# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_nh2-low
_database_code_depnum_ccdc_archive 'CCDC 1582847'
_audit_update_record             
;
2017-10-30 deposited with the CCDC.	2019-04-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H40 N4 O2'
_chemical_formula_sum            'C32 H40 N4 O2'
_chemical_formula_weight         512.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   10.1957(4)
_cell_length_b                   12.2494(5)
_cell_length_c                   23.2226(10)
_cell_angle_alpha                92.193(3)
_cell_angle_beta                 93.573(3)
_cell_angle_gamma                106.021(3)
_cell_volume                     2777.56(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    13408
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      29.44

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_F_000             1104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.077
_shelx_estimated_absorpt_T_min   0.990
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  BRUKER
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26510
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.868
_diffrn_reflns_theta_max         29.436
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.594
_diffrn_reflns_point_group_measured_fraction_full 0.729
_reflns_number_total             18229
_reflns_number_gt                15610
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.389
_reflns_Friedel_fraction_max     0.332
_reflns_Friedel_fraction_full    0.460

_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       Bruker
_computing_cell_refinement       Bruker
_computing_data_reduction        Bruker
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0889P)²+3.7106P] 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_abs_structure_details 
;
 Flack x determined using 3692 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.8(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         18229
_refine_ls_number_parameters     1389
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0735
_refine_ls_wR_factor_ref         0.2046
_refine_ls_wR_factor_gt          0.1941
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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 0.9479(6) 0.0285(4) 0.7550(3) 0.0184(11) Uani 1 1 d . . . . .
C2 C 0.9946(6) -0.0690(4) 0.7559(3) 0.0194(11) Uani 1 1 d . . . . .
H2 H 0.9661 -0.1260 0.7252 0.023 Uiso 1 1 calc R U . . .
C3 C 1.0824(6) -0.0822(4) 0.8016(3) 0.0189(11) Uani 1 1 d . . . . .
C4 C 1.1247(6) 0.0055(5) 0.8445(3) 0.0242(12) Uani 1 1 d . . . . .
H4 H 1.1856 -0.0013 0.8759 0.029 Uiso 1 1 calc R U . . .
C5 C 1.0799(6) 0.1025(5) 0.8425(3) 0.0236(12) Uani 1 1 d . . . . .
H5 H 1.1114 0.1608 0.8724 0.028 Uiso 1 1 calc R U . . .
C6 C 0.9896(6) 0.1161(4) 0.7975(2) 0.0179(11) Uani 1 1 d . . . . .
C7 C 0.9399(5) 0.2220(4) 0.7957(2) 0.0157(10) Uani 1 1 d . . . . .
C8 C 0.8654(6) 0.2245(4) 0.7377(2) 0.0172(11) Uani 1 1 d . . . . .
C9 C 0.8291(5) 0.3208(4) 0.7197(3) 0.0186(11) Uani 1 1 d . . . . .
H9 H 0.8571 0.3886 0.7440 0.022 Uiso 1 1 calc R U . . .
C10 C 0.7546(6) 0.3214(4) 0.6684(3) 0.0214(12) Uani 1 1 d . . . . .
H10 H 0.7343 0.3893 0.6576 0.026 Uiso 1 1 calc R U . . .
C11 C 0.7083(6) 0.2224(5) 0.6318(3) 0.0212(12) Uani 1 1 d . . . . .
C12 C 0.7450(6) 0.1263(5) 0.6479(3) 0.0221(12) Uani 1 1 d . . . . .
H12 H 0.7162 0.0585 0.6236 0.027 Uiso 1 1 calc R U . . .
C13 C 0.8235(6) 0.1285(4) 0.6993(3) 0.0180(11) Uani 1 1 d . . . . .
C14 C 1.0542(5) 0.3292(4) 0.8123(2) 0.0172(11) Uani 1 1 d . . . . .
C15 C 1.1699(6) 0.3753(5) 0.7843(3) 0.0234(12) Uani 1 1 d . . . . .
H15 H 1.1843 0.3437 0.7480 0.028 Uiso 1 1 calc R U . . .
C16 C 1.2658(6) 0.4709(5) 0.8116(3) 0.0289(14) Uani 1 1 d . . . . .
H16 H 1.3474 0.5037 0.7935 0.035 Uiso 1 1 calc R U . . .
C17 C 1.2462(6) 0.5188(4) 0.8637(3) 0.0237(12) Uani 1 1 d . . . . .
H17 H 1.3149 0.5824 0.8813 0.028 Uiso 1 1 calc R U . . .
C18 C 1.1265(6) 0.4750(5) 0.8910(3) 0.0223(12) Uani 1 1 d . . . . .
C19 C 1.0317(6) 0.3779(4) 0.8640(3) 0.0192(11) Uani 1 1 d . . . . .
C20 C 0.9031(6) 0.3106(5) 0.8847(3) 0.0215(12) Uani 1 1 d . . . . .
C21 C 0.7264(8) 0.1309(5) 0.8514(3) 0.0361(17) Uani 1 1 d . . . . .
H21A H 0.7091 0.1305 0.8929 0.043 Uiso 1 1 calc R U . . .
H21B H 0.7460 0.0583 0.8408 0.043 Uiso 1 1 calc R U . . .
C22 C 0.5964(8) 0.1354(7) 0.8164(4) 0.048(2) Uani 1 1 d . . . . .
H22A H 0.6162 0.1422 0.7753 0.058 Uiso 1 1 calc R U . . .
H22B H 0.5257 0.0623 0.8193 0.058 Uiso 1 1 calc R U . . .
C23 C 0.5388(8) 0.2290(7) 0.8339(3) 0.0429(18) Uani 1 1 d . . . . .
H23A H 0.4658 0.2323 0.8044 0.051 Uiso 1 1 calc R U . . .
H23B H 0.6117 0.3019 0.8346 0.051 Uiso 1 1 calc R U . . .
C24 C 0.4800(8) 0.2183(6) 0.8922(4) 0.0425(17) Uani 1 1 d . . . . .
H24A H 0.4128 0.1438 0.8932 0.064 Uiso 1 1 calc R U . . .
H24B H 0.4353 0.2785 0.8987 0.064 Uiso 1 1 calc R U . . .
H24C H 0.5538 0.2255 0.9225 0.064 Uiso 1 1 calc R U . . .
C25 C 1.1151(6) -0.2563(4) 0.7528(3) 0.0209(11) Uani 1 1 d . . . . .
H25A H 1.1973 -0.2844 0.7527 0.025 Uiso 1 1 calc R U . . .
H25B H 1.1112 -0.2144 0.7174 0.025 Uiso 1 1 calc R U . . .
C26 C 0.9891(6) -0.3569(5) 0.7513(3) 0.0282(13) Uani 1 1 d . . . . .
H26A H 0.9954 -0.4019 0.7848 0.042 Uiso 1 1 calc R U . . .
H26B H 0.9826 -0.4043 0.7157 0.042 Uiso 1 1 calc R U . . .
H26C H 0.9075 -0.3296 0.7524 0.042 Uiso 1 1 calc R U . . .
C27 C 1.1872(6) -0.2091(5) 0.8563(3) 0.0234(12) Uani 1 1 d . . . . .
H27A H 1.1540 -0.2926 0.8586 0.028 Uiso 1 1 calc R U . . .
H27B H 1.1547 -0.1736 0.8896 0.028 Uiso 1 1 calc R U . . .
C28 C 1.3413(7) -0.1739(6) 0.8612(3) 0.0338(15) Uani 1 1 d . . . . .
H28A H 1.3745 -0.2066 0.8278 0.051 Uiso 1 1 calc R U . . .
H28B H 1.3745 -0.2015 0.8968 0.051 Uiso 1 1 calc R U . . .
H28C H 1.3752 -0.0908 0.8623 0.051 Uiso 1 1 calc R U . . .
C29 C 0.5626(6) 0.1110(5) 0.5488(3) 0.0268(13) Uani 1 1 d . . . . .
H29A H 0.4791 0.1174 0.5267 0.032 Uiso 1 1 calc R U . . .
H29B H 0.5337 0.0507 0.5763 0.032 Uiso 1 1 calc R U . . .
C30 C 0.6517(8) 0.0734(6) 0.5071(3) 0.0392(17) Uani 1 1 d . . . . .
H30A H 0.6697 0.1262 0.4759 0.059 Uiso 1 1 calc R U . . .
H30B H 0.6047 -0.0033 0.4906 0.059 Uiso 1 1 calc R U . . .
H30C H 0.7385 0.0730 0.5276 0.059 Uiso 1 1 calc R U . . .
C31 C 0.6123(7) 0.3223(6) 0.5560(3) 0.0338(15) Uani 1 1 d . . . . .
H31A H 0.6049 0.3774 0.5871 0.041 Uiso 1 1 calc R U . . .
H31B H 0.5264 0.3035 0.5307 0.041 Uiso 1 1 calc R U . . .
C32 C 0.7311(9) 0.3789(6) 0.5206(4) 0.046(2) Uani 1 1 d . . . . .
H32A H 0.8139 0.4102 0.5465 0.069 Uiso 1 1 calc R U . . .
H32B H 0.7089 0.4404 0.4998 0.069 Uiso 1 1 calc R U . . .
H32C H 0.7468 0.3225 0.4928 0.069 Uiso 1 1 calc R U . . .
C33 C 0.9259(5) 0.3903(4) 0.2533(2) 0.0168(11) Uani 1 1 d . . . . .
C34 C 0.8818(6) 0.4870(4) 0.2563(2) 0.0182(11) Uani 1 1 d . . . . .
H34 H 0.8949 0.5370 0.2256 0.022 Uiso 1 1 calc R U . . .
C35 C 0.8178(6) 0.5114(4) 0.3047(2) 0.0193(11) Uani 1 1 d . . . . .
C36 C 0.8012(6) 0.4344(4) 0.3495(2) 0.0226(11) Uani 1 1 d . . . . .
H36 H 0.7582 0.4484 0.3831 0.027 Uiso 1 1 calc R U . . .
C37 C 0.8474(6) 0.3390(4) 0.3444(2) 0.0214(11) Uani 1 1 d . . . . .
H37 H 0.8360 0.2890 0.3751 0.026 Uiso 1 1 calc R U . . .
C38 C 0.9103(5) 0.3126(4) 0.2959(2) 0.0166(10) Uani 1 1 d . . . . .
C39 C 0.9629(5) 0.2084(4) 0.2921(2) 0.0147(10) Uani 1 1 d . . . . .
C40 C 1.0070(6) 0.1930(4) 0.2324(2) 0.0176(11) Uani 1 1 d . . . . .
C41 C 1.0446(6) 0.0957(4) 0.2143(3) 0.0207(11) Uani 1 1 d . . . . .
H41 H 1.0370 0.0365 0.2402 0.025 Uiso 1 1 calc R U . . .
C42 C 1.0917(6) 0.0817(4) 0.1612(3) 0.0226(12) Uani 1 1 d . . . . .
H42 H 1.1152 0.0140 0.1510 0.027 Uiso 1 1 calc R U . . .
C43 C 1.1052(6) 0.1693(5) 0.1211(3) 0.0262(13) Uani 1 1 d . . . . .
C44 C 1.0677(6) 0.2651(5) 0.1385(3) 0.0251(13) Uani 1 1 d . . . . .
H44 H 1.0731 0.3242 0.1126 0.030 Uiso 1 1 calc R U . . .
C45 C 1.0225(6) 0.2766(4) 0.1928(2) 0.0181(11) Uani 1 1 d . . . . .
C46 C 0.8586(6) 0.1045(4) 0.3113(2) 0.0181(11) Uani 1 1 d . . . . .
C47 C 0.7300(6) 0.0499(4) 0.2868(3) 0.0221(11) Uani 1 1 d . . . . .
H47 H 0.6968 0.0712 0.2510 0.026 Uiso 1 1 calc R U . . .
C48 C 0.6499(6) -0.0382(4) 0.3164(3) 0.0244(12) Uani 1 1 d . . . . .
H48 H 0.5599 -0.0765 0.3006 0.029 Uiso 1 1 calc R U . . .
C49 C 0.6974(6) -0.0716(4) 0.3679(3) 0.0211(11) Uani 1 1 d . . . . .
H49 H 0.6398 -0.1321 0.3867 0.025 Uiso 1 1 calc R U . . .
C50 C 0.8300(6) -0.0173(4) 0.3929(3) 0.0203(11) Uani 1 1 d . . . . .
C51 C 0.9070(6) 0.0729(4) 0.3634(3) 0.0184(11) Uani 1 1 d . . . . .
C52 C 1.0454(6) 0.1507(4) 0.3803(2) 0.0167(11) Uani 1 1 d . . . . .
C53 C 1.2023(6) 0.3145(4) 0.3388(3) 0.0246(13) Uani 1 1 d . . . . .
H53A H 1.2358 0.3371 0.3797 0.029 Uiso 1 1 calc R U . . .
H53B H 1.1794 0.3804 0.3217 0.029 Uiso 1 1 calc R U . . .
C54 C 1.3183(7) 0.2888(5) 0.3069(3) 0.0340(15) Uani 1 1 d . . . . .
H54A H 1.2840 0.2649 0.2662 0.041 Uiso 1 1 calc R U . . .
H54B H 1.3934 0.3600 0.3065 0.041 Uiso 1 1 calc R U . . .
C55 C 1.3765(8) 0.1982(7) 0.3317(4) 0.0427(18) Uani 1 1 d . . . . .
H55A H 1.3002 0.1288 0.3348 0.051 Uiso 1 1 calc R U . . .
H55B H 1.4383 0.1792 0.3042 0.051 Uiso 1 1 calc R U . . .
C56 C 1.4522(8) 0.2285(6) 0.3885(4) 0.0411(18) Uani 1 1 d . . . . .
H56A H 1.5241 0.3001 0.3869 0.062 Uiso 1 1 calc R U . . .
H56B H 1.4937 0.1681 0.3991 0.062 Uiso 1 1 calc R U . . .
H56C H 1.3893 0.2374 0.4174 0.062 Uiso 1 1 calc R U . . .
C57 C 0.7661(6) 0.6777(4) 0.2606(3) 0.0206(11) Uani 1 1 d . . . . .
H57A H 0.6858 0.7079 0.2629 0.025 Uiso 1 1 calc R U . . .
H57B H 0.7519 0.6288 0.2245 0.025 Uiso 1 1 calc R U . . .
C58 C 0.8937(6) 0.7770(5) 0.2574(3) 0.0276(13) Uani 1 1 d . . . . .
H58A H 0.9180 0.8182 0.2953 0.041 Uiso 1 1 calc R U . . .
H58B H 0.8756 0.8285 0.2287 0.041 Uiso 1 1 calc R U . . .
H58C H 0.9696 0.7480 0.2463 0.041 Uiso 1 1 calc R U . . .
C59 C 0.7329(6) 0.6458(4) 0.3640(2) 0.0217(11) Uani 1 1 d . . . . .
H59A H 0.7632 0.7300 0.3678 0.026 Uiso 1 1 calc R U . . .
H59B H 0.7805 0.6173 0.3961 0.026 Uiso 1 1 calc R U . . .
C60 C 0.5811(7) 0.6062(6) 0.3698(3) 0.0382(15) Uani 1 1 d . . . . .
H60A H 0.5330 0.6342 0.3383 0.057 Uiso 1 1 calc R U . . .
H60B H 0.5605 0.6358 0.4070 0.057 Uiso 1 1 calc R U . . .
H60C H 0.5508 0.5229 0.3680 0.057 Uiso 1 1 calc R U . . .
C61 C 1.1520(8) 0.2458(6) 0.0235(3) 0.0399(16) Uani 1 1 d . . . . .
H61A H 1.1394 0.2086 -0.0158 0.048 Uiso 1 1 calc R U . . .
H61B H 1.0738 0.2776 0.0287 0.048 Uiso 1 1 calc R U . . .
C62 C 1.2822(8) 0.3409(6) 0.0288(4) 0.052(2) Uani 1 1 d . . . . .
H62A H 1.2934 0.3798 0.0673 0.077 Uiso 1 1 calc R U . . .
H62B H 1.2783 0.3951 -0.0007 0.077 Uiso 1 1 calc R U . . .
H62C H 1.3598 0.3099 0.0235 0.077 Uiso 1 1 calc R U . . .
C63 C 1.1906(7) 0.0589(5) 0.0468(3) 0.0318(14) Uani 1 1 d . . . . .
H63A H 1.2263 0.0254 0.0804 0.038 Uiso 1 1 calc R U . . .
H63B H 1.2655 0.0830 0.0208 0.038 Uiso 1 1 calc R U . . .
C64 C 1.0746(8) -0.0303(6) 0.0152(3) 0.0419(17) Uani 1 1 d . . . . .
H64A H 1.0096 -0.0670 0.0428 0.063 Uiso 1 1 calc R U . . .
H64B H 1.1103 -0.0874 -0.0041 0.063 Uiso 1 1 calc R U . . .
H64C H 1.0280 0.0052 -0.0136 0.063 Uiso 1 1 calc R U . . .
C65 C 0.3327(6) 0.6479(4) 0.2395(3) 0.0191(11) Uani 1 1 d . . . . .
C66 C 0.2701(5) 0.6533(4) 0.2907(2) 0.0165(10) Uani 1 1 d . . . . .
H66 H 0.2496 0.5892 0.3138 0.020 Uiso 1 1 calc R U . . .
C67 C 0.2371(5) 0.7524(4) 0.3085(2) 0.0174(10) Uani 1 1 d . . . . .
C68 C 0.2717(6) 0.8455(4) 0.2723(3) 0.0205(11) Uani 1 1 d . . . . .
H68 H 0.2541 0.9153 0.2834 0.025 Uiso 1 1 calc R U . . .
C69 C 0.3299(5) 0.8360(4) 0.2217(3) 0.0180(11) Uani 1 1 d . . . . .
H69 H 0.3493 0.8992 0.1980 0.022 Uiso 1 1 calc R U . . .
C70 C 0.3623(5) 0.7368(4) 0.2031(2) 0.0140(10) Uani 1 1 d . . . . .
C71 C 0.4168(6) 0.7238(4) 0.1453(2) 0.0169(11) Uani 1 1 d . . . . .
C72 C 0.4787(5) 0.6243(4) 0.1449(2) 0.0180(11) Uani 1 1 d . . . . .
C73 C 0.5661(6) 0.6081(4) 0.1039(3) 0.0235(12) Uani 1 1 d . . . . .
H73 H 0.5897 0.6625 0.0755 0.028 Uiso 1 1 calc R U . . .
C74 C 0.6205(6) 0.5163(5) 0.1025(3) 0.0246(12) Uani 1 1 d . . . . .
H74 H 0.6819 0.5099 0.0742 0.030 Uiso 1 1 calc R U . . .
C75 C 0.5845(6) 0.4317(4) 0.1433(2) 0.0205(11) Uani 1 1 d . . . . .
C76 C 0.4954(6) 0.4458(4) 0.1840(3) 0.0198(11) Uani 1 1 d . . . . .
H76 H 0.4680 0.3900 0.2115 0.024 Uiso 1 1 calc R U . . .
C77 C 0.4461(5) 0.5404(4) 0.1849(2) 0.0161(10) Uani 1 1 d . . . . .
C78 C 0.5145(5) 0.8292(4) 0.1246(2) 0.0174(11) Uani 1 1 d . . . . .
C79 C 0.6387(6) 0.8922(4) 0.1514(3) 0.0218(11) Uani 1 1 d . . . . .
H79 H 0.6701 0.8757 0.1886 0.026 Uiso 1 1 calc R U . . .
C80 C 0.7160(6) 0.9811(5) 0.1212(3) 0.0262(12) Uani 1 1 d . . . . .
H80 H 0.8031 1.0247 0.1378 0.031 Uiso 1 1 calc R U . . .
C81 C 0.6688(6) 1.0076(4) 0.0675(3) 0.0231(12) Uani 1 1 d . . . . .
H81 H 0.7244 1.0684 0.0481 0.028 Uiso 1 1 calc R U . . .
C82 C 0.5400(6) 0.9457(4) 0.0414(2) 0.0185(11) Uani 1 1 d . . . . .
