# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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_2-TBACl
_database_code_depnum_ccdc_archive 'CCDC 1965677'
loop_
_audit_author_name
_audit_author_address
'He Qing'
;Hunan University
China
;
_audit_update_record             
;
2019-11-14 deposited with the CCDC.	2020-01-02 downloaded from the CCDC.
;
_audit_creation_date             2019-11-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C46 H50 N8 O2, C15.564 H31 N, C H Cl3, Cl, 0.436(C1), O'
_chemical_formula_sum            'C63 H82 Cl4 N9 O3'
_chemical_formula_weight         1155.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   13.0780(8)
_cell_length_b                   14.7017(11)
_cell_length_c                   16.4585(12)
_cell_angle_alpha                89.009(6)
_cell_angle_beta                 84.136(6)
_cell_angle_gamma                81.419(6)
_cell_volume                     3112.7(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4386
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      22.4930
_cell_measurement_theta_min      1.8630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.242
_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            colorless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.059
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_unetI/netI     0.1537
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26770
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        22.771
_diffrn_reflns_theta_max         22.771
_diffrn_reflns_theta_min         1.583
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4072
_reflns_number_total             8306
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         8306
_refine_ls_number_restraints     456
_refine_ls_R_factor_all          0.2048
_refine_ls_R_factor_gt           0.1052
_refine_ls_restrained_S_all      1.006
_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)+(0.1480P)²+1.6617P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2447
_refine_ls_wR_factor_ref         0.3060
_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
 C62-C63 \\sim C62-C63A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
4. Others
 Sof(C63A)=1-FVAR(1)
 Sof(C63)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C47(H47)
5.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C56(H56A,H56B), C57(H57A,H57B),
  C58(H58A,H58B), C60(H60A,H60B), C61(H61A,H61B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C3(H3), N3(H3A), C4(H4), N4(H4A), N5(H5), C8(H8), N8(H8A),
 C9(H9), C13(H13), C14(H14), C18(H18), C19(H19), C26(H26), C27(H27), C30(H30),
 C31(H31), C34(H34), C35(H35)
5.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C51(H51A,H51B,H51C), C55(H55A,
 H55B,H55C), C59(H59A,H59B,H59C)
;
_atom_sites_solution_hydrogens   geom
_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 0.8948(6) 0.8067(5) 0.0457(5) 0.040(2) Uani 1 1 d . U . . .
N1 N 0.9978(5) 0.8395(4) 0.1599(5) 0.0416(18) Uani 1 1 d . U . . .
H1 H 0.958531 0.814269 0.197823 0.050 Uiso 1 1 calc R U . . .
O1 O 0.8424(5) 0.4439(4) 0.1064(4) 0.0629(19) Uani 1 1 d . U . . .
C2 C 0.9799(6) 0.8463(5) 0.0787(5) 0.035(2) Uani 1 1 d . U . . .
N2 N 0.9527(5) 0.9263(4) 0.3507(4) 0.0388(18) Uani 1 1 d . U . . .
H2 H 0.932061 0.872251 0.348360 0.047 Uiso 1 1 calc R U . . .
O2 O 0.6728(5) 0.6827(4) 0.6269(4) 0.0542(17) Uani 1 1 d . U . . .
C3 C 1.0583(7) 0.8899(6) 0.0430(6) 0.050(2) Uani 1 1 d . U . . .
H3 H 1.068096 0.905079 -0.013312 0.059 Uiso 1 1 calc R U . . .
N3 N 0.6984(5) 0.9540(4) 0.3320(4) 0.0369(17) Uani 1 1 d . U . . .
H3A H 0.746932 0.909425 0.312814 0.044 Uiso 1 1 calc R U . . .
C4 C 1.1214(7) 0.9087(6) 0.1013(6) 0.045(2) Uani 1 1 d . U . . .
H4 H 1.180867 0.938942 0.091772 0.054 Uiso 1 1 calc R U . . .
N4 N 0.7396(5) 0.8614(4) 0.1487(4) 0.0414(18) Uani 1 1 d . U . . .
H4A H 0.764153 0.827683 0.188980 0.050 Uiso 1 1 calc R U . . .
C5 C 1.0839(6) 0.8765(6) 0.1741(5) 0.039(2) Uani 1 1 d . U . . .
N5 N 0.7995(5) 0.5726(5) 0.1840(4) 0.0454(19) Uani 1 1 d . U . . .
H5 H 0.804117 0.598113 0.231211 0.054 Uiso 1 1 calc R U . . .
C6 C 1.1171(6) 0.8802(5) 0.2586(5) 0.041(2) Uani 1 1 d . U . . .
N6 N 0.8683(5) 0.4718(4) 0.3146(5) 0.0390(18) Uani 1 1 d . U . . .
C7 C 1.0436(6) 0.9485(6) 0.3114(5) 0.039(2) Uani 1 1 d . U . . .
N7 N 0.8141(5) 0.5407(4) 0.4713(5) 0.0393(18) Uani 1 1 d . U . . .
C8 C 1.0464(6) 1.0382(6) 0.3287(5) 0.047(2) Uani 1 1 d . U . . .
H8 H 1.099547 1.073008 0.309177 0.057 Uiso 1 1 calc R U . . .
N8 N 0.7143(5) 0.7176(4) 0.4958(4) 0.0418(18) Uani 1 1 d . U . . .
H8A H 0.749185 0.698325 0.449169 0.050 Uiso 1 1 calc R U . . .
C9 C 0.9545(6) 1.0708(6) 0.3818(5) 0.046(2) Uani 1 1 d . U . . .
H9 H 0.936378 1.130862 0.404134 0.056 Uiso 1 1 calc R U . . .
C10 C 0.8984(6) 1.0006(5) 0.3943(5) 0.037(2) Uani 1 1 d . U . . .
