# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_A
_database_code_depnum_ccdc_archive 'CCDC 2303849'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2023-10-26 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H35 N9 O4'
_chemical_formula_weight         621.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0. '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'

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

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

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

_cell_length_a                   19.0635(2)
_cell_length_b                   15.8724(2)
_cell_length_c                   21.4307(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.9570(10)
_cell_angle_gamma                90
_cell_volume                     6480.79(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10348
_cell_measurement_theta_min      2.319
_cell_measurement_theta_max      62.499

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             2624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.711
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.79129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            56351
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.319
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_full        62.499
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10348
_reflns_number_gt                8930
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_structure_solution    'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0761P)²+4.7571P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10348
_refine_ls_number_parameters     883
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.1355
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.74023(10) 0.39696(12) 0.43998(9) 0.0250(4) Uani 1 1 d . . . . .
C2 C 0.76072(10) 0.38269(12) 0.50213(9) 0.0248(4) Uani 1 1 d . . . . .
C3 C 0.72503(11) 0.41937(13) 0.55034(10) 0.0284(5) Uani 1 1 d . . . . .
H3A H 0.740534 0.409338 0.592287 0.034 Uiso 1 1 calc R U . . .
C4 C 0.66688(11) 0.47066(13) 0.53850(10) 0.0318(5) Uani 1 1 d D . . . .
C5 C 0.64638(11) 0.48334(13) 0.47606(10) 0.0305(5) Uani 1 1 d . . . . .
H5A H 0.606548 0.517590 0.466621 0.037 Uiso 1 1 calc R U . . .
C6 C 0.68200(11) 0.44781(13) 0.42744(10) 0.0273(5) Uani 1 1 d . . . . .
C7 C 0.68524(14) 0.54396(15) 0.33631(12) 0.0437(6) Uani 1 1 d . . . . .
H7A H 0.722403 0.568120 0.363504 0.066 Uiso 1 1 calc R U . . .
H7B H 0.703973 0.531658 0.295279 0.066 Uiso 1 1 calc R U . . .
H7C H 0.646494 0.584288 0.331555 0.066 Uiso 1 1 calc R U . . .
C8 C 0.60804(10) 0.42075(13) 0.33528(9) 0.0249(4) Uani 1 1 d . . . . .
C9 C 0.53185(10) 0.40292(14) 0.25559(9) 0.0282(5) Uani 1 1 d . . . . .
C10 C 0.53534(10) 0.30940(13) 0.33391(9) 0.0237(4) Uani 1 1 d . . . . .
C11 C 0.59878(10) 0.17006(12) 0.42597(9) 0.0220(4) Uani 1 1 d . . . . .
H11A H 0.628280 0.165375 0.391296 0.026 Uiso 1 1 calc R U . . .
C12 C 0.53294(10) 0.20703(12) 0.41923(9) 0.0242(4) Uani 1 1 d . . . . .
C13 C 0.48940(11) 0.20978(15) 0.46935(10) 0.0350(5) Uani 1 1 d . . . . .
H13A H 0.443617 0.232970 0.464327 0.042 Uiso 1 1 calc R U . . .
C14 C 0.51226(12) 0.17885(18) 0.52686(11) 0.0426(6) Uani 1 1 d . . . . .
H14A H 0.482153 0.181328 0.561233 0.051 Uiso 1 1 calc R U . . .
C15 C 0.57865(11) 0.14433(15) 0.53472(10) 0.0323(5) Uani 1 1 d . . . . .
H15A H 0.594803 0.123940 0.574341 0.039 Uiso 1 1 calc R U . . .
C16 C 0.62066(10) 0.14019(12) 0.48404(9) 0.0221(4) Uani 1 1 d . . . . .
C17 C 0.74546(10) 0.13250(12) 0.49983(8) 0.0191(4) Uani 1 1 d . . . . .
C18 C 0.85964(10) 0.11587(12) 0.51696(8) 0.0216(4) Uani 1 1 d . . . . .
C19 C 0.81386(10) 0.24539(12) 0.51144(8) 0.0203(4) Uani 1 1 d . . . . .
C20 C 0.88859(11) 0.37002(14) 0.52322(11) 0.0338(5) Uani 1 1 d . . . . .
H20A H 0.882489 0.431214 0.525839 0.051 Uiso 1 1 calc R U . . .
H20B H 0.912619 0.349579 0.561441 0.051 Uiso 1 1 calc R U . . .
H20C H 0.916723 0.356383 0.487151 0.051 Uiso 1 1 calc R U . . .
C21 C 0.62579(12) 0.51108(16) 0.59132(11) 0.0439(6) Uani 1 1 d D . . . .
C22 C 0.6292(4) 0.4533(4) 0.6532(3) 0.0627(16) Uani 0.5 1 d D U P A 1
H22A H 0.678340 0.441139 0.664861 0.094 Uiso 0.5 1 calc R U P A 1
H22B H 0.607231 0.483173 0.687412 0.094 Uiso 0.5 1 calc R U P A 1
H22C H 0.604179 0.400290 0.644885 0.094 Uiso 0.5 1 calc R U P A 1
C23 C 0.6642(4) 0.5912(4) 0.6147(3) 0.078(2) Uani 0.5 1 d D U P A 1
H23A H 0.714045 0.578663 0.622339 0.117 Uiso 0.5 1 calc R U P A 1
H23B H 0.659169 0.635535 0.582962 0.117 Uiso 0.5 1 calc R U P A 1
H23C H 0.643665 0.610426 0.653488 0.117 Uiso 0.5 1 calc R U P A 1
C24 C 0.5495(3) 0.5249(7) 0.5785(3) 0.079(3) Uani 0.5 1 d D U P A 1
H24A H 0.528734 0.550787 0.615077 0.119 Uiso 0.5 1 calc R U P A 1
H24B H 0.542895 0.562305 0.542397 0.119 Uiso 0.5 1 calc R U P A 1
H24C H 0.526555 0.470764 0.569625 0.119 Uiso 0.5 1 calc R U P A 1
C22A C 0.6648(3) 0.5109(4) 0.6508(2) 0.0569(16) Uani 0.5 1 d D U P A 2
H22D H 0.708379 0.542939 0.646847 0.085 Uiso 0.5 1 calc R U P A 2
H22E H 0.636324 0.536887 0.682773 0.085 Uiso 0.5 1 calc R U P A 2
H22F H 0.676031 0.452754 0.662828 0.085 Uiso 0.5 1 calc R U P A 2
C23A C 0.6096(4) 0.6045(3) 0.5700(3) 0.0650(18) Uani 0.5 1 d D U P A 2
H23D H 0.583308 0.603828 0.529854 0.097 Uiso 0.5 1 calc R U P A 2
H23E H 0.581641 0.632562 0.601367 0.097 Uiso 0.5 1 calc R U P A 2
H23F H 0.653802 0.635033 0.565382 0.097 Uiso 0.5 1 calc R U P A 2
C24A C 0.5563(3) 0.4626(5) 0.5918(3) 0.0599(17) Uani 0.5 1 d D U P A 2
H24D H 0.533105 0.465568 0.550282 0.090 Uiso 0.5 1 calc R U P A 2
H24E H 0.565466 0.403602 0.602668 0.090 Uiso 0.5 1 calc R U P A 2
H24F H 0.525759 0.487735 0.622613 0.090 Uiso 0.5 1 calc R U P A 2
C25 C 0.74683(10) 0.29274(13) 0.36049(9) 0.0244(4) Uani 1 1 d . . . . .
H25A H 0.698951 0.284106 0.375822 0.029 Uiso 1 1 calc R U . . .
H25B H 0.774238 0.240841 0.369250 0.029 Uiso 1 1 calc R U . . .
C26 C 0.74261(11) 0.30796(14) 0.29126(9) 0.0282(5) Uani 1 1 d . . . . .
C27 C 0.77809(12) 0.37274(18) 0.26289(11) 0.0429(6) Uani 1 1 d . . . . .
H27A H 0.806537 0.409841 0.287635 0.052 Uiso 1 1 calc R U . . .
C28 C 0.77267(14) 0.3841(2) 0.19898(12) 0.0572(8) Uani 1 1 d . . . . .
H28A H 0.797232 0.429025 0.180144 0.069 Uiso 1 1 calc R U . . .
C29 C 0.73216(17) 0.3312(2) 0.16282(12) 0.0630(9) Uani 1 1 d . . . . .
H29A H 0.728766 0.339089 0.118875 0.076 Uiso 1 1 calc R U . . .
C30 C 0.69592(19) 0.2658(2) 0.19025(13) 0.0670(9) Uani 1 1 d . . . . .
H30A H 0.667605 0.229033 0.165139 0.080 Uiso 1 1 calc R U . . .
C31 C 0.70117(15) 0.25439(17) 0.25455(11) 0.0477(6) Uani 1 1 d . . . . .
H31A H 0.676307 0.209762 0.273394 0.057 Uiso 1 1 calc R U . . .
C32 C 0.52222(15) 0.50353(17) 0.17388(12) 0.0476(7) Uani 1 1 d . . . . .
H32A H 0.495475 0.513211 0.134669 0.071 Uiso 1 1 calc R U . . .
H32B H 0.513864 0.550012 0.202801 0.071 Uiso 1 1 calc R U . . .
H32C H 0.572374 0.500482 0.165529 0.071 Uiso 1 1 calc R U . . .
C33 C 0.90811(11) -0.02158(13) 0.52620(10) 0.0296(5) Uani 1 1 d . . . . .
H33A H 0.953932 -0.049093 0.531628 0.044 Uiso 1 1 calc R U . . .
H33B H 0.878749 -0.036249 0.561254 0.044 Uiso 1 1 calc R U . . .
H33C H 0.885206 -0.040633 0.487067 0.044 Uiso 1 1 calc R U . . .
C34 C 0.09839(10) 0.27675(12) 0.20344(9) 0.0219(4) Uani 1 1 d . . . . .
C35 C 0.06895(10) 0.31594(12) 0.15079(9) 0.0222(4) Uani 1 1 d . . . . .
C36 C 0.07441(10) 0.28052(12) 0.09194(9) 0.0232(4) Uani 1 1 d . . . . .
H36A H 0.052832 0.307912 0.056847 0.028 Uiso 1 1 calc R U . . .
C37 C 0.11082(10) 0.20577(12) 0.08333(9) 0.0243(4) Uani 1 1 d . . . . .
C38 C 0.13959(10) 0.16653(12) 0.13676(9) 0.0236(4) Uani 1 1 d . . . . .
H38A H 0.163968 0.114773 0.132421 0.028 Uiso 1 1 calc R U . . .
C39 C 0.13364(9) 0.20079(12) 0.19581(9) 0.0212(4) Uani 1 1 d . . . . .
C40 C 0.11578(11) 0.11088(15) 0.28839(10) 0.0331(5) Uani 1 1 d . . . . .
H40A H 0.069885 0.105998 0.266673 0.050 Uiso 1 1 calc R U . . .
H40B H 0.134984 0.054498 0.296433 0.050 Uiso 1 1 calc R U . . .
H40C H 0.110477 0.140434 0.328101 0.050 Uiso 1 1 calc R U . . .
C41 C 0.23051(10) 0.17435(12) 0.26814(8) 0.0197(4) Uani 1 1 d . . . . .
C42 C 0.32212(10) 0.15452(12) 0.33382(8) 0.0200(4) Uani 1 1 d . . . . .
C43 C 0.33195(10) 0.24273(12) 0.25357(9) 0.0218(4) Uani 1 1 d . . . . .
C44 C 0.30686(10) 0.41767(13) 0.17659(9) 0.0230(4) Uani 1 1 d . . . . .
H44A H 0.307438 0.444130 0.216368 0.028 Uiso 1 1 calc R U . . .
C45 C 0.34008(10) 0.34076(13) 0.16850(9) 0.0243(4) Uani 1 1 d . . . . .
C46 C 0.34109(10) 0.30372(13) 0.11029(9) 0.0264(4) Uani 1 1 d . . . . .
H46A H 0.364564 0.251541 0.104976 0.032 Uiso 1 1 calc R U . . .
C47 C 0.30779(11) 0.34278(13) 0.05960(9) 0.0268(4) Uani 1 1 d . . . . .
H47A H 0.308988 0.317615 0.019429 0.032 Uiso 1 1 calc R U . . .
C48 C 0.27263(10) 0.41863(12) 0.06725(9) 0.0232(4) Uani 1 1 d . . . . .
H48A H 0.248773 0.445017 0.032856 0.028 Uiso 1 1 calc R U . . .
C49 C 0.27308(10) 0.45486(12) 0.12590(9) 0.0207(4) Uani 1 1 d . . . . .
C50 C 0.16937(10) 0.53319(12) 0.13733(8) 0.0194(4) Uani 1 1 d . . . . .
C51 C 0.07172(10) 0.60707(12) 0.14449(8) 0.0216(4) Uani 1 1 d . . . . .
C52 C 0.06747(10) 0.46688(12) 0.14931(8) 0.0199(4) Uani 1 1 d . . . . .
C53 C -0.04168(10) 0.39029(13) 0.17152(10) 0.0276(4) Uani 1 1 d . . . . .
H53A H -0.056167 0.331264 0.174783 0.041 Uiso 1 1 calc R U . . .
H53B H -0.048825 0.418930 0.211310 0.041 Uiso 1 1 calc R U . . .
H53C H -0.069799 0.418068 0.138367 0.041 Uiso 1 1 calc R U . . .
C54 C 0.11951(12) 0.16756(14) 0.01820(10) 0.0328(5) Uani 1 1 d . . . . .
C55 C 0.1377(6) 0.2439(6) -0.0303(4) 0.0320(19) Uani 0.25 1 d . U P B 1
H55A H 0.177581 0.276555 -0.013320 0.048 Uiso 0.25 1 calc R U P B 1
H55B H 0.149631 0.219896 -0.070720 0.048 Uiso 0.25 1 calc R U P B 1
H55C H 0.096751 0.280803 -0.035839 0.048 Uiso 0.25 1 calc R U P B 1
C56 C 0.1963(14) 0.1163(13) 0.0184(10) 0.054(6) Uani 0.25 1 d . U P B 1
H56A H 0.233485 0.152864 0.035884 0.080 Uiso 0.25 1 calc R U P B 1
H56B H 0.193226 0.065268 0.043947 0.080 Uiso 0.25 1 calc R U P B 1
H56C H 0.207260 0.100705 -0.024414 0.080 Uiso 0.25 1 calc R U P B 1
C57 C 0.0640(6) 0.1220(9) -0.0053(5) 0.044(3) Uani 0.25 1 d . U P B 1
H57A H 0.074929 0.100592 -0.046760 0.065 Uiso 0.25 1 calc R U P B 1
H57B H 0.054954 0.074580 0.022561 0.065 Uiso 0.25 1 calc R U P B 1
H57C H 0.022370 0.158094 -0.008616 0.065 Uiso 0.25 1 calc R U P B 1
C55A C 0.0835(2) 0.2217(2) -0.03297(15) 0.0472(9) Uani 0.75 1 d . U P B 2
H55D H 0.034447 0.231491 -0.022617 0.071 Uiso 0.75 1 calc R U P B 2
H55E H 0.107842 0.275885 -0.035806 0.071 Uiso 0.75 1 calc R U P B 2
H55F H 0.085105 0.192365 -0.073120 0.071 Uiso 0.75 1 calc R U P B 2
C56A C 0.1932(4) 0.1503(4) 0.0058(3) 0.0522(16) Uani 0.75 1 d . U P B 2
H56D H 0.196672 0.126074 -0.036009 0.078 Uiso 0.75 1 calc R U P B 2
H56E H 0.220081 0.202940 0.008316 0.078 Uiso 0.75 1 calc R U P B 2
H56F H 0.212288 0.110407 0.036915 0.078 Uiso 0.75 1 calc R U P B 2
C57A C 0.0786(2) 0.0812(2) 0.01653(19) 0.0410(8) Uani 0.75 1 d . U P B 2
H57D H 0.029005 0.091298 0.024712 0.062 Uiso 0.75 1 calc R U P B 2
H57E H 0.082471 0.055229 -0.024687 0.062 Uiso 0.75 1 calc R U P B 2
H57F H 0.098787 0.043438 0.048539 0.062 Uiso 0.75 1 calc R U P B 2
C58 C 0.14593(11) 0.36922(13) 0.28200(9) 0.0271(4) Uani 1 1 d . . . . .
H58A H 0.180465 0.374681 0.248778 0.032 Uiso 1 1 calc R U . . .
H58B H 0.170722 0.346903 0.319837 0.032 Uiso 1 1 calc R U . . .
C59 C 0.11563(11) 0.45489(13) 0.29611(9) 0.0242(4) Uani 1 1 d . . . . .
C60 C 0.04839(11) 0.46365(14) 0.31782(10) 0.0307(5) Uani 1 1 d . . . . .
H60A H 0.020691 0.414937 0.324529 0.037 Uiso 1 1 calc R U . . .
C61 C 0.02115(13) 0.54259(16) 0.32984(11) 0.0396(6) Uani 1 1 d . . . . .
H61A H -0.025107 0.547645 0.344562 0.048 Uiso 1 1 calc R U . . .
C62 C 0.06082(15) 0.61413(15) 0.32057(11) 0.0429(6) Uani 1 1 d . . . . .
H62A H 0.041791 0.668256 0.328480 0.051 Uiso 1 1 calc R U . . .
C63 C 0.12788(14) 0.60648(14) 0.29985(10) 0.0399(6) Uani 1 1 d . . . . .
H63A H 0.155568 0.655386 0.293822 0.048 Uiso 1 1 calc R U . . .
C64 C 0.15536(12) 0.52707(14) 0.28765(9) 0.0303(5) Uani 1 1 d . . . . .
H64A H 0.201827 0.522238 0.273370 0.036 Uiso 1 1 calc R U . . .
C65 C 0.31604(12) 0.05486(13) 0.41536(9) 0.0288(5) Uani 1 1 d . . . . .
H65A H 0.344188 0.034013 0.451235 0.043 Uiso 1 1 calc R U . . .
H65B H 0.271776 0.078002 0.429785 0.043 Uiso 1 1 calc R U . . .
H65C H 0.306124 0.008380 0.386276 0.043 Uiso 1 1 calc R U . . .
C66 C 0.07428(12) 0.75617(13) 0.14182(12) 0.0376(5) Uani 1 1 d . . . . .
H66A H 0.041944 0.804118 0.142835 0.056 Uiso 1 1 calc R U . . .
H66B H 0.107842 0.759667 0.177399 0.056 Uiso 1 1 calc R U . . .
H66C H 0.099691 0.757377 0.102849 0.056 Uiso 1 1 calc R U . . .
N1 N 0.65964(9) 0.46611(11) 0.36406(8) 0.0290(4) Uani 1 1 d . . . . .
N2 N 0.58668(8) 0.35088(10) 0.36455(7) 0.0230(4) Uani 1 1 d . . . . .
N3 N 0.58255(9) 0.45021(11) 0.27984(8) 0.0285(4) Uani 1 1 d . . . . .
N4 N 0.50543(9) 0.33283(11) 0.27873(8) 0.0284(4) Uani 1 1 d . . . . .
H4A H 0.471412 0.304159 0.259784 0.034 Uiso 1 1 calc R U . . .
N5 N 0.50910(9) 0.23858(11) 0.35970(8) 0.0263(4) Uani 1 1 d . . . . .
H5B H 0.475928 0.210783 0.338874 0.032 Uiso 1 1 calc R U . . .
N6 N 0.74810(8) 0.21499(10) 0.50021(7) 0.0203(3) Uani 1 1 d . . . . .
N7 N 0.79818(8) 0.07786(10) 0.50909(7) 0.0207(3) Uani 1 1 d . . . . .
N8 N 0.87216(8) 0.19856(10) 0.51899(7) 0.0239(4) Uani 1 1 d . . . . .
N9 N 0.82005(9) 0.32970(10) 0.51613(8) 0.0255(4) Uani 1 1 d . . . . .
N10 N 0.16347(8) 0.15816(10) 0.24959(7) 0.0230(4) Uani 1 1 d . . . . .
N11 N 0.26590(8) 0.22885(10) 0.23346(7) 0.0217(3) Uani 1 1 d . . . . .
N12 N 0.25621(8) 0.13462(10) 0.31993(7) 0.0207(3) Uani 1 1 d . . . . .
N13 N 0.36417(8) 0.20677(10) 0.30436(7) 0.0225(4) Uani 1 1 d . . . . .
N14 N 0.37071(9) 0.29792(11) 0.22159(8) 0.0287(4) Uani 1 1 d . . . . .
N15 N 0.13744(8) 0.46021(10) 0.14145(7) 0.0202(3) Uani 1 1 d . . . . .
N16 N 0.14092(8) 0.61038(10) 0.13772(7) 0.0219(3) Uani 1 1 d . . . . .
N17 N 0.03148(8) 0.53945(10) 0.15079(7) 0.0220(3) Uani 1 1 d . . . . .
N18 N 0.03236(8) 0.39419(10) 0.15676(8) 0.0239(4) Uani 1 1 d . . . . .
O1 O 0.68332(7) 0.09350(8) 0.49031(6) 0.0228(3) Uani 1 1 d . . . . .
O2 O 0.77964(7) 0.36304(9) 0.39357(6) 0.0288(3) Uani 1 1 d . . . . .
O3 O 0.50009(8) 0.42554(10) 0.20127(7) 0.0378(4) Uani 1 1 d . . . . .
O4 O 0.91761(7) 0.06886(9) 0.52422(6) 0.0276(3) Uani 1 1 d . . . . .
O5 O 0.24011(7) 0.53383(8) 0.13356(6) 0.0218(3) Uani 1 1 d . . . . .
O6 O 0.09125(7) 0.31098(9) 0.26201(6) 0.0282(3) Uani 1 1 d . . . . .
O7 O 0.35417(7) 0.11957(8) 0.38428(6) 0.0232(3) Uani 1 1 d . . . . .
O8 O 0.03520(7) 0.67896(8) 0.14533(7) 0.0288(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.376(3) . ?
C1 C6 1.391(3) . ?
C1 C2 1.394(3) . ?
C2 C3 1.385(3) . ?
C2 N9 1.433(3) . ?
C3 C4 1.392(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.396(3) . ?
C4 C21 1.539(3) . ?
C5 C6 1.383(3) . ?
C5 H5A 0.9500 . ?
C6 N1 1.439(3) . ?
C7 N1 1.462(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N2 1.344(3) . ?
C8 N1 1.351(3) . ?
C8 N3 1.352(3) . ?
C9 N3 1.316(3) . ?
C9 N4 1.325(3) . ?
C9 O3 1.343(2) . ?
C10 N2 1.334(3) . ?
C10 N4 1.348(3) . ?
C10 N5 1.356(3) . ?
C11 C16 1.383(3) . ?
C11 C12 1.389(3) . ?
C11 H11A 0.9500 . ?
C12 C13 1.380(3) . ?
C12 N5 1.430(2) . ?
C13 C14 1.383(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.384(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.373(3) . ?
C15 H15A 0.9500 . ?
C16 O1 1.408(2) . ?
C17 N6 1.310(3) . ?
C17 N7 1.337(2) . ?
C17 O1 1.346(2) . ?
C18 N7 1.323(3) . ?
C18 N8 1.334(3) . ?
C18 O4 1.338(2) . ?
C19 N8 1.342(3) . ?
C19 N9 1.347(3) . ?
C19 N6 1.357(2) . ?
C20 N9 1.458(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22A 1.454(5) . ?
C21 C24 1.487(5) . ?
C21 C24A 1.533(6) . ?
C21 C23 1.542(5) . ?
C21 C23A 1.579(5) . ?
C21 C22 1.612(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25 O2 1.452(2) . ?
C25 C26 1.503(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.383(3) . ?
C26 C31 1.387(3) . ?
C27 C28 1.382(4) . ?
C27 H27A 0.9500 . ?
C28 C29 1.364(5) . ?
C28 H28A 0.9500 . ?
C29 C30 1.388(5) . ?
C29 H29A 0.9500 . ?
C30 C31 1.390(4) . ?
C30 H30A 0.9500 . ?
C31 H31A 0.9500 . ?
C32 O3 1.439(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 O4 1.448(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 O6 1.378(2) . ?
C34 C35 1.390(3) . ?
C34 C39 1.393(3) . ?
C35 C36 1.388(3) . ?
C35 N18 1.432(3) . ?
C36 C37 1.390(3) . ?
C36 H36A 0.9500 . ?
C37 C38 1.399(3) . ?
C37 C54 1.536(3) . ?
C38 C39 1.385(3) . ?
C38 H38A 0.9500 . ?
C39 N10 1.437(2) . ?
C40 N10 1.460(3) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 N11 1.338(2) . ?
C41 N10 1.350(2) . ?
C41 N12 1.354(2) . ?
C42 N12 1.320(2) . ?
C42 N13 1.328(3) . ?
C42 O7 1.344(2) . ?
C43 N11 1.335(2) . ?
C43 N14 1.348(3) . ?
C43 N13 1.357(2) . ?
C44 C49 1.377(3) . ?
C44 C45 1.389(3) . ?
C44 H44A 0.9500 . ?
C45 C46 1.380(3) . ?
C45 N14 1.433(2) . ?
C46 C47 1.386(3) . ?
C46 H46A 0.9500 . ?
C47 C48 1.390(3) . ?
C47 H47A 0.9500 . ?
C48 C49 1.382(3) . ?
C48 H48A 0.9500 . ?
C49 O5 1.414(2) . ?
C50 N15 1.313(2) . ?
C50 N16 1.340(2) . ?
C50 O5 1.354(2) . ?
C51 N17 1.329(3) . ?
C51 N16 1.333(3) . ?
C51 O8 1.337(2) . ?
C52 N17 1.342(2) . ?
C52 N18 1.346(3) . ?
C52 N15 1.354(2) . ?
C53 N18 1.458(3) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C57 1.363(11) . ?
C54 C56A 1.465(7) . ?
C54 C55A 1.537(4) . ?
C54 C57A 1.577(4) . ?
C54 C55 1.641(9) . ?
C54 C56 1.68(2) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C55A H55D 0.9800 . ?
C55A H55E 0.9800 . ?
C55A H55F 0.9800 . ?
C56A H56D 0.9800 . ?
C56A H56E 0.9800 . ?
C56A H56F 0.9800 . ?
C57A H57D 0.9800 . ?
C57A H57E 0.9800 . ?
C57A H57F 0.9800 . ?
C58 O6 1.447(2) . ?
C58 C59 1.512(3) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.386(3) . ?
C59 C64 1.389(3) . ?
C60 C61 1.384(3) . ?
C60 H60A 0.9500 . ?
C61 C62 1.382(4) . ?
C61 H61A 0.9500 . ?
C62 C63 1.373(4) . ?
C62 H62A 0.9500 . ?
C63 C64 1.393(3) . ?
C63 H63A 0.9500 . ?
C64 H64A 0.9500 . ?
C65 O7 1.435(2) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 O8 1.438(3) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
N4 H4A 0.8800 . ?
N5 H5B 0.8800 . ?