C83 C 0.4659(5) 0.8551(4) 0.0720(2) 0.0152(10) Uani 1 1 d . . . . .
C84 C 0.3359(6) 0.7707(4) 0.0530(3) 0.0180(11) Uani 1 1 d . . . . .
C85 C 0.1839(6) 0.6021(4) 0.0965(3) 0.0231(12) Uani 1 1 d . . . . .
H85A H 0.2123 0.5398 0.1149 0.028 Uiso 1 1 calc R U . . .
H85B H 0.1524 0.5765 0.0558 0.028 Uiso 1 1 calc R U . . .
C86 C 0.0638(6) 0.6234(5) 0.1274(3) 0.0268(13) Uani 1 1 d . . . . .
H86A H -0.0081 0.5502 0.1278 0.032 Uiso 1 1 calc R U . . .
H86B H 0.0961 0.6492 0.1680 0.032 Uiso 1 1 calc R U . . .
C87 C -0.0004(7) 0.7104(6) 0.1010(3) 0.0308(14) Uani 1 1 d . . . . .
H87A H 0.0702 0.7844 0.1012 0.037 Uiso 1 1 calc R U . . .
H87B H -0.0731 0.7207 0.1252 0.037 Uiso 1 1 calc R U . . .
C88 C -0.0627(7) 0.6749(6) 0.0382(3) 0.0344(15) Uani 1 1 d . . . . .
H88A H 0.0108 0.6889 0.0118 0.052 Uiso 1 1 calc R U . . .
H88B H -0.1260 0.7195 0.0277 0.052 Uiso 1 1 calc R U . . .
H88C H -0.1123 0.5938 0.0355 0.052 Uiso 1 1 calc R U . . .
C89 C 0.1227(6) 0.6567(5) 0.3901(2) 0.0243(12) Uani 1 1 d . . . . .
H89A H 0.0905 0.5901 0.3622 0.029 Uiso 1 1 calc R U . . .
H89B H 0.0429 0.6636 0.4107 0.029 Uiso 1 1 calc R U . . .
C90 C 0.2279(9) 0.6332(6) 0.4341(3) 0.0448(18) Uani 1 1 d . . . . .
H90A H 0.3090 0.6287 0.4147 0.067 Uiso 1 1 calc R U . . .
H90B H 0.1880 0.5609 0.4515 0.067 Uiso 1 1 calc R U . . .
H90C H 0.2541 0.6948 0.4644 0.067 Uiso 1 1 calc R U . . .
C91 C 0.1599(7) 0.8649(5) 0.3832(3) 0.0272(13) Uani 1 1 d . . . . .
H91A H 0.0842 0.8492 0.4091 0.033 Uiso 1 1 calc R U . . .
H91B H 0.1362 0.9103 0.3518 0.033 Uiso 1 1 calc R U . . .
C92 C 0.2906(9) 0.9360(6) 0.4176(4) 0.0431(18) Uani 1 1 d . . . . .
H92A H 0.3050 0.8988 0.4531 0.065 Uiso 1 1 calc R U . . .
H92B H 0.2815 1.0120 0.4275 0.065 Uiso 1 1 calc R U . . .
H92C H 0.3689 0.9428 0.3942 0.065 Uiso 1 1 calc R U . . .
C93 C 0.6058(6) 0.2550(4) 0.1842(3) 0.0236(12) Uani 1 1 d . . . . .
H93A H 0.6000 0.2935 0.2219 0.028 Uiso 1 1 calc R U . . .
H93B H 0.6816 0.2193 0.1889 0.028 Uiso 1 1 calc R U . . .
C94 C 0.4739(7) 0.1620(5) 0.1701(3) 0.0346(15) Uani 1 1 d . . . . .
H94A H 0.4004 0.1960 0.1589 0.052 Uiso 1 1 calc R U . . .
H94B H 0.4503 0.1179 0.2042 0.052 Uiso 1 1 calc R U . . .
H94C H 0.4856 0.1117 0.1382 0.052 Uiso 1 1 calc R U . . .
C95 C 0.7267(6) 0.3233(5) 0.0966(3) 0.0292(13) Uani 1 1 d . . . . .
H95A H 0.7748 0.2668 0.1085 0.035 Uiso 1 1 calc R U . . .
H95B H 0.7968 0.3958 0.0917 0.035 Uiso 1 1 calc R U . . .
C96 C 0.6456(7) 0.2824(5) 0.0396(3) 0.0341(14) Uani 1 1 d . . . . .
H96A H 0.5800 0.2082 0.0436 0.051 Uiso 1 1 calc R U . . .
H96B H 0.7079 0.2751 0.0101 0.051 Uiso 1 1 calc R U . . .
H96C H 0.5962 0.3372 0.0280 0.051 Uiso 1 1 calc R U . . .
C97 C 0.4295(5) 0.8686(4) 0.6824(2) 0.0159(10) Uani 1 1 d . . . . .
C98 C 0.3815(6) 0.9638(4) 0.6809(3) 0.0195(11) Uani 1 1 d . . . . .
H98 H 0.4117 1.0221 0.7108 0.023 Uiso 1 1 calc R U . . .
C99 C 0.2899(6) 0.9757(4) 0.6362(3) 0.0196(11) Uani 1 1 d . . . . .
C100 C 0.2446(6) 0.8841(5) 0.5931(3) 0.0249(13) Uani 1 1 d . . . . .
H100 H 0.1806 0.8880 0.5623 0.030 Uiso 1 1 calc R U . . .
C101 C 0.2929(6) 0.7912(5) 0.5962(3) 0.0236(12) Uani 1 1 d . . . . .
H101 H 0.2619 0.7320 0.5667 0.028 Uiso 1 1 calc R U . . .
C102 C 0.3869(6) 0.7783(4) 0.6410(2) 0.0170(11) Uani 1 1 d . . . . .
C103 C 0.4413(6) 0.6749(4) 0.6422(2) 0.0177(11) Uani 1 1 d . . . . .
C104 C 0.5152(5) 0.6741(4) 0.7006(2) 0.0152(10) Uani 1 1 d . . . . .
C105 C 0.5541(6) 0.5794(4) 0.7188(3) 0.0179(11) Uani 1 1 d . . . . .
H105 H 0.5275 0.5117 0.6945 0.022 Uiso 1 1 calc R U . . .
C106 C 0.6286(6) 0.5790(4) 0.7701(3) 0.0193(11) Uani 1 1 d . . . . .
H106 H 0.6489 0.5111 0.7810 0.023 Uiso 1 1 calc R U . . .
C107 C 0.6760(6) 0.6801(4) 0.8073(2) 0.0177(11) Uani 1 1 d . . . . .
C108 C 0.6358(6) 0.7753(4) 0.7892(3) 0.0196(11) Uani 1 1 d . . . . .
H108 H 0.6632 0.8440 0.8128 0.024 Uiso 1 1 calc R U . . .
C109 C 0.5577(6) 0.7713(4) 0.7382(2) 0.0168(11) Uani 1 1 d . . . . .
C110 C 0.3272(6) 0.5665(4) 0.6245(2) 0.0178(11) Uani 1 1 d . . . . .
C111 C 0.2116(6) 0.5187(5) 0.6532(3) 0.0245(12) Uani 1 1 d . . . . .
H111 H 0.1975 0.5495 0.6897 0.029 Uiso 1 1 calc R U . . .
C112 C 0.1175(6) 0.4236(5) 0.6260(3) 0.0261(13) Uani 1 1 d . . . . .
H112 H 0.0359 0.3897 0.6439 0.031 Uiso 1 1 calc R U . . .
C113 C 0.1397(6) 0.3762(5) 0.5727(3) 0.0234(12) Uani 1 1 d . . . . .
H113 H 0.0719 0.3126 0.5547 0.028 Uiso 1 1 calc R U . . .
C114 C 0.2613(6) 0.4218(4) 0.5455(3) 0.0200(11) Uani 1 1 d . . . . .
C115 C 0.3519(6) 0.5187(4) 0.5729(2) 0.0166(11) Uani 1 1 d . . . . .
C116 C 0.4827(5) 0.5889(4) 0.5535(2) 0.0162(11) Uani 1 1 d . . . . .
C117 C 0.6521(6) 0.7711(5) 0.5879(3) 0.0290(14) Uani 1 1 d . . . . .
H11A H 0.6332 0.8415 0.6029 0.035 Uiso 1 1 calc R U . . .
H11B H 0.6651 0.7784 0.5462 0.035 Uiso 1 1 calc R U . . .
C118 C 0.7853(7) 0.7618(6) 0.6187(3) 0.0336(15) Uani 1 1 d . . . . .
H11C H 0.7696 0.7473 0.6597 0.040 Uiso 1 1 calc R U . . .
H11D H 0.8554 0.8359 0.6178 0.040 Uiso 1 1 calc R U . . .
C119 C 0.8423(7) 0.6682(6) 0.5928(3) 0.0386(16) Uani 1 1 d . . . . .
H11E H 0.9231 0.6643 0.6177 0.046 Uiso 1 1 calc R U . . .
H11F H 0.7721 0.5941 0.5933 0.046 Uiso 1 1 calc R U . . .
C120 C 0.8839(7) 0.6864(6) 0.5308(4) 0.0411(17) Uani 1 1 d . . . . .
H12A H 0.8021 0.6777 0.5046 0.062 Uiso 1 1 calc R U . . .
H12B H 0.9307 0.6299 0.5193 0.062 Uiso 1 1 calc R U . . .
H12C H 0.9457 0.7630 0.5289 0.062 Uiso 1 1 calc R U . . .
C121 C 0.2618(6) 1.1527(4) 0.6815(3) 0.0233(12) Uani 1 1 d . . . . .
H12D H 0.2675 1.1134 0.7176 0.028 Uiso 1 1 calc R U . . .
H12E H 0.1802 1.1816 0.6818 0.028 Uiso 1 1 calc R U . . .
C122 C 0.3881(7) 1.2532(5) 0.6811(3) 0.0293(14) Uani 1 1 d . . . . .
H12F H 0.4701 1.2261 0.6831 0.044 Uiso 1 1 calc R U . . .
H12G H 0.3921 1.3057 0.7145 0.044 Uiso 1 1 calc R U . . .
H12H H 0.3839 1.2928 0.6454 0.044 Uiso 1 1 calc R U . . .
C123 C 0.1843(6) 1.1014(5) 0.5772(3) 0.0256(13) Uani 1 1 d . . . . .
H12I H 0.2117 1.0604 0.5445 0.031 Uiso 1 1 calc R U . . .
H12J H 0.2213 1.1840 0.5727 0.031 Uiso 1 1 calc R U . . .
C124 C 0.0302(7) 1.0709(6) 0.5755(4) 0.0381(17) Uani 1 1 d . . . . .
H12K H -0.0070 0.9882 0.5759 0.057 Uiso 1 1 calc R U . . .
H12L H -0.0055 1.0977 0.5403 0.057 Uiso 1 1 calc R U . . .
H12M H 0.0029 1.1072 0.6094 0.057 Uiso 1 1 calc R U . . .
C125 C 0.8122(6) 0.7928(5) 0.8914(3) 0.0280(14) Uani 1 1 d . . . . .
H12N H 0.8399 0.8546 0.8646 0.034 Uiso 1 1 calc R U . . .
H12O H 0.8955 0.7895 0.9147 0.034 Uiso 1 1 calc R U . . .
C126 C 0.7140(8) 0.8235(6) 0.9319(3) 0.0361(16) Uani 1 1 d . . . . .
H12P H 0.6331 0.8314 0.9092 0.054 Uiso 1 1 calc R U . . .
H12Q H 0.7599 0.8955 0.9536 0.054 Uiso 1 1 calc R U . . .
H12R H 0.6858 0.7632 0.9589 0.054 Uiso 1 1 calc R U . . .
C127 C 0.7736(6) 0.5822(5) 0.8822(3) 0.0267(13) Uani 1 1 d . . . . .
H12S H 0.8572 0.6024 0.9090 0.032 Uiso 1 1 calc R U . . .
H12T H 0.7876 0.5306 0.8507 0.032 Uiso 1 1 calc R U . . .
C128 C 0.6551(8) 0.5186(6) 0.9144(4) 0.0405(17) Uani 1 1 d . . . . .
H12U H 0.6405 0.5685 0.9459 0.061 Uiso 1 1 calc R U . . .
H12V H 0.6752 0.4516 0.9304 0.061 Uiso 1 1 calc R U . . .
H12W H 0.5725 0.4945 0.8879 0.061 Uiso 1 1 calc R U . . .
N1 N 1.1284(5) -0.1778(4) 0.8037(2) 0.0224(10) Uani 1 1 d . . . . .
N2 N 0.6251(5) 0.2188(4) 0.5820(2) 0.0272(12) Uani 1 1 d . . . . .
N3 N 0.8481(5) 0.2245(4) 0.8436(2) 0.0214(10) Uani 1 1 d . . . . .
N4 N 1.1018(6) 0.5232(4) 0.9420(2) 0.0317(12) Uani 1 1 d . . . . .
H4A H 1.1625 0.5837 0.9585 0.038 Uiso 1 1 calc R U . . .
H4B H 1.0252 0.4936 0.9582 0.038 Uiso 1 1 calc R U . . .
N5 N 0.7729(5) 0.6083(4) 0.3098(2) 0.0243(11) Uani 1 1 d . . . . .
N6 N 1.1515(6) 0.1584(4) 0.0671(3) 0.0374(14) Uani 1 1 d . . . . .
N7 N 1.0771(5) 0.2202(4) 0.3375(2) 0.0181(9) Uani 1 1 d . . . . .
N8 N 0.8837(5) -0.0517(4) 0.4421(2) 0.0255(11) Uani 1 1 d . . . . .
H8A H 0.9681 -0.0170 0.4557 0.031 Uiso 1 1 calc R U . . .
H8B H 0.8339 -0.1087 0.4602 0.031 Uiso 1 1 calc R U . . .
N9 N 0.1698(5) 0.7577(4) 0.3579(2) 0.0227(10) Uani 1 1 d . . . . .
N10 N 0.6402(5) 0.3406(4) 0.1421(2) 0.0274(11) Uani 1 1 d . . . . .
N11 N 0.3018(5) 0.7010(4) 0.0975(2) 0.0174(9) Uani 1 1 d . . . . .
N12 N 0.4877(5) 0.9736(4) -0.0102(2) 0.0269(11) Uani 1 1 d . . . . .
H2A H 0.4058 0.9343 -0.0248 0.032 Uiso 1 1 calc R U . . .
H2B H 0.5360 1.0307 -0.0286 0.032 Uiso 1 1 calc R U . . .
N13 N 0.2432(6) 1.0708(4) 0.6328(2) 0.0291(12) Uani 1 1 d . . . . .
N14 N 0.7581(5) 0.6853(4) 0.8573(2) 0.0217(10) Uani 1 1 d . . . . .
N15 N 0.5335(5) 0.6757(3) 0.5944(2) 0.0176(9) Uani 1 1 d . . . . .
N16 N 0.2877(6) 0.3750(4) 0.4950(2) 0.0279(11) Uani 1 1 d . . . . .
H16A H 0.3639 0.4062 0.4788 0.034 Uiso 1 1 calc R U . . .
H16B H 0.2287 0.3136 0.4785 0.034 Uiso 1 1 calc R U . . .
O1 O 0.8566(4) 0.0295(3) 0.70918(18) 0.0241(9) Uani 1 1 d . . . . .
O2 O 0.8521(5) 0.3266(4) 0.9300(2) 0.0340(11) Uani 1 1 d . . . . .
O3 O 0.9882(4) 0.3762(3) 0.20317(17) 0.0230(9) Uani 1 1 d . . . . .
O4 O 1.1145(4) 0.1523(3) 0.42669(18) 0.0237(9) Uani 1 1 d . . . . .
O5 O 0.3610(4) 0.5459(3) 0.22783(18) 0.0235(9) Uani 1 1 d . . . . .
O6 O 0.2672(4) 0.7614(3) 0.00638(18) 0.0252(9) Uani 1 1 d . . . . .
O7 O 0.5232(4) 0.8702(3) 0.72779(18) 0.0224(9) Uani 1 1 d . . . . .
O8 O 0.5355(5) 0.5737(3) 0.50897(19) 0.0265(9) 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 O1 1.373(7) . ?
C1 C6 1.386(8) . ?
C1 C2 1.402(6) . ?
C2 C3 1.389(8) . ?
C3 N1 1.378(6) . ?
C3 C4 1.394(8) . ?
C4 C5 1.386(7) . ?
C5 C6 1.395(8) . ?
C6 C7 1.519(6) . ?
C7 N3 1.502(7) . ?
C7 C8 1.511(8) . ?
C7 C14 1.513(7) . ?
C8 C13 1.399(8) . ?
C8 C9 1.401(7) . ?
C9 C10 1.374(8) . ?
C10 C11 1.404(8) . ?
C11 N2 1.381(7) . ?
C11 C12 1.387(7) . ?
C12 C13 1.390(8) . ?
C13 O1 1.369(6) . ?
C14 C15 1.375(8) . ?
C14 C19 1.381(8) . ?
C15 C16 1.401(9) . ?
C16 C17 1.375(9) . ?
C17 C18 1.392(9) . ?
C18 N4 1.371(8) . ?
C18 C19 1.405(8) . ?
C19 C20 1.464(8) . ?
C20 O2 1.235(7) . ?
C20 N3 1.366(8) . ?
C21 N3 1.465(8) . ?
C21 C22 1.526(12) . ?
C22 C23 1.481(12) . ?
C23 C24 1.509(11) . ?
C25 N1 1.471(7) . ?
C25 C26 1.513(8) . ?
C27 N1 1.439(7) . ?
C27 C28 1.506(9) . ?
C29 N2 1.464(8) . ?
C29 C30 1.510(10) . ?
C31 N2 1.459(7) . ?
C31 C32 1.525(10) . ?
C33 C34 1.380(6) . ?
C33 C38 1.386(7) . ?
C33 O3 1.387(7) . ?
C34 C35 1.397(8) . ?
C35 N5 1.388(6) . ?
C35 C36 1.418(7) . ?
C36 C37 1.378(7) . ?
C37 C38 1.399(8) . ?
C38 C39 1.516(6) . ?
C39 N7 1.494(7) . ?
C39 C40 1.504(8) . ?
C39 C46 1.518(7) . ?
C40 C45 1.386(7) . ?
C40 C41 1.406(7) . ?
C41 C42 1.373(9) . ?
C42 C43 1.431(8) . ?
C43 N6 1.383(8) . ?
C43 C44 1.385(8) . ?
C44 C45 1.384(8) . ?
C45 O3 1.376(6) . ?
C46 C47 1.373(8) . ?
C46 C51 1.387(8) . ?
C47 C48 1.394(8) . ?
C48 C49 1.381(8) . ?
C49 C50 1.409(8) . ?
C50 N8 1.368(7) . ?
C50 C51 1.398(8) . ?
C51 C52 1.488(8) . ?
C52 O4 1.247(6) . ?
C52 N7 1.331(7) . ?
C53 N7 1.464(7) . ?
C53 C54 1.532(10) . ?
C54 C55 1.512(9) . ?
C55 C56 1.466(11) . ?
C57 N5 1.459(7) . ?
C57 C58 1.524(8) . ?
C59 N5 1.445(7) . ?
C59 C60 1.506(9) . ?
C61 C62 1.500(11) . ?
C61 N6 1.500(9) . ?
C63 N6 1.454(7) . ?
C63 C64 1.500(10) . ?
C65 O5 1.379(6) . ?
C65 C70 1.381(7) . ?
C65 C66 1.392(8) . ?
C66 C67 1.402(7) . ?
C67 N9 1.382(7) . ?
C67 C68 1.421(7) . ?
C68 C69 1.364(8) . ?
C69 C70 1.404(6) . ?
C70 C71 1.506(8) . ?
C71 C78 1.512(7) . ?
C71 C72 1.519(6) . ?
C71 N11 1.522(7) . ?
C72 C73 1.390(8) . ?
C72 C77 1.397(7) . ?
C73 C74 1.385(7) . ?
C74 C75 1.420(7) . ?
C75 N10 1.385(6) . ?
