Sof(C67A)=Sof(C68A)=
 Sof(H68A)=Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=
 Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=1-FVAR(1)
 Sof(C64)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(C68)=Sof(H68)=
 Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C71)=Sof(H71A)=
 Sof(H71B)=Sof(H71C)=FVAR(1)
 Sof(C81A)=Sof(C82A)=Sof(H82A)=Sof(C83A)=Sof(H83A)=Sof(C84A)=Sof(C85A)=
 Sof(H85A)=Sof(C86A)=Sof(H86A)=Sof(C87A)=Sof(H87D)=Sof(H87E)=Sof(H87F)=
 Sof(C88A)=Sof(H88D)=Sof(H88E)=Sof(H88F)=0.5*(1-FVAR(3))
 Sof(C81)=Sof(C82)=Sof(H82)=Sof(C83)=Sof(H83)=Sof(C84)=Sof(C85)=Sof(H85)=
 Sof(C86)=Sof(H86)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C88)=Sof(H88A)=
 Sof(H88B)=Sof(H88C)=0.5*FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C23(H23), C40(H40), C57(H57)
7.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C15(H15), C19(H19), C20(H20), C21(H21),
 C27(H27), C29(H29), C30(H30), C32(H32), C36(H36), C37(H37), C38(H38), C44(H44),
  C46(H46), C47(H47), C49(H49), C53(H53), C54(H54), C55(H55), N5(H5), N10(H10A),
  N15(H15A), C62(H62), C63(H63), C65(H65), C66(H66), C68(H68), C69(H69),
 C65A(H65A), C66A(H66A), C68A(H68A), C69A(H69A), C73(H73), C74(H74), C76(H76),
 C77(H77), C82(H82), C83(H83), C85(H85), C86(H86), C82A(H82A), C83A(H83A),
 C85A(H85A), C86A(H86A)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C70(H70A,H70B,
 H70C), C71(H71A,H71B,H71C), C70A(H70D,H70E,H70F), C71A(H71D,H71E,H71F),
 C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C87(H87A,H87B,H87C), C88(H88A,H88B,
 H88C), C87A(H87D,H87E,H87F), C88A(H88D,H88E,H88F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.99306(17) 0.52917(19) 0.28879(15) 0.0346(5) Uani 1 1 d . . . . .
H1A H 1.020278 0.481179 0.262326 0.052 Uiso 1 1 calc R U . . .
H1B H 1.032800 0.529337 0.329467 0.052 Uiso 1 1 calc R U . . .
H1C H 0.988708 0.588981 0.246530 0.052 Uiso 1 1 calc R U . . .
C2 C 0.89540(15) 0.51047(16) 0.33256(13) 0.0260(5) Uani 1 1 d . . . . .
C3 C 0.82615(15) 0.50963(16) 0.27014(13) 0.0255(4) Uani 1 1 d . . . . .
C4 C 0.89740(15) 0.41377(16) 0.40146(13) 0.0262(4) Uani 1 1 d . . . . .
C5 C 0.84666(15) 0.58454(15) 0.37836(12) 0.0252(4) Uani 1 1 d . . . . .
C6 C 0.86414(17) 0.53575(18) 0.17758(13) 0.0321(5) Uani 1 1 d . . . . .
H6A H 0.881731 0.597787 0.160360 0.048 Uiso 1 1 calc R U . . .
H6B H 0.815805 0.533911 0.145080 0.048 Uiso 1 1 calc R U . . .
H6C H 0.919140 0.492226 0.168253 0.048 Uiso 1 1 calc R U . . .
C7 C 0.99398(17) 0.35579(18) 0.41236(15) 0.0340(5) Uani 1 1 d . . . . .
H7A H 1.021811 0.343853 0.359820 0.051 Uiso 1 1 calc R U . . .
H7B H 0.986755 0.297438 0.455362 0.051 Uiso 1 1 calc R U . . .
H7C H 1.034751 0.389234 0.428816 0.051 Uiso 1 1 calc R U . . .
C8 C 0.89955(18) 0.66662(17) 0.36499(14) 0.0324(5) Uani 1 1 d . . . . .
H8A H 0.959856 0.644592 0.386778 0.049 Uiso 1 1 calc R U . . .
H8B H 0.862412 0.708969 0.394123 0.049 Uiso 1 1 calc R U . . .
H8C H 0.910021 0.698530 0.305554 0.049 Uiso 1 1 calc R U . . .
C9 C 0.79922(15) 0.41403(16) 0.30086(13) 0.0261(4) Uani 1 1 d . . . . .
C10 C 0.74331(16) 0.37625(16) 0.26528(14) 0.0286(5) Uani 1 1 d . . . . .
H10 H 0.720328 0.410756 0.214320 0.034 Uiso 1 1 calc R U . . .
C11 C 0.72139(17) 0.28861(16) 0.30421(14) 0.0305(5) Uani 1 1 d . . . . .
H11 H 0.683597 0.262459 0.280003 0.037 Uiso 1 1 calc R U . . .
C12 C 0.75494(17) 0.23865(16) 0.37918(14) 0.0298(5) Uani 1 1 d . . . . .
C13 C 0.81227(16) 0.27501(16) 0.41501(14) 0.0282(5) Uani 1 1 d . . . . .
H13 H 0.835677 0.240360 0.465747 0.034 Uiso 1 1 calc R U . . .
C14 C 0.83411(15) 0.36262(16) 0.37484(13) 0.0257(4) Uani 1 1 d . . . . .
C15 C 0.66672(17) 0.10689(16) 0.40205(14) 0.0315(5) Uani 1 1 d . . . . .
H15 H 0.623922 0.131842 0.362115 0.038 Uiso 1 1 calc R U . . .
C16 C 0.67635(18) 0.02076(17) 0.45601(14) 0.0332(5) Uani 1 1 d . . . . .
C17 C 0.62286(18) -0.05504(16) 0.46749(14) 0.0318(5) Uani 1 1 d . . . . .
C18 C 0.50375(18) -0.10466(16) 0.42844(14) 0.0323(5) Uani 1 1 d . . . . .
C19 C 0.51803(19) -0.19049(17) 0.48545(15) 0.0360(5) Uani 1 1 d . . . . .
H19 H 0.479855 -0.236181 0.490843 0.043 Uiso 1 1 calc R U . . .
C20 C 0.5892(2) -0.20784(17) 0.53418(15) 0.0377(6) Uani 1 1 d . . . . .
H20 H 0.600889 -0.266069 0.573675 0.045 Uiso 1 1 calc R U . . .
C21 C 0.64312(19) -0.13983(17) 0.52500(15) 0.0361(5) Uani 1 1 d . . . . .
H21 H 0.693046 -0.150726 0.557300 0.043 Uiso 1 1 calc R U . . .
C22 C 0.42873(19) -0.08449(17) 0.37274(16) 0.0354(5) Uani 1 1 d . . . . .
C23 C 0.3433(2) 0.02831(19) 0.26578(18) 0.0437(6) Uani 1 1 d . . . . .
H23 H 0.286921 -0.001305 0.295896 0.052 Uiso 1 1 calc R U . . .
C24 C 0.3760(2) -0.0042(2) 0.1888(2) 0.0530(7) Uani 1 1 d . . . . .
H24A H 0.323810 0.007464 0.156178 0.079 Uiso 1 1 calc R U . . .
H24B H 0.398137 -0.070146 0.205757 0.079 Uiso 1 1 calc R U . . .
H24C H 0.427039 0.029032 0.155130 0.079 Uiso 1 1 calc R U . . .
C25 C 0.3161(3) 0.1307(2) 0.2427(2) 0.0572(8) Uani 1 1 d . . . . .
H25A H 0.369836 0.161181 0.211113 0.086 Uiso 1 1 calc R U . . .
H25B H 0.296301 0.149735 0.293200 0.086 Uiso 1 1 calc R U . . .
H25C H 0.264481 0.147941 0.208711 0.086 Uiso 1 1 calc R U . . .
C26 C 0.83365(14) 0.53063(15) 0.46918(12) 0.0236(4) Uani 1 1 d . . . . .
C27 C 0.79827(15) 0.56598(15) 0.53534(12) 0.0236(4) Uani 1 1 d . . . . .
H27 H 0.781086 0.630088 0.526540 0.028 Uiso 1 1 calc R U . . .
C28 C 0.78875(14) 0.50518(15) 0.61443(12) 0.0230(4) Uani 1 1 d . . . . .
C29 C 0.81405(16) 0.41152(15) 0.62820(13) 0.0258(4) Uani 1 1 d D . . . .
H29 H 0.807684 0.371099 0.682987 0.031 Uiso 1 1 calc R U . . .
C30 C 0.84893(16) 0.37683(15) 0.56119(13) 0.0262(4) Uani 1 1 d D . . . .
H30 H 0.866118 0.312721 0.570007 0.031 Uiso 1 1 calc DR U . . .
C31 C 0.85829(15) 0.43729(15) 0.48112(13) 0.0240(4) Uani 1 1 d D . . . .
C32 C 0.72900(15) 0.49219(15) 0.76352(12) 0.0247(4) Uani 1 1 d . . . . .
H32 H 0.739902 0.427712 0.787981 0.030 Uiso 1 1 calc R U . . .
C33 C 0.68817(16) 0.55733(16) 0.80195(13) 0.0260(4) Uani 1 1 d . . . . .
C34 C 0.65206(16) 0.54352(16) 0.88979(13) 0.0279(5) Uani 1 1 d . . . . .
C35 C 0.62381(17) 0.44070(19) 1.01756(14) 0.0326(5) Uani 1 1 d . . . . .
C36 C 0.58905(18) 0.5099(2) 1.05432(14) 0.0377(6) Uani 1 1 d . . . . .
H36 H 0.568091 0.495860 1.112052 0.045 Uiso 1 1 calc R U . . .
C37 C 0.58566(19) 0.5992(2) 1.00531(15) 0.0403(6) Uani 1 1 d . . . . .
H37 H 0.562096 0.648190 1.028593 0.048 Uiso 1 1 calc R U . . .
C38 C 0.61705(18) 0.61703(19) 0.92144(15) 0.0355(5) Uani 1 1 d . . . . .
H38 H 0.614711 0.678283 0.886170 0.043 Uiso 1 1 calc R U . . .
C39 C 0.62434(18) 0.34260(19) 1.06931(14) 0.0355(5) Uani 1 1 d . . . . .
C40 C 0.6419(2) 0.1820(2) 1.07192(16) 0.0466(7) Uani 1 1 d . . . . .
H40 H 0.587116 0.173268 1.115977 0.056 Uiso 1 1 calc R U . . .
C41 C 0.7300(3) 0.1477(2) 1.1134(2) 0.0655(9) Uani 1 1 d . . . . .
H41A H 0.727251 0.084691 1.149242 0.098 Uiso 1 1 calc R U . . .
H41B H 0.735563 0.187155 1.146970 0.098 Uiso 1 1 calc R U . . .
H41C H 0.784360 0.148983 1.071054 0.098 Uiso 1 1 calc R U . . .
C42 C 0.6334(3) 0.1310(2) 1.0118(2) 0.0637(10) Uani 1 1 d . . . . .
H42A H 0.689468 0.133725 0.971145 0.096 Uiso 1 1 calc R U . . .
H42B H 0.578244 0.159294 0.983084 0.096 Uiso 1 1 calc R U . . .
H42C H 0.626933 0.066810 1.042265 0.096 Uiso 1 1 calc R U . . .
C43 C 0.74192(15) 0.57780(15) 0.28600(12) 0.0241(4) Uani 1 1 d . . . . .
C44 C 0.66026(15) 0.59940(15) 0.24897(12) 0.0246(4) Uani 1 1 d . . . . .
H44 H 0.653512 0.573516 0.207005 0.029 Uiso 1 1 calc R U . . .
C45 C 0.58889(15) 0.65966(15) 0.27481(12) 0.0240(4) Uani 1 1 d . . . . .
C46 C 0.59819(17) 0.69875(15) 0.33591(13) 0.0282(5) Uani 1 1 d . . . . .
H46 H 0.548438 0.740046 0.352770 0.034 Uiso 1 1 calc R U . . .
C47 C 0.68003(17) 0.67703(15) 0.37157(13) 0.0281(5) Uani 1 1 d . . . . .
H47 H 0.686996 0.703225 0.413260 0.034 Uiso 1 1 calc R U . . .
C48 C 0.75253(15) 0.61648(15) 0.34625(12) 0.0237(4) Uani 1 1 d . . . . .
C49 C 0.42044(16) 0.72461(15) 0.26433(13) 0.0262(4) Uani 1 1 d . . . . .
H49 H 0.405545 0.747657 0.310982 0.031 Uiso 1 1 calc R U . . .
C50 C 0.36224(16) 0.72753(15) 0.20808(13) 0.0250(4) Uani 1 1 d . . . . .
C51 C 0.26310(16) 0.76399(15) 0.20450(13) 0.0269(5) Uani 1 1 d . . . . .
C52 C 0.12560(16) 0.76188(16) 0.15715(14) 0.0295(5) Uani 1 1 d . . . . .
C53 C 0.07743(18) 0.82564(18) 0.19638(17) 0.0385(6) Uani 1 1 d . . . . .
H53 H 0.012987 0.846608 0.191866 0.046 Uiso 1 1 calc R U . . .
C54 C 0.12574(19) 0.85792(19) 0.24228(18) 0.0419(6) Uani 1 1 d . . . . .
H54 H 0.094463 0.901345 0.269955 0.050 Uiso 1 1 calc R U . . .
C55 C 0.21958(18) 0.82665(17) 0.24760(16) 0.0343(5) Uani 1 1 d . . . . .
H55 H 0.253570 0.847095 0.279592 0.041 Uiso 1 1 calc R U . . .
C56 C 0.07374(17) 0.72124(17) 0.11087(14) 0.0312(5) Uani 1 1 d . . . . .
C57 C 0.08464(18) 0.6158(2) 0.02728(15) 0.0370(6) Uani 1 1 d . . . . .
H57 H 0.015271 0.623407 0.042329 0.044 Uiso 1 1 calc R U . . .
C58 C 0.1051(2) 0.6641(2) -0.06473(17) 0.0511(7) Uani 1 1 d . . . . .
H58A H 0.172592 0.655630 -0.081704 0.077 Uiso 1 1 calc R U . . .
H58B H 0.082593 0.729751 -0.075408 0.077 Uiso 1 1 calc R U . . .
H58C H 0.073133 0.638209 -0.096417 0.077 Uiso 1 1 calc R U . . .
C59 C 0.1184(2) 0.5143(2) 0.04758(17) 0.0413(6) Uani 1 1 d . . . . .
H59A H 0.083548 0.485830 0.020311 0.062 Uiso 1 1 calc R U . . .
H59B H 0.108453 0.486354 0.107763 0.062 Uiso 1 1 calc R U . . .
H59C H 0.185214 0.504792 0.027861 0.062 Uiso 1 1 calc R U . . .
N1 N 0.73181(15) 0.14865(14) 0.41824(12) 0.0320(4) Uani 1 1 d . . . . .
N2 N 0.77987(16) 0.09097(15) 0.48004(14) 0.0381(5) Uani 1 1 d . . . . .
N3 N 0.74590(16) 0.01315(15) 0.50297(14) 0.0380(5) Uani 1 1 d . . . . .
N4 N 0.55428(15) -0.03706(13) 0.41909(12) 0.0324(4) Uani 1 1 d . . . . .
N5 N 0.41546(17) 0.00063(15) 0.32168(14) 0.0392(5) Uani 1 1 d . . . . .
H5 H 0.450944 0.040965 0.321700 0.047 Uiso 1 1 calc R U . . .
N6 N 0.75035(13) 0.53937(13) 0.68354(10) 0.0243(4) Uani 1 1 d . . . . .
N7 N 0.72363(15) 0.63053(13) 0.67205(12) 0.0319(4) Uani 1 1 d . . . . .
N8 N 0.68596(16) 0.64108(14) 0.74415(12) 0.0340(5) Uani 1 1 d . . . . .
N9 N 0.65585(13) 0.45619(14) 0.93672(11) 0.0290(4) Uani 1 1 d . . . . .
N10 N 0.63892(16) 0.28026(15) 1.02878(12) 0.0383(5) Uani 1 1 d . . . . .
H10A H 0.647067 0.298416 0.974191 0.046 Uiso 1 1 calc R U . . .
N11 N 0.50317(13) 0.68195(12) 0.23887(10) 0.0242(4) Uani 1 1 d . . . . .
N12 N 0.49719(14) 0.65886(14) 0.16988(11) 0.0282(4) Uani 1 1 d . . . . .
N13 N 0.41204(13) 0.68594(14) 0.15153(11) 0.0282(4) Uani 1 1 d . . . . .
N14 N 0.21701(13) 0.73234(13) 0.15992(11) 0.0260(4) Uani 1 1 d . . . . .
N15 N 0.12494(14) 0.65915(15) 0.07592(12) 0.0314(4) Uani 1 1 d . . . . .
H15A H 0.184597 0.643995 0.082393 0.038 Uiso 1 1 calc R U . . .
O1 O 0.38309(13) -0.14579(12) 0.37474(12) 0.0389(4) Uani 1 1 d . . . . .
O2 O 0.61048(14) 0.32468(14) 1.14598(10) 0.0440(5) Uani 1 1 d . . . . .
O3 O -0.01068(13) 0.74272(14) 0.10927(13) 0.0443(5) Uani 1 1 d . . . . .
C60 C 0.4861(2) 0.4501(2) 0.35151(19) 0.0503(7) Uani 1 1 d . . . . .
H60A H 0.449709 0.398605 0.366551 0.075 Uiso 1 1 calc R U . . .
H60B H 0.548968 0.432224 0.326321 0.075 Uiso 1 1 calc R U . . .
H60C H 0.455088 0.502782 0.311769 0.075 Uiso 1 1 calc R U . . .
C61 C 0.49295(18) 0.47573(19) 0.42825(17) 0.0406(6) Uani 1 1 d . . . . .
C62 C 0.42174(18) 0.53199(19) 0.46014(18) 0.0422(6) Uani 1 1 d . . . . .
H62 H 0.367043 0.554573 0.433106 0.051 Uiso 1 1 calc R U . . .
C63 C 0.42830(19) 0.55600(19) 0.53010(18) 0.0423(6) Uani 1 1 d . . . . .
H63 H 0.378275 0.594780 0.550105 0.051 Uiso 1 1 calc R U . . .