C11 C 0.7962(6) 0.9952(5) 0.4467(5) 0.036(2) Uani 1 1 d . U . . .
C12 C 0.7066(6) 1.0072(5) 0.3976(5) 0.036(2) Uani 1 1 d . U . . .
C13 C 0.6149(6) 1.0690(6) 0.4059(5) 0.045(2) Uani 1 1 d . U . . .
H13 H 0.597061 1.115739 0.446177 0.054 Uiso 1 1 calc R U . . .
C14 C 0.5528(7) 1.0511(6) 0.3450(6) 0.046(2) Uani 1 1 d . U . . .
H14 H 0.486206 1.083636 0.336888 0.055 Uiso 1 1 calc R U . . .
C15 C 0.6051(6) 0.9785(5) 0.2993(5) 0.039(2) Uani 1 1 d . U . . .
C16 C 0.5712(6) 0.9275(6) 0.2308(6) 0.047(2) Uani 1 1 d . U . . .
C17 C 0.6467(6) 0.9199(5) 0.1542(6) 0.040(2) Uani 1 1 d . U . . .
C18 C 0.6372(7) 0.9599(6) 0.0794(6) 0.052(3) Uani 1 1 d . U . . .
H18 H 0.580813 1.003826 0.065294 0.062 Uiso 1 1 calc R U . . .
C19 C 0.7274(7) 0.9240(6) 0.0256(6) 0.046(2) Uani 1 1 d . U . . .
H19 H 0.741380 0.939470 -0.030339 0.055 Uiso 1 1 calc R U . . .
C20 C 0.7890(6) 0.8636(5) 0.0700(5) 0.040(2) Uani 1 1 d . U . . .
C21 C 0.8984(7) 0.7059(5) 0.0752(6) 0.046(2) Uani 1 1 d . U . . .
H21A H 0.966208 0.671057 0.053693 0.056 Uiso 1 1 calc R U . . .
H21B H 0.895877 0.705349 0.135487 0.056 Uiso 1 1 calc R U . . .
C22 C 0.8133(7) 0.6555(6) 0.0512(5) 0.050(2) Uani 1 1 d . U . . .
H22A H 0.845785 0.600555 0.018997 0.060 Uiso 1 1 calc R U . . .
H22B H 0.769997 0.696085 0.015356 0.060 Uiso 1 1 calc R U . . .
C23 C 0.7429(7) 0.6250(6) 0.1230(6) 0.052(2) Uani 1 1 d . U . . .
H23A H 0.700344 0.680053 0.149216 0.062 Uiso 1 1 calc R U . . .
H23B H 0.694883 0.586934 0.102124 0.062 Uiso 1 1 calc R U . . .
C24 C 0.8449(7) 0.4856(6) 0.1691(6) 0.046(2) Uani 1 1 d . U . . .
C25 C 0.8974(6) 0.4405(5) 0.2401(6) 0.043(2) Uani 1 1 d . U . . .
C26 C 0.9727(7) 0.3619(6) 0.2225(6) 0.051(3) Uani 1 1 d . U . . .
H26 H 0.993778 0.342283 0.167871 0.061 Uiso 1 1 calc R U . . .
C27 C 1.0133(7) 0.3164(6) 0.2855(7) 0.052(3) Uani 1 1 d . U . . .
H27 H 1.063049 0.262749 0.275241 0.063 Uiso 1 1 calc R U . . .
C28 C 0.9845(7) 0.3453(6) 0.3655(6) 0.047(2) Uani 1 1 d . U . . .
C29 C 0.9096(6) 0.4279(5) 0.3785(6) 0.042(2) Uani 1 1 d . U . . .
C30 C 1.0247(7) 0.2973(6) 0.4348(7) 0.052(3) Uani 1 1 d . U . . .
H30 H 1.073719 0.242951 0.426369 0.063 Uiso 1 1 calc R U . . .
C31 C 0.9951(7) 0.3270(5) 0.5097(7) 0.050(3) Uani 1 1 d . U . . .
H31 H 1.022486 0.293246 0.554383 0.060 Uiso 1 1 calc R U . . .
C32 C 0.9209(7) 0.4110(6) 0.5253(6) 0.048(2) Uani 1 1 d . U . . .
C33 C 0.8808(6) 0.4601(6) 0.4607(6) 0.039(2) Uani 1 1 d . U . . .
C34 C 0.8879(7) 0.4439(6) 0.6045(7) 0.057(3) Uani 1 1 d . U . . .
H34 H 0.912993 0.411246 0.650444 0.069 Uiso 1 1 calc R U . . .
C35 C 0.8191(7) 0.5238(6) 0.6148(6) 0.053(3) Uani 1 1 d . U . . .
H35 H 0.794182 0.547064 0.667792 0.064 Uiso 1 1 calc R U . . .
C36 C 0.7874(7) 0.5688(6) 0.5461(6) 0.044(2) Uani 1 1 d . U . . .
C37 C 0.7175(6) 0.6619(6) 0.5602(6) 0.041(2) Uani 1 1 d . U . . .
C38 C 0.6542(6) 0.8105(6) 0.5004(5) 0.046(2) Uani 1 1 d . U . . .
H38A H 0.585751 0.807559 0.531343 0.055 Uiso 1 1 calc R U . . .
H38B H 0.641748 0.831955 0.444448 0.055 Uiso 1 1 calc R U . . .
C39 C 0.7071(6) 0.8792(5) 0.5405(5) 0.047(2) Uani 1 1 d . U . . .
H39A H 0.724434 0.855119 0.594760 0.056 Uiso 1 1 calc R U . . .
H39B H 0.657629 0.936875 0.549481 0.056 Uiso 1 1 calc R U . . .
C40 C 0.8066(6) 0.9018(5) 0.4919(5) 0.039(2) Uani 1 1 d . U . . .
H40A H 0.831161 0.852489 0.451248 0.047 Uiso 1 1 calc R U . . .