C75 C76 1.390(8) . ?
C76 C77 1.384(7) . ?
C77 O5 1.373(7) . ?
C78 C83 1.370(7) . ?
C78 C79 1.384(8) . ?
C79 C80 1.398(8) . ?
C80 C81 1.390(9) . ?
C81 C82 1.408(8) . ?
C82 N12 1.375(7) . ?
C82 C83 1.404(7) . ?
C83 C84 1.469(8) . ?
C84 O6 1.236(7) . ?
C84 N11 1.367(7) . ?
C85 N11 1.450(7) . ?
C85 C86 1.534(9) . ?
C86 C87 1.525(9) . ?
C87 C88 1.548(10) . ?
C89 N9 1.451(7) . ?
C89 C90 1.529(9) . ?
C91 N9 1.449(7) . ?
C91 C92 1.532(10) . ?
C93 N10 1.448(7) . ?
C93 C94 1.511(9) . ?
C95 N10 1.464(8) . ?
C95 C96 1.507(9) . ?
C97 O7 1.373(6) . ?
C97 C98 1.385(7) . ?
C97 C102 1.393(7) . ?
C98 C99 1.392(8) . ?
C99 N13 1.378(6) . ?
C99 C100 1.430(8) . ?
C100 C101 1.362(7) . ?
C101 C102 1.414(8) . ?
C102 C103 1.517(6) . ?
C103 N15 1.497(7) . ?
C103 C104 1.511(8) . ?
C103 C110 1.526(8) . ?
C104 C105 1.397(7) . ?
C104 C109 1.399(7) . ?
C105 C106 1.374(8) . ?
C106 C107 1.431(8) . ?
C107 N14 1.376(7) . ?
C107 C108 1.408(7) . ?
C108 C109 1.377(8) . ?
C109 O7 1.378(6) . ?
C110 C115 1.381(8) . ?
C110 C111 1.387(8) . ?
C111 C112 1.388(9) . ?
C112 C113 1.405(9) . ?
C113 C114 1.410(8) . ?
C114 N16 1.360(8) . ?
C114 C115 1.389(7) . ?
C115 C116 1.481(7) . ?
C116 O8 1.226(7) . ?
C116 N15 1.364(7) . ?
C117 N15 1.451(7) . ?
C117 C118 1.529(10) . ?
C118 C119 1.540(10) . ?
C119 C120 1.534(11) . ?
C121 N13 1.450(8) . ?
C121 C122 1.517(9) . ?
C123 N13 1.493(8) . ?
C123 C124 1.510(9) . ?
C125 N14 1.459(8) . ?
C125 C126 1.525(10) . ?
C127 N14 1.453(7) . ?
C127 C128 1.505(9) . ?

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
O1 C1 C6 122.8(4) . . ?
O1 C1 C2 114.7(5) . . ?
C6 C1 C2 122.5(5) . . ?
C3 C2 C1 120.0(5) . . ?
N1 C3 C2 121.0(5) . . ?
N1 C3 C4 121.2(5) . . ?
C2 C3 C4 117.8(5) . . ?
C5 C4 C3 121.6(5) . . ?
C4 C5 C6 121.3(5) . . ?
C1 C6 C5 116.8(5) . . ?
C1 C6 C7 122.1(5) . . ?
C5 C6 C7 121.1(5) . . ?
N3 C7 C8 110.5(4) . . ?
N3 C7 C14 100.3(4) . . ?
C8 C7 C14 113.6(4) . . ?
N3 C7 C6 110.1(4) . . ?
C8 C7 C6 109.9(4) . . ?
C14 C7 C6 112.0(4) . . ?
C13 C8 C9 115.6(5) . . ?
C13 C8 C7 121.7(4) . . ?
C9 C8 C7 122.6(5) . . ?
C10 C9 C8 122.8(5) . . ?
C9 C10 C11 120.6(5) . . ?
N2 C11 C12 120.5(5) . . ?
N2 C11 C10 121.5(5) . . ?
C12 C11 C10 118.0(5) . . ?
C11 C12 C13 120.6(5) . . ?
O1 C13 C12 114.8(5) . . ?
O1 C13 C8 122.8(5) . . ?
C12 C13 C8 122.5(5) . . ?
C15 C14 C19 121.2(5) . . ?
C15 C14 C7 128.7(5) . . ?
C19 C14 C7 110.1(5) . . ?
C14 C15 C16 117.1(6) . . ?
C17 C16 C15 122.4(6) . . ?
C16 C17 C18 120.6(6) . . ?
N4 C18 C17 122.0(6) . . ?
N4 C18 C19 121.1(6) . . ?
C17 C18 C19 116.9(5) . . ?
C14 C19 C18 121.8(5) . . ?
C14 C19 C20 109.7(5) . . ?
C18 C19 C20 128.4(5) . . ?
O2 C20 N3 125.8(6) . . ?
O2 C20 C19 127.8(6) . . ?
N3 C20 C19 106.4(5) . . ?
N3 C21 C22 115.2(6) . . ?
C23 C22 C21 115.7(6) . . ?
C22 C23 C24 114.5(7) . . ?
N1 C25 C26 112.8(5) . . ?
N1 C27 C28 113.6(5) . . ?
N2 C29 C30 116.0(6) . . ?
N2 C31 C32 114.2(5) . . ?
C34 C33 C38 123.8(5) . . ?
C34 C33 O3 114.2(4) . . ?
C38 C33 O3 122.0(4) . . ?
C33 C34 C35 119.9(5) . . ?
N5 C35 C34 121.8(5) . . ?
N5 C35 C36 120.4(5) . . ?
C34 C35 C36 117.8(5) . . ?
C37 C36 C35 120.0(5) . . ?
C36 C37 C38 123.0(5) . . ?
C33 C38 C37 115.5(4) . . ?
C33 C38 C39 122.7(5) . . ?
C37 C38 C39 121.8(4) . . ?
N7 C39 C40 111.8(4) . . ?
N7 C39 C38 109.5(4) . . ?
C40 C39 C38 109.8(4) . . ?
N7 C39 C46 100.5(4) . . ?
C40 C39 C46 113.8(4) . . ?
C38 C39 C46 111.0(4) . . ?
C45 C40 C41 115.2(5) . . ?
C45 C40 C39 122.5(4) . . ?
C41 C40 C39 122.2(5) . . ?
C42 C41 C40 123.5(5) . . ?
C41 C42 C43 119.8(5) . . ?
N6 C43 C44 121.3(5) . . ?
N6 C43 C42 121.7(5) . . ?
C44 C43 C42 117.0(5) . . ?
C45 C44 C43 121.4(5) . . ?
O3 C45 C44 114.2(4) . . ?
O3 C45 C40 122.6(5) . . ?
C44 C45 C40 123.1(5) . . ?
C47 C46 C51 121.2(5) . . ?
C47 C46 C39 129.2(5) . . ?
C51 C46 C39 109.4(5) . . ?
C46 C47 C48 117.4(5) . . ?
C49 C48 C47 122.0(5) . . ?
C48 C49 C50 121.0(5) . . ?
N8 C50 C51 121.1(5) . . ?
N8 C50 C49 122.8(5) . . ?
C51 C50 C49 116.0(5) . . ?
C46 C51 C50 122.3(5) . . ?
C46 C51 C52 108.8(5) . . ?
C50 C51 C52 128.8(5) . . ?
O4 C52 N7 127.4(5) . . ?
O4 C52 C51 126.1(5) . . ?
N7 C52 C51 106.5(4) . . ?
N7 C53 C54 114.9(5) . . ?
C55 C54 C53 115.5(6) . . ?
C56 C55 C54 115.5(7) . . ?
N5 C57 C58 113.7(5) . . ?
N5 C59 C60 113.5(5) . . ?
C62 C61 N6 112.4(6) . . ?
N6 C63 C64 113.1(6) . . ?
O5 C65 C70 123.0(5) . . ?
O5 C65 C66 114.2(4) . . ?
C70 C65 C66 122.8(4) . . ?
C65 C66 C67 120.5(5) . . ?
N9 C67 C66 121.3(5) . . ?
N9 C67 C68 121.8(5) . . ?
C66 C67 C68 116.9(5) . . ?
C69 C68 C67 120.8(5) . . ?
C68 C69 C70 122.7(5) . . ?
C65 C70 C69 116.2(5) . . ?
C65 C70 C71 121.3(4) . . ?
C69 C70 C71 122.4(4) . . ?
C70 C71 C78 116.1(4) . . ?
C70 C71 C72 109.4(4) . . ?
C78 C71 C72 111.3(4) . . ?
C70 C71 N11 110.3(4) . . ?
C78 C71 N11 100.5(4) . . ?
C72 C71 N11 108.8(4) . . ?
C73 C72 C77 115.8(4) . . ?
C73 C72 C71 122.7(5) . . ?
C77 C72 C71 121.5(5) . . ?
C74 C73 C72 123.1(5) . . ?
C73 C74 C75 119.9(5) . . ?
N10 C75 C76 122.6(5) . . ?
N10 C75 C74 119.8(5) . . ?
C76 C75 C74 117.6(4) . . ?
C77 C76 C75 120.7(5) . . ?
O5 C77 C76 115.2(4) . . ?
O5 C77 C72 121.9(4) . . ?
C76 C77 C72 122.9(5) . . ?
C83 C78 C79 122.0(5) . . ?
C83 C78 C71 110.3(5) . . ?
C79 C78 C71 127.6(5) . . ?
C78 C79 C80 116.7(5) . . ?
C81 C80 C79 121.9(6) . . ?
C80 C81 C82 121.0(5) . . ?
N12 C82 C83 121.7(5) . . ?
N12 C82 C81 122.3(5) . . ?
C83 C82 C81 116.0(5) . . ?
C78 C83 C82 122.3(5) . . ?
C78 C83 C84 109.9(4) . . ?
C82 C83 C84 127.6(5) . . ?
O6 C84 N11 124.8(5) . . ?
O6 C84 C83 128.5(5) . . ?
N11 C84 C83 106.7(5) . . ?
N11 C85 C86 113.9(5) . . ?
C87 C86 C85 115.5(5) . . ?
C86 C87 C88 112.9(6) . . ?
N9 C89 C90 116.0(5) . . ?
N9 C91 C92 114.4(5) . . ?
N10 C93 C94 115.7(5) . . ?
N10 C95 C96 112.3(5) . . ?
O7 C97 C98 114.8(5) . . ?
O7 C97 C102 122.5(4) . . ?
C98 C97 C102 122.7(5) . . ?
C97 C98 C99 121.2(5) . . ?
N13 C99 C98 122.4(5) . . ?
N13 C99 C100 120.5(5) . . ?
C98 C99 C100 117.2(5) . . ?
C101 C100 C99 120.2(5) . . ?
C100 C101 C102 123.3(5) . . ?
C97 C102 C101 115.5(4) . . ?
C97 C102 C103 122.6(5) . . ?
C101 C102 C103 121.9(5) . . ?
N15 C103 C104 111.3(4) . . ?
N15 C103 C102 110.3(4) . . ?
C104 C103 C102 109.1(4) . . ?
N15 C103 C110 100.5(4) . . ?
C104 C103 C110 114.6(4) . . ?
C102 C103 C110 110.8(4) . . ?
C105 C104 C109 115.6(5) . . ?
C105 C104 C103 122.5(5) . . ?
C109 C104 C103 121.8(4) . . ?
C106 C105 C104 123.5(5) . . ?
C105 C106 C107 120.5(4) . . ?
N14 C107 C108 121.7(5) . . ?
N14 C107 C106 122.3(4) . . ?
C108 C107 C106 116.0(5) . . ?
C109 C108 C107 121.7(5) . . ?
C108 C109 O7 114.4(5) . . ?
C108 C109 C104 122.7(4) . . ?
O7 C109 C104 122.9(5) . . ?
C115 C110 C111 121.9(5) . . ?
C115 C110 C103 110.2(5) . . ?
C111 C110 C103 127.8(5) . . ?
C110 C111 C112 116.8(6) . . ?
C111 C112 C113 121.7(6) . . ?
C112 C113 C114 120.9(6) . . ?
N16 C114 C115 121.8(6) . . ?
N16 C114 C113 122.2(5) . . ?
C115 C114 C113 116.0(5) . . ?
C110 C115 C114 122.5(5) . . ?
C110 C115 C116 109.0(5) . . ?
C114 C115 C116 128.5(5) . . ?
O8 C116 N15 126.0(5) . . ?
O8 C116 C115 127.1(5) . . ?
N15 C116 C115 106.8(5) . . ?
N15 C117 C118 114.7(5) . . ?
C117 C118 C119 114.9(6) . . ?
C120 C119 C118 114.1(6) . . ?
N13 C121 C122 114.3(5) . . ?
N13 C123 C124 111.0(6) . . ?
N14 C125 C126 115.4(6) . . ?
N14 C127 C128 115.1(5) . . ?
C3 N1 C27 122.0(5) . . ?
C3 N1 C25 121.9(5) . . ?
C27 N1 C25 116.1(4) . . ?
C11 N2 C31 121.8(5) . . ?
C11 N2 C29 120.5(5) . . ?
C31 N2 C29 117.0(5) . . ?
C20 N3 C21 123.0(5) . . ?
C20 N3 C7 113.2(5) . . ?
C21 N3 C7 122.6(5) . . ?
C35 N5 C59 121.6(4) . . ?
C35 N5 C57 121.3(5) . . ?
C59 N5 C57 117.1(4) . . ?
C43 N6 C63 123.1(5) . . ?
C43 N6 C61 121.0(5) . . ?
C63 N6 C61 115.7(5) . . ?
C52 N7 C53 123.8(5) . . ?
C52 N7 C39 114.2(4) . . ?
C53 N7 C39 121.1(4) . . ?
C67 N9 C91 121.6(5) . . ?
C67 N9 C89 120.0(4) . . ?
C91 N9 C89 117.9(5) . . ?
C75 N10 C93 120.1(5) . . ?
C75 N10 C95 121.7(4) . . ?
C93 N10 C95 118.1(4) . . ?
C84 N11 C85 125.5(5) . . ?
C84 N11 C71 111.9(4) . . ?
C85 N11 C71 121.5(4) . . ?
C99 N13 C121 121.6(5) . . ?
C99 N13 C123 121.7(5) . . ?
C121 N13 C123 116.4(4) . . ?
C107 N14 C127 120.9(5) . . ?
C107 N14 C125 120.2(4) . . ?
C127 N14 C125 118.1(5) . . ?
C116 N15 C117 123.7(5) . . ?
C116 N15 C103 113.3(4) . . ?
C117 N15 C103 122.1(5) . . ?
C13 O1 C1 118.7(4) . . ?
C45 O3 C33 118.9(4) . . ?
C77 O5 C65 118.1(4) . . ?
C97 O7 C109 118.2(4) . . ?

_refine_diff_density_max         0.418
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.077

####################################################################### 
# 
# 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_p6
_database_code_depnum_ccdc_archive 'CCDC 1901370'
loop_
_audit_author_name
_audit_author_address
'Qingkai QI'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-04 downloaded from the CCDC.
;
_audit_creation_date             2019-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H44 N4 O2'
_chemical_formula_sum            'C34 H44 N4 O2'
_chemical_formula_weight         540.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.0084(7)
_cell_length_b                   12.0389(7)
_cell_length_c                   12.2322(8)
_cell_angle_alpha                79.257(5)
_cell_angle_beta                 66.321(6)
_cell_angle_gamma                78.199(5)
_cell_volume                     1443.40(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2863
_cell_measurement_temperature    130(6)
_cell_measurement_theta_max      29.3070
_cell_measurement_theta_min      3.7810
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.990
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11619
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.387
_diffrn_reflns_theta_min         2.867
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4070
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -78.00  11.00   1.00   97.18    --  -11.91 -77.00  90.00   89
  2  ω    -10.00  77.00   1.00   97.18    --   12.07  57.00   0.00   87
  3  ω     45.00  72.00   1.00   97.18    --   12.07  37.00-180.00   27
  4  ω    -61.00  42.00   1.00   97.18    --   12.07 -57.00-150.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0282730000
_diffrn_orient_matrix_UB_12      0.0285372000
_diffrn_orient_matrix_UB_13      -0.0423805000
_diffrn_orient_matrix_UB_21      -0.0532819000
_diffrn_orient_matrix_UB_22      -0.0331288000
_diffrn_orient_matrix_UB_23      0.0268618000
_diffrn_orient_matrix_UB_31      -0.0376373000
_diffrn_orient_matrix_UB_32      0.0419591000
_diffrn_orient_matrix_UB_33      0.0393236000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3685
_reflns_number_total             6788
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6788
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0665
_refine_ls_restrained_S_all      0.985
_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)+(0.1041P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1948
_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. Restrained distances
 C21-C20
 1.54 with sigma of 0.01
 H21E_$1-H10
 2.1 with sigma of 0.005
 H21F_$1-H10
 2.1 with sigma of 0.005
 N2-C20 \\sim N2-C20A
 with sigma of 0.02
 C21-C20 \\sim C21A-C20A
 with sigma of 0.02
 C22-C20 \\sim C22-C20A
 with sigma of 0.02
3. Rigid bond restraints
 C25, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(C21A)
Uanis(C20) = Uanis(C20A)
5. Others
 Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B), C26(H26A,H26B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C20A(H20C,H20D)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C16(H16), C18(H18),
 C19(H19)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C21A(H21D,H21E,H21F)
;
_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
O1 O 0.43497(15) 0.08382(13) 0.88459(13) 0.0348(4) Uani 1 1 d . . . . .
O2 O 0.33820(17) 0.55717(13) 0.58580(13) 0.0387(4) Uani 1 1 d . . . . .
N1 N 0.40758(17) 0.25013(14) 0.76625(16) 0.0310(5) Uani 1 1 d . . . . .
N2 N 0.4602(2) 0.75738(17) 0.8170(2) 0.0433(5) Uani 1 1 d D . . . .
N3 N 0.2162(2) 0.40515(18) 0.32131(18) 0.0436(5) Uani 1 1 d . . . . .
N4 N 0.1492(2) 0.04438(17) 1.08011(16) 0.0379(5) Uani 1 1 d . . . . .
C00D C 0.2824(2) 0.36459(18) 0.6454(2) 0.0311(5) Uani 1 1 d . . . . .
C1 C 0.3635(2) 0.16922(17) 0.86186(18) 0.0272(5) Uani 1 1 d . . . . .
C2 C 0.2178(2) 0.20843(18) 0.92687(18) 0.0272(5) Uani 1 1 d . . . . .
C3 C 0.1189(2) 0.15441(19) 1.02521(19) 0.0304(5) Uani 1 1 d . . . . .
C4 C -0.0104(2) 0.2160(2) 1.0620(2) 0.0385(6) Uani 1 1 d . . . . .
H4 H -0.080316 0.183097 1.127555 0.046 Uiso 1 1 calc R . . . .
C5 C -0.0400(2) 0.3228(2) 1.0065(2) 0.0423(6) Uani 1 1 d . . . . .
H5 H -0.129124 0.361831 1.035585 0.051 Uiso 1 1 calc R . . . .
C6 C 0.0570(2) 0.3745(2) 0.9095(2) 0.0368(6) Uani 1 1 d . . . . .
H6 H 0.036579 0.448159 0.871507 0.044 Uiso 1 1 calc R . . . .
C7 C 0.1849(2) 0.31420(18) 0.87043(19) 0.0287(5) Uani 1 1 d . . . . .
C8 C 0.3052(2) 0.35051(18) 0.7613(2) 0.0306(5) Uani 1 1 d . . . . .
C9 C 0.3453(2) 0.45828(18) 0.7747(2) 0.0294(5) Uani 1 1 d . . . . .
C10 C 0.3703(2) 0.46819(19) 0.8754(2) 0.0368(6) Uani 1 1 d . . . . .
H10 H 0.360837 0.405210 0.936481 0.044 Uiso 1 1 calc DR . . . .
C11 C 0.4078(2) 0.5642(2) 0.8906(2) 0.0381(6) Uani 1 1 d . . . . .
H11 H 0.424284 0.565999 0.960706 0.046 Uiso 1 1 calc R . . . .