C64 C 0.3189(3) 0.1743(3) -0.0778(2) 0.0501(9) Uani 0.816(4) 1 d D U P A 1
C65 C 0.2395(4) 0.1959(4) -0.1060(3) 0.0674(13) Uani 0.816(4) 1 d D U P A 1
H65 H 0.192403 0.232514 -0.080466 0.081 Uiso 0.816(4) 1 calc R U P A 1
C66 C 0.2169(3) 0.1713(3) -0.1690(2) 0.0523(9) Uani 0.816(4) 1 d D U P A 1
H66 H 0.155881 0.188748 -0.185420 0.063 Uiso 0.816(4) 1 calc R U P A 1
C67 C 0.2856(3) 0.1197(2) -0.2090(2) 0.0454(8) Uani 0.816(4) 1 d D U P A 1
C68 C 0.3742(3) 0.0959(3) -0.1838(3) 0.0511(10) Uani 0.816(4) 1 d D U P A 1
H68 H 0.422422 0.061332 -0.210478 0.061 Uiso 0.816(4) 1 calc R U P A 1
C69 C 0.3901(3) 0.1241(4) -0.1183(3) 0.0552(11) Uani 0.816(4) 1 d D U P A 1
H69 H 0.450444 0.109176 -0.100432 0.066 Uiso 0.816(4) 1 calc R U P A 1
C70 C 0.3402(4) 0.2021(4) -0.0043(3) 0.0778(14) Uani 0.816(4) 1 d D U P A 1
H70A H 0.318240 0.267445 -0.012081 0.117 Uiso 0.816(4) 1 calc R U P A 1
H70B H 0.407723 0.190593 -0.001565 0.117 Uiso 0.816(4) 1 calc R U P A 1
H70C H 0.308046 0.165913 0.047445 0.117 Uiso 0.816(4) 1 calc R U P A 1
C71 C 0.2632(3) 0.0916(3) -0.2794(2) 0.0562(10) Uani 0.816(4) 1 d D U P A 1
H71A H 0.196697 0.084843 -0.271295 0.084 Uiso 0.816(4) 1 calc R U P A 1
H71B H 0.300798 0.032981 -0.280892 0.084 Uiso 0.816(4) 1 calc R U P A 1
H71C H 0.277601 0.138571 -0.331821 0.084 Uiso 0.816(4) 1 calc R U P A 1
C64A C 0.2664(12) 0.2110(8) -0.0476(9) 0.072(3) Uani 0.184(4) 1 d D U P A 2
C65A C 0.2239(15) 0.2002(11) -0.1048(10) 0.059(3) Uani 0.184(4) 1 d D U P A 2
H65A H 0.160315 0.224990 -0.109802 0.070 Uiso 0.184(4) 1 calc R U P A 2
C66A C 0.2718(13) 0.1536(11) -0.1559(11) 0.062(2) Uani 0.184(4) 1 d D U P A 2
H66A H 0.236305 0.148602 -0.195616 0.075 Uiso 0.184(4) 1 calc R U P A 2
C67A C 0.3614(14) 0.1120(10) -0.1622(12) 0.060(3) Uani 0.184(4) 1 d D U P A 2
C68A C 0.4134(15) 0.1198(14) -0.1024(12) 0.061(3) Uani 0.184(4) 1 d D U P A 2
H68A H 0.476917 0.095119 -0.096852 0.073 Uiso 0.184(4) 1 calc R U P A 2
C69A C 0.3579(13) 0.1680(11) -0.0545(12) 0.068(3) Uani 0.184(4) 1 d D U P A 2
H69A H 0.391095 0.174362 -0.013841 0.081 Uiso 0.184(4) 1 calc R U P A 2
C70A C 0.2123(10) 0.2653(9) 0.0131(8) 0.040(3) Uani 0.184(4) 1 d D U P A 2
H70D H 0.198465 0.330138 -0.017636 0.060 Uiso 0.184(4) 1 calc R U P A 2
H70E H 0.250828 0.259475 0.056599 0.060 Uiso 0.184(4) 1 calc R U P A 2
H70F H 0.153702 0.240278 0.038511 0.060 Uiso 0.184(4) 1 calc R U P A 2
C71A C 0.4123(19) 0.0603(13) -0.2209(13) 0.098(6) Uani 0.184(4) 1 d D U P A 2
H71D H 0.377772 0.010627 -0.218518 0.147 Uiso 0.184(4) 1 calc R U P A 2
H71E H 0.474951 0.034409 -0.205059 0.147 Uiso 0.184(4) 1 calc R U P A 2
H71F H 0.417711 0.102025 -0.277432 0.147 Uiso 0.184(4) 1 calc R U P A 2
C72 C 0.0273(2) 1.1610(2) 0.28387(19) 0.0564(8) Uani 1 1 d . . . . .
C73 C -0.0524(3) 1.1351(3) 0.2706(2) 0.0633(10) Uani 1 1 d . . . . .
H73 H -0.089354 1.176504 0.230502 0.076 Uiso 1 1 calc R U . . .
C74 C -0.0805(3) 1.0508(3) 0.3139(2) 0.0630(9) Uani 1 1 d . . . . .
H74 H -0.135648 1.034949 0.302590 0.076 Uiso 1 1 calc R U . . .
C75 C -0.0290(3) 0.9885(2) 0.3741(2) 0.0583(9) Uani 1 1 d . . . . .
C76 C 0.0498(3) 1.0144(3) 0.3887(2) 0.0640(10) Uani 1 1 d . . . . .
H76 H 0.085817 0.973557 0.429813 0.077 Uiso 1 1 calc R U . . .
C77 C 0.0780(3) 1.0991(3) 0.3447(2) 0.0636(9) Uani 1 1 d . . . . .
H77 H 0.132985 1.115080 0.356220 0.076 Uiso 1 1 calc R U . . .
C78 C 0.0594(3) 1.2509(3) 0.2347(2) 0.0689(10) Uani 1 1 d . . . . .
H78A H 0.082291 1.249775 0.177704 0.103 Uiso 1 1 calc R U . . .
H78B H 0.109984 1.261819 0.259985 0.103 Uiso 1 1 calc R U . . .
H78C H 0.007115 1.300162 0.234184 0.103 Uiso 1 1 calc R U . . .
C79 C -0.0587(3) 0.8968(3) 0.4212(2) 0.0750(11) Uani 1 1 d . . . . .
H79A H -0.126652 0.903526 0.435977 0.113 Uiso 1 1 calc R U . . .
H79B H -0.028100 0.871629 0.471870 0.113 Uiso 1 1 calc R U . . .
H79C H -0.040669 0.855097 0.386668 0.113 Uiso 1 1 calc R U . . .
C81 C 0.0587(13) 1.0470(9) 0.0402(10) 0.057(3) Uani 0.359(3) 1 d D U P B -1
C82 C -0.0365(13) 1.0365(9) 0.0669(11) 0.061(3) Uani 0.359(3) 1 d D U P B -1
H82 H -0.066823 1.057682 0.112405 0.074 Uiso 0.359(3) 1 calc R U P B -1
C83 C -0.0873(12) 0.9969(8) 0.0298(10) 0.048(3) Uani 0.359(3) 1 d D U P B -1
H83 H -0.151108 0.991436 0.050339 0.057 Uiso 0.359(3) 1 calc R U P B -1
C84 C -0.0463(11) 0.9641(9) -0.0385(10) 0.049(2) Uani 0.359(3) 1 d D U P B -1
C85 C 0.0485(11) 0.9740(9) -0.0661(10) 0.042(2) Uani 0.359(3) 1 d D U P B -1
H85 H 0.078919 0.953533 -0.112013 0.050 Uiso 0.359(3) 1 calc R U P B -1
C86 C 0.0976(12) 1.0135(10) -0.0269(10) 0.049(2) Uani 0.359(3) 1 d D U P B -1
H86 H 0.161693 1.018063 -0.046798 0.059 Uiso 0.359(3) 1 calc R U P B -1
C87 C 0.1221(11) 1.0901(10) 0.0764(11) 0.062(4) Uani 0.359(3) 1 d D U P B -1
H87A H 0.114319 1.156775 0.051176 0.093 Uiso 0.359(3) 1 calc R U P B -1
H87B H 0.187448 1.065004 0.064561 0.093 Uiso 0.359(3) 1 calc R U P B -1
H87C H 0.104941 1.076190 0.136558 0.093 Uiso 0.359(3) 1 calc R U P B -1
C88 C -0.0978(8) 0.9189(8) -0.0827(9) 0.045(3) Uani 0.359(3) 1 d D U P B -1
H88A H -0.075969 0.852909 -0.068280 0.067 Uiso 0.359(3) 1 calc R U P B -1
H88B H -0.085236 0.945983 -0.142815 0.067 Uiso 0.359(3) 1 calc R U P B -1
H88C H -0.165135 0.928776 -0.065294 0.067 Uiso 0.359(3) 1 calc R U P B -1
C81A C -0.0105(14) 1.0045(12) -0.0026(12) 0.052(2) Uani 0.141(3) 1 d D U P B -2
C82A C -0.1091(14) 1.0213(12) 0.0057(12) 0.060(3) Uani 0.141(3) 1 d D U P B -2
H82A H -0.135597 1.053443 0.045034 0.071 Uiso 0.141(3) 1 calc R U P B -2
C83A C -0.1764(12) 0.9992(11) -0.0338(10) 0.047(3) Uani 0.141(3) 1 d D U P B -2
H83A H -0.242296 1.013853 -0.024275 0.057 Uiso 0.141(3) 1 calc R U P B -2
C84A C -0.1240(14) 0.9484(11) -0.0935(11) 0.056(4) Uani 0.141(3) 1 d D U P B -2
C85A C -0.0256(12) 0.9251(12) -0.1121(11) 0.048(3) Uani 0.141(3) 1 d D U P B -2
H85A H 0.002968 0.893545 -0.151360 0.058 Uiso 0.141(3) 1 calc R U P B -2
C86A C 0.0243(18) 0.9568(13) -0.0619(13) 0.053(3) Uani 0.141(3) 1 d D U P B -2
H86A H 0.090484 0.943401 -0.070212 0.064 Uiso 0.141(3) 1 calc R U P B -2
C87A C 0.059(2) 1.0302(17) 0.0418(16) 0.041(4) Uani 0.141(3) 1 d D U P B -2
H87D H 0.088723 1.081847 0.003873 0.061 Uiso 0.141(3) 1 calc R U P B -2
H87E H 0.106098 0.977453 0.059675 0.061 Uiso 0.141(3) 1 calc R U P B -2
H87F H 0.024878 1.047631 0.090422 0.061 Uiso 0.141(3) 1 calc R U P B -2
C88A C -0.187(2) 0.9201(17) -0.1418(17) 0.118(9) Uani 0.141(3) 1 d D U P B -2
H88D H -0.186990 0.962810 -0.197851 0.177 Uiso 0.141(3) 1 calc R U P B -2
H88E H -0.251069 0.921524 -0.113108 0.177 Uiso 0.141(3) 1 calc R U P B -2
H88F H -0.163764 0.857887 -0.145138 0.177 Uiso 0.141(3) 1 calc R U P B -2
O4 O 0.50254(16) 0.20972(15) 0.27151(12) 0.0466(5) Uani 1 1 d . . . . .
H4A H 0.532(3) 0.247(3) 0.223(3) 0.070 Uiso 1 1 d . U . . .
H4B H 0.441(3) 0.241(3) 0.269(2) 0.070 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.529(3) . ?
C2 C3 1.596(3) . ?
C2 C4 1.589(3) . ?
C2 C5 1.588(3) . ?
C3 C6 1.536(3) . ?
C3 C9 1.507(3) . ?
C3 C43 1.522(3) . ?
C4 C7 1.542(3) . ?
C4 C14 1.523(3) . ?
C4 C31 1.513(3) . ?
C5 C8 1.540(3) . ?
C5 C26 1.513(3) . ?
C5 C48 1.514(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.393(3) . ?
C9 C14 1.393(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.380(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.393(3) . ?
C12 C13 1.397(3) . ?
C12 N1 1.418(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.382(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.363(3) . ?
C15 N1 1.349(3) . ?
C16 C17 1.469(4) . ?
C16 N3 1.368(3) . ?
C17 C21 1.390(3) . ?
C17 N4 1.345(3) . ?
C18 C19 1.386(4) . ?
C18 C22 1.503(4) . ?
C18 N4 1.340(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.381(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.380(4) . ?
C21 H21 0.9500 . ?
C22 N5 1.336(3) . ?
C22 O1 1.242(3) . ?
C23 H23 1.0000 . ?
C23 C24 1.527(4) . ?
C23 C25 1.506(4) . ?
C23 N5 1.462(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.392(3) . ?
C26 C31 1.385(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(3) . ?
C28 C29 1.386(3) . ?
C28 N6 1.433(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.397(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.396(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.369(3) . ?
C32 N6 1.347(3) . ?
C33 C34 1.467(3) . ?
C33 N8 1.362(3) . ?
C34 C38 1.391(3) . ?
C34 N9 1.336(3) . ?
C35 C36 1.387(4) . ?
C35 C39 1.499(4) . ?
C35 N9 1.342(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.372(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.385(3) . ?
C38 H38 0.9500 . ?
C39 N10 1.324(3) . ?
C39 O2 1.241(3) . ?
C40 H40 1.0000 . ?
C40 C41 1.511(5) . ?
C40 C42 1.510(4) . ?
C40 N10 1.465(3) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.387(3) . ?
C43 C48 1.384(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.384(3) . ?
C45 C46 1.396(3) . ?
C45 N11 1.431(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.377(3) . ?
C47 H47 0.9500 . ?
C47 C48 1.393(3) . ?
C49 H49 0.9500 . ?
C49 C50 1.375(3) . ?
C49 N11 1.346(3) . ?
C50 C51 1.466(3) . ?
C50 N13 1.366(3) . ?
C51 C55 1.400(3) . ?
C51 N14 1.342(3) . ?
C52 C53 1.389(3) . ?
C52 C56 1.510(3) . ?
C52 N14 1.340(3) . ?
C53 H53 0.9500 . ?
C53 C54 1.387(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.382(4) . ?
C55 H55 0.9500 . ?
C56 N15 1.340(3) . ?
C56 O3 1.225(3) . ?
C57 H57 1.0000 . ?
C57 C58 1.519(4) . ?
C57 C59 1.509(4) . ?
C57 N15 1.465(3) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
N1 N2 1.360(3) . ?
N2 N3 1.305(3) . ?
N5 H5 0.8800 . ?
N6 N7 1.357(3) . ?
N7 N8 1.310(3) . ?
N10 H10A 0.8800 . ?
N11 N12 1.355(2) . ?
N12 N13 1.302(3) . ?
N15 H15A 0.8800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C60 C61 1.508(4) . ?
C61 C62 1.388(4) . ?
C61 C63 1.392(4) 2_666 ?
C62 H62 0.9500 . ?
C62 C63 1.381(4) . ?
C63 H63 0.9500 . ?
C64 C65 1.284(7) . ?
C64 C69 1.405(7) . ?
C64 C70 1.543(6) . ?
C65 H65 0.9500 . ?
C65 C66 1.354(7) . ?
C66 H66 0.9500 . ?
C66 C67 1.395(5) . ?
C67 C68 1.387(6) . ?
C67 C71 1.501(5) . ?
C68 H68 0.9500 . ?
C68 C69 1.389(7) . ?
C69 H69 0.9500 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C64A C65A 1.309(17) . ?
C64A C69A 1.391(17) . ?
C64A C70A 1.563(16) . ?
C65A H65A 0.9500 . ?
C65A C66A 1.336(17) . ?
C66A H66A 0.9500 . ?
C66A C67A 1.358(17) . ?
C67A C68A 1.419(19) . ?
C67A C71A 1.496(17) . ?
C68A H68A 0.9500 . ?
C68A C69A 1.353(19) . ?
C69A H69A 0.9500 . ?
C70A H70D 0.9800 . ?
C70A H70E 0.9800 . ?
C70A H70F 0.9800 . ?
C71A H71D 0.9800 . ?
C71A H71E 0.9800 . ?
C71A H71F 0.9800 . ?
C72 C73 1.373(5) . ?
C72 C77 1.392(5) . ?
C72 C78 1.494(6) . ?
C73 H73 0.9500 . ?
C73 C74 1.380(6) . ?
C74 H74 0.9500 . ?
C74 C75 1.394(5) . ?
C75 C76 1.369(5) . ?
C75 C79 1.496(6) . ?
C76 H76 0.9500 . ?
C76 C77 1.388(6) . ?
C77 H77 0.9500 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C81 C82 1.413(9) . ?
C81 C86 1.399(9) . ?
C81 C87 1.537(9) . ?
C82 H82 0.9500 . ?
C82 C83 1.376(9) . ?
C83 H83 0.9500 . ?
C83 C84 1.415(8) . ?
C84 C85 1.407(8) . ?
C84 C88 1.530(9) . ?
C85 H85 0.9500 . ?
C85 C86 1.382(8) . ?
C86 H86 0.9500 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C81A C82A 1.411(18) . ?
C81A C86A 1.411(19) . ?
C81A C87A 1.533(19) . ?
C82A H82A 0.9500 . ?
C82A C83A 1.425(18) . ?
C83A H83A 0.9500 . ?
C83A C84A 1.507(18) . ?
C84A C85A 1.429(18) . ?
C84A C88A 1.53(2) . ?
C85A H85A 0.9500 . ?
C85A C86A 1.454(19) . ?
C86A H86A 0.9500 . ?
C87A H87D 0.9800 . ?
C87A H87E 0.9800 . ?
C87A H87F 0.9800 . ?
C88A H88D 0.9800 . ?
C88A H88E 0.9800 . ?
C88A H88F 0.9800 . ?
O4 H4A 0.94(4) . ?
O4 H4B 0.95(4) . ?

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
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C3 112.48(17) . . ?
C1 C2 C4 112.04(19) . . ?
C1 C2 C5 112.77(19) . . ?
C4 C2 C3 106.32(17) . . ?
C5 C2 C3 106.54(17) . . ?
C5 C2 C4 106.20(16) . . ?
C6 C3 C2 116.37(18) . . ?
C9 C3 C2 104.36(17) . . ?
C9 C3 C6 112.06(18) . . ?
C9 C3 C43 109.48(18) . . ?
C43 C3 C2 103.92(16) . . ?
C43 C3 C6 110.14(18) . . ?
C7 C4 C2 116.47(19) . . ?
C14 C4 C2 104.31(17) . . ?
C14 C4 C7 109.70(19) . . ?
C31 C4 C2 104.08(17) . . ?
C31 C4 C7 108.89(17) . . ?
C31 C4 C14 113.40(18) . . ?
C8 C5 C2 116.24(18) . . ?
C26 C5 C2 104.47(17) . . ?
C26 C5 C8 110.95(17) . . ?
C26 C5 C48 109.85(17) . . ?
C48 C5 C2 104.17(16) . . ?
C48 C5 C8 110.75(19) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C3 127.4(2) . . ?
C14 C9 C3 112.65(19) . . ?
C14 C9 C10 119.9(2) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.9(2) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.7(2) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C13 121.1(2) . . ?
C11 C12 N1 118.9(2) . . ?
C13 C12 N1 119.9(2) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 C12 118.4(2) . . ?
C14 C13 H13 120.8 . . ?
C9 C14 C4 112.1(2) . . ?
C13 C14 C4 126.9(2) . . ?
C13 C14 C9 121.0(2) . . ?
C16 C15 H15 127.9 . . ?
N1 C15 H15 127.9 . . ?
N1 C15 C16 104.3(2) . . ?
C15 C16 C17 128.8(2) . . ?
C15 C16 N3 109.0(2) . . ?
N3 C16 C17 122.2(2) . . ?
C21 C17 C16 121.3(2) . . ?
N4 C17 C16 115.9(2) . . ?
N4 C17 C21 122.8(2) . . ?
C19 C18 C22 119.6(2) . . ?
N4 C18 C19 123.5(2) . . ?
N4 C18 C22 116.9(2) . . ?
C18 C19 H19 120.9 . . ?
C20 C19 C18 118.3(2) . . ?
C20 C19 H19 120.9 . . ?
C19 C20 H20 120.3 . . ?
C21 C20 C19 119.4(2) . . ?
C21 C20 H20 120.3 . . ?
C17 C21 H21 120.7 . . ?
C20 C21 C17 118.6(2) . . ?
C20 C21 H21 120.7 . . ?
N5 C22 C18 116.8(2) . . ?
O1 C22 C18 120.2(2) . . ?
O1 C22 N5 123.0(2) . . ?
C24 C23 H23 108.1 . . ?
C25 C23 H23 108.1 . . ?
C25 C23 C24 111.3(3) . . ?
N5 C23 H23 108.1 . . ?
N5 C23 C24 111.0(2) . . ?
N5 C23 C25 110.2(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C5 126.5(2) . . ?
C31 C26 C5 111.97(18) . . ?