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
O2 C1 C6 122.62(18) . . ?
O2 C1 C2 119.00(18) . . ?
C6 C1 C2 118.33(19) . . ?
C3 C2 C1 121.07(19) . . ?
C3 C2 N9 119.66(17) . . ?
C1 C2 N9 119.27(18) . . ?
C2 C3 C4 121.22(19) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
C3 C4 C5 117.0(2) . . ?
C3 C4 C21 122.15(19) . . ?
C5 C4 C21 120.82(19) . . ?
C6 C5 C4 122.33(19) . . ?
C6 C5 H5A 118.8 . . ?
C4 C5 H5A 118.8 . . ?
C5 C6 C1 120.00(18) . . ?
C5 C6 N1 119.43(18) . . ?
C1 C6 N1 120.54(19) . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 N1 117.00(17) . . ?
N2 C8 N3 126.17(18) . . ?
N1 C8 N3 116.83(17) . . ?
N3 C9 N4 127.91(18) . . ?
N3 C9 O3 119.55(18) . . ?
N4 C9 O3 112.53(17) . . ?
N2 C10 N4 125.25(18) . . ?
N2 C10 N5 118.92(17) . . ?
N4 C10 N5 115.82(17) . . ?
C16 C11 C12 118.83(18) . . ?
C16 C11 H11A 120.6 . . ?
C12 C11 H11A 120.6 . . ?
C13 C12 C11 119.86(18) . . ?
C13 C12 N5 120.12(18) . . ?
C11 C12 N5 119.95(18) . . ?
C12 C13 C14 120.2(2) . . ?
C12 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
C13 C14 C15 120.5(2) . . ?
C13 C14 H14A 119.7 . . ?
C15 C14 H14A 119.7 . . ?
C16 C15 C14 118.57(19) . . ?
C16 C15 H15A 120.7 . . ?
C14 C15 H15A 120.7 . . ?
C15 C16 C11 121.97(18) . . ?
C15 C16 O1 117.74(17) . . ?
C11 C16 O1 119.67(17) . . ?
N6 C17 N7 128.22(17) . . ?
N6 C17 O1 119.59(16) . . ?
N7 C17 O1 112.18(16) . . ?
N7 C18 N8 127.52(17) . . ?
N7 C18 O4 118.99(17) . . ?
N8 C18 O4 113.49(17) . . ?
N8 C19 N9 118.11(17) . . ?
N8 C19 N6 125.49(17) . . ?
N9 C19 N6 116.40(17) . . ?
N9 C20 H20A 109.5 . . ?
N9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22A C21 C24A 114.2(4) . . ?
C22A C21 C4 112.7(3) . . ?
C24 C21 C4 116.4(3) . . ?
C24A C21 C4 104.9(3) . . ?
C24 C21 C23 112.8(5) . . ?
C4 C21 C23 109.6(3) . . ?
C22A C21 C23A 110.2(4) . . ?
C24A C21 C23A 108.2(4) . . ?
C4 C21 C23A 106.1(3) . . ?
C24 C21 C22 104.3(4) . . ?
C4 C21 C22 111.1(3) . . ?
C23 C21 C22 101.4(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C22A H22D 109.5 . . ?
C21 C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21 C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C21 C23A H23D 109.5 . . ?
C21 C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C21 C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C21 C24A H24D 109.5 . . ?
C21 C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C21 C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
O2 C25 C26 111.47(16) . . ?
O2 C25 H25A 109.3 . . ?
C26 C25 H25A 109.3 . . ?
O2 C25 H25B 109.3 . . ?
C26 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
C27 C26 C31 119.0(2) . . ?
C27 C26 C25 122.9(2) . . ?
C31 C26 C25 118.1(2) . . ?
C28 C27 C26 120.8(3) . . ?
C28 C27 H27A 119.6 . . ?
C26 C27 H27A 119.6 . . ?
C29 C28 C27 120.3(3) . . ?
C29 C28 H28A 119.9 . . ?
C27 C28 H28A 119.9 . . ?
C28 C29 C30 120.0(2) . . ?
C28 C29 H29A 120.0 . . ?
C30 C29 H29A 120.0 . . ?
C29 C30 C31 119.8(3) . . ?
C29 C30 H30A 120.1 . . ?
C31 C30 H30A 120.1 . . ?
C26 C31 C30 120.2(3) . . ?
C26 C31 H31A 119.9 . . ?
C30 C31 H31A 119.9 . . ?
O3 C32 H32A 109.5 . . ?
O3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C33 H33A 109.5 . . ?
O4 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O4 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O6 C34 C35 120.87(17) . . ?
O6 C34 C39 120.74(17) . . ?
C35 C34 C39 118.36(17) . . ?
C36 C35 C34 121.05(18) . . ?
C36 C35 N18 118.96(17) . . ?
C34 C35 N18 119.99(17) . . ?
C35 C36 C37 121.30(18) . . ?
C35 C36 H36A 119.4 . . ?
C37 C36 H36A 119.4 . . ?
C36 C37 C38 117.06(18) . . ?
C36 C37 C54 121.83(17) . . ?
C38 C37 C54 121.11(18) . . ?
C39 C38 C37 122.07(18) . . ?
C39 C38 H38A 119.0 . . ?
C37 C38 H38A 119.0 . . ?
C38 C39 C34 120.13(17) . . ?
C38 C39 N10 120.35(17) . . ?
C34 C39 N10 119.52(17) . . ?
N10 C40 H40A 109.5 . . ?
N10 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N10 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N11 C41 N10 116.72(16) . . ?
N11 C41 N12 125.56(17) . . ?
N10 C41 N12 117.72(16) . . ?
N12 C42 N13 128.89(17) . . ?
N12 C42 O7 119.07(16) . . ?
N13 C42 O7 112.04(16) . . ?
N11 C43 N14 118.05(16) . . ?
N11 C43 N13 125.83(17) . . ?
N14 C43 N13 116.11(17) . . ?
C49 C44 C45 118.77(18) . . ?
C49 C44 H44A 120.6 . . ?
C45 C44 H44A 120.6 . . ?
C46 C45 C44 120.52(17) . . ?
C46 C45 N14 119.85(19) . . ?
C44 C45 N14 119.56(18) . . ?
C45 C46 C47 119.86(19) . . ?
C45 C46 H46A 120.1 . . ?
C47 C46 H46A 120.1 . . ?
C46 C47 C48 120.32(19) . . ?
C46 C47 H47A 119.8 . . ?
C48 C47 H47A 119.8 . . ?
C49 C48 C47 118.65(18) . . ?
C49 C48 H48A 120.7 . . ?
C47 C48 H48A 120.7 . . ?
C44 C49 C48 121.84(18) . . ?
C44 C49 O5 119.09(17) . . ?
C48 C49 O5 119.03(16) . . ?
N15 C50 N16 128.14(17) . . ?
N15 C50 O5 118.40(16) . . ?
N16 C50 O5 113.44(16) . . ?
N17 C51 N16 128.30(17) . . ?
N17 C51 O8 112.65(16) . . ?
N16 C51 O8 119.05(17) . . ?
N17 C52 N18 118.45(17) . . ?
N17 C52 N15 125.22(17) . . ?
N18 C52 N15 116.33(16) . . ?
N18 C53 H53A 109.5 . . ?
N18 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
N18 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C57 C54 C37 116.0(5) . . ?
C56A C54 C37 111.8(3) . . ?
C56A C54 C55A 112.6(3) . . ?
C37 C54 C55A 111.6(2) . . ?
C56A C54 C57A 108.1(3) . . ?
C37 C54 C57A 107.2(2) . . ?
C55A C54 C57A 105.1(3) . . ?
C57 C54 C55 109.6(7) . . ?
C37 C54 C55 108.4(3) . . ?
C57 C54 C56 114.2(11) . . ?
C37 C54 C56 108.1(8) . . ?
C55 C54 C56 99.0(8) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C54 C55A H55D 109.5 . . ?
C54 C55A H55E 109.5 . . ?
H55D C55A H55E 109.5 . . ?
C54 C55A H55F 109.5 . . ?
H55D C55A H55F 109.5 . . ?
H55E C55A H55F 109.5 . . ?
C54 C56A H56D 109.5 . . ?
C54 C56A H56E 109.5 . . ?
H56D C56A H56E 109.5 . . ?
C54 C56A H56F 109.5 . . ?
H56D C56A H56F 109.5 . . ?
H56E C56A H56F 109.5 . . ?
C54 C57A H57D 109.5 . . ?
C54 C57A H57E 109.5 . . ?
H57D C57A H57E 109.5 . . ?
C54 C57A H57F 109.5 . . ?
H57D C57A H57F 109.5 . . ?
H57E C57A H57F 109.5 . . ?
O6 C58 C59 110.95(16) . . ?
O6 C58 H58A 109.4 . . ?
C59 C58 H58A 109.4 . . ?
O6 C58 H58B 109.4 . . ?
C59 C58 H58B 109.4 . . ?
H58A C58 H58B 108.0 . . ?
C60 C59 C64 118.43(19) . . ?
C60 C59 C58 121.43(19) . . ?
C64 C59 C58 120.14(18) . . ?
C61 C60 C59 120.7(2) . . ?
C61 C60 H60A 119.6 . . ?
C59 C60 H60A 119.6 . . ?
C62 C61 C60 120.4(2) . . ?
C62 C61 H61A 119.8 . . ?
C60 C61 H61A 119.8 . . ?
C63 C62 C61 119.6(2) . . ?
C63 C62 H62A 120.2 . . ?
C61 C62 H62A 120.2 . . ?
C62 C63 C64 120.1(2) . . ?
C62 C63 H63A 120.0 . . ?
C64 C63 H63A 120.0 . . ?
C59 C64 C63 120.8(2) . . ?
C59 C64 H64A 119.6 . . ?
C63 C64 H64A 119.6 . . ?
O7 C65 H65A 109.5 . . ?
O7 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
O7 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
O8 C66 H66A 109.5 . . ?
O8 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
O8 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C8 N1 C6 120.73(16) . . ?
C8 N1 C7 120.84(17) . . ?
C6 N1 C7 117.52(17) . . ?
C10 N2 C8 113.98(16) . . ?
C9 N3 C8 112.76(17) . . ?
C9 N4 C10 113.92(17) . . ?
C9 N4 H4A 123.0 . . ?
C10 N4 H4A 123.0 . . ?
C10 N5 C12 122.92(16) . . ?
C10 N5 H5B 118.5 . . ?
C12 N5 H5B 118.5 . . ?
C17 N6 C19 113.04(16) . . ?
C18 N7 C17 112.39(16) . . ?
C18 N8 C19 113.22(16) . . ?
C19 N9 C2 120.07(16) . . ?
C19 N9 C20 121.32(17) . . ?
C2 N9 C20 117.52(16) . . ?
C41 N10 C39 119.42(15) . . ?
C41 N10 C40 122.11(16) . . ?
C39 N10 C40 117.49(15) . . ?
C43 N11 C41 114.53(16) . . ?
C42 N12 C41 112.86(16) . . ?
C42 N13 C43 112.33(16) . . ?
C43 N14 C45 119.77(16) . . ?
C50 N15 C52 113.59(16) . . ?
C51 N16 C50 111.53(16) . . ?
C51 N17 C52 113.17(16) . . ?
C52 N18 C35 119.15(15) . . ?
C52 N18 C53 123.43(16) . . ?
C35 N18 C53 117.41(16) . . ?
C17 O1 C16 120.78(15) . . ?
C1 O2 C25 114.62(15) . . ?
C9 O3 C32 116.98(17) . . ?
C18 O4 C33 116.91(15) . . ?
C50 O5 C49 116.60(14) . . ?
C34 O6 C58 115.40(14) . . ?
C42 O7 C65 116.45(15) . . ?
C51 O8 C66 117.11(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C3 176.37(18) . . . . ?
C6 C1 C2 C3 -1.2(3) . . . . ?
O2 C1 C2 N9 -3.1(3) . . . . ?
C6 C1 C2 N9 179.26(17) . . . . ?
C1 C2 C3 C4 1.0(3) . . . . ?
N9 C2 C3 C4 -179.50(18) . . . . ?
C2 C3 C4 C5 0.0(3) . . . . ?
C2 C3 C4 C21 179.1(2) . . . . ?
C3 C4 C5 C6 -0.7(3) . . . . ?
C21 C4 C5 C6 -179.8(2) . . . . ?
C4 C5 C6 C1 0.4(3) . . . . ?
C4 C5 C6 N1 -177.63(19) . . . . ?
O2 C1 C6 C5 -176.97(18) . . . . ?
C2 C1 C6 C5 0.5(3) . . . . ?
O2 C1 C6 N1 1.0(3) . . . . ?
C2 C1 C6 N1 178.56(17) . . . . ?
C16 C11 C12 C13 -3.1(3) . . . . ?
C16 C11 C12 N5 179.89(17) . . . . ?
C11 C12 C13 C14 2.6(3) . . . . ?
N5 C12 C13 C14 179.6(2) . . . . ?
C12 C13 C14 C15 -0.5(4) . . . . ?
C13 C14 C15 C16 -1.1(4) . . . . ?
C14 C15 C16 C11 0.6(3) . . . . ?
C14 C15 C16 O1 -170.4(2) . . . . ?
C12 C11 C16 C15 1.5(3) . . . . ?
C12 C11 C16 O1 172.31(17) . . . . ?
C3 C4 C21 C22A 16.9(5) . . . . ?
C5 C4 C21 C22A -163.9(4) . . . . ?
C3 C4 C21 C24 -149.2(5) . . . . ?
C5 C4 C21 C24 30.0(6) . . . . ?
C3 C4 C21 C24A -107.9(4) . . . . ?
C5 C4 C21 C24A 71.2(4) . . . . ?
C3 C4 C21 C23 81.3(4) . . . . ?
C5 C4 C21 C23 -99.6(4) . . . . ?
C3 C4 C21 C23A 137.6(3) . . . . ?
C5 C4 C21 C23A -43.2(4) . . . . ?
C3 C4 C21 C22 -29.9(4) . . . . ?
C5 C4 C21 C22 149.2(4) . . . . ?
O2 C25 C26 C27 11.9(3) . . . . ?
O2 C25 C26 C31 -168.1(2) . . . . ?
C31 C26 C27 C28 -0.1(4) . . . . ?
C25 C26 C27 C28 179.9(2) . . . . ?
C26 C27 C28 C29 -0.2(4) . . . . ?
C27 C28 C29 C30 0.3(5) . . . . ?
C28 C29 C30 C31 -0.2(5) . . . . ?
C27 C26 C31 C30 0.3(4) . . . . ?
C25 C26 C31 C30 -179.7(2) . . . . ?
C29 C30 C31 C26 -0.1(5) . . . . ?
O6 C34 C35 C36 -178.26(17) . . . . ?
C39 C34 C35 C36 0.0(3) . . . . ?
O6 C34 C35 N18 1.8(3) . . . . ?
C39 C34 C35 N18 -179.92(16) . . . . ?
C34 C35 C36 C37 -1.5(3) . . . . ?
N18 C35 C36 C37 178.39(17) . . . . ?
C35 C36 C37 C38 2.1(3) . . . . ?
C35 C36 C37 C54 -177.77(19) . . . . ?
C36 C37 C38 C39 -1.2(3) . . . . ?
C54 C37 C38 C39 178.62(18) . . . . ?
C37 C38 C39 C34 -0.2(3) . . . . ?
C37 C38 C39 N10 179.51(17) . . . . ?
O6 C34 C39 C38 179.11(17) . . . . ?
C35 C34 C39 C38 0.9(3) . . . . ?
O6 C34 C39 N10 -0.6(3) . . . . ?
C35 C34 C39 N10 -178.88(16) . . . . ?
C49 C44 C45 C46 2.1(3) . . . . ?
C49 C44 C45 N14 -175.09(17) . . . . ?
C44 C45 C46 C47 -1.0(3) . . . . ?
N14 C45 C46 C47 176.13(18) . . . . ?
C45 C46 C47 C48 -0.8(3) . . . . ?
C46 C47 C48 C49 1.5(3) . . . . ?
C45 C44 C49 C48 -1.3(3) . . . . ?
C45 C44 C49 O5 -178.98(16) . . . . ?
C47 C48 C49 C44 -0.4(3) . . . . ?
C47 C48 C49 O5 177.22(17) . . . . ?
C36 C37 C54 C57 -81.4(7) . . . . ?
C38 C37 C54 C57 98.8(7) . . . . ?
C36 C37 C54 C56A 126.9(3) . . . . ?
C38 C37 C54 C56A -52.9(4) . . . . ?
C36 C37 C54 C55A -0.2(3) . . . . ?
C38 C37 C54 C55A 180.0(2) . . . . ?
C36 C37 C54 C57A -114.8(2) . . . . ?
C38 C37 C54 C57A 65.4(3) . . . . ?
C36 C37 C54 C55 42.4(5) . . . . ?
C38 C37 C54 C55 -137.5(4) . . . . ?
C36 C37 C54 C56 148.8(9) . . . . ?
C38 C37 C54 C56 -31.0(9) . . . . ?
O6 C58 C59 C60 30.3(2) . . . . ?
O6 C58 C59 C64 -149.98(17) . . . . ?
C64 C59 C60 C61 1.0(3) . . . . ?
C58 C59 C60 C61 -179.27(19) . . . . ?
C59 C60 C61 C62 -0.2(3) . . . . ?
C60 C61 C62 C63 -0.6(3) . . . . ?
C61 C62 C63 C64 0.7(3) . . . . ?
C60 C59 C64 C63 -0.9(3) . . . . ?
C58 C59 C64 C63 179.34(18) . . . . ?
C62 C63 C64 C59 0.1(3) . . . . ?
N2 C8 N1 C6 -10.0(3) . . . . ?
N3 C8 N1 C6 169.73(19) . . . . ?
N2 C8 N1 C7 -178.8(2) . . . . ?
N3 C8 N1 C7 1.0(3) . . . . ?
C5 C6 N1 C8 -85.5(2) . . . . ?
C1 C6 N1 C8 96.4(2) . . . . ?
C5 C6 N1 C7 83.6(3) . . . . ?
C1 C6 N1 C7 -94.4(2) . . . . ?
N4 C10 N2 C8 -0.4(3) . . . . ?
N5 C10 N2 C8 -179.06(18) . . . . ?
N1 C8 N2 C10 179.54(18) . . . . ?
N3 C8 N2 C10 -0.1(3) . . . . ?
N4 C9 N3 C8 -0.7(3) . . . . ?
O3 C9 N3 C8 178.26(19) . . . . ?
N2 C8 N3 C9 0.6(3) . . . . ?
N1 C8 N3 C9 -179.06(19) . . . . ?
N3 C9 N4 C10 0.2(3) . . . . ?
O3 C9 N4 C10 -178.76(18) . . . . ?
N2 C10 N4 C9 0.4(3) . . . . ?
N5 C10 N4 C9 179.07(18) . . . . ?
N2 C10 N5 C12 1.4(3) . . . . ?
N4 C10 N5 C12 -177.37(18) . . . . ?
C13 C12 N5 C10 110.8(2) . . . . ?
C11 C12 N5 C10 -72.1(3) . . . . ?
N7 C17 N6 C19 0.2(3) . . . . ?
O1 C17 N6 C19 178.88(15) . . . . ?
N8 C19 N6 C17 2.7(2) . . . . ?
N9 C19 N6 C17 -176.28(16) . . . . ?
N8 C18 N7 C17 3.0(3) . . . . ?
O4 C18 N7 C17 -177.35(15) . . . . ?
N6 C17 N7 C18 -2.8(3) . . . . ?
O1 C17 N7 C18 178.45(14) . . . . ?
N7 C18 N8 C19 -0.5(3) . . . . ?
O4 C18 N8 C19 179.76(15) . . . . ?
N9 C19 N8 C18 176.41(16) . . . . ?
N6 C19 N8 C18 -2.6(3) . . . . ?
N8 C19 N9 C2 173.58(17) . . . . ?
N6 C19 N9 C2 -7.3(3) . . . . ?
N8 C19 N9 C20 5.8(3) . . . . ?
N6 C19 N9 C20 -175.12(17) . . . . ?
C3 C2 N9 C19 104.0(2) . . . . ?
C1 C2 N9 C19 -76.5(2) . . . . ?
C3 C2 N9 C20 -87.8(2) . . . . ?
C1 C2 N9 C20 91.7(2) . . . . ?
N11 C41 N10 C39 -1.5(3) . . . . ?
N12 C41 N10 C39 178.33(17) . . . . ?
N11 C41 N10 C40 -169.97(18) . . . . ?
N12 C41 N10 C40 9.9(3) . . . . ?
C38 C39 N10 C41 89.2(2) . . . . ?
C34 C39 N10 C41 -91.1(2) . . . . ?
C38 C39 N10 C40 -101.8(2) . . . . ?
C34 C39 N10 C40 77.9(2) . . . . ?
N14 C43 N11 C41 -179.02(18) . . . . ?
N13 C43 N11 C41 0.2(3) . . . . ?
N10 C41 N11 C43 -179.90(17) . . . . ?
N12 C41 N11 C43 0.2(3) . . . . ?
N13 C42 N12 C41 0.2(3) . . . . ?
O7 C42 N12 C41 179.93(16) . . . . ?
N11 C41 N12 C42 -0.4(3) . . . . ?
N10 C41 N12 C42 179.72(16) . . . . ?
N12 C42 N13 C43 0.1(3) . . . . ?
O7 C42 N13 C43 -179.58(15) . . . . ?
N11 C43 N13 C42 -0.4(3) . . . . ?
N14 C43 N13 C42 178.85(17) . . . . ?
N11 C43 N14 C45 1.2(3) . . . . ?
N13 C43 N14 C45 -178.05(18) . . . . ?
C46 C45 N14 C43 -87.0(2) . . . . ?
C44 C45 N14 C43 90.2(2) . . . . ?
N16 C50 N15 C52 -2.6(3) . . . . ?
O5 C50 N15 C52 175.70(15) . . . . ?
N17 C52 N15 C50 2.3(3) . . . . ?
N18 C52 N15 C50 -177.01(15) . . . . ?
N17 C51 N16 C50 0.4(3) . . . . ?
O8 C51 N16 C50 -179.50(16) . . . . ?
N15 C50 N16 C51 1.4(3) . . . . ?
O5 C50 N16 C51 -177.00(15) . . . . ?
N16 C51 N17 C52 -0.6(3) . . . . ?
O8 C51 N17 C52 179.30(15) . . . . ?
N18 C52 N17 C51 178.42(16) . . . . ?
N15 C52 N17 C51 -0.9(3) . . . . ?
N17 C52 N18 C35 175.50(16) . . . . ?
N15 C52 N18 C35 -5.1(2) . . . . ?
N17 C52 N18 C53 -5.3(3) . . . . ?
N15 C52 N18 C53 174.10(17) . . . . ?
C36 C35 N18 C52 -86.3(2) . . . . ?
C34 C35 N18 C52 93.6(2) . . . . ?
C36 C35 N18 C53 94.4(2) . . . . ?
C34 C35 N18 C53 -85.7(2) . . . . ?
N6 C17 O1 C16 -3.4(2) . . . . ?
N7 C17 O1 C16 175.48(15) . . . . ?
C15 C16 O1 C17 -101.7(2) . . . . ?
C11 C16 O1 C17 87.1(2) . . . . ?
C6 C1 O2 C25 -74.8(2) . . . . ?
C2 C1 O2 C25 107.7(2) . . . . ?
C26 C25 O2 C1 125.05(18) . . . . ?
N3 C9 O3 C32 -2.5(3) . . . . ?
N4 C9 O3 C32 176.6(2) . . . . ?
N7 C18 O4 C33 -3.2(2) . . . . ?
N8 C18 O4 C33 176.54(16) . . . . ?
N15 C50 O5 C49 8.3(2) . . . . ?
N16 C50 O5 C49 -173.16(14) . . . . ?
C44 C49 O5 C50 -102.71(19) . . . . ?
C48 C49 O5 C50 79.6(2) . . . . ?
C35 C34 O6 C58 -90.1(2) . . . . ?
C39 C34 O6 C58 91.7(2) . . . . ?
C59 C58 O6 C34 120.90(18) . . . . ?
N12 C42 O7 C65 7.1(2) . . . . ?
N13 C42 O7 C65 -173.10(16) . . . . ?
N17 C51 O8 C66 177.12(17) . . . . ?
N16 C51 O8 C66 -3.0(3) . . . . ?