C12 C 0.4221(2) 0.66069(19) 0.8028(2) 0.0345(6) Uani 1 1 d . . . . .
C13 C 0.3974(2) 0.65173(19) 0.7021(2) 0.0346(6) Uani 1 1 d . . . . .
H13 H 0.406180 0.714459 0.640791 0.042 Uiso 1 1 calc R . . . .
C14 C 0.3603(2) 0.55313(18) 0.68940(19) 0.0312(5) Uani 1 1 d . . . . .
C15 C 0.2983(2) 0.46414(18) 0.56597(19) 0.0304(5) Uani 1 1 d . . . . .
C16 C 0.2758(2) 0.4777(2) 0.4611(2) 0.0352(6) Uani 1 1 d . . . . .
H16 H 0.287538 0.548050 0.410340 0.042 Uiso 1 1 calc R . . . .
C17 C 0.2365(2) 0.3914(2) 0.4277(2) 0.0360(6) Uani 1 1 d . . . . .
C18 C 0.2205(3) 0.2894(2) 0.5072(2) 0.0427(6) Uani 1 1 d . . . . .
H18 H 0.193498 0.227728 0.488403 0.051 Uiso 1 1 calc R . . . .
C19 C 0.2435(2) 0.2780(2) 0.6114(2) 0.0401(6) Uani 1 1 d . . . . .
H19 H 0.232243 0.207807 0.662437 0.048 Uiso 1 1 calc R . . . .
C20 C 0.4662(6) 0.7718(5) 0.9270(4) 0.0674(17) Uani 0.863(7) 1 d D . P A 1
H20A H 0.524662 0.705454 0.949757 0.081 Uiso 0.863(7) 1 calc R . P A 1
H20B H 0.507552 0.840990 0.915225 0.081 Uiso 0.863(7) 1 calc R . P A 1
C21 C 0.3410(7) 0.7821(5) 1.0207(5) 0.128(3) Uani 0.863(7) 1 d D . P A 1
H21A H 0.283719 0.849551 1.000297 0.193 Uiso 0.863(7) 1 calc GR . P A 1
H21B H 0.351769 0.790383 1.094363 0.193 Uiso 0.863(7) 1 calc GR . P A 1
H21C H 0.299571 0.713716 1.033215 0.193 Uiso 0.863(7) 1 calc GR . P A 1
C22 C 0.4741(3) 0.8567(2) 0.7272(3) 0.0473(7) Uani 1 1 d D . . . .
H22A H 0.517743 0.830424 0.646457 0.057 Uiso 1 1 calc R . . . .
H22B H 0.534022 0.903010 0.735362 0.057 Uiso 1 1 calc R . . . .
C23 C 0.3443(3) 0.9312(2) 0.7357(3) 0.0532(7) Uani 1 1 d . . . . .
H23A H 0.361792 0.995847 0.672280 0.080 Uiso 1 1 calc GR . . . .
H23B H 0.301512 0.959761 0.814402 0.080 Uiso 1 1 calc GR . . . .
H23C H 0.284874 0.886710 0.725837 0.080 Uiso 1 1 calc GR . . . .
C24 C 0.2186(3) 0.5151(2) 0.2497(2) 0.0491(7) Uani 1 1 d . U . . .
H24A H 0.221213 0.504627 0.170324 0.059 Uiso 1 1 calc R . . . .
H24B H 0.302434 0.543529 0.235864 0.059 Uiso 1 1 calc R . . . .
C25 C 0.1052(4) 0.6030(3) 0.3015(3) 0.0872(12) Uani 1 1 d . U . . .
H25A H 0.115807 0.674289 0.246931 0.131 Uiso 1 1 calc GR . . . .
H25B H 0.102522 0.615913 0.379199 0.131 Uiso 1 1 calc GR . . . .
H25C H 0.021453 0.577424 0.312846 0.131 Uiso 1 1 calc GR . . . .
C26 C 0.1756(3) 0.3155(3) 0.2849(2) 0.0524(7) Uani 1 1 d . . . . .
H26A H 0.222084 0.240941 0.307762 0.063 Uiso 1 1 calc R . . . .
H26B H 0.205056 0.326166 0.196235 0.063 Uiso 1 1 calc R . . . .
C27 C 0.0291(3) 0.3120(3) 0.3383(3) 0.0709(10) Uani 1 1 d . . . . .
H27A H 0.009263 0.250211 0.308828 0.106 Uiso 1 1 calc GR . . . .
H27B H -0.017963 0.385047 0.315316 0.106 Uiso 1 1 calc GR . . . .
H27C H -0.000622 0.298278 0.426053 0.106 Uiso 1 1 calc GR . . . .
C28 C 0.5477(2) 0.24885(19) 0.6867(2) 0.0367(6) Uani 1 1 d . . . . .
H28A H 0.600486 0.251429 0.735196 0.044 Uiso 1 1 calc R . . . .
H28B H 0.556184 0.318801 0.628546 0.044 Uiso 1 1 calc R . . . .
C29 C 0.6072(2) 0.1471(2) 0.6184(2) 0.0414(6) Uani 1 1 d . . . . .
H29A H 0.560199 0.147660 0.564216 0.050 Uiso 1 1 calc R . . . .
H29B H 0.593296 0.076557 0.675720 0.050 Uiso 1 1 calc R . . . .
C30 C 0.7563(3) 0.1455(2) 0.5446(2) 0.0488(7) Uani 1 1 d . . . . .
H30A H 0.768860 0.206391 0.476005 0.059 Uiso 1 1 calc R . . . .
H30B H 0.800152 0.162254 0.595051 0.059 Uiso 1 1 calc R . . . .
C31 C 0.8229(3) 0.0322(3) 0.4976(2) 0.0629(9) Uani 1 1 d . . . . .
H31A H 0.916855 0.037117 0.445718 0.094 Uiso 1 1 calc GR . . . .
H31B H 0.776621 0.013141 0.451322 0.094 Uiso 1 1 calc GR . . . .
H31C H 0.818422 -0.027264 0.565244 0.094 Uiso 1 1 calc GR . . . .
C32 C 0.2445(3) 0.0342(2) 1.1388(2) 0.0506(7) Uani 1 1 d . . . . .
H32A H 0.320204 0.074190 1.085836 0.076 Uiso 1 1 calc GR . . . .
H32B H 0.277322 -0.046725 1.155241 0.076 Uiso 1 1 calc GR . . . .
H32C H 0.199753 0.068160 1.214502 0.076 Uiso 1 1 calc GR . . . .
C33 C 0.0346(3) -0.0152(3) 1.1544(2) 0.0572(8) Uani 1 1 d . . . . .
H33A H -0.015414 0.020013 1.228982 0.086 Uiso 1 1 calc GR . . . .
H33B H 0.066599 -0.095734 1.173656 0.086 Uiso 1 1 calc GR . . . .
H33C H -0.024054 -0.009934 1.110447 0.086 Uiso 1 1 calc GR . . . .
C20A C 0.431(5) 0.779(4) 0.9369(16) 0.0674(17) Uani 0.137(7) 1 d D . P A 2
H20C H 0.396180 0.862123 0.932819 0.081 Uiso 0.137(7) 1 calc R . P A 2
H20D H 0.350131 0.741711 0.982804 0.081 Uiso 0.137(7) 1 calc R . P A 2
C21A C 0.487(4) 0.7677(12) 1.021(3) 0.128(3) Uani 0.137(7) 1 d D . P A 2
H21D H 0.458675 0.837108 1.061071 0.193 Uiso 0.137(7) 1 calc GR . P A 2
H21E H 0.584976 0.755468 0.981237 0.193 Uiso 0.137(7) 1 calc DGR . P A 2
H21F H 0.457748 0.702050 1.080516 0.193 Uiso 0.137(7) 1 calc DGR . 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
O1 C1 1.221(2) . ?
O2 C14 1.374(3) . ?
O2 C15 1.376(3) . ?
N1 C1 1.366(3) . ?
N1 C8 1.485(3) . ?
N1 C28 1.455(3) . ?
N2 C12 1.376(3) . ?
N2 C20 1.416(5) . ?
N2 C22 1.452(3) . ?
N2 C20A 1.433(18) . ?
N3 C17 1.381(3) . ?
N3 C24 1.444(3) . ?
N3 C26 1.449(4) . ?
N4 C3 1.409(3) . ?
N4 C32 1.467(3) . ?
N4 C33 1.462(3) . ?
C00D C8 1.510(3) . ?
C00D C15 1.388(3) . ?
C00D C19 1.390(3) . ?
C1 C2 1.495(3) . ?
C2 C3 1.415(3) . ?
C2 C7 1.384(3) . ?
C3 C4 1.399(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.379(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(3) . ?
C7 C8 1.525(3) . ?
C8 C9 1.509(3) . ?
C9 C10 1.395(3) . ?
C9 C14 1.384(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.371(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.414(3) . ?
C12 C13 1.391(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(3) . ?
C15 C16 1.377(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.385(3) . ?
C17 C18 1.411(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.373(4) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.394(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.500(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.467(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.483(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.498(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.521(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.508(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C20A H20C 0.9900 . ?
C20A H20D 0.9900 . ?
C20A C21A 1.37(2) . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 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
C14 O2 C15 119.13(17) . . ?
C1 N1 C8 114.46(17) . . ?
C1 N1 C28 123.24(17) . . ?
C28 N1 C8 121.55(16) . . ?
C12 N2 C20 121.6(3) . . ?
C12 N2 C22 121.0(2) . . ?
C12 N2 C20A 117.9(17) . . ?
C20 N2 C22 116.6(3) . . ?
C20A N2 C22 115.9(16) . . ?
C17 N3 C24 120.5(2) . . ?
C17 N3 C26 121.9(2) . . ?
C24 N3 C26 117.2(2) . . ?
C3 N4 C32 115.5(2) . . ?
C3 N4 C33 116.0(2) . . ?
C33 N4 C32 112.0(2) . . ?
C15 C00D C8 122.7(2) . . ?
C15 C00D C19 115.5(2) . . ?
C19 C00D C8 121.9(2) . . ?
O1 C1 N1 123.94(19) . . ?
O1 C1 C2 129.80(19) . . ?
N1 C1 C2 106.25(17) . . ?
C3 C2 C1 131.1(2) . . ?
C7 C2 C1 107.96(17) . . ?
C7 C2 C3 120.85(19) . . ?
N4 C3 C2 121.68(19) . . ?
C4 C3 N4 122.54(19) . . ?
C4 C3 C2 115.8(2) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 C3 122.3(2) . . ?
C5 C4 H4 118.8 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.5(2) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 H6 121.5 . . ?
C7 C6 C5 117.1(2) . . ?
C7 C6 H6 121.5 . . ?
C2 C7 C8 111.25(18) . . ?
C6 C7 C2 122.4(2) . . ?
C6 C7 C8 126.3(2) . . ?
N1 C8 C00D 110.88(18) . . ?
N1 C8 C7 99.94(16) . . ?
N1 C8 C9 111.11(19) . . ?
C00D C8 C7 112.47(19) . . ?
C9 C8 C00D 110.03(17) . . ?
C9 C8 C7 112.08(18) . . ?
C10 C9 C8 121.49(19) . . ?
C14 C9 C8 123.0(2) . . ?
C14 C9 C10 115.5(2) . . ?
C9 C10 H10 118.4 . . ?
C11 C10 C9 123.3(2) . . ?
C11 C10 H10 118.4 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.6(2) . . ?
C12 C11 H11 119.7 . . ?
N2 C12 C11 121.0(2) . . ?
N2 C12 C13 122.4(2) . . ?
C13 C12 C11 116.6(2) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.3(2) . . ?
C14 C13 H13 119.4 . . ?
O2 C14 C9 122.5(2) . . ?
O2 C14 C13 114.71(19) . . ?
C9 C14 C13 122.8(2) . . ?
O2 C15 C00D 122.6(2) . . ?
O2 C15 C16 114.63(19) . . ?
C16 C15 C00D 122.8(2) . . ?
C15 C16 H16 119.2 . . ?
C15 C16 C17 121.6(2) . . ?
C17 C16 H16 119.2 . . ?
N3 C17 C16 121.2(2) . . ?
N3 C17 C18 122.5(2) . . ?
C16 C17 C18 116.3(2) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.0(2) . . ?
C19 C18 H18 119.5 . . ?
C00D C19 H19 118.6 . . ?
C18 C19 C00D 122.8(2) . . ?
C18 C19 H19 118.6 . . ?
N2 C20 H20A 108.9 . . ?
N2 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 N2 113.3(4) . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 108.7 . . ?
N2 C22 H22B 108.7 . . ?
N2 C22 C23 114.3(2) . . ?
H22A C22 H22B 107.6 . . ?
C23 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C24 H24A 108.4 . . ?
N3 C24 H24B 108.4 . . ?
N3 C24 C25 115.4(2) . . ?
H24A C24 H24B 107.5 . . ?
C25 C24 H24A 108.4 . . ?
C25 C24 H24B 108.4 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 H26A 108.7 . . ?
N3 C26 H26B 108.7 . . ?
N3 C26 C27 114.2(2) . . ?
H26A C26 H26B 107.6 . . ?
C27 C26 H26A 108.7 . . ?
C27 C26 H26B 108.7 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N1 C28 H28A 108.6 . . ?
N1 C28 H28B 108.6 . . ?
N1 C28 C29 114.5(2) . . ?
H28A C28 H28B 107.6 . . ?
C29 C28 H28A 108.6 . . ?
C29 C28 H28B 108.6 . . ?
C28 C29 H29A 109.2 . . ?
C28 C29 H29B 109.2 . . ?
C28 C29 C30 112.2(2) . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 H29A 109.2 . . ?
C30 C29 H29B 109.2 . . ?
C29 C30 H30A 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 C29 112.4(2) . . ?
C31 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N4 C32 H32A 109.5 . . ?
N4 C32 H32B 109.5 . . ?
N4 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N4 C33 H33A 109.5 . . ?
N4 C33 H33B 109.5 . . ?
N4 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N2 C20A H20C 101.4 . . ?
N2 C20A H20D 101.4 . . ?
H20C C20A H20D 104.6 . . ?
C21A C20A N2 142(4) . . ?
C21A C20A H20C 101.4 . . ?
C21A C20A H20D 101.4 . . ?
C20A C21A H21D 109.5 . . ?
C20A C21A H21E 109.5 . . ?
C20A C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C21A H21D O1 0.98 2.01 2.73(3) 128.8 2_667 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -6.6(4) . . . . ?
O1 C1 C2 C7 176.2(2) . . . . ?
O2 C15 C16 C17 179.35(19) . . . . ?
N1 C1 C2 C3 173.7(2) . . . . ?
N1 C1 C2 C7 -3.6(3) . . . . ?
N1 C8 C9 C10 -57.8(3) . . . . ?
N1 C8 C9 C14 122.0(2) . . . . ?
N1 C28 C29 C30 -175.4(2) . . . . ?
N2 C12 C13 C14 179.4(2) . . . . ?
N3 C17 C18 C19 179.0(2) . . . . ?
N4 C3 C4 C5 -178.8(2) . . . . ?
C00D C8 C9 C10 178.99(19) . . . . ?
C00D C8 C9 C14 -1.2(3) . . . . ?
C00D C15 C16 C17 -0.6(3) . . . . ?
C1 N1 C8 C00D -121.3(2) . . . . ?
C1 N1 C8 C7 -2.5(3) . . . . ?
C1 N1 C8 C9 116.0(2) . . . . ?
C1 N1 C28 C29 62.9(3) . . . . ?
C1 C2 C3 N4 -0.1(4) . . . . ?
C1 C2 C3 C4 -178.6(2) . . . . ?
C1 C2 C7 C6 -179.5(2) . . . . ?
C1 C2 C7 C8 2.1(3) . . . . ?
C2 C3 C4 C5 -0.2(4) . . . . ?
C2 C7 C8 N1 0.0(2) . . . . ?
C2 C7 C8 C00D 117.7(2) . . . . ?
C2 C7 C8 C9 -117.7(2) . . . . ?
C3 C2 C7 C6 3.0(4) . . . . ?
C3 C2 C7 C8 -175.5(2) . . . . ?
C3 C4 C5 C6 1.0(4) . . . . ?
C4 C5 C6 C7 0.2(4) . . . . ?
C5 C6 C7 C2 -2.1(4) . . . . ?
C5 C6 C7 C8 176.0(2) . . . . ?
C6 C7 C8 N1 -178.3(2) . . . . ?
C6 C7 C8 C00D -60.7(3) . . . . ?
C6 C7 C8 C9 63.9(3) . . . . ?
C7 C2 C3 N4 176.9(2) . . . . ?
C7 C2 C3 C4 -1.7(3) . . . . ?
C7 C8 C9 C10 53.1(3) . . . . ?
C7 C8 C9 C14 -127.1(2) . . . . ?
C8 N1 C1 O1 -176.0(2) . . . . ?
C8 N1 C1 C2 3.8(3) . . . . ?
C8 N1 C28 C29 -127.6(2) . . . . ?
C8 C00D C15 O2 1.0(3) . . . . ?
C8 C00D C15 C16 -179.1(2) . . . . ?
C8 C00D C19 C18 179.2(2) . . . . ?
C8 C9 C10 C11 179.6(2) . . . . ?
C8 C9 C14 O2 0.7(3) . . . . ?
C8 C9 C14 C13 -179.9(2) . . . . ?
C9 C10 C11 C12 0.6(4) . . . . ?
C10 C9 C14 O2 -179.42(19) . . . . ?
C10 C9 C14 C13 0.0(3) . . . . ?
C10 C11 C12 N2 -179.7(2) . . . . ?
C10 C11 C12 C13 -0.5(3) . . . . ?
C11 C12 C13 C14 0.2(3) . . . . ?
C12 N2 C20 C21 -66.5(6) . . . . ?
C12 N2 C22 C23 80.4(3) . . . . ?
C12 N2 C20A C21A 98(5) . . . . ?
C12 C13 C14 O2 179.48(19) . . . . ?
C12 C13 C14 C9 0.0(3) . . . . ?
C14 O2 C15 C00D -1.5(3) . . . . ?
C14 O2 C15 C16 178.53(19) . . . . ?
C14 C9 C10 C11 -0.3(3) . . . . ?
C15 O2 C14 C9 0.7(3) . . . . ?
C15 O2 C14 C13 -178.76(18) . . . . ?
C15 C00D C8 N1 -123.0(2) . . . . ?
C15 C00D C8 C7 126.1(2) . . . . ?
C15 C00D C8 C9 0.3(3) . . . . ?
C15 C00D C19 C18 -0.7(3) . . . . ?
C15 C16 C17 N3 -178.9(2) . . . . ?
C15 C16 C17 C18 0.2(3) . . . . ?
C16 C17 C18 C19 -0.1(4) . . . . ?
C17 N3 C24 C25 -69.8(4) . . . . ?
C17 N3 C26 C27 83.5(3) . . . . ?
C17 C18 C19 C00D 0.4(4) . . . . ?
C19 C00D C8 N1 57.1(3) . . . . ?
C19 C00D C8 C7 -53.8(3) . . . . ?
C19 C00D C8 C9 -179.6(2) . . . . ?
C19 C00D C15 O2 -179.11(19) . . . . ?
C19 C00D C15 C16 0.8(3) . . . . ?
C20 N2 C12 C11 -10.1(4) . . . . ?
C20 N2 C12 C13 170.7(3) . . . . ?
C20 N2 C22 C23 -89.6(4) . . . . ?
C22 N2 C12 C11 -179.6(2) . . . . ?
C22 N2 C12 C13 1.2(3) . . . . ?
C22 N2 C20 C21 103.5(5) . . . . ?
C22 N2 C20A C21A -107(5) . . . . ?
C24 N3 C17 C16 -8.1(3) . . . . ?
C24 N3 C17 C18 172.8(2) . . . . ?
C24 N3 C26 C27 -88.8(3) . . . . ?
C26 N3 C17 C16 179.8(2) . . . . ?
C26 N3 C17 C18 0.7(4) . . . . ?
C26 N3 C24 C25 102.7(3) . . . . ?
C28 N1 C1 O1 -5.8(4) . . . . ?