C31 C26 C27 121.4(2) . . ?
C26 C27 H27 120.9 . . ?
C28 C27 C26 118.2(2) . . ?
C28 C27 H27 120.9 . . ?
C27 C28 C29 121.47(19) . . ?
C27 C28 N6 119.48(19) . . ?
C29 C28 N6 119.03(18) . . ?
C28 C29 H29 120.1 . . ?
C28 C29 C30 119.7(2) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 H30 120.3 . . ?
C31 C30 C29 119.4(2) . . ?
C31 C30 H30 120.3 . . ?
C26 C31 C4 112.87(19) . . ?
C26 C31 C30 119.75(19) . . ?
C30 C31 C4 127.3(2) . . ?
C33 C32 H32 127.5 . . ?
N6 C32 H32 127.5 . . ?
N6 C32 C33 105.02(19) . . ?
C32 C33 C34 127.9(2) . . ?
N8 C33 C32 108.34(18) . . ?
N8 C33 C34 123.7(2) . . ?
C38 C34 C33 121.7(2) . . ?
N9 C34 C33 115.5(2) . . ?
N9 C34 C38 122.8(2) . . ?
C36 C35 C39 119.2(2) . . ?
N9 C35 C36 123.6(2) . . ?
N9 C35 C39 117.2(2) . . ?
C35 C36 H36 120.8 . . ?
C37 C36 C35 118.4(2) . . ?
C37 C36 H36 120.8 . . ?
C36 C37 H37 120.4 . . ?
C36 C37 C38 119.1(2) . . ?
C38 C37 H37 120.4 . . ?
C34 C38 H38 120.6 . . ?
C37 C38 C34 118.8(2) . . ?
C37 C38 H38 120.6 . . ?
N10 C39 C35 116.6(2) . . ?
O2 C39 C35 119.2(2) . . ?
O2 C39 N10 124.2(3) . . ?
C41 C40 H40 108.2 . . ?
C42 C40 H40 108.2 . . ?
C42 C40 C41 112.7(3) . . ?
N10 C40 H40 108.2 . . ?
N10 C40 C41 109.7(2) . . ?
N10 C40 C42 109.8(2) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C3 126.55(19) . . ?
C48 C43 C3 112.36(19) . . ?
C48 C43 C44 121.0(2) . . ?
C43 C44 H44 120.9 . . ?
C45 C44 C43 118.21(19) . . ?
C45 C44 H44 120.9 . . ?
C44 C45 C46 121.5(2) . . ?
C44 C45 N11 119.51(18) . . ?
C46 C45 N11 119.0(2) . . ?
C45 C46 H46 120.2 . . ?
C47 C46 C45 119.5(2) . . ?
C47 C46 H46 120.2 . . ?
C46 C47 H47 120.1 . . ?
C46 C47 C48 119.7(2) . . ?
C48 C47 H47 120.1 . . ?
C43 C48 C5 112.84(19) . . ?
C43 C48 C47 120.0(2) . . ?
C47 C48 C5 127.12(19) . . ?
C50 C49 H49 127.5 . . ?
N11 C49 H49 127.5 . . ?
N11 C49 C50 104.92(18) . . ?
C49 C50 C51 130.1(2) . . ?
N13 C50 C49 108.07(19) . . ?
N13 C50 C51 121.76(19) . . ?
C55 C51 C50 120.9(2) . . ?
N14 C51 C50 116.47(19) . . ?
N14 C51 C55 122.6(2) . . ?
C53 C52 C56 119.6(2) . . ?
N14 C52 C53 122.8(2) . . ?
N14 C52 C56 117.5(2) . . ?
C52 C53 H53 120.8 . . ?
C54 C53 C52 118.4(2) . . ?
C54 C53 H53 120.8 . . ?
C53 C54 H54 120.1 . . ?
C55 C54 C53 119.7(2) . . ?
C55 C54 H54 120.1 . . ?
C51 C55 H55 121.0 . . ?
C54 C55 C51 118.1(2) . . ?
C54 C55 H55 121.0 . . ?
N15 C56 C52 115.9(2) . . ?
O3 C56 C52 120.4(2) . . ?
O3 C56 N15 123.6(2) . . ?
C58 C57 H57 107.7 . . ?
C59 C57 H57 107.7 . . ?
C59 C57 C58 111.9(2) . . ?
N15 C57 H57 107.7 . . ?
N15 C57 C58 110.1(2) . . ?
N15 C57 C59 111.5(2) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C15 N1 C12 129.0(2) . . ?
C15 N1 N2 110.9(2) . . ?
N2 N1 C12 120.0(2) . . ?
N3 N2 N1 107.0(2) . . ?
N2 N3 C16 108.7(2) . . ?
C18 N4 C17 117.4(2) . . ?
C22 N5 C23 121.5(2) . . ?
C22 N5 H5 119.2 . . ?
C23 N5 H5 119.2 . . ?
C32 N6 C28 128.91(19) . . ?
C32 N6 N7 110.40(17) . . ?
N7 N6 C28 120.52(17) . . ?
N8 N7 N6 107.22(18) . . ?
N7 N8 C33 109.02(19) . . ?
C34 N9 C35 117.3(2) . . ?
C39 N10 C40 122.1(2) . . ?
C39 N10 H10A 119.0 . . ?
C40 N10 H10A 119.0 . . ?
C49 N11 C45 129.09(18) . . ?
C49 N11 N12 110.35(18) . . ?
N12 N11 C45 120.55(18) . . ?
N13 N12 N11 107.66(17) . . ?
N12 N13 C50 109.00(17) . . ?
C52 N14 C51 118.3(2) . . ?
C56 N15 C57 122.0(2) . . ?
C56 N15 H15A 119.0 . . ?
C57 N15 H15A 119.0 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
C62 C61 C60 121.7(3) . . ?
C62 C61 C63 117.2(3) . 2_666 ?
C63 C61 C60 121.0(3) 2_666 . ?
C61 C62 H62 119.1 . . ?
C63 C62 C61 121.8(3) . . ?
C63 C62 H62 119.1 . . ?
C61 C63 H63 119.5 2_666 . ?
C62 C63 C61 121.0(3) . 2_666 ?
C62 C63 H63 119.5 . . ?
C65 C64 C69 117.1(4) . . ?
C65 C64 C70 123.7(5) . . ?
C69 C64 C70 119.2(4) . . ?
C64 C65 H65 117.1 . . ?
C64 C65 C66 125.8(6) . . ?
C66 C65 H65 117.1 . . ?
C65 C66 H66 120.9 . . ?
C65 C66 C67 118.2(5) . . ?
C67 C66 H66 120.9 . . ?
C66 C67 C71 119.7(4) . . ?
C68 C67 C66 119.4(4) . . ?
C68 C67 C71 120.9(3) . . ?
C67 C68 H68 121.1 . . ?
C67 C68 C69 117.8(4) . . ?
C69 C68 H68 121.1 . . ?
C64 C69 H69 119.3 . . ?
C68 C69 C64 121.5(4) . . ?
C68 C69 H69 119.3 . . ?
C64 C70 H70A 109.5 . . ?
C64 C70 H70B 109.5 . . ?
C64 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C67 C71 H71A 109.5 . . ?
C67 C71 H71B 109.5 . . ?
C67 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C65A C64A C69A 108.3(16) . . ?
C65A C64A C70A 119.9(15) . . ?
C69A C64A C70A 131.7(15) . . ?
C64A C65A H65A 120.6 . . ?
C64A C65A C66A 118.7(19) . . ?
C66A C65A H65A 120.6 . . ?
C65A C66A H66A 113.7 . . ?
C65A C66A C67A 132.5(19) . . ?
C67A C66A H66A 113.7 . . ?
C66A C67A C68A 113.0(16) . . ?
C66A C67A C71A 131(2) . . ?
C68A C67A C71A 116.2(18) . . ?
C67A C68A H68A 125.5 . . ?
C69A C68A C67A 109.1(17) . . ?
C69A C68A H68A 125.5 . . ?
C64A C69A H69A 110.8 . . ?
C68A C69A C64A 138.4(19) . . ?
C68A C69A H69A 110.8 . . ?
C64A C70A H70D 109.5 . . ?
C64A C70A H70E 109.5 . . ?
C64A C70A H70F 109.5 . . ?
H70D C70A H70E 109.5 . . ?
H70D C70A H70F 109.5 . . ?
H70E C70A H70F 109.5 . . ?
C67A C71A H71D 109.5 . . ?
C67A C71A H71E 109.5 . . ?
C67A C71A H71F 109.5 . . ?
H71D C71A H71E 109.5 . . ?
H71D C71A H71F 109.5 . . ?
H71E C71A H71F 109.5 . . ?
C73 C72 C77 117.0(4) . . ?
C73 C72 C78 121.8(3) . . ?
C77 C72 C78 121.1(4) . . ?
C72 C73 H73 119.0 . . ?
C72 C73 C74 121.9(3) . . ?
C74 C73 H73 119.0 . . ?
C73 C74 H74 119.6 . . ?
C73 C74 C75 120.9(4) . . ?
C75 C74 H74 119.6 . . ?
C74 C75 C79 121.3(4) . . ?
C76 C75 C74 117.6(4) . . ?
C76 C75 C79 121.2(3) . . ?
C75 C76 H76 119.3 . . ?
C75 C76 C77 121.4(3) . . ?
C77 C76 H76 119.3 . . ?
C72 C77 H77 119.4 . . ?
C76 C77 C72 121.2(4) . . ?
C76 C77 H77 119.4 . . ?
C72 C78 H78A 109.5 . . ?
C72 C78 H78B 109.5 . . ?
C72 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C75 C79 H79A 109.5 . . ?
C75 C79 H79B 109.5 . . ?
C75 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C82 C81 C87 127.5(12) . . ?
C86 C81 C82 114.6(7) . . ?
C86 C81 C87 117.9(11) . . ?
C81 C82 H82 118.6 . . ?
C83 C82 C81 122.9(8) . . ?
C83 C82 H82 118.6 . . ?
C82 C83 H83 119.3 . . ?
C82 C83 C84 121.3(7) . . ?
C84 C83 H83 119.3 . . ?
C83 C84 C88 124.4(10) . . ?
C85 C84 C83 116.7(7) . . ?
C85 C84 C88 118.8(9) . . ?
C84 C85 H85 119.8 . . ?
C86 C85 C84 120.4(7) . . ?
C86 C85 H85 119.8 . . ?
C81 C86 H86 118.0 . . ?
C85 C86 C81 124.1(7) . . ?
C85 C86 H86 118.0 . . ?
C81 C87 H87A 109.5 . . ?
C81 C87 H87B 109.5 . . ?
C81 C87 H87C 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C84 C88 H88A 109.5 . . ?
C84 C88 H88B 109.5 . . ?
C84 C88 H88C 109.5 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C82A C81A C87A 130(2) . . ?
C86A C81A C82A 111.2(17) . . ?
C86A C81A C87A 119.1(19) . . ?
C81A C82A H82A 114.0 . . ?
C81A C82A C83A 132.1(18) . . ?
C83A C82A H82A 114.0 . . ?
C82A C83A H83A 126.2 . . ?
C82A C83A C84A 107.6(15) . . ?
C84A C83A H83A 126.2 . . ?
C83A C84A C88A 114.0(18) . . ?
C85A C84A C83A 129.5(16) . . ?
C85A C84A C88A 116.5(18) . . ?
C84A C85A H85A 125.1 . . ?
C84A C85A C86A 109.8(16) . . ?
C86A C85A H85A 125.1 . . ?
C81A C86A C85A 130(2) . . ?
C81A C86A H86A 115.1 . . ?
C85A C86A H86A 115.1 . . ?
C81A C87A H87D 109.5 . . ?
C81A C87A H87E 109.5 . . ?
C81A C87A H87F 109.5 . . ?
H87D C87A H87E 109.5 . . ?
H87D C87A H87F 109.5 . . ?
H87E C87A H87F 109.5 . . ?
C84A C88A H88D 109.5 . . ?
C84A C88A H88E 109.5 . . ?
C84A C88A H88F 109.5 . . ?
H88D C88A H88E 109.5 . . ?
H88D C88A H88F 109.5 . . ?
H88E C88A H88F 109.5 . . ?
H4A O4 H4B 99(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C11 H11 O2 0.95 2.53 3.238(3) 131.3 1_554 yes
C15 H15 O4 0.95 2.45 3.397(3) 171.9 . yes
C20 H20 N7 0.95 2.64 3.441(3) 142.9 1_545 yes
C25 H25A O4 0.98 2.66 3.346(4) 127.2 . yes
C32 H32 N14 0.95 2.36 3.311(3) 173.8 2_666 yes
C37 H37 N12 0.95 2.49 3.227(3) 134.8 1_556 yes
C49 H49 O1 0.95 2.20 3.085(3) 155.1 1_565 yes
C59 H59C N9 0.98 2.71 3.480(3) 135.7 2_666 yes
N5 H5 O4 0.88 2.69 3.492(3) 152.9 . yes
N10 H10A N13 0.88 2.38 3.157(3) 147.6 2_666 yes
N15 H15A N9 0.88 2.60 3.394(3) 150.9 2_666 yes
C66 H66 O3 0.95 2.54 3.212(5) 127.5 2_565 yes
C65A H65A O3 0.95 2.16 3.10(2) 169.9 2_565 yes
C76 H76 N2 0.95 2.57 3.477(4) 159.5 2_666 yes
C79 H79A N3 0.98 2.66 3.434(5) 136.6 1_465 yes
C87A H87D O3 0.98 2.97 3.69(2) 131.4 2_575 yes
O4 H4A O2 0.94(4) 1.87(4) 2.780(3) 164(4) 1_554 yes
O4 H4B N8 0.95(4) 2.35(4) 3.262(3) 161(3) 2_666 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C6 -5.4(3) . . . . ?
C1 C2 C3 C9 118.7(2) . . . . ?
C1 C2 C3 C43 -126.6(2) . . . . ?
C1 C2 C4 C7 -0.5(3) . . . . ?
C1 C2 C4 C14 -121.53(19) . . . . ?
C1 C2 C4 C31 119.36(19) . . . . ?
C1 C2 C5 C8 5.6(3) . . . . ?
C1 C2 C5 C26 -117.0(2) . . . . ?
C1 C2 C5 C48 127.75(19) . . . . ?
C2 C3 C9 C10 -176.5(2) . . . . ?
C2 C3 C9 C14 5.7(2) . . . . ?
C2 C3 C43 C44 -177.5(2) . . . . ?
C2 C3 C43 C48 0.2(2) . . . . ?
C2 C4 C14 C9 1.8(2) . . . . ?
C2 C4 C14 C13 -179.5(2) . . . . ?
C2 C4 C31 C26 0.6(2) . . . . ?
C2 C4 C31 C30 -176.9(2) . . . . ?
C2 C5 C26 C27 176.2(2) . . . . ?
C2 C5 C26 C31 -6.1(2) . . . . ?
C2 C5 C48 C43 -4.0(2) . . . . ?
C2 C5 C48 C47 175.2(2) . . . . ?
C3 C2 C4 C7 122.76(19) . . . . ?
C3 C2 C4 C14 1.7(2) . . . . ?
C3 C2 C4 C31 -117.38(18) . . . . ?
C3 C2 C5 C8 -118.3(2) . . . . ?
C3 C2 C5 C26 119.14(18) . . . . ?
C3 C2 C5 C48 3.9(2) . . . . ?
C3 C9 C10 C11 -176.5(2) . . . . ?
C3 C9 C14 C4 -4.9(3) . . . . ?
C3 C9 C14 C13 176.31(19) . . . . ?
C3 C43 C44 C45 176.5(2) . . . . ?
C3 C43 C48 C5 2.5(3) . . . . ?
C3 C43 C48 C47 -176.78(19) . . . . ?
C4 C2 C3 C6 -128.3(2) . . . . ?
C4 C2 C3 C9 -4.3(2) . . . . ?
C4 C2 C3 C43 110.41(18) . . . . ?
C4 C2 C5 C8 128.70(19) . . . . ?
C4 C2 C5 C26 6.1(2) . . . . ?
C4 C2 C5 C48 -109.17(18) . . . . ?
C5 C2 C3 C6 118.7(2) . . . . ?
C5 C2 C3 C9 -117.28(18) . . . . ?
C5 C2 C3 C43 -2.6(2) . . . . ?
C5 C2 C4 C7 -124.03(19) . . . . ?
C5 C2 C4 C14 114.94(18) . . . . ?
C5 C2 C4 C31 -4.2(2) . . . . ?
C5 C26 C27 C28 177.98(19) . . . . ?
C5 C26 C31 C4 3.6(3) . . . . ?
C5 C26 C31 C30 -178.74(19) . . . . ?
C6 C3 C9 C10 -49.8(3) . . . . ?
C6 C3 C9 C14 132.5(2) . . . . ?
C6 C3 C43 C44 57.2(3) . . . . ?
C6 C3 C43 C48 -125.2(2) . . . . ?
C7 C4 C14 C9 -123.7(2) . . . . ?
C7 C4 C14 C13 55.0(3) . . . . ?
C7 C4 C31 C26 125.4(2) . . . . ?
C7 C4 C31 C30 -52.0(3) . . . . ?
C8 C5 C26 C27 50.2(3) . . . . ?
C8 C5 C26 C31 -132.1(2) . . . . ?
C8 C5 C48 C43 121.7(2) . . . . ?
C8 C5 C48 C47 -59.1(3) . . . . ?
C9 C3 C43 C44 -66.5(3) . . . . ?
C9 C3 C43 C48 111.2(2) . . . . ?
C9 C10 C11 C12 0.4(3) . . . . ?
C10 C9 C14 C4 177.14(19) . . . . ?
C10 C9 C14 C13 -1.6(3) . . . . ?
C10 C11 C12 C13 -1.4(4) . . . . ?
C10 C11 C12 N1 -179.9(2) . . . . ?
C11 C12 C13 C14 0.9(3) . . . . ?
C11 C12 N1 C15 -13.5(4) . . . . ?
C11 C12 N1 N2 164.8(2) . . . . ?
C12 C13 C14 C4 -177.9(2) . . . . ?
C12 C13 C14 C9 0.6(3) . . . . ?
C12 N1 N2 N3 -178.5(2) . . . . ?
C13 C12 N1 C15 168.0(2) . . . . ?
C13 C12 N1 N2 -13.7(3) . . . . ?
C14 C4 C31 C26 -112.2(2) . . . . ?
C14 C4 C31 C30 70.4(3) . . . . ?
C14 C9 C10 C11 1.1(3) . . . . ?
C15 C16 C17 C21 178.9(2) . . . . ?
C15 C16 C17 N4 -0.9(4) . . . . ?
C15 C16 N3 N2 -0.2(3) . . . . ?
C15 N1 N2 N3 0.1(3) . . . . ?
C16 C15 N1 C12 178.2(2) . . . . ?
C16 C15 N1 N2 -0.2(3) . . . . ?
C16 C17 C21 C20 178.7(2) . . . . ?
C16 C17 N4 C18 -179.6(2) . . . . ?
C17 C16 N3 N2 -179.1(2) . . . . ?
C18 C19 C20 C21 0.2(4) . . . . ?
C18 C22 N5 C23 -179.0(2) . . . . ?
C19 C18 C22 N5 177.1(2) . . . . ?
C19 C18 C22 O1 -3.8(3) . . . . ?
C19 C18 N4 C17 0.8(3) . . . . ?
C19 C20 C21 C17 1.0(4) . . . . ?
C21 C17 N4 C18 0.6(3) . . . . ?
C22 C18 C19 C20 178.2(2) . . . . ?
C22 C18 N4 C17 -178.7(2) . . . . ?
C24 C23 N5 C22 -79.6(3) . . . . ?