_refine_diff_density_max         0.679
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2303851'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2023-10-26 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H43 N9 O4'
_chemical_formula_weight         773.88

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'

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

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

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

_cell_length_a                   10.0108(2)
_cell_length_b                   12.9368(3)
_cell_length_c                   17.2186(4)
_cell_angle_alpha                105.174(2)
_cell_angle_beta                 98.881(2)
_cell_angle_gamma                107.685(2)
_cell_volume                     1983.04(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6323
_cell_measurement_theta_min      2.749
_cell_measurement_theta_max      62.489

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.691
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.77729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            33123
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.749
_diffrn_reflns_theta_max         62.489
_diffrn_reflns_theta_full        62.489
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6323
_reflns_number_gt                6153
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0445P)²+1.2500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0046(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6323
_refine_ls_number_parameters     524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.53041(14) 0.81768(11) 0.36774(8) 0.0172(3) Uani 1 1 d . . . . .
C2 C 0.52264(14) 0.83668(11) 0.29161(8) 0.0171(3) Uani 1 1 d . . . . .
C3 C 0.62650(14) 0.82417(11) 0.24845(8) 0.0181(3) Uani 1 1 d . . . . .
H3A H 0.617995 0.836041 0.196025 0.022 Uiso 1 1 calc R U . . .
C4 C 0.74204(14) 0.79511(12) 0.27862(8) 0.0185(3) Uani 1 1 d . . . . .
C5 C 0.74596(15) 0.77257(12) 0.35377(9) 0.0192(3) Uani 1 1 d . . . . .
H5A H 0.822038 0.750869 0.376079 0.023 Uiso 1 1 calc R U . . .
C6 C 0.64115(15) 0.78120(12) 0.39646(8) 0.0185(3) Uani 1 1 d . . . . .
C7 C 0.75688(16) 0.84891(14) 0.54686(9) 0.0285(4) Uani 1 1 d . . . . .
H7A H 0.833692 0.897157 0.528850 0.043 Uiso 1 1 calc R U . . .
H7B H 0.709599 0.896228 0.577457 0.043 Uiso 1 1 calc R U . . .
H7C H 0.799029 0.813642 0.583104 0.043 Uiso 1 1 calc R U . . .
C8 C 0.53323(15) 0.68185(12) 0.48497(9) 0.0192(3) Uani 1 1 d . . . . .
C9 C 0.40968(15) 0.61322(12) 0.56901(8) 0.0202(3) Uani 1 1 d . . . . .
C10 C 0.32552(15) 0.53162(12) 0.43275(8) 0.0192(3) Uani 1 1 d . . . . .
C11 C 0.18456(15) 0.47962(12) 0.23692(9) 0.0198(3) Uani 1 1 d . . . . .
H11A H 0.154399 0.541761 0.258663 0.024 Uiso 1 1 calc R U . . .
C12 C 0.22784(15) 0.42270(12) 0.28761(8) 0.0202(3) Uani 1 1 d . . . . .
C13 C 0.26856(16) 0.33013(13) 0.25770(9) 0.0261(3) Uani 1 1 d . . . . .
H13A H 0.297042 0.291447 0.293370 0.031 Uiso 1 1 calc R U . . .
C14 C 0.26674(17) 0.29525(14) 0.17435(10) 0.0288(3) Uani 1 1 d . . . . .
H14A H 0.293637 0.231292 0.152463 0.035 Uiso 1 1 calc R U . . .
C15 C 0.22638(16) 0.35192(13) 0.12213(9) 0.0236(3) Uani 1 1 d . . . . .
H15A H 0.226568 0.327312 0.065109 0.028 Uiso 1 1 calc R U . . .
C16 C 0.18575(14) 0.44463(12) 0.15347(8) 0.0185(3) Uani 1 1 d . . . . .
C17 C 0.17373(14) 0.61131(12) 0.11282(8) 0.0167(3) Uani 1 1 d . . . . .
C18 C 0.13378(14) 0.75435(12) 0.07481(8) 0.0169(3) Uani 1 1 d . . . . .
C19 C 0.30540(14) 0.79576(12) 0.18919(8) 0.0159(3) Uani 1 1 d . . . . .
C20 C 0.44023(16) 0.99647(12) 0.27917(9) 0.0241(3) Uani 1 1 d . . . . .
H20A H 0.521621 1.037732 0.328769 0.036 Uiso 1 1 calc R U . . .
H20B H 0.463956 1.023668 0.233187 0.036 Uiso 1 1 calc R U . . .
H20C H 0.353482 1.010495 0.291090 0.036 Uiso 1 1 calc R U . . .
C21 C 0.86246(15) 0.79611(13) 0.23300(9) 0.0217(3) Uani 1 1 d . . . . .
C22 C 0.80154(18) 0.75930(15) 0.13850(10) 0.0305(4) Uani 1 1 d . . . . .
H22A H 0.751900 0.809834 0.125843 0.046 Uiso 1 1 calc R U . . .
H22B H 0.881134 0.764702 0.111175 0.046 Uiso 1 1 calc R U . . .
H22C H 0.732697 0.679865 0.118184 0.046 Uiso 1 1 calc R U . . .
C23 C 0.97401(18) 0.91913(14) 0.26403(12) 0.0361(4) Uani 1 1 d . . . . .
H23A H 0.926148 0.971606 0.253311 0.054 Uiso 1 1 calc R U . . .
H23B H 1.016251 0.941708 0.323923 0.054 Uiso 1 1 calc R U . . .
H23C H 1.050843 0.922613 0.234656 0.054 Uiso 1 1 calc R U . . .
C24 C 0.93900(16) 0.71530(14) 0.25021(10) 0.0268(3) Uani 1 1 d . . . . .
H24A H 0.868695 0.636429 0.230623 0.040 Uiso 1 1 calc R U . . .
H24B H 1.015928 0.719338 0.220878 0.040 Uiso 1 1 calc R U . . .
H24C H 0.981336 0.738433 0.310146 0.040 Uiso 1 1 calc R U . . .
C25 C 0.28974(15) 0.79844(13) 0.38642(9) 0.0213(3) Uani 1 1 d . . . . .
H25A H 0.256526 0.722553 0.342599 0.026 Uiso 1 1 calc R U . . .
H25B H 0.264460 0.852872 0.361338 0.026 Uiso 1 1 calc R U . . .
C26 C 0.21750(14) 0.78901(12) 0.45588(8) 0.0187(3) Uani 1 1 d . . . . .
C27 C 0.25138(16) 0.88525(13) 0.52533(9) 0.0273(3) Uani 1 1 d . . . . .
H27A H 0.321942 0.956025 0.529167 0.033 Uiso 1 1 calc R U . . .
C28 C 0.18310(18) 0.87879(15) 0.58897(10) 0.0346(4) Uani 1 1 d . . . . .
H28A H 0.207111 0.944944 0.636233 0.041 Uiso 1 1 calc R U . . .
C29 C 0.07977(17) 0.77588(15) 0.58375(10) 0.0313(4) Uani 1 1 d . . . . .
H29A H 0.033554 0.771493 0.627631 0.038 Uiso 1 1 calc R U . . .
C30 C 0.04397(16) 0.67987(14) 0.51495(10) 0.0278(3) Uani 1 1 d . . . . .
H30A H -0.027611 0.609543 0.511018 0.033 Uiso 1 1 calc R U . . .
C31 C 0.11317(16) 0.68657(13) 0.45141(9) 0.0231(3) Uani 1 1 d . . . . .
H31A H 0.088863 0.620216 0.404259 0.028 Uiso 1 1 calc R U . . .
C32 C 0.27798(18) 0.53982(14) 0.65800(9) 0.0305(4) Uani 1 1 d . . . . .
H32A H 0.272990 0.461081 0.629597 0.037 Uiso 1 1 calc R U . . .
H32B H 0.186987 0.548218 0.633962 0.037 Uiso 1 1 calc R U . . .
C33 C 0.29774(17) 0.56115(13) 0.74976(9) 0.0287(4) Uani 1 1 d . . . . .
C34 C 0.21283(19) 0.61048(14) 0.79181(10) 0.0328(4) Uani 1 1 d . . . . .
H34A H 0.145543 0.634342 0.762758 0.039 Uiso 1 1 calc R U . . .
C35 C 0.2252(2) 0.62529(15) 0.87579(10) 0.0361(4) Uani 1 1 d . . . . .
H35A H 0.165999 0.658384 0.903887 0.043 Uiso 1 1 calc R U . . .
C36 C 0.3239(2) 0.59167(15) 0.91818(10) 0.0393(4) Uani 1 1 d . . . . .
H36A H 0.332006 0.600945 0.975505 0.047 Uiso 1 1 calc R U . . .
C37 C 0.41147(19) 0.54435(16) 0.87741(11) 0.0377(4) Uani 1 1 d . . . . .
H37A H 0.480920 0.523025 0.907172 0.045 Uiso 1 1 calc R U . . .
C38 C 0.39762(18) 0.52811(15) 0.79299(10) 0.0327(4) Uani 1 1 d . . . . .
H38A H 0.456388 0.494467 0.764907 0.039 Uiso 1 1 calc R U . . .
C39 C 0.07632(16) 0.90093(13) 0.03013(9) 0.0242(3) Uani 1 1 d . . . . .
H39A H 0.103793 0.944093 0.090412 0.029 Uiso 1 1 calc R U . . .
H39B H -0.015558 0.907064 0.004893 0.029 Uiso 1 1 calc R U . . .
C40 C 0.19245(16) 0.95322(13) -0.00850(10) 0.0257(3) Uani 1 1 d . . . . .
C41 C 0.31769(18) 1.04447(14) 0.04042(12) 0.0358(4) Uani 1 1 d . . . . .
H41A H 0.330883 1.072534 0.098932 0.043 Uiso 1 1 calc R U . . .
C42 C 0.4236(2) 1.09496(17) 0.00464(16) 0.0498(5) Uani 1 1 d . . . . .
H42A H 0.507501 1.159002 0.038245 0.060 Uiso 1 1 calc R U . . .
C43 C 0.4069(2) 1.0521(2) -0.07947(16) 0.0549(6) Uani 1 1 d . . . . .
H43A H 0.480149 1.085572 -0.103984 0.066 Uiso 1 1 calc R U . . .
C44 C 0.2840(2) 0.9606(2) -0.12852(13) 0.0481(5) Uani 1 1 d . . . . .
H44A H 0.273423 0.930869 -0.186672 0.058 Uiso 1 1 calc R U . . .
C45 C 0.17576(19) 0.91151(15) -0.09367(11) 0.0341(4) Uani 1 1 d . . . . .
H45A H 0.090374 0.849509 -0.127979 0.041 Uiso 1 1 calc R U . . .
N1 N 0.64985(12) 0.75890(10) 0.47397(7) 0.0200(3) Uani 1 1 d . . . . .
N2 N 0.43438(12) 0.60131(10) 0.41551(7) 0.0199(3) Uani 1 1 d . . . . .
N3 N 0.52722(12) 0.69108(10) 0.56332(7) 0.0212(3) Uani 1 1 d . . . . .
N4 N 0.30382(13) 0.53053(10) 0.50712(7) 0.0215(3) Uani 1 1 d . . . . .
N5 N 0.13686(13) 0.49753(10) 0.09798(7) 0.0197(3) Uani 1 1 d . . . . .
H5B H 0.077163 0.451797 0.049606 0.024 Uiso 1 1 calc R U . . .
N6 N 0.28026(12) 0.68471(10) 0.17935(7) 0.0174(3) Uani 1 1 d . . . . .
N7 N 0.09755(12) 0.64187(10) 0.05645(7) 0.0181(3) Uani 1 1 d . . . . .
N8 N 0.23285(12) 0.83742(10) 0.13938(7) 0.0174(3) Uani 1 1 d . . . . .
N9 N 0.41280(12) 0.87337(10) 0.25600(7) 0.0171(2) Uani 1 1 d . . . . .
O1 O 0.21455(11) 0.44937(8) 0.37008(6) 0.0233(2) Uani 1 1 d . . . . .
O2 O 0.44477(10) 0.83889(8) 0.42033(6) 0.0199(2) Uani 1 1 d . . . . .
O3 O 0.40181(11) 0.62395(9) 0.64729(6) 0.0245(2) Uani 1 1 d . . . . .
O4 O 0.05434(10) 0.78119(8) 0.01832(6) 0.0211(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.3721(16) . ?
C1 C2 1.3905(19) . ?
C1 C6 1.403(2) . ?
C2 C3 1.392(2) . ?
C2 N9 1.4393(17) . ?
C3 C4 1.389(2) . ?
C3 H3A 0.9500 . ?
C4 C5 1.396(2) . ?
C4 C21 1.5358(19) . ?
C5 C6 1.386(2) . ?
C5 H5A 0.9500 . ?
C6 N1 1.4326(18) . ?
C7 N1 1.4632(18) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N3 1.3353(18) . ?
C8 N2 1.3605(18) . ?
C8 N1 1.3612(18) . ?
C9 N4 1.3299(19) . ?
C9 N3 1.3326(19) . ?
C9 O3 1.3357(17) . ?
C10 N2 1.3159(18) . ?
C10 N4 1.3345(18) . ?
C10 O1 1.3569(17) . ?
C11 C12 1.380(2) . ?
C11 C16 1.392(2) . ?
C11 H11A 0.9500 . ?
C12 C13 1.380(2) . ?
C12 O1 1.4081(17) . ?
C13 C14 1.383(2) . ?
C13 H13A 0.9500 . ?
C14 C15 1.387(2) . ?
C14 H14A 0.9500 . ?
C15 C16 1.386(2) . ?
C15 H15A 0.9500 . ?
C16 N5 1.4221(18) . ?
C17 N6 1.3376(18) . ?
C17 N5 1.3461(18) . ?
C17 N7 1.3548(18) . ?
C18 N7 1.3236(18) . ?
C18 N8 1.3271(18) . ?
C18 O4 1.3435(16) . ?
C19 N6 1.3400(18) . ?
C19 N8 1.3568(18) . ?
C19 N9 1.3583(18) . ?
C20 N9 1.4624(18) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C24 1.532(2) . ?
C21 C23 1.535(2) . ?
C21 C22 1.535(2) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 O2 1.4458(16) . ?
C25 C26 1.5027(19) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C31 1.391(2) . ?
C26 C27 1.391(2) . ?
C27 C28 1.385(2) . ?
C27 H27A 0.9500 . ?
C28 C29 1.387(2) . ?
C28 H28A 0.9500 . ?
C29 C30 1.379(2) . ?
C29 H29A 0.9500 . ?
C30 C31 1.390(2) . ?
C30 H30A 0.9500 . ?
C31 H31A 0.9500 . ?
C32 O3 1.4530(18) . ?
C32 C33 1.501(2) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.390(2) . ?
C33 C38 1.390(2) . ?
C34 C35 1.389(2) . ?
C34 H34A 0.9500 . ?
C35 C36 1.380(3) . ?
C35 H35A 0.9500 . ?
C36 C37 1.388(3) . ?
C36 H36A 0.9500 . ?
C37 C38 1.392(2) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
C39 O4 1.4503(17) . ?
C39 C40 1.499(2) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C45 1.387(2) . ?
C40 C41 1.389(2) . ?
C41 C42 1.387(3) . ?
C41 H41A 0.9500 . ?
C42 C43 1.371(3) . ?
C42 H42A 0.9500 . ?
C43 C44 1.378(3) . ?
C43 H43A 0.9500 . ?
C44 C45 1.385(3) . ?
C44 H44A 0.9500 . ?
C45 H45A 0.9500 . ?
N5 H5B 0.8800 . ?

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
O2 C1 C2 125.54(12) . . ?
O2 C1 C6 116.56(12) . . ?
C2 C1 C6 117.75(12) . . ?
C1 C2 C3 119.93(13) . . ?
C1 C2 N9 122.37(12) . . ?
C3 C2 N9 117.66(12) . . ?
C4 C3 C2 122.93(13) . . ?
C4 C3 H3A 118.5 . . ?
C2 C3 H3A 118.5 . . ?
C3 C4 C5 116.54(12) . . ?
C3 C4 C21 120.38(12) . . ?
C5 C4 C21 122.96(12) . . ?
C6 C5 C4 121.36(13) . . ?
C6 C5 H5A 119.3 . . ?
C4 C5 H5A 119.3 . . ?
C5 C6 C1 121.29(13) . . ?
C5 C6 N1 119.76(12) . . ?
C1 C6 N1 118.85(12) . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 N2 125.75(13) . . ?
N3 C8 N1 116.89(12) . . ?
N2 C8 N1 117.36(12) . . ?
N4 C9 N3 127.64(13) . . ?
N4 C9 O3 118.91(12) . . ?
N3 C9 O3 113.45(12) . . ?
N2 C10 N4 128.54(13) . . ?
N2 C10 O1 119.92(12) . . ?
N4 C10 O1 111.52(12) . . ?
C12 C11 C16 119.04(13) . . ?
C12 C11 H11A 120.5 . . ?
C16 C11 H11A 120.5 . . ?
C13 C12 C11 122.07(13) . . ?
C13 C12 O1 117.54(12) . . ?
C11 C12 O1 119.95(13) . . ?
C12 C13 C14 118.14(14) . . ?
C12 C13 H13A 120.9 . . ?
C14 C13 H13A 120.9 . . ?
C13 C14 C15 121.19(14) . . ?
C13 C14 H14A 119.4 . . ?
C15 C14 H14A 119.4 . . ?
C16 C15 C14 119.70(14) . . ?
C16 C15 H15A 120.1 . . ?
C14 C15 H15A 120.1 . . ?
C15 C16 C11 119.83(13) . . ?
C15 C16 N5 118.85(12) . . ?
C11 C16 N5 121.18(12) . . ?
N6 C17 N5 119.57(12) . . ?
N6 C17 N7 125.04(12) . . ?
N5 C17 N7 115.39(12) . . ?
N7 C18 N8 128.57(12) . . ?
N7 C18 O4 111.70(12) . . ?
N8 C18 O4 119.72(12) . . ?
N6 C19 N8 126.16(12) . . ?
N6 C19 N9 116.50(12) . . ?
N8 C19 N9 117.34(12) . . ?
N9 C20 H20A 109.5 . . ?
N9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C24 C21 C23 108.78(13) . . ?
C24 C21 C22 107.89(12) . . ?
C23 C21 C22 109.24(13) . . ?
C24 C21 C4 111.94(12) . . ?
C23 C21 C4 107.82(12) . . ?
C22 C21 C4 111.13(12) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C25 C26 108.30(11) . . ?
O2 C25 H25A 110.0 . . ?
C26 C25 H25A 110.0 . . ?
O2 C25 H25B 110.0 . . ?
C26 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
C31 C26 C27 118.67(13) . . ?
C31 C26 C25 121.50(13) . . ?
C27 C26 C25 119.80(13) . . ?
C28 C27 C26 120.56(14) . . ?
C28 C27 H27A 119.7 . . ?
C26 C27 H27A 119.7 . . ?
C27 C28 C29 120.08(15) . . ?
C27 C28 H28A 120.0 . . ?
C29 C28 H28A 120.0 . . ?
C30 C29 C28 120.10(14) . . ?
C30 C29 H29A 119.9 . . ?
C28 C29 H29A 119.9 . . ?
C29 C30 C31 119.65(14) . . ?
C29 C30 H30A 120.2 . . ?
C31 C30 H30A 120.2 . . ?
C30 C31 C26 120.94(14) . . ?
C30 C31 H31A 119.5 . . ?
C26 C31 H31A 119.5 . . ?
O3 C32 C33 107.30(12) . . ?
O3 C32 H32A 110.3 . . ?
C33 C32 H32A 110.3 . . ?
O3 C32 H32B 110.3 . . ?
C33 C32 H32B 110.3 . . ?
H32A C32 H32B 108.5 . . ?
C34 C33 C38 119.29(15) . . ?
C34 C33 C32 120.34(15) . . ?
C38 C33 C32 120.33(15) . . ?
C35 C34 C33 120.79(17) . . ?
C35 C34 H34A 119.6 . . ?
C33 C34 H34A 119.6 . . ?
C36 C35 C34 119.61(16) . . ?
C36 C35 H35A 120.2 . . ?
C34 C35 H35A 120.2 . . ?
C35 C36 C37 120.26(15) . . ?
C35 C36 H36A 119.9 . . ?
C37 C36 H36A 119.9 . . ?
C36 C37 C38 120.07(17) . . ?
C36 C37 H37A 120.0 . . ?
C38 C37 H37A 120.0 . . ?
C33 C38 C37 119.97(16) . . ?
C33 C38 H38A 120.0 . . ?
C37 C38 H38A 120.0 . . ?
O4 C39 C40 111.47(11) . . ?
O4 C39 H39A 109.3 . . ?
C40 C39 H39A 109.3 . . ?
O4 C39 H39B 109.3 . . ?
C40 C39 H39B 109.3 . . ?
H39A C39 H39B 108.0 . . ?
C45 C40 C41 119.16(15) . . ?
C45 C40 C39 120.40(15) . . ?
C41 C40 C39 120.44(15) . . ?
C42 C41 C40 120.60(19) . . ?
C42 C41 H41A 119.7 . . ?
C40 C41 H41A 119.7 . . ?
C43 C42 C41 119.73(19) . . ?
C43 C42 H42A 120.1 . . ?
C41 C42 H42A 120.1 . . ?
C42 C43 C44 120.20(18) . . ?
C42 C43 H43A 119.9 . . ?
C44 C43 H43A 119.9 . . ?
C43 C44 C45 120.5(2) . . ?
C43 C44 H44A 119.8 . . ?
C45 C44 H44A 119.8 . . ?
C44 C45 C40 119.80(18) . . ?
C44 C45 H45A 120.1 . . ?
C40 C45 H45A 120.1 . . ?
C8 N1 C6 119.60(11) . . ?
C8 N1 C7 119.20(11) . . ?
C6 N1 C7 116.83(11) . . ?
C10 N2 C8 112.66(12) . . ?
C9 N3 C8 113.36(12) . . ?
C9 N4 C10 112.04(12) . . ?
C17 N5 C16 125.83(11) . . ?
C17 N5 H5B 117.1 . . ?
C16 N5 H5B 117.1 . . ?
C17 N6 C19 114.51(11) . . ?
C18 N7 C17 113.46(11) . . ?
C18 N8 C19 112.17(11) . . ?
C19 N9 C2 117.92(11) . . ?
C19 N9 C20 121.90(11) . . ?
C2 N9 C20 118.41(11) . . ?
C10 O1 C12 120.29(11) . . ?
C1 O2 C25 118.84(10) . . ?
C9 O3 C32 116.26(11) . . ?
C18 O4 C39 119.18(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C3 172.60(12) . . . . ?
C6 C1 C2 C3 -2.76(19) . . . . ?
O2 C1 C2 N9 -5.1(2) . . . . ?
C6 C1 C2 N9 179.52(12) . . . . ?
C1 C2 C3 C4 -1.3(2) . . . . ?
N9 C2 C3 C4 176.56(12) . . . . ?
C2 C3 C4 C5 3.3(2) . . . . ?
C2 C3 C4 C21 -172.96(12) . . . . ?
C3 C4 C5 C6 -1.2(2) . . . . ?
C21 C4 C5 C6 174.88(13) . . . . ?
C4 C5 C6 C1 -2.8(2) . . . . ?
C4 C5 C6 N1 -179.16(12) . . . . ?
O2 C1 C6 C5 -171.03(12) . . . . ?
C2 C1 C6 C5 4.8(2) . . . . ?
O2 C1 C6 N1 5.40(18) . . . . ?
C2 C1 C6 N1 -178.82(12) . . . . ?
C16 C11 C12 C13 -1.8(2) . . . . ?
C16 C11 C12 O1 -174.00(12) . . . . ?
C11 C12 C13 C14 0.7(2) . . . . ?
O1 C12 C13 C14 173.08(13) . . . . ?
C12 C13 C14 C15 0.5(2) . . . . ?
C13 C14 C15 C16 -0.6(2) . . . . ?
C14 C15 C16 C11 -0.5(2) . . . . ?
C14 C15 C16 N5 -176.47(13) . . . . ?
C12 C11 C16 C15 1.7(2) . . . . ?
C12 C11 C16 N5 177.53(12) . . . . ?
C3 C4 C21 C24 -154.97(13) . . . . ?
C5 C4 C21 C24 29.05(19) . . . . ?
C3 C4 C21 C23 85.43(16) . . . . ?
C5 C4 C21 C23 -90.56(16) . . . . ?
C3 C4 C21 C22 -34.26(18) . . . . ?
C5 C4 C21 C22 149.75(14) . . . . ?
O2 C25 C26 C31 -124.12(14) . . . . ?
O2 C25 C26 C27 58.01(17) . . . . ?
C31 C26 C27 C28 0.4(2) . . . . ?
C25 C26 C27 C28 178.35(14) . . . . ?
C26 C27 C28 C29 -0.1(3) . . . . ?
C27 C28 C29 C30 -0.4(3) . . . . ?
C28 C29 C30 C31 0.7(2) . . . . ?
C29 C30 C31 C26 -0.4(2) . . . . ?
C27 C26 C31 C30 -0.1(2) . . . . ?
C25 C26 C31 C30 -178.02(13) . . . . ?
O3 C32 C33 C34 107.01(16) . . . . ?
O3 C32 C33 C38 -75.24(18) . . . . ?
C38 C33 C34 C35 -1.0(2) . . . . ?
C32 C33 C34 C35 176.75(15) . . . . ?
C33 C34 C35 C36 0.6(2) . . . . ?
C34 C35 C36 C37 0.6(3) . . . . ?
C35 C36 C37 C38 -1.5(3) . . . . ?
C34 C33 C38 C37 0.1(2) . . . . ?
C32 C33 C38 C37 -177.63(15) . . . . ?
C36 C37 C38 C33 1.1(2) . . . . ?
O4 C39 C40 C45 62.31(17) . . . . ?
O4 C39 C40 C41 -118.08(15) . . . . ?
C45 C40 C41 C42 1.3(2) . . . . ?
C39 C40 C41 C42 -178.33(14) . . . . ?
C40 C41 C42 C43 -2.1(3) . . . . ?
C41 C42 C43 C44 1.2(3) . . . . ?
C42 C43 C44 C45 0.5(3) . . . . ?
C43 C44 C45 C40 -1.4(3) . . . . ?
C41 C40 C45 C44 0.5(2) . . . . ?
C39 C40 C45 C44 -179.93(15) . . . . ?
N3 C8 N1 C6 -158.40(12) . . . . ?
N2 C8 N1 C6 22.59(19) . . . . ?
N3 C8 N1 C7 -2.61(19) . . . . ?
N2 C8 N1 C7 178.38(13) . . . . ?
C5 C6 N1 C8 -127.26(14) . . . . ?
C1 C6 N1 C8 56.26(18) . . . . ?
C5 C6 N1 C7 76.38(17) . . . . ?
C1 C6 N1 C7 -100.10(15) . . . . ?
N4 C10 N2 C8 -1.0(2) . . . . ?
O1 C10 N2 C8 177.26(12) . . . . ?
N3 C8 N2 C10 1.5(2) . . . . ?
N1 C8 N2 C10 -179.54(12) . . . . ?
N4 C9 N3 C8 0.7(2) . . . . ?
O3 C9 N3 C8 -178.55(12) . . . . ?
N2 C8 N3 C9 -1.5(2) . . . . ?
N1 C8 N3 C9 179.63(12) . . . . ?
N3 C9 N4 C10 -0.2(2) . . . . ?
O3 C9 N4 C10 179.02(12) . . . . ?
N2 C10 N4 C9 0.4(2) . . . . ?
O1 C10 N4 C9 -177.98(12) . . . . ?
N6 C17 N5 C16 10.1(2) . . . . ?
N7 C17 N5 C16 -170.53(12) . . . . ?
C15 C16 N5 C17 -137.13(14) . . . . ?
C11 C16 N5 C17 47.0(2) . . . . ?
N5 C17 N6 C19 -178.42(12) . . . . ?
N7 C17 N6 C19 2.28(19) . . . . ?
N8 C19 N6 C17 0.77(19) . . . . ?
N9 C19 N6 C17 -179.99(11) . . . . ?
N8 C18 N7 C17 0.4(2) . . . . ?
O4 C18 N7 C17 -178.95(10) . . . . ?
N6 C17 N7 C18 -2.81(18) . . . . ?
N5 C17 N7 C18 177.86(11) . . . . ?
N7 C18 N8 C19 2.15(19) . . . . ?
O4 C18 N8 C19 -178.57(11) . . . . ?
N6 C19 N8 C18 -2.76(18) . . . . ?
N9 C19 N8 C18 178.00(11) . . . . ?
N6 C19 N9 C2 22.43(17) . . . . ?
N8 C19 N9 C2 -158.25(11) . . . . ?
N6 C19 N9 C20 -172.95(12) . . . . ?
N8 C19 N9 C20 6.37(18) . . . . ?
C1 C2 N9 C19 -107.59(15) . . . . ?
C3 C2 N9 C19 74.64(16) . . . . ?
C1 C2 N9 C20 87.24(16) . . . . ?
C3 C2 N9 C20 -90.53(15) . . . . ?
N2 C10 O1 C12 12.73(19) . . . . ?
N4 C10 O1 C12 -168.76(12) . . . . ?
C13 C12 O1 C10 96.66(15) . . . . ?
C11 C12 O1 C10 -90.79(16) . . . . ?
C2 C1 O2 C25 47.84(18) . . . . ?
C6 C1 O2 C25 -136.75(13) . . . . ?
C26 C25 O2 C1 157.85(12) . . . . ?
N4 C9 O3 C32 2.13(19) . . . . ?
N3 C9 O3 C32 -178.50(13) . . . . ?
C33 C32 O3 C9 174.97(13) . . . . ?
N7 C18 O4 C39 178.00(11) . . . . ?
N8 C18 O4 C39 -1.39(17) . . . . ?
C40 C39 O4 C18 88.75(15) . . . . ?