C28 N1 C1 C2 174.0(2) . . . . ?
C28 N1 C8 C00D 68.3(3) . . . . ?
C28 N1 C8 C7 -172.8(2) . . . . ?
C28 N1 C8 C9 -54.4(3) . . . . ?
C28 C29 C30 C31 167.5(2) . . . . ?
C32 N4 C3 C2 63.9(3) . . . . ?
C32 N4 C3 C4 -117.6(3) . . . . ?
C33 N4 C3 C2 -162.3(2) . . . . ?
C33 N4 C3 C4 16.2(4) . . . . ?
C20A N2 C12 C11 -26(2) . . . . ?
C20A N2 C12 C13 155(2) . . . . ?
C20A N2 C22 C23 -74(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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.600
####################################################################### 
# 
# 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_qqk190304_tw
_database_code_depnum_ccdc_archive 'CCDC 1901371'
loop_
_audit_author_name
_audit_author_address
'Qingkai QI'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-04 downloaded from the CCDC.
;
_audit_creation_date             2019-03-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H42 N4 O3'
_chemical_formula_sum            'C34 H42 N4 O3'
_chemical_formula_weight         554.71
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   21.0138(12)
_cell_length_b                   10.9924(7)
_cell_length_c                   26.6620(16)
_cell_angle_alpha                90
_cell_angle_beta                 97.694(5)
_cell_angle_gamma                90
_cell_volume                     6103.3(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4750
_cell_measurement_temperature    128(2)
_cell_measurement_theta_max      28.9510
_cell_measurement_theta_min      3.8400
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.991
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            8465
_diffrn_reflns_point_group_measured_fraction_full 0.698
_diffrn_reflns_point_group_measured_fraction_max 0.679
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.414
_diffrn_reflns_theta_min         3.217
_diffrn_ambient_temperature      128.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.361
_reflns_Friedel_fraction_full    0.398
_reflns_Friedel_fraction_max     0.361
_reflns_number_gt                7843
_reflns_number_total             8465
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 
;
 Flack x determined using 1894 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -2.5(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         8465
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0799
_refine_ls_restrained_S_all      1.132
_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)+(0.0419P)²+35.7226P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.1963
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.733(3)
 0.267(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C28B-C27 = C28-C27
 1.54 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C28) = Uanis(C28B)
5. Others
 Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C27(H27A,H27B), C27(H27C,
 H27D), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B), C21A(H21C,H21D),
 C22A(H22C,H22D), C23A(H23C,H23D), C27A(H27E,H27F), C29A(H29C,H29D), C31A(H31C,
 H31D), C33A(H33C,H33D)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C16(H16),
 C18(H18), C19(H19), N2A(H2A), C4A(H4A), C5A(H5A), C6A(H6A), C10A(H10A),
 C11A(H11A), C13A(H13A), C16A(H16A), C18A(H18A), C19A(H19A)
6.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C24A(H24D,H24E,H24F),
 C26A(H26D,H26E,H26F), C28A(H28G,H28H,H28I), C30A(H30D,H30E,H30F), C32A(H32D,
 H32E,H32F), C34A(H34D,H34E,H34F), C28B(H28D,H28E,H28F)
;
_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
O1 O 0.3231(2) 0.1805(5) 0.5285(2) 0.0197(11) Uani 1 1 d . . . . .
O2 O 0.2990(3) -0.0248(7) 0.3513(3) 0.053(2) Uani 1 1 d . . . . .
O3 O 0.6071(2) 0.0010(5) 0.6202(2) 0.0199(11) Uani 1 1 d . . . . .
N1 N 0.4164(3) 0.1210(5) 0.5789(2) 0.0121(12) Uani 1 1 d . . . . .
N2 N 0.3199(3) 0.0748(6) 0.4265(2) 0.0211(14) Uani 1 1 d . . . . .
H2 H 0.303847 0.130311 0.444959 0.025 Uiso 1 1 calc R . . . .
N3 N 0.6900(3) 0.3811(6) 0.5712(3) 0.0302(17) Uani 1 1 d . . . . .
N4 N 0.5424(3) -0.3319(6) 0.7150(3) 0.0275(16) Uani 1 1 d . . . . .
C1 C 0.3739(3) 0.1254(6) 0.5353(3) 0.0135(14) Uani 1 1 d . . . . .
C2 C 0.4016(4) 0.0475(6) 0.4982(3) 0.0163(15) Uani 1 1 d . . . . .
C3 C 0.3779(3) 0.0205(6) 0.4487(3) 0.0168(15) Uani 1 1 d . . . . .
C4 C 0.4128(4) -0.0596(7) 0.4219(3) 0.0178(15) Uani 1 1 d . . . . .
H4 H 0.397008 -0.081921 0.388093 0.021 Uiso 1 1 calc R . . . .
C5 C 0.4710(4) -0.1061(6) 0.4455(3) 0.0189(16) Uani 1 1 d . . . . .
H5 H 0.494128 -0.161528 0.427366 0.023 Uiso 1 1 calc R . . . .
C6 C 0.4964(3) -0.0739(6) 0.4946(3) 0.0164(15) Uani 1 1 d . . . . .
H6 H 0.536747 -0.104359 0.509826 0.020 Uiso 1 1 calc R . . . .
C7 C 0.4606(3) 0.0041(6) 0.5205(3) 0.0137(14) Uani 1 1 d . . . . .
C8 C 0.4762(3) 0.0563(6) 0.5739(3) 0.0130(14) Uani 1 1 d . . . . .
C9 C 0.5319(3) 0.1453(7) 0.5758(3) 0.0158(15) Uani 1 1 d . . . . .
C10 C 0.5252(4) 0.2609(7) 0.5537(3) 0.0197(16) Uani 1 1 d . . . . .
H10 H 0.483788 0.286349 0.538644 0.024 Uiso 1 1 calc R . . . .
C11 C 0.5758(4) 0.3385(7) 0.5530(3) 0.0233(17) Uani 1 1 d . . . . .
H11 H 0.568418 0.417378 0.538850 0.028 Uiso 1 1 calc R . . . .
C12 C 0.6394(3) 0.3037(7) 0.5731(3) 0.0185(16) Uani 1 1 d . . . . .
C13 C 0.6465(3) 0.1875(7) 0.5949(3) 0.0167(15) Uani 1 1 d . . . . .
H13 H 0.687752 0.160200 0.609457 0.020 Uiso 1 1 calc R . . . .
C14 C 0.5937(3) 0.1125(6) 0.5952(3) 0.0147(15) Uani 1 1 d . . . . .
C15 C 0.5566(3) -0.0660(7) 0.6327(3) 0.0144(15) Uani 1 1 d . . . . .
C16 C 0.5738(3) -0.1617(7) 0.6663(3) 0.0166(15) Uani 1 1 d . . . . .
H16 H 0.617685 -0.175958 0.678712 0.020 Uiso 1 1 calc R . . . .
C17 C 0.5259(3) -0.2363(7) 0.6814(3) 0.0172(15) Uani 1 1 d . . . . .
C18 C 0.4619(3) -0.2146(7) 0.6622(3) 0.0166(15) Uani 1 1 d . . . . .
H18 H 0.429081 -0.265200 0.672029 0.020 Uiso 1 1 calc R . . . .
C19 C 0.4460(3) -0.1185(7) 0.6284(3) 0.0168(15) Uani 1 1 d . . . . .
H19 H 0.402088 -0.104932 0.615876 0.020 Uiso 1 1 calc R . . . .
C20 C 0.4925(3) -0.0418(6) 0.6125(3) 0.0141(14) Uani 1 1 d . . . . .
C21 C 0.4083(3) 0.1983(7) 0.6221(3) 0.0178(15) Uani 1 1 d . . . . .
H21A H 0.399327 0.282466 0.610032 0.021 Uiso 1 1 calc R . . . .
H21B H 0.449088 0.199466 0.645550 0.021 Uiso 1 1 calc R . . . .
C22 C 0.3541(4) 0.1561(7) 0.6512(3) 0.0195(16) Uani 1 1 d . . . . .
H22A H 0.363921 0.073800 0.665135 0.023 Uiso 1 1 calc R . . . .
H22B H 0.313405 0.151726 0.627773 0.023 Uiso 1 1 calc R . . . .
C23 C 0.3464(4) 0.2448(7) 0.6944(3) 0.0228(17) Uani 1 1 d . . . . .
H23A H 0.387349 0.249480 0.717512 0.027 Uiso 1 1 calc R . . . .
H23B H 0.336648 0.326981 0.680255 0.027 Uiso 1 1 calc R . . . .
C24 C 0.2929(4) 0.2051(9) 0.7243(3) 0.033(2) Uani 1 1 d . . . . .
H24A H 0.251661 0.207517 0.702208 0.049 Uiso 1 1 calc GR . . . .
H24B H 0.291381 0.260223 0.752962 0.049 Uiso 1 1 calc GR . . . .
H24C H 0.301229 0.122010 0.736782 0.049 Uiso 1 1 calc GR . . . .
C25 C 0.2859(4) 0.0529(8) 0.3807(3) 0.0272(18) Uani 1 1 d . . . . .
C26 C 0.2291(4) 0.1379(8) 0.3670(4) 0.031(2) Uani 1 1 d . . . . .
H26A H 0.195168 0.117768 0.387442 0.047 Uiso 1 1 calc GR . . . .
H26B H 0.212702 0.128496 0.331020 0.047 Uiso 1 1 calc GR . . . .
H26C H 0.242956 0.222187 0.373612 0.047 Uiso 1 1 calc GR . . . .
C27 C 0.6809(5) 0.5011(9) 0.5497(5) 0.061(4) Uani 1 1 d D . . . .
H27A H 0.652126 0.494727 0.517244 0.073 Uiso 0.717(17) 1 calc R . P A 1
H27B H 0.722907 0.531400 0.542029 0.073 Uiso 0.717(17) 1 calc R . P A 1
H27C H 0.714051 0.550128 0.570555 0.073 Uiso 0.283(17) 1 calc R . P A 2
H27D H 0.639565 0.527352 0.560172 0.073 Uiso 0.283(17) 1 calc R . P A 2
C28 C 0.6531(7) 0.5944(12) 0.5825(7) 0.060(5) Uani 0.717(17) 1 d D . P A 1
H28A H 0.610961 0.566762 0.589765 0.089 Uiso 0.717(17) 1 calc GR . P A 1
H28B H 0.648490 0.672444 0.564655 0.089 Uiso 0.717(17) 1 calc GR . P A 1
H28C H 0.681937 0.604202 0.614322 0.089 Uiso 0.717(17) 1 calc GR . P A 1
C29 C 0.7536(4) 0.3506(9) 0.5983(4) 0.038(2) Uani 1 1 d . . . . .
H29A H 0.786392 0.400941 0.584690 0.046 Uiso 1 1 calc R . . . .
H29B H 0.763126 0.264277 0.591825 0.046 Uiso 1 1 calc R . . . .
C30 C 0.7589(5) 0.3704(10) 0.6547(4) 0.048(3) Uani 1 1 d . . . . .
H30A H 0.750787 0.456256 0.661592 0.072 Uiso 1 1 calc GR . . . .
H30B H 0.802129 0.348273 0.670568 0.072 Uiso 1 1 calc GR . . . .
H30C H 0.727176 0.319685 0.668705 0.072 Uiso 1 1 calc GR . . . .
C31 C 0.6097(4) -0.3667(9) 0.7306(4) 0.040(2) Uani 1 1 d . . . . .
H31A H 0.634324 -0.354751 0.701746 0.048 Uiso 1 1 calc R . . . .
H31B H 0.611791 -0.454073 0.739614 0.048 Uiso 1 1 calc R . . . .
C32 C 0.6399(5) -0.2935(14) 0.7748(4) 0.061(4) Uani 1 1 d . . . . .
H32A H 0.642623 -0.208074 0.764692 0.091 Uiso 1 1 calc GR . . . .
H32B H 0.683164 -0.324551 0.786116 0.091 Uiso 1 1 calc GR . . . .
H32C H 0.613747 -0.299805 0.802434 0.091 Uiso 1 1 calc GR . . . .
C33 C 0.4950(4) -0.3947(8) 0.7407(4) 0.034(2) Uani 1 1 d . . . . .
H33A H 0.460504 -0.336539 0.745783 0.041 Uiso 1 1 calc R . . . .
H33B H 0.515782 -0.420549 0.774505 0.041 Uiso 1 1 calc R . . . .
C34 C 0.4650(5) -0.5044(9) 0.7133(5) 0.050(3) Uani 1 1 d . . . . .
H34A H 0.437176 -0.478298 0.682747 0.075 Uiso 1 1 calc GR . . . .
H34B H 0.439389 -0.548594 0.735515 0.075 Uiso 1 1 calc GR . . . .
H34C H 0.498771 -0.557799 0.703871 0.075 Uiso 1 1 calc GR . . . .
O1A O 0.3077(2) 0.3646(5) 0.4314(2) 0.0197(11) Uani 1 1 d . . . . .
O2A O 0.3127(3) 0.5476(6) 0.6111(3) 0.0415(17) Uani 1 1 d . . . . .
O3A O 0.5838(3) 0.5360(5) 0.3783(2) 0.0282(14) Uani 1 1 d . . . . .
N1A N 0.3950(3) 0.4258(6) 0.3932(2) 0.0166(13) Uani 1 1 d . . . . .
N2A N 0.3231(3) 0.4548(6) 0.5365(3) 0.0223(14) Uani 1 1 d . . . . .
H2A H 0.303942 0.402400 0.514475 0.027 Uiso 1 1 calc R . . . .
N3A N 0.6692(3) 0.1476(6) 0.4276(3) 0.0257(16) Uani 1 1 d . . . . .
N4A N 0.5119(3) 0.8740(6) 0.2757(3) 0.0285(16) Uani 1 1 d . . . . .
C1A C 0.3597(3) 0.4166(6) 0.4330(3) 0.0142(14) Uani 1 1 d . . . . .
C2A C 0.3959(3) 0.4850(6) 0.4757(3) 0.0133(14) Uani 1 1 d . . . . .
C3A C 0.3791(4) 0.5095(7) 0.5236(3) 0.0193(16) Uani 1 1 d . . . . .
C4A C 0.4200(4) 0.5830(7) 0.5566(3) 0.0193(16) Uani 1 1 d . . . . .
H4A H 0.409854 0.601906 0.589374 0.023 Uiso 1 1 calc R . . . .
C5A C 0.4770(4) 0.6287(7) 0.5401(3) 0.0229(17) Uani 1 1 d . . . . .
H5A H 0.504760 0.679050 0.562169 0.027 Uiso 1 1 calc R . . . .
C6A C 0.4933(3) 0.6014(6) 0.4919(3) 0.0166(15) Uani 1 1 d . . . . .
H6A H 0.531566 0.632093 0.481269 0.020 Uiso 1 1 calc R . . . .
C7A C 0.4519(3) 0.5285(6) 0.4608(3) 0.0125(14) Uani 1 1 d . . . . .
C8A C 0.4593(3) 0.4838(6) 0.4074(3) 0.0123(14) Uani 1 1 d . . . . .
C9A C 0.5121(3) 0.3905(6) 0.4088(3) 0.0139(14) Uani 1 1 d . . . . .
C10A C 0.5058(4) 0.2710(6) 0.4256(3) 0.0167(15) Uani 1 1 d . . . . .
H10A H 0.465320 0.244696 0.433686 0.020 Uiso 1 1 calc R . . . .
C11A C 0.5566(3) 0.1900(7) 0.4309(3) 0.0211(16) Uani 1 1 d . . . . .
H11A H 0.549983 0.108813 0.441277 0.025 Uiso 1 1 calc R . . . .
C12A C 0.6177(4) 0.2265(7) 0.4211(3) 0.0225(17) Uani 1 1 d . . . . .
C13A C 0.6243(4) 0.3451(7) 0.4030(3) 0.0212(16) Uani 1 1 d . . . . .
H13A H 0.664615 0.372247 0.394980 0.025 Uiso 1 1 calc R . . . .
C14A C 0.5712(3) 0.4235(6) 0.3969(3) 0.0166(15) Uani 1 1 d . . . . .
C15A C 0.5323(3) 0.6075(7) 0.3594(3) 0.0195(16) Uani 1 1 d . . . . .
C16A C 0.5469(4) 0.7020(7) 0.3287(3) 0.0217(17) Uani 1 1 d . . . . .
H16A H 0.589576 0.711849 0.321380 0.026 Uiso 1 1 calc R . . . .
C17A C 0.4986(4) 0.7840(7) 0.3082(3) 0.0210(17) Uani 1 1 d . . . . .
C18A C 0.4361(4) 0.7652(7) 0.3218(3) 0.0198(16) Uani 1 1 d . . . . .
H18A H 0.402176 0.818847 0.309356 0.024 Uiso 1 1 calc R . . . .
C19A C 0.4245(3) 0.6703(7) 0.3527(3) 0.0142(14) Uani 1 1 d . . . . .
H19A H 0.382447 0.661487 0.361615 0.017 Uiso 1 1 calc R . . . .
C20A C 0.4707(3) 0.5870(6) 0.3717(3) 0.0132(14) Uani 1 1 d . . . . .
C21A C 0.3757(4) 0.3636(7) 0.3456(3) 0.0212(16) Uani 1 1 d . . . . .
H21C H 0.359902 0.281271 0.352581 0.025 Uiso 1 1 calc R . . . .
H21D H 0.413624 0.353936 0.327522 0.025 Uiso 1 1 calc R . . . .
C22A C 0.3235(4) 0.4316(8) 0.3117(3) 0.0274(19) Uani 1 1 d . . . . .
H22C H 0.340128 0.512553 0.303671 0.033 Uiso 1 1 calc R . . . .
H22D H 0.286536 0.444659 0.330541 0.033 Uiso 1 1 calc R . . . .
C23A C 0.2998(4) 0.3659(9) 0.2620(3) 0.030(2) Uani 1 1 d . . . . .
H23C H 0.336947 0.346069 0.244302 0.037 Uiso 1 1 calc R . . . .
H23D H 0.278895 0.288502 0.269619 0.037 Uiso 1 1 calc R . . . .
C24A C 0.2521(5) 0.4436(10) 0.2275(3) 0.041(2) Uani 1 1 d . . . . .
H24D H 0.273803 0.516779 0.217434 0.061 Uiso 1 1 calc GR . . . .
H24E H 0.216444 0.467106 0.245678 0.061 Uiso 1 1 calc GR . . . .
H24F H 0.235542 0.396692 0.197320 0.061 Uiso 1 1 calc GR . . . .
C25A C 0.2952(4) 0.4734(8) 0.5789(3) 0.0255(18) Uani 1 1 d . . . . .
C26A C 0.2374(4) 0.3916(8) 0.5816(3) 0.030(2) Uani 1 1 d . . . . .
H26D H 0.223173 0.399414 0.615004 0.046 Uiso 1 1 calc GR . . . .
H26E H 0.249362 0.306883 0.576186 0.046 Uiso 1 1 calc GR . . . .
H26F H 0.202470 0.415642 0.555404 0.046 Uiso 1 1 calc GR . . . .
C27A C 0.6643(4) 0.0309(7) 0.4518(3) 0.0262(18) Uani 1 1 d . . . . .
H27E H 0.633910 0.037532 0.477053 0.031 Uiso 1 1 calc R . . . .
H27F H 0.706780 0.008042 0.469947 0.031 Uiso 1 1 calc R . . . .
C28A C 0.6410(5) -0.0693(8) 0.4133(5) 0.052(3) Uani 1 1 d . . . . .
H28G H 0.601802 -0.042120 0.392180 0.078 Uiso 1 1 calc GR . . . .
H28H H 0.631912 -0.143535 0.431433 0.078 Uiso 1 1 calc GR . . . .
H28I H 0.674388 -0.085879 0.391903 0.078 Uiso 1 1 calc GR . . . .
C29A C 0.7327(4) 0.1838(8) 0.4182(4) 0.033(2) Uani 1 1 d . . . . .
H29C H 0.728751 0.238622 0.388530 0.040 Uiso 1 1 calc R . . . .
H29D H 0.756651 0.110606 0.409866 0.040 Uiso 1 1 calc R . . . .
