# Electronic Supplementary Material (ESI) for ChemComm.
# 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_crystalclear_sq
_database_code_depnum_ccdc_archive 'CCDC 1864209'
loop_
_audit_author_name
_audit_author_address
'Shin-ichiro Kawano'
;Nagoya University
Japan
;
_audit_update_record             
;
2019-02-05 deposited with the CCDC.	2019-02-13 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         ?
_chemical_formula_sum            'C92 H90 N8 O16'
_chemical_formula_weight         1563.71

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/a'
_space_group_name_Hall           '-P 2yba'

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

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

_cell_length_a                   13.051(14)
_cell_length_b                   18.73(2)
_cell_length_c                   19.67(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.889(10)
_cell_angle_gamma                90
_cell_volume                     4808(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    7490
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      25.20

_exptl_crystal_description       platelet
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.075
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39056
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.004
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8441
_reflns_number_gt                6681
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1178P)²+4.0689P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8441
_refine_ls_number_parameters     550
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.2270
_refine_ls_wR_factor_gt          0.2119
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.002
_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
N1 N 0.5405(2) 0.04371(16) 0.59696(16) 0.0334(6) Uani 1 1 d . . . . .
N2 N 0.52562(19) -0.10196(14) 0.53971(13) 0.0322(6) Uani 1 1 d . . . . .
O1 O 0.5674(2) -0.1806(2) 0.97782(14) 0.0746(10) Uani 1 1 d . . . . .
O2 O 0.5092(3) -0.2527(2) 1.09332(16) 0.0564(15) Uani 0.811(11) 1 d . . P A 1
O3 O 1.08766(18) -0.11006(14) 0.75062(15) 0.0503(7) Uani 1 1 d . . . . .
O4 O 1.24028(18) -0.21192(14) 0.70849(13) 0.0481(6) Uani 1 1 d . . . . .
O6 O 0.2841(3) -0.63405(17) 0.48795(16) 0.0686(8) Uani 1 1 d . . . . .
O8 O 0.8480(2) -0.45724(16) 0.12129(14) 0.0569(7) Uani 1 1 d . . . B 2
C2 C 0.5853(3) 0.12509(19) 0.67936(16) 0.0363(7) Uani 1 1 d . . . . .
H2 H 0.5942 0.1689 0.7030 0.044 Uiso 1 1 calc R U . . .
C3 C 0.6105(3) 0.05768(18) 0.70379(17) 0.0378(8) Uani 1 1 d . . . . .
H3 H 0.6407 0.0472 0.7469 0.045 Uiso 1 1 calc R U . . .
C4 C 0.5825(2) 0.00586(17) 0.65161(16) 0.0330(7) Uani 1 1 d . . . . .
C5 C 0.5988(2) -0.06922(18) 0.65366(16) 0.0337(7) Uani 1 1 d . . . . .
C7 C 0.5910(2) -0.19814(18) 0.60697(17) 0.0352(7) Uani 1 1 d . . . . .
H7 H 0.6197 -0.2234 0.6446 0.042 Uiso 1 1 calc R U . . .
C8 C 0.5594(2) -0.22662(18) 0.54559(17) 0.0346(7) Uani 1 1 d . . . . .
H8 H 0.5624 -0.2753 0.5323 0.042 Uiso 1 1 calc R U . . .
C10 C 0.4883(2) -0.17293(17) 0.43393(16) 0.0316(7) Uani 1 1 d . . . . .
C11 C 0.7686(2) -0.09642(17) 0.71434(17) 0.0353(7) Uani 1 1 d . . . . .
C13 C 0.9437(3) -0.0818(2) 0.6786(2) 0.0441(9) Uani 1 1 d . . . . .
H13 H 0.9919 -0.0684 0.6453 0.053 Uiso 1 1 calc R U . . .
C16 C 0.8031(2) -0.12141(18) 0.77966(17) 0.0347(7) Uani 1 1 d . . . . .
C17 C 0.7114(2) -0.13598(18) 0.81921(16) 0.0350(7) Uani 1 1 d . . . . .
C12 C 0.8380(3) -0.07561(19) 0.66316(18) 0.0397(8) Uani 1 1 d . . . . .
H12 H 0.8144 -0.0582 0.6203 0.048 Uiso 1 1 calc R U . . .
C14 C 0.9797(3) -0.10741(18) 0.74228(19) 0.0406(8) Uani 1 1 d . . . . .
C18 C 0.6958(3) -0.1600(2) 0.88771(18) 0.0437(9) Uani 1 1 d . . . . .
H18 H 0.7519 -0.1731 0.9164 0.052 Uiso 1 1 calc R U . . .
C19 C 0.5944(3) -0.1635(2) 0.91072(19) 0.0524(10) Uani 1 1 d . . . . .
C20 C 0.5083(3) -0.1473(2) 0.86725(19) 0.0541(10) Uani 1 1 d . . . . .
H20 H 0.4408 -0.1520 0.8841 0.065 Uiso 1 1 calc R U . . .
C21 C 0.5226(3) -0.1244(2) 0.79987(18) 0.0449(9) Uani 1 1 d . . . . .
H21 H 0.4658 -0.1132 0.7711 0.054 Uiso 1 1 calc R U . . .
C22 C 0.6239(2) -0.11878(17) 0.77635(16) 0.0336(7) Uani 1 1 d . . . . .
C23 C 0.4143(2) -0.29877(17) 0.41779(17) 0.0340(7) Uani 1 1 d . . . . .
C24 C 0.3360(3) -0.30070(18) 0.46692(17) 0.0380(8) Uani 1 1 d . . . . .
H59 H 0.3243 -0.2614 0.4963 0.046 Uiso 1 1 calc R U . . .
C15 C 0.9106(3) -0.12807(19) 0.79397(18) 0.0394(8) Uani 1 1 d . . . . .
H15 H 0.9350 -0.1457 0.8365 0.047 Uiso 1 1 calc R U . . .
C26 C 0.2909(3) -0.42176(18) 0.42570(19) 0.0402(8) Uani 1 1 d . . . . .
C27 C 0.3690(3) -0.42047(18) 0.37534(18) 0.0386(8) Uani 1 1 d . . . . .
H27 H 0.3789 -0.4596 0.3455 0.046 Uiso 1 1 calc R U . . .
C28 C 0.4314(2) -0.35763(17) 0.37184(17) 0.0349(7) Uani 1 1 d . . . . .
C29 C 0.5192(2) -0.33688(17) 0.32897(17) 0.0343(7) Uani 1 1 d . . . . .
C30 C 0.5726(2) -0.37209(18) 0.27509(16) 0.0344(7) Uani 1 1 d . . . . .
H30 H 0.5523 -0.4182 0.2598 0.041 Uiso 1 1 calc R U . . .
C31 C 0.6554(2) -0.33656(18) 0.24570(16) 0.0360(7) Uani 1 1 d . . . . .
C32 C 0.6879(3) -0.26743(18) 0.26917(16) 0.0359(7) Uani 1 1 d . . . . .
H32 H 0.7450 -0.2451 0.2486 0.043 Uiso 1 1 calc R U . . .