_refine_diff_density_max         0.493
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.037

####################################################################### 
# 
# 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_exp_13456_auto
_database_code_depnum_ccdc_archive 'CCDC 2304018'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2023-10-27 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;
_audit_creation_date             2023-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        lxc-200-3
_chemical_formula_moiety         'C40 H40 Br N9 O4'
_chemical_formula_sum            'C40 H40 Br N9 O4'
_chemical_formula_weight         790.72
_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'
Br Br -0.6763 1.2805 '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                   11.19970(10)
_cell_length_b                   11.6776(2)
_cell_length_c                   15.8142(3)
_cell_angle_alpha                74.250(2)
_cell_angle_beta                 73.2240(10)
_cell_angle_gamma                70.731(2)
_cell_volume                     1833.45(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    62369
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.8410
_cell_measurement_theta_min      4.0710
_shelx_estimated_absorpt_T_max   0.980
_shelx_estimated_absorpt_T_min   0.980
_exptl_absorpt_coefficient_mu    1.985
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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    1.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             820
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            79604
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.430
_diffrn_reflns_theta_min         4.089
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     34.00 122.00   0.50    0.05    --   46.63  17.00 131.00  176
  2  ω     26.00 122.00   0.50    0.05    --   50.00  79.00  12.99  192
  3  ω     34.00 120.00   0.50    0.05    --   46.63  37.00   0.00  172
  4  ω     34.00 120.00   0.50    0.05    --   46.63  37.00-180.00  172
  5  ω     30.00 126.00   0.50    0.05    --   54.00  80.00 -51.56  192
  6  ω     48.00 143.00   0.50    0.05    --   70.00  75.00 -35.50  190
  7  ω     30.00 126.00   0.50    0.05    --   54.00  79.00  59.09  192
  8  ω     31.00 126.00   0.50    0.05    --   54.00  77.00  93.84  190
  9  ω     37.00 131.00   0.50    0.05    --   58.00  73.00 125.19  188
 10  ω     44.00 139.00   0.50    0.05    --   66.00  76.00  67.61  190
 11  ω     92.00 178.00   0.50    0.05    --  104.75  17.00 131.00  172
 12  ω     42.00 135.00   0.50    0.05    --   62.00  70.00  63.88  186
 13  ω     42.00 135.00   0.50    0.05    --   62.00  70.00  30.89  186
 14  ω     83.00 108.00   0.50    0.05    --  104.75 -77.00 -30.00   50
 15  ω     34.00  62.00   0.50    0.05    --  104.75 -61.00 -90.00   56
 16  ω     35.00  65.00   0.50    0.05    --  104.75 -77.00 -30.00   60
 17  ω     35.00  72.00   0.50    0.05    --  104.75 -61.00 -30.00   74
 18  ω     32.00  59.00   0.50    0.05    --  104.75 -77.00 150.00   54
 19  ω     82.00 108.00   0.50    0.05    --  104.75 -77.00 150.00   52
 20  ω     62.00 105.00   0.50    0.05    --  104.75 -77.00 120.00   86
 21  ω     33.00 106.00   0.50    0.05    --  104.75 -94.00  60.00  146
 22  ω     15.00  94.00   0.50    0.05    --   46.63-125.00  90.00  158
 23  ω     48.00  74.00   0.50    0.05    --  104.75-125.00 -60.00   52
 24  ω     32.00  57.00   0.50    0.05    --  104.75 -94.00 -60.00   50
 25  ω     78.00 107.00   0.50    0.05    --  104.75 -94.00 -30.00   58
 26  ω     90.00 117.00   0.50    0.05    --  104.75-125.00 -60.00   54
 27  ω     35.00 117.00   0.50    0.05    --  104.75-125.00-180.00  164
 28  ω     36.00 103.00   0.50    0.05    --  104.75 -94.00-120.00  134
 29  ω     68.00  97.00   0.50    0.05    --  104.75 -94.00 -60.00   58
 30  ω     32.00  64.00   0.50    0.05    --  104.75 -94.00 -30.00   64
 31  ω    -28.00  27.00   0.50    0.05    --   46.63 -17.00 -36.00  110
 32  ω    -25.00  62.00   0.50    0.05    --   46.63 -57.00 -60.00  174
 33  ω    -13.00  16.00   0.50    0.05    --   22.00 102.00-102.45   58
 34  ω     13.00  45.00   0.50    0.05    --   42.00  90.00-102.63   64
 35  ω    -43.00 -12.00   0.50    0.05    --    6.00 127.00-120.25   62
 36  ω     29.00 126.00   0.50    0.05    --   54.00  83.00 140.59  194
 37  ω      3.00  33.00   0.50    0.05    --   34.00  95.00 145.30   60
 38  ω    -13.00  16.00   0.50    0.05    --   22.00 102.00 121.66   58
 39  ω     14.00  45.00   0.50    0.05    --   42.00  89.00 107.14   62
 40  ω     17.00  45.00   0.50    0.05    --   46.00  90.00  45.69   56
 41  ω     17.00  45.00   0.50    0.05    --   46.00  90.00 -54.91   56
 42  ω     25.00 122.00   0.50    0.05    --   50.00  83.00-174.02  194
 43  ω   -139.00 -40.00   0.50    0.05    --  -66.00 -83.00-179.70  198
 44  ω   -158.00-111.00   0.50    0.05    --  -86.00 -83.00-118.20   94
 45  ω    -88.00 -60.00   0.50    0.05    --  -86.00 -83.00-118.20   56
 46  ω   -146.00 -48.00   0.50    0.05    --  -74.00 -83.00-102.71  196
 47  ω   -143.00 -45.00   0.50    0.05    --  -70.00 -82.00-100.96  196
 48  ω   -135.00 -37.00   0.50    0.05    --  -62.00 -82.00-139.89  196
 49  ω    -80.00 -54.00   0.50    0.05    --  -78.00 -83.00  26.07   52
 50  ω   -143.00 -44.00   0.50    0.05    --  -70.00 -83.00  77.02  198
 51  ω   -150.00-124.00   0.50    0.05    --  -78.00 -82.00 165.13   52
 52  ω    -83.00 -53.00   0.50    0.05    --  -78.00 -82.00 165.13   60
 53  ω   -121.00 -33.00   0.50    0.05    --  -46.63 -17.00 -36.00  176
 54  ω   -102.00 -76.00   0.50    0.05    --  -98.00 -78.00 124.74   52
 55  ω   -154.00-128.00   0.50    0.05    --  -98.00 -78.00 124.74   52
 56  ω   -169.00-115.00   0.50    0.05    --  -98.00 -76.00 -76.82  108
 57  ω   -163.00-111.00   0.50    0.05    --  -94.00 -76.00 -68.25  104
 58  ω   -106.00 -78.00   0.50    0.05    --  -98.00 -76.00 -76.82   56
 59  ω   -146.00 -51.00   0.50    0.05    --  -74.00 -78.00-176.42  190
 60  ω   -143.00 -77.00   0.50    0.05    --  -98.00 -77.00 -93.49  132
 61  ω   -107.00 -72.00   0.50    0.05    --  -94.00 -76.00 -68.25   70
 62  ω    -94.00 -64.00   0.50    0.05    --  -86.00 -75.00 -66.39   60
 63  ω   -107.00 -70.00   0.50    0.05    --  -90.00 -74.00  -7.48   74
 64  ω   -108.00 -74.00   0.50    0.05    --  -94.00 -74.00  35.89   68
 65  ω   -165.00-117.00   0.50    0.05    --  -94.00 -74.00  35.89   96
 66  ω   -146.00 -52.00   0.50    0.05    --  -74.00 -75.00 135.77  188
 67  ω   -115.00 -79.00   0.50    0.05    -- -102.00 -76.00 170.73   72
 68  ω   -173.00-123.00   0.50    0.05    -- -102.00 -76.00 170.73  100
 69  ω   -146.00 -52.00   0.50    0.05    --  -74.00 -74.00 106.19  188
 70  ω    -93.00 -68.00   0.50    0.05    --  -90.00 -74.00  57.53   50
 71  ω   -156.00-113.00   0.50    0.05    --  -90.00 -74.00  57.53   86
 72  ω   -161.00-131.00   0.50    0.05    --  -90.00 -74.00  49.24   60
 73  ω   -162.00-122.00   0.50    0.05    --  -90.00 -74.00  -7.48   80
 74  ω   -135.00 -40.00   0.50    0.05    --  -62.00 -74.00 -90.21  190
 75  ω   -146.00 -52.00   0.50    0.05    --  -74.00 -74.00 -17.28  188
 76  ω   -152.00 -69.00   0.50    0.05    --  -90.00 -74.00  17.02  166
 77  ω    -88.00 -62.00   0.50    0.05    --  -82.00 -73.00 -42.94   52
 78  ω   -143.00 -49.00   0.50    0.05    --  -70.00 -73.00 -41.19  188
 79  ω    -95.00 -70.00   0.50    0.05    --  -90.00 -74.00  49.24   50
 80  ω    -86.00 -61.00   0.50    0.05    --  -82.00 -73.00 101.23   50
 81  ω    -92.00 -60.00   0.50    0.05    --  -78.00 -73.00  78.12   64
 82  ω    -94.00 -69.00   0.50    0.05    --  -90.00 -72.00 136.79   50
 83  ω    -88.00 -62.00   0.50    0.05    --  -82.00 -73.00  57.27   52
 84  ω   -138.00 -81.00   0.50    0.05    -- -102.00 -72.00  77.59  114
 85  ω   -162.00-109.00   0.50    0.05    --  -90.00 -72.00 136.79  106
 86  ω   -101.00 -65.00   0.50    0.05    --  -86.00 -72.00 170.40   72
 87  ω    -84.00 -58.00   0.50    0.05    --  -78.00 -73.00  33.10   52
 88  ω    -99.00 -62.00   0.50    0.05    --  -82.00 -73.00   0.56   74
 89  ω   -175.00-142.00   0.50    0.05    -- -102.00 -72.00  77.59   66
 90  ω   -162.00 -70.00   0.50    0.05    --  -90.00 -71.00 -24.91  184
 91  ω    -92.00 -65.00   0.50    0.05    --  -86.00 -72.00 -57.35   54
 92  ω   -142.00 -78.00   0.50    0.05    --  -98.00 -69.00-164.00  128
 93  ω   -163.00 -74.00   0.50    0.05    --  -94.00 -71.00-154.74  178
 94  ω   -146.00 -54.00   0.50    0.05    --  -74.00 -69.00-155.52  184
 95  ω    -91.00 -65.00   0.50    0.05    --  -82.00 -72.00-104.32   52
 96  ω   -147.00-121.00   0.50    0.05    --  -90.00 -64.00-137.26   52
 97  ω   -159.00-106.00   0.50    0.05    --  -86.00 -68.00  65.56  106
 98  ω    -92.00 -67.00   0.50    0.05    --  -86.00 -68.00  65.56   50
 99  ω   -101.00 -76.00   0.50    0.05    --  -94.00 -65.00  87.32   50
100  ω   -165.00-107.00   0.50    0.05    --  -94.00 -65.00  87.32  116
101  ω   -152.00 -86.00   0.50    0.05    -- -102.00 -62.00 117.08  132
102  ω   -160.00 -75.00   0.50    0.05    --  -90.00 -63.00 -48.13  170
103  ω   -106.00 -80.00   0.50    0.05    --  -90.00 -64.00-137.26   52
104  ω   -153.00-111.00   0.50    0.05    --  -90.00 -58.00-123.18   84
105  ω   -175.00 -89.00   0.50    0.05    -- -102.00 -17.00 -36.00  172
106  ω   -102.00 -60.00   0.50    0.05    -- -102.00  77.00 150.00   84
107  ω    -68.00 -34.00   0.50    0.05    -- -102.00  61.00 120.00   68
108  ω    -23.00  29.00   0.50    0.05    --  -46.63  17.00 131.00  104
109  ω    -66.00 -40.00   0.50    0.05    -- -102.00  61.00-150.00   52
110  ω   -116.00 -32.00   0.50    0.05    -- -102.00 125.00-150.00  168
111  ω    -69.00 -33.00   0.50    0.05    -- -102.00 125.00   0.00   72
112  ω   -112.00 -82.00   0.50    0.05    -- -102.00 125.00   0.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525998000
_diffrn_orient_matrix_UB_12      0.1333223000
_diffrn_orient_matrix_UB_13      0.0169793000
_diffrn_orient_matrix_UB_21      0.1312148000
_diffrn_orient_matrix_UB_22      -0.0090030000
_diffrn_orient_matrix_UB_23      0.0179232000
_diffrn_orient_matrix_UB_31      0.0481646000
_diffrn_orient_matrix_UB_32      0.0494654000
_diffrn_orient_matrix_UB_33      -0.1007561000
_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                7041
_reflns_number_total             7356
_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 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0313
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0386P)²+1.3658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0808
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00X(H00A,H00B), C017(H01D,H01E)
2.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00P(H00P), C00S(H00S), C00V(H00V), C00Z(H00Z), C011(H011),
 C012(H012), C013(H013), C014(H014), C016(H016), C018(H018), C01A(H01I),
 C01B(H01J), C01C(H01K), C01F(H01R)
2.c Idealised Me refined as rotating group:
 C015(H01A,H01B,H01C), C019(H01F,H01G,H01H), C01D(H01L,H01M,H01N), C01E(H01O,
 H01P,H01Q), C01G(H01S,H01T,H01U), C01H(H01V,H01W,H01X), C01I(H01Y,H,HA)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br01 Br -0.36216(2) 1.01520(2) 0.91392(2) 0.02907(7) Uani 1 1 d . . . . .
O002 O 0.25631(11) 0.58046(10) 0.97329(7) 0.0200(2) Uani 1 1 d . . . . .
O003 O 0.16242(10) 0.23825(10) 0.96040(8) 0.0207(2) Uani 1 1 d . . . . .
O004 O 0.27599(11) 1.07566(10) 0.45294(7) 0.0201(2) Uani 1 1 d . . . . .
O005 O 0.44334(10) 0.53765(11) 0.61953(8) 0.0223(2) Uani 1 1 d . . . . .
N006 N 0.38939(12) 0.46686(12) 0.86707(9) 0.0178(3) Uani 1 1 d . . . . .
N007 N 0.27996(12) 1.01664(12) 0.59910(9) 0.0178(3) Uani 1 1 d . . . . .
N008 N 0.43071(12) 0.82693(11) 0.64930(9) 0.0171(3) Uani 1 1 d . . . . .
N009 N 0.33662(12) 0.28550(12) 0.86269(9) 0.0185(3) Uani 1 1 d . . . . .
N00A N 0.29409(12) 0.95030(12) 0.74889(9) 0.0183(3) Uani 1 1 d . . . . .
N00B N 0.42849(12) 0.89614(12) 0.49226(9) 0.0168(3) Uani 1 1 d . . . . .
N00C N 0.57600(12) 0.71682(12) 0.54417(9) 0.0180(3) Uani 1 1 d . . . . .
N00D N 0.20625(12) 0.41120(12) 0.97117(9) 0.0188(3) Uani 1 1 d . . . . .
N00E N 0.51230(13) 0.34590(12) 0.76321(9) 0.0194(3) Uani 1 1 d . . . . .
C00F C 0.77040(14) 0.50787(14) 0.71094(10) 0.0168(3) Uani 1 1 d . . . . .
C00G C 0.28765(14) 0.48174(14) 0.93379(10) 0.0170(3) Uani 1 1 d . . . . .
C00H C 0.32182(15) 0.67190(14) 0.93076(11) 0.0182(3) Uani 1 1 d . . . . .
C00I C 0.69600(14) 0.42426(14) 0.75157(11) 0.0179(3) Uani 1 1 d . . . . .
H00I H 0.721816 0.358167 0.798845 0.021 Uiso 1 1 calc R U . . .
C00J C 0.54483(14) 0.53172(14) 0.65466(11) 0.0177(3) Uani 1 1 d . . . . .
C00K C 0.47470(14) 0.81573(14) 0.56262(11) 0.0163(3) Uani 1 1 d . . . . .
C00L C 0.41018(14) 0.36509(14) 0.83270(11) 0.0175(3) Uani 1 1 d . . . . .
C00M C 0.61557(14) 0.61886(14) 0.61595(10) 0.0173(3) Uani 1 1 d . . . . .
C00N C 0.58444(14) 0.43627(14) 0.72382(11) 0.0178(3) Uani 1 1 d . . . . .
C00O C 0.23260(14) 0.67327(14) 0.60171(11) 0.0182(3) Uani 1 1 d . . . . .
C00P C 0.27978(14) 0.76028(14) 0.85936(11) 0.0178(3) Uani 1 1 d . . . . .
H00P H 0.212086 0.755574 0.836638 0.021 Uiso 1 1 calc R U . . .
C00Q C 0.23774(14) 0.31515(14) 0.93105(11) 0.0175(3) Uani 1 1 d . . . . .
C00R C 0.33573(14) 0.93065(14) 0.66245(11) 0.0164(3) Uani 1 1 d . . . . .
C00S C 0.41869(16) 0.67653(15) 0.96647(11) 0.0210(3) Uani 1 1 d . . . . .
H00S H 0.445251 0.615479 1.016042 0.025 Uiso 1 1 calc R U . . .
C00T C 0.89744(15) 0.49454(14) 0.73596(11) 0.0198(3) Uani 1 1 d . . . . .
C00U C -0.19116(15) 1.03296(15) 0.87021(11) 0.0211(3) Uani 1 1 d . . . . .
C00V C 0.72688(14) 0.60585(14) 0.64351(10) 0.0171(3) Uani 1 1 d . . . . .
H00V H 0.774830 0.665029 0.615867 0.021 Uiso 1 1 calc R U . . .
C00W C 0.33200(14) 0.99142(14) 0.51691(11) 0.0167(3) Uani 1 1 d . . . . .
C00X C 0.19825(15) 1.06480(14) 0.77206(11) 0.0186(3) Uani 1 1 d . . . . .
H00A H 0.199905 1.131499 0.717840 0.022 Uiso 1 1 calc R U . . .
H00B H 0.223151 1.089669 0.818185 0.022 Uiso 1 1 calc R U . . .
C00Y C 0.06158(14) 1.05159(13) 0.80750(11) 0.0173(3) Uani 1 1 d . . . . .
C00Z C 0.47620(16) 0.77265(15) 0.92808(12) 0.0232(3) Uani 1 1 d . . . . .
H00Z H 0.543615 0.777102 0.951227 0.028 Uiso 1 1 calc R U . . .
C010 C 0.33818(14) 0.85591(14) 0.82151(10) 0.0173(3) Uani 1 1 d . . . . .
C011 C -0.13651(15) 1.06839(15) 0.92364(11) 0.0206(3) Uani 1 1 d . . . . .
H011 H -0.184500 1.086609 0.980908 0.025 Uiso 1 1 calc R U . . .
C012 C -0.12271(16) 1.00760(16) 0.78589(12) 0.0241(3) Uani 1 1 d . . . . .
H012 H -0.161643 0.983460 0.750007 0.029 Uiso 1 1 calc R U . . .
C013 C 0.25420(15) 0.65070(15) 0.51597(11) 0.0218(3) Uani 1 1 d . . . . .
H013 H 0.328549 0.588555 0.494987 0.026 Uiso 1 1 calc R U . . .
C014 C 0.43623(15) 0.86256(15) 0.85608(11) 0.0209(3) Uani 1 1 d . . . . .
H014 H 0.475762 0.928366 0.830553 0.025 Uiso 1 1 calc R U . . .
C015 C 0.32248(16) 1.05104(15) 0.36327(11) 0.0227(3) Uani 1 1 d . . . . .
H01A H 0.276695 1.119088 0.322150 0.034 Uiso 1 1 calc R U . . .
H01B H 0.306815 0.973676 0.362354 0.034 Uiso 1 1 calc R U . . .
H01C H 0.415675 1.043544 0.344109 0.034 Uiso 1 1 calc R U . . .
C016 C 0.12540(16) 0.76782(15) 0.62993(12) 0.0230(3) Uani 1 1 d . . . . .
H016 H 0.110606 0.785669 0.687831 0.028 Uiso 1 1 calc R U . . .
C017 C 0.31589(14) 0.59456(15) 0.66728(11) 0.0203(3) Uani 1 1 d . . . . .
H01D H 0.322611 0.646420 0.704987 0.024 Uiso 1 1 calc R U . . .
H01E H 0.275490 0.529743 0.707433 0.024 Uiso 1 1 calc R U . . .
C018 C 0.00273(16) 1.01789(15) 0.75477(11) 0.0218(3) Uani 1 1 d . . . . .
H018 H 0.049540 1.001832 0.696763 0.026 Uiso 1 1 calc R U . . .
C019 C 0.54784(16) 0.24179(15) 0.71790(12) 0.0239(3) Uani 1 1 d . . . . .
H01F H 0.634432 0.189344 0.724815 0.036 Uiso 1 1 calc R U . . .
H01G H 0.548062 0.273047 0.653756 0.036 Uiso 1 1 calc R U . . .
H01H H 0.484841 0.193214 0.744772 0.036 Uiso 1 1 calc R U . . .
C01A C -0.00956(15) 1.07668(14) 0.89143(11) 0.0191(3) Uani 1 1 d . . . . .
H01I H 0.029392 1.100062 0.927724 0.023 Uiso 1 1 calc R U . . .
C01B C 0.16810(17) 0.71817(16) 0.46066(12) 0.0253(3) Uani 1 1 d . . . . .
H01J H 0.183224 0.701096 0.402472 0.030 Uiso 1 1 calc R U . . .
C01C C 0.05986(17) 0.81058(16) 0.48996(12) 0.0270(4) Uani 1 1 d . . . . .
H01K H 0.000065 0.855751 0.452565 0.032 Uiso 1 1 calc R U . . .
C01D C 0.63970(16) 0.69879(15) 0.45264(11) 0.0235(3) Uani 1 1 d . . . . .
H01L H 0.606566 0.640666 0.437564 0.035 Uiso 1 1 calc R U . . .
H01M H 0.733418 0.665348 0.448046 0.035 Uiso 1 1 calc R U . . .
H01N H 0.621992 0.778227 0.410687 0.035 Uiso 1 1 calc R U . . .
C01E C 0.05195(16) 0.26833(16) 1.03334(12) 0.0254(4) Uani 1 1 d . . . . .
H01O H -0.002876 0.351440 1.014908 0.038 Uiso 1 1 calc R U . . .
H01P H 0.082149 0.265795 1.086308 0.038 Uiso 1 1 calc R U . . .
H01Q H 0.001763 0.208118 1.048203 0.038 Uiso 1 1 calc R U . . .
C01F C 0.04019(16) 0.83604(16) 0.57432(12) 0.0270(4) Uani 1 1 d . . . . .
H01R H -0.032139 0.900658 0.594177 0.032 Uiso 1 1 calc R U . . .
C01G C 1.00694(16) 0.48739(17) 0.65094(12) 0.0274(4) Uani 1 1 d . . . . .
H01S H 1.013106 0.417513 0.625343 0.041 Uiso 1 1 calc R U . . .
H01T H 1.089228 0.475777 0.666621 0.041 Uiso 1 1 calc R U . . .
H01U H 0.988343 0.564305 0.606622 0.041 Uiso 1 1 calc R U . . .
C01H C 0.93395(17) 0.37763(17) 0.80589(13) 0.0297(4) Uani 1 1 d . . . . .
H01V H 0.866499 0.381472 0.861445 0.044 Uiso 1 1 calc R U . . .
H01W H 1.016836 0.371187 0.818537 0.044 Uiso 1 1 calc R U . . .
H01X H 0.941955 0.305128 0.782613 0.044 Uiso 1 1 calc R U . . .
C01I C 0.88400(18) 0.60635(17) 0.77473(13) 0.0294(4) Uani 1 1 d . . . . .
H01Y H 0.864947 0.682179 0.729528 0.044 Uiso 1 1 calc R U . . .
H H 0.965211 0.597193 0.790977 0.044 Uiso 1 1 calc R U . . .
HA H 0.813273 0.611078 0.828453 0.044 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br01 C00U 1.8997(16) . ?
O002 C00G 1.3563(18) . ?
O002 C00H 1.4047(19) . ?
O003 C00Q 1.3346(19) . ?
O003 C01E 1.4470(19) . ?
O004 C00W 1.3430(18) . ?
O004 C015 1.4355(19) . ?
O005 C00J 1.3772(18) . ?
O005 C017 1.4400(18) . ?
N006 C00G 1.310(2) . ?
N006 C00L 1.363(2) . ?
N007 C00R 1.343(2) . ?
N007 C00W 1.332(2) . ?
N008 C00K 1.343(2) . ?
N008 C00R 1.3418(19) . ?
N009 C00L 1.345(2) . ?
N009 C00Q 1.332(2) . ?
N00A C00R 1.368(2) . ?
N00A C00X 1.4717(18) . ?
N00A C010 1.435(2) . ?
N00B C00K 1.353(2) . ?
N00B C00W 1.3253(19) . ?
N00C C00K 1.3540(19) . ?
N00C C00M 1.430(2) . ?
N00C C01D 1.456(2) . ?
N00D C00G 1.334(2) . ?
N00D C00Q 1.335(2) . ?
N00E C00L 1.343(2) . ?
N00E C00N 1.439(2) . ?
N00E C019 1.4625(19) . ?
C00F C00I 1.396(2) . ?
C00F C00T 1.533(2) . ?
C00F C00V 1.398(2) . ?
C00H C00P 1.384(2) . ?
C00H C00S 1.381(2) . ?
C00I H00I 0.9500 . ?
C00I C00N 1.393(2) . ?
C00J C00M 1.397(2) . ?
C00J C00N 1.388(2) . ?
C00M C00V 1.386(2) . ?
C00O C013 1.389(2) . ?
C00O C016 1.394(2) . ?
C00O C017 1.505(2) . ?
C00P H00P 0.9500 . ?
C00P C010 1.388(2) . ?
C00S H00S 0.9500 . ?
C00S C00Z 1.387(2) . ?
C00T C01G 1.536(2) . ?
C00T C01H 1.525(2) . ?
C00T C01I 1.535(2) . ?
C00U C011 1.384(2) . ?
C00U C012 1.388(2) . ?
C00V H00V 0.9500 . ?
C00X H00A 0.9900 . ?
C00X H00B 0.9900 . ?
C00X C00Y 1.515(2) . ?
C00Y C018 1.397(2) . ?
C00Y C01A 1.389(2) . ?
C00Z H00Z 0.9500 . ?
C00Z C014 1.391(2) . ?
C010 C014 1.392(2) . ?
C011 H011 0.9500 . ?
C011 C01A 1.392(2) . ?
C012 H012 0.9500 . ?
C012 C018 1.382(2) . ?
C013 H013 0.9500 . ?
C013 C01B 1.388(2) . ?
C014 H014 0.9500 . ?
C015 H01A 0.9800 . ?
C015 H01B 0.9800 . ?
C015 H01C 0.9800 . ?
C016 H016 0.9500 . ?
C016 C01F 1.386(2) . ?
C017 H01D 0.9900 . ?
C017 H01E 0.9900 . ?
C018 H018 0.9500 . ?
C019 H01F 0.9800 . ?
C019 H01G 0.9800 . ?
C019 H01H 0.9800 . ?
C01A H01I 0.9500 . ?
C01B H01J 0.9500 . ?
C01B C01C 1.390(2) . ?
C01C H01K 0.9500 . ?
C01C C01F 1.385(3) . ?
C01D H01L 0.9800 . ?
C01D H01M 0.9800 . ?
C01D H01N 0.9800 . ?
C01E H01O 0.9800 . ?
C01E H01P 0.9800 . ?
C01E H01Q 0.9800 . ?
C01F H01R 0.9500 . ?
C01G H01S 0.9800 . ?
C01G H01T 0.9800 . ?
C01G H01U 0.9800 . ?
C01H H01V 0.9800 . ?
C01H H01W 0.9800 . ?
C01H H01X 0.9800 . ?
C01I H01Y 0.9800 . ?
C01I H 0.9800 . ?
C01I HA 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
C00G O002 C00H 117.50(12) . . ?
C00Q O003 C01E 116.08(12) . . ?
C00W O004 C015 116.45(12) . . ?
C00J O005 C017 115.78(12) . . ?
C00G N006 C00L 113.13(13) . . ?
C00W N007 C00R 112.62(13) . . ?
C00R N008 C00K 113.98(13) . . ?
C00Q N009 C00L 113.43(13) . . ?
C00R N00A C00X 122.02(13) . . ?
C00R N00A C010 120.52(12) . . ?
C010 N00A C00X 117.38(12) . . ?
C00W N00B C00K 112.88(13) . . ?
C00K N00C C00M 119.89(13) . . ?
C00K N00C C01D 122.55(13) . . ?
C00M N00C C01D 117.25(12) . . ?
C00G N00D C00Q 111.69(13) . . ?
C00L N00E C00N 120.19(13) . . ?
C00L N00E C019 123.00(13) . . ?
C00N N00E C019 116.50(13) . . ?
C00I C00F C00T 122.78(14) . . ?
C00I C00F C00V 117.66(14) . . ?
C00V C00F C00T 119.55(14) . . ?
N006 C00G O002 118.68(14) . . ?
N006 C00G N00D 128.87(14) . . ?
N00D C00G O002 112.45(13) . . ?
C00P C00H O002 118.80(14) . . ?
C00S C00H O002 118.71(14) . . ?
C00S C00H C00P 122.26(15) . . ?
C00F C00I H00I 119.5 . . ?
C00N C00I C00F 120.98(14) . . ?
C00N C00I H00I 119.5 . . ?
O005 C00J C00M 119.40(14) . . ?
O005 C00J C00N 121.60(14) . . ?
C00N C00J C00M 118.85(14) . . ?
N008 C00K N00B 125.63(13) . . ?
N008 C00K N00C 116.91(13) . . ?
N00B C00K N00C 117.44(14) . . ?
N009 C00L N006 125.03(14) . . ?
N00E C00L N006 115.86(14) . . ?
N00E C00L N009 119.11(14) . . ?
C00J C00M N00C 119.16(14) . . ?
C00V C00M N00C 120.66(14) . . ?
C00V C00M C00J 120.08(14) . . ?
C00I C00N N00E 120.36(14) . . ?
C00J C00N N00E 118.89(14) . . ?
C00J C00N C00I 120.67(14) . . ?
C013 C00O C016 118.76(15) . . ?
C013 C00O C017 122.44(14) . . ?
C016 C00O C017 118.70(14) . . ?
C00H C00P H00P 120.6 . . ?
C00H C00P C010 118.89(14) . . ?
C010 C00P H00P 120.6 . . ?
N009 C00Q O003 114.09(13) . . ?
N009 C00Q N00D 127.84(14) . . ?
N00D C00Q O003 118.07(14) . . ?
N007 C00R N00A 117.61(13) . . ?
N008 C00R N007 126.33(14) . . ?
N008 C00R N00A 116.05(13) . . ?
C00H C00S H00S 120.9 . . ?
C00H C00S C00Z 118.28(15) . . ?
C00Z C00S H00S 120.9 . . ?
C00F C00T C01G 108.81(13) . . ?
C00F C00T C01I 109.75(13) . . ?
C01H C00T C00F 112.03(13) . . ?
C01H C00T C01G 108.13(14) . . ?
C01H C00T C01I 108.25(14) . . ?
C01I C00T C01G 109.85(14) . . ?
C011 C00U Br01 119.44(12) . . ?
C011 C00U C012 121.41(15) . . ?
C012 C00U Br01 119.14(12) . . ?
C00F C00V H00V 119.2 . . ?
C00M C00V C00F 121.67(14) . . ?
C00M C00V H00V 119.2 . . ?
N007 C00W O004 113.35(13) . . ?
N00B C00W O004 118.18(14) . . ?
N00B C00W N007 128.47(14) . . ?
N00A C00X H00A 109.0 . . ?
N00A C00X H00B 109.0 . . ?
N00A C00X C00Y 113.08(12) . . ?
H00A C00X H00B 107.8 . . ?
C00Y C00X H00A 109.0 . . ?
C00Y C00X H00B 109.0 . . ?
C018 C00Y C00X 120.42(14) . . ?
C01A C00Y C00X 121.03(14) . . ?
C01A C00Y C018 118.52(14) . . ?
C00S C00Z H00Z 119.6 . . ?
C00S C00Z C014 120.72(15) . . ?
C014 C00Z H00Z 119.6 . . ?
C00P C010 N00A 119.90(14) . . ?
C00P C010 C014 120.00(15) . . ?
C014 C010 N00A 120.06(14) . . ?
C00U C011 H011 120.8 . . ?
C00U C011 C01A 118.38(15) . . ?
C01A C011 H011 120.8 . . ?
C00U C012 H012 120.4 . . ?
C018 C012 C00U 119.23(15) . . ?
C018 C012 H012 120.4 . . ?
C00O C013 H013 119.7 . . ?
C01B C013 C00O 120.57(15) . . ?
C01B C013 H013 119.7 . . ?
C00Z C014 C010 119.85(15) . . ?
C00Z C014 H014 120.1 . . ?
C010 C014 H014 120.1 . . ?
O004 C015 H01A 109.5 . . ?
O004 C015 H01B 109.5 . . ?
O004 C015 H01C 109.5 . . ?
H01A C015 H01B 109.5 . . ?
H01A C015 H01C 109.5 . . ?
H01B C015 H01C 109.5 . . ?
C00O C016 H016 119.7 . . ?
C01F C016 C00O 120.62(15) . . ?
C01F C016 H016 119.7 . . ?
O005 C017 C00O 110.17(13) . . ?
O005 C017 H01D 109.6 . . ?
O005 C017 H01E 109.6 . . ?
C00O C017 H01D 109.6 . . ?
C00O C017 H01E 109.6 . . ?
H01D C017 H01E 108.1 . . ?
C00Y C018 H018 119.6 . . ?
C012 C018 C00Y 120.87(15) . . ?
C012 C018 H018 119.6 . . ?
N00E C019 H01F 109.5 . . ?
N00E C019 H01G 109.5 . . ?
N00E C019 H01H 109.5 . . ?
H01F C019 H01G 109.5 . . ?
H01F C019 H01H 109.5 . . ?
H01G C019 H01H 109.5 . . ?
C00Y C01A C011 121.58(15) . . ?
C00Y C01A H01I 119.2 . . ?
C011 C01A H01I 119.2 . . ?
C013 C01B H01J 119.8 . . ?
C013 C01B C01C 120.36(16) . . ?
C01C C01B H01J 119.8 . . ?
C01B C01C H01K 120.4 . . ?
C01F C01C C01B 119.23(16) . . ?
C01F C01C H01K 120.4 . . ?
N00C C01D H01L 109.5 . . ?
N00C C01D H01M 109.5 . . ?
N00C C01D H01N 109.5 . . ?
H01L C01D H01M 109.5 . . ?
H01L C01D H01N 109.5 . . ?
H01M C01D H01N 109.5 . . ?
O003 C01E H01O 109.5 . . ?
O003 C01E H01P 109.5 . . ?
O003 C01E H01Q 109.5 . . ?
H01O C01E H01P 109.5 . . ?
H01O C01E H01Q 109.5 . . ?
H01P C01E H01Q 109.5 . . ?
C016 C01F H01R 119.8 . . ?
C01C C01F C016 120.40(15) . . ?
C01C C01F H01R 119.8 . . ?
C00T C01G H01S 109.5 . . ?
C00T C01G H01T 109.5 . . ?
C00T C01G H01U 109.5 . . ?
H01S C01G H01T 109.5 . . ?
H01S C01G H01U 109.5 . . ?
H01T C01G H01U 109.5 . . ?
C00T C01H H01V 109.5 . . ?
C00T C01H H01W 109.5 . . ?
C00T C01H H01X 109.5 . . ?
H01V C01H H01W 109.5 . . ?
H01V C01H H01X 109.5 . . ?
H01W C01H H01X 109.5 . . ?
C00T C01I H01Y 109.5 . . ?
C00T C01I H 109.5 . . ?
C00T C01I HA 109.5 . . ?
H01Y C01I H 109.5 . . ?
H01Y C01I HA 109.5 . . ?
H C01I HA 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
Br01 C00U C011 C01A 177.84(12) . . . . ?
Br01 C00U C012 C018 -178.62(13) . . . . ?
O002 C00H C00P C010 175.34(13) . . . . ?
O002 C00H C00S C00Z -175.28(14) . . . . ?
O005 C00J C00M N00C 3.8(2) . . . . ?
O005 C00J C00M C00V -172.50(13) . . . . ?
O005 C00J C00N N00E -3.9(2) . . . . ?
O005 C00J C00N C00I 172.79(13) . . . . ?
N00A C00X C00Y C018 -59.13(19) . . . . ?
N00A C00X C00Y C01A 123.11(15) . . . . ?
N00A C010 C014 C00Z 178.25(14) . . . . ?
N00C C00M C00V C00F -177.29(13) . . . . ?
C00F C00I C00N N00E 176.88(13) . . . . ?
C00F C00I C00N C00J 0.3(2) . . . . ?
C00G O002 C00H C00P 81.51(17) . . . . ?
C00G O002 C00H C00S -103.88(16) . . . . ?
C00G N006 C00L N009 -0.4(2) . . . . ?
C00G N006 C00L N00E 179.14(13) . . . . ?
C00G N00D C00Q O003 -178.48(13) . . . . ?
C00G N00D C00Q N009 0.6(2) . . . . ?
C00H O002 C00G N006 10.4(2) . . . . ?
C00H O002 C00G N00D -169.95(13) . . . . ?
C00H C00P C010 N00A -178.46(13) . . . . ?
C00H C00P C010 C014 -0.7(2) . . . . ?
C00H C00S C00Z C014 0.6(2) . . . . ?
C00I C00F C00T C01G 122.20(16) . . . . ?
C00I C00F C00T C01H 2.7(2) . . . . ?
C00I C00F C00T C01I -117.57(16) . . . . ?