C30A C 0.7708(5) 0.2481(9) 0.4631(4) 0.046(3) Uani 1 1 d . . . . .
H30D H 0.815150 0.259710 0.456614 0.069 Uiso 1 1 calc GR . . . .
H30E H 0.770388 0.198573 0.493664 0.069 Uiso 1 1 calc GR . . . .
H30F H 0.751234 0.327437 0.468058 0.069 Uiso 1 1 calc GR . . . .
C31A C 0.4659(4) 0.9741(8) 0.2611(3) 0.0292(19) Uani 1 1 d . . . . .
H31C H 0.421574 0.942004 0.257995 0.035 Uiso 1 1 calc R . . . .
H31D H 0.473132 1.006644 0.227708 0.035 Uiso 1 1 calc R . . . .
C32A C 0.4734(7) 1.0756(10) 0.2997(5) 0.061(4) Uani 1 1 d . . . . .
H32D H 0.442553 1.140383 0.288876 0.092 Uiso 1 1 calc GR . . . .
H32E H 0.517131 1.108148 0.302498 0.092 Uiso 1 1 calc GR . . . .
H32F H 0.465311 1.043956 0.332585 0.092 Uiso 1 1 calc GR . . . .
C33A C 0.5754(4) 0.8857(9) 0.2620(4) 0.037(2) Uani 1 1 d . . . . .
H33C H 0.607095 0.875965 0.292710 0.045 Uiso 1 1 calc R . . . .
H33D H 0.580550 0.968445 0.248467 0.045 Uiso 1 1 calc R . . . .
C34A C 0.5894(5) 0.7920(11) 0.2224(4) 0.047(3) Uani 1 1 d . . . . .
H34D H 0.554998 0.793747 0.193765 0.070 Uiso 1 1 calc GR . . . .
H34E H 0.591905 0.710638 0.237631 0.070 Uiso 1 1 calc GR . . . .
H34F H 0.630421 0.811532 0.210592 0.070 Uiso 1 1 calc GR . . . .
C28B C 0.6791(19) 0.556(3) 0.4973(8) 0.060(5) Uani 0.283(17) 1 d D . P A 2
H28D H 0.722012 0.551827 0.486846 0.089 Uiso 0.283(17) 1 calc GR . P A 2
H28E H 0.665522 0.641291 0.498076 0.089 Uiso 0.283(17) 1 calc GR . P A 2
H28F H 0.648675 0.510687 0.473272 0.089 Uiso 0.283(17) 1 calc GR . 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
O1 C1 1.219(9) . ?
O2 C25 1.216(11) . ?
O3 C14 1.405(8) . ?
O3 C15 1.368(8) . ?
N1 C1 1.368(9) . ?
N1 C8 1.465(9) . ?
N1 C21 1.459(9) . ?
N2 H2 0.8800 . ?
N2 C3 1.412(9) . ?
N2 C25 1.350(10) . ?
N3 C12 1.368(10) . ?
N3 C27 1.442(11) . ?
N3 C29 1.471(11) . ?
N4 C17 1.396(9) . ?
N4 C31 1.471(11) . ?
N4 C33 1.455(10) . ?
C1 C2 1.485(10) . ?
C2 C3 1.379(10) . ?
C2 C7 1.386(10) . ?
C3 C4 1.402(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.396(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.385(10) . ?
C7 C8 1.528(10) . ?
C8 C9 1.522(10) . ?
C8 C20 1.499(10) . ?
C9 C10 1.399(10) . ?
C9 C14 1.380(9) . ?
C10 H10 0.9500 . ?
C10 C11 1.366(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.423(11) . ?
C12 C13 1.403(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(10) . ?
C15 C16 1.397(10) . ?
C15 C20 1.408(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.399(10) . ?
C17 C18 1.394(10) . ?
C18 H18 0.9500 . ?
C18 C19 1.399(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.398(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.532(10) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.535(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.526(11) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.522(12) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 H27C 0.9900 . ?
C27 H27D 0.9900 . ?
C27 C28 1.514(11) . ?
C27 C28B 1.517(12) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.509(15) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.496(16) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.503(14) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O1A C1A 1.228(9) . ?
O2A C25A 1.205(10) . ?
O3A C14A 1.372(9) . ?
O3A C15A 1.378(9) . ?
N1A C1A 1.377(9) . ?
N1A C8A 1.495(9) . ?
N1A C21A 1.452(9) . ?
N2A H2A 0.8800 . ?
N2A C3A 1.404(10) . ?
N2A C25A 1.360(10) . ?
N3A C12A 1.378(10) . ?
N3A C27A 1.447(10) . ?
N3A C29A 1.445(11) . ?
N4A C17A 1.369(10) . ?
N4A C31A 1.482(10) . ?
N4A C33A 1.434(11) . ?
C1A C2A 1.487(10) . ?
C2A C3A 1.395(10) . ?
C2A C7A 1.378(9) . ?
C3A C4A 1.400(11) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.422(11) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.404(11) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.377(10) . ?
C7A C8A 1.532(10) . ?
C8A C9A 1.508(10) . ?
C8A C20A 1.522(9) . ?
C9A C10A 1.401(10) . ?
C9A C14A 1.371(10) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.381(10) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.404(11) . ?
C12A C13A 1.403(11) . ?
C13A H13A 0.9500 . ?
C13A C14A 1.401(10) . ?
C15A C16A 1.382(10) . ?
C15A C20A 1.394(10) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.410(11) . ?
C17A C18A 1.424(11) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.372(10) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.381(10) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C21A C22A 1.522(11) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C22A C23A 1.531(11) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?
C23A C24A 1.527(13) . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25A C26A 1.520(12) . ?
C26A H26D 0.9800 . ?
C26A H26E 0.9800 . ?
C26A H26F 0.9800 . ?
C27A H27E 0.9900 . ?
C27A H27F 0.9900 . ?
C27A C28A 1.539(14) . ?
C28A H28G 0.9800 . ?
C28A H28H 0.9800 . ?
C28A H28I 0.9800 . ?
C29A H29C 0.9900 . ?
C29A H29D 0.9900 . ?
C29A C30A 1.522(15) . ?
C30A H30D 0.9800 . ?
C30A H30E 0.9800 . ?
C30A H30F 0.9800 . ?
C31A H31C 0.9900 . ?
C31A H31D 0.9900 . ?
C31A C32A 1.510(14) . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?
C33A H33C 0.9900 . ?
C33A H33D 0.9900 . ?
C33A C34A 1.531(15) . ?
C34A H34D 0.9800 . ?
C34A H34E 0.9800 . ?
C34A H34F 0.9800 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 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
C15 O3 C14 118.1(5) . . ?
C1 N1 C8 114.2(6) . . ?
C1 N1 C21 121.3(6) . . ?
C21 N1 C8 123.1(6) . . ?
C3 N2 H2 115.6 . . ?
C25 N2 H2 115.6 . . ?
C25 N2 C3 128.7(7) . . ?
C12 N3 C27 121.4(7) . . ?
C12 N3 C29 120.1(7) . . ?
C27 N3 C29 117.9(7) . . ?
C17 N4 C31 121.6(7) . . ?
C17 N4 C33 122.2(7) . . ?
C33 N4 C31 116.0(7) . . ?
O1 C1 N1 127.0(7) . . ?
O1 C1 C2 127.0(7) . . ?
N1 C1 C2 106.1(6) . . ?
C3 C2 C1 129.7(7) . . ?
C3 C2 C7 121.7(7) . . ?
C7 C2 C1 108.6(6) . . ?
C2 C3 N2 119.4(7) . . ?
C2 C3 C4 118.4(6) . . ?
C4 C3 N2 122.2(7) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(6) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 118.9 . . ?
C6 C5 C4 122.2(6) . . ?
C6 C5 H5 118.9 . . ?
C5 C6 H6 121.3 . . ?
C7 C6 C5 117.4(6) . . ?
C7 C6 H6 121.3 . . ?
C2 C7 C8 109.8(6) . . ?
C6 C7 C2 120.9(6) . . ?
C6 C7 C8 129.3(6) . . ?
N1 C8 C7 100.8(5) . . ?
N1 C8 C9 110.5(5) . . ?
N1 C8 C20 114.0(6) . . ?
C9 C8 C7 109.9(6) . . ?
C20 C8 C7 111.8(6) . . ?
C20 C8 C9 109.6(6) . . ?
C10 C9 C8 122.4(6) . . ?
C14 C9 C8 121.7(6) . . ?
C14 C9 C10 115.6(6) . . ?
C9 C10 H10 118.7 . . ?
C11 C10 C9 122.6(7) . . ?
C11 C10 H10 118.7 . . ?
C10 C11 H11 119.3 . . ?
C10 C11 C12 121.4(7) . . ?
C12 C11 H11 119.3 . . ?
N3 C12 C11 121.0(7) . . ?
N3 C12 C13 122.7(7) . . ?
C13 C12 C11 116.3(6) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.3(6) . . ?
C14 C13 H13 119.9 . . ?
C9 C14 O3 121.6(6) . . ?
C9 C14 C13 123.9(6) . . ?
C13 C14 O3 114.4(6) . . ?
O3 C15 C16 114.7(6) . . ?
O3 C15 C20 122.7(6) . . ?
C16 C15 C20 122.6(6) . . ?
C15 C16 H16 120.3 . . ?
C15 C16 C17 119.4(7) . . ?
C17 C16 H16 120.3 . . ?
N4 C17 C16 120.0(6) . . ?
C18 C17 N4 120.6(7) . . ?
C18 C17 C16 119.4(7) . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.1(7) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 118.9 . . ?
C20 C19 C18 122.3(7) . . ?
C20 C19 H19 118.9 . . ?
C15 C20 C8 121.1(6) . . ?
C19 C20 C8 122.5(6) . . ?
C19 C20 C15 116.3(6) . . ?
N1 C21 H21A 108.9 . . ?
N1 C21 H21B 108.9 . . ?
N1 C21 C22 113.3(6) . . ?
H21A C21 H21B 107.7 . . ?
C22 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C21 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C21 C22 C23 110.4(6) . . ?
H22A C22 H22B 108.1 . . ?
C23 C22 H22A 109.6 . . ?
C23 C22 H22B 109.6 . . ?
C22 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 C22 111.7(7) . . ?
C24 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C25 N2 124.8(8) . . ?
O2 C25 C26 120.9(8) . . ?
N2 C25 C26 114.3(8) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C27 H27A 108.4 . . ?
N3 C27 H27B 108.4 . . ?
N3 C27 H27C 103.2 . . ?
N3 C27 H27D 103.2 . . ?
N3 C27 C28 115.5(11) . . ?
N3 C27 C28B 135.8(18) . . ?
H27A C27 H27B 107.5 . . ?
H27C C27 H27D 105.2 . . ?
C28 C27 H27A 108.4 . . ?
C28 C27 H27B 108.4 . . ?
C28B C27 H27C 103.2 . . ?
C28B C27 H27D 103.2 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 H29A 108.9 . . ?
N3 C29 H29B 108.9 . . ?
N3 C29 C30 113.4(8) . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N4 C31 H31A 109.3 . . ?
N4 C31 H31B 109.3 . . ?
N4 C31 C32 111.8(8) . . ?
H31A C31 H31B 107.9 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N4 C33 H33A 108.5 . . ?
N4 C33 H33B 108.5 . . ?
N4 C33 C34 115.0(8) . . ?
H33A C33 H33B 107.5 . . ?
C34 C33 H33A 108.5 . . ?
C34 C33 H33B 108.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C14A O3A C15A 117.8(6) . . ?
C1A N1A C8A 113.5(6) . . ?
C1A N1A C21A 121.5(6) . . ?
C21A N1A C8A 124.0(6) . . ?
C3A N2A H2A 116.3 . . ?
C25A N2A H2A 116.3 . . ?
C25A N2A C3A 127.5(7) . . ?
C12A N3A C27A 120.8(7) . . ?
C12A N3A C29A 122.2(7) . . ?
C29A N3A C27A 116.3(6) . . ?
C17A N4A C31A 121.4(7) . . ?
C17A N4A C33A 120.1(7) . . ?
C33A N4A C31A 117.6(7) . . ?
O1A C1A N1A 125.2(7) . . ?
O1A C1A C2A 128.5(7) . . ?
N1A C1A C2A 106.2(6) . . ?
C3A C2A C1A 129.3(7) . . ?
C7A C2A C1A 108.8(6) . . ?
C7A C2A C3A 121.8(7) . . ?
C2A C3A N2A 117.6(7) . . ?
C2A C3A C4A 118.5(7) . . ?
C4A C3A N2A 123.9(7) . . ?
C3A C4A H4A 120.6 . . ?
C3A C4A C5A 118.7(7) . . ?
C5A C4A H4A 120.6 . . ?
C4A C5A H5A 119.1 . . ?
C6A C5A C4A 121.8(7) . . ?
C6A C5A H5A 119.1 . . ?
C5A C6A H6A 121.2 . . ?
C7A C6A C5A 117.6(7) . . ?
C7A C6A H6A 121.2 . . ?
C2A C7A C8A 110.7(6) . . ?
C6A C7A C2A 121.5(7) . . ?
C6A C7A C8A 127.8(6) . . ?
N1A C8A C7A 99.9(5) . . ?
N1A C8A C9A 110.7(5) . . ?
N1A C8A C20A 111.9(6) . . ?
C9A C8A C7A 111.2(6) . . ?
C9A C8A C20A 110.1(6) . . ?
C20A C8A C7A 112.8(6) . . ?
C10A C9A C8A 123.0(6) . . ?
C14A C9A C8A 120.1(6) . . ?
C14A C9A C10A 116.7(6) . . ?
C9A C10A H10A 118.9 . . ?
C11A C10A C9A 122.2(7) . . ?
C11A C10A H10A 118.9 . . ?
C10A C11A H11A 119.6 . . ?
C10A C11A C12A 120.7(7) . . ?
C12A C11A H11A 119.6 . . ?
N3A C12A C11A 121.3(7) . . ?
N3A C12A C13A 121.0(7) . . ?
C13A C12A C11A 117.6(7) . . ?
C12A C13A H13A 120.1 . . ?
C14A C13A C12A 119.9(7) . . ?
C14A C13A H13A 120.1 . . ?
O3A C14A C13A 114.0(7) . . ?
C9A C14A O3A 123.2(6) . . ?
C9A C14A C13A 122.8(7) . . ?
O3A C15A C16A 114.8(7) . . ?
O3A C15A C20A 122.0(6) . . ?
C16A C15A C20A 123.2(7) . . ?
C15A C16A H16A 119.8 . . ?
C15A C16A C17A 120.3(7) . . ?
C17A C16A H16A 119.8 . . ?
N4A C17A C16A 120.7(7) . . ?
N4A C17A C18A 122.7(7) . . ?
C16A C17A C18A 116.6(7) . . ?
C17A C18A H18A 119.7 . . ?
C19A C18A C17A 120.5(7) . . ?
C19A C18A H18A 119.7 . . ?
C18A C19A H19A 118.3 . . ?
C18A C19A C20A 123.4(7) . . ?
C20A C19A H19A 118.3 . . ?
C15A C20A C8A 119.8(6) . . ?
C19A C20A C8A 124.1(7) . . ?
C19A C20A C15A 115.9(6) . . ?
N1A C21A H21C 109.1 . . ?
N1A C21A H21D 109.1 . . ?
N1A C21A C22A 112.5(6) . . ?
H21C C21A H21D 107.8 . . ?
C22A C21A H21C 109.1 . . ?
C22A C21A H21D 109.1 . . ?
C21A C22A H22C 108.8 . . ?
C21A C22A H22D 108.8 . . ?
C21A C22A C23A 114.0(7) . . ?
H22C C22A H22D 107.7 . . ?
C23A C22A H22C 108.8 . . ?
C23A C22A H22D 108.8 . . ?
C22A C23A H23C 109.3 . . ?
C22A C23A H23D 109.3 . . ?
H23C C23A H23D 108.0 . . ?
C24A C23A C22A 111.6(8) . . ?
C24A C23A H23C 109.3 . . ?
C24A C23A H23D 109.3 . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
O2A C25A N2A 124.7(8) . . ?
O2A C25A C26A 122.5(8) . . ?
N2A C25A C26A 112.8(7) . . ?
C25A C26A H26D 109.5 . . ?
C25A C26A H26E 109.5 . . ?
C25A C26A H26F 109.5 . . ?
H26D C26A H26E 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
N3A C27A H27E 109.2 . . ?
N3A C27A H27F 109.2 . . ?
N3A C27A C28A 111.9(8) . . ?
H27E C27A H27F 107.9 . . ?
C28A C27A H27E 109.2 . . ?
C28A C27A H27F 109.2 . . ?
C27A C28A H28G 109.5 . . ?
C27A C28A H28H 109.5 . . ?
C27A C28A H28I 109.5 . . ?
H28G C28A H28H 109.5 . . ?
H28G C28A H28I 109.5 . . ?
H28H C28A H28I 109.5 . . ?
N3A C29A H29C 109.0 . . ?
N3A C29A H29D 109.0 . . ?
N3A C29A C30A 113.1(8) . . ?
H29C C29A H29D 107.8 . . ?
C30A C29A H29C 109.0 . . ?
C30A C29A H29D 109.0 . . ?
C29A C30A H30D 109.5 . . ?
C29A C30A H30E 109.5 . . ?
C29A C30A H30F 109.5 . . ?
H30D C30A H30E 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
N4A C31A H31C 109.3 . . ?
N4A C31A H31D 109.3 . . ?
N4A C31A C32A 111.5(8) . . ?
H31C C31A H31D 108.0 . . ?
C32A C31A H31C 109.3 . . ?
C32A C31A H31D 109.3 . . ?
C31A C32A H32D 109.5 . . ?
C31A C32A H32E 109.5 . . ?
C31A C32A H32F 109.5 . . ?
H32D C32A H32E 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
N4A C33A H33C 109.0 . . ?
N4A C33A H33D 109.0 . . ?
N4A C33A C34A 112.7(8) . . ?
H33C C33A H33D 107.8 . . ?
C34A C33A H33C 109.0 . . ?
C34A C33A H33D 109.0 . . ?
C33A C34A H34D 109.5 . . ?
C33A C34A H34E 109.5 . . ?
C33A C34A H34F 109.5 . . ?
H34D C34A H34E 109.5 . . ?
H34D C34A H34F 109.5 . . ?
H34E C34A H34F 109.5 . . ?
C27 C28B H28D 109.5 . . ?
C27 C28B H28E 109.5 . . ?
C27 C28B H28F 109.5 . . ?
H28D C28B H28E 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 O1 0.88 2.28 2.951(9) 133.1 . yes
N2 H2 O1A 0.88 2.60 3.200(8) 126.0 . yes
C4 H4 O2 0.95 2.25 2.863(10) 121.6 . yes
N2A H2A O1 0.88 2.49 3.023(8) 119.3 . yes
N2A H2A O1A 0.88 2.26 2.947(9) 134.3 . yes
C4A H4A O2A 0.95 2.27 2.867(10) 119.8 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 0.8(12) . . . . ?
O1 C1 C2 C7 178.6(7) . . . . ?
O3 C15 C16 C17 -179.8(6) . . . . ?
O3 C15 C20 C8 3.1(10) . . . . ?
O3 C15 C20 C19 179.5(6) . . . . ?
N1 C1 C2 C3 179.7(7) . . . . ?
N1 C1 C2 C7 -2.5(8) . . . . ?
N1 C8 C9 C10 -37.3(10) . . . . ?
N1 C8 C9 C14 149.1(7) . . . . ?
N1 C8 C20 C15 -144.4(6) . . . . ?
N1 C8 C20 C19 39.4(9) . . . . ?
N1 C21 C22 C23 -177.3(6) . . . . ?
N2 C3 C4 C5 177.4(7) . . . . ?
N3 C12 C13 C14 -179.4(8) . . . . ?
N4 C17 C18 C19 180.0(7) . . . . ?
C1 N1 C8 C7 -7.5(7) . . . . ?
C1 N1 C8 C9 108.7(7) . . . . ?
C1 N1 C8 C20 -127.4(6) . . . . ?