H40B H 0.860785 0.900872 0.529890 0.047 Uiso 1 1 calc R U . . .
C41 C 0.7815(7) 1.0718(6) 0.5097(5) 0.052(2) Uani 1 1 d . U . . .
H41A H 0.841178 1.064687 0.541957 0.078 Uiso 1 1 calc R U . . .
H41B H 0.717822 1.068631 0.545869 0.078 Uiso 1 1 calc R U . . .
H41C H 0.776086 1.131488 0.481728 0.078 Uiso 1 1 calc R U . . .
C42 C 0.4665(6) 0.9793(6) 0.2078(6) 0.062(3) Uani 1 1 d . U . . .
H42A H 0.412971 0.976640 0.253678 0.094 Uiso 1 1 calc R U . . .
H42B H 0.446564 0.950439 0.159780 0.094 Uiso 1 1 calc R U . . .
H42C H 0.473563 1.043628 0.195459 0.094 Uiso 1 1 calc R U . . .
C43 C 0.5549(7) 0.8309(6) 0.2612(6) 0.055(3) Uani 1 1 d . U . . .
H43A H 0.621241 0.796697 0.274612 0.083 Uiso 1 1 calc R U . . .
H43B H 0.528175 0.798372 0.218319 0.083 Uiso 1 1 calc R U . . .
H43C H 0.504773 0.836007 0.310008 0.083 Uiso 1 1 calc R U . . .
C44 C 0.9130(7) 0.8066(6) -0.0486(5) 0.054(3) Uani 1 1 d . U . . .
H44A H 0.909205 0.870033 -0.068587 0.080 Uiso 1 1 calc R U . . .
H44B H 0.859665 0.777061 -0.071016 0.080 Uiso 1 1 calc R U . . .
H44C H 0.981873 0.772494 -0.065924 0.080 Uiso 1 1 calc R U . . .
C45 C 1.2260(6) 0.9112(6) 0.2516(6) 0.055(3) Uani 1 1 d . U . . .
H45A H 1.274821 0.868660 0.215839 0.083 Uiso 1 1 calc R U . . .
H45B H 1.250593 0.911035 0.305866 0.083 Uiso 1 1 calc R U . . .
H45C H 1.221507 0.973385 0.228495 0.083 Uiso 1 1 calc R U . . .
C46 C 1.1260(6) 0.7838(5) 0.2988(6) 0.048(2) Uani 1 1 d . U . . .
H46A H 1.057299 0.764030 0.305991 0.071 Uiso 1 1 calc R U . . .
H46B H 1.152582 0.786404 0.352100 0.071 Uiso 1 1 calc R U . . .
H46C H 1.173726 0.739842 0.263627 0.071 Uiso 1 1 calc R U . . .
N9 N 0.4031(5) 0.6735(5) 0.7564(4) 0.0440(19) Uani 1 1 d . U . . .
C48 C 0.4783(6) 0.7159(6) 0.7989(6) 0.046(2) Uani 1 1 d . U . . .
H48A H 0.472541 0.781785 0.783561 0.055 Uiso 1 1 calc R U . . .
H48B H 0.549405 0.686346 0.779413 0.055 Uiso 1 1 calc R U . . .
C49 C 0.4639(7) 0.7087(6) 0.8907(6) 0.058(3) Uani 1 1 d . U . . .
H49A H 0.473222 0.642995 0.906618 0.069 Uiso 1 1 calc R U . . .
H49B H 0.392105 0.736187 0.910507 0.069 Uiso 1 1 calc R U . . .
C50 C 0.5414(8) 0.7578(7) 0.9317(7) 0.069(3) Uani 1 1 d . U . . .
H50A H 0.612999 0.727730 0.914342 0.083 Uiso 1 1 calc R U . . .
H50B H 0.535166 0.822491 0.912743 0.083 Uiso 1 1 calc R U . . .
C51 C 0.5238(9) 0.7564(8) 1.0245(7) 0.083(4) Uani 1 1 d . U . . .
H51A H 0.453339 0.786887 1.042183 0.124 Uiso 1 1 calc R U . . .
H51B H 0.574540 0.788912 1.047198 0.124 Uiso 1 1 calc R U . . .
H51C H 0.532056 0.692586 1.043827 0.124 Uiso 1 1 calc R U . . .
C52 C 0.2914(6) 0.7132(5) 0.7859(5) 0.042(2) Uani 1 1 d . U . . .
H52A H 0.244545 0.687541 0.751760 0.051 Uiso 1 1 calc R U . . .
H52B H 0.275880 0.692310 0.842670 0.051 Uiso 1 1 calc R U . . .
C53 C 0.2667(6) 0.8176(6) 0.7836(6) 0.046(2) Uani 1 1 d . U . . .
H53A H 0.312427 0.844833 0.817733 0.056 Uiso 1 1 calc R U . . .
H53B H 0.279062 0.839948 0.726922 0.056 Uiso 1 1 calc R U . . .
C54 C 0.1540(6) 0.8463(5) 0.8158(5) 0.043(2) Uani 1 1 d . U . . .
H54A H 0.108691 0.825975 0.777233 0.051 Uiso 1 1 calc R U . . .
H54B H 0.139734 0.815727 0.868950 0.051 Uiso 1 1 calc R U . . .
C55 C 0.1291(7) 0.9481(6) 0.8264(5) 0.046(2) Uani 1 1 d . U . . .
H55A H 0.145071 0.978545 0.774213 0.069 Uiso 1 1 calc R U . . .
H55B H 0.170812 0.967859 0.867194 0.069 Uiso 1 1 calc R U . . .
H55C H 0.055121 0.964743 0.844875 0.069 Uiso 1 1 calc R U . . .
C56 C 0.4111(6) 0.5714(6) 0.7719(6) 0.052(3) Uani 1 1 d . U . . .