C33 C 0.6371(2) -0.23224(18) 0.32181(16) 0.0361(7) Uani 1 1 d . . . . .
H33 H 0.6591 -0.1868 0.3377 0.043 Uiso 1 1 calc R U . . .
C35 C 0.6470(3) -0.2072(3) 1.0242(2) 0.0628(12) Uani 1 1 d . . . . .
H35 H 0.7078 -0.1757 1.0237 0.075 Uiso 1 1 calc R U . A 1
H35A H 0.6682 -0.2561 1.0112 0.075 Uiso 1 1 calc R U . A 1
C36 C 0.5977(7) -0.2074(5) 1.0956(3) 0.0530(19) Uani 0.811(11) 1 d . . P A 1
H49 H 0.6476 -0.2253 1.1300 0.064 Uiso 0.811(11) 1 calc R U P A 1
H50 H 0.5777 -0.1583 1.1084 0.064 Uiso 0.811(11) 1 calc R U P A 1
C37 C 0.4409(4) -0.2321(4) 1.1484(3) 0.0860(17) Uani 1 1 d . . . . .
H53 H 0.3800 -0.2627 1.1474 0.129 Uiso 1 1 calc R U . A 1
H54 H 0.4769 -0.2377 1.1922 0.129 Uiso 1 1 calc R U . A 1
H55 H 0.4202 -0.1822 1.1425 0.129 Uiso 1 1 calc R U . A 1
C38 C 1.1298(3) -0.1662(2) 0.79544(19) 0.0442(8) Uani 1 1 d . . . . .
H38 H 1.0900 -0.2109 0.7900 0.053 Uiso 1 1 calc R U . . .
H38A H 1.1269 -0.1510 0.8436 0.053 Uiso 1 1 calc R U . . .
C39 C 1.2414(3) -0.1778(2) 0.77445(19) 0.0455(9) Uani 1 1 d . . . . .
H39 H 1.2776 -0.1315 0.7721 0.055 Uiso 1 1 calc R U . . .
H39A H 1.2774 -0.2084 0.8082 0.055 Uiso 1 1 calc R U . . .
C40 C 1.3412(3) -0.2198(2) 0.6795(2) 0.0490(9) Uani 1 1 d . . . . .
H40 H 1.3690 -0.1726 0.6689 0.074 Uiso 1 1 calc R U . . .
H40A H 1.3361 -0.2482 0.6378 0.074 Uiso 1 1 calc R U . . .
H40B H 1.3868 -0.2439 0.7122 0.074 Uiso 1 1 calc R U . . .
C41 C 0.2329(3) -0.54401(19) 0.3988(2) 0.0458(9) Uani 1 1 d . . . . .
H41 H 0.2518 -0.5330 0.3514 0.055 Uiso 1 1 calc R U . . .
H41A H 0.1658 -0.5687 0.3974 0.055 Uiso 1 1 calc R U . . .
C42 C 0.3147(4) -0.5955(2) 0.4303(2) 0.0579(11) Uani 1 1 d . . . . .
H42 H 0.3351 -0.6300 0.3948 0.070 Uiso 1 1 calc R U . . .
H42A H 0.3762 -0.5671 0.4427 0.070 Uiso 1 1 calc R U . . .
C43 C 0.2955(4) -0.5949(3) 0.5510(2) 0.0669(12) Uani 1 1 d . . . . .
H43 H 0.3662 -0.5778 0.5558 0.100 Uiso 1 1 calc R U . . .
H43A H 0.2795 -0.6263 0.5892 0.100 Uiso 1 1 calc R U . . .
H43B H 0.2485 -0.5541 0.5506 0.100 Uiso 1 1 calc R U . . .
C44 C 0.6775(3) -0.4290(2) 0.15889(18) 0.0439(8) Uani 1 1 d . . . . .
H44 H 0.6054 -0.4238 0.1434 0.053 Uiso 1 1 calc R U . . .
H44A H 0.6817 -0.4689 0.1918 0.053 Uiso 1 1 calc R U . . .
C45 C 0.7460(3) -0.4442(2) 0.0982(2) 0.0516(10) Uani 1 1 d . . . . .
H70 H 0.7198 -0.4863 0.0731 0.062 Uiso 1 1 calc R U . B 2
H71 H 0.7450 -0.4028 0.0669 0.062 Uiso 1 1 calc R U . B 2
C46 C 0.9169(3) -0.4704(3) 0.0658(2) 0.0690(13) Uani 1 1 d . . . B 2
H72 H 0.8937 -0.5124 0.0402 0.104 Uiso 1 1 calc R U . B 2
H73 H 0.9862 -0.4789 0.0840 0.104 Uiso 1 1 calc R U . B 2
H74 H 0.9176 -0.4288 0.0356 0.104 Uiso 1 1 calc R U . B 2
N3 N 0.6596(2) -0.09546(15) 0.71187(14) 0.0356(6) Uani 1 1 d . . . . .
N4 N 0.4875(2) -0.24401(14) 0.40490(14) 0.0347(6) Uani 1 1 d . . . . .
O5 O 0.22228(19) -0.47802(13) 0.43564(15) 0.0528(7) Uani 1 1 d . . . . .
O7 O 0.71284(18) -0.36310(13) 0.19090(12) 0.0402(6) Uani 1 1 d . . . . .
C1 C 0.5427(2) 0.11644(17) 0.61071(16) 0.0329(7) Uani 1 1 d . . . . .
C6 C 0.5713(2) -0.12019(17) 0.60280(15) 0.0316(7) Uani 1 1 d . . . . .
C9 C 0.5197(2) -0.16588(17) 0.50417(16) 0.0325(7) Uani 1 1 d . . . . .
C34 C 0.5514(2) -0.26740(17) 0.35053(16) 0.0330(7) Uani 1 1 d . . . . .
H3A H 0.528(3) 0.028(2) 0.566(2) 0.042(13) Uiso 1 1 d . . . . .
O22 O 0.5446(16) -0.1825(12) 1.1079(10) 0.075(8) Uani 0.189(11) 1 d . . P A -1
C366 C 0.605(3) -0.247(2) 1.0860(17) 0.064(10) Uani 0.189(11) 1 d . . P A -1
H51 H 0.5616 -0.2882 1.0736 0.077 Uiso 0.189(11) 1 calc R U P A -1
H52 H 0.6591 -0.2609 1.1192 0.077 Uiso 0.189(11) 1 calc R U P A -1
C25 C 0.2763(3) -0.36297(19) 0.47045(18) 0.0406(8) Uani 1 1 d . . . . .
H60 H 0.2246 -0.3660 0.5038 0.049 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.389(5) . ?
N1 C4 1.393(4) . ?
N2 C9 1.388(4) . ?
N2 C6 1.410(4) . ?
O1 C19 1.408(5) . ?
O1 C35 1.460(5) . ?
O2 C366 1.27(4) . ?
O2 O22 1.42(2) . ?
O2 C36 1.434(9) . ?
O2 C37 1.466(6) . ?
O3 C14 1.417(4) . ?
O3 C38 1.473(4) . ?
O4 C39 1.446(5) . ?
O4 C40 1.451(4) . ?
O6 C42 1.408(5) . ?
O6 C43 1.446(5) . ?