C00I C00F C00V C00M -1.5(2) . . . . ?
C00J O005 C017 C00O 140.64(14) . . . . ?
C00J C00M C00V C00F -1.1(2) . . . . ?
C00K N008 C00R N007 3.3(2) . . . . ?
C00K N008 C00R N00A -175.60(13) . . . . ?
C00K N00B C00W O004 -178.21(13) . . . . ?
C00K N00B C00W N007 1.5(2) . . . . ?
C00K N00C C00M C00J 78.54(18) . . . . ?
C00K N00C C00M C00V -105.20(17) . . . . ?
C00L N006 C00G O002 -179.55(13) . . . . ?
C00L N006 C00G N00D 0.8(2) . . . . ?
C00L N009 C00Q O003 178.79(13) . . . . ?
C00L N009 C00Q N00D -0.4(2) . . . . ?
C00L N00E C00N C00I 94.97(18) . . . . ?
C00L N00E C00N C00J -88.34(18) . . . . ?
C00M N00C C00K N008 11.5(2) . . . . ?
C00M N00C C00K N00B -170.00(13) . . . . ?
C00M C00J C00N N00E -179.48(13) . . . . ?
C00M C00J C00N C00I -2.8(2) . . . . ?
C00N N00E C00L N006 -6.0(2) . . . . ?
C00N N00E C00L N009 173.54(14) . . . . ?
C00N C00J C00M N00C 179.48(13) . . . . ?
C00N C00J C00M C00V 3.2(2) . . . . ?
C00O C013 C01B C01C 0.9(3) . . . . ?
C00O C016 C01F C01C 0.5(3) . . . . ?
C00P C00H C00S C00Z -0.9(2) . . . . ?
C00P C010 C014 C00Z 0.5(2) . . . . ?
C00Q N009 C00L N006 0.2(2) . . . . ?
C00Q N009 C00L N00E -179.32(14) . . . . ?
C00Q N00D C00G O002 179.44(12) . . . . ?
C00Q N00D C00G N006 -0.9(2) . . . . ?
C00R N007 C00W O004 179.08(12) . . . . ?
C00R N007 C00W N00B -0.6(2) . . . . ?
C00R N008 C00K N00B -2.3(2) . . . . ?
C00R N008 C00K N00C 176.08(13) . . . . ?
C00R N00A C00X C00Y 97.83(17) . . . . ?
C00R N00A C010 C00P -81.61(18) . . . . ?
C00R N00A C010 C014 100.67(17) . . . . ?
C00S C00H C00P C010 0.9(2) . . . . ?
C00S C00Z C014 C010 -0.5(2) . . . . ?
C00T C00F C00I C00N -176.83(14) . . . . ?
C00T C00F C00V C00M 177.28(14) . . . . ?
C00U C011 C01A C00Y 0.7(2) . . . . ?
C00U C012 C018 C00Y 0.9(3) . . . . ?
C00V C00F C00I C00N 1.9(2) . . . . ?
C00V C00F C00T C01G -56.47(18) . . . . ?
C00V C00F C00T C01H -175.97(14) . . . . ?
C00V C00F C00T C01I 63.76(19) . . . . ?
C00W N007 C00R N008 -2.0(2) . . . . ?
C00W N007 C00R N00A 176.89(13) . . . . ?
C00W N00B C00K N008 0.1(2) . . . . ?
C00W N00B C00K N00C -178.21(13) . . . . ?
C00X N00A C00R N007 -4.1(2) . . . . ?
C00X N00A C00R N008 174.91(13) . . . . ?
C00X N00A C010 C00P 95.28(17) . . . . ?
C00X N00A C010 C014 -82.44(18) . . . . ?
C00X C00Y C018 C012 -178.91(15) . . . . ?
C00X C00Y C01A C011 178.10(14) . . . . ?
C010 N00A C00R N007 172.62(13) . . . . ?
C010 N00A C00R N008 -8.3(2) . . . . ?
C010 N00A C00X C00Y -79.02(17) . . . . ?
C011 C00U C012 C018 0.1(3) . . . . ?
C012 C00U C011 C01A -0.8(2) . . . . ?
C013 C00O C016 C01F 1.6(2) . . . . ?
C013 C00O C017 O005 26.0(2) . . . . ?
C013 C01B C01C C01F 1.2(3) . . . . ?
C015 O004 C00W N007 -176.77(13) . . . . ?
C015 O004 C00W N00B 2.9(2) . . . . ?
C016 C00O C013 C01B -2.3(2) . . . . ?
C016 C00O C017 O005 -157.79(14) . . . . ?
C017 O005 C00J C00M -99.85(16) . . . . ?
C017 O005 C00J C00N 84.58(17) . . . . ?
C017 C00O C013 C01B 173.95(15) . . . . ?
C017 C00O C016 C01F -174.78(16) . . . . ?
C018 C00Y C01A C011 0.3(2) . . . . ?
C019 N00E C00L N006 -179.49(14) . . . . ?
C019 N00E C00L N009 0.1(2) . . . . ?
C019 N00E C00N C00I -91.17(18) . . . . ?
C019 N00E C00N C00J 85.51(17) . . . . ?
C01A C00Y C018 C012 -1.1(2) . . . . ?
C01B C01C C01F C016 -1.8(3) . . . . ?
C01D N00C C00K N008 -174.98(14) . . . . ?
C01D N00C C00K N00B 3.5(2) . . . . ?
C01D N00C C00M C00J -95.31(17) . . . . ?
C01D N00C C00M C00V 80.95(18) . . . . ?
C01E O003 C00Q N009 -178.66(14) . . . . ?
C01E O003 C00Q N00D 0.6(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 7.169
_oxdiff_exptl_absorpt_empirical_full_min 0.711
####################################################################### 
# 
# 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_exp_16702_auto
_database_code_depnum_ccdc_archive 'CCDC 2304021'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2023-10-27 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;
_audit_creation_date             2023-08-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H37 N9 O4'
_chemical_formula_sum            'C34 H37 N9 O4'
_chemical_formula_weight         635.72
_chemical_absolute_configuration ?
_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'
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      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   24.6160(7)
_cell_length_b                   13.0934(5)
_cell_length_c                   9.9979(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3222.39(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19984
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.6230
_cell_measurement_theta_min      3.3260
_shelx_estimated_absorpt_T_max   0.965
_shelx_estimated_absorpt_T_min   0.899
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            27752
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.093
_diffrn_reflns_theta_min         3.591
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_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   -118.00 -24.00   0.50    0.05    --  -46.63 -77.00  90.00  188
  2  ω   -118.00 -47.00   0.50    0.05    --  -46.63 -77.00 -30.00  142
  3  ω   -118.00 -32.00   0.50    0.05    --  -46.63 -57.00-180.00  172
  4  ω    -40.00  27.00   0.50    0.05    --  -46.63  37.00-150.00  134
  5  ω    -69.00 -29.00   0.50    0.05    -- -102.00  61.00 150.00   80
  6  ω    -69.00 -29.00   0.50    0.05    -- -102.00  61.00  60.00   80
  7  ω    -69.00 -29.00   0.50    0.05    -- -102.00  61.00 -30.00   80
  8  ω     82.00 178.00   0.50    0.05    --  104.75  77.00   0.00  192
  9  ω     91.00 178.00   0.50    0.05    --  104.75  15.00 -77.00  174
 10  ω     32.00  73.00   0.50    0.05    --  104.75 -61.00  30.00   82
 11  ω     32.00  73.00   0.50    0.05    --  104.75 -61.00   0.00   82
 12  ω     92.00 177.00   0.50    0.05    --  104.75  45.00-150.00  170
 13  ω     32.00  73.00   0.50    0.05    --  104.75 -61.00-180.00   82
 14  ω    -28.00  28.00   0.50    0.05    --   46.63 -19.00   0.00  112
 15  ω     32.00  73.00   0.50    0.05    --  104.75 -61.00  90.00   82
 16  ω     32.00 109.00   0.50    0.05    --  104.75 -94.00  30.00  154
 17  ω      7.00  85.00   0.50    0.05    --   46.63-113.00 -52.00  156
 18  ω     32.00 132.00   0.50    0.05    --  104.75-147.00-120.00  200
 19  ω     36.00 112.00   0.50    0.05    --  104.75-113.00 -52.00  152
 20  ω     35.00 117.00   0.50    0.05    --  104.75-125.00   0.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0109198000
_diffrn_orient_matrix_UB_12      0.1151992000
_diffrn_orient_matrix_UB_13      -0.0163860000
_diffrn_orient_matrix_UB_21      -0.0042007000
_diffrn_orient_matrix_UB_22      -0.0139763000
_diffrn_orient_matrix_UB_23      -0.1526239000
_diffrn_orient_matrix_UB_31      -0.0614504000
_diffrn_orient_matrix_UB_32      -0.0197450000
_diffrn_orient_matrix_UB_33      0.0134040000
_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         0.764
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                6031
_reflns_number_total             6548
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 2417 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6548
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      1.116
_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)+(0.0541P)²+0.9332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1140
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C00Q-C015 \\sim C00Q-C0
 with sigma of 0.02
 C015-C019 \\sim C0-C3
 with sigma of 0.02
 C015-C1 \\sim C0-C1A
 with sigma of 0.02
 C015-C2 \\sim C0-C2A
 with sigma of 0.02
 C00Q-C019 \\sim C00Q-C3
 with sigma of 0.04
 C00Q-C1 \\sim C00Q-C1A
 with sigma of 0.04
 C00Q-C2 \\sim C00Q-C2A
 with sigma of 0.04
 C019-C1 \\sim C3-C1A
 with sigma of 0.04
 C019-C2 \\sim C3-C2A
 with sigma of 0.04
 C1-C2 \\sim C1A-C2A
 with sigma of 0.04
2. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C0)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C015)=Sof(C019)=Sof(H01J)=Sof(H01K)=Sof(H01L)=Sof(C1)=Sof(H1A)=Sof(H1B)=
 Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C00X(H00G,H00H)
3.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00Y(H00Y),
 C00Z(H00Z), C011(H011), C013(H013), C014(H014), C017(H017)
3.c Idealised Me refined as rotating group:
 C00V(H00A,H00B,H00C), C00W(H00D,H00E,H00F), C012(H01A,H01B,H01C), C016(H01D,
 H01E,H01F), C018(H01G,H01H,H01I), C019(H01J,H01K,H01L), C1(H1A,H1B,H1C),
 C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC), C3(H3A,H3B,H3C), C1A(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
O001 O 0.33358(8) 0.64575(15) 0.71784(19) 0.0323(4) Uani 1 1 d . . . . .
O002 O 0.43929(8) 0.73734(16) 0.2879(2) 0.0339(4) Uani 1 1 d . . . . .
O003 O 0.39663(10) 0.95970(16) 0.8241(2) 0.0393(5) Uani 1 1 d . . . . .
O004 O 0.45797(8) 0.25922(15) 0.0614(2) 0.0351(4) Uani 1 1 d . . . . .
N005 N 0.37607(9) 0.47795(18) 0.2539(2) 0.0303(5) Uani 1 1 d . . . . .
N006 N 0.40639(9) 0.30446(18) 0.2431(2) 0.0299(5) Uani 1 1 d . . . . .
N007 N 0.38256(9) 0.92463(18) 0.6079(2) 0.0286(5) Uani 1 1 d . . . . .
N008 N 0.43297(9) 0.42228(18) 0.0728(2) 0.0301(5) Uani 1 1 d . . . . .
N009 N 0.36691(10) 0.88034(18) 0.3872(2) 0.0312(5) Uani 1 1 d . . . . .
N00A N 0.34921(10) 0.36106(18) 0.4110(2) 0.0326(5) Uani 1 1 d . . . . .
N00B N 0.40556(9) 0.59006(18) 0.0917(2) 0.0295(5) Uani 1 1 d . . . . .
N00C N 0.36536(10) 0.79938(18) 0.7763(2) 0.0313(5) Uani 1 1 d . . . . .
N00D N 0.34875(9) 0.75944(18) 0.5473(2) 0.0275(5) Uani 1 1 d . . . . .
C00E C 0.40462(10) 0.4939(2) 0.1407(3) 0.0280(6) Uani 1 1 d . . . . .
C00F C 0.37831(11) 0.3823(2) 0.2989(3) 0.0294(6) Uani 1 1 d . . . . .
C00G C 0.31047(11) 0.5822(2) 0.6206(3) 0.0288(6) Uani 1 1 d . . . . .
C00H C 0.36645(10) 0.8549(2) 0.5175(3) 0.0265(5) Uani 1 1 d . . . . .
C00I C 0.43111(11) 0.3314(2) 0.1313(3) 0.0293(6) Uani 1 1 d . . . . .
C00J C 0.34989(10) 0.7395(2) 0.6766(3) 0.0272(5) Uani 1 1 d . . . . .
C00K C 0.35013(11) 0.8084(2) 0.2875(3) 0.0293(6) Uani 1 1 d . . . . .
C00L C 0.38102(11) 0.8910(2) 0.7336(3) 0.0290(6) Uani 1 1 d . . . . .
C00M C 0.31794(11) 0.4413(2) 0.4711(3) 0.0295(6) Uani 1 1 d . . . . .
C00N C 0.38648(10) 0.7349(2) 0.2418(3) 0.0281(5) Uani 1 1 d . . . . .
C00O C 0.29844(11) 0.8159(2) 0.2330(3) 0.0311(6) Uani 1 1 d . . . . .
H00O H 0.274376 0.867117 0.265029 0.037 Uiso 1 1 calc R U . . .
C00P C 0.36931(11) 0.6661(2) 0.1442(3) 0.0280(6) Uani 1 1 d . . . . .
C00Q C 0.28109(11) 0.7498(2) 0.1322(3) 0.0320(6) Uani 1 1 d D . . . .
C00R C 0.34116(11) 0.5041(2) 0.5681(3) 0.0299(6) Uani 1 1 d . . . . .
H00R H 0.377406 0.493128 0.597377 0.036 Uiso 1 1 calc R U . . .
C00S C 0.26476(12) 0.4567(2) 0.4311(3) 0.0342(6) Uani 1 1 d . . . . .
H00S H 0.249024 0.413544 0.365177 0.041 Uiso 1 1 calc R U . . .
C00T C 0.25723(12) 0.5978(2) 0.5832(3) 0.0333(6) Uani 1 1 d . . . . .
H00T H 0.236463 0.650977 0.622864 0.040 Uiso 1 1 calc R U . . .
C00U C 0.31749(11) 0.6748(2) 0.0907(3) 0.0309(6) Uani 1 1 d . . . . .
H00U H 0.306466 0.627938 0.023441 0.037 Uiso 1 1 calc R U . . .
C00V C 0.43289(12) 0.6119(2) -0.0353(3) 0.0346(6) Uani 1 1 d . . . . .
H00A H 0.469522 0.582621 -0.033837 0.052 Uiso 1 1 calc R U . . .
H00B H 0.435322 0.686008 -0.047932 0.052 Uiso 1 1 calc R U . . .
H00C H 0.412125 0.581785 -0.109000 0.052 Uiso 1 1 calc R U . . .
C00W C 0.38921(13) 0.9772(2) 0.3395(3) 0.0370(7) Uani 1 1 d . . . . .
H00D H 0.399343 1.019724 0.416194 0.056 Uiso 1 1 calc R U . . .
H00E H 0.361823 1.012806 0.285789 0.056 Uiso 1 1 calc R U . . .
H00F H 0.421412 0.963947 0.284538 0.056 Uiso 1 1 calc R U . . .
C00X C 0.45455(12) 0.6617(2) 0.3848(3) 0.0353(6) Uani 1 1 d . . . . .
H00G H 0.479204 0.611253 0.342885 0.042 Uiso 1 1 calc R U . . .
H00H H 0.421740 0.624996 0.416078 0.042 Uiso 1 1 calc R U . . .
C00Y C 0.23446(11) 0.5349(2) 0.4871(3) 0.0358(6) Uani 1 1 d . . . . .
H00Y H 0.197956 0.545417 0.459467 0.043 Uiso 1 1 calc R U . . .
C00Z C 0.52418(13) 0.8544(3) 0.6168(3) 0.0455(8) Uani 1 1 d . . . . .
H00Z H 0.533915 0.924613 0.616940 0.055 Uiso 1 1 calc R U . . .
C010 C 0.48271(11) 0.7110(2) 0.5030(3) 0.0326(6) Uani 1 1 d . . . . .
C011 C 0.49760(12) 0.8127(2) 0.5059(3) 0.0359(6) Uani 1 1 d . . . . .
H011 H 0.489662 0.855010 0.431190 0.043 Uiso 1 1 calc R U . . .
C012 C 0.45928(13) 0.1589(2) 0.1180(3) 0.0390(7) Uani 1 1 d . . . . .
H01A H 0.476610 0.111752 0.054960 0.059 Uiso 1 1 calc R U . . .
H01B H 0.422104 0.135975 0.136232 0.059 Uiso 1 1 calc R U . . .
H01C H 0.480018 0.160187 0.201683 0.059 Uiso 1 1 calc R U . . .
C013 C 0.49469(13) 0.6517(3) 0.6142(3) 0.0483(8) Uani 1 1 d . . . . .
H013 H 0.484350 0.581770 0.615376 0.058 Uiso 1 1 calc R U . . .
C014 C 0.52178(14) 0.6933(4) 0.7247(3) 0.0546(10) Uani 1 1 d . . . . .
H014 H 0.530187 0.651319 0.799446 0.066 Uiso 1 1 calc R U . . .
C015 C 0.2232(4) 0.7568(11) 0.0738(13) 0.042(4) Uani 0.598(8) 1 d D . P A 1
C016 C 0.35579(13) 0.2670(2) 0.4855(3) 0.0380(7) Uani 1 1 d . . . . .
H01D H 0.365883 0.211853 0.424089 0.057 Uiso 1 1 calc R U . . .
H01E H 0.321539 0.249810 0.530060 0.057 Uiso 1 1 calc R U . . .
H01F H 0.384398 0.275792 0.552666 0.057 Uiso 1 1 calc R U . . .
C017 C 0.53623(12) 0.7947(3) 0.7252(3) 0.0486(9) Uani 1 1 d . . . . .
H017 H 0.554449 0.823173 0.800174 0.058 Uiso 1 1 calc R U . . .
C018 C 0.39453(19) 0.9264(3) 0.9611(3) 0.0553(10) Uani 1 1 d . . . . .
H01G H 0.421685 0.872825 0.975573 0.083 Uiso 1 1 calc R U . . .
H01H H 0.358271 0.899461 0.980777 0.083 Uiso 1 1 calc R U . . .
H01I H 0.402218 0.984347 1.020218 0.083 Uiso 1 1 calc R U . . .
C019 C 0.1909(2) 0.8476(6) 0.1279(7) 0.056(2) Uani 0.598(8) 1 d D . P A 1
H01J H 0.186236 0.840167 0.224714 0.085 Uiso 0.598(8) 1 calc R U P A 1
H01K H 0.155206 0.849779 0.084620 0.085 Uiso 0.598(8) 1 calc R U P A 1
H01L H 0.210591 0.911039 0.108907 0.085 Uiso 0.598(8) 1 calc R U P A 1
C1 C 0.2287(3) 0.7679(10) -0.0779(6) 0.079(3) Uani 0.598(8) 1 d D . P A 1
H1A H 0.247736 0.831693 -0.098746 0.118 Uiso 0.598(8) 1 calc R U P A 1
H1B H 0.192511 0.769021 -0.118679 0.118 Uiso 0.598(8) 1 calc R U P A 1
H1C H 0.249415 0.710038 -0.113611 0.118 Uiso 0.598(8) 1 calc R U P A 1
C2 C 0.1917(3) 0.6606(6) 0.1077(10) 0.072(3) Uani 0.598(8) 1 d D . P A 1
H2A H 0.210443 0.601072 0.070272 0.109 Uiso 0.598(8) 1 calc R U P A 1
H2B H 0.155074 0.665123 0.069554 0.109 Uiso 0.598(8) 1 calc R U P A 1
H2C H 0.189133 0.653455 0.205039 0.109 Uiso 0.598(8) 1 calc R U P A 1
C2A C 0.1817(3) 0.7626(10) 0.1608(10) 0.057(3) Uani 0.402(8) 1 d D . P A 2
H2AA H 0.181479 0.695942 0.205266 0.085 Uiso 0.402(8) 1 calc R U P A 2
H2AB H 0.146665 0.773656 0.116293 0.085 Uiso 0.402(8) 1 calc R U P A 2
H2AC H 0.187613 0.816455 0.227269 0.085 Uiso 0.402(8) 1 calc R U P A 2
C0 C 0.2272(7) 0.7655(13) 0.0571(19) 0.037(5) Uani 0.402(8) 1 d D . P A 2
C3 C 0.2278(4) 0.8688(9) -0.0128(12) 0.069(4) Uani 0.402(8) 1 d D . P A 2
H3A H 0.239853 0.921444 0.050278 0.104 Uiso 0.402(8) 1 calc R U P A 2
H3B H 0.191156 0.885141 -0.044514 0.104 Uiso 0.402(8) 1 calc R U P A 2
H3C H 0.252801 0.866302 -0.088970 0.104 Uiso 0.402(8) 1 calc R U P A 2
C1A C 0.2160(4) 0.6801(11) -0.0452(12) 0.067(4) Uani 0.402(8) 1 d D . P A 2
H1AA H 0.245868 0.677182 -0.109986 0.100 Uiso 0.402(8) 1 calc R U P A 2
H1AB H 0.181901 0.694254 -0.092164 0.100 Uiso 0.402(8) 1 calc R U P A 2
H1AC H 0.213214 0.614459 0.001415 0.100 Uiso 0.402(8) 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
O001 C00G 1.400(3) . ?
O001 C00J 1.356(3) . ?
O002 C00N 1.380(3) . ?
O002 C00X 1.436(3) . ?
O003 C00L 1.332(3) . ?
O003 C018 1.438(4) . ?
O004 C00I 1.348(3) . ?
O004 C012 1.431(4) . ?
N005 C00E 1.349(3) . ?
N005 C00F 1.331(4) . ?
N006 C00F 1.352(4) . ?
N006 C00I 1.320(4) . ?
N007 C00H 1.345(3) . ?
N007 C00L 1.332(3) . ?
N008 C00E 1.352(4) . ?
N008 C00I 1.327(4) . ?
N009 C00H 1.345(3) . ?
N009 C00K 1.433(4) . ?
N009 C00W 1.462(4) . ?
N00A C00F 1.359(4) . ?
N00A C00M 1.434(4) . ?
N00A C016 1.448(4) . ?
N00B C00E 1.351(4) . ?
N00B C00P 1.436(4) . ?
N00B C00V 1.465(3) . ?
N00C C00J 1.324(4) . ?
N00C C00L 1.330(4) . ?
N00D C00H 1.356(3) . ?
N00D C00J 1.319(3) . ?
C00G C00R 1.376(4) . ?
C00G C00T 1.378(4) . ?
C00K C00N 1.391(4) . ?
C00K C00O 1.387(4) . ?
C00M C00R 1.394(4) . ?
C00M C00S 1.384(4) . ?
C00N C00P 1.394(4) . ?
C00O H00O 0.9500 . ?
C00O C00Q 1.396(4) . ?
C00P C00U 1.388(4) . ?
C00Q C00U 1.393(4) . ?
C00Q C015 1.542(10) . ?
C00Q C0 1.539(16) . ?
C00R H00R 0.9500 . ?
C00S H00S 0.9500 . ?
C00S C00Y 1.386(4) . ?
C00T H00T 0.9500 . ?
C00T C00Y 1.385(4) . ?
C00U H00U 0.9500 . ?
C00V H00A 0.9800 . ?
C00V H00B 0.9800 . ?
C00V H00C 0.9800 . ?
C00W H00D 0.9800 . ?
C00W H00E 0.9800 . ?
C00W H00F 0.9800 . ?
C00X H00G 0.9900 . ?
C00X H00H 0.9900 . ?
C00X C010 1.515(4) . ?
C00Y H00Y 0.9500 . ?
C00Z H00Z 0.9500 . ?
C00Z C011 1.399(4) . ?
C00Z C017 1.368(5) . ?
C010 C011 1.381(4) . ?
C010 C013 1.388(4) . ?
C011 H011 0.9500 . ?
C012 H01A 0.9800 . ?
C012 H01B 0.9800 . ?
C012 H01C 0.9800 . ?
C013 H013 0.9500 . ?
C013 C014 1.401(5) . ?
C014 H014 0.9500 . ?
C014 C017 1.375(6) . ?
C015 C019 1.529(14) . ?
C015 C1 1.530(14) . ?
C015 C2 1.519(15) . ?
C016 H01D 0.9800 . ?
C016 H01E 0.9800 . ?
C016 H01F 0.9800 . ?
C017 H017 0.9500 . ?
C018 H01G 0.9800 . ?
C018 H01H 0.9800 . ?
C018 H01I 0.9800 . ?
C019 H01J 0.9800 . ?
C019 H01K 0.9800 . ?
C019 H01L 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2A C0 1.53(2) . ?
C0 C3 1.522(18) . ?
C0 C1A 1.540(17) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 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
C00J O001 C00G 116.5(2) . . ?
C00N O002 C00X 117.1(2) . . ?
C00L O003 C018 115.6(2) . . ?
C00I O004 C012 116.7(2) . . ?
C00F N005 C00E 114.0(2) . . ?
C00I N006 C00F 112.6(2) . . ?
C00L N007 C00H 113.7(2) . . ?
C00I N008 C00E 112.5(2) . . ?
C00H N009 C00K 120.6(2) . . ?
C00H N009 C00W 122.3(2) . . ?
C00K N009 C00W 116.8(2) . . ?
C00F N00A C00M 118.5(2) . . ?
C00F N00A C016 122.6(2) . . ?
C00M N00A C016 117.9(2) . . ?
C00E N00B C00P 120.2(2) . . ?
C00E N00B C00V 120.3(2) . . ?
C00P N00B C00V 117.8(2) . . ?
C00J N00C C00L 112.0(2) . . ?
C00J N00D C00H 113.0(2) . . ?
N005 C00E N008 125.7(3) . . ?
N005 C00E N00B 117.2(2) . . ?
N00B C00E N008 117.1(2) . . ?
N005 C00F N006 126.2(3) . . ?
N005 C00F N00A 116.7(2) . . ?
N006 C00F N00A 117.1(2) . . ?
C00R C00G O001 118.9(2) . . ?
C00R C00G C00T 121.9(3) . . ?
C00T C00G O001 119.1(3) . . ?
N007 C00H N009 118.7(2) . . ?
N007 C00H N00D 125.0(2) . . ?
N009 C00H N00D 116.3(2) . . ?
N006 C00I O004 118.6(2) . . ?
N006 C00I N008 128.9(3) . . ?
N008 C00I O004 112.5(2) . . ?
N00C C00J O001 113.0(2) . . ?
N00D C00J O001 118.1(2) . . ?
N00D C00J N00C 128.9(3) . . ?
C00N C00K N009 119.9(2) . . ?
C00O C00K N009 119.4(3) . . ?
C00O C00K C00N 120.7(3) . . ?
N007 C00L O003 114.1(2) . . ?
N00C C00L O003 118.3(2) . . ?
N00C C00L N007 127.5(3) . . ?
C00R C00M N00A 120.2(3) . . ?
C00S C00M N00A 119.5(3) . . ?
C00S C00M C00R 120.2(3) . . ?
O002 C00N C00K 118.7(2) . . ?
O002 C00N C00P 122.3(2) . . ?
C00K C00N C00P 118.8(2) . . ?
C00K C00O H00O 119.3 . . ?
C00K C00O C00Q 121.3(3) . . ?
C00Q C00O H00O 119.3 . . ?
C00N C00P N00B 121.1(2) . . ?
C00U C00P N00B 119.2(3) . . ?
C00U C00P C00N 119.7(3) . . ?
C00O C00Q C015 121.3(6) . . ?
C00O C00Q C0 122.3(7) . . ?
C00U C00Q C00O 117.1(3) . . ?
C00U C00Q C015 121.6(6) . . ?
C00U C00Q C0 120.3(7) . . ?
C00G C00R C00M 118.6(3) . . ?
C00G C00R H00R 120.7 . . ?
C00M C00R H00R 120.7 . . ?
C00M C00S H00S 120.0 . . ?
C00M C00S C00Y 120.0(3) . . ?
C00Y C00S H00S 120.0 . . ?
C00G C00T H00T 120.5 . . ?
C00G C00T C00Y 119.0(3) . . ?
C00Y C00T H00T 120.5 . . ?
C00P C00U C00Q 122.3(3) . . ?
C00P C00U H00U 118.8 . . ?
C00Q C00U H00U 118.8 . . ?
N00B C00V H00A 109.5 . . ?
N00B C00V H00B 109.5 . . ?
N00B C00V H00C 109.5 . . ?
H00A C00V H00B 109.5 . . ?
H00A C00V H00C 109.5 . . ?
H00B C00V H00C 109.5 . . ?
N009 C00W H00D 109.5 . . ?
N009 C00W H00E 109.5 . . ?
N009 C00W H00F 109.5 . . ?
H00D C00W H00E 109.5 . . ?
H00D C00W H00F 109.5 . . ?
H00E C00W H00F 109.5 . . ?
O002 C00X H00G 109.5 . . ?
O002 C00X H00H 109.5 . . ?
O002 C00X C010 110.6(2) . . ?
H00G C00X H00H 108.1 . . ?
C010 C00X H00G 109.5 . . ?
C010 C00X H00H 109.5 . . ?
C00S C00Y H00Y 119.9 . . ?
C00T C00Y C00S 120.2(3) . . ?
C00T C00Y H00Y 119.9 . . ?
C011 C00Z H00Z 119.8 . . ?
C017 C00Z H00Z 119.8 . . ?
C017 C00Z C011 120.4(3) . . ?
C011 C010 C00X 123.3(3) . . ?
C011 C010 C013 117.8(3) . . ?
C013 C010 C00X 118.9(3) . . ?
C00Z C011 H011 119.4 . . ?
C010 C011 C00Z 121.1(3) . . ?
C010 C011 H011 119.4 . . ?
O004 C012 H01A 109.5 . . ?
O004 C012 H01B 109.5 . . ?
O004 C012 H01C 109.5 . . ?
H01A C012 H01B 109.5 . . ?
H01A C012 H01C 109.5 . . ?
H01B C012 H01C 109.5 . . ?
C010 C013 H013 119.5 . . ?
C010 C013 C014 121.0(3) . . ?
C014 C013 H013 119.5 . . ?
C013 C014 H014 120.0 . . ?
C017 C014 C013 120.1(3) . . ?
C017 C014 H014 120.0 . . ?
C019 C015 C00Q 113.1(8) . . ?
C019 C015 C1 108.8(10) . . ?
C1 C015 C00Q 107.4(8) . . ?
C2 C015 C00Q 109.8(8) . . ?
C2 C015 C019 107.4(9) . . ?
C2 C015 C1 110.2(10) . . ?
N00A C016 H01D 109.5 . . ?
N00A C016 H01E 109.5 . . ?
N00A C016 H01F 109.5 . . ?
H01D C016 H01E 109.5 . . ?
H01D C016 H01F 109.5 . . ?
H01E C016 H01F 109.5 . . ?
C00Z C017 C014 119.5(3) . . ?
C00Z C017 H017 120.2 . . ?
C014 C017 H017 120.2 . . ?
O003 C018 H01G 109.5 . . ?
O003 C018 H01H 109.5 . . ?
O003 C018 H01I 109.5 . . ?
H01G C018 H01H 109.5 . . ?
H01G C018 H01I 109.5 . . ?
H01H C018 H01I 109.5 . . ?
C015 C019 H01J 109.5 . . ?
C015 C019 H01K 109.5 . . ?
C015 C019 H01L 109.5 . . ?
H01J C019 H01K 109.5 . . ?
H01J C019 H01L 109.5 . . ?
H01K C019 H01L 109.5 . . ?
C015 C1 H1A 109.5 . . ?
C015 C1 H1B 109.5 . . ?
C015 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C015 C2 H2A 109.5 . . ?
C015 C2 H2B 109.5 . . ?
C015 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C0 C2A H2AA 109.5 . . ?
C0 C2A H2AB 109.5 . . ?
C0 C2A H2AC 109.5 . . ?
C00Q C0 C1A 112.4(11) . . ?
C2A C0 C00Q 107.4(12) . . ?
C2A C0 C1A 107.6(12) . . ?
C3 C0 C00Q 109.5(11) . . ?
C3 C0 C2A 109.9(12) . . ?
C3 C0 C1A 110.0(14) . . ?
C0 C3 H3A 109.5 . . ?
C0 C3 H3B 109.5 . . ?
C0 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C0 C1A H1AA 109.5 . . ?
C0 C1A H1AB 109.5 . . ?
C0 C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 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
O001 C00G C00R C00M -179.8(2) . . . . ?
O001 C00G C00T C00Y -180.0(3) . . . . ?
O002 C00N C00P N00B 3.3(4) . . . . ?
O002 C00N C00P C00U -172.6(2) . . . . ?
O002 C00X C010 C011 -8.0(4) . . . . ?
O002 C00X C010 C013 172.4(3) . . . . ?
N009 C00K C00N O002 -4.1(4) . . . . ?
N009 C00K C00N C00P -179.7(2) . . . . ?
N009 C00K C00O C00Q 177.6(2) . . . . ?
N00A C00M C00R C00G 178.1(2) . . . . ?
N00A C00M C00S C00Y -179.1(3) . . . . ?
N00B C00P C00U C00Q -176.9(2) . . . . ?
C00E N005 C00F N006 1.0(4) . . . . ?
C00E N005 C00F N00A -178.4(2) . . . . ?
C00E N008 C00I O004 178.1(2) . . . . ?
C00E N008 C00I N006 -0.6(4) . . . . ?
C00E N00B C00P C00N 97.4(3) . . . . ?
C00E N00B C00P C00U -86.7(3) . . . . ?
C00F N005 C00E N008 1.2(4) . . . . ?
C00F N005 C00E N00B -178.0(2) . . . . ?
C00F N006 C00I O004 -176.2(2) . . . . ?
C00F N006 C00I N008 2.4(4) . . . . ?
C00F N00A C00M C00R -89.7(3) . . . . ?
C00F N00A C00M C00S 89.6(3) . . . . ?
C00G O001 C00J N00C 172.6(2) . . . . ?
C00G O001 C00J N00D -7.7(3) . . . . ?
C00G C00T C00Y C00S 0.9(4) . . . . ?
C00H N007 C00L O003 -179.7(2) . . . . ?
C00H N007 C00L N00C -0.6(4) . . . . ?
C00H N009 C00K C00N -82.2(3) . . . . ?
C00H N009 C00K C00O 100.8(3) . . . . ?
C00H N00D C00J O001 -179.3(2) . . . . ?
C00H N00D C00J N00C 0.4(4) . . . . ?
C00I N006 C00F N005 -2.6(4) . . . . ?
C00I N006 C00F N00A 176.8(2) . . . . ?
C00I N008 C00E N005 -1.4(4) . . . . ?
C00I N008 C00E N00B 177.8(2) . . . . ?
C00J O001 C00G C00R 103.2(3) . . . . ?
C00J O001 C00G C00T -78.7(3) . . . . ?
C00J N00C C00L O003 178.7(2) . . . . ?
C00J N00C C00L N007 -0.4(4) . . . . ?
C00J N00D C00H N007 -1.5(4) . . . . ?
C00J N00D C00H N009 179.4(2) . . . . ?
C00K N009 C00H N007 179.9(2) . . . . ?
C00K N009 C00H N00D -0.9(4) . . . . ?
C00K C00N C00P N00B 178.7(2) . . . . ?
C00K C00N C00P C00U 2.8(4) . . . . ?
C00K C00O C00Q C00U 1.3(4) . . . . ?
C00K C00O C00Q C015 178.7(7) . . . . ?
C00K C00O C00Q C0 -171.5(9) . . . . ?
C00L N007 C00H N009 -179.3(2) . . . . ?
C00L N007 C00H N00D 1.6(4) . . . . ?
C00L N00C C00J O001 -179.8(2) . . . . ?
C00L N00C C00J N00D 0.5(4) . . . . ?
C00M N00A C00F N005 0.9(4) . . . . ?
C00M N00A C00F N006 -178.6(2) . . . . ?
C00M C00S C00Y C00T -0.1(5) . . . . ?
C00N O002 C00X C010 -130.5(2) . . . . ?
C00N C00K C00O C00Q 0.7(4) . . . . ?
C00N C00P C00U C00Q -0.8(4) . . . . ?
C00O C00K C00N O002 172.9(2) . . . . ?
C00O C00K C00N C00P -2.7(4) . . . . ?
C00O C00Q C00U C00P -1.2(4) . . . . ?
C00O C00Q C015 C019 5.5(12) . . . . ?
C00O C00Q C015 C1 125.6(9) . . . . ?
C00O C00Q C015 C2 -114.5(8) . . . . ?
C00O C00Q C0 C2A -59.5(13) . . . . ?
C00O C00Q C0 C3 59.8(15) . . . . ?
C00O C00Q C0 C1A -177.6(9) . . . . ?
C00P N00B C00E N005 -11.5(4) . . . . ?
C00P N00B C00E N008 169.3(2) . . . . ?
C00R C00G C00T C00Y -2.0(4) . . . . ?
C00R C00M C00S C00Y 0.3(4) . . . . ?
C00S C00M C00R C00G -1.3(4) . . . . ?
C00T C00G C00R C00M 2.2(4) . . . . ?
C00U C00Q C015 C019 -177.2(6) . . . . ?
C00U C00Q C015 C1 -57.1(12) . . . . ?
C00U C00Q C015 C2 62.8(10) . . . . ?
C00U C00Q C0 C2A 127.9(9) . . . . ?
C00U C00Q C0 C3 -112.8(10) . . . . ?
C00U C00Q C0 C1A 9.8(17) . . . . ?
C00V N00B C00E N005 -176.2(2) . . . . ?
C00V N00B C00E N008 4.6(4) . . . . ?
C00V N00B C00P C00N -97.6(3) . . . . ?
C00V N00B C00P C00U 78.4(3) . . . . ?
C00W N009 C00H N007 6.1(4) . . . . ?
C00W N009 C00H N00D -174.7(2) . . . . ?
C00W N009 C00K C00N 92.0(3) . . . . ?
C00W N009 C00K C00O -85.1(3) . . . . ?
C00X O002 C00N C00K 105.2(3) . . . . ?
C00X O002 C00N C00P -79.4(3) . . . . ?
C00X C010 C011 C00Z -179.2(3) . . . . ?
C00X C010 C013 C014 178.6(3) . . . . ?
C010 C013 C014 C017 1.0(5) . . . . ?
C011 C00Z C017 C014 -0.3(5) . . . . ?
C011 C010 C013 C014 -1.0(5) . . . . ?
C012 O004 C00I N006 -2.5(4) . . . . ?
C012 O004 C00I N008 178.7(2) . . . . ?
C013 C010 C011 C00Z 0.4(4) . . . . ?
C013 C014 C017 C00Z -0.3(5) . . . . ?
C015 C00Q C00U C00P -178.6(7) . . . . ?
C016 N00A C00F N005 -167.9(3) . . . . ?
C016 N00A C00F N006 12.6(4) . . . . ?
C016 N00A C00M C00R 79.6(3) . . . . ?
C016 N00A C00M C00S -101.0(3) . . . . ?
C017 C00Z C011 C010 0.3(5) . . . . ?
C018 O003 C00L N007 178.9(3) . . . . ?
C018 O003 C00L N00C -0.2(4) . . . . ?
C0 C00Q C00U C00P 171.8(9) . . . . ?