C1 N1 C21 C22 74.5(8) . . . . ?
C1 C2 C3 N2 2.6(11) . . . . ?
C1 C2 C3 C4 -178.0(7) . . . . ?
C1 C2 C7 C6 178.3(6) . . . . ?
C1 C2 C7 C8 -2.2(8) . . . . ?
C2 C3 C4 C5 -2.0(11) . . . . ?
C2 C7 C8 N1 5.6(7) . . . . ?
C2 C7 C8 C9 -111.0(7) . . . . ?
C2 C7 C8 C20 127.0(6) . . . . ?
C3 N2 C25 O2 4.0(14) . . . . ?
C3 N2 C25 C26 -174.0(7) . . . . ?
C3 C2 C7 C6 -3.7(11) . . . . ?
C3 C2 C7 C8 175.8(6) . . . . ?
C3 C4 C5 C6 -1.2(11) . . . . ?
C4 C5 C6 C7 2.0(11) . . . . ?
C5 C6 C7 C2 0.4(10) . . . . ?
C5 C6 C7 C8 -179.0(7) . . . . ?
C6 C7 C8 N1 -175.0(7) . . . . ?
C6 C7 C8 C9 68.4(9) . . . . ?
C6 C7 C8 C20 -53.5(10) . . . . ?
C7 C2 C3 N2 -175.0(7) . . . . ?
C7 C2 C3 C4 4.4(11) . . . . ?
C7 C8 C9 C10 73.1(9) . . . . ?
C7 C8 C9 C14 -100.5(8) . . . . ?
C7 C8 C20 C15 102.2(7) . . . . ?
C7 C8 C20 C19 -74.1(8) . . . . ?
C8 N1 C1 O1 -174.6(7) . . . . ?
C8 N1 C1 C2 6.5(8) . . . . ?
C8 N1 C21 C22 -120.3(7) . . . . ?
C8 C9 C10 C11 -176.4(8) . . . . ?
C8 C9 C14 O3 -8.5(11) . . . . ?
C8 C9 C14 C13 175.7(7) . . . . ?
C9 C8 C20 C15 -20.0(9) . . . . ?
C9 C8 C20 C19 163.8(6) . . . . ?
C9 C10 C11 C12 2.7(13) . . . . ?
C10 C9 C14 O3 177.5(7) . . . . ?
C10 C9 C14 C13 1.7(11) . . . . ?
C10 C11 C12 N3 178.6(8) . . . . ?
C10 C11 C12 C13 -2.0(12) . . . . ?
C11 C12 C13 C14 1.3(11) . . . . ?
C12 N3 C27 C28 76.0(13) . . . . ?
C12 N3 C27 C28B -88(3) . . . . ?
C12 N3 C29 C30 -76.1(11) . . . . ?
C12 C13 C14 O3 -177.3(6) . . . . ?
C12 C13 C14 C9 -1.2(12) . . . . ?
C14 O3 C15 C16 -167.3(6) . . . . ?
C14 O3 C15 C20 13.8(10) . . . . ?
C14 C9 C10 C11 -2.4(12) . . . . ?
C15 O3 C14 C9 -11.0(10) . . . . ?
C15 O3 C14 C13 165.2(7) . . . . ?
C15 C16 C17 N4 -179.7(7) . . . . ?
C15 C16 C17 C18 0.7(11) . . . . ?
C16 C15 C20 C8 -175.8(7) . . . . ?
C16 C15 C20 C19 0.7(10) . . . . ?
C16 C17 C18 C19 -0.5(11) . . . . ?
C17 N4 C31 C32 86.4(10) . . . . ?
C17 N4 C33 C34 91.1(10) . . . . ?
C17 C18 C19 C20 0.3(11) . . . . ?
C18 C19 C20 C8 176.0(7) . . . . ?
C18 C19 C20 C15 -0.4(10) . . . . ?
C20 C8 C9 C10 -163.7(7) . . . . ?
C20 C8 C9 C14 22.7(10) . . . . ?
C20 C15 C16 C17 -0.9(11) . . . . ?
C21 N1 C1 O1 -8.1(11) . . . . ?
C21 N1 C1 C2 173.0(6) . . . . ?
C21 N1 C8 C7 -173.7(6) . . . . ?
C21 N1 C8 C9 -57.5(8) . . . . ?
C21 N1 C8 C20 66.5(8) . . . . ?
C21 C22 C23 C24 -179.8(7) . . . . ?
C25 N2 C3 C2 -173.6(8) . . . . ?
C25 N2 C3 C4 7.0(12) . . . . ?
C27 N3 C12 C11 0.9(13) . . . . ?
C27 N3 C12 C13 -178.4(9) . . . . ?
C27 N3 C29 C30 94.7(11) . . . . ?
C29 N3 C12 C11 171.4(8) . . . . ?
C29 N3 C12 C13 -7.9(12) . . . . ?
C29 N3 C27 C28 -94.6(11) . . . . ?
C29 N3 C27 C28B 101(2) . . . . ?
C31 N4 C17 C16 -7.7(12) . . . . ?
C31 N4 C17 C18 171.8(8) . . . . ?
C31 N4 C33 C34 -94.8(10) . . . . ?
C33 N4 C17 C16 166.0(8) . . . . ?
C33 N4 C17 C18 -14.4(12) . . . . ?
C33 N4 C31 C32 -87.8(10) . . . . ?
O1A C1A C2A C3A -2.0(12) . . . . ?
O1A C1A C2A C7A -179.9(7) . . . . ?
O3A C15A C16A C17A -178.1(7) . . . . ?
O3A C15A C20A C8A 0.7(11) . . . . ?
O3A C15A C20A C19A 175.9(7) . . . . ?
N1A C1A C2A C3A 175.9(7) . . . . ?
N1A C1A C2A C7A -2.0(7) . . . . ?
N1A C8A C9A C10A -36.4(9) . . . . ?
N1A C8A C9A C14A 148.8(6) . . . . ?
N1A C8A C20A C15A -144.9(7) . . . . ?
N1A C8A C20A C19A 40.3(9) . . . . ?
N1A C21A C22A C23A -177.5(7) . . . . ?
N2A C3A C4A C5A 177.1(7) . . . . ?
N3A C12A C13A C14A -179.9(8) . . . . ?
N4A C17A C18A C19A 177.0(8) . . . . ?
C1A N1A C8A C7A -9.5(7) . . . . ?
C1A N1A C8A C9A 107.8(7) . . . . ?
C1A N1A C8A C20A -129.0(6) . . . . ?
C1A N1A C21A C22A 80.7(8) . . . . ?
C1A C2A C3A N2A 6.2(11) . . . . ?
C1A C2A C3A C4A -176.1(7) . . . . ?
C1A C2A C7A C6A 176.3(6) . . . . ?
C1A C2A C7A C8A -4.1(7) . . . . ?
C2A C3A C4A C5A -0.5(11) . . . . ?
C2A C7A C8A N1A 7.9(7) . . . . ?
C2A C7A C8A C9A -109.0(6) . . . . ?
C2A C7A C8A C20A 126.8(6) . . . . ?
C3A N2A C25A O2A 5.2(13) . . . . ?
C3A N2A C25A C26A -176.0(7) . . . . ?
C3A C2A C7A C6A -1.8(10) . . . . ?
C3A C2A C7A C8A 177.8(6) . . . . ?
C3A C4A C5A C6A -0.4(11) . . . . ?
C4A C5A C6A C7A 0.2(11) . . . . ?
C5A C6A C7A C2A 0.9(10) . . . . ?
C5A C6A C7A C8A -178.7(7) . . . . ?
C6A C7A C8A N1A -172.5(7) . . . . ?
C6A C7A C8A C9A 70.7(9) . . . . ?
C6A C7A C8A C20A -53.6(9) . . . . ?
C7A C2A C3A N2A -176.1(6) . . . . ?
C7A C2A C3A C4A 1.6(10) . . . . ?
C7A C8A C9A C10A 73.7(8) . . . . ?
C7A C8A C9A C14A -101.1(7) . . . . ?
C7A C8A C20A C15A 103.5(8) . . . . ?
C7A C8A C20A C19A -71.3(9) . . . . ?
C8A N1A C1A O1A -174.4(6) . . . . ?
C8A N1A C1A C2A 7.6(8) . . . . ?
C8A N1A C21A C22A -111.6(8) . . . . ?
C8A C9A C10A C11A -174.0(7) . . . . ?
C8A C9A C14A O3A -7.3(11) . . . . ?
C8A C9A C14A C13A 172.4(7) . . . . ?
C9A C8A C20A C15A -21.4(9) . . . . ?
C9A C8A C20A C19A 163.8(6) . . . . ?
C9A C10A C11A C12A 2.3(12) . . . . ?
C10A C9A C14A O3A 177.6(7) . . . . ?
C10A C9A C14A C13A -2.7(11) . . . . ?
C10A C11A C12A N3A 178.2(8) . . . . ?
C10A C11A C12A C13A -3.7(12) . . . . ?
C11A C12A C13A C14A 2.0(12) . . . . ?
C12A N3A C27A C28A 90.2(10) . . . . ?
C12A N3A C29A C30A 84.0(10) . . . . ?
C12A C13A C14A O3A -179.0(7) . . . . ?
C12A C13A C14A C9A 1.2(12) . . . . ?
C14A O3A C15A C16A -162.5(7) . . . . ?
C14A O3A C15A C20A 19.2(11) . . . . ?
C14A C9A C10A C11A 0.9(11) . . . . ?
C15A O3A C14A C9A -16.0(11) . . . . ?
C15A O3A C14A C13A 164.3(7) . . . . ?
C15A C16A C17A N4A -176.5(8) . . . . ?
C15A C16A C17A C18A 1.4(12) . . . . ?
C16A C15A C20A C8A -177.5(7) . . . . ?
C16A C15A C20A C19A -2.3(11) . . . . ?
C16A C17A C18A C19A -0.9(11) . . . . ?
C17A N4A C31A C32A 84.4(10) . . . . ?
C17A N4A C33A C34A 77.8(10) . . . . ?
C17A C18A C19A C20A -1.3(11) . . . . ?
C18A C19A C20A C8A 177.8(7) . . . . ?
C18A C19A C20A C15A 2.8(11) . . . . ?
C20A C8A C9A C10A -160.6(7) . . . . ?
C20A C8A C9A C14A 24.7(9) . . . . ?
C20A C15A C16A C17A 0.2(13) . . . . ?
C21A N1A C1A O1A -5.6(11) . . . . ?
C21A N1A C1A C2A 176.5(6) . . . . ?
C21A N1A C8A C7A -178.0(6) . . . . ?
C21A N1A C8A C9A -60.7(8) . . . . ?
C21A N1A C8A C20A 62.4(9) . . . . ?
C21A C22A C23A C24A -174.6(8) . . . . ?
C25A N2A C3A C2A -174.2(7) . . . . ?
C25A N2A C3A C4A 8.2(12) . . . . ?
C27A N3A C12A C11A -9.4(12) . . . . ?
C27A N3A C12A C13A 172.6(8) . . . . ?
C27A N3A C29A C30A -86.4(9) . . . . ?
C29A N3A C12A C11A -179.3(8) . . . . ?
C29A N3A C12A C13A 2.6(13) . . . . ?
C29A N3A C27A C28A -99.3(9) . . . . ?
C31A N4A C17A C16A -168.7(8) . . . . ?
C31A N4A C17A C18A 13.5(12) . . . . ?
C31A N4A C33A C34A -113.0(9) . . . . ?
C33A N4A C17A C16A 0.0(12) . . . . ?
C33A N4A C17A C18A -177.8(8) . . . . ?
C33A N4A C31A C32A -84.6(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.733(3)
2 0.267(3)

####################################################################### 
# 
# 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_p8_tw
_database_code_depnum_ccdc_archive 'CCDC 1901372'
loop_
_audit_author_name
_audit_author_address
'Qingkai QI'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-04 downloaded from the CCDC.
;
_audit_creation_date             2019-03-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H46 N4 O4 S'
_chemical_formula_sum            'C39 H46 N4 O4 S'
_chemical_formula_weight         666.86
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.7633(8)
_cell_length_b                   12.4781(9)
_cell_length_c                   13.0623(9)
_cell_angle_alpha                106.839(6)
_cell_angle_beta                 100.035(6)
_cell_angle_gamma                93.786(6)
_cell_volume                     1793.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4616
_cell_measurement_temperature    126(2)
_cell_measurement_theta_max      29.2910
_cell_measurement_theta_min      3.8780
_shelx_estimated_absorpt_T_max   0.987
_shelx_estimated_absorpt_T_min   0.984
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8324
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.306
_diffrn_reflns_theta_min         2.944
_diffrn_ambient_temperature      126.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6225
_reflns_number_total             8324
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8324
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0800
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0737P)²+3.1830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2216
_refine_ls_wR_factor_ref         0.2367
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.725(3)
 0.275(3)
2. 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
3. Restrained distances
 N4-H4
 0.88 with sigma of 0.01
 N2-C23A \\sim N2-C23
 with sigma of 0.02
 C24-C23 \\sim C24A-C23A
 with sigma of 0.02
4. Others
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23A)=Sof(H23C)=Sof(H23D)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C23A(H23C,H23D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C16(H16), C18(H18),
 C19(H19), C34(H34), C35(H35), C37(H37), C38(H38)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C32(H32A,H32B,H32C), C39(H39A,H39B,H39C), C24A(H24D,H24E,H24F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.82392(9) 0.24160(8) 0.62074(8) 0.0308(2) Uani 1 1 d . . . . .
O1 O 0.8268(2) 0.2280(2) 0.2983(2) 0.0310(6) Uani 1 1 d . . . . .
O2 O 0.4650(2) 0.53382(19) 0.1334(2) 0.0251(5) Uani 1 1 d . . . . .
O3 O 0.9315(3) 0.1950(2) 0.6164(3) 0.0412(8) Uani 1 1 d . . . . .
O4 O 0.7465(3) 0.2107(2) 0.6832(2) 0.0410(7) Uani 1 1 d . . . . .
N1 N 0.6958(3) 0.3192(2) 0.2101(2) 0.0229(6) Uani 1 1 d . . . . .
N2 N 0.7134(3) 0.8609(3) 0.3676(3) 0.0361(8) Uani 1 1 d D . . . .
N3 N 0.1895(3) 0.2390(3) -0.1154(3) 0.0296(7) Uani 1 1 d . . . . .
N4 N 0.7569(3) 0.2059(2) 0.4927(3) 0.0279(7) Uani 1 1 d D . . . .
C1 C 0.7371(3) 0.2737(3) 0.2898(3) 0.0242(7) Uani 1 1 d . . . . .
C2 C 0.6548(3) 0.2896(3) 0.3643(3) 0.0209(7) Uani 1 1 d . . . . .
C3 C 0.6592(3) 0.2590(3) 0.4588(3) 0.0235(7) Uani 1 1 d . . . . .
C4 C 0.5699(3) 0.2826(3) 0.5153(3) 0.0274(8) Uani 1 1 d . . . . .
H4A H 0.569481 0.260854 0.579172 0.033 Uiso 1 1 calc R . . . .
C5 C 0.4808(3) 0.3383(3) 0.4779(3) 0.0290(8) Uani 1 1 d . . . . .
H5 H 0.420024 0.354040 0.517202 0.035 Uiso 1 1 calc R . . . .
C6 C 0.4780(3) 0.3715(3) 0.3849(3) 0.0268(8) Uani 1 1 d . . . . .
H6 H 0.416742 0.409900 0.360672 0.032 Uiso 1 1 calc R . . . .
C7 C 0.5671(3) 0.3469(3) 0.3289(3) 0.0221(7) Uani 1 1 d . . . . .
C8 C 0.5924(3) 0.3801(3) 0.2314(3) 0.0218(7) Uani 1 1 d . . . . .
C9 C 0.6263(3) 0.5065(3) 0.2630(3) 0.0217(7) Uani 1 1 d . . . . .
C10 C 0.7231(3) 0.5606(3) 0.3455(3) 0.0254(7) Uani 1 1 d . . . . .
H10 H 0.770649 0.515996 0.378321 0.031 Uiso 1 1 calc R . . . .
C11 C 0.7521(3) 0.6756(3) 0.3806(3) 0.0252(7) Uani 1 1 d . . . . .
H11 H 0.818563 0.708567 0.436851 0.030 Uiso 1 1 calc R . . . .
C12 C 0.6842(3) 0.7456(3) 0.3342(3) 0.0245(7) Uani 1 1 d . . . . .
C13 C 0.5870(3) 0.6917(3) 0.2510(3) 0.0241(7) Uani 1 1 d . . . . .
H13 H 0.538572 0.735637 0.218008 0.029 Uiso 1 1 calc R . . . .
C14 C 0.5613(3) 0.5752(3) 0.2167(3) 0.0211(7) Uani 1 1 d . . . . .
C15 C 0.4329(3) 0.4189(3) 0.0941(3) 0.0218(7) Uani 1 1 d . . . . .
C16 C 0.3342(3) 0.3859(3) 0.0114(3) 0.0242(7) Uani 1 1 d . . . . .
H16 H 0.298159 0.441176 -0.015098 0.029 Uiso 1 1 calc R . . . .
C17 C 0.2868(3) 0.2721(3) -0.0336(3) 0.0250(7) Uani 1 1 d . . . . .
C18 C 0.3437(3) 0.1939(3) 0.0105(3) 0.0290(8) Uani 1 1 d . . . . .
H18 H 0.313898 0.116102 -0.016234 0.035 Uiso 1 1 calc R . . . .
C19 C 0.4420(3) 0.2302(3) 0.0921(3) 0.0290(8) Uani 1 1 d . . . . .
H19 H 0.479072 0.175738 0.119280 0.035 Uiso 1 1 calc R . . . .
C20 C 0.4897(3) 0.3428(3) 0.1365(3) 0.0230(7) Uani 1 1 d . . . . .
C21 C 0.8088(4) 0.9150(3) 0.4601(4) 0.0386(10) Uani 1 1 d . . . . .
H21A H 0.833129 0.991597 0.457744 0.046 Uiso 1 1 calc R . . . .
H21B H 0.875819 0.871481 0.452163 0.046 Uiso 1 1 calc R . . . .
C22 C 0.7798(5) 0.9248(4) 0.5701(4) 0.0526(13) Uani 1 1 d . . . . .
H22A H 0.751980 0.849818 0.572269 0.079 Uiso 1 1 calc GR . . . .
H22B H 0.718912 0.974286 0.582183 0.079 Uiso 1 1 calc GR . . . .
H22C H 0.849482 0.956505 0.627314 0.079 Uiso 1 1 calc GR . . . .
C23 C 0.6488(5) 0.9329(4) 0.3145(5) 0.0289(14) Uani 0.763(11) 1 d D . P A 1
H23A H 0.621394 0.891890 0.235773 0.035 Uiso 0.763(11) 1 calc R . P A 1
H23B H 0.700795 1.001308 0.321194 0.035 Uiso 0.763(11) 1 calc R . P A 1
C24 C 0.5450(5) 0.9671(5) 0.3657(5) 0.0370(16) Uani 0.763(11) 1 d D . P A 1
H24A H 0.506468 1.019761 0.332531 0.056 Uiso 0.763(11) 1 calc GR . P A 1
H24B H 0.571609 1.003831 0.444425 0.056 Uiso 0.763(11) 1 calc GR . P A 1
H24C H 0.490048 0.899956 0.353311 0.056 Uiso 0.763(11) 1 calc GR . P A 1
C25 C 0.1315(3) 0.3228(3) -0.1562(3) 0.0327(8) Uani 1 1 d . . . . .
H25A H 0.083805 0.284352 -0.229883 0.039 Uiso 1 1 calc R . . . .
H25B H 0.191394 0.377990 -0.163691 0.039 Uiso 1 1 calc R . . . .
C26 C 0.0537(4) 0.3864(4) -0.0844(4) 0.0485(11) Uani 1 1 d . . . . .
H26A H 0.022809 0.444610 -0.114192 0.073 Uiso 1 1 calc GR . . . .
H26B H 0.099066 0.421995 -0.010179 0.073 Uiso 1 1 calc GR . . . .