O8 C45 1.421(5) . ?
O8 C46 1.447(5) . ?
C2 C3 1.389(5) . ?
C2 C1 1.462(5) . ?
C3 C4 1.455(5) . ?
C4 C5 1.423(5) . ?
C5 C6 1.425(5) . ?
C5 N3 1.467(4) . ?
C7 C8 1.377(5) . ?
C7 C6 1.484(5) . ?
C8 C9 1.488(5) . ?
C10 C1 1.429(5) 3_656 ?
C10 C9 1.441(5) . ?
C10 N4 1.449(4) . ?
C11 C12 1.420(5) . ?
C11 N3 1.423(4) . ?
C11 C16 1.433(5) . ?
C13 C12 1.412(5) . ?
C13 C14 1.415(5) . ?
C16 C15 1.432(5) . ?
C16 C17 1.463(5) . ?
C17 C18 1.438(5) . ?
C17 C22 1.445(5) . ?
C14 C15 1.423(5) . ?
C18 C19 1.407(5) . ?
C19 C20 1.434(5) . ?
C20 C21 1.408(5) . ?
C21 C22 1.411(5) . ?
C22 N3 1.426(4) . ?
C23 C24 1.418(5) . ?
C23 N4 1.427(4) . ?
C23 C28 1.445(5) . ?
C24 C25 1.405(5) . ?
C26 O5 1.399(4) . ?
C26 C25 1.424(5) . ?
C26 C27 1.432(5) . ?
C27 C28 1.434(5) . ?
C28 C29 1.486(5) . ?
C29 C34 1.430(5) . ?
C29 C30 1.437(5) . ?
C30 C31 1.401(5) . ?
C31 O7 1.413(4) . ?
C31 C32 1.437(5) . ?
C32 C33 1.402(5) . ?
C33 C34 1.423(5) . ?
C35 C366 1.53(4) . ?
C35 C36 1.554(9) . ?
C36 C366 0.77(3) . ?
C36 O22 0.873(18) . ?
C37 O22 1.83(2) . ?
C38 C39 1.536(5) . ?
C41 O5 1.441(5) . ?
C41 C42 1.560(6) . ?
C44 O7 1.457(4) . ?
C44 C45 1.528(5) . ?
N4 C34 1.435(4) . ?
C1 C10 1.429(5) 3_656 ?
O22 C366 1.51(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C4 110.0(3) . . ?
C9 N2 C6 104.7(3) . . ?
C19 O1 C35 118.5(3) . . ?
C366 O2 O22 67.9(18) . . ?
C366 O2 C36 32.3(16) . . ?
O22 O2 C36 35.6(7) . . ?
C366 O2 C37 132.4(16) . . ?
O22 O2 C37 78.9(9) . . ?
C36 O2 C37 108.7(5) . . ?
C14 O3 C38 117.1(3) . . ?
C39 O4 C40 113.6(3) . . ?
C42 O6 C43 113.8(3) . . ?
C45 O8 C46 112.3(3) . . ?
C3 C2 C1 107.7(3) . . ?
C2 C3 C4 107.9(3) . . ?
N1 C4 C5 125.6(3) . . ?
N1 C4 C3 107.2(3) . . ?
C5 C4 C3 127.1(3) . . ?
C4 C5 C6 127.3(3) . . ?
C4 C5 N3 115.6(3) . . ?
C6 C5 N3 116.8(3) . . ?
C8 C7 C6 106.5(3) . . ?
C7 C8 C9 106.3(3) . . ?
C1 C10 C9 126.5(3) 3_656 . ?
C1 C10 N4 116.0(3) 3_656 . ?
C9 C10 N4 117.5(3) . . ?
C12 C11 N3 128.4(3) . . ?
C12 C11 C16 122.0(3) . . ?
N3 C11 C16 109.6(3) . . ?
C12 C13 C14 121.9(3) . . ?
C15 C16 C11 119.9(3) . . ?
C15 C16 C17 133.3(3) . . ?
C11 C16 C17 106.8(3) . . ?
C18 C17 C22 119.6(3) . . ?
C18 C17 C16 133.3(3) . . ?
C22 C17 C16 107.1(3) . . ?
C13 C12 C11 117.2(3) . . ?
C13 C14 O3 115.5(3) . . ?
C13 C14 C15 121.3(3) . . ?
O3 C14 C15 123.2(3) . . ?
C19 C18 C17 117.6(3) . . ?
C18 C19 O1 124.2(3) . . ?
C18 C19 C20 122.1(3) . . ?
O1 C19 C20 113.7(3) . . ?
C21 C20 C19 120.7(3) . . ?
C20 C21 C22 118.1(3) . . ?
C21 C22 N3 129.4(3) . . ?
C21 C22 C17 121.8(3) . . ?
N3 C22 C17 108.7(3) . . ?
C24 C23 N4 129.1(3) . . ?
C24 C23 C28 121.8(3) . . ?
N4 C23 C28 109.1(3) . . ?
C25 C24 C23 117.5(3) . . ?
C14 C15 C16 117.7(3) . . ?
O5 C26 C25 113.8(3) . . ?
O5 C26 C27 125.0(3) . . ?
C25 C26 C27 121.2(3) . . ?
C26 C27 C28 117.3(3) . . ?
C27 C28 C23 120.2(3) . . ?
C27 C28 C29 133.3(3) . . ?
C23 C28 C29 106.5(3) . . ?
C34 C29 C30 119.6(3) . . ?
C34 C29 C28 107.2(3) . . ?
C30 C29 C28 133.3(3) . . ?
C31 C30 C29 118.1(3) . . ?
C30 C31 O7 124.7(3) . . ?
C30 C31 C32 121.4(3) . . ?
O7 C31 C32 113.9(3) . . ?
C33 C32 C31 121.3(3) . . ?
C32 C33 C34 117.3(3) . . ?
O1 C35 C366 113.7(15) . . ?
O1 C35 C36 105.4(4) . . ?
C366 C35 C36 28.8(13) . . ?
C366 C36 O22 133(4) . . ?
C366 C36 O2 62(3) . . ?
O22 C36 O2 71.4(16) . . ?
C366 C36 C35 74(3) . . ?
O22 C36 C35 126.2(16) . . ?
O2 C36 C35 108.5(5) . . ?
O2 C37 O22 49.5(6) . . ?
O3 C38 C39 106.7(3) . . ?
O4 C39 C38 107.9(3) . . ?
O5 C41 C42 113.6(3) . . ?
O6 C42 C41 115.8(3) . . ?
O7 C44 C45 108.1(3) . . ?
O8 C45 C44 109.8(3) . . ?
C11 N3 C22 107.8(3) . . ?
C11 N3 C5 124.0(3) . . ?
C22 N3 C5 128.1(3) . . ?
C23 N4 C34 108.1(3) . . ?
C23 N4 C10 126.2(3) . . ?
C34 N4 C10 125.0(3) . . ?
C26 O5 C41 120.6(3) . . ?
C31 O7 C44 117.4(3) . . ?
N1 C1 C10 127.0(3) . 3_656 ?
N1 C1 C2 107.2(3) . . ?
C10 C1 C2 125.8(3) 3_656 . ?