C25 C23 N5 C22 156.7(3) . . . . ?
C26 C5 C48 C43 -115.4(2) . . . . ?
C26 C5 C48 C47 63.8(3) . . . . ?
C26 C27 C28 C29 0.4(3) . . . . ?
C26 C27 C28 N6 -178.46(18) . . . . ?
C27 C26 C31 C4 -178.55(19) . . . . ?
C27 C26 C31 C30 -0.9(3) . . . . ?
C27 C28 C29 C30 -0.8(3) . . . . ?
C27 C28 N6 C32 174.7(2) . . . . ?
C27 C28 N6 N7 -0.2(3) . . . . ?
C28 C29 C30 C31 0.3(3) . . . . ?
C28 N6 N7 N8 175.93(19) . . . . ?
C29 C28 N6 C32 -4.2(3) . . . . ?
C29 C28 N6 N7 -179.1(2) . . . . ?
C29 C30 C31 C4 177.8(2) . . . . ?
C29 C30 C31 C26 0.5(3) . . . . ?
C31 C4 C14 C9 114.4(2) . . . . ?
C31 C4 C14 C13 -67.0(3) . . . . ?
C31 C26 C27 C28 0.5(3) . . . . ?
C32 C33 C34 C38 176.2(2) . . . . ?
C32 C33 C34 N9 -3.4(3) . . . . ?
C32 C33 N8 N7 -0.1(3) . . . . ?
C32 N6 N7 N8 0.2(3) . . . . ?
C33 C32 N6 C28 -175.5(2) . . . . ?
C33 C32 N6 N7 -0.3(2) . . . . ?
C33 C34 C38 C37 -178.8(2) . . . . ?
C33 C34 N9 C35 179.7(2) . . . . ?
C34 C33 N8 N7 179.7(2) . . . . ?
C35 C36 C37 C38 -0.1(4) . . . . ?
C35 C39 N10 C40 179.5(2) . . . . ?
C36 C35 C39 N10 165.9(2) . . . . ?
C36 C35 C39 O2 -13.4(3) . . . . ?
C36 C35 N9 C34 -1.2(3) . . . . ?
C36 C37 C38 C34 -0.7(4) . . . . ?
C38 C34 N9 C35 0.2(3) . . . . ?
C39 C35 C36 C37 -177.4(2) . . . . ?
C39 C35 N9 C34 177.4(2) . . . . ?
C41 C40 N10 C39 -70.8(4) . . . . ?
C42 C40 N10 C39 164.8(3) . . . . ?
C43 C3 C9 C10 72.7(3) . . . . ?
C43 C3 C9 C14 -105.0(2) . . . . ?
C43 C44 C45 C46 0.5(3) . . . . ?
C43 C44 C45 N11 -178.86(19) . . . . ?
C44 C43 C48 C5 -179.65(19) . . . . ?
C44 C43 C48 C47 1.0(3) . . . . ?
C44 C45 C46 C47 -0.1(3) . . . . ?
C44 C45 N11 C49 166.8(2) . . . . ?
C44 C45 N11 N12 -12.4(3) . . . . ?
C45 C46 C47 C48 0.1(3) . . . . ?
C45 N11 N12 N13 179.15(18) . . . . ?
C46 C45 N11 C49 -12.6(3) . . . . ?
C46 C45 N11 N12 168.2(2) . . . . ?
C46 C47 C48 C5 -179.8(2) . . . . ?
C46 C47 C48 C43 -0.5(3) . . . . ?
C48 C5 C26 C27 -72.6(3) . . . . ?
C48 C5 C26 C31 105.1(2) . . . . ?
C48 C43 C44 C45 -1.0(3) . . . . ?
C49 C50 C51 C55 19.1(4) . . . . ?
C49 C50 C51 N14 -159.2(2) . . . . ?
C49 C50 N13 N12 -0.6(3) . . . . ?
C49 N11 N12 N13 -0.2(2) . . . . ?
C50 C49 N11 C45 -179.4(2) . . . . ?
C50 C49 N11 N12 -0.2(2) . . . . ?
C50 C51 C55 C54 -179.5(2) . . . . ?
C50 C51 N14 C52 178.03(19) . . . . ?
C51 C50 N13 N12 -178.95(19) . . . . ?
C52 C53 C54 C55 0.3(4) . . . . ?
C52 C56 N15 C57 -178.4(2) . . . . ?
C53 C52 C56 N15 -178.9(2) . . . . ?
C53 C52 C56 O3 -1.6(4) . . . . ?
C53 C52 N14 C51 1.9(3) . . . . ?
C53 C54 C55 C51 1.2(4) . . . . ?
C55 C51 N14 C52 -0.3(3) . . . . ?
C56 C52 C53 C54 176.4(2) . . . . ?
C56 C52 N14 C51 -176.46(19) . . . . ?
C58 C57 N15 C56 97.9(3) . . . . ?
C59 C57 N15 C56 -137.3(2) . . . . ?
N1 C12 C13 C14 179.4(2) . . . . ?
N1 C15 C16 C17 179.0(2) . . . . ?
N1 C15 C16 N3 0.2(3) . . . . ?
N1 N2 N3 C16 0.1(3) . . . . ?
N3 C16 C17 C21 -2.5(4) . . . . ?
N3 C16 C17 N4 177.7(2) . . . . ?
N4 C17 C21 C20 -1.5(4) . . . . ?
N4 C18 C19 C20 -1.2(4) . . . . ?
N4 C18 C22 N5 -3.4(3) . . . . ?
N4 C18 C22 O1 175.7(2) . . . . ?
N6 C28 C29 C30 178.1(2) . . . . ?
N6 C32 C33 C34 -179.6(2) . . . . ?
N6 C32 C33 N8 0.2(3) . . . . ?
N6 N7 N8 C33 0.0(3) . . . . ?
N8 C33 C34 C38 -3.7(4) . . . . ?
N8 C33 C34 N9 176.8(2) . . . . ?
N9 C34 C38 C37 0.7(4) . . . . ?
N9 C35 C36 C37 1.1(4) . . . . ?
N9 C35 C39 N10 -12.7(3) . . . . ?
N9 C35 C39 O2 168.0(2) . . . . ?
N11 C45 C46 C47 179.3(2) . . . . ?
N11 C49 C50 C51 178.6(2) . . . . ?
N11 C49 C50 N13 0.5(2) . . . . ?
N11 N12 N13 C50 0.5(2) . . . . ?
N13 C50 C51 C55 -163.0(2) . . . . ?
N13 C50 C51 N14 18.7(3) . . . . ?
N14 C51 C55 C54 -1.2(4) . . . . ?
N14 C52 C53 C54 -1.9(4) . . . . ?
N14 C52 C56 N15 -0.5(3) . . . . ?
N14 C52 C56 O3 176.9(2) . . . . ?
O1 C22 N5 C23 1.9(4) . . . . ?
O2 C39 N10 C40 -1.3(4) . . . . ?
O3 C56 N15 C57 4.3(4) . . . . ?
C60 C61 C62 C63 -179.5(2) . . . . ?
C61 C62 C63 C61 -0.2(4) . . . 2_666 ?
C63 C61 C62 C63 0.2(4) 2_666 . . . ?
C64 C65 C66 C67 -1.7(8) . . . . ?
C65 C64 C69 C68 -2.6(6) . . . . ?
C65 C66 C67 C68 -0.4(6) . . . . ?
C65 C66 C67 C71 -179.7(4) . . . . ?
C66 C67 C68 C69 0.7(6) . . . . ?
C67 C68 C69 C64 0.7(6) . . . . ?
C69 C64 C65 C66 3.1(8) . . . . ?
C70 C64 C65 C66 -178.3(5) . . . . ?
C70 C64 C69 C68 178.8(4) . . . . ?
C71 C67 C68 C69 180.0(4) . . . . ?
C64A C65A C66A C67A -0.1(4) . . . . ?
C65A C64A C69A C68A 0.0(9) . . . . ?
C65A C66A C67A C68A 0.2(7) . . . . ?
C65A C66A C67A C71A -180.0(5) . . . . ?
C66A C67A C68A C69A -0.2(8) . . . . ?
C67A C68A C69A C64A 0.1(11) . . . . ?
C69A C64A C65A C66A 0.0(3) . . . . ?
C70A C64A C65A C66A 179.9(3) . . . . ?
C70A C64A C69A C68A -179.9(7) . . . . ?
C71A C67A C68A C69A 180.0(6) . . . . ?
C72 C73 C74 C75 0.8(5) . . . . ?
C73 C72 C77 C76 1.1(5) . . . . ?
C73 C74 C75 C76 0.3(5) . . . . ?
C73 C74 C75 C79 -179.8(3) . . . . ?
C74 C75 C76 C77 -0.7(5) . . . . ?
C75 C76 C77 C72 0.0(5) . . . . ?
C77 C72 C73 C74 -1.5(5) . . . . ?
C78 C72 C73 C74 177.7(3) . . . . ?
C78 C72 C77 C76 -178.1(3) . . . . ?
C79 C75 C76 C77 179.4(3) . . . . ?
C81 C82 C83 C84 -0.1(3) . . . . ?
C82 C81 C86 C85 0.9(6) . . . . ?
C82 C83 C84 C85 0.0(6) . . . . ?
C82 C83 C84 C88 179.7(4) . . . . ?
C83 C84 C85 C86 0.5(8) . . . . ?
C84 C85 C86 C81 -1.0(8) . . . . ?
C86 C81 C82 C83 -0.3(3) . . . . ?
C87 C81 C82 C83 179.8(3) . . . . ?
C87 C81 C86 C85 -179.2(5) . . . . ?
C88 C84 C85 C86 -179.1(5) . . . . ?
C81A C82A C83A C84A 0.3(3) . . . . ?
C82A C81A C86A C85A 0.0(8) . . . . ?
C82A C83A C84A C85A -1.0(7) . . . . ?
C82A C83A C84A C88A -179.6(4) . . . . ?
C83A C84A C85A C86A 1.1(9) . . . . ?
C84A C85A C86A C81A -0.5(10) . . . . ?
C86A C81A C82A C83A 0.1(3) . . . . ?
C87A C81A C82A C83A 180.0(3) . . . . ?
C87A C81A C86A C85A -179.9(6) . . . . ?
C88A C84A C85A C86A 179.7(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.786
_oxdiff_exptl_absorpt_empirical_full_min 0.490
####################################################################### 
# 
# 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_m-xylene
_audit_block_doi                 10.5517/ccdc.csd.cc2mbq3t
_database_code_depnum_ccdc_archive 'CCDC 2423366'
loop_
_audit_author_name
_audit_author_address
'Tianshu Yang'
;FUJIAN NORMAL UNIVERSITY
China
;
_audit_update_record             
;
2025-02-14 deposited with the CCDC.	2025-02-27 downloaded from the CCDC.
;
_audit_creation_date             2025-02-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C59 H57 N15 O3), 4(C8 H10), C H Cl3, 2(H2 O)'
_chemical_formula_sum            'C150.98 H158.98 Cl3 N30 O8'
_chemical_formula_weight         2628.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.7305(5)
_cell_length_b                   15.2894(5)
_cell_length_c                   17.0209(5)
_cell_angle_alpha                72.734(3)
_cell_angle_beta                 80.346(3)
_cell_angle_gamma                79.345(3)
_cell_volume                     3571.5(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    16155
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9040
_cell_measurement_theta_min      2.6920
_shelx_estimated_absorpt_T_max   0.850
_shelx_estimated_absorpt_T_min   0.815
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.127a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47371
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.556
_diffrn_reflns_theta_min         2.738
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -91.00 -65.00   0.50    0.74    --  -46.22 142.00 158.00   52
  2  ω    -78.00 -51.00   0.50    0.74    --  -46.22 129.00 -12.00   54
  3  ω   -102.00 -76.00   0.50    0.74    --  -46.22-142.00 102.00   52
  4  ω     43.00  95.00   0.50    0.74    --   46.22-129.00 -86.00  104
  5  ω     61.00  99.00   0.50    0.74    --   46.22-142.00 102.00   76
  6  ω     65.00 119.00   0.50    0.74    --   46.22 142.00 158.00  108
  7  ω   -144.00-119.00   0.50    2.97    --  -97.00-142.00 102.00   50
  8  ω   -124.00 -84.00   0.50    2.97    --  -97.00-129.00 -86.00   80
  9  ω   -113.00 -41.00   0.50    2.97    --  -97.00 129.00 -12.00  144
 10  ω   -124.00 -42.00   0.50    2.97    --  -97.00 142.00 158.00  164
 11  ω     94.00 119.00   0.50    2.97    --  107.47 142.00 158.00   50
 12  ω     60.00 114.00   0.50    2.97    --  107.47-142.00 102.00  108
 13  ω     86.00 112.00   0.50    2.97    --  107.47-129.00 -86.00   52
 14  ω     78.00 162.00   0.50    2.97    --  107.47 129.00 -12.00  168
 15  ω   -114.00 -23.00   0.50    0.74    --  -46.22 -77.00 -60.00  182
 16  ω    -28.00  28.00   0.50    0.74    --  -46.22  19.00-180.00  112
 17  ω    -29.00  29.00   0.50    0.74    --  -46.22  19.00 -90.00  116
 18  ω    -27.00  19.00   0.50    0.74    --   46.22 -19.00 -60.00   92
 19  ω    -24.00  18.00   0.50    0.74    --   46.22 -19.00  90.00   84
 20  ω    -25.00  23.00   0.50    0.74    --   46.22 -19.00 -30.00   96
 21  ω    -71.00 -32.00   0.50    2.97    --  -97.00  61.00  30.00   78
 22  ω   -162.00 -84.00   0.50    2.97    --  -97.00 -15.00 -30.00  156
 23  ω    -54.00 -29.00   0.50    2.97    --  -97.00  45.00 -60.00   50
 24  ω   -106.00 -27.00   0.50    2.97    --  -97.00 106.00 136.18  158
 25  ω    -51.00 -24.00   0.50    2.97    --  -97.00  45.00 -90.00   54
 26  ω   -158.00-132.00   0.50    2.97    --  -97.00 -61.00 150.00   52
 27  ω   -158.00-130.00   0.50    2.97    --  -97.00 -45.00 -30.00   56
 28  ω   -160.00 -81.00   0.50    2.97    --  -97.00 -15.00  90.00  158
 29  ω   -110.00 -79.00   0.50    2.97    --  -97.00 -61.00 150.00   62
 30  ω   -132.00-105.00   0.50    2.97    --  -97.00 -95.00-150.00   54
 31  ω   -169.00 -80.00   0.50    2.97    --  -97.00 -61.00 -60.00  178
 32  ω    -50.00 -25.00   0.50    2.97    --  -97.00  61.00-150.00   50
 33  ω   -122.00 -96.00   0.50    2.97    --  -97.00 -45.00 -30.00   52
 34  ω   -107.00 -66.00   0.50    2.97    --  -97.00 106.00  12.23   82
 35  ω   -112.00 -28.00   0.50    2.97    --  -97.00 125.00 150.00  168
 36  ω     35.00  66.00   0.50    2.97    --  107.47 -77.00  60.00   62
 37  ω     71.00 110.00   0.50    2.97    --  107.47-125.00 -60.00   78
 38  ω     95.00 174.00   0.50    2.97    --  107.47  45.00 150.00  158
 39  ω     95.00 175.00   0.50    2.97    --  107.47  45.00  30.00  160
 40  ω     58.00 111.00   0.50    2.97    --  107.47-125.00 120.00  106
 41  ω     67.00  93.00   0.50    2.97    --  107.47 -95.00 -60.00   52
 42  ω     41.00  66.00   0.50    2.97    --  107.47 -61.00  60.00   50
 43  ω     36.00 101.00   0.50    2.97    --  107.47 -95.00 -90.00  130
 44  ω     35.00  65.00   0.50    2.97    --  107.47 -61.00  90.00   60
 45  ω     37.00 100.00   0.50    2.97    --  107.47 -77.00 -60.00  126
 46  ω     73.00  98.00   0.50    2.97    --  107.47 -77.00  60.00   50
 47  ω     35.00  61.00   0.50    2.97    --  107.47 -61.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0684942000
_diffrn_orient_matrix_UB_12      0.0597735000
_diffrn_orient_matrix_UB_13      -0.0617668000
_diffrn_orient_matrix_UB_21      0.0370243000
_diffrn_orient_matrix_UB_22      0.0173740000
_diffrn_orient_matrix_UB_23      0.0726804000
_diffrn_orient_matrix_UB_31      0.0736786000
_diffrn_orient_matrix_UB_32      -0.0865611000
_diffrn_orient_matrix_UB_33      0.0041985000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9017
_reflns_number_total             14050
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.127a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0035(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1252
_refine_ls_number_reflns         14050
_refine_ls_number_restraints     1065
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0850
_refine_ls_restrained_S_all      1.028
_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)+(0.1828P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2310
_refine_ls_wR_factor_ref         0.2611
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C83-C82 \\sim C84-C81
 with sigma of 0.02
 Cl3-C85 \\sim Cl2-C85 \\sim Cl1-C85
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1-Cl3 \\sim Cl3-Cl2
 with sigma of 0.02
 C75-C70 \\sim C74-C68
 with sigma of 0.02
 C74-C69 \\sim C74-C73
 with sigma of 0.02
 C75-C69 \\sim C75-C71
 with sigma of 0.02
 Cl1B-Cl2B \\sim Cl1B-Cl3B \\sim Cl2B-Cl3B
 with sigma of 0.02
3. Restrained planarity
 C68, C69, C70, C71, C72, C73, C74, C75
 with sigma of 0.01
 C68A, C69A, C70A, C71A, C72A, C73A, C74A, C75A
 with sigma of 0.01
 C68B, C69B, C70B, C71B, C72B, C73B, C74B, C75B
 with sigma of 0.01
 C60, C61, C62, C63, C64, C65, C66, C67
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C85A \\sim Cl1A \\sim Cl2A \\sim Cl3A \\sim C85 \\sim C85 \\sim Cl1 \\sim Cl1
\\sim Cl2 \\sim Cl2 \\sim Cl3 \\sim Cl3 \\sim C85B \\sim Cl1B \\sim Cl2B:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim
C68A \\sim C69A \\sim C70A \\sim C71A \\sim C72A \\sim C73A \\sim C74A \\sim
C75A \\sim C68B \\sim C69B \\sim C70B \\sim C71B \\sim C72B \\sim C73B \\sim
C74B \\sim C75B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
N5 \\sim N6 \\sim N6 \\sim N7 \\sim N7 \\sim N8 \\sim N8 \\sim N9 \\sim N9
\\sim N10 \\sim N10 \\sim N11 \\sim N11 \\sim N12 \\sim N12 \\sim N13 \\sim N13
\\sim N14 \\sim N14 \\sim N15 \\sim N15 \\sim O1 \\sim O1 \\sim O2 \\sim O2
\\sim O3 \\sim O3 \\sim C23 \\sim C24 \\sim C24 \\sim C25 \\sim C25 \\sim C23A
\\sim C23A \\sim C24A \\sim C25A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C40 \\sim C41 \\sim C42 \\sim C41A \\sim C42A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C85B) \\sim Ueq, Uanis(Cl3B) \\sim Ueq, Uanis(Cl2B) \\sim Ueq,
Uanis(Cl1B) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(Cl3)
\\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Same fragment restrains
{C40, C41A, C42A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C40, C41, C42}
{C68A, C69A, C70A, C71A, C72A, C73A, C74A, C75A} sigma for 1-2: 0.01, 1-3: 0.01
{C68B, C69B, C70B, C71B, C72B, C73B, C74B, C75B} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C68, C69, C70, C71, C72, C73, C74, C75}
{N5, C23A, C24A, C25A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{N5, C23, C24, C25}
{C85A, Cl1A, Cl3A, Cl2A} sigma for 1-2: 0.02, 1-3: 0.02
{C85B, Cl1B, Cl2B} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C85, Cl1, Cl2, Cl3}
6. Others
 1*[Sof(C68)+Sof(C69)+Sof(H69)+Sof(C70)+Sof(C71)+Sof(H71)+Sof(C72)+Sof(H72)+
 Sof(C73)+Sof(H73)+Sof(C74)+Sof(H74A)+Sof(H74B)+Sof(H74C)+Sof(C75)+Sof(H75A)+
 Sof(H75B)+Sof(H75C)]+1*[Sof(C68A)+Sof(C69A)+Sof(H69A)+Sof(C70A)+Sof(C71A)+
 Sof(H71A)+Sof(C72A)+Sof(H72A)+Sof(C73A)+Sof(H73A)+Sof(C74A)+Sof(H74D)+
 Sof(H74E)+Sof(H74F)+Sof(C75A)+Sof(H75D)+Sof(H75E)+Sof(H75F)]+1*[Sof(C68B)+
 Sof(C69B)+Sof(H69B)+Sof(C70B)+Sof(C71B)+Sof(H71B)+Sof(C72B)+Sof(H72B)+
 Sof(C73B)+Sof(H73B)+Sof(C74B)+Sof(H74G)+Sof(H74H)+Sof(H74I)+Sof(C75B)+
 Sof(H75G)+Sof(H75H)+Sof(H75I)]=1 with esd of 0
 1*[Sof(C85)+Sof(H85)+Sof(Cl1)+Sof(Cl2)+Sof(Cl3)]+1*[Sof(C85A)+Sof(H85A)+
 Sof(Cl1A)+Sof(Cl3A)+Sof(Cl2A)]+1*[Sof(C85B)+Sof(H85B)+Sof(Cl1B)+Sof(Cl2B)+
 Sof(Cl3B)]=0.5 with esd of 0
 Sof(C68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72)=
 Sof(C73)=Sof(H73)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C75)=Sof(H75A)=
 Sof(H75B)=Sof(H75C)=FVAR(1)
 Sof(H5B)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(2)
 Sof(H5A)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(2)
 Sof(H40A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42D)=
 Sof(H42E)=Sof(H42F)=1-FVAR(3)
 Sof(H40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=FVAR(3)
 Sof(C85)=Sof(H85)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(4)
 Sof(C68A)=Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(C71A)=Sof(H71A)=Sof(C72A)=
 Sof(H72A)=Sof(C73A)=Sof(H73A)=Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=
 Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=FVAR(5)
 Sof(C68B)=Sof(C69B)=Sof(H69B)=Sof(C70B)=Sof(C71B)=Sof(H71B)=Sof(C72B)=
 Sof(H72B)=Sof(C73B)=Sof(H73B)=Sof(C74B)=Sof(H74G)=Sof(H74H)=Sof(H74I)=
 Sof(C75B)=Sof(H75G)=Sof(H75H)=Sof(H75I)=FVAR(6)
 Sof(C85A)=Sof(H85A)=Sof(Cl1A)=Sof(Cl3A)=Sof(Cl2A)=FVAR(7)
 Sof(C85B)=Sof(H85B)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=FVAR(8)
 Fixed Sof: C60(0.5) C61(0.5) H61(0.5) C62(0.5) C63(0.5) H63(0.5) C64(0.5)
 H64(0.5) C65(0.5) H65(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) C67(0.5)
 H67A(0.5) H67B(0.5) H67C(0.5) C76(0.5) H76(0.5) C78(0.5) H78(0.5) C79(0.5)
 H79(0.5) C80(0.5) H80(0.5) C81(0.5) H81A(0.5) H81B(0.5) H81C(0.5) C82(0.5)
 H82A(0.5) H82B(0.5) H82C(0.5) C83(0.5) C84(0.5)
7.a Free rotating group:
 O4(H4A,H4B)
7.b Ternary CH refined with riding coordinates:
 C40(H40A), C40(H40), C57(H57), C23(H23), C85B(H85B), C85A(H85A), C85(H85),
 C23A(H23A)
7.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C15(H15), C19(H19), C20(H20), C21(H21),
 C27(H27), C28(H28), C30(H30), C32(H32), C36(H36), C37(H37), C38(H38), C44(H44),
  C46(H46), C47(H47), C49(H49), C53(H53), C54(H54), C55(H55), N5(H5A), N5(H5B),
 N10(H10A), N15(H15A), C69(H69), C71(H71), C72(H72), C73(H73), C69A(H69A),
 C71A(H71A), C72A(H72A), C73A(H73A), C69B(H69B), C71B(H71B), C72B(H72B),
 C73B(H73B), C61(H61), C63(H63), C64(H64), C65(H65), C76(H76), C78(H78),
 C79(H79), C80(H80)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C), C74A(H74D,H74E,H74F), C75A(H75D,H75E,H75F), C74B(H74G,H74H,H74I),
 C75B(H75G,H75H,H75I), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C81(H81A,H81B,
 H81C), C82(H82A,H82B,H82C), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F),
 C41A(H41D,H41E,H41F), C42A(H42D,H42E,H42F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.9958(2) 0.5317(2) 0.28130(18) 0.0616(7) Uani 1 1 d . . . . .