H26C H -0.010829 0.333676 -0.082490 0.073 Uiso 1 1 calc GR . . . .
C27 C 0.1345(4) 0.1216(3) -0.1586(3) 0.0378(9) Uani 1 1 d . . . . .
H27A H 0.196068 0.071077 -0.162860 0.045 Uiso 1 1 calc R . . . .
H27B H 0.090154 0.108595 -0.233757 0.045 Uiso 1 1 calc R . . . .
C28 C 0.0528(5) 0.0903(5) -0.0905(6) 0.0663(16) Uani 1 1 d . . . . .
H28A H 0.025105 0.009441 -0.119875 0.099 Uiso 1 1 calc GR . . . .
H28B H -0.013669 0.133477 -0.093123 0.099 Uiso 1 1 calc GR . . . .
H28C H 0.094496 0.107820 -0.014671 0.099 Uiso 1 1 calc GR . . . .
C29 C 0.7636(4) 0.3366(3) 0.1310(3) 0.0314(8) Uani 1 1 d . . . . .
H29A H 0.845178 0.325580 0.155782 0.038 Uiso 1 1 calc R . . . .
H29B H 0.763353 0.415889 0.130794 0.038 Uiso 1 1 calc R . . . .
C30 C 0.7206(4) 0.2597(4) 0.0145(3) 0.0372(9) Uani 1 1 d . . . . .
H30A H 0.637465 0.266603 -0.009134 0.045 Uiso 1 1 calc R . . . .
H30B H 0.764353 0.285220 -0.034154 0.045 Uiso 1 1 calc R . . . .
C31 C 0.7337(5) 0.1370(4) 0.0014(4) 0.0430(11) Uani 1 1 d . . . . .
H31A H 0.688425 0.110469 0.048407 0.052 Uiso 1 1 calc R . . . .
H31B H 0.816569 0.129756 0.025957 0.052 Uiso 1 1 calc R . . . .
C32 C 0.6921(7) 0.0630(5) -0.1166(4) 0.075(2) Uani 1 1 d . . . . .
H32A H 0.737239 0.088670 -0.163310 0.113 Uiso 1 1 calc GR . . . .
H32B H 0.609515 0.068198 -0.140487 0.113 Uiso 1 1 calc GR . . . .
H32C H 0.702855 -0.015497 -0.121852 0.113 Uiso 1 1 calc GR . . . .
C33 C 0.8505(3) 0.3900(3) 0.6640(3) 0.0260(7) Uani 1 1 d . . . . .
C34 C 0.7860(3) 0.4535(3) 0.7337(3) 0.0301(8) Uani 1 1 d . . . . .
H34 H 0.729042 0.417724 0.760480 0.036 Uiso 1 1 calc R . . . .
C35 C 0.8064(3) 0.5698(3) 0.7633(3) 0.0306(8) Uani 1 1 d . . . . .
H35 H 0.763533 0.613709 0.811745 0.037 Uiso 1 1 calc R . . . .
C36 C 0.8875(3) 0.6241(3) 0.7243(3) 0.0301(8) Uani 1 1 d . . . . .
C37 C 0.9514(4) 0.5588(3) 0.6544(3) 0.0347(9) Uani 1 1 d . . . . .
H37 H 1.007649 0.594614 0.626904 0.042 Uiso 1 1 calc R . . . .
C38 C 0.9333(3) 0.4419(3) 0.6248(3) 0.0328(9) Uani 1 1 d . . . . .
H38 H 0.977486 0.397821 0.577838 0.039 Uiso 1 1 calc R . . . .
C39 C 0.9071(4) 0.7522(3) 0.7572(4) 0.0436(11) Uani 1 1 d . . . . .
H39A H 0.831891 0.781443 0.748487 0.065 Uiso 1 1 calc GR . . . .
H39B H 0.954195 0.775505 0.710610 0.065 Uiso 1 1 calc GR . . . .
H39C H 0.947827 0.782232 0.833667 0.065 Uiso 1 1 calc GR . . . .
H4 H 0.810(3) 0.201(4) 0.452(4) 0.052 Uiso 1 1 d DR . . . .
C24A C 0.6120(17) 0.9836(14) 0.2696(15) 0.038(5) Uani 0.237(11) 1 d D . P A 2
H24D H 0.604398 0.924296 0.199708 0.056 Uiso 0.237(11) 1 calc GR . P A 2
H24E H 0.685526 1.032501 0.284882 0.056 Uiso 0.237(11) 1 calc GR . P A 2
H24F H 0.546982 1.028452 0.265888 0.056 Uiso 0.237(11) 1 calc GR . P A 2
C23A C 0.6106(15) 0.9302(13) 0.3598(16) 0.033(5) Uani 0.237(11) 1 d D . P A 2
H23C H 0.536496 0.880473 0.344521 0.039 Uiso 0.237(11) 1 calc R . P A 2
H23D H 0.616104 0.989746 0.430265 0.039 Uiso 0.237(11) 1 calc R . 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
S1 O3 1.431(3) . ?
S1 O4 1.429(3) . ?
S1 N4 1.638(3) . ?
S1 C33 1.761(4) . ?
O1 C1 1.236(4) . ?
O2 C14 1.380(4) . ?
O2 C15 1.377(4) . ?
N1 C1 1.357(5) . ?
N1 C8 1.501(4) . ?
N1 C29 1.465(5) . ?
N2 C12 1.378(4) . ?
N2 C21 1.460(5) . ?
N2 C23 1.460(6) . ?
N2 C23A 1.538(14) . ?
N3 C17 1.370(5) . ?
N3 C25 1.461(5) . ?
N3 C27 1.467(5) . ?
N4 C3 1.431(4) . ?
N4 H4 0.883(10) . ?
C1 C2 1.471(5) . ?
C2 C3 1.388(5) . ?
C2 C7 1.383(5) . ?
C3 C4 1.386(5) . ?
C4 H4A 0.9500 . ?
C4 C5 1.390(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.382(5) . ?
C7 C8 1.518(5) . ?
C8 C9 1.516(4) . ?
C8 C20 1.511(5) . ?
C9 C10 1.402(5) . ?
C9 C14 1.382(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.373(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.413(5) . ?
C12 C13 1.409(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.387(5) . ?
C15 C16 1.388(5) . ?
C15 C20 1.383(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.404(5) . ?
C17 C18 1.418(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.379(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.392(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.506(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.519(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.519(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.522(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.521(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.511(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.523(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.391(5) . ?
C33 C38 1.384(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.382(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.383(6) . ?
C36 C37 1.398(5) . ?
C36 C39 1.520(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.387(5) . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C24A C23A 1.514(16) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 S1 N4 103.95(18) . . ?
O3 S1 C33 109.77(18) . . ?
O4 S1 O3 120.47(19) . . ?
O4 S1 N4 108.88(18) . . ?
O4 S1 C33 107.30(19) . . ?
N4 S1 C33 105.52(16) . . ?
C15 O2 C14 118.4(3) . . ?
C1 N1 C8 112.8(3) . . ?
C1 N1 C29 123.0(3) . . ?
C29 N1 C8 121.9(3) . . ?
C12 N2 C21 120.3(3) . . ?
C12 N2 C23 121.7(3) . . ?
C12 N2 C23A 115.5(7) . . ?
C21 N2 C23 118.0(3) . . ?
C21 N2 C23A 114.0(7) . . ?
C17 N3 C25 120.2(3) . . ?
C17 N3 C27 122.0(3) . . ?
C25 N3 C27 117.6(3) . . ?
S1 N4 H4 108(3) . . ?
C3 N4 S1 121.4(3) . . ?
C3 N4 H4 114(3) . . ?
O1 C1 N1 126.5(4) . . ?
O1 C1 C2 126.5(3) . . ?
N1 C1 C2 106.9(3) . . ?
C3 C2 C1 129.1(3) . . ?
C7 C2 C1 109.3(3) . . ?
C7 C2 C3 121.6(3) . . ?
C2 C3 N4 117.7(3) . . ?
C4 C3 N4 124.0(3) . . ?
C4 C3 C2 118.3(3) . . ?
C3 C4 H4A 120.2 . . ?
C3 C4 C5 119.6(3) . . ?
C5 C4 H4A 120.2 . . ?
C4 C5 H5 118.9 . . ?
C6 C5 C4 122.1(4) . . ?
C6 C5 H5 118.9 . . ?
C5 C6 H6 121.1 . . ?
C7 C6 C5 117.8(3) . . ?
C7 C6 H6 121.1 . . ?
C2 C7 C8 109.7(3) . . ?
C6 C7 C2 120.5(3) . . ?
C6 C7 C8 129.7(3) . . ?
N1 C8 C7 100.6(3) . . ?
N1 C8 C9 110.2(3) . . ?
N1 C8 C20 113.4(3) . . ?
C9 C8 C7 110.4(3) . . ?
C20 C8 C7 111.5(3) . . ?
C20 C8 C9 110.2(3) . . ?
C10 C9 C8 121.1(3) . . ?
C14 C9 C8 122.5(3) . . ?
C14 C9 C10 116.3(3) . . ?
C9 C10 H10 118.7 . . ?
C11 C10 C9 122.6(3) . . ?
C11 C10 H10 118.7 . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.8(3) . . ?
C12 C11 H11 119.6 . . ?
N2 C12 C11 121.4(3) . . ?
N2 C12 C13 121.7(3) . . ?
C13 C12 C11 116.9(3) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.6(3) . . ?
C14 C13 H13 119.7 . . ?
O2 C14 C9 122.9(3) . . ?
O2 C14 C13 114.4(3) . . ?
C9 C14 C13 122.7(3) . . ?
O2 C15 C16 114.0(3) . . ?
O2 C15 C20 123.5(3) . . ?
C20 C15 C16 122.4(3) . . ?
C15 C16 H16 119.5 . . ?
C15 C16 C17 121.1(3) . . ?
C17 C16 H16 119.5 . . ?
N3 C17 C16 121.3(3) . . ?
N3 C17 C18 122.0(3) . . ?
C16 C17 C18 116.7(3) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.3(3) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 118.4 . . ?
C18 C19 C20 123.1(3) . . ?
C20 C19 H19 118.4 . . ?
C15 C20 C8 122.2(3) . . ?
C15 C20 C19 116.3(3) . . ?
C19 C20 C8 121.3(3) . . ?
N2 C21 H21A 108.7 . . ?
N2 C21 H21B 108.7 . . ?
N2 C21 C22 114.4(4) . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
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 . . ?
N2 C23 H23A 109.4 . . ?
N2 C23 H23B 109.4 . . ?
N2 C23 C24 111.0(5) . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 108.6 . . ?
N3 C25 H25B 108.6 . . ?
N3 C25 C26 114.5(4) . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 H25A 108.6 . . ?
C26 C25 H25B 108.6 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C27 H27A 108.8 . . ?
N3 C27 H27B 108.8 . . ?
N3 C27 C28 113.8(4) . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1 C29 H29A 108.5 . . ?
N1 C29 H29B 108.5 . . ?
N1 C29 C30 115.1(3) . . ?
H29A C29 H29B 107.5 . . ?
C30 C29 H29A 108.5 . . ?
C30 C29 H29B 108.5 . . ?
C29 C30 H30A 108.9 . . ?
C29 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C31 C30 C29 113.4(3) . . ?
C31 C30 H30A 108.9 . . ?
C31 C30 H30B 108.9 . . ?
C30 C31 H31A 109.2 . . ?
C30 C31 H31B 109.2 . . ?
C30 C31 C32 111.9(4) . . ?
H31A C31 H31B 107.9 . . ?
C32 C31 H31A 109.2 . . ?
C32 C31 H31B 109.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 S1 120.1(3) . . ?
C38 C33 S1 119.0(3) . . ?
C38 C33 C34 120.8(3) . . ?
C33 C34 H34 120.7 . . ?
C35 C34 C33 118.6(4) . . ?
C35 C34 H34 120.7 . . ?
C34 C35 H35 119.0 . . ?
C34 C35 C36 121.9(4) . . ?
C36 C35 H35 119.0 . . ?
C35 C36 C37 118.6(3) . . ?
C35 C36 C39 120.7(4) . . ?
C37 C36 C39 120.7(4) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 C36 120.4(4) . . ?
C38 C37 H37 119.8 . . ?
C33 C38 C37 119.6(4) . . ?
C33 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
N2 C23A H23C 109.7 . . ?
N2 C23A H23D 109.7 . . ?
C24A C23A N2 109.9(14) . . ?
C24A C23A H23C 109.7 . . ?
C24A C23A H23D 109.7 . . ?
H23C C23A H23D 108.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N4 H4 O1 0.883(10) 2.17(4) 2.882(4) 138(5) . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 N4 C3 C2 136.4(3) . . . . ?
S1 N4 C3 C4 -42.8(5) . . . . ?
S1 C33 C34 C35 -178.0(3) . . . . ?
S1 C33 C38 C37 177.2(3) . . . . ?
O1 C1 C2 C3 0.7(6) . . . . ?
O1 C1 C2 C7 178.4(3) . . . . ?
O2 C15 C16 C17 -176.8(3) . . . . ?
O2 C15 C20 C8 0.5(5) . . . . ?
O2 C15 C20 C19 176.1(3) . . . . ?
O3 S1 N4 C3 -164.4(3) . . . . ?
O3 S1 C33 C34 -141.8(3) . . . . ?
O3 S1 C33 C38 40.3(4) . . . . ?
O4 S1 N4 C3 66.0(3) . . . . ?
O4 S1 C33 C34 -9.2(4) . . . . ?
O4 S1 C33 C38 172.9(3) . . . . ?
N1 C1 C2 C3 -179.2(3) . . . . ?
N1 C1 C2 C7 -1.4(4) . . . . ?
N1 C8 C9 C10 -50.7(4) . . . . ?
N1 C8 C9 C14 132.5(3) . . . . ?
N1 C8 C20 C15 -128.8(3) . . . . ?
N1 C8 C20 C19 55.8(4) . . . . ?
N1 C29 C30 C31 -66.8(5) . . . . ?
N2 C12 C13 C14 178.2(4) . . . . ?
N3 C17 C18 C19 179.4(4) . . . . ?
N4 S1 C33 C34 106.8(3) . . . . ?
N4 S1 C33 C38 -71.1(3) . . . . ?
N4 C3 C4 C5 177.6(3) . . . . ?
C1 N1 C8 C7 -8.7(3) . . . . ?
C1 N1 C8 C9 107.9(3) . . . . ?
C1 N1 C8 C20 -128.0(3) . . . . ?
C1 N1 C29 C30 110.0(4) . . . . ?
C1 C2 C3 N4 1.2(5) . . . . ?
C1 C2 C3 C4 -179.6(3) . . . . ?
C1 C2 C7 C6 179.4(3) . . . . ?
C1 C2 C7 C8 -4.2(4) . . . . ?
C2 C3 C4 C5 -1.6(5) . . . . ?
C2 C7 C8 N1 7.5(3) . . . . ?
C2 C7 C8 C9 -108.9(3) . . . . ?
C2 C7 C8 C20 128.1(3) . . . . ?
C3 C2 C7 C6 -2.6(5) . . . . ?
C3 C2 C7 C8 173.8(3) . . . . ?
C3 C4 C5 C6 0.0(6) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C5 C6 C7 C2 0.9(5) . . . . ?
C5 C6 C7 C8 -174.6(3) . . . . ?
C6 C7 C8 N1 -176.6(3) . . . . ?
C6 C7 C8 C9 67.0(4) . . . . ?
C6 C7 C8 C20 -56.0(5) . . . . ?
C7 C2 C3 N4 -176.3(3) . . . . ?
C7 C2 C3 C4 2.9(5) . . . . ?
C7 C8 C9 C10 59.6(4) . . . . ?
C7 C8 C9 C14 -117.2(4) . . . . ?
C7 C8 C20 C15 118.4(4) . . . . ?
C7 C8 C20 C19 -57.0(4) . . . . ?
C8 N1 C1 O1 -173.2(3) . . . . ?
C8 N1 C1 C2 6.7(4) . . . . ?
C8 N1 C29 C30 -88.8(4) . . . . ?
C8 C9 C10 C11 -176.0(3) . . . . ?
C8 C9 C14 O2 -4.3(5) . . . . ?
C8 C9 C14 C13 175.1(3) . . . . ?
C9 C8 C20 C15 -4.7(5) . . . . ?
C9 C8 C20 C19 180.0(3) . . . . ?
C9 C10 C11 C12 -0.1(6) . . . . ?
C10 C9 C14 O2 178.7(3) . . . . ?
C10 C9 C14 C13 -1.9(5) . . . . ?
C10 C11 C12 N2 -179.0(4) . . . . ?
C10 C11 C12 C13 -0.2(5) . . . . ?
C11 C12 C13 C14 -0.6(5) . . . . ?
C12 N2 C21 C22 -76.0(5) . . . . ?
C12 N2 C23 C24 87.3(5) . . . . ?
C12 N2 C23A C24A -110.0(12) . . . . ?
C12 C13 C14 O2 -178.9(3) . . . . ?
C12 C13 C14 C9 1.7(5) . . . . ?
C14 O2 C15 C16 179.2(3) . . . . ?
C14 O2 C15 C20 2.4(5) . . . . ?
C14 C9 C10 C11 1.1(5) . . . . ?
C15 O2 C14 C9 -0.5(5) . . . . ?
C15 O2 C14 C13 180.0(3) . . . . ?
C15 C16 C17 N3 -179.9(3) . . . . ?
C15 C16 C17 C18 0.8(5) . . . . ?
C16 C15 C20 C8 -175.9(3) . . . . ?
C16 C15 C20 C19 -0.4(5) . . . . ?
C16 C17 C18 C19 -1.3(6) . . . . ?
C17 N3 C25 C26 -79.2(5) . . . . ?
C17 N3 C27 C28 82.6(5) . . . . ?
C17 C18 C19 C20 1.0(6) . . . . ?
C18 C19 C20 C8 175.5(4) . . . . ?
C18 C19 C20 C15 -0.1(6) . . . . ?
C20 C8 C9 C10 -176.7(3) . . . . ?
C20 C8 C9 C14 6.5(5) . . . . ?
C20 C15 C16 C17 0.0(5) . . . . ?
C21 N2 C12 C11 -6.4(6) . . . . ?
C21 N2 C12 C13 174.9(4) . . . . ?
C21 N2 C23 C24 -91.0(5) . . . . ?
C21 N2 C23A C24A 104.5(12) . . . . ?
C23 N2 C12 C11 175.4(4) . . . . ?
C23 N2 C12 C13 -3.3(6) . . . . ?
C23 N2 C21 C22 102.2(5) . . . . ?
C25 N3 C17 C16 -1.2(5) . . . . ?
C25 N3 C17 C18 178.1(3) . . . . ?
C25 N3 C27 C28 -92.4(5) . . . . ?
C27 N3 C17 C16 -176.0(4) . . . . ?
C27 N3 C17 C18 3.2(6) . . . . ?
C27 N3 C25 C26 95.9(4) . . . . ?
C29 N1 C1 O1 -10.4(5) . . . . ?
C29 N1 C1 C2 169.5(3) . . . . ?
C29 N1 C8 C7 -171.7(3) . . . . ?
C29 N1 C8 C9 -55.1(4) . . . . ?
C29 N1 C8 C20 69.0(4) . . . . ?
C29 C30 C31 C32 -178.8(5) . . . . ?
C33 S1 N4 C3 -48.9(3) . . . . ?
C33 C34 C35 C36 0.9(6) . . . . ?
C34 C33 C38 C37 -0.7(6) . . . . ?
C34 C35 C36 C37 -0.9(6) . . . . ?
C34 C35 C36 C39 179.2(4) . . . . ?
C35 C36 C37 C38 0.1(6) . . . . ?
C36 C37 C38 C33 0.7(6) . . . . ?
C38 C33 C34 C35 -0.1(6) . . . . ?
C39 C36 C37 C38 179.9(4) . . . . ?
C23A N2 C12 C11 -149.6(9) . . . . ?
C23A N2 C12 C13 31.7(10) . . . . ?
C23A N2 C21 C22 67.7(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.725(3)
2 0.275(3)