N2 C6 C5 123.6(3) . . ?
N2 C6 C7 110.9(3) . . ?
C5 C6 C7 125.4(3) . . ?
N2 C9 C10 125.1(3) . . ?
N2 C9 C8 111.6(3) . . ?
C10 C9 C8 123.1(3) . . ?
C33 C34 C29 122.2(3) . . ?
C33 C34 N4 128.6(3) . . ?
C29 C34 N4 109.1(3) . . ?
C36 O22 O2 73.0(16) . . ?
C36 O22 C366 21.8(19) . . ?
O2 O22 C366 51.2(16) . . ?
C36 O22 C37 116(2) . . ?
O2 O22 C37 51.6(8) . . ?
C366 O22 C37 96.5(18) . . ?
C36 C366 O2 86(4) . . ?
C36 C366 O22 25(2) . . ?
O2 C366 O22 60.9(18) . . ?
C36 C366 C35 77(3) . . ?
O2 C366 C35 120(2) . . ?
O22 C366 C35 92(2) . . ?
C24 C25 C26 122.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.0(4) . . . . ?
C1 N1 C4 C5 -175.7(3) . . . . ?
C1 N1 C4 C3 1.5(4) . . . . ?
C2 C3 C4 N1 -0.2(4) . . . . ?
C2 C3 C4 C5 176.9(3) . . . . ?
N1 C4 C5 C6 -3.5(5) . . . . ?
C3 C4 C5 C6 179.9(3) . . . . ?
N1 C4 C5 N3 170.2(3) . . . . ?
C3 C4 C5 N3 -6.5(5) . . . . ?
C6 C7 C8 C9 -0.4(3) . . . . ?
C12 C11 C16 C15 -2.0(5) . . . . ?
N3 C11 C16 C15 179.1(3) . . . . ?
C12 C11 C16 C17 178.6(3) . . . . ?
N3 C11 C16 C17 -0.4(4) . . . . ?
C15 C16 C17 C18 2.5(7) . . . . ?
C11 C16 C17 C18 -178.2(4) . . . . ?
C15 C16 C17 C22 -179.7(4) . . . . ?
C11 C16 C17 C22 -0.3(4) . . . . ?
C14 C13 C12 C11 -0.2(5) . . . . ?
N3 C11 C12 C13 180.0(3) . . . . ?
C16 C11 C12 C13 1.2(5) . . . . ?
C12 C13 C14 O3 -179.5(3) . . . . ?
C12 C13 C14 C15 -0.1(6) . . . . ?
C38 O3 C14 C13 -149.4(3) . . . . ?
C38 O3 C14 C15 31.3(5) . . . . ?
C22 C17 C18 C19 -2.0(5) . . . . ?
C16 C17 C18 C19 175.6(4) . . . . ?
C17 C18 C19 O1 -174.9(4) . . . . ?
C17 C18 C19 C20 3.0(6) . . . . ?
C35 O1 C19 C18 -10.0(7) . . . . ?
C35 O1 C19 C20 172.0(4) . . . . ?
C18 C19 C20 C21 -2.4(7) . . . . ?
O1 C19 C20 C21 175.7(4) . . . . ?
C19 C20 C21 C22 0.7(6) . . . . ?
C20 C21 C22 N3 -178.2(4) . . . . ?
C20 C21 C22 C17 0.3(5) . . . . ?
C18 C17 C22 C21 0.4(5) . . . . ?
C16 C17 C22 C21 -177.8(3) . . . . ?
C18 C17 C22 N3 179.1(3) . . . . ?
C16 C17 C22 N3 1.0(4) . . . . ?
N4 C23 C24 C25 -177.7(3) . . . . ?
C28 C23 C24 C25 1.3(5) . . . . ?
C13 C14 C15 C16 -0.6(5) . . . . ?
O3 C14 C15 C16 178.7(3) . . . . ?
C11 C16 C15 C14 1.6(5) . . . . ?
C17 C16 C15 C14 -179.1(3) . . . . ?
O5 C26 C27 C28 179.0(3) . . . . ?
C25 C26 C27 C28 -0.1(5) . . . . ?
C26 C27 C28 C23 -0.2(5) . . . . ?
C26 C27 C28 C29 178.4(3) . . . . ?
C24 C23 C28 C27 -0.4(5) . . . . ?
N4 C23 C28 C27 178.7(3) . . . . ?
C24 C23 C28 C29 -179.4(3) . . . . ?
N4 C23 C28 C29 -0.2(4) . . . . ?
C27 C28 C29 C34 -178.6(4) . . . . ?
C23 C28 C29 C34 0.1(4) . . . . ?
C27 C28 C29 C30 0.7(6) . . . . ?
C23 C28 C29 C30 179.5(3) . . . . ?
C34 C29 C30 C31 0.3(5) . . . . ?
C28 C29 C30 C31 -179.0(3) . . . . ?
C29 C30 C31 O7 -177.7(3) . . . . ?
C29 C30 C31 C32 1.1(5) . . . . ?
C30 C31 C32 C33 -1.0(5) . . . . ?
O7 C31 C32 C33 178.0(3) . . . . ?
C31 C32 C33 C34 -0.7(5) . . . . ?
C19 O1 C35 C366 -160.7(16) . . . . ?
C19 O1 C35 C36 169.9(5) . . . . ?
O22 O2 C36 C366 178(3) . . . . ?
C37 O2 C36 C366 143(3) . . . . ?
C366 O2 C36 O22 -178(3) . . . . ?
C37 O2 C36 O22 -34.7(15) . . . . ?
C366 O2 C36 C35 59(3) . . . . ?
O22 O2 C36 C35 -123.0(16) . . . . ?
C37 O2 C36 C35 -157.7(5) . . . . ?
O1 C35 C36 C366 111(3) . . . . ?
O1 C35 C36 O22 -21(2) . . . . ?
C366 C35 C36 O22 -132(4) . . . . ?
O1 C35 C36 O2 59.3(7) . . . . ?
C366 C35 C36 O2 -52(3) . . . . ?
C366 O2 C37 O22 46(2) . . . . ?
C36 O2 C37 O22 19.7(9) . . . . ?
C14 O3 C38 C39 157.7(3) . . . . ?
C40 O4 C39 C38 174.3(3) . . . . ?
O3 C38 C39 O4 -70.2(4) . . . . ?
C43 O6 C42 C41 -83.8(5) . . . . ?
O5 C41 C42 O6 78.1(4) . . . . ?
C46 O8 C45 C44 -178.7(4) . . . . ?
O7 C44 C45 O8 64.5(4) . . . . ?
C12 C11 N3 C22 -177.9(3) . . . . ?
C16 C11 N3 C22 1.0(4) . . . . ?
C12 C11 N3 C5 -2.2(5) . . . . ?
C16 C11 N3 C5 176.7(3) . . . . ?
C21 C22 N3 C11 177.4(3) . . . . ?
C17 C22 N3 C11 -1.2(4) . . . . ?
C21 C22 N3 C5 1.9(6) . . . . ?
C17 C22 N3 C5 -176.7(3) . . . . ?
C4 C5 N3 C11 -84.0(4) . . . . ?