H56A H 0.359139 0.547333 0.741755 0.062 Uiso 1 1 calc R U . . .
H56B H 0.392053 0.561616 0.830854 0.062 Uiso 1 1 calc R U . . .
C57 C 0.5171(7) 0.5148(6) 0.7479(6) 0.057(3) Uani 1 1 d . U . . .
H57A H 0.537014 0.522908 0.688821 0.068 Uiso 1 1 calc R U . . .
H57B H 0.569979 0.537070 0.778361 0.068 Uiso 1 1 calc R U . . .
C58 C 0.5148(8) 0.4158(7) 0.7660(9) 0.104(5) Uani 1 1 d . U . . .
H58A H 0.465104 0.392602 0.732854 0.124 Uiso 1 1 calc R U . . .
H58B H 0.490630 0.408154 0.824334 0.124 Uiso 1 1 calc R U . . .
C59 C 0.6245(9) 0.3589(8) 0.7465(11) 0.137(6) Uani 1 1 d . U . . .
H59A H 0.640558 0.352746 0.687218 0.206 Uiso 1 1 calc R U . . .
H59B H 0.625673 0.297668 0.771281 0.206 Uiso 1 1 calc R U . . .
H59C H 0.676438 0.390338 0.768816 0.206 Uiso 1 1 calc R U . . .
C60 C 0.4238(7) 0.6939(6) 0.6656(5) 0.049(2) Uani 1 1 d . U . A 1
H60A H 0.418661 0.761367 0.658773 0.058 Uiso 1 1 calc R U . A 1
H60B H 0.496358 0.667019 0.647525 0.058 Uiso 1 1 calc R U . A 1
C61 C 0.3548(8) 0.6600(7) 0.6095(6) 0.069(3) Uani 1 1 d . U . A 1
H61A H 0.284021 0.695375 0.618957 0.082 Uiso 1 1 calc R U . A 1
H61B H 0.349945 0.594449 0.621210 0.082 Uiso 1 1 calc R U . A 1
C62 C 0.3978(11) 0.6709(9) 0.5199(8) 0.098(4) Uiso 1 1 d . . . A 1
C63 C 0.3450(18) 0.6420(16) 0.4596(14) 0.099(10) Uiso 0.56(3) 1 d . . P A 1
Cl2 Cl 0.8337(3) 0.4865(2) -0.1441(2) 0.1141(13) Uani 1 1 d . U . . .
Cl3 Cl 0.6379(3) 0.4826(2) -0.0433(2) 0.0970(11) Uani 1 1 d . U . . .
Cl4 Cl 0.7865(2) 0.3165(2) -0.0692(2) 0.0922(11) Uani 1 1 d . U . . .
C47 C 0.7741(9) 0.4337(7) -0.0578(7) 0.081(3) Uani 1 1 d . U . . .
H47 H 0.807975 0.447261 -0.008525 0.097 Uiso 1 1 calc R U . . .
Cl1 Cl 0.83963(16) 0.74545(13) 0.30549(13) 0.0408(6) Uani 1 1 d . U . . .
C63A C 0.467(2) 0.587(2) 0.4938(17) 0.095(12) Uiso 0.44(3) 1 d . . P A 2
O3 O 0.3514(13) 0.4157(11) 0.6440(10) 0.243(7) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.484(11) . ?
C1 C20 1.526(11) . ?
C1 C21 1.547(11) . ?
C1 C44 1.545(11) . ?
N1 H1 0.8800 . ?
N1 C2 1.379(10) . ?
N1 C5 1.364(10) . ?
O1 C24 1.214(10) . ?
C2 C3 1.367(11) . ?
N2 H2 0.8800 . ?
N2 C7 1.374(9) . ?
N2 C10 1.380(10) . ?
O2 C37 1.211(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(12) . ?
N3 H3A 0.8800 . ?
N3 C12 1.366(10) . ?
N3 C15 1.380(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.353(11) . ?
N4 H4A 0.8800 . ?
N4 C17 1.375(10) . ?
N4 C20 1.389(10) . ?
C5 C6 1.504(11) . ?
N5 H5 0.8800 . ?
N5 C23 1.450(11) . ?
N5 C24 1.343(11) . ?
C6 C7 1.502(11) . ?
C6 C45 1.552(11) . ?
C6 C46 1.547(11) . ?
N6 C25 1.318(10) . ?
N6 C29 1.342(10) . ?
C7 C8 1.361(11) . ?
N7 C33 1.365(10) . ?
N7 C36 1.302(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.438(11) . ?
N8 H8A 0.8800 . ?
N8 C37 1.327(10) . ?
N8 C38 1.470(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.354(11) . ?
C10 C11 1.526(11) . ?
C11 C12 1.478(11) . ?
C11 C40 1.544(10) . ?
C11 C41 1.522(11) . ?
C12 C13 1.389(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.404(11) . ?
C14 H14 0.9500 . ?
C14 C15 1.370(11) . ?
C15 C16 1.503(12) . ?
C16 C17 1.515(12) . ?
C16 C42 1.543(12) . ?
C16 C43 1.535(11) . ?
C17 C18 1.365(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.440(12) . ?
C19 H19 0.9500 . ?
C19 C20 1.362(11) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.513(11) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.527(11) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.509(12) . ?
C25 C26 1.414(11) . ?
C26 H26 0.9500 . ?
C26 C27 1.337(12) . ?
C27 H27 0.9500 . ?
C27 C28 1.388(12) . ?
C28 C29 1.447(11) . ?
C28 C30 1.434(12) . ?
C29 C33 1.436(12) . ?
C30 H30 0.9500 . ?
C30 C31 1.316(12) . ?
C31 H31 0.9500 . ?
C31 C32 1.462(12) . ?
C32 C33 1.378(11) . ?
C32 C34 1.401(12) . ?
C34 H34 0.9500 . ?