_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 2.634
_oxdiff_exptl_absorpt_empirical_full_min 0.571
####################################################################### 
# 
# 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_A_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2303853'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2023-10-26 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;
_audit_creation_date             2023-10-10
# end Validation Reply Form 
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H37 N9 O5, 4(C0.125 Cl0.25)'
_chemical_formula_sum            'C34.50 H38 Cl N9 O5'
_chemical_formula_weight         694.19
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   14.2497(2)
_cell_length_b                   36.7753(5)
_cell_length_c                   14.4950(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7595.92(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6052
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.500
_cell_measurement_theta_min      3.326
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            34722
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         3.326
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5582
_reflns_number_total             6052
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_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, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.021
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00052(11)
_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   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6052
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0857
_refine_ls_restrained_S_all      1.246
_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)+(0.1464P)²+10.8090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2538
_refine_ls_wR_factor_ref         0.2575
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{C35, C35A}
2. Restrained distances
 C35-Cl1 = C35A-Cl1A
 1.76 with sigma of 0.01
 C36-Cl2 = C36-Cl3
 1.76 with sigma of 0.01
 Cl2-Cl3
 2.85 with sigma of 0.02
 C37-Cl4 = C37-Cl5
 1.76 with sigma of 0.01
 Cl4-Cl5
 2.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(Cl1)
\\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl4) \\sim Ueq,
Uanis(Cl5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq, Uanis(Cl1A) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C35A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) = Uanis(C35A)
Uanis(C36) = Uanis(Cl2) = Uanis(Cl3)
Uanis(Cl4) = Uanis(Cl5) = Uanis(C37)
Uanis(C35) = Uanis(C35A) = Uanis(Cl1) = Uanis(Cl1A)
4. Others
 Fixed Sof: C35(0.125) C35A(0.125) C36(0.125) C37(0.125) Cl1(0.25) Cl1A(0.25)
 Cl2(0.125) Cl3(0.125) Cl4(0.125) Cl5(0.125)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
5.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5A), C11(H11A), C13(H13A), C14(H14A), C27(H27A), C28(H28A),
 C29(H29A), C30(H30A), C31(H31A), N5(H5B)
;
_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 0.4039(2) 0.61787(9) 0.3435(2) 0.0222(7) Uani 1 1 d . . . . .
C2 C 0.4210(2) 0.58137(9) 0.3231(2) 0.0226(7) Uani 1 1 d . . . . .
C3 C 0.4529(2) 0.57119(9) 0.2370(2) 0.0228(7) Uani 1 1 d . . . . .
H3A H 0.462334 0.546148 0.223817 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4717(2) 0.59723(9) 0.1684(2) 0.0256(7) Uani 1 1 d . . . . .
C5 C 0.4567(2) 0.63344(10) 0.1910(2) 0.0266(8) Uani 1 1 d . . . . .
H5A H 0.469831 0.651670 0.146420 0.032 Uiso 1 1 calc R U . . .
C6 C 0.4231(2) 0.64377(9) 0.2767(2) 0.0247(7) Uani 1 1 d . . . . .
C7 C 0.3092(3) 0.69410(10) 0.2967(3) 0.0389(9) Uani 1 1 d . . . . .
H7A H 0.267565 0.673864 0.280721 0.058 Uiso 1 1 calc R U . . .
H7B H 0.293094 0.703219 0.358263 0.058 Uiso 1 1 calc R U . . .
H7C H 0.301822 0.713666 0.251430 0.058 Uiso 1 1 calc R U . . .
C8 C 0.4789(2) 0.70369(9) 0.3162(2) 0.0252(7) Uani 1 1 d . . . . .
C9 C 0.5376(2) 0.75921(9) 0.3410(3) 0.0297(8) Uani 1 1 d . . . . .
C10 C 0.6341(2) 0.71129(9) 0.3388(2) 0.0255(7) Uani 1 1 d . . . . .
C11 C 0.7052(2) 0.64027(9) 0.4318(2) 0.0256(7) Uani 1 1 d . . . . .
H11A H 0.677711 0.653300 0.481457 0.031 Uiso 1 1 calc R U . . .
C12 C 0.7350(2) 0.65882(9) 0.3533(2) 0.0266(7) Uani 1 1 d . . . . .
C13 C 0.7757(2) 0.63948(9) 0.2820(2) 0.0274(7) Uani 1 1 d . . . . .
H13A H 0.795733 0.651885 0.227973 0.033 Uiso 1 1 calc R U . . .
C14 C 0.7876(2) 0.60188(9) 0.2886(2) 0.0269(7) Uani 1 1 d . . . . .
H14A H 0.816325 0.588894 0.239512 0.032 Uiso 1 1 calc R U . . .
C15 C 0.7576(2) 0.58349(9) 0.3664(2) 0.0233(7) Uani 1 1 d . . . . .
C16 C 0.7155(2) 0.60325(9) 0.4376(2) 0.0234(7) Uani 1 1 d . . . . .
C17 C 0.6078(2) 0.56808(8) 0.5234(2) 0.0205(7) Uani 1 1 d . . . . .
C18 C 0.5084(2) 0.53591(8) 0.6070(2) 0.0215(7) Uani 1 1 d . . . . .
C19 C 0.4677(2) 0.55375(8) 0.4653(2) 0.0201(7) Uani 1 1 d . . . . .
C20 C 0.3115(2) 0.53980(9) 0.4052(2) 0.0264(7) Uani 1 1 d . . . . .
H20A H 0.276573 0.542863 0.347500 0.040 Uiso 1 1 calc R U . . .
H20B H 0.315688 0.513878 0.420322 0.040 Uiso 1 1 calc R U . . .
H20C H 0.278834 0.552637 0.455062 0.040 Uiso 1 1 calc R U . . .
C21 C 0.5076(2) 0.58526(11) 0.0733(2) 0.0317(8) Uani 1 1 d . . . . .
C22 C 0.5414(5) 0.61766(15) 0.0166(4) 0.0719(17) Uani 1 1 d . . . . .
H22A H 0.489864 0.635064 0.009122 0.108 Uiso 1 1 calc R U . . .
H22B H 0.593816 0.629490 0.048443 0.108 Uiso 1 1 calc R U . . .
H22C H 0.562195 0.609257 -0.044228 0.108 Uiso 1 1 calc R U . . .
C23 C 0.5890(3) 0.55921(15) 0.0830(3) 0.0562(13) Uani 1 1 d . . . . .
H23A H 0.640148 0.571130 0.116665 0.084 Uiso 1 1 calc R U . . .
H23B H 0.568589 0.537591 0.117081 0.084 Uiso 1 1 calc R U . . .
H23C H 0.611166 0.551999 0.021681 0.084 Uiso 1 1 calc R U . . .
C24 C 0.4279(4) 0.5670(2) 0.0211(3) 0.0764(19) Uani 1 1 d . . . . .
H24A H 0.375350 0.584017 0.014981 0.115 Uiso 1 1 calc R U . . .
H24B H 0.449758 0.559796 -0.040358 0.115 Uiso 1 1 calc R U . . .
H24C H 0.407181 0.545388 0.055042 0.115 Uiso 1 1 calc R U . . .
C25 C 0.4213(2) 0.64713(9) 0.4908(2) 0.0286(8) Uani 1 1 d . . . . .
H25A H 0.403117 0.673100 0.488970 0.034 Uiso 1 1 calc R U . . .
H25B H 0.488492 0.645143 0.474135 0.034 Uiso 1 1 calc R U . . .
C26 C 0.4048(2) 0.63175(9) 0.5855(2) 0.0242(7) Uani 1 1 d . . . . .
C27 C 0.3139(2) 0.62143(9) 0.6117(2) 0.0291(8) Uani 1 1 d . . . . .
H27A H 0.263091 0.625044 0.570295 0.035 Uiso 1 1 calc R U . . .
C28 C 0.2978(2) 0.60603(10) 0.6971(3) 0.0306(8) Uani 1 1 d . . . . .
H28A H 0.235938 0.599183 0.714386 0.037 Uiso 1 1 calc R U . . .
C29 C 0.3715(3) 0.60057(10) 0.7577(3) 0.0324(8) Uani 1 1 d . . . . .
H29A H 0.360592 0.589804 0.816268 0.039 Uiso 1 1 calc R U . . .
C30 C 0.4613(3) 0.61088(11) 0.7324(3) 0.0341(8) Uani 1 1 d . . . . .
H30A H 0.512021 0.607293 0.773927 0.041 Uiso 1 1 calc R U . . .
C31 C 0.4777(2) 0.62639(10) 0.6468(2) 0.0295(8) Uani 1 1 d . . . . .
H31A H 0.539552 0.633408 0.630146 0.035 Uiso 1 1 calc R U . . .
C32 C 0.4344(3) 0.80931(11) 0.3483(4) 0.0494(11) Uani 1 1 d . . . . .
H32A H 0.436007 0.835720 0.357114 0.074 Uiso 1 1 calc R U . . .
H32B H 0.406579 0.803722 0.288109 0.074 Uiso 1 1 calc R U . . .
H32C H 0.396584 0.798156 0.397166 0.074 Uiso 1 1 calc R U . . .
C33 C 0.8213(3) 0.52739(10) 0.3166(3) 0.0367(9) Uani 1 1 d . . . . .
H33A H 0.822905 0.501627 0.333783 0.055 Uiso 1 1 calc R U . . .
H33B H 0.793777 0.529954 0.255015 0.055 Uiso 1 1 calc R U . . .
H33C H 0.885357 0.537130 0.316272 0.055 Uiso 1 1 calc R U . . .
C34 C 0.3964(2) 0.50599(10) 0.6995(2) 0.0292(8) Uani 1 1 d . . . . .
H34A H 0.390433 0.495104 0.760947 0.044 Uiso 1 1 calc R U . . .
H34B H 0.350782 0.525772 0.693006 0.044 Uiso 1 1 calc R U . . .
H34C H 0.384290 0.487439 0.652436 0.044 Uiso 1 1 calc R U . . .
C35 C 0.250000 0.750000 0.4944(10) 0.120(2) Uani 0.25 2 d DS TU P A 1
C35A C 0.250000 0.750000 0.4944(10) 0.120(2) Uani 0.25 2 d DS TU P B 2
C36 C 0.5961(11) 0.7152(5) 0.599(3) 0.081(2) Uani 0.125 1 d D U P C 1
C37 C 0.5265(14) 0.7357(6) 0.588(5) 0.110(3) Uani 0.125 1 d D U P D 2
N1 N 0.40596(19) 0.68157(8) 0.2965(2) 0.0273(7) Uani 1 1 d . . . . .
N2 N 0.56322(19) 0.68789(7) 0.3240(2) 0.0261(6) Uani 1 1 d . . . . .
N3 N 0.4603(2) 0.73943(8) 0.3275(2) 0.0307(7) Uani 1 1 d . . . . .
N4 N 0.6261(2) 0.74780(8) 0.3460(2) 0.0294(7) Uani 1 1 d . . . . .
N5 N 0.72061(19) 0.69697(8) 0.3470(2) 0.0295(7) Uani 1 1 d . . . . .
H5B H 0.769460 0.711597 0.348511 0.035 Uiso 1 1 calc R U . . .
N6 N 0.55050(18) 0.57107(7) 0.45272(18) 0.0217(6) Uani 1 1 d . . . . .
N7 N 0.59403(18) 0.55075(7) 0.60264(18) 0.0227(6) Uani 1 1 d . . . . .
N8 N 0.44299(18) 0.53573(7) 0.54176(18) 0.0217(6) Uani 1 1 d . . . . .
N9 N 0.40622(18) 0.55482(7) 0.39453(18) 0.0222(6) Uani 1 1 d . . . . .
O1 O 0.69141(14) 0.58556(6) 0.52001(15) 0.0234(5) Uani 1 1 d . . . . .
O2 O 0.36454(15) 0.62634(6) 0.42719(15) 0.0266(6) Uani 1 1 d . . . . .
O3 O 0.52871(18) 0.79505(6) 0.3520(2) 0.0392(7) Uani 1 1 d . . . . .
O4 O 0.76600(16) 0.54700(6) 0.38178(16) 0.0279(6) Uani 1 1 d . . . . .
O5 O 0.48977(16) 0.52014(6) 0.68796(16) 0.0266(6) Uani 1 1 d . . . . .
Cl1 Cl 0.2201(8) 0.7065(2) 0.5486(7) 0.120(2) Uani 0.25 1 d D U P A 1
Cl1A Cl 0.2569(9) 0.7144(3) 0.5692(6) 0.120(2) Uani 0.25 1 d D U P B 2
Cl2 Cl 0.7019(9) 0.7409(4) 0.5929(7) 0.081(2) Uani 0.125 1 d D U P C 1
Cl3 Cl 0.5117(9) 0.7497(4) 0.5861(8) 0.081(2) Uani 0.125 1 d D U P C 1
Cl4 Cl 0.6175(12) 0.7682(5) 0.5895(8) 0.110(3) Uani 0.125 1 d D U P D 2
Cl5 Cl 0.4253(12) 0.7633(5) 0.5798(9) 0.110(3) Uani 0.125 1 d D U P D 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 C2 1.396(5) . ?
C1 C6 1.385(5) . ?
C1 O2 1.373(4) . ?
C2 C3 1.381(5) . ?
C2 N9 1.438(4) . ?
C3 H3A 0.9500 . ?
C3 C4 1.406(5) . ?
C4 C5 1.388(5) . ?
C4 C21 1.535(5) . ?
C5 H5A 0.9500 . ?
C5 C6 1.384(5) . ?
C6 N1 1.440(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 N1 1.453(4) . ?
C8 N1 1.350(4) . ?
C8 N2 1.340(4) . ?
C8 N3 1.351(4) . ?
C9 N3 1.335(5) . ?
C9 N4 1.330(5) . ?
C9 O3 1.334(4) . ?
C10 N2 1.344(4) . ?
C10 N4 1.352(4) . ?
C10 N5 1.346(4) . ?
C11 H11A 0.9500 . ?
C11 C12 1.392(5) . ?
C11 C16 1.372(5) . ?
C12 C13 1.382(5) . ?
C12 N5 1.421(4) . ?
C13 H13A 0.9500 . ?
C13 C14 1.397(5) . ?
C14 H14A 0.9500 . ?
C14 C15 1.382(5) . ?
C15 C16 1.398(5) . ?
C15 O4 1.366(4) . ?
C16 O1 1.403(4) . ?
C17 N6 1.315(4) . ?
C17 N7 1.328(4) . ?
C17 O1 1.355(4) . ?
C18 N7 1.338(4) . ?
C18 N8 1.328(4) . ?
C18 O5 1.336(4) . ?
C19 N6 1.353(4) . ?
C19 N8 1.338(4) . ?
C19 N9 1.350(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 N9 1.467(4) . ?
C21 C22 1.525(6) . ?
C21 C23 1.511(6) . ?
C21 C24 1.521(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.504(5) . ?
C25 O2 1.445(4) . ?
C26 C27 1.401(5) . ?
C26 C31 1.380(5) . ?
C27 H27A 0.9500 . ?
C27 C28 1.382(5) . ?
C28 H28A 0.9500 . ?
C28 C29 1.384(5) . ?
C29 H29A 0.9500 . ?
C29 C30 1.384(5) . ?
C30 H30A 0.9500 . ?
C30 C31 1.385(5) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32 O3 1.443(5) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 O4 1.426(4) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C34 O5 1.439(4) . ?
C35 Cl1 1.832(9) . ?
C35 Cl1 1.833(9) 2_565 ?
C35A Cl1A 1.704(9) . ?
C35A Cl1A 1.704(9) 2_565 ?
C36 Cl2 1.780(10) . ?
C36 Cl3 1.759(10) . ?
C37 Cl4 1.764(10) . ?
C37 Cl5 1.766(10) . ?
N5 H5B 0.8800 . ?
Cl2 Cl2 1.53(3) 2_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 118.6(3) . . ?
O2 C1 C2 118.5(3) . . ?
O2 C1 C6 122.8(3) . . ?
C1 C2 N9 118.4(3) . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 N9 121.0(3) . . ?
C2 C3 H3A 119.4 . . ?
C2 C3 C4 121.2(3) . . ?
C4 C3 H3A 119.4 . . ?
C3 C4 C21 120.2(3) . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 C21 122.6(3) . . ?
C4 C5 H5A 119.0 . . ?
C6 C5 C4 121.9(3) . . ?
C6 C5 H5A 119.0 . . ?
C1 C6 N1 119.4(3) . . ?
C5 C6 C1 120.4(3) . . ?
C5 C6 N1 120.1(3) . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
N1 C8 N3 117.4(3) . . ?
N2 C8 N1 116.5(3) . . ?
N2 C8 N3 126.0(3) . . ?
N4 C9 N3 128.2(3) . . ?
N4 C9 O3 113.3(3) . . ?
O3 C9 N3 118.5(3) . . ?
N2 C10 N4 125.8(3) . . ?
N2 C10 N5 116.9(3) . . ?
N5 C10 N4 117.3(3) . . ?
C12 C11 H11A 119.9 . . ?
C16 C11 H11A 119.9 . . ?
C16 C11 C12 120.3(3) . . ?
C11 C12 N5 119.5(3) . . ?
C13 C12 C11 119.1(3) . . ?
C13 C12 N5 121.4(3) . . ?
C12 C13 H13A 119.7 . . ?
C12 C13 C14 120.6(3) . . ?
C14 C13 H13A 119.7 . . ?
C13 C14 H14A 119.9 . . ?
C15 C14 C13 120.2(3) . . ?
C15 C14 H14A 119.9 . . ?
C14 C15 C16 118.7(3) . . ?
O4 C15 C14 126.0(3) . . ?
O4 C15 C16 115.3(3) . . ?
C11 C16 C15 121.0(3) . . ?
C11 C16 O1 119.1(3) . . ?
C15 C16 O1 119.5(3) . . ?
N6 C17 N7 128.5(3) . . ?
N6 C17 O1 118.5(3) . . ?
N7 C17 O1 112.9(3) . . ?
N8 C18 N7 127.5(3) . . ?
N8 C18 O5 118.9(3) . . ?
O5 C18 N7 113.6(3) . . ?
N8 C19 N6 125.1(3) . . ?
N8 C19 N9 118.2(3) . . ?
N9 C19 N6 116.7(3) . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N9 C20 H20A 109.5 . . ?
N9 C20 H20B 109.5 . . ?
N9 C20 H20C 109.5 . . ?
C22 C21 C4 111.4(3) . . ?
C23 C21 C4 110.7(3) . . ?
C23 C21 C22 107.7(4) . . ?
C23 C21 C24 109.9(4) . . ?
C24 C21 C4 108.9(3) . . ?
C24 C21 C22 108.2(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H25A C25 H25B 108.5 . . ?
C26 C25 H25A 110.3 . . ?
C26 C25 H25B 110.3 . . ?
O2 C25 H25A 110.3 . . ?
O2 C25 H25B 110.3 . . ?
O2 C25 C26 107.2(3) . . ?
C27 C26 C25 119.6(3) . . ?
C31 C26 C25 121.6(3) . . ?
C31 C26 C27 118.9(3) . . ?
C26 C27 H27A 119.8 . . ?
C28 C27 C26 120.5(3) . . ?
C28 C27 H27A 119.8 . . ?
C27 C28 H28A 120.0 . . ?
C27 C28 C29 120.1(3) . . ?
C29 C28 H28A 120.0 . . ?
C28 C29 H29A 120.2 . . ?
C28 C29 C30 119.6(3) . . ?
C30 C29 H29A 120.2 . . ?
C29 C30 H30A 119.8 . . ?
C29 C30 C31 120.4(3) . . ?
C31 C30 H30A 119.8 . . ?
C26 C31 C30 120.5(3) . . ?
C26 C31 H31A 119.7 . . ?
C30 C31 H31A 119.7 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O3 C32 H32A 109.5 . . ?
O3 C32 H32B 109.5 . . ?
O3 C32 H32C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O4 C33 H33A 109.5 . . ?
O4 C33 H33B 109.5 . . ?
O4 C33 H33C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O5 C34 H34A 109.5 . . ?
O5 C34 H34B 109.5 . . ?
O5 C34 H34C 109.5 . . ?
Cl1 C35 Cl1 129.2(11) . 2_565 ?
Cl1A C35A Cl1A 101.0(11) 2_565 . ?
Cl3 C36 Cl2 101.0(9) . . ?
Cl4 C37 Cl5 102.3(10) . . ?
C6 N1 C7 117.9(3) . . ?
C8 N1 C6 119.5(3) . . ?
C8 N1 C7 122.6(3) . . ?
C8 N2 C10 114.2(3) . . ?
C9 N3 C8 112.7(3) . . ?
C9 N4 C10 112.9(3) . . ?
C10 N5 C12 121.6(3) . . ?
C10 N5 H5B 119.2 . . ?
C12 N5 H5B 119.2 . . ?
C17 N6 C19 113.4(3) . . ?
C17 N7 C18 111.8(3) . . ?
C18 N8 C19 113.7(3) . . ?
C2 N9 C20 117.8(3) . . ?
C19 N9 C2 118.1(3) . . ?
C19 N9 C20 120.4(3) . . ?
C17 O1 C16 117.8(2) . . ?
C1 O2 C25 117.1(2) . . ?
C9 O3 C32 116.3(3) . . ?
C15 O4 C33 115.9(3) . . ?
C18 O5 C34 116.3(2) . . ?
Cl2 Cl2 C36 173.4(13) 2_665 . ?