C6 C5 N3 C11 90.4(4) . . . . ?
C4 C5 N3 C22 90.9(4) . . . . ?
C6 C5 N3 C22 -94.8(4) . . . . ?
C24 C23 N4 C34 179.3(3) . . . . ?
C28 C23 N4 C34 0.2(4) . . . . ?
C24 C23 N4 C10 -9.3(5) . . . . ?
C28 C23 N4 C10 171.7(3) . . . . ?
C1 C10 N4 C23 -105.9(4) 3_656 . . . ?
C9 C10 N4 C23 74.1(4) . . . . ?
C1 C10 N4 C34 64.1(4) 3_656 . . . ?
C9 C10 N4 C34 -115.9(3) . . . . ?
C25 C26 O5 C41 -174.3(3) . . . . ?
C27 C26 O5 C41 6.5(5) . . . . ?
C42 C41 O5 C26 81.3(4) . . . . ?
C30 C31 O7 C44 5.8(5) . . . . ?
C32 C31 O7 C44 -173.1(3) . . . . ?
C45 C44 O7 C31 175.8(3) . . . . ?
C4 N1 C1 C10 176.4(3) . . . 3_656 ?
C4 N1 C1 C2 -2.2(4) . . . . ?
C3 C2 C1 N1 2.0(4) . . . . ?
C3 C2 C1 C10 -176.6(3) . . . 3_656 ?
C9 N2 C6 C5 175.3(3) . . . . ?
C9 N2 C6 C7 -1.9(3) . . . . ?
C4 C5 C6 N2 2.6(5) . . . . ?
N3 C5 C6 N2 -171.0(3) . . . . ?
C4 C5 C6 C7 179.3(3) . . . . ?
N3 C5 C6 C7 5.8(4) . . . . ?
C8 C7 C6 N2 1.5(4) . . . . ?
C8 C7 C6 C5 -175.6(3) . . . . ?
C6 N2 C9 C10 -173.0(3) . . . . ?
C6 N2 C9 C8 1.6(3) . . . . ?
C1 C10 C9 N2 -0.5(5) 3_656 . . . ?
N4 C10 C9 N2 179.5(3) . . . . ?
C1 C10 C9 C8 -174.6(3) 3_656 . . . ?
N4 C10 C9 C8 5.4(4) . . . . ?
C7 C8 C9 N2 -0.8(4) . . . . ?
C7 C8 C9 C10 174.0(3) . . . . ?
C32 C33 C34 C29 2.2(5) . . . . ?
C32 C33 C34 N4 179.0(3) . . . . ?
C30 C29 C34 C33 -2.0(5) . . . . ?
C28 C29 C34 C33 177.4(3) . . . . ?
C30 C29 C34 N4 -179.4(3) . . . . ?
C28 C29 C34 N4 0.0(4) . . . . ?
C23 N4 C34 C33 -177.4(3) . . . . ?
C10 N4 C34 C33 11.1(5) . . . . ?
C23 N4 C34 C29 -0.2(3) . . . . ?
C10 N4 C34 C29 -171.7(3) . . . . ?
C366 C36 O22 O2 -3(4) . . . . ?
C35 C36 O22 O2 99.7(15) . . . . ?
O2 C36 O22 C366 3(4) . . . . ?
C35 C36 O22 C366 103(4) . . . . ?
C366 C36 O22 C37 26(5) . . . . ?
O2 C36 O22 C37 28.8(11) . . . . ?
C35 C36 O22 C37 128.5(14) . . . . ?
C366 O2 O22 C36 1.3(19) . . . . ?
C37 O2 O22 C36 146.6(14) . . . . ?
C36 O2 O22 C366 -1.3(19) . . . . ?
C37 O2 O22 C366 145.3(18) . . . . ?
C366 O2 O22 C37 -145.3(18) . . . . ?
C36 O2 O22 C37 -146.6(14) . . . . ?
O2 C37 O22 C36 -35.9(15) . . . . ?
O2 C37 O22 C366 -26.5(14) . . . . ?
O22 C36 C366 O2 3(4) . . . . ?
C35 C36 C366 O2 -121.9(18) . . . . ?
O2 C36 C366 O22 -3(4) . . . . ?
C35 C36 C366 O22 -125(3) . . . . ?
O22 C36 C366 C35 125(3) . . . . ?
O2 C36 C366 C35 121.9(18) . . . . ?
O22 O2 C366 C36 -1(2) . . . . ?
C37 O2 C366 C36 -51(4) . . . . ?
C36 O2 C366 O22 1(2) . . . . ?
C37 O2 C366 O22 -49(2) . . . . ?
O22 O2 C366 C35 -74(3) . . . . ?
C36 O2 C366 C35 -73(3) . . . . ?
C37 O2 C366 C35 -123(2) . . . . ?
O2 O22 C366 C36 177(5) . . . . ?
C37 O22 C366 C36 -157(4) . . . . ?
C36 O22 C366 O2 -177(5) . . . . ?
C37 O22 C366 O2 26.7(13) . . . . ?
C36 O22 C366 C35 -53(4) . . . . ?
O2 O22 C366 C35 123(2) . . . . ?
C37 O22 C366 C35 150.1(15) . . . . ?
O1 C35 C366 C36 -79(3) . . . . ?
O1 C35 C366 O2 -1(4) . . . . ?
C36 C35 C366 O2 78(4) . . . . ?
O1 C35 C366 O22 -58(2) . . . . ?
C36 C35 C366 O22 20.3(19) . . . . ?
C23 C24 C25 C26 -1.6(5) . . . . ?
O5 C26 C25 C24 -178.2(3) . . . . ?
C27 C26 C25 C24 1.1(5) . . . . ?

_refine_diff_density_max         0.721
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.066



####################################################################### 
# 
# 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_shelxl_sq
_database_code_depnum_ccdc_archive 'CCDC 1868761'
loop_
_audit_author_name
_audit_author_address
'Shin-ichiro Kawano'
;Nagoya University
Japan
;
_audit_update_record             
;
2019-02-05 deposited with the CCDC.	2019-02-13 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         ?
_chemical_formula_sum            'C96 H92 F12 N8 O28 S4'
_chemical_formula_weight         2162.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1222 0.1213 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           213
_space_group_name_H-M_alt        'P 41 3 2'
_space_group_name_Hall           'P 4bd 2ab 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/4, -z+1/4, y+3/4'
'x+3/4, z+1/4, -y+1/4'
'z+3/4, y+1/4, -x+1/4'
'y+1/2, -z+1/2, -x'
'-z, x+1/2, -y+1/2'
'z+1/4, -y+1/4, x+3/4'
'y+1/4, -x+1/4, z+3/4'
'-z+1/2, -x, y+1/2'
'x+1/2, -y+1/2, -z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x, y+1/2, -z+1/2'
'-y+1/2, -z, x+1/2'
'-x+1/2, -y, z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'-y, z+1/2, -x+1/2'
'-x+3/4, -z+3/4, -y+3/4'
'-z+3/4, -y+3/4, -x+3/4'
'z+1/2, -x+1/2, -y'
'z, x, y'
'y+3/4, x+1/4, -z+1/4'
'y, z, x'
'-z+1/4, y+3/4, x+1/4'

_cell_length_a                   33.668(2)
_cell_length_b                   33.668(2)
_cell_length_c                   33.668(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     38164(7)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    166991
_cell_measurement_theta_min      0.84
_cell_measurement_theta_max      27.20

_exptl_crystal_description       cubic
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_F_000             13440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.149
_shelx_estimated_absorpt_T_min   0.971
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7015
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            250749
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         0.844
_diffrn_reflns_theta_max         27.084
_diffrn_reflns_theta_full        24.891
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14618
_reflns_number_gt                10864
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3813 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.122(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         14618
_refine_ls_number_parameters     645
_refine_ls_number_restraints     204
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.1133
_refine_ls_wR_factor_ref         0.3369
_refine_ls_wR_factor_gt          0.3122
_refine_ls_goodness_of_fit_ref   1.349
_refine_ls_restrained_S_all      1.414
_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 0.76957(13) 0.58779(13) 0.51444(13) 0.0295(9) Uani 1 1 d . . . . .