H1A H 1.024114 0.482893 0.254653 0.092 Uiso 1 1 calc R U . . .
H1B H 1.035348 0.533826 0.321414 0.092 Uiso 1 1 calc R U . . .
H1C H 0.989367 0.591525 0.239159 0.092 Uiso 1 1 calc R U . . .
C2 C 0.89950(18) 0.5114(2) 0.32617(15) 0.0503(6) Uani 1 1 d . . . . .
C3 C 0.83049(18) 0.5096(2) 0.26439(15) 0.0499(6) Uani 1 1 d . . . . .
C4 C 0.90547(18) 0.4131(2) 0.39386(16) 0.0505(6) Uani 1 1 d . . . . .
C5 C 0.85005(18) 0.58573(19) 0.37366(15) 0.0485(6) Uani 1 1 d . . . . .
C6 C 0.8665(2) 0.5373(2) 0.17163(16) 0.0582(7) Uani 1 1 d . . . . .
H6A H 0.880235 0.601072 0.155252 0.087 Uiso 1 1 calc R U . . .
H6B H 0.819031 0.533024 0.139485 0.087 Uiso 1 1 calc R U . . .
H6C H 0.923338 0.495620 0.160976 0.087 Uiso 1 1 calc R U . . .
C7 C 1.0027(2) 0.3568(2) 0.4020(2) 0.0619(7) Uani 1 1 d . . . . .
H7A H 1.029723 0.345352 0.348684 0.093 Uiso 1 1 calc R U . . .
H7B H 0.997959 0.297546 0.444174 0.093 Uiso 1 1 calc R U . . .
H7C H 1.042507 0.391418 0.418427 0.093 Uiso 1 1 calc R U . . .
C8 C 0.9010(2) 0.6682(2) 0.36248(17) 0.0592(7) Uani 1 1 d . . . . .
H8A H 0.960320 0.646188 0.385597 0.089 Uiso 1 1 calc R U . . .
H8B H 0.862486 0.711446 0.391368 0.089 Uiso 1 1 calc R U . . .
H8C H 0.912661 0.699827 0.303335 0.089 Uiso 1 1 calc R U . . .
C9 C 0.80803(18) 0.4119(2) 0.29320(16) 0.0499(6) Uani 1 1 d . . . . .
C10 C 0.75400(19) 0.3723(2) 0.25634(17) 0.0544(6) Uani 1 1 d . . . . .
H10 H 0.730989 0.406400 0.205431 0.065 Uiso 1 1 calc R U . . .
C11 C 0.7344(2) 0.2837(2) 0.29427(19) 0.0597(7) Uani 1 1 d . . . . .
H11 H 0.697689 0.256570 0.269627 0.072 Uiso 1 1 calc R U . . .
C12 C 0.7687(2) 0.2336(2) 0.36917(19) 0.0575(7) Uani 1 1 d . . . . .
C13 C 0.82496(19) 0.2707(2) 0.40500(18) 0.0552(6) Uani 1 1 d . . . . .
H13 H 0.849638 0.235835 0.454954 0.066 Uiso 1 1 calc R U . . .
C14 C 0.84431(18) 0.3603(2) 0.36601(16) 0.0506(6) Uani 1 1 d . . . . .
C15 C 0.6759(2) 0.1043(2) 0.3953(2) 0.0608(7) Uani 1 1 d . . . . .
H15 H 0.632295 0.130661 0.356292 0.073 Uiso 1 1 calc R U . . .
C16 C 0.6829(2) 0.0183(2) 0.4492(2) 0.0656(8) Uani 1 1 d . . . . .
C17 C 0.6255(2) -0.0554(2) 0.4625(2) 0.0608(7) Uani 1 1 d . . . . .
C18 C 0.5028(2) -0.0988(2) 0.42475(19) 0.0602(7) Uani 1 1 d . . . . .
C19 C 0.5122(2) -0.1836(2) 0.4844(2) 0.0657(8) Uani 1 1 d . . . . .
H19 H 0.470577 -0.226620 0.491219 0.079 Uiso 1 1 calc R U . . .
C20 C 0.5827(3) -0.2040(2) 0.5332(2) 0.0719(9) Uani 1 1 d . . . . .
H20 H 0.591502 -0.261968 0.573744 0.086 Uiso 1 1 calc R U . . .
C21 C 0.6407(3) -0.1389(2) 0.5223(2) 0.0684(8) Uani 1 1 d . . . . .
H21 H 0.690154 -0.151251 0.555163 0.082 Uiso 1 1 calc R U . . .
C22 C 0.4286(3) -0.0776(2) 0.3690(2) 0.0684(8) Uani 1 1 d . . . . .
C26 C 0.86517(17) 0.43656(18) 0.47431(15) 0.0464(6) Uani 1 1 d . . . . .
C27 C 0.85601(19) 0.37562(19) 0.55398(16) 0.0501(6) Uani 1 1 d . . . . .
H27 H 0.875553 0.311136 0.561863 0.060 Uiso 1 1 calc R U . . .
C28 C 0.81868(19) 0.40916(19) 0.62086(16) 0.0497(6) Uani 1 1 d . . . . .
H28 H 0.812983 0.367918 0.675000 0.060 Uiso 1 1 calc R U . . .
C29 C 0.78925(18) 0.50366(18) 0.60910(15) 0.0462(6) Uani 1 1 d . . . . .
C30 C 0.79887(18) 0.56549(18) 0.53044(15) 0.0461(6) Uani 1 1 d . . . . .
H30 H 0.779753 0.630041 0.522517 0.055 Uiso 1 1 calc R U . . .
C31 C 0.83714(17) 0.53016(18) 0.46402(15) 0.0457(6) Uani 1 1 d . . . . .
C32 C 0.73056(18) 0.49184(19) 0.75865(15) 0.0480(6) Uani 1 1 d . . . . .
H32 H 0.744359 0.427131 0.782999 0.058 Uiso 1 1 calc R U . . .
C33 C 0.6881(2) 0.55799(19) 0.79758(16) 0.0519(6) Uani 1 1 d . . . . .
C34 C 0.65422(19) 0.54531(19) 0.88599(15) 0.0495(6) Uani 1 1 d . . . . .
C35 C 0.62646(18) 0.4429(2) 1.01391(15) 0.0512(6) Uani 1 1 d . . . . .
C36 C 0.5943(2) 0.5138(2) 1.05103(16) 0.0574(7) Uani 1 1 d . . . . .
H36 H 0.573670 0.500494 1.108738 0.069 Uiso 1 1 calc R U . . .
C37 C 0.5927(2) 0.6046(2) 1.00240(18) 0.0603(7) Uani 1 1 d . . . . .
H37 H 0.571966 0.654622 1.026361 0.072 Uiso 1 1 calc R U . . .
C38 C 0.6218(2) 0.6208(2) 0.91830(18) 0.0580(7) Uani 1 1 d . . . . .
H38 H 0.619676 0.682273 0.883221 0.070 Uiso 1 1 calc R U . . .
C39 C 0.6273(2) 0.3445(2) 1.06426(16) 0.0575(7) Uani 1 1 d . . . . .
C40 C 0.6459(3) 0.1812(2) 1.0632(2) 0.0778(10) Uani 1 1 d D U . . .
H40A H 0.661664 0.170461 1.120574 0.093 Uiso 0.195(7) 1 calc R U P A 2
H40 H 0.598699 0.173342 1.113506 0.093 Uiso 0.805(7) 1 calc R U P A 1
C41 C 0.7389(5) 0.1439(4) 1.0920(5) 0.115(2) Uani 0.805(7) 1 d D U P A 1
H41A H 0.787418 0.157160 1.044873 0.173 Uiso 0.805(7) 1 calc R U P A 1
H41B H 0.743014 0.076872 1.116458 0.173 Uiso 0.805(7) 1 calc R U P A 1
H41C H 0.747577 0.173221 1.133719 0.173 Uiso 0.805(7) 1 calc R U P A 1
C42 C 0.6189(4) 0.1345(3) 1.0074(3) 0.0894(16) Uani 0.805(7) 1 d D U P A 1
H42A H 0.556248 0.162169 0.992962 0.134 Uiso 0.805(7) 1 calc R U P A 1
H42B H 0.619473 0.068476 1.035518 0.134 Uiso 0.805(7) 1 calc R U P A 1
H42C H 0.663144 0.142128 0.956774 0.134 Uiso 0.805(7) 1 calc R U P A 1
C43 C 0.74543(18) 0.57603(18) 0.28245(15) 0.0466(6) Uani 1 1 d . . . . .
C44 C 0.66222(18) 0.59684(19) 0.24747(16) 0.0498(6) Uani 1 1 d . . . . .
H44 H 0.654946 0.569869 0.205711 0.060 Uiso 1 1 calc R U . . .
C45 C 0.59044(18) 0.65736(18) 0.27455(15) 0.0481(6) Uani 1 1 d . . . . .
C46 C 0.6005(2) 0.6986(2) 0.33438(17) 0.0528(6) Uani 1 1 d . . . . .
H46 H 0.550588 0.740099 0.352260 0.063 Uiso 1 1 calc R U . . .
C47 C 0.6835(2) 0.67908(19) 0.36776(16) 0.0525(6) Uani 1 1 d . . . . .
H47 H 0.690960 0.707553 0.408417 0.063 Uiso 1 1 calc R U . . .
C48 C 0.75625(18) 0.61772(18) 0.34197(14) 0.0463(6) Uani 1 1 d . . . . .
C49 C 0.42239(19) 0.72420(19) 0.26680(16) 0.0507(6) Uani 1 1 d . . . . .
H49 H 0.409058 0.749989 0.312539 0.061 Uiso 1 1 calc R U . . .
C50 C 0.36252(18) 0.72529(18) 0.21198(16) 0.0484(6) Uani 1 1 d . . . . .
C51 C 0.26463(19) 0.76482(18) 0.20993(17) 0.0506(6) Uani 1 1 d . . . . .
C52 C 0.12634(19) 0.76570(19) 0.16290(17) 0.0524(6) Uani 1 1 d . . . . .
C53 C 0.0801(2) 0.8286(2) 0.2046(2) 0.0694(8) Uani 1 1 d . . . . .
H53 H 0.015665 0.850184 0.201712 0.083 Uiso 1 1 calc R U . . .
C54 C 0.1293(2) 0.8600(2) 0.2509(3) 0.0762(9) Uani 1 1 d . . . . .
H54 H 0.098949 0.903610 0.280045 0.091 Uiso 1 1 calc R U . . .
C55 C 0.2223(2) 0.8274(2) 0.2542(2) 0.0644(8) Uani 1 1 d . . . . .
H55 H 0.257025 0.847374 0.286210 0.077 Uiso 1 1 calc R U . . .
C56 C 0.07410(19) 0.72771(19) 0.11408(17) 0.0523(6) Uani 1 1 d . . . . .
C57 C 0.0819(2) 0.6228(2) 0.02781(18) 0.0601(7) Uani 1 1 d . . . . .
H57 H 0.013326 0.628514 0.045400 0.072 Uiso 1 1 calc R U . . .
C58 C 0.1193(2) 0.5206(2) 0.0433(2) 0.0652(8) Uani 1 1 d . . . . .
H58A H 0.085355 0.492400 0.014619 0.098 Uiso 1 1 calc R U . . .
H58B H 0.110999 0.490212 0.102967 0.098 Uiso 1 1 calc R U . . .
H58C H 0.185597 0.513056 0.022431 0.098 Uiso 1 1 calc R U . . .
C59 C 0.0971(3) 0.6748(3) -0.0625(2) 0.0830(10) Uani 1 1 d . . . . .
H59A H 0.163861 0.668485 -0.081918 0.125 Uiso 1 1 calc R U . . .
H59B H 0.072411 0.740352 -0.069566 0.125 Uiso 1 1 calc R U . . .
H59C H 0.064913 0.649291 -0.094739 0.125 Uiso 1 1 calc R U . . .
N1 N 0.74385(18) 0.14441(18) 0.40886(17) 0.0623(6) Uani 1 1 d . . . . .
N2 N 0.7901(2) 0.0858(2) 0.4705(2) 0.0817(8) Uani 1 1 d . . . . .
N3 N 0.7533(2) 0.0094(2) 0.4953(2) 0.0828(9) Uani 1 1 d . . . . .
N4 N 0.55816(18) -0.03424(16) 0.41347(16) 0.0601(6) Uani 1 1 d . . . . .
N5 N 0.4190(3) 0.0068(2) 0.3173(2) 0.0891(10) Uani 1 1 d D U . . .
H5A H 0.458903 0.044955 0.312415 0.107 Uiso 0.420(9) 1 calc R U P B 1
H5B H 0.451736 0.047431 0.321670 0.107 Uiso 0.580(9) 1 calc R U P B 2
C23 C 0.3382(9) 0.0356(9) 0.2673(7) 0.112(3) Uani 0.420(9) 1 d D U P B 1
H23 H 0.275603 0.023462 0.297698 0.134 Uiso 0.420(9) 1 calc R U P B 1
C24 C 0.3668(10) 0.0057(8) 0.1894(6) 0.116(4) Uani 0.420(9) 1 d D U P B 1
H24A H 0.431675 -0.024401 0.188380 0.174 Uiso 0.420(9) 1 calc R U P B 1
H24B H 0.360881 0.059862 0.141250 0.174 Uiso 0.420(9) 1 calc R U P B 1
H24C H 0.326703 -0.038022 0.187699 0.174 Uiso 0.420(9) 1 calc R U P B 1
C25 C 0.3490(16) 0.1455(8) 0.2120(11) 0.149(5) Uani 0.420(9) 1 d D U P B 1
H25A H 0.305267 0.188289 0.238118 0.224 Uiso 0.420(9) 1 calc R U P B 1
H25B H 0.335253 0.155301 0.155426 0.224 Uiso 0.420(9) 1 calc R U P B 1
H25C H 0.412712 0.156826 0.210456 0.224 Uiso 0.420(9) 1 calc R U P B 1
N6 N 0.74858(16) 0.53864(15) 0.67805(12) 0.0497(5) Uani 1 1 d . U . . .
N7 N 0.7178(2) 0.62921(18) 0.66756(15) 0.0716(7) Uani 1 1 d . U . . .
N8 N 0.6816(2) 0.64134(18) 0.73980(16) 0.0747(8) Uani 1 1 d . U . . .
N9 N 0.65712(15) 0.45777(16) 0.93249(12) 0.0492(5) Uani 1 1 d . . . . .