C34 C35 1.370(12) . ?
C35 H35 0.9500 . ?
C35 C36 1.370(12) . ?
C36 C37 1.536(12) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.504(11) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.533(10) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
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 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
N9 C48 1.477(10) . ?
N9 C52 1.523(10) . ?
N9 C56 1.508(10) . ?
N9 C60 1.524(10) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.507(12) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.543(12) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.521(13) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.521(11) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.514(11) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C55 1.493(11) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.525(11) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.486(12) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.555(14) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.495(12) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.538(15) . ?
C62 C63 1.37(2) . ?
Cl2 C47 1.773(11) . ?
Cl3 C47 1.813(11) . ?
Cl4 C47 1.718(11) . ?
C47 H47 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C20 111.7(7) . . ?
C2 C1 C21 108.8(7) . . ?
C2 C1 C44 108.7(7) . . ?
C20 C1 C21 111.6(7) . . ?
C20 C1 C44 107.7(7) . . ?
C44 C1 C21 108.2(7) . . ?
C2 N1 H1 124.2 . . ?
C5 N1 H1 124.2 . . ?
C5 N1 C2 111.7(7) . . ?
N1 C2 C1 122.8(7) . . ?
C3 C2 C1 132.9(8) . . ?
C3 C2 N1 104.1(7) . . ?
C7 N2 H2 124.7 . . ?
C7 N2 C10 110.7(6) . . ?
C10 N2 H2 124.7 . . ?
C2 C3 H3 125.1 . . ?
C2 C3 C4 109.8(8) . . ?
C4 C3 H3 125.1 . . ?
C12 N3 H3A 124.0 . . ?
C12 N3 C15 112.1(7) . . ?
C15 N3 H3A 124.0 . . ?
C3 C4 H4 125.9 . . ?
C5 C4 C3 108.2(8) . . ?
C5 C4 H4 125.9 . . ?
C17 N4 H4A 125.0 . . ?
C17 N4 C20 109.9(7) . . ?
C20 N4 H4A 125.0 . . ?
N1 C5 C6 121.5(7) . . ?
C4 C5 N1 106.2(8) . . ?
C4 C5 C6 132.2(8) . . ?
C23 N5 H5 119.7 . . ?
C24 N5 H5 119.7 . . ?
C24 N5 C23 120.6(8) . . ?
C5 C6 C45 108.3(7) . . ?
C5 C6 C46 110.5(7) . . ?
C7 C6 C5 111.5(7) . . ?
C7 C6 C45 108.1(7) . . ?
C7 C6 C46 110.3(7) . . ?
C46 C6 C45 108.1(7) . . ?
C25 N6 C29 119.9(8) . . ?
N2 C7 C6 121.7(7) . . ?
C8 C7 N2 106.9(7) . . ?
C8 C7 C6 131.4(7) . . ?
C36 N7 C33 116.8(8) . . ?
C7 C8 H8 126.2 . . ?
C7 C8 C9 107.7(7) . . ?
C9 C8 H8 126.2 . . ?
C37 N8 H8A 119.1 . . ?
C37 N8 C38 121.7(7) . . ?
C38 N8 H8A 119.1 . . ?
C8 C9 H9 126.1 . . ?
C10 C9 C8 107.8(8) . . ?
C10 C9 H9 126.1 . . ?
N2 C10 C11 122.4(7) . . ?
C9 C10 N2 106.9(7) . . ?
C9 C10 C11 130.7(8) . . ?
C10 C11 C40 108.1(6) . . ?
C12 C11 C10 112.0(7) . . ?
C12 C11 C40 111.5(7) . . ?
C12 C11 C41 109.1(7) . . ?
C41 C11 C10 107.4(7) . . ?
C41 C11 C40 108.6(7) . . ?
N3 C12 C11 124.4(7) . . ?
N3 C12 C13 105.0(7) . . ?
C13 C12 C11 130.6(8) . . ?
C12 C13 H13 125.6 . . ?
C12 C13 C14 108.8(8) . . ?
C14 C13 H13 125.6 . . ?
C13 C14 H14 126.0 . . ?
C15 C14 C13 108.0(8) . . ?
C15 C14 H14 126.0 . . ?
N3 C15 C16 123.9(7) . . ?
C14 C15 N3 106.0(7) . . ?
C14 C15 C16 130.0(8) . . ?
C15 C16 C17 114.0(7) . . ?
C15 C16 C42 108.4(7) . . ?
C15 C16 C43 108.6(8) . . ?
C17 C16 C42 107.5(8) . . ?
C17 C16 C43 109.5(7) . . ?
C43 C16 C42 108.6(7) . . ?
N4 C17 C16 122.5(8) . . ?
C18 C17 N4 107.2(8) . . ?
C18 C17 C16 130.2(8) . . ?
C17 C18 H18 125.9 . . ?
C17 C18 C19 108.2(8) . . ?
C19 C18 H18 125.9 . . ?
C18 C19 H19 126.5 . . ?
C20 C19 C18 107.0(8) . . ?
C20 C19 H19 126.5 . . ?
N4 C20 C1 121.9(7) . . ?
C19 C20 C1 130.4(8) . . ?
C19 C20 N4 107.7(8) . . ?
C1 C21 H21A 108.2 . . ?
C1 C21 H21B 108.2 . . ?
H21A C21 H21B 107.3 . . ?
C22 C21 C1 116.4(7) . . ?
C22 C21 H21A 108.2 . . ?
C22 C21 H21B 108.2 . . ?
C21 C22 H22A 108.6 . . ?
C21 C22 H22B 108.6 . . ?
C21 C22 C23 114.5(7) . . ?
H22A C22 H22B 107.6 . . ?
C23 C22 H22A 108.6 . . ?
C23 C22 H22B 108.6 . . ?
N5 C23 C22 113.3(7) . . ?
N5 C23 H23A 108.9 . . ?