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 1.9(5) . . . . ?
C1 C2 N9 C19 -71.8(4) . . . . ?
C1 C2 N9 C20 86.8(4) . . . . ?
C1 C6 N1 C7 -74.9(4) . . . . ?
C1 C6 N1 C8 103.5(4) . . . . ?
C2 C1 C6 C5 1.4(5) . . . . ?
C2 C1 C6 N1 -179.9(3) . . . . ?
C2 C1 O2 C25 114.8(3) . . . . ?
C2 C3 C4 C5 -0.1(4) . . . . ?
C2 C3 C4 C21 179.7(3) . . . . ?
C3 C2 N9 C19 107.2(3) . . . . ?
C3 C2 N9 C20 -94.2(4) . . . . ?
C3 C4 C5 C6 -1.1(5) . . . . ?
C3 C4 C21 C22 -168.8(4) . . . . ?
C3 C4 C21 C23 -49.0(5) . . . . ?
C3 C4 C21 C24 71.9(5) . . . . ?
C4 C5 C6 C1 0.5(5) . . . . ?
C4 C5 C6 N1 -178.2(3) . . . . ?
C5 C4 C21 C22 10.9(5) . . . . ?
C5 C4 C21 C23 130.7(4) . . . . ?
C5 C4 C21 C24 -108.4(5) . . . . ?
C5 C6 N1 C7 103.8(4) . . . . ?
C5 C6 N1 C8 -77.8(4) . . . . ?
C6 C1 C2 C3 -2.6(4) . . . . ?
C6 C1 C2 N9 176.4(3) . . . . ?
C6 C1 O2 C25 -68.4(4) . . . . ?
C11 C12 C13 C14 -0.5(5) . . . . ?
C11 C12 N5 C10 -68.4(4) . . . . ?
C11 C16 O1 C17 101.4(3) . . . . ?
C12 C11 C16 C15 1.4(5) . . . . ?
C12 C11 C16 O1 175.3(3) . . . . ?
C12 C13 C14 C15 0.8(5) . . . . ?
C13 C12 N5 C10 109.8(4) . . . . ?
C13 C14 C15 C16 0.0(5) . . . . ?
C13 C14 C15 O4 -179.2(3) . . . . ?
C14 C15 C16 C11 -1.1(5) . . . . ?
C14 C15 C16 O1 -175.0(3) . . . . ?
C14 C15 O4 C33 8.5(5) . . . . ?
C15 C16 O1 C17 -84.7(3) . . . . ?
C16 C11 C12 C13 -0.6(5) . . . . ?
C16 C11 C12 N5 177.6(3) . . . . ?
C16 C15 O4 C33 -170.8(3) . . . . ?
C21 C4 C5 C6 179.1(3) . . . . ?
C25 C26 C27 C28 177.7(3) . . . . ?
C25 C26 C31 C30 -177.5(3) . . . . ?
C26 C25 O2 C1 -140.0(3) . . . . ?
C26 C27 C28 C29 -0.2(5) . . . . ?
C27 C26 C31 C30 0.4(5) . . . . ?
C27 C28 C29 C30 0.5(5) . . . . ?
C28 C29 C30 C31 -0.4(6) . . . . ?
C29 C30 C31 C26 -0.1(5) . . . . ?
C31 C26 C27 C28 -0.3(5) . . . . ?
N1 C8 N2 C10 176.7(3) . . . . ?
N1 C8 N3 C9 -176.1(3) . . . . ?
N2 C8 N1 C6 -5.8(5) . . . . ?
N2 C8 N1 C7 172.5(3) . . . . ?
N2 C8 N3 C9 5.0(5) . . . . ?
N2 C10 N4 C9 2.8(5) . . . . ?
N2 C10 N5 C12 -8.9(5) . . . . ?
N3 C8 N1 C6 175.2(3) . . . . ?
N3 C8 N1 C7 -6.5(5) . . . . ?
N3 C8 N2 C10 -4.4(5) . . . . ?
N3 C9 N4 C10 -2.0(5) . . . . ?
N3 C9 O3 C32 0.1(5) . . . . ?
N4 C9 N3 C8 -1.5(5) . . . . ?
N4 C9 O3 C32 -179.3(4) . . . . ?
N4 C10 N2 C8 0.1(5) . . . . ?
N4 C10 N5 C12 171.1(3) . . . . ?
N5 C10 N2 C8 -179.9(3) . . . . ?
N5 C10 N4 C9 -177.3(3) . . . . ?
N5 C12 C13 C14 -178.7(3) . . . . ?
N6 C17 N7 C18 -1.9(4) . . . . ?
N6 C17 O1 C16 -5.5(4) . . . . ?
N6 C19 N8 C18 -0.3(4) . . . . ?
N6 C19 N9 C2 -16.1(4) . . . . ?
N6 C19 N9 C20 -174.2(3) . . . . ?
N7 C17 N6 C19 -0.2(5) . . . . ?
N7 C17 O1 C16 176.8(3) . . . . ?
N7 C18 N8 C19 -2.2(5) . . . . ?
N7 C18 O5 C34 175.6(3) . . . . ?
N8 C18 N7 C17 3.1(4) . . . . ?
N8 C18 O5 C34 -3.7(4) . . . . ?
N8 C19 N6 C17 1.4(4) . . . . ?
N8 C19 N9 C2 164.2(3) . . . . ?
N8 C19 N9 C20 6.1(4) . . . . ?
N9 C2 C3 C4 -177.0(3) . . . . ?
N9 C19 N6 C17 -178.3(3) . . . . ?
N9 C19 N8 C18 179.3(3) . . . . ?
O1 C17 N6 C19 -177.4(3) . . . . ?
O1 C17 N7 C18 175.5(2) . . . . ?
O2 C1 C2 C3 174.4(3) . . . . ?
O2 C1 C2 N9 -6.7(4) . . . . ?
O2 C1 C6 C5 -175.4(3) . . . . ?
O2 C1 C6 N1 3.3(5) . . . . ?
O2 C25 C26 C27 -40.3(4) . . . . ?
O2 C25 C26 C31 137.6(3) . . . . ?
O3 C9 N3 C8 179.2(3) . . . . ?
O3 C9 N4 C10 177.3(3) . . . . ?
O4 C15 C16 C11 178.2(3) . . . . ?
O4 C15 C16 O1 4.4(4) . . . . ?
O5 C18 N7 C17 -176.1(3) . . . . ?
O5 C18 N8 C19 177.0(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT097_A                   
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.02 eA-3  
RESPONSE: Due to the disorder of solvent CH2Cl2 molecules.
;
####################################################################### 
# 
# 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_A_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2304020'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2023-10-27 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36.25 H42 N9 O4.50'
_chemical_formula_weight         675.79

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'

_space_group_crystal_system      hexagonal
_space_group_IT_number           180
_space_group_name_H-M_alt        'P 62 2 2'
_space_group_name_Hall           'P 62 2c (0 0 1)'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z'
'y, -x+y, z+2/3'
'x-y, x, z+1/3'
'y, x, -z+2/3'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'-y, -x, -z+2/3'
'-x+y, y, -z'
'x, x-y, -z+1/3'

_cell_length_a                   17.07750(10)
_cell_length_b                   17.07750(10)
_cell_length_c                   48.3005(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     12199.18(16)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6484
_cell_measurement_theta_min      3.504
_cell_measurement_theta_max      62.491