N10 N 0.64112(19) 0.28094(18) 1.02256(15) 0.0637(6) Uani 1 1 d . . . . .
H10A H 0.647738 0.299608 0.968056 0.076 Uiso 1 1 calc R U . . .
N11 N 0.50372(15) 0.67854(15) 0.24108(13) 0.0488(5) Uani 1 1 d . U . . .
N12 N 0.49662(16) 0.65274(17) 0.17303(14) 0.0545(5) Uani 1 1 d . U . . .
N13 N 0.41104(16) 0.68082(17) 0.15584(14) 0.0545(5) Uani 1 1 d . U . . .
N14 N 0.21746(15) 0.73412(15) 0.16392(13) 0.0483(5) Uani 1 1 d . . . . .
N15 N 0.12321(16) 0.66494(17) 0.07798(14) 0.0544(6) Uani 1 1 d . . . . .
H15A H 0.182556 0.648017 0.084335 0.065 Uiso 1 1 calc R U . . .
O1 O 0.38124(18) -0.13738(16) 0.37178(16) 0.0769(6) Uani 1 1 d . . . . .
O2 O 0.61542(17) 0.32557(18) 1.14110(12) 0.0732(6) Uani 1 1 d . . . . .
O3 O -0.00973(14) 0.75347(16) 0.11146(16) 0.0698(6) Uani 1 1 d . . . . .
O4 O 0.5062(2) 0.21185(18) 0.26791(15) 0.0821(7) Uani 1 1 d G . . . .
H4A H 0.537741 0.246888 0.226540 0.123 Uiso 1 1 d G U . . .
H4B H 0.450402 0.242671 0.270183 0.123 Uiso 1 1 d G U . . .
C68 C 1.0032(8) 0.0807(8) 0.5687(7) 0.123(2) Uani 0.462(3) 1 d D U P C -1
C69 C 0.9658(9) -0.0243(8) 0.6153(7) 0.114(2) Uani 0.462(3) 1 d D U P C -1
H69 H 0.918199 -0.042761 0.595002 0.137 Uiso 0.462(3) 1 calc R U P C -1
C70 C 1.0094(8) -0.0847(9) 0.6874(7) 0.123(2) Uani 0.462(3) 1 d D U P C -1
C71 C 1.0778(9) -0.0419(8) 0.7053(8) 0.121(2) Uani 0.462(3) 1 d D U P C -1
H71 H 1.108916 -0.077693 0.751607 0.145 Uiso 0.462(3) 1 calc R U P C -1
C72 C 1.1067(8) 0.0421(9) 0.6674(7) 0.117(2) Uani 0.462(3) 1 d D U P C -1
H72 H 1.154077 0.061493 0.687158 0.140 Uiso 0.462(3) 1 calc R U P C -1
C73 C 1.0614(7) 0.1025(9) 0.5939(7) 0.120(2) Uani 0.462(3) 1 d D U P C -1
H73 H 1.081025 0.160980 0.566790 0.144 Uiso 0.462(3) 1 calc R U P C -1
C74 C 0.9570(11) 0.1059(10) 0.5193(9) 0.228(8) Uani 0.462(3) 1 d D U P C -1
H74A H 0.992374 0.099661 0.466596 0.342 Uiso 0.462(3) 1 calc R U P C -1
H74B H 0.931990 0.171174 0.514000 0.342 Uiso 0.462(3) 1 calc R U P C -1
H74C H 0.905544 0.069344 0.533352 0.342 Uiso 0.462(3) 1 calc R U P C -1
C75 C 0.9864(9) -0.1669(8) 0.7280(7) 0.125(4) Uani 0.462(3) 1 d D U P C -1
H75A H 0.953816 -0.165025 0.782752 0.187 Uiso 0.462(3) 1 calc R U P C -1
H75B H 1.042805 -0.212643 0.734600 0.187 Uiso 0.462(3) 1 calc R U P C -1
H75C H 0.945624 -0.184267 0.696953 0.187 Uiso 0.462(3) 1 calc R U P C -1
C68A C 1.0851(9) -0.0780(10) 0.7366(8) 0.126(3) Uani 0.371(3) 1 d D U P D -2
C69A C 1.0019(9) -0.1449(10) 0.7417(9) 0.130(3) Uani 0.371(3) 1 d D U P D -2
H69A H 0.997403 -0.201679 0.783457 0.156 Uiso 0.371(3) 1 calc R U P D -2
C70A C 0.9379(8) -0.1101(9) 0.6783(8) 0.118(3) Uani 0.371(3) 1 d D U P D -2
C71A C 0.9579(11) -0.0250(9) 0.6234(8) 0.116(2) Uani 0.371(3) 1 d D U P D -2
H71A H 0.918139 0.000401 0.581196 0.139 Uiso 0.371(3) 1 calc R U P D -2
C72A C 1.0253(10) 0.0273(10) 0.6206(9) 0.116(2) Uani 0.371(3) 1 d D U P D -2
H72A H 1.030529 0.084239 0.579179 0.140 Uiso 0.371(3) 1 calc R U P D -2
C73A C 1.0891(10) -0.0086(10) 0.6847(8) 0.122(2) Uani 0.371(3) 1 d D U P D -2
H73A H 1.136123 0.026817 0.683586 0.146 Uiso 0.371(3) 1 calc R U P D -2
C74A C 1.1198(11) -0.1212(13) 0.7898(10) 0.178(6) Uani 0.371(3) 1 d D U P D -2
H74D H 1.087211 -0.106269 0.840376 0.267 Uiso 0.371(3) 1 calc R U P D -2
H74E H 1.184365 -0.109422 0.782102 0.267 Uiso 0.371(3) 1 calc R U P D -2
H74F H 1.119055 -0.186516 0.794696 0.267 Uiso 0.371(3) 1 calc R U P D -2
C75A C 0.8702(10) -0.1548(11) 0.6750(10) 0.155(6) Uani 0.371(3) 1 d D U P D -2
H75D H 0.887234 -0.221270 0.699891 0.232 Uiso 0.371(3) 1 calc R U P D -2
H75E H 0.860707 -0.144060 0.617037 0.232 Uiso 0.371(3) 1 calc R U P D -2
H75F H 0.812555 -0.132232 0.705542 0.232 Uiso 0.371(3) 1 calc R U P D -2
C68B C 1.1419(11) 0.0204(13) 0.7164(13) 0.128(3) Uani 0.166(3) 1 d D U P E -3
C69B C 1.0861(13) 0.0669(14) 0.6293(12) 0.123(3) Uani 0.166(3) 1 d D U P E -3
H69B H 1.099474 0.123299 0.590268 0.148 Uiso 0.166(3) 1 calc R U P E -3
C70B C 1.0168(14) 0.0157(15) 0.6181(14) 0.121(2) Uani 0.166(3) 1 d D U P E -3
C71B C 1.0089(15) -0.0654(15) 0.6836(15) 0.121(2) Uani 0.166(3) 1 d D U P E -3
H71B H 0.964561 -0.101115 0.679169 0.146 Uiso 0.166(3) 1 calc R U P E -3
C72B C 1.0545(17) -0.1015(16) 0.7528(15) 0.125(3) Uani 0.166(3) 1 d D U P E -3
H72B H 1.041944 -0.157969 0.792280 0.150 Uiso 0.166(3) 1 calc R U P E -3
C73B C 1.1241(15) -0.0485(15) 0.7632(13) 0.128(3) Uani 0.166(3) 1 d D U P E -3
H73B H 1.155955 -0.072202 0.810892 0.153 Uiso 0.166(3) 1 calc R U P E -3
C74B C 1.1867(11) 0.0740(13) 0.7054(13) 0.069(4) Uani 0.166(3) 1 d D U P E -3
H74G H 1.208772 0.094165 0.646122 0.103 Uiso 0.166(3) 1 calc R U P E -3
H74H H 1.240148 0.048616 0.736761 0.103 Uiso 0.166(3) 1 calc R U P E -3
H74I H 1.151168 0.126919 0.723414 0.103 Uiso 0.166(3) 1 calc R U P E -3
C75B C 0.969(2) 0.045(2) 0.5536(17) 0.146(6) Uani 0.166(3) 1 d D U P E -3
H75G H 0.925044 0.099771 0.557939 0.219 Uiso 0.166(3) 1 calc R U P E -3
H75H H 0.935255 -0.004430 0.552641 0.219 Uiso 0.166(3) 1 calc R U P E -3
H75I H 1.012204 0.059600 0.502535 0.219 Uiso 0.166(3) 1 calc R U P E -3
C85B C 0.998(4) 0.023(11) 1.053(4) 0.129(6) Uani 0.055(2) 1 d D U P F -3
H85B H 0.972224 0.088243 1.023464 0.155 Uiso 0.055(2) 1 calc R U P F -3
Cl1B Cl 1.1046(17) 0.0506(19) 1.0549(18) 0.138(6) Uani 0.055(2) 1 d D U P F -3
Cl2B Cl 0.924(2) 0.023(2) 1.1421(16) 0.174(8) Uani 0.055(2) 1 d D U P F -3
Cl3B Cl 0.978(2) -0.0177(17) 0.9860(15) 0.116(9) Uani 0.055(2) 1 d D U P F -3
C85A C 1.1882(14) 0.1782(9) 0.9870(10) 0.133(6) Uani 0.254(2) 1 d D U P G -2
H85A H 1.127936 0.194992 0.962678 0.159 Uiso 0.254(2) 1 calc R U P G -2
Cl1A Cl 1.1921(6) 0.2662(4) 1.0275(6) 0.142(3) Uani 0.254(2) 1 d D U P G -2
Cl3A Cl 1.2721(9) 0.1740(8) 0.9039(8) 0.190(7) Uani 0.254(2) 1 d D U P G -2
Cl2A Cl 1.1796(5) 0.0738(4) 1.0588(4) 0.134(2) Uani 0.254(2) 1 d D U P G -2
C60 C 0.4584(5) 0.5387(5) 0.5070(5) 0.0745(18) Uani 0.5 1 d . U P H -1
C61 C 0.4467(9) 0.5172(8) 0.4382(10) 0.070(3) Uani 0.5 1 d . U P H -1
H61 H 0.392269 0.544844 0.411933 0.084 Uiso 0.5 1 calc R U P H -1
C62 C 0.5137(4) 0.4541(4) 0.4039(4) 0.0679(15) Uani 0.5 1 d . U P H -1
C63 C 0.5926(8) 0.4145(8) 0.4439(9) 0.063(2) Uani 0.5 1 d . U P H -1
H63 H 0.638258 0.371958 0.422621 0.076 Uiso 0.5 1 calc R U P H -1
C64 C 0.6055(5) 0.4364(5) 0.5143(4) 0.0709(17) Uani 0.5 1 d . U P H -1
H64 H 0.659641 0.409149 0.540955 0.085 Uiso 0.5 1 calc R U P H -1
C65 C 0.5368(10) 0.5003(9) 0.5468(10) 0.075(3) Uani 0.5 1 d . U P H -1
H65 H 0.544891 0.516015 0.594874 0.090 Uiso 0.5 1 calc R U P H -1
C66 C 0.3836(10) 0.6062(9) 0.5388(12) 0.103(5) Uani 0.5 1 d . U P H -1
H66A H 0.361741 0.656352 0.491913 0.154 Uiso 0.5 1 calc R U P H -1
H66B H 0.409180 0.632079 0.575227 0.154 Uiso 0.5 1 calc R U P H -1
H66C H 0.331515 0.574071 0.569919 0.154 Uiso 0.5 1 calc R U P H -1
C67 C 0.4991(5) 0.4335(6) 0.3291(5) 0.086(2) Uani 0.5 1 d . U P H -1
H67A H 0.437345 0.414847 0.336457 0.129 Uiso 0.5 1 calc R U P H -1
H67B H 0.546758 0.382971 0.318537 0.129 Uiso 0.5 1 calc R U P H -1
H67C H 0.503357 0.488636 0.281936 0.129 Uiso 0.5 1 calc R U P H -1
C76 C 1.2398(6) 0.1712(8) 0.8684(6) 0.067(2) Uani 0.5 1 d . . P I -1
H76 H 1.175702 0.189829 0.861837 0.080 Uiso 0.5 1 calc R U P I -1
C78 C 1.3676(5) 0.1663(4) 0.9420(4) 0.0650(16) Uani 0.5 1 d . . P I -1
H78 H 1.392270 0.177867 0.985456 0.078 Uiso 0.5 1 calc R U P I -1
C79 C 1.4240(4) 0.1234(4) 0.8897(4) 0.0591(14) Uani 0.5 1 d . . P I -1
H79 H 1.488440 0.108020 0.895576 0.071 Uiso 0.5 1 calc R U P I -1
C80 C 1.3915(4) 0.1009(4) 0.8280(4) 0.0617(15) Uani 0.5 1 d . . P I -1
H80 H 1.432573 0.069639 0.792507 0.074 Uiso 0.5 1 calc R U P I -1
C81 C 1.2579(5) 0.1021(5) 0.7515(4) 0.0706(17) Uani 0.5 1 d D . P I -1
H81A H 1.190669 0.101948 0.765692 0.106 Uiso 0.5 1 calc R U P I -1
H81B H 1.287984 0.040858 0.746657 0.106 Uiso 0.5 1 calc R U P I -1
H81C H 1.270220 0.148545 0.698628 0.106 Uiso 0.5 1 calc R U P I -1
C82 C 1.2125(11) 0.2410(11) 0.9899(8) 0.132(6) Uani 0.5 1 d D . P I -1
H82A H 1.148741 0.235365 0.984779 0.198 Uiso 0.5 1 calc R U P I -1
H82B H 1.220077 0.306599 0.973721 0.198 Uiso 0.5 1 calc R U P I -1
H82C H 1.225011 0.212822 1.047491 0.198 Uiso 0.5 1 calc R U P I -1
C83 C 1.2803(9) 0.1920(12) 0.9338(7) 0.077(3) Uani 0.5 1 d D . P I -1
C84 C 1.2964(4) 0.1253(4) 0.8187(4) 0.0551(14) Uani 0.5 1 d D . P I -1
C85 C 1.0762(9) 0.0376(19) 1.0162(14) 0.116(5) Uani 0.191(2) 1 d D U P J -1
H85 H 1.079612 0.100253 0.976319 0.139 Uiso 0.191(2) 1 calc R U P J -1
Cl1 Cl 1.1867(4) -0.0010(4) 1.0418(5) 0.108(2) Uani 0.191(2) 1 d D U P J -1
Cl2 Cl 0.9989(7) 0.0577(5) 1.0989(5) 0.162(4) Uani 0.191(2) 1 d D U P J -1
Cl3 Cl 1.0421(7) -0.0253(6) 0.9615(6) 0.136(3) Uani 0.191(2) 1 d D U P J -1
C23A C 0.3552(7) 0.0355(7) 0.2523(6) 0.111(3) Uani 0.580(9) 1 d D U P B 2
H23A H 0.324695 -0.014910 0.246105 0.133 Uiso 0.580(9) 1 calc R U P B 2
C24A C 0.3948(8) 0.0963(9) 0.1740(6) 0.144(4) Uani 0.580(9) 1 d D U P B 2
H24D H 0.413837 0.149111 0.185316 0.216 Uiso 0.580(9) 1 calc R U P B 2
H24E H 0.347868 0.118767 0.135348 0.216 Uiso 0.580(9) 1 calc R U P B 2
H24F H 0.449074 0.061412 0.149488 0.216 Uiso 0.580(9) 1 calc R U P B 2
C25A C 0.2818(7) 0.1272(7) 0.2725(7) 0.120(3) Uani 0.580(9) 1 d D U P B 2
H25D H 0.250458 0.109150 0.329198 0.180 Uiso 0.580(9) 1 calc R U P B 2
H25E H 0.235391 0.148032 0.233352 0.180 Uiso 0.580(9) 1 calc R U P B 2
H25F H 0.317131 0.177645 0.266724 0.180 Uiso 0.580(9) 1 calc R U P B 2
C41A C 0.7216(12) 0.1263(12) 1.0199(13) 0.097(5) Uani 0.195(7) 1 d D U P A 2
H41D H 0.709407 0.137123 0.962657 0.145 Uiso 0.195(7) 1 calc R U P A 2
H41E H 0.723465 0.060353 1.048808 0.145 Uiso 0.195(7) 1 calc R U P A 2
H41F H 0.781496 0.145585 1.019770 0.145 Uiso 0.195(7) 1 calc R U P A 2
C42A C 0.5522(9) 0.1543(15) 1.0712(14) 0.100(6) Uani 0.195(7) 1 d D U P A 2
H42D H 0.507938 0.187707 1.105808 0.149 Uiso 0.195(7) 1 calc R U P A 2
H42E H 0.555006 0.087506 1.096874 0.149 Uiso 0.195(7) 1 calc R U P A 2
H42F H 0.531853 0.169820 1.016122 0.149 Uiso 0.195(7) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.533(4) . ?
C2 C3 1.589(3) . ?
C2 C4 1.598(4) . ?
C2 C5 1.586(4) . ?
C3 C6 1.536(4) . ?
C3 C9 1.509(4) . ?
C3 C43 1.510(4) . ?
C4 C7 1.533(4) . ?
C4 C14 1.526(4) . ?
C4 C26 1.516(4) . ?
C5 C8 1.533(4) . ?
C5 C31 1.520(3) . ?
C5 C48 1.511(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.402(4) . ?
C9 C14 1.389(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.378(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.400(4) . ?
C12 C13 1.389(4) . ?
C12 N1 1.416(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.392(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.359(5) . ?
C15 N1 1.349(4) . ?
C16 C17 1.474(4) . ?
C16 N3 1.366(5) . ?
C17 C21 1.385(5) . ?
C17 N4 1.336(4) . ?
C18 C19 1.389(5) . ?
C18 C22 1.495(5) . ?
C18 N4 1.345(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.372(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.381(5) . ?
C21 H21 0.9500 . ?
C22 N5 1.327(5) . ?
C22 O1 1.234(4) . ?
C26 C27 1.400(4) . ?
C26 C31 1.381(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.376(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.393(4) . ?
C29 C30 1.393(3) . ?
C29 N6 1.428(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.387(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.370(4) . ?
C32 N6 1.353(3) . ?
C33 C34 1.470(4) . ?
C33 N8 1.357(4) . ?
C34 C38 1.396(4) . ?
C34 N9 1.335(4) . ?
C35 C36 1.384(4) . ?
C35 C39 1.493(4) . ?
C35 N9 1.348(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.388(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.385(4) . ?
C38 H38 0.9500 . ?
C39 N10 1.333(4) . ?
C39 O2 1.242(3) . ?
C40 H40A 1.0000 . ?
C40 H40 1.0000 . ?
C40 C41 1.488(7) . ?
C40 C42 1.486(6) . ?
C40 N10 1.469(4) . ?
C40 C41A 1.496(11) . ?
C40 C42A 1.486(11) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.395(4) . ?
C43 C48 1.390(4) . ?
C44 H44 0.9500 . ?
C44 C45 1.384(4) . ?
C45 C46 1.387(4) . ?
C45 N11 1.429(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.379(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.392(4) . ?
C49 H49 0.9500 . ?
C49 C50 1.382(4) . ?
C49 N11 1.346(4) . ?
C50 C51 1.459(4) . ?
C50 N13 1.365(4) . ?
C51 C55 1.386(4) . ?
C51 N14 1.356(3) . ?
C52 C53 1.377(4) . ?
C52 C56 1.512(4) . ?
C52 N14 1.341(4) . ?
C53 H53 0.9500 . ?
C53 C54 1.385(5) . ?
C54 H54 0.9500 . ?
C54 C55 1.373(5) . ?
C55 H55 0.9500 . ?
C56 N15 1.329(4) . ?
C56 O3 1.229(3) . ?