N5 C23 H23B 108.9 . . ?
C22 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
O1 C24 N5 124.9(9) . . ?
O1 C24 C25 121.5(8) . . ?
N5 C24 C25 113.6(8) . . ?
N6 C25 C24 119.8(8) . . ?
N6 C25 C26 123.2(9) . . ?
C26 C25 C24 116.9(9) . . ?
C25 C26 H26 121.2 . . ?
C27 C26 C25 117.7(9) . . ?
C27 C26 H26 121.2 . . ?
C26 C27 H27 119.1 . . ?
C26 C27 C28 121.7(9) . . ?
C28 C27 H27 119.1 . . ?
C27 C28 C29 117.4(9) . . ?
C27 C28 C30 123.4(9) . . ?
C30 C28 C29 119.1(9) . . ?
N6 C29 C28 120.0(9) . . ?
N6 C29 C33 121.8(8) . . ?
C33 C29 C28 118.2(8) . . ?
C28 C30 H30 119.2 . . ?
C31 C30 C28 121.5(9) . . ?
C31 C30 H30 119.2 . . ?
C30 C31 H31 119.5 . . ?
C30 C31 C32 121.0(9) . . ?
C32 C31 H31 119.5 . . ?
C33 C32 C31 119.8(9) . . ?
C33 C32 C34 118.1(9) . . ?
C34 C32 C31 122.2(9) . . ?
N7 C33 C29 117.3(8) . . ?
N7 C33 C32 122.4(9) . . ?
C32 C33 C29 120.3(8) . . ?
C32 C34 H34 120.4 . . ?
C35 C34 C32 119.3(9) . . ?
C35 C34 H34 120.4 . . ?
C34 C35 H35 121.2 . . ?
C34 C35 C36 117.6(9) . . ?
C36 C35 H35 121.2 . . ?
N7 C36 C35 125.7(9) . . ?
N7 C36 C37 118.3(8) . . ?
C35 C36 C37 115.9(9) . . ?
O2 C37 N8 123.8(8) . . ?
O2 C37 C36 121.0(8) . . ?
N8 C37 C36 115.2(8) . . ?
N8 C38 H38A 108.9 . . ?
N8 C38 H38B 108.9 . . ?
N8 C38 C39 113.4(7) . . ?
H38A C38 H38B 107.7 . . ?
C39 C38 H38A 108.9 . . ?
C39 C38 H38B 108.9 . . ?
C38 C39 H39A 108.6 . . ?
C38 C39 H39B 108.6 . . ?
C38 C39 C40 114.6(7) . . ?
H39A C39 H39B 107.6 . . ?
C40 C39 H39A 108.6 . . ?
C40 C39 H39B 108.6 . . ?
C11 C40 H40A 108.4 . . ?
C11 C40 H40B 108.4 . . ?
C39 C40 C11 115.6(6) . . ?
C39 C40 H40A 108.4 . . ?
C39 C40 H40B 108.4 . . ?
H40A C40 H40B 107.4 . . ?
C11 C41 H41A 109.5 . . ?
C11 C41 H41B 109.5 . . ?
C11 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C16 C42 H42A 109.5 . . ?
C16 C42 H42B 109.5 . . ?
C16 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C16 C43 H43A 109.5 . . ?
C16 C43 H43B 109.5 . . ?
C16 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C1 C44 H44A 109.5 . . ?
C1 C44 H44B 109.5 . . ?
C1 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C6 C45 H45A 109.5 . . ?
C6 C45 H45B 109.5 . . ?
C6 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C6 C46 H46A 109.5 . . ?
C6 C46 H46B 109.5 . . ?
C6 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 N9 C52 111.6(6) . . ?
C48 N9 C56 112.4(7) . . ?
C48 N9 C60 107.2(6) . . ?
C52 N9 C60 109.1(6) . . ?
C56 N9 C52 105.4(6) . . ?
C56 N9 C60 111.1(7) . . ?
N9 C48 H48A 108.6 . . ?
N9 C48 H48B 108.6 . . ?
N9 C48 C49 114.5(7) . . ?
H48A C48 H48B 107.6 . . ?
C49 C48 H48A 108.6 . . ?
C49 C48 H48B 108.6 . . ?
C48 C49 H49A 109.2 . . ?
C48 C49 H49B 109.2 . . ?
C48 C49 C50 112.2(8) . . ?
H49A C49 H49B 107.9 . . ?
C50 C49 H49A 109.2 . . ?
C50 C49 H49B 109.2 . . ?
C49 C50 H50A 109.0 . . ?
C49 C50 H50B 109.0 . . ?
H50A C50 H50B 107.8 . . ?
C51 C50 C49 113.0(9) . . ?
C51 C50 H50A 109.0 . . ?
C51 C50 H50B 109.0 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N9 C52 H52A 108.5 . . ?
N9 C52 H52B 108.4 . . ?
H52A C52 H52B 107.5 . . ?
C53 C52 N9 115.3(6) . . ?
C53 C52 H52A 108.5 . . ?
C53 C52 H52B 108.4 . . ?
C52 C53 H53A 109.9 . . ?
C52 C53 H53B 109.9 . . ?
H53A C53 H53B 108.3 . . ?
C54 C53 C52 109.0(7) . . ?
C54 C53 H53A 109.9 . . ?
C54 C53 H53B 109.9 . . ?
C53 C54 H54A 109.3 . . ?
C53 C54 H54B 109.3 . . ?
H54A C54 H54B 108.0 . . ?
C55 C54 C53 111.4(7) . . ?
C55 C54 H54A 109.3 . . ?
C55 C54 H54B 109.3 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N9 C56 H56A 108.3 . . ?
N9 C56 H56B 108.3 . . ?
N9 C56 C57 116.0(7) . . ?
H56A C56 H56B 107.4 . . ?
C57 C56 H56A 108.3 . . ?