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_F_000             4302
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.611
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.47671
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            238456
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_theta_min         3.504
_diffrn_reflns_theta_max         62.491
_diffrn_reflns_theta_full        62.491
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6484
_reflns_number_gt                6082
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.688
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0925P)²+8.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00044(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 2396 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6484
_refine_ls_number_parameters     482
_refine_ls_number_restraints     131
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1486
_refine_ls_wR_factor_gt          0.1454
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1777(2) 0.6482(3) 0.54327(8) 0.0322(8) Uani 1 1 d . . . . .
C2 C 0.2914(2) 0.6370(2) 0.56080(8) 0.0322(8) Uani 1 1 d . . . . .
C3 C 0.2232(2) 0.6944(2) 0.58646(8) 0.0315(8) Uani 1 1 d . . . . .
C4 C 0.2818(3) 0.7577(3) 0.63227(8) 0.0402(9) Uani 1 1 d . . . . .
H4A H 0.265086 0.783534 0.647734 0.060 Uiso 1 1 calc R U . . .
H4B H 0.283690 0.704171 0.638647 0.060 Uiso 1 1 calc R U . . .
H4C H 0.341481 0.802658 0.625259 0.060 Uiso 1 1 calc R U . . .
C5 C 0.1543(3) 0.8353(3) 0.61279(7) 0.0322(8) Uani 1 1 d . . . . .
C6 C 0.1407(3) 0.7474(3) 0.61378(8) 0.0322(8) Uani 1 1 d . . . . .
C7 C 0.0546(3) 0.6747(3) 0.61795(7) 0.0321(8) Uani 1 1 d . . . . .
H7A H 0.046424 0.615444 0.617937 0.039 Uiso 1 1 calc R U . . .
C8 C -0.0203(3) 0.6849(3) 0.62217(7) 0.0315(8) Uani 1 1 d . . . . .
C9 C -0.0047(3) 0.7735(3) 0.62143(7) 0.0319(8) Uani 1 1 d . . . . .
H9A H -0.054002 0.783485 0.624504 0.038 Uiso 1 1 calc R U . . .
C10 C 0.0799(3) 0.8470(2) 0.61638(7) 0.0322(8) Uani 1 1 d . . . . .
C11 C 0.1245(4) 0.9965(3) 0.63671(8) 0.0504(11) Uani 1 1 d . . . . .
H11A H 0.113451 0.961536 0.653791 0.076 Uiso 1 1 calc R U . . .
H11B H 0.189630 1.037838 0.634526 0.076 Uiso 1 1 calc R U . . .
H11C H 0.093339 1.031499 0.637685 0.076 Uiso 1 1 calc R U . . .
C12 C 0.0978(2) 0.9671(2) 0.58699(8) 0.0303(8) Uani 1 1 d . . . . .
C13 C 0.1353(2) 1.0807(2) 0.55781(8) 0.0313(8) Uani 1 1 d . . . . .
C14 C 0.0836(2) 0.9414(2) 0.54108(7) 0.0302(8) Uani 1 1 d . . . . .
C15 C 0.0954(3) 0.7612(3) 0.52097(8) 0.0321(8) Uani 1 1 d . . . . .
H15A H 0.158354 0.802838 0.519534 0.038 Uiso 1 1 calc R U . . .
C16 C 0.0339(2) 0.7920(2) 0.52139(7) 0.0291(8) Uani 1 1 d . . . . .
C17 C -0.0584(3) 0.7299(3) 0.52340(7) 0.0320(8) Uani 1 1 d . . . . .
H17A H -0.100791 0.750408 0.524131 0.038 Uiso 1 1 calc R U . . .
C18 C -0.0877(3) 0.6385(2) 0.52434(8) 0.0336(8) Uani 1 1 d . . . . .
H18A H -0.150715 0.596292 0.525136 0.040 Uiso 1 1 calc R U . . .
C19 C -0.0268(3) 0.6076(2) 0.52412(8) 0.0327(8) Uani 1 1 d . . . . .
H19A H -0.047355 0.544653 0.524975 0.039 Uiso 1 1 calc R U . . .
C20 C 0.0640(3) 0.6696(2) 0.52266(7) 0.0301(8) Uani 1 1 d . . . . .
C21 C 0.3621(3) 0.5717(3) 0.53437(8) 0.0359(9) Uani 1 1 d . . . . .
H21A H 0.376996 0.613441 0.518483 0.043 Uiso 1 1 calc R U . . .
H21B H 0.304369 0.515665 0.530408 0.043 Uiso 1 1 calc R U . . .
C22 C 0.4362(3) 0.5506(3) 0.53919(8) 0.0374(9) Uani 1 1 d . . . . .
H22A H 0.443820 0.521902 0.522632 0.056 Uiso 1 1 calc R U . . .
H22B H 0.492701 0.606617 0.543116 0.056 Uiso 1 1 calc R U . . .
H22C H 0.420441 0.509337 0.554981 0.056 Uiso 1 1 calc R U . . .
C23 C -0.1158(3) 0.6027(3) 0.62451(8) 0.0337(8) Uani 1 1 d . . . . .
C24 C -0.1158(3) 0.5272(3) 0.64155(9) 0.0407(9) Uani 1 1 d . . . . .
H24A H -0.073970 0.510363 0.633211 0.061 Uiso 1 1 calc R U . . .
H24B H -0.096543 0.548381 0.660527 0.061 Uiso 1 1 calc R U . . .
H24C H -0.176905 0.474440 0.641823 0.061 Uiso 1 1 calc R U . . .
C25 C -0.1485(3) 0.5672(3) 0.59523(9) 0.0475(10) Uani 1 1 d . . . . .
H25A H -0.106233 0.551575 0.586504 0.071 Uiso 1 1 calc R U . . .
H25B H -0.208671 0.513256 0.596154 0.071 Uiso 1 1 calc R U . . .
H25C H -0.151375 0.613933 0.584262 0.071 Uiso 1 1 calc R U . . .
C26 C -0.1815(3) 0.6270(3) 0.63809(9) 0.0416(10) Uani 1 1 d . . . . .
H26A H -0.182703 0.675350 0.627518 0.062 Uiso 1 1 calc R U . . .
H26B H -0.242207 0.573615 0.638384 0.062 Uiso 1 1 calc R U . . .
H26C H -0.161846 0.647556 0.657087 0.062 Uiso 1 1 calc R U . . .
C27 C 0.2875(3) 0.9123(3) 0.58434(9) 0.0462(10) Uani 1 1 d . . . . .
H27A H 0.245402 0.875057 0.569461 0.055 Uiso 1 1 calc R U . . .
H27B H 0.327554 0.887602 0.588744 0.055 Uiso 1 1 calc R U . . .
C28 C 0.3423(3) 1.0083(3) 0.57514(9) 0.0391(9) Uani 1 1 d . . . . .
C29 C 0.4237(3) 1.0671(3) 0.58838(11) 0.0564(12) Uani 1 1 d . . . . .
H29A H 0.444796 1.045458 0.603072 0.068 Uiso 1 1 calc R U . . .
C30 C 0.4735(4) 1.1563(4) 0.58024(16) 0.0828(19) Uani 1 1 d . . . . .
H30A H 0.529416 1.195835 0.589028 0.099 Uiso 1 1 calc R U . . .
C31 C 0.4416(5) 1.1876(4) 0.55921(17) 0.088(2) Uani 1 1 d . . . . .
H31A H 0.475211 1.249169 0.553720 0.106 Uiso 1 1 calc R U . . .
C32 C 0.3638(4) 1.1320(4) 0.54656(15) 0.0781(19) Uani 1 1 d . . . . .
H32A H 0.342261 1.154564 0.532269 0.094 Uiso 1 1 calc R U . . .
C33 C 0.3142(3) 1.0419(4) 0.55399(10) 0.0557(12) Uani 1 1 d . . . . .
H33A H 0.260002 1.002753 0.544323 0.067 Uiso 1 1 calc R U . . .
C34 C 0.2034(4) 1.2336(3) 0.57388(9) 0.0513(12) Uani 1 1 d . . . . .
H34A H 0.227054 1.212668 0.589152 0.062 Uiso 1 1 calc R U . . .
H34B H 0.153234 1.241013 0.581141 0.062 Uiso 1 1 calc R U . . .
C35 C 0.2765(3) 1.3211(3) 0.56251(10) 0.0468(11) Uani 1 1 d . . . . .
H35A H 0.299704 1.366769 0.577200 0.070 Uiso 1 1 calc R U . . .
H35B H 0.325680 1.312824 0.555418 0.070 Uiso 1 1 calc R U . . .
H35C H 0.252183 1.341046 0.547441 0.070 Uiso 1 1 calc R U . . .
C36 C 0.4729(9) 0.9126(13) 0.5059(3) 0.054(3) Uani 0.25 1 d D . P . .
C37 C -0.588(2) 0.296(4) 0.6242(6) 0.089(4) Uani 0.125 1 d D U P A 1
H37A H -0.600435 0.325628 0.608568 0.107 Uiso 0.125 1 calc R U P A 1
H37B H -0.587196 0.242202 0.617076 0.107 Uiso 0.125 1 calc R U P A 1
C38 C -0.4949(18) 0.362(4) 0.6368(8) 0.089(4) Uani 0.125 1 d D U P A 1
H38A H -0.461142 0.415836 0.624685 0.107 Uiso 0.125 1 calc R U P A 1
H38B H -0.458386 0.332605 0.639388 0.107 Uiso 0.125 1 calc R U P A 1
C39 C -0.517(2) 0.390(3) 0.6651(8) 0.089(4) Uani 0.125 1 d D U P A 1
H39A H -0.492595 0.370660 0.680599 0.107 Uiso 0.125 1 calc R U P A 1
H39B H -0.490594 0.456701 0.666166 0.107 Uiso 0.125 1 calc R U P A 1
C40 C -0.620(2) 0.342(3) 0.6660(9) 0.089(4) Uani 0.125 1 d D U P A 1
H40A H -0.641243 0.316093 0.684704 0.107 Uiso 0.125 1 calc R U P A 1
H40B H -0.640617 0.385515 0.662239 0.107 Uiso 0.125 1 calc R U P A 1
C41 C -0.503(2) 0.390(3) 0.6198(8) 0.089(4) Uani 0.125 1 d D U P B 2
H41A H -0.506618 0.371286 0.600156 0.107 Uiso 0.125 1 calc R U P B 2
H41B H -0.482966 0.455004 0.620173 0.107 Uiso 0.125 1 calc R U P B 2
C42 C -0.596(2) 0.336(4) 0.6332(10) 0.089(4) Uani 0.125 1 d D U P B 2
H42A H -0.642644 0.299273 0.619246 0.107 Uiso 0.125 1 calc R U P B 2
H42B H -0.613597 0.377270 0.642246 0.107 Uiso 0.125 1 calc R U P B 2
C43 C -0.586(2) 0.275(3) 0.6548(9) 0.089(4) Uani 0.125 1 d D U P B 2
H43A H -0.594732 0.291363 0.673796 0.107 Uiso 0.125 1 calc R U P B 2
H43B H -0.630915 0.210657 0.651433 0.107 Uiso 0.125 1 calc R U P B 2
C44 C -0.489(2) 0.293(3) 0.6506(9) 0.089(4) Uani 0.125 1 d D U P B 2
H44A H -0.460193 0.300846 0.668894 0.107 Uiso 0.125 1 calc R U P B 2
H44B H -0.491216 0.241031 0.641251 0.107 Uiso 0.125 1 calc R U P B 2
N1 N 0.1649(2) 0.6837(2) 0.56592(6) 0.0319(7) Uani 1 1 d . . . . .
N2 N 0.2372(2) 0.6209(2) 0.53894(6) 0.0337(7) Uani 1 1 d . . . . .
N3 N 0.2895(2) 0.6745(2) 0.58478(6) 0.0336(7) Uani 1 1 d . . . . .
N4 N 0.2151(2) 0.7319(2) 0.61022(6) 0.0329(7) Uani 1 1 d . . . . .
N5 N 0.0905(2) 0.9351(2) 0.61308(6) 0.0342(7) Uani 1 1 d . . . . .
N6 N 0.0742(2) 0.9061(2) 0.56640(6) 0.0317(7) Uani 1 1 d . . . . .
N7 N 0.1272(2) 1.0561(2) 0.58389(6) 0.0321(7) Uani 1 1 d . . . . .
N8 N 0.1140(2) 1.02924(19) 0.53523(6) 0.0311(7) Uani 1 1 d . . . . .
N9 N 0.0643(2) 0.8859(2) 0.51908(6) 0.0332(7) Uani 1 1 d . . . . .
H9B H 0.070953 0.909120 0.502397 0.040 Uiso 1 1 calc R U . . .
O1 O 0.12511(18) 0.63707(18) 0.52095(5) 0.0357(6) Uani 1 1 d . . . . .
O2 O 0.35471(17) 0.61366(18) 0.55957(5) 0.0352(6) Uani 1 1 d . . . . .
O3 O 0.23729(18) 0.91052(17) 0.60870(6) 0.0382(6) Uani 1 1 d . . . . .
O4 O 0.17166(19) 1.16878(17) 0.55140(5) 0.0370(6) Uani 1 1 d . . . . .
O5 O 0.3771(7) 0.8538(9) 0.5155(2) 0.054(3) Uani 0.25 1 d D . P . .
O6 O -0.6583(17) 0.269(2) 0.6454(6) 0.089(4) Uani 0.125 1 d D . P A 1
O7 O -0.4358(17) 0.375(3) 0.6340(6) 0.089(4) Uani 0.125 1 d D . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.320(5) . ?
C1 N2 1.330(5) . ?
C1 O1 1.355(4) . ?
C2 O2 1.328(4) . ?
C2 N3 1.332(5) . ?
C2 N2 1.338(5) . ?
C3 N3 1.336(5) . ?
C3 N1 1.352(5) . ?
C3 N4 1.355(5) . ?
C4 N4 1.457(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 O3 1.371(5) . ?
C5 C10 1.392(6) . ?
C5 C6 1.400(5) . ?
C6 C7 1.384(5) . ?
C6 N4 1.433(5) . ?
C7 C8 1.390(6) . ?
C7 H7A 0.9500 . ?
C8 C9 1.399(5) . ?
C8 C23 1.534(5) . ?
C9 C10 1.381(6) . ?
C9 H9A 0.9500 . ?
C10 N5 1.432(5) . ?
C11 N5 1.461(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N6 1.347(5) . ?
C12 N7 1.350(5) . ?
C12 N5 1.354(5) . ?
C13 N7 1.313(5) . ?
C13 N8 1.332(5) . ?
C13 O4 1.346(4) . ?
C14 N6 1.337(5) . ?
C14 N8 1.350(5) . ?
C14 N9 1.351(5) . ?
C15 C20 1.379(5) . ?
C15 C16 1.390(5) . ?
C15 H15A 0.9500 . ?
C16 C17 1.394(5) . ?
C16 N9 1.421(5) . ?
C17 C18 1.381(5) . ?
C17 H17A 0.9500 . ?
C18 C19 1.382(5) . ?
C18 H18A 0.9500 . ?
C19 C20 1.375(6) . ?
C19 H19A 0.9500 . ?
C20 O1 1.409(4) . ?
C21 O2 1.450(5) . ?
C21 C22 1.497(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C26 1.525(6) . ?
C23 C24 1.530(5) . ?
C23 C25 1.530(6) . ?
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 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 O3 1.447(5) . ?
C27 C28 1.493(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C33 1.370(6) . ?
C28 C29 1.398(6) . ?
C29 C30 1.379(8) . ?
C29 H29A 0.9500 . ?
C30 C31 1.382(10) . ?
C30 H30A 0.9500 . ?
C31 C32 1.333(10) . ?
C31 H31A 0.9500 . ?
C32 C33 1.383(8) . ?
C32 H32A 0.9500 . ?
C33 H33A 0.9500 . ?
C34 O4 1.448(5) . ?
C34 C35 1.493(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C36 0.80(3) 11_556 ?
C36 O5 1.47(2) 11_556 ?
C36 O5 1.502(12) . ?
C37 O6 1.467(13) . ?
C37 C38 1.537(13) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.555(13) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.528(13) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 O6 1.466(13) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 O7 1.461(13) . ?
C41 C42 1.533(13) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.542(13) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.536(13) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 O7 1.463(14) . ?
C44 C44 2.03(6) 12_566 ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
N9 H9B 0.8800 . ?

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
N1 C1 N2 128.5(3) . . ?
N1 C1 O1 118.2(3) . . ?
N2 C1 O1 113.3(3) . . ?
O2 C2 N3 113.7(3) . . ?
O2 C2 N2 119.1(3) . . ?
N3 C2 N2 127.2(3) . . ?
N3 C3 N1 125.5(3) . . ?
N3 C3 N4 118.1(3) . . ?
N1 C3 N4 116.3(3) . . ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C5 C10 118.3(3) . . ?
O3 C5 C6 123.3(3) . . ?
C10 C5 C6 118.4(4) . . ?
C7 C6 C5 119.9(3) . . ?
C7 C6 N4 119.6(3) . . ?
C5 C6 N4 120.4(3) . . ?
C6 C7 C8 122.7(4) . . ?
C6 C7 H7A 118.7 . . ?
C8 C7 H7A 118.7 . . ?
C7 C8 C9 116.3(4) . . ?
C7 C8 C23 121.3(3) . . ?
C9 C8 C23 122.2(3) . . ?
C10 C9 C8 122.2(4) . . ?
C10 C9 H9A 118.9 . . ?
C8 C9 H9A 118.9 . . ?
C9 C10 C5 120.5(3) . . ?
C9 C10 N5 120.0(3) . . ?
C5 C10 N5 119.5(4) . . ?
N5 C11 H11A 109.5 . . ?
N5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C12 N7 126.0(3) . . ?
N6 C12 N5 116.3(3) . . ?
N7 C12 N5 117.7(3) . . ?
N7 C13 N8 128.6(3) . . ?
N7 C13 O4 119.6(3) . . ?
N8 C13 O4 111.7(3) . . ?
N6 C14 N8 125.8(3) . . ?
N6 C14 N9 118.2(3) . . ?
N8 C14 N9 116.0(3) . . ?
C20 C15 C16 119.3(3) . . ?
C20 C15 H15A 120.4 . . ?
C16 C15 H15A 120.4 . . ?
C15 C16 C17 119.6(3) . . ?
C15 C16 N9 120.4(3) . . ?
C17 C16 N9 120.0(3) . . ?
C18 C17 C16 119.7(3) . . ?
C18 C17 H17A 120.1 . . ?
C16 C17 H17A 120.1 . . ?
C17 C18 C19 120.9(4) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C20 C19 C18 118.7(3) . . ?
C20 C19 H19A 120.6 . . ?
C18 C19 H19A 120.6 . . ?
C19 C20 C15 121.7(3) . . ?
C19 C20 O1 118.2(3) . . ?
C15 C20 O1 120.0(3) . . ?
O2 C21 C22 106.3(3) . . ?
O2 C21 H21A 110.5 . . ?
C22 C21 H21A 110.5 . . ?
O2 C21 H21B 110.5 . . ?
C22 C21 H21B 110.5 . . ?
H21A C21 H21B 108.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C26 C23 C24 107.9(3) . . ?
C26 C23 C25 109.5(4) . . ?
C24 C23 C25 108.5(3) . . ?
C26 C23 C8 111.9(3) . . ?
C24 C23 C8 111.3(3) . . ?
C25 C23 C8 107.7(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O3 C27 C28 107.7(3) . . ?
O3 C27 H27A 110.2 . . ?
C28 C27 H27A 110.2 . . ?
O3 C27 H27B 110.2 . . ?
C28 C27 H27B 110.2 . . ?
H27A C27 H27B 108.5 . . ?
C33 C28 C29 118.2(4) . . ?
C33 C28 C27 121.5(4) . . ?
C29 C28 C27 120.3(4) . . ?
C30 C29 C28 120.4(5) . . ?
C30 C29 H29A 119.8 . . ?
C28 C29 H29A 119.8 . . ?
C29 C30 C31 119.5(6) . . ?
C29 C30 H30A 120.3 . . ?
C31 C30 H30A 120.3 . . ?
C32 C31 C30 120.5(5) . . ?
C32 C31 H31A 119.8 . . ?
C30 C31 H31A 119.8 . . ?
C31 C32 C33 120.8(6) . . ?
C31 C32 H32A 119.6 . . ?
C33 C32 H32A 119.6 . . ?
C28 C33 C32 120.7(5) . . ?
C28 C33 H33A 119.6 . . ?
C32 C33 H33A 119.6 . . ?
O4 C34 C35 107.2(4) . . ?
O4 C34 H34A 110.3 . . ?
C35 C34 H34A 110.3 . . ?
O4 C34 H34B 110.3 . . ?
C35 C34 H34B 110.3 . . ?
H34A C34 H34B 108.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C36 C36 O5 76.8(19) 11_556 11_556 ?
C36 C36 O5 72(2) 11_556 . ?
O5 C36 O5 99.6(15) 11_556 . ?
O6 C37 C38 109.9(15) . . ?
O6 C37 H37A 109.7 . . ?
C38 C37 H37A 109.7 . . ?
O6 C37 H37B 109.7 . . ?
C38 C37 H37B 109.7 . . ?
H37A C37 H37B 108.2 . . ?
C37 C38 C39 104.8(12) . . ?
C37 C38 H38A 110.8 . . ?
C39 C38 H38A 110.8 . . ?
C37 C38 H38B 110.8 . . ?
C39 C38 H38B 110.8 . . ?
H38A C38 H38B 108.9 . . ?
C40 C39 C38 104.3(13) . . ?
C40 C39 H39A 110.9 . . ?
C38 C39 H39A 110.9 . . ?
C40 C39 H39B 110.9 . . ?
C38 C39 H39B 110.9 . . ?
H39A C39 H39B 108.9 . . ?
O6 C40 C39 110.2(15) . . ?
O6 C40 H40A 109.6 . . ?
C39 C40 H40A 109.6 . . ?
O6 C40 H40B 109.6 . . ?
C39 C40 H40B 109.6 . . ?
H40A C40 H40B 108.1 . . ?
O7 C41 C42 111.6(15) . . ?
O7 C41 H41A 109.3 . . ?
C42 C41 H41A 109.3 . . ?
O7 C41 H41B 109.3 . . ?
C42 C41 H41B 109.3 . . ?
H41A C41 H41B 108.0 . . ?
C41 C42 C43 104.8(12) . . ?
C41 C42 H42A 110.8 . . ?
C43 C42 H42A 110.8 . . ?
C41 C42 H42B 110.8 . . ?
C43 C42 H42B 110.8 . . ?
H42A C42 H42B 108.9 . . ?
C44 C43 C42 104.2(12) . . ?
C44 C43 H43A 110.9 . . ?
C42 C43 H43A 110.9 . . ?
C44 C43 H43B 110.9 . . ?
C42 C43 H43B 110.9 . . ?
H43A C43 H43B 108.9 . . ?
O7 C44 C43 111.3(15) . . ?
O7 C44 H44A 109.4 . . ?
C43 C44 H44A 109.4 . . ?
C44 C44 H44A 40.3 12_566 . ?
O7 C44 H44B 109.4 . . ?
C43 C44 H44B 109.4 . . ?
C44 C44 H44B 77.2 12_566 . ?
H44A C44 H44B 108.0 . . ?
C1 N1 C3 113.0(3) . . ?
C1 N2 C2 112.0(3) . . ?
C2 N3 C3 113.7(3) . . ?
C3 N4 C6 119.9(3) . . ?
C3 N4 C4 120.8(3) . . ?
C6 N4 C4 119.2(3) . . ?
C12 N5 C10 117.7(3) . . ?
C12 N5 C11 120.9(3) . . ?
C10 N5 C11 117.7(3) . . ?
C14 N6 C12 113.9(3) . . ?
C13 N7 C12 112.7(3) . . ?
C13 N8 C14 112.8(3) . . ?
C14 N9 C16 123.6(3) . . ?
C14 N9 H9B 118.2 . . ?
C16 N9 H9B 118.2 . . ?
C1 O1 C20 117.9(3) . . ?
C2 O2 C21 118.1(3) . . ?
C5 O3 C27 117.5(3) . . ?
C13 O4 C34 118.0(3) . . ?
C36 O5 C36 31.3(12) 11_556 . ?
C40 O6 C37 105(2) . . ?
C41 O7 C44 104.5(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C5 C6 C7 -179.9(3) . . . . ?
C10 C5 C6 C7 0.7(5) . . . . ?
O3 C5 C6 N4 -0.5(6) . . . . ?
C10 C5 C6 N4 -180.0(3) . . . . ?
C5 C6 C7 C8 -2.1(6) . . . . ?
N4 C6 C7 C8 178.5(3) . . . . ?
C6 C7 C8 C9 1.3(5) . . . . ?
C6 C7 C8 C23 175.3(3) . . . . ?
C7 C8 C9 C10 1.0(5) . . . . ?
C23 C8 C9 C10 -173.0(3) . . . . ?
C8 C9 C10 C5 -2.4(6) . . . . ?
C8 C9 C10 N5 173.7(3) . . . . ?
O3 C5 C10 C9 -178.0(3) . . . . ?
C6 C5 C10 C9 1.5(5) . . . . ?
O3 C5 C10 N5 5.9(5) . . . . ?
C6 C5 C10 N5 -174.6(3) . . . . ?
C20 C15 C16 C17 -0.2(6) . . . . ?
C20 C15 C16 N9 -178.6(3) . . . . ?
C15 C16 C17 C18 -1.4(6) . . . . ?
N9 C16 C17 C18 177.0(3) . . . . ?
C16 C17 C18 C19 1.9(6) . . . . ?
C17 C18 C19 C20 -0.7(6) . . . . ?
C18 C19 C20 C15 -1.0(6) . . . . ?
C18 C19 C20 O1 -176.6(3) . . . . ?
C16 C15 C20 C19 1.5(6) . . . . ?
C16 C15 C20 O1 177.0(3) . . . . ?
C7 C8 C23 C26 161.5(3) . . . . ?
C9 C8 C23 C26 -24.8(5) . . . . ?
C7 C8 C23 C24 40.7(5) . . . . ?
C9 C8 C23 C24 -145.7(4) . . . . ?
C7 C8 C23 C25 -78.1(4) . . . . ?
C9 C8 C23 C25 95.5(4) . . . . ?
O3 C27 C28 C33 -99.1(5) . . . . ?
O3 C27 C28 C29 79.9(5) . . . . ?
C33 C28 C29 C30 0.2(8) . . . . ?
C27 C28 C29 C30 -178.8(5) . . . . ?
C28 C29 C30 C31 1.2(9) . . . . ?
C29 C30 C31 C32 -0.9(10) . . . . ?
C30 C31 C32 C33 -0.7(10) . . . . ?
C29 C28 C33 C32 -1.9(7) . . . . ?
C27 C28 C33 C32 177.1(5) . . . . ?
C31 C32 C33 C28 2.2(9) . . . . ?
O6 C37 C38 C39 -12(6) . . . . ?
C37 C38 C39 C40 -3(6) . . . . ?
C38 C39 C40 O6 17(6) . . . . ?
O7 C41 C42 C43 -8(6) . . . . ?
C41 C42 C43 C44 -4(5) . . . . ?
C42 C43 C44 O7 15(5) . . . . ?
C42 C43 C44 C44 175(4) . . . 12_566 ?
N2 C1 N1 C3 2.0(6) . . . . ?
O1 C1 N1 C3 -177.9(3) . . . . ?
N3 C3 N1 C1 1.7(5) . . . . ?
N4 C3 N1 C1 178.9(3) . . . . ?
N1 C1 N2 C2 -3.1(6) . . . . ?
O1 C1 N2 C2 176.8(3) . . . . ?
O2 C2 N2 C1 -179.8(3) . . . . ?
N3 C2 N2 C1 0.7(6) . . . . ?
O2 C2 N3 C3 -177.3(3) . . . . ?
N2 C2 N3 C3 2.2(6) . . . . ?
N1 C3 N3 C2 -3.6(5) . . . . ?
N4 C3 N3 C2 179.3(3) . . . . ?
N3 C3 N4 C6 -174.8(3) . . . . ?
N1 C3 N4 C6 7.8(5) . . . . ?
N3 C3 N4 C4 5.7(5) . . . . ?
N1 C3 N4 C4 -171.7(3) . . . . ?
C7 C6 N4 C3 71.9(5) . . . . ?
C5 C6 N4 C3 -107.5(4) . . . . ?
C7 C6 N4 C4 -108.6(4) . . . . ?
C5 C6 N4 C4 72.1(5) . . . . ?
N6 C12 N5 C10 14.5(5) . . . . ?
N7 C12 N5 C10 -165.9(3) . . . . ?
N6 C12 N5 C11 172.5(4) . . . . ?
N7 C12 N5 C11 -7.9(5) . . . . ?
C9 C10 N5 C12 -100.6(4) . . . . ?
C5 C10 N5 C12 75.5(5) . . . . ?
C9 C10 N5 C11 100.7(5) . . . . ?
C5 C10 N5 C11 -83.2(5) . . . . ?
N8 C14 N6 C12 0.4(5) . . . . ?
N9 C14 N6 C12 177.9(3) . . . . ?
N7 C12 N6 C14 1.1(5) . . . . ?
N5 C12 N6 C14 -179.3(3) . . . . ?
N8 C13 N7 C12 4.1(5) . . . . ?
O4 C13 N7 C12 -174.1(3) . . . . ?
N6 C12 N7 C13 -3.1(5) . . . . ?
N5 C12 N7 C13 177.4(3) . . . . ?
N7 C13 N8 C14 -2.8(5) . . . . ?
O4 C13 N8 C14 175.4(3) . . . . ?
N6 C14 N8 C13 0.3(5) . . . . ?
N9 C14 N8 C13 -177.3(3) . . . . ?
N6 C14 N9 C16 0.6(5) . . . . ?
N8 C14 N9 C16 178.3(3) . . . . ?
C15 C16 N9 C14 -92.5(5) . . . . ?
C17 C16 N9 C14 89.1(5) . . . . ?
N1 C1 O1 C20 4.2(5) . . . . ?
N2 C1 O1 C20 -175.7(3) . . . . ?
C19 C20 O1 C1 -109.5(4) . . . . ?
C15 C20 O1 C1 74.8(4) . . . . ?
N3 C2 O2 C21 179.6(3) . . . . ?
N2 C2 O2 C21 0.1(5) . . . . ?
C22 C21 O2 C2 -178.3(3) . . . . ?
C10 C5 O3 C27 -125.4(4) . . . . ?
C6 C5 O3 C27 55.1(5) . . . . ?
C28 C27 O3 C5 148.3(3) . . . . ?
N7 C13 O4 C34 2.1(5) . . . . ?
N8 C13 O4 C34 -176.3(4) . . . . ?
C35 C34 O4 C13 153.1(4) . . . . ?
O5 C36 O5 C36 -72.6(15) 11_556 . . 11_556 ?
C39 C40 O6 C37 -25(5) . . . . ?
C38 C37 O6 C40 23(6) . . . . ?
C42 C41 O7 C44 17(5) . . . . ?
C43 C44 O7 C41 -19(5) . . . . ?
C44 C44 O7 C41 -163(7) 12_566 . . . ?

_refine_diff_density_max         0.716
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.069