C2 C 0.79320(16) 0.55321(16) 0.51473(15) 0.0377(11) Uani 1 1 d . . . . .
H1 H 0.8183 0.5503 0.5274 0.045 Uiso 1 1 calc R U . . .
C3 C 0.77350(16) 0.52457(15) 0.49351(15) 0.0364(10) Uani 1 1 d . . . . .
H2 H 0.7827 0.4985 0.4881 0.044 Uiso 1 1 calc R U . . .
C4 C 0.73667(15) 0.54134(14) 0.48114(14) 0.0333(10) Uani 1 1 d . . . . .
C5 C 0.70777(15) 0.52253(14) 0.45772(14) 0.0325(9) Uani 1 1 d . . . . .
C6 C 0.67751(17) 0.54116(16) 0.43560(15) 0.0395(11) Uani 1 1 d . . . . .
C7 C 0.64429(17) 0.52374(18) 0.41820(16) 0.0434(12) Uani 1 1 d . . . . .
H53 H 0.6368 0.4966 0.4206 0.052 Uiso 1 1 calc R U . . .
C8 C 0.62452(17) 0.55158(18) 0.39752(17) 0.0448(13) Uani 1 1 d . . . . .
H4 H 0.6009 0.5477 0.3826 0.054 Uiso 1 1 calc R U . . .
C9 C 0.64519(16) 0.58761(17) 0.40211(15) 0.0412(12) Uani 1 1 d . . . . .
C10 C 0.63595(14) 0.6250 0.38595(14) 0.0423(17) Uani 1 2 d S T P . .
C11 C 0.77980(13) 0.6250 0.52980(13) 0.0313(13) Uani 1 2 d S T P . .
C12 C 0.84811(14) 0.63987(16) 0.55484(14) 0.0345(10) Uani 1 1 d . . . . .
C13 C 0.86864(14) 0.63456(16) 0.59137(14) 0.0350(10) Uani 1 1 d . . . . .
C14 C 0.90793(16) 0.64486(17) 0.59381(16) 0.0421(12) Uani 1 1 d . . . . .
H8 H 0.9220 0.6412 0.6180 0.051 Uiso 1 1 calc R U . . .
C15 C 0.92704(15) 0.66054(19) 0.56126(16) 0.0448(13) Uani 1 1 d . . . . .
C16 C 0.90496(17) 0.66692(19) 0.52546(17) 0.0468(13) Uani 1 1 d . . . . .
H9 H 0.9177 0.6787 0.5032 0.056 Uiso 1 1 calc R U . . .
C17 C 0.86616(17) 0.65638(18) 0.52290(17) 0.0452(13) Uani 1 1 d . . . . .
H10 H 0.8518 0.6605 0.4990 0.054 Uiso 1 1 calc R U . . .
C18 C 0.6127(3) 0.6254(3) 0.3157(3) 0.0756(17) Uani 1 1 d . U . . .
C19 C 0.5759(3) 0.6254(4) 0.2954(3) 0.093(2) Uani 1 1 d . U . . .
C20 C 0.5764(4) 0.6257(4) 0.2537(4) 0.110(3) Uani 1 1 d . U . . .
H5 H 0.5520 0.6272 0.2397 0.132 Uiso 1 1 calc R U . . .
C21 C 0.6058(5) 0.6242(5) 0.2358(5) 0.122(4) Uani 1 1 d . U . . .
C22 C 0.6454(4) 0.6291(4) 0.2537(3) 0.101(3) Uani 1 1 d . U . . .
H6 H 0.6685 0.6318 0.2377 0.121 Uiso 1 1 calc R U . . .
C23 C 0.6475(3) 0.6295(3) 0.2942(3) 0.086(2) Uani 1 1 d . U . . .
H7 H 0.6723 0.6325 0.3074 0.103 Uiso 1 1 calc R U . . .
C24 C 0.71391(18) 0.45214(16) 0.48362(15) 0.0413(12) Uani 1 1 d . . . . .
C25 C 0.7064(2) 0.45594(16) 0.52422(16) 0.0451(13) Uani 1 1 d . . . . .
H15 H 0.6987 0.4806 0.5357 0.054 Uiso 1 1 calc R U . . .
C26 C 0.7106(3) 0.4223(2) 0.5466(2) 0.0618(19) Uani 1 1 d . . . . .
H16 H 0.7068 0.4239 0.5745 0.074 Uiso 1 1 calc R U . . .
C27 C 0.7204(3) 0.38563(19) 0.5297(2) 0.072(2) Uani 1 1 d . . . . .
C28 C 0.7281(3) 0.38183(18) 0.4895(2) 0.063(2) Uani 1 1 d . . . . .
H17 H 0.7360 0.3572 0.4784 0.076 Uiso 1 1 calc R U . . .
C29 C 0.7238(2) 0.41560(18) 0.46614(16) 0.0503(15) Uani 1 1 d . . . . .
C30 C 0.7305(2) 0.42311(17) 0.42410(16) 0.0481(14) Uani 1 1 d . . . . .
C31 C 0.7455(2) 0.39764(17) 0.39483(19) 0.0523(15) Uani 1 1 d . . . . .
H18 H 0.7518 0.3707 0.4003 0.063 Uiso 1 1 calc R U . . .
C32 C 0.75073(19) 0.41408(18) 0.35767(17) 0.0485(14) Uani 1 1 d . . . . .
C33 C 0.7411(2) 0.45464(19) 0.35007(18) 0.0523(15) Uani 1 1 d . . . . .
H19 H 0.7439 0.4650 0.3240 0.051(18) Uiso 1 1 calc R . . . .
C34 C 0.72795(19) 0.47907(17) 0.38020(16) 0.0445(12) Uani 1 1 d . . . . .
H20 H 0.7230 0.5065 0.3756 0.053 Uiso 1 1 calc R U . . .
C35 C 0.72217(18) 0.46256(17) 0.41733(15) 0.0407(12) Uani 1 1 d . . . . .
C36 C 0.9892(2) 0.6666(3) 0.5949(3) 0.077(3) Uani 1 1 d . . . . .
H11 H 0.9886 0.6385 0.6034 0.092 Uiso 1 1 calc R U . . .