C57 H57 1.0000 . ?
C57 C58 1.517(5) . ?
C57 C59 1.507(5) . ?
C57 N15 1.470(4) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
N1 N2 1.351(4) . ?
N2 N3 1.304(4) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C23 1.502(9) . ?
N5 C23A 1.486(7) . ?
C23 H23 1.0000 . ?
C23 C24 1.498(14) . ?
C23 C25 1.686(12) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
N6 N7 1.343(3) . ?
N7 N8 1.307(4) . ?
N10 H10A 0.8800 . ?
N11 N12 1.355(3) . ?
N12 N13 1.307(3) . ?
N15 H15A 0.8800 . ?
O4 H4A 0.8698 . ?
O4 H4B 0.8701 . ?
C68 C69 1.714(17) . ?
C68 C73 1.158(14) . ?
C68 C74 1.107(13) . ?
C69 H69 0.9500 . ?
C69 C70 1.464(18) . ?
C70 C71 1.415(16) . ?
C70 C75 1.318(14) . ?
C71 H71 0.9500 . ?
C71 C72 1.366(16) . ?
C72 H72 0.9500 . ?
C72 C73 1.493(13) . ?
C73 H73 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C68A C69A 1.713(17) . ?
C68A C73A 1.166(14) . ?
C68A C74A 1.092(14) . ?
C69A H69A 0.9500 . ?
C69A C70A 1.467(18) . ?
C70A C71A 1.407(16) . ?
C70A C75A 1.327(15) . ?
C71A H71A 0.9500 . ?
C71A C72A 1.372(17) . ?
C72A H72A 0.9500 . ?
C72A C73A 1.474(14) . ?
C73A H73A 0.9500 . ?
C74A H74D 0.9800 . ?
C74A H74E 0.9800 . ?
C74A H74F 0.9800 . ?
C75A H75D 0.9800 . ?
C75A H75E 0.9800 . ?
C75A H75F 0.9800 . ?
C68B C69B 1.716(18) . ?
C68B C73B 1.161(15) . ?
C68B C74B 1.099(14) . ?
C69B H69B 0.9500 . ?
C69B C70B 1.463(19) . ?
C70B C71B 1.408(17) . ?
C70B C75B 1.322(15) . ?
C71B H71B 0.9500 . ?
C71B C72B 1.373(18) . ?
C72B H72B 0.9500 . ?
C72B C73B 1.481(15) . ?
C73B H73B 0.9500 . ?
C74B H74G 0.9800 . ?
C74B H74H 0.9800 . ?
C74B H74I 0.9800 . ?
C75B H75G 0.9800 . ?
C75B H75H 0.9800 . ?
C75B H75I 0.9800 . ?
C85B H85B 1.0000 . ?
C85B Cl1B 1.713(17) . ?
C85B Cl2B 1.712(17) . ?
C85B Cl3B 1.54(4) . ?
C85A H85A 1.0000 . ?
C85A Cl1A 1.698(13) . ?
C85A Cl3A 1.723(13) . ?
C85A Cl2A 1.710(12) . ?
C60 C61 1.35(2) . ?
C60 C65 1.382(17) . ?
C60 C66 1.511(19) . ?
C61 H61 0.9500 . ?
C61 C62 1.43(2) . ?
C62 C63 1.394(13) . ?
C62 C67 1.457(11) . ?
C63 H63 0.9500 . ?
C63 C64 1.39(2) . ?
C64 H64 0.9500 . ?
C64 C65 1.43(2) . ?
C65 H65 0.9500 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C76 H76 0.9500 . ?
C76 C83 1.483(14) . ?
C76 C84 1.343(12) . ?
C78 H78 0.9500 . ?
C78 C79 1.346(10) . ?
C78 C83 1.292(15) . ?
C79 H79 0.9500 . ?
C79 C80 1.374(10) . ?
C80 H80 0.9500 . ?
C80 C84 1.405(8) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C81 C84 1.511(9) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C82 C83 1.515(14) . ?
C85 H85 1.0000 . ?
C85 Cl1 1.708(14) . ?
C85 Cl2 1.720(14) . ?
C85 Cl3 1.707(14) . ?
C23A H23A 1.0000 . ?
C23A C24A 1.478(13) . ?
C23A C25A 1.689(11) . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C41A H41D 0.9800 . ?
C41A H41E 0.9800 . ?
C41A H41F 0.9800 . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 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
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C3 112.3(2) . . ?
C1 C2 C4 111.6(2) . . ?
C1 C2 C5 112.7(2) . . ?
C3 C2 C4 106.7(2) . . ?
C5 C2 C3 106.6(2) . . ?
C5 C2 C4 106.53(19) . . ?
C6 C3 C2 116.3(2) . . ?
C9 C3 C2 104.0(2) . . ?
C9 C3 C6 111.9(2) . . ?
C9 C3 C43 109.9(2) . . ?
C43 C3 C2 104.2(2) . . ?
C43 C3 C6 110.1(2) . . ?
C7 C4 C2 116.4(2) . . ?
C14 C4 C2 103.8(2) . . ?
C14 C4 C7 109.4(2) . . ?
C26 C4 C2 103.7(2) . . ?
C26 C4 C7 110.1(2) . . ?
C26 C4 C14 113.3(2) . . ?
C8 C5 C2 116.5(2) . . ?
C31 C5 C2 104.2(2) . . ?
C31 C5 C8 111.3(2) . . ?
C48 C5 C2 104.1(2) . . ?
C48 C5 C8 110.9(2) . . ?
C48 C5 C31 109.4(2) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C3 127.1(2) . . ?
C14 C9 C3 113.1(2) . . ?
C14 C9 C10 119.7(3) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 119.9(3) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 N1 118.8(3) . . ?
C13 C12 C11 121.0(3) . . ?
C13 C12 N1 120.2(3) . . ?
C12 C13 H13 120.8 . . ?
C12 C13 C14 118.4(3) . . ?
C14 C13 H13 120.8 . . ?
C9 C14 C4 112.0(2) . . ?
C9 C14 C13 121.1(3) . . ?
C13 C14 C4 126.9(2) . . ?
C16 C15 H15 127.3 . . ?
N1 C15 H15 127.3 . . ?
N1 C15 C16 105.4(3) . . ?
C15 C16 C17 129.1(3) . . ?
C15 C16 N3 108.3(3) . . ?
N3 C16 C17 122.5(3) . . ?
C21 C17 C16 121.7(3) . . ?
N4 C17 C16 114.7(3) . . ?
N4 C17 C21 123.6(3) . . ?
C19 C18 C22 119.1(3) . . ?
N4 C18 C19 123.3(3) . . ?
N4 C18 C22 117.6(3) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 H19 120.6 . . ?
C19 C20 H20 120.6 . . ?
C19 C20 C21 118.8(3) . . ?
C21 C20 H20 120.6 . . ?
C17 C21 H21 120.6 . . ?
C20 C21 C17 118.8(3) . . ?
C20 C21 H21 120.6 . . ?
N5 C22 C18 116.2(3) . . ?
O1 C22 C18 120.2(3) . . ?
O1 C22 N5 123.6(3) . . ?
C27 C26 C4 127.6(2) . . ?
C31 C26 C4 113.1(2) . . ?
C31 C26 C27 119.3(2) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 119.9(2) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 N6 120.2(2) . . ?
C30 C29 C28 120.9(2) . . ?
C30 C29 N6 118.9(2) . . ?
C29 C30 H30 120.9 . . ?
C31 C30 C29 118.1(2) . . ?
C31 C30 H30 120.9 . . ?
C26 C31 C5 112.3(2) . . ?
C26 C31 C30 121.8(2) . . ?
C30 C31 C5 125.9(2) . . ?
C33 C32 H32 127.5 . . ?
N6 C32 H32 127.5 . . ?
N6 C32 C33 105.1(2) . . ?
C32 C33 C34 128.1(2) . . ?
N8 C33 C32 108.1(2) . . ?
N8 C33 C34 123.8(2) . . ?
C38 C34 C33 121.4(3) . . ?
N9 C34 C33 115.7(2) . . ?
N9 C34 C38 122.8(2) . . ?
C36 C35 C39 120.0(2) . . ?
N9 C35 C36 123.1(3) . . ?
N9 C35 C39 116.9(2) . . ?
C35 C36 H36 120.6 . . ?
C35 C36 C37 118.8(2) . . ?
C37 C36 H36 120.6 . . ?
C36 C37 H37 120.6 . . ?
C38 C37 C36 118.8(3) . . ?
C38 C37 H37 120.6 . . ?
C34 C38 H38 120.6 . . ?
C37 C38 C34 118.8(3) . . ?
C37 C38 H38 120.6 . . ?
N10 C39 C35 116.7(2) . . ?
O2 C39 C35 119.8(3) . . ?
O2 C39 N10 123.5(3) . . ?
C41 C40 H40 107.4 . . ?
C42 C40 H40 107.4 . . ?
C42 C40 C41 115.1(5) . . ?
N10 C40 H40A 107.4 . . ?
N10 C40 H40 107.4 . . ?
N10 C40 C41 109.7(3) . . ?
N10 C40 C42 109.6(3) . . ?
N10 C40 C41A 111.4(8) . . ?
N10 C40 C42A 108.8(9) . . ?
C41A C40 H40A 107.4 . . ?
C42A C40 H40A 107.4 . . ?
C42A C40 C41A 114.2(10) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C3 127.5(2) . . ?
C48 C43 C3 112.4(2) . . ?
C48 C43 C44 120.1(2) . . ?
C43 C44 H44 120.5 . . ?
C45 C44 C43 119.0(2) . . ?
C45 C44 H44 120.5 . . ?
C44 C45 C46 121.2(2) . . ?
C44 C45 N11 120.2(2) . . ?
C46 C45 N11 118.5(2) . . ?
C45 C46 H46 120.2 . . ?
C47 C46 C45 119.6(3) . . ?
C47 C46 H46 120.2 . . ?
C46 C47 H47 120.0 . . ?
C46 C47 C48 120.1(2) . . ?
C48 C47 H47 120.0 . . ?
C43 C48 C5 112.6(2) . . ?
C43 C48 C47 120.0(2) . . ?
C47 C48 C5 127.3(2) . . ?
C50 C49 H49 127.6 . . ?
N11 C49 H49 127.6 . . ?
N11 C49 C50 104.8(2) . . ?
C49 C50 C51 129.2(2) . . ?
N13 C50 C49 107.8(2) . . ?
N13 C50 C51 123.0(2) . . ?
C55 C51 C50 122.1(3) . . ?
N14 C51 C50 115.5(2) . . ?
N14 C51 C55 122.4(3) . . ?
C53 C52 C56 120.1(3) . . ?
N14 C52 C53 123.0(3) . . ?
N14 C52 C56 116.8(2) . . ?
C52 C53 H53 120.6 . . ?
C52 C53 C54 118.8(3) . . ?
C54 C53 H53 120.6 . . ?
C53 C54 H54 120.3 . . ?
C55 C54 C53 119.3(3) . . ?
C55 C54 H54 120.3 . . ?
C51 C55 H55 120.6 . . ?
C54 C55 C51 118.8(3) . . ?
C54 C55 H55 120.6 . . ?
N15 C56 C52 116.3(2) . . ?
O3 C56 C52 119.8(3) . . ?
O3 C56 N15 123.8(3) . . ?
C58 C57 H57 107.7 . . ?
C59 C57 H57 107.7 . . ?
C59 C57 C58 112.3(3) . . ?
N15 C57 H57 107.7 . . ?
N15 C57 C58 111.0(2) . . ?
N15 C57 C59 110.2(3) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C15 N1 C12 129.4(3) . . ?
C15 N1 N2 109.8(3) . . ?
N2 N1 C12 120.8(3) . . ?
N3 N2 N1 107.8(3) . . ?
N2 N3 C16 108.6(3) . . ?
C17 N4 C18 116.7(3) . . ?
C22 N5 H5A 120.8 . . ?
C22 N5 H5B 118.7 . . ?
C22 N5 C23 118.3(6) . . ?
C22 N5 C23A 122.7(5) . . ?
C23 N5 H5A 120.8 . . ?
C23A N5 H5B 118.7 . . ?
N5 C23 H23 117.1 . . ?
N5 C23 C25 104.0(8) . . ?
C24 C23 N5 108.3(9) . . ?
C24 C23 H23 117.1 . . ?
C24 C23 C25 89.4(8) . . ?
C25 C23 H23 117.1 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C32 N6 C29 129.1(2) . . ?
N7 N6 C29 121.0(2) . . ?
N7 N6 C32 109.9(2) . . ?
N8 N7 N6 108.1(2) . . ?
N7 N8 C33 108.8(2) . . ?
C34 N9 C35 117.8(2) . . ?
C39 N10 C40 123.1(3) . . ?
C39 N10 H10A 118.4 . . ?
C40 N10 H10A 118.4 . . ?
C49 N11 C45 129.2(2) . . ?
C49 N11 N12 110.9(2) . . ?
N12 N11 C45 119.9(2) . . ?
N13 N12 N11 107.1(2) . . ?
N12 N13 C50 109.5(2) . . ?
C52 N14 C51 117.6(2) . . ?
C56 N15 C57 122.3(2) . . ?
C56 N15 H15A 118.8 . . ?
C57 N15 H15A 118.8 . . ?
H4A O4 H4B 104.5 . . ?
C73 C68 C69 120.5(12) . . ?
C74 C68 C69 98.1(12) . . ?
C74 C68 C73 141.4(16) . . ?
C68 C69 H69 121.1 . . ?
C70 C69 C68 117.9(11) . . ?
C70 C69 H69 121.1 . . ?
C71 C70 C69 110.3(11) . . ?
C75 C70 C69 123.3(12) . . ?
C75 C70 C71 126.4(12) . . ?
C70 C71 H71 114.5 . . ?
C72 C71 C70 131.0(12) . . ?
C72 C71 H71 114.5 . . ?
C71 C72 H72 121.1 . . ?
C71 C72 C73 117.9(11) . . ?
C73 C72 H72 121.1 . . ?
C68 C73 C72 122.5(12) . . ?
C68 C73 H73 118.8 . . ?
C72 C73 H73 118.8 . . ?
C68 C74 H74A 109.5 . . ?
C68 C74 H74B 109.5 . . ?
C68 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C70 C75 H75A 109.5 . . ?
C70 C75 H75B 109.5 . . ?
C70 C75 H75C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C73A C68A C69A 120.2(13) . . ?
C74A C68A C69A 99.0(13) . . ?
C74A C68A C73A 140.8(17) . . ?
C68A C69A H69A 121.7 . . ?
C70A C69A C68A 116.6(11) . . ?
C70A C69A H69A 121.7 . . ?
C71A C70A C69A 111.4(11) . . ?
C75A C70A C69A 123.0(13) . . ?
C75A C70A C71A 125.6(13) . . ?
C70A C71A H71A 114.6 . . ?
C72A C71A C70A 130.9(13) . . ?
C72A C71A H71A 114.6 . . ?
C71A C72A H72A 121.5 . . ?
C71A C72A C73A 117.0(11) . . ?
C73A C72A H72A 121.5 . . ?
C68A C73A C72A 123.8(13) . . ?
C68A C73A H73A 118.1 . . ?
C72A C73A H73A 118.1 . . ?
C68A C74A H74D 109.5 . . ?
C68A C74A H74E 109.5 . . ?
C68A C74A H74F 109.5 . . ?
H74D C74A H74E 109.5 . . ?
H74D C74A H74F 109.5 . . ?
H74E C74A H74F 109.5 . . ?
C70A C75A H75D 109.5 . . ?
C70A C75A H75E 109.5 . . ?
C70A C75A H75F 109.5 . . ?
H75D C75A H75E 109.5 . . ?
H75D C75A H75F 109.5 . . ?
H75E C75A H75F 109.5 . . ?
C73B C68B C69B 120.1(13) . . ?
C74B C68B C69B 97.9(13) . . ?
C74B C68B C73B 142.0(17) . . ?
C68B C69B H69B 121.6 . . ?
C70B C69B C68B 116.8(11) . . ?
C70B C69B H69B 121.6 . . ?
C71B C70B C69B 111.5(12) . . ?
C75B C70B C69B 122.4(14) . . ?
C75B C70B C71B 126.1(14) . . ?
C70B C71B H71B 114.6 . . ?
C72B C71B C70B 130.8(13) . . ?
C72B C71B H71B 114.6 . . ?
C71B C72B H72B 121.5 . . ?
C71B C72B C73B 116.9(12) . . ?
C73B C72B H72B 121.5 . . ?
C68B C73B C72B 123.9(14) . . ?
C68B C73B H73B 118.1 . . ?
C72B C73B H73B 118.1 . . ?
C68B C74B H74G 109.5 . . ?
C68B C74B H74H 109.5 . . ?
C68B C74B H74I 109.5 . . ?
H74G C74B H74H 109.5 . . ?
H74G C74B H74I 109.5 . . ?
H74H C74B H74I 109.5 . . ?
C70B C75B H75G 109.5 . . ?
C70B C75B H75H 109.5 . . ?
C70B C75B H75I 109.5 . . ?
H75G C75B H75H 109.5 . . ?
H75G C75B H75I 109.5 . . ?
H75H C75B H75I 109.5 . . ?
Cl1B C85B H85B 94.0 . . ?
Cl2B C85B H85B 94.0 . . ?
Cl2B C85B Cl1B 113.3(16) . . ?
Cl3B C85B H85B 94.0 . . ?
Cl3B C85B Cl1B 123(3) . . ?
Cl3B C85B Cl2B 123(2) . . ?
Cl1A C85A H85A 104.6 . . ?
Cl1A C85A Cl3A 112.7(10) . . ?
Cl1A C85A Cl2A 114.5(10) . . ?
Cl3A C85A H85A 104.6 . . ?
Cl2A C85A H85A 104.6 . . ?
Cl2A C85A Cl3A 114.3(9) . . ?
C61 C60 C65 120.9(14) . . ?
C61 C60 C66 118.0(12) . . ?
C65 C60 C66 121.1(14) . . ?
C60 C61 H61 119.1 . . ?
C60 C61 C62 121.8(11) . . ?
C62 C61 H61 119.1 . . ?
C61 C62 C67 120.2(9) . . ?
C63 C62 C61 117.8(12) . . ?
C63 C62 C67 122.0(10) . . ?
C62 C63 H63 119.6 . . ?
C64 C63 C62 120.9(13) . . ?
C64 C63 H63 119.6 . . ?
C63 C64 H64 120.1 . . ?
C63 C64 C65 119.8(10) . . ?
C65 C64 H64 120.1 . . ?
C60 C65 C64 118.9(15) . . ?
C60 C65 H65 120.5 . . ?
C64 C65 H65 120.5 . . ?
C60 C66 H66A 109.5 . . ?
C60 C66 H66B 109.5 . . ?
C60 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C62 C67 H67A 109.5 . . ?
C62 C67 H67B 109.5 . . ?
C62 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C83 C76 H76 120.9 . . ?
C84 C76 H76 120.9 . . ?
C84 C76 C83 118.1(9) . . ?
C79 C78 H78 119.6 . . ?
C83 C78 H78 119.6 . . ?
C83 C78 C79 120.8(7) . . ?
C78 C79 H79 118.9 . . ?
C78 C79 C80 122.3(6) . . ?
C80 C79 H79 118.9 . . ?
C79 C80 H80 120.7 . . ?
C79 C80 C84 118.6(6) . . ?
C84 C80 H80 120.7 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C84 C81 H81A 109.5 . . ?
C84 C81 H81B 109.5 . . ?
C84 C81 H81C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C83 C82 H82A 109.5 . . ?
C83 C82 H82B 109.5 . . ?