C57 C56 H56B 108.3 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 108.1 . . ?
C58 C57 C56 110.7(8) . . ?
C58 C57 H57A 109.5 . . ?
C58 C57 H57B 109.5 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 C59 110.8(9) . . ?
H58A C58 H58B 108.1 . . ?
C59 C58 H58A 109.5 . . ?
C59 C58 H58B 109.5 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N9 C60 H60A 108.0 . . ?
N9 C60 H60B 108.0 . . ?
H60A C60 H60B 107.2 . . ?
C61 C60 N9 117.4(7) . . ?
C61 C60 H60A 108.0 . . ?
C61 C60 H60B 108.0 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
C60 C61 C62 110.5(9) . . ?
H61A C61 H61B 108.1 . . ?
C62 C61 H61A 109.5 . . ?
C62 C61 H61B 109.5 . . ?
C63 C62 C61 118.6(14) . . ?
Cl2 C47 Cl3 108.7(6) . . ?
Cl2 C47 H47 108.8 . . ?
Cl3 C47 H47 108.8 . . ?
Cl4 C47 Cl2 111.7(7) . . ?
Cl4 C47 Cl3 110.1(6) . . ?
Cl4 C47 H47 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -176.4(8) . . . . ?
C1 C21 C22 C23 -117.4(8) . . . . ?
N1 C2 C3 C4 0.0(9) . . . . ?
N1 C5 C6 C7 -70.4(9) . . . . ?
N1 C5 C6 C45 170.9(7) . . . . ?
N1 C5 C6 C46 52.6(9) . . . . ?
O1 C24 C25 N6 -155.0(8) . . . . ?
O1 C24 C25 C26 21.5(12) . . . . ?
C2 C1 C20 N4 -74.6(9) . . . . ?
C2 C1 C20 C19 103.9(10) . . . . ?
C2 C1 C21 C22 176.8(7) . . . . ?
C2 N1 C5 C4 0.7(9) . . . . ?
C2 N1 C5 C6 177.8(7) . . . . ?
C2 C3 C4 C5 0.5(10) . . . . ?
N2 C7 C8 C9 1.1(10) . . . . ?
N2 C10 C11 C12 -82.4(9) . . . . ?
N2 C10 C11 C40 40.8(10) . . . . ?
N2 C10 C11 C41 157.9(7) . . . . ?
C3 C4 C5 N1 -0.7(9) . . . . ?
C3 C4 C5 C6 -177.3(8) . . . . ?
N3 C12 C13 C14 0.4(9) . . . . ?
N3 C15 C16 C17 -56.7(11) . . . . ?
N3 C15 C16 C42 -176.4(7) . . . . ?
N3 C15 C16 C43 65.8(10) . . . . ?
C4 C5 C6 C7 105.9(10) . . . . ?
C4 C5 C6 C45 -12.9(12) . . . . ?
C4 C5 C6 C46 -131.1(9) . . . . ?
N4 C17 C18 C19 0.5(9) . . . . ?
C5 N1 C2 C1 176.4(7) . . . . ?
C5 N1 C2 C3 -0.4(9) . . . . ?
C5 C6 C7 N2 82.6(9) . . . . ?
C5 C6 C7 C8 -94.9(11) . . . . ?
N5 C24 C25 N6 22.5(11) . . . . ?
N5 C24 C25 C26 -161.0(7) . . . . ?
C6 C7 C8 C9 179.0(9) . . . . ?
N6 C25 C26 C27 2.2(12) . . . . ?
N6 C29 C33 N7 -4.0(11) . . . . ?
N6 C29 C33 C32 176.8(7) . . . . ?
C7 N2 C10 C9 0.7(9) . . . . ?
C7 N2 C10 C11 -177.6(7) . . . . ?
C7 C8 C9 C10 -0.7(10) . . . . ?
N7 C36 C37 O2 164.4(8) . . . . ?
N7 C36 C37 N8 -18.6(11) . . . . ?
C8 C9 C10 N2 0.0(9) . . . . ?
C8 C9 C10 C11 178.2(8) . . . . ?
N8 C38 C39 C40 67.5(9) . . . . ?
C9 C10 C11 C12 99.7(10) . . . . ?
C9 C10 C11 C40 -137.1(9) . . . . ?
C9 C10 C11 C41 -20.1(12) . . . . ?
C10 N2 C7 C6 -179.3(8) . . . . ?
C10 N2 C7 C8 -1.2(10) . . . . ?
C10 C11 C12 N3 56.5(10) . . . . ?
C10 C11 C12 C13 -124.9(9) . . . . ?
C10 C11 C40 C39 -173.5(7) . . . . ?
C11 C12 C13 C14 -178.4(8) . . . . ?
C12 N3 C15 C14 1.1(9) . . . . ?
C12 N3 C15 C16 -175.2(7) . . . . ?
C12 C11 C40 C39 -50.0(10) . . . . ?
C12 C13 C14 C15 0.2(10) . . . . ?
C13 C14 C15 N3 -0.8(9) . . . . ?
C13 C14 C15 C16 175.2(8) . . . . ?
C14 C15 C16 C17 128.0(9) . . . . ?
C14 C15 C16 C42 8.3(12) . . . . ?
C14 C15 C16 C43 -109.6(10) . . . . ?
C15 N3 C12 C11 178.0(7) . . . . ?
C15 N3 C12 C13 -1.0(9) . . . . ?
C15 C16 C17 N4 73.9(10) . . . . ?
C15 C16 C17 C18 -111.0(10) . . . . ?
C16 C17 C18 C19 -175.1(8) . . . . ?
C17 N4 C20 C1 179.1(7) . . . . ?
C17 N4 C20 C19 0.3(9) . . . . ?
C17 C18 C19 C20 -0.4(10) . . . . ?
C18 C19 C20 C1 -178.6(8) . . . . ?