H12 H 0.9790 0.6833 0.6168 0.092 Uiso 1 1 calc R U . . .
C37 C 1.0304(2) 0.6787(3) 0.5841(2) 0.076(3) Uani 1 1 d . . . . .
H13 H 1.0420 0.6599 0.5647 0.091 Uiso 1 1 calc R U . . .
H14 H 1.0306 0.7057 0.5725 0.091 Uiso 1 1 calc R U . . .
C38 C 1.0936(3) 0.6889(4) 0.6142(3) 0.106(4) Uani 1 1 d . . . . .
H21 H 1.1045 0.6735 0.5920 0.158 Uiso 1 1 calc R U . . .
H22 H 1.1089 0.6834 0.6383 0.158 Uiso 1 1 calc R U . . .
H23 H 1.0953 0.7173 0.6080 0.158 Uiso 1 1 calc R U . . .
C39 C 0.5739(8) 0.6034(9) 0.1736(7) 0.214(8) Uani 1 1 d D U . . .
H41 H 0.5667 0.5779 0.1863 0.257 Uiso 1 1 calc R U . . .
H42 H 0.5523 0.6227 0.1784 0.257 Uiso 1 1 calc R U . . .
C40 C 0.5800(9) 0.5974(7) 0.1282(7) 0.232(9) Uani 1 1 d D U . . .
H51 H 0.5997 0.5765 0.1216 0.279 Uiso 1 1 calc R U . . .
H52 H 0.5550 0.5933 0.1134 0.279 Uiso 1 1 calc R U . . .
C41 C 0.5678(13) 0.6633(9) 0.1070(12) 0.332(16) Uani 1 1 d D U . . .
H56 H 0.5799 0.6897 0.1058 0.498 Uiso 1 1 calc R U . . .
H57 H 0.5616 0.6542 0.0800 0.498 Uiso 1 1 calc R U . . .
H58 H 0.5433 0.6645 0.1227 0.498 Uiso 1 1 calc R U . . .
C42 C 0.7759(3) 0.3533(2) 0.3318(3) 0.086(3) Uani 1 1 d . . . . .
H54 H 0.7934 0.3523 0.3553 0.104 Uiso 1 1 calc R U . . .
H55 H 0.7520 0.3373 0.3378 0.104 Uiso 1 1 calc R U . . .
C43 C 0.7961(3) 0.3358(3) 0.2990(3) 0.092(3) Uani 1 1 d D U . . .
H33 H 0.8167 0.3543 0.2891 0.110 Uiso 1 1 calc R U . . .
H34 H 0.8095 0.3111 0.3077 0.110 Uiso 1 1 calc R U . . .
C44 C 0.7598(6) 0.3577(5) 0.2428(5) 0.174(6) Uani 1 1 d D U . . .
H48 H 0.7557 0.3821 0.2581 0.262 Uiso 1 1 calc R U . . .
H49 H 0.7353 0.3510 0.2285 0.262 Uiso 1 1 calc R U . . .
H50 H 0.7814 0.3616 0.2238 0.262 Uiso 1 1 calc R U . . .
C45 C 0.7324(4) 0.3153(3) 0.5399(3) 0.090(3) Uani 1 1 d . U . . .
H24 H 0.7173 0.3103 0.5152 0.108 Uiso 1 1 calc R U . . .
H25 H 0.7611 0.3145 0.5334 0.108 Uiso 1 1 calc R U . . .
C46 C 0.7235(5) 0.2861(5) 0.5682(4) 0.130(4) Uani 1 1 d D U . . .
H26 H 0.7257 0.2591 0.5567 0.156 Uiso 1 1 calc R U . . .
H27 H 0.6964 0.2898 0.5790 0.156 Uiso 1 1 calc R U . . .
C47 C 0.7407(6) 0.2683(7) 0.6322(5) 0.181(7) Uani 1 1 d D U . . .
H28 H 0.7637 0.2534 0.6419 0.272 Uiso 1 1 calc R U . . .
H29 H 0.7197 0.2498 0.6244 0.272 Uiso 1 1 calc R U . . .
H30 H 0.7309 0.2859 0.6532 0.272 Uiso 1 1 calc R U . . .
C48 C 0.8014(3) 0.5881(3) 0.3733(3) 0.081(3) Uani 1 1 d . . . . .
C49 C 0.7556(4) 0.2627(5) 0.4205(5) 0.144(5) Uani 1 1 d D U . . .
O1 O 1.05185(17) 0.6779(3) 0.6205(2) 0.102(3) Uani 1 1 d . . . . .
N1 N 0.73490(11) 0.57923(12) 0.49410(11) 0.0299(8) Uani 1 1 d . . . . .
H39 H 0.7150 0.5957 0.4903 0.036 Uiso 1 1 calc R U . . .
N2 N 0.67723(13) 0.58020(13) 0.42605(12) 0.0373(9) Uani 1 1 d . . . . .
H40 H 0.6948 0.5979 0.4339 0.045 Uiso 1 1 calc R U . . .
N3 N 0.80946(11) 0.6250 0.55946(11) 0.0350(13) Uani 1 2 d S T P . .
N4 N 0.71092(15) 0.48095(12) 0.45308(12) 0.0389(10) Uani 1 1 d . . . . .
N5 N 0.60552(14) 0.6250 0.35552(14) 0.0565(19) Uani 1 2 d S T P . .
S1 S 0.75818(5) 0.62014(6) 0.37502(5) 0.0588(5) Uani 1 1 d . . . . .
F1 F 0.81063(18) 0.5790(2) 0.3366(2) 0.111(2) Uani 1 1 d . . . . .
F4 F 0.7530(9) 0.2234(6) 0.4100(10) 0.368(14) Uiso 1 1 d D . . . .
F3 F 0.83058(16) 0.6018(3) 0.3924(3) 0.133(3) Uani 1 1 d . . . . .
F2 F 0.7894(3) 0.5542(2) 0.3927(3) 0.157(4) Uani 1 1 d . . . . .
O2 O 0.96579(12) 0.67205(16) 0.56001(13) 0.0552(12) Uani 1 1 d . . . . .
O3 O 0.76402(19) 0.39372(14) 0.32518(14) 0.0707(16) Uani 1 1 d . . . . .
O4 O 0.7694(3) 0.3271(3) 0.2684(3) 0.139(3) Uani 1 1 d D U . . .
O5 O 0.7219(2) 0.35444(14) 0.55618(16) 0.090(2) Uani 1 1 d . . . . .
O6 O 0.7525(4) 0.2922(4) 0.5977(4) 0.170(4) Uani 1 1 d D U . . .
O7 O 0.7743(3) 0.6559(2) 0.3579(3) 0.134(4) Uani 1 1 d . . . . .
O17 O 0.8191(8) 0.2785(8) 0.3874(5) 0.291(11) Uiso 1 1 d D . . . .
O9 O 0.74988(11) 0.62246(12) 0.41733(10) 0.0401(8) Uani 1 1 d . . . . .
O11 O 0.6139(4) 0.6194(4) 0.1914(4) 0.168(4) Uani 1 1 d . U . . .