C83 C82 H82C 109.5 . . ?
C76 C83 C82 115.8(11) . . ?
C78 C83 C76 120.3(11) . . ?
C78 C83 C82 123.9(9) . . ?
C76 C84 C80 119.8(6) . . ?
C76 C84 C81 119.9(6) . . ?
C80 C84 C81 120.3(6) . . ?
Cl1 C85 H85 104.7 . . ?
Cl1 C85 Cl2 112.2(10) . . ?
Cl2 C85 H85 104.7 . . ?
Cl3 C85 H85 104.7 . . ?
Cl3 C85 Cl1 113.1(10) . . ?
Cl3 C85 Cl2 116.0(12) . . ?
N5 C23A H23A 115.4 . . ?
N5 C23A C25A 105.0(6) . . ?
C24A C23A N5 112.5(8) . . ?
C24A C23A H23A 115.4 . . ?
C24A C23A C25A 90.1(7) . . ?
C25A C23A H23A 115.4 . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C23A C25A H25D 109.5 . . ?
C23A C25A H25E 109.5 . . ?
C23A C25A H25F 109.5 . . ?
H25D C25A H25E 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
C40 C41A H41D 109.5 . . ?
C40 C41A H41E 109.5 . . ?
C40 C41A H41F 109.5 . . ?
H41D C41A H41E 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
C40 C42A H42D 109.5 . . ?
C40 C42A H42E 109.5 . . ?
C40 C42A H42F 109.5 . . ?
H42D C42A H42E 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C11 H11 O2 0.95 2.53 3.226(4) 129.9 1_554 yes
C15 H15 O4 0.95 2.50 3.439(4) 172.0 . yes
C20 H20 N7 0.95 2.66 3.447(5) 141.0 1_545 yes
C32 H32 N14 0.95 2.36 3.304(4) 176.8 2_666 yes
C37 H37 N12 0.95 2.55 3.238(4) 129.4 1_556 yes
C49 H49 O1 0.95 2.19 3.074(4) 154.9 1_565 yes
C58 H58C N9 0.98 2.71 3.474(4) 135.2 2_666 yes
N5 H5A O4 0.88 2.63 3.428(4) 151.7 . yes
C25 H25C O4 0.98 2.22 3.079(18) 145.5 . yes
N10 H10A N13 0.88 2.33 3.117(3) 148.9 2_666 yes
N15 H15A N9 0.88 2.63 3.433(3) 152.3 2_666 yes
O4 H4A O2 0.87 1.95 2.813(3) 174.8 1_554 yes
O4 H4B N8 0.87 2.37 3.219(4) 165.7 2_666 yes
C74 H74C N1 0.98 3.27 3.791(17) 114.8 . yes
C74 H74C N2 0.98 2.10 2.818(17) 129.1 . yes
C75B H75H N3 0.98 2.95 3.66(2) 129.9 . yes
C85B H85B O3 1.00 2.86 3.72(15) 144.5 2_666 yes
C85A H85A O3 1.00 2.21 3.20(2) 169.5 2_666 yes
C67 H67A N7 0.98 2.52 3.489(8) 171.5 2_666 yes
C76 H76 O3 0.95 2.45 3.366(9) 161.4 2_666 yes
C85 H85 O3 1.00 2.44 3.36(3) 152.6 2_666 yes
C24A H24D O4 0.98 2.58 3.463(14) 149.4 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C6 -5.8(4) . . . . ?
C1 C2 C3 C9 117.7(3) . . . . ?
C1 C2 C3 C43 -127.2(3) . . . . ?
C1 C2 C4 C7 -0.6(3) . . . . ?
C1 C2 C4 C14 -120.9(2) . . . . ?
C1 C2 C4 C26 120.6(2) . . . . ?
C1 C2 C5 C8 4.4(3) . . . . ?
C1 C2 C5 C31 -118.6(2) . . . . ?
C1 C2 C5 C48 126.8(2) . . . . ?
C2 C3 C9 C10 -175.9(3) . . . . ?
C2 C3 C9 C14 6.4(3) . . . . ?
C2 C3 C43 C44 -177.0(2) . . . . ?
C2 C3 C43 C48 2.3(3) . . . . ?
C2 C4 C14 C9 1.8(3) . . . . ?
C2 C4 C14 C13 -179.0(2) . . . . ?
C2 C4 C26 C27 -178.3(2) . . . . ?
C2 C4 C26 C31 0.4(3) . . . . ?
C2 C5 C31 C26 -4.1(3) . . . . ?
C2 C5 C31 C30 178.1(2) . . . . ?
C2 C5 C48 C43 -1.9(3) . . . . ?
C2 C5 C48 C47 175.9(2) . . . . ?
C3 C2 C4 C7 122.4(2) . . . . ?
C3 C2 C4 C14 2.1(3) . . . . ?
C3 C2 C4 C26 -116.5(2) . . . . ?
C3 C2 C5 C8 -119.2(2) . . . . ?
C3 C2 C5 C31 117.8(2) . . . . ?
C3 C2 C5 C48 3.2(2) . . . . ?
C3 C9 C10 C11 -175.1(3) . . . . ?
C3 C9 C14 C4 -5.4(3) . . . . ?
C3 C9 C14 C13 175.3(2) . . . . ?
C3 C43 C44 C45 177.5(2) . . . . ?
C3 C43 C48 C5 -0.2(3) . . . . ?
C3 C43 C48 C47 -178.2(2) . . . . ?
C4 C2 C3 C6 -128.4(2) . . . . ?
C4 C2 C3 C9 -4.9(2) . . . . ?
C4 C2 C3 C43 110.2(2) . . . . ?
C4 C2 C5 C8 127.1(2) . . . . ?
C4 C2 C5 C31 4.1(2) . . . . ?
C4 C2 C5 C48 -110.5(2) . . . . ?
C4 C26 C27 C28 179.1(2) . . . . ?
C4 C26 C31 C5 2.5(3) . . . . ?
C4 C26 C31 C30 -179.7(2) . . . . ?
C5 C2 C3 C6 118.1(3) . . . . ?
C5 C2 C3 C9 -118.5(2) . . . . ?
C5 C2 C3 C43 -3.3(3) . . . . ?
C5 C2 C4 C7 -124.0(2) . . . . ?
C5 C2 C4 C14 115.7(2) . . . . ?
C5 C2 C4 C26 -2.9(2) . . . . ?
C6 C3 C9 C10 -49.6(4) . . . . ?
C6 C3 C9 C14 132.8(2) . . . . ?
C6 C3 C43 C44 57.6(3) . . . . ?
C6 C3 C43 C48 -123.1(2) . . . . ?
C7 C4 C14 C9 -123.1(3) . . . . ?
C7 C4 C14 C13 56.1(3) . . . . ?
C7 C4 C26 C27 -53.0(4) . . . . ?
C7 C4 C26 C31 125.6(3) . . . . ?
C8 C5 C31 C26 -130.5(2) . . . . ?
C8 C5 C31 C30 51.8(3) . . . . ?
C8 C5 C48 C43 124.1(2) . . . . ?
C8 C5 C48 C47 -58.1(3) . . . . ?
C9 C3 C43 C44 -66.1(3) . . . . ?
C9 C3 C43 C48 113.2(2) . . . . ?
C9 C10 C11 C12 -0.2(4) . . . . ?
C10 C9 C14 C4 176.7(2) . . . . ?
C10 C9 C14 C13 -2.5(4) . . . . ?
C10 C11 C12 C13 -2.0(5) . . . . ?
C10 C11 C12 N1 177.0(3) . . . . ?
C11 C12 C13 C14 1.9(4) . . . . ?
C11 C12 N1 C15 -15.0(5) . . . . ?
C11 C12 N1 N2 165.6(3) . . . . ?
C12 C13 C14 C4 -178.8(3) . . . . ?
C12 C13 C14 C9 0.4(4) . . . . ?
C12 N1 N2 N3 -179.7(3) . . . . ?
C13 C12 N1 C15 164.0(3) . . . . ?
C13 C12 N1 N2 -15.4(4) . . . . ?
C14 C4 C26 C27 69.9(3) . . . . ?
C14 C4 C26 C31 -111.4(3) . . . . ?
C14 C9 C10 C11 2.4(4) . . . . ?
C15 C16 C17 C21 -178.1(3) . . . . ?
C15 C16 C17 N4 1.0(5) . . . . ?
C15 C16 N3 N2 -1.1(4) . . . . ?
C15 N1 N2 N3 0.7(4) . . . . ?
C16 C15 N1 C12 179.2(3) . . . . ?
C16 C15 N1 N2 -1.4(4) . . . . ?
C16 C17 C21 C20 178.1(3) . . . . ?
C16 C17 N4 C18 -178.6(3) . . . . ?
C17 C16 N3 N2 -178.8(3) . . . . ?
C18 C19 C20 C21 1.2(5) . . . . ?
C18 C22 N5 C23 -172.7(7) . . . . ?
C18 C22 N5 C23A 173.7(6) . . . . ?
C19 C18 C22 N5 175.5(3) . . . . ?
C19 C18 C22 O1 -5.4(5) . . . . ?
C19 C18 N4 C17 0.8(4) . . . . ?
C19 C20 C21 C17 0.0(5) . . . . ?
C21 C17 N4 C18 0.5(4) . . . . ?
C22 C18 C19 C20 177.5(3) . . . . ?
C22 C18 N4 C17 -178.3(3) . . . . ?
C22 N5 C23 C24 -87.0(9) . . . . ?
C22 N5 C23 C25 178.9(9) . . . . ?
C22 N5 C23A C24A -141.3(7) . . . . ?
C22 N5 C23A C25A 122.1(7) . . . . ?
C26 C4 C14 C9 113.6(3) . . . . ?
C26 C4 C14 C13 -67.2(4) . . . . ?
C26 C27 C28 C29 0.6(4) . . . . ?
C27 C26 C31 C5 -178.8(2) . . . . ?
C27 C26 C31 C30 -0.9(4) . . . . ?
C27 C28 C29 C30 -1.4(4) . . . . ?
C27 C28 C29 N6 178.6(2) . . . . ?
C28 C29 C30 C31 1.0(4) . . . . ?
C28 C29 N6 C32 -1.7(4) . . . . ?
C28 C29 N6 N7 -178.4(3) . . . . ?
C29 C30 C31 C5 177.7(2) . . . . ?
C29 C30 C31 C26 0.1(4) . . . . ?
C29 N6 N7 N8 178.0(3) . . . . ?
C30 C29 N6 C32 178.3(2) . . . . ?
C30 C29 N6 N7 1.6(4) . . . . ?
C31 C5 C48 C43 -112.8(2) . . . . ?
C31 C5 C48 C47 65.0(3) . . . . ?
C31 C26 C27 C28 0.5(4) . . . . ?
C32 C33 C34 C38 172.6(3) . . . . ?
C32 C33 C34 N9 -7.1(4) . . . . ?
C32 C33 N8 N7 0.1(4) . . . . ?
C32 N6 N7 N8 0.7(4) . . . . ?
C33 C32 N6 C29 -177.6(3) . . . . ?
C33 C32 N6 N7 -0.6(3) . . . . ?
C33 C34 C38 C37 -178.6(3) . . . . ?
C33 C34 N9 C35 -179.8(2) . . . . ?
C34 C33 N8 N7 -180.0(3) . . . . ?
C35 C36 C37 C38 1.1(4) . . . . ?
C35 C39 N10 C40 178.6(3) . . . . ?
C36 C35 C39 N10 167.0(3) . . . . ?
C36 C35 C39 O2 -13.1(4) . . . . ?
C36 C35 N9 C34 -1.3(4) . . . . ?
C36 C37 C38 C34 -1.9(4) . . . . ?
C38 C34 N9 C35 0.5(4) . . . . ?
C39 C35 C36 C37 -178.8(3) . . . . ?
C39 C35 N9 C34 178.0(2) . . . . ?
C41 C40 N10 C39 -78.4(5) . . . . ?
C42 C40 N10 C39 154.4(4) . . . . ?
C43 C3 C9 C10 73.1(3) . . . . ?
C43 C3 C9 C14 -104.6(3) . . . . ?
C43 C44 C45 C46 1.2(4) . . . . ?
C43 C44 C45 N11 -178.7(2) . . . . ?
C44 C43 C48 C5 179.1(2) . . . . ?
C44 C43 C48 C47 1.1(4) . . . . ?
C44 C45 C46 C47 -0.1(4) . . . . ?
C44 C45 N11 C49 169.6(3) . . . . ?
C44 C45 N11 N12 -11.6(4) . . . . ?
C45 C46 C47 C48 -0.5(4) . . . . ?
C45 N11 N12 N13 -179.7(2) . . . . ?
C46 C45 N11 C49 -10.4(4) . . . . ?
C46 C45 N11 N12 168.5(2) . . . . ?
C46 C47 C48 C5 -177.6(2) . . . . ?
C46 C47 C48 C43 0.0(4) . . . . ?
C48 C5 C31 C26 106.7(2) . . . . ?
C48 C5 C31 C30 -71.1(3) . . . . ?
C48 C43 C44 C45 -1.7(4) . . . . ?
C49 C50 C51 C55 15.4(4) . . . . ?
C49 C50 C51 N14 -162.7(3) . . . . ?
C49 C50 N13 N12 0.0(3) . . . . ?
C49 N11 N12 N13 -0.7(3) . . . . ?
C50 C49 N11 C45 179.6(2) . . . . ?
C50 C49 N11 N12 0.6(3) . . . . ?
C50 C51 C55 C54 -178.4(3) . . . . ?
C50 C51 N14 C52 177.4(2) . . . . ?
C51 C50 N13 N12 -179.9(2) . . . . ?
C52 C53 C54 C55 -0.2(6) . . . . ?
C52 C56 N15 C57 -179.3(2) . . . . ?
C53 C52 C56 N15 -177.8(3) . . . . ?
C53 C52 C56 O3 0.3(4) . . . . ?
C53 C52 N14 C51 1.5(4) . . . . ?
C53 C54 C55 C51 0.9(5) . . . . ?
C55 C51 N14 C52 -0.7(4) . . . . ?
C56 C52 C53 C54 178.0(3) . . . . ?
C56 C52 N14 C51 -177.6(2) . . . . ?
C58 C57 N15 C56 -140.6(3) . . . . ?
C59 C57 N15 C56 94.4(3) . . . . ?
N1 C12 C13 C14 -177.1(3) . . . . ?
N1 C15 C16 C17 179.0(3) . . . . ?
N1 C15 C16 N3 1.5(4) . . . . ?
N1 N2 N3 C16 0.2(4) . . . . ?
N3 C16 C17 C21 -0.9(5) . . . . ?
N3 C16 C17 N4 178.3(3) . . . . ?
N4 C17 C21 C20 -0.9(5) . . . . ?
N4 C18 C19 C20 -1.6(5) . . . . ?
N4 C18 C22 N5 -5.4(4) . . . . ?
N4 C18 C22 O1 173.7(3) . . . . ?
N6 C29 C30 C31 -179.0(2) . . . . ?
N6 C32 C33 C34 -179.6(3) . . . . ?
N6 C32 C33 N8 0.3(3) . . . . ?
N6 N7 N8 C33 -0.5(4) . . . . ?
N8 C33 C34 C38 -7.2(5) . . . . ?
N8 C33 C34 N9 173.1(3) . . . . ?
N9 C34 C38 C37 1.1(4) . . . . ?
N9 C35 C36 C37 0.5(4) . . . . ?
N9 C35 C39 N10 -12.3(4) . . . . ?
N9 C35 C39 O2 167.6(3) . . . . ?
N11 C45 C46 C47 179.8(2) . . . . ?
N11 C49 C50 C51 179.5(3) . . . . ?
N11 C49 C50 N13 -0.4(3) . . . . ?
N11 N12 N13 C50 0.4(3) . . . . ?
N13 C50 C51 C55 -164.7(3) . . . . ?
N13 C50 C51 N14 17.2(4) . . . . ?
N14 C51 C55 C54 -0.4(5) . . . . ?
N14 C52 C53 C54 -1.0(5) . . . . ?
N14 C52 C56 N15 1.3(4) . . . . ?
N14 C52 C56 O3 179.4(3) . . . . ?
O1 C22 N5 C23 8.3(8) . . . . ?
O1 C22 N5 C23A -5.3(8) . . . . ?
O2 C39 N10 C40 -1.4(5) . . . . ?
O3 C56 N15 C57 2.7(4) . . . . ?
C68 C69 C70 C71 0.0(2) . . . . ?
C68 C69 C70 C75 -179.9(2) . . . . ?
C69 C68 C73 C72 -0.3(5) . . . . ?
C69 C70 C71 C72 0.0(5) . . . . ?
C70 C71 C72 C73 -0.2(7) . . . . ?
C71 C72 C73 C68 0.3(6) . . . . ?
C73 C68 C69 C70 0.1(3) . . . . ?
C74 C68 C69 C70 -179.9(2) . . . . ?
C74 C68 C73 C72 179.8(4) . . . . ?
C75 C70 C71 C72 179.9(4) . . . . ?
C68A C69A C70A C71A 0.0(2) . . . . ?
C68A C69A C70A C75A -180.0(2) . . . . ?
C69A C68A C73A C72A 0.1(5) . . . . ?
C69A C70A C71A C72A 0.1(5) . . . . ?
C70A C71A C72A C73A -0.1(7) . . . . ?
C71A C72A C73A C68A 0.0(7) . . . . ?
C73A C68A C69A C70A -0.1(3) . . . . ?
C74A C68A C69A C70A -179.9(2) . . . . ?
C74A C68A C73A C72A 179.9(4) . . . . ?
C75A C70A C71A C72A -180.0(4) . . . . ?
C68B C69B C70B C71B 0.0(2) . . . . ?
C68B C69B C70B C75B 180.0(2) . . . . ?
C69B C68B C73B C72B 0.3(5) . . . . ?
C69B C70B C71B C72B -0.1(6) . . . . ?
C70B C71B C72B C73B 0.3(7) . . . . ?
C71B C72B C73B C68B -0.4(7) . . . . ?
C73B C68B C69B C70B -0.1(3) . . . . ?
C74B C68B C69B C70B 179.9(2) . . . . ?
C74B C68B C73B C72B -179.7(5) . . . . ?
C75B C70B C71B C72B 179.9(5) . . . . ?
C60 C61 C62 C63 0.2(3) . . . . ?
C60 C61 C62 C67 -179.3(3) . . . . ?
C61 C60 C65 C64 -0.5(5) . . . . ?
C61 C62 C63 C64 -0.4(6) . . . . ?
C62 C63 C64 C65 0.2(7) . . . . ?
C63 C64 C65 C60 0.3(7) . . . . ?
C65 C60 C61 C62 0.3(3) . . . . ?
C66 C60 C61 C62 180.0(3) . . . . ?
C66 C60 C65 C64 179.8(4) . . . . ?
C67 C62 C63 C64 179.1(4) . . . . ?
C78 C79 C80 C84 1.1(8) . . . . ?
C79 C78 C83 C76 2(2) . . . . ?
C79 C78 C83 C82 -179.7(13) . . . . ?
C79 C80 C84 C76 1.4(9) . . . . ?
C79 C80 C84 C81 179.8(5) . . . . ?
C83 C76 C84 C80 -1.9(16) . . . . ?
C83 C76 C84 C81 179.6(11) . . . . ?
C83 C78 C79 C80 -3.0(12) . . . . ?
C84 C76 C83 C78 0(2) . . . . ?
C84 C76 C83 C82 -178.0(10) . . . . ?
C41A C40 N10 C39 -138.7(11) . . . . ?
C42A C40 N10 C39 94.5(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.441
_oxdiff_exptl_absorpt_empirical_full_min 0.493