C18 C19 C20 N4 0.0(9) . . . . ?
C20 C1 C2 N1 74.6(10) . . . . ?
C20 C1 C2 C3 -109.6(10) . . . . ?
C20 C1 C21 C22 53.1(10) . . . . ?
C20 N4 C17 C16 175.5(7) . . . . ?
C20 N4 C17 C18 -0.5(9) . . . . ?
C21 C1 C2 N1 -49.1(10) . . . . ?
C21 C1 C2 C3 126.7(10) . . . . ?
C21 C1 C20 N4 47.4(10) . . . . ?
C21 C1 C20 C19 -134.1(9) . . . . ?
C21 C22 C23 N5 -52.5(10) . . . . ?
C23 N5 C24 O1 -0.7(13) . . . . ?
C23 N5 C24 C25 -178.1(7) . . . . ?
C24 N5 C23 C22 -73.1(10) . . . . ?
C24 C25 C26 C27 -174.2(7) . . . . ?
C25 N6 C29 C28 -1.2(11) . . . . ?
C25 N6 C29 C33 179.5(7) . . . . ?
C25 C26 C27 C28 -1.1(13) . . . . ?
C26 C27 C28 C29 -0.9(12) . . . . ?
C26 C27 C28 C30 178.8(8) . . . . ?
C27 C28 C29 N6 2.1(11) . . . . ?
C27 C28 C29 C33 -178.6(7) . . . . ?
C27 C28 C30 C31 -179.8(8) . . . . ?
C28 C29 C33 N7 176.7(7) . . . . ?
C28 C29 C33 C32 -2.5(11) . . . . ?
C28 C30 C31 C32 -0.8(13) . . . . ?
C29 N6 C25 C24 175.3(7) . . . . ?
C29 N6 C25 C26 -0.9(12) . . . . ?
C29 C28 C30 C31 -0.2(12) . . . . ?
C30 C28 C29 N6 -177.5(7) . . . . ?
C30 C28 C29 C33 1.8(11) . . . . ?
C30 C31 C32 C33 0.1(12) . . . . ?
C30 C31 C32 C34 179.8(8) . . . . ?
C31 C32 C33 N7 -177.6(7) . . . . ?
C31 C32 C33 C29 1.5(12) . . . . ?
C31 C32 C34 C35 179.2(8) . . . . ?
C32 C34 C35 C36 -1.4(13) . . . . ?
C33 N7 C36 C35 -1.1(12) . . . . ?
C33 N7 C36 C37 176.6(6) . . . . ?
C33 C32 C34 C35 -1.1(12) . . . . ?
C34 C32 C33 N7 2.7(12) . . . . ?
C34 C32 C33 C29 -178.2(7) . . . . ?
C34 C35 C36 N7 2.6(13) . . . . ?
C34 C35 C36 C37 -175.1(7) . . . . ?
C35 C36 C37 O2 -17.6(12) . . . . ?
C35 C36 C37 N8 159.4(7) . . . . ?
C36 N7 C33 C29 179.2(7) . . . . ?
C36 N7 C33 C32 -1.6(11) . . . . ?
C37 N8 C38 C39 77.9(9) . . . . ?
C38 N8 C37 O2 -0.6(12) . . . . ?
C38 N8 C37 C36 -177.6(7) . . . . ?
C38 C39 C40 C11 103.6(8) . . . . ?
C40 C11 C12 N3 -64.8(10) . . . . ?
C40 C11 C12 C13 113.9(9) . . . . ?
C41 C11 C12 N3 175.2(7) . . . . ?
C41 C11 C12 C13 -6.1(12) . . . . ?
C41 C11 C40 C39 70.2(9) . . . . ?
C42 C16 C17 N4 -165.9(7) . . . . ?
C42 C16 C17 C18 9.2(12) . . . . ?
C43 C16 C17 N4 -48.0(10) . . . . ?
C43 C16 C17 C18 127.1(9) . . . . ?
C44 C1 C2 N1 -166.7(7) . . . . ?
C44 C1 C2 C3 9.1(12) . . . . ?
C44 C1 C20 N4 166.1(7) . . . . ?
C44 C1 C20 C19 -15.5(12) . . . . ?
C44 C1 C21 C22 -65.2(9) . . . . ?
C45 C6 C7 N2 -158.5(7) . . . . ?
C45 C6 C7 C8 23.9(13) . . . . ?
C46 C6 C7 N2 -40.5(11) . . . . ?
C46 C6 C7 C8 141.9(9) . . . . ?
N9 C48 C49 C50 -177.5(7) . . . . ?
N9 C52 C53 C54 -179.1(7) . . . . ?
N9 C56 C57 C58 -179.9(9) . . . . ?
N9 C60 C61 C62 -169.9(8) . . . . ?
C48 N9 C52 C53 52.4(10) . . . . ?
C48 N9 C56 C57 -57.9(10) . . . . ?
C48 N9 C60 C61 -178.2(8) . . . . ?
C48 C49 C50 C51 176.4(8) . . . . ?
C52 N9 C48 C49 56.2(9) . . . . ?
C52 N9 C56 C57 -179.6(8) . . . . ?
C52 N9 C60 C61 -57.2(10) . . . . ?
C52 C53 C54 C55 171.8(7) . . . . ?
C56 N9 C48 C49 -62.0(9) . . . . ?
C56 N9 C52 C53 174.7(7) . . . . ?
C56 N9 C60 C61 58.6(10) . . . . ?
C56 C57 C58 C59 -176.5(11) . . . . ?
C60 N9 C48 C49 175.6(7) . . . . ?
C60 N9 C52 C53 -65.9(9) . . . . ?
C60 N9 C56 C57 62.3(10) . . . . ?
C60 C61 C62 C63 179.1(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_THETM01_2-TBACl             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: This may caused by the weak diffraction at high angles.
;
# end Validation Reply Form