O12 O 0.7297(2) 0.6034(3) 0.3516(2) 0.124(3) Uani 1 1 d . . . . .
O16 O 0.5950(7) 0.6359(8) 0.1253(8) 0.296(10) Uani 1 1 d D U . . .
O18 O 0.7980(6) 0.3233(4) 0.4280(8) 0.297(11) Uiso 1 1 d D . . . .
S2 S 0.8045(2) 0.28051(17) 0.4262(2) 0.192(2) Uani 1 1 d D U . . .
O19 O 0.8224(8) 0.2551(12) 0.4556(12) 0.50(3) Uiso 1 1 d D . . . .
F5 F 0.7356(6) 0.2823(9) 0.3958(10) 0.58(3) Uiso 1 1 d D . . . .
F6 F 0.7383(7) 0.2630(12) 0.4566(7) 0.64(3) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.384(6) . ?
C1 C11 1.398(5) . ?
C1 C2 1.410(7) . ?
C2 C3 1.371(8) . ?
C2 H1 0.9500 . ?
C3 C4 1.425(7) . ?
C3 H2 0.9500 . ?
C4 N1 1.350(6) . ?
C4 C5 1.404(7) . ?
C5 C6 1.409(8) . ?
C5 N4 1.413(6) . ?
C6 N2 1.353(7) . ?
C6 C7 1.392(8) . ?
C7 C8 1.344(9) . ?
C7 H53 0.9500 . ?
C8 C9 1.407(8) . ?
C8 H4 0.9500 . ?
C9 N2 1.370(7) . ?
C9 C10 1.406(7) . ?
C10 C9 1.406(7) 7_564 ?
C10 N5 1.449(9) . ?
C11 C1 1.398(5) 7_564 ?
C11 N3 1.412(8) . ?
C12 C17 1.355(7) . ?
C12 N3 1.403(5) . ?
C12 C13 1.422(7) . ?
C13 C14 1.370(7) . ?
C13 C13 1.449(9) 7_564 ?
C14 C15 1.376(7) . ?
C14 H8 0.9500 . ?
C15 O2 1.362(6) . ?
C15 C16 1.432(8) . ?
C16 C17 1.356(8) . ?
C16 H9 0.9500 . ?
C17 H10 0.9500 . ?
C18 N5 1.364(10) . ?
C18 C23 1.384(14) . ?
C18 C19 1.416(12) . ?
C19 C20 1.403(16) . ?
C19 C19 1.45(2) 7_564 ?
C20 C21 1.159(19) . ?
C20 H5 0.9500 . ?
C21 C22 1.472(19) . ?
C21 O11 1.53(2) . ?
C22 C23 1.366(14) . ?
C22 H6 0.9500 . ?
C23 H7 0.9500 . ?
C24 C25 1.396(7) . ?
C24 C29 1.404(8) . ?
C24 N4 1.417(7) . ?
C25 C26 1.368(8) . ?
C25 H15 0.9500 . ?
C26 C27 1.399(9) . ?
C26 H16 0.9500 . ?
C27 O5 1.379(8) . ?
C27 C28 1.383(10) . ?
C28 C29 1.391(9) . ?
C28 H17 0.9500 . ?
C29 C30 1.455(7) . ?
C30 C35 1.376(9) . ?
C30 C31 1.401(7) . ?
C31 C32 1.379(9) . ?
C31 H18 0.9500 . ?
C32 O3 1.366(6) . ?
C32 C33 1.426(10) . ?
C33 C34 1.379(8) . ?
C33 H19 0.9500 . ?
C34 C35 1.382(8) . ?
C34 H20 0.9500 . ?
C35 N4 1.405(6) . ?
C36 O2 1.426(8) . ?
C36 C37 1.488(9) . ?
C36 H11 0.9900 . ?
C36 H12 0.9900 . ?
C37 O1 1.423(9) . ?
C37 H13 0.9900 . ?
C37 H14 0.9900 . ?
C38 O1 1.470(10) . ?
C38 H21 0.9800 . ?
C38 H22 0.9800 . ?
C38 H23 0.9800 . ?
C39 C40 1.553(13) . ?
C39 O11 1.57(3) . ?
C39 H41 0.9900 . ?
C39 H42 0.9900 . ?
C40 O16 1.395(13) . ?
C40 H51 0.9900 . ?
C40 H52 0.9900 . ?
C41 O16 1.439(13) . ?
C41 H56 0.9800 . ?
C41 H57 0.9800 . ?
C41 H58 0.9800 . ?
C42 C43 1.425(12) . ?
C42 O3 1.436(10) . ?
C42 H54 0.9900 . ?
C42 H55 0.9900 . ?
C43 O4 1.400(10) . ?
C43 H33 0.9900 . ?
C43 H34 0.9900 . ?
C44 O4 1.381(11) . ?
C44 H48 0.9800 . ?
C44 H49 0.9800 . ?
C44 H50 0.9800 . ?
C45 C46 1.401(17) . ?
C45 O5 1.472(10) . ?
C45 H24 0.9900 . ?
C45 H25 0.9900 . ?
C46 O6 1.408(11) . ?
C46 H26 0.9900 . ?
C46 H27 0.9900 . ?
C47 O6 1.467(11) . ?
C47 H28 0.9800 . ?
C47 H29 0.9800 . ?
C47 H30 0.9800 . ?
C48 F3 1.262(12) . ?
C48 F1 1.313(10) . ?
C48 F2 1.374(12) . ?
C48 S1 1.812(9) . ?
C49 F5 1.26(2) . ?
C49 F6 1.347(13) . ?
C49 F4 1.372(13) . ?
C49 S2 1.764(11) . ?
N1 H39 0.8800 . ?
N2 H40 0.8800 . ?
N3 C12 1.403(5) 7_564 ?
N5 C18 1.364(10) 7_564 ?
S1 O12 1.364(7) . ?
S1 O7 1.439(8) . ?
S1 O9 1.454(4) . ?
O17 S2 1.396(13) . ?
O18 S2 1.459(12) . ?
S2 O19 1.443(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C11 125.3(4) . . ?
N1 C1 C2 107.9(4) . . ?
C11 C1 C2 126.7(5) . . ?
C3 C2 C1 107.7(5) . . ?
C3 C2 H1 126.1 . . ?
C1 C2 H1 126.1 . . ?
C2 C3 C4 107.1(4) . . ?
C2 C3 H2 126.4 . . ?
C4 C3 H2 126.4 . . ?
N1 C4 C5 125.3(4) . . ?
N1 C4 C3 108.6(4) . . ?
C5 C4 C3 126.1(4) . . ?
C4 C5 C6 126.7(4) . . ?
C4 C5 N4 117.2(4) . . ?
C6 C5 N4 115.9(4) . . ?
N2 C6 C7 107.7(5) . . ?
N2 C6 C5 124.3(5) . . ?
C7 C6 C5 128.0(5) . . ?
C8 C7 C6 108.8(5) . . ?
C8 C7 H53 125.6 . . ?
C6 C7 H53 125.6 . . ?
C7 C8 C9 107.4(5) . . ?
C7 C8 H4 126.3 . . ?
C9 C8 H4 126.3 . . ?
N2 C9 C10 124.4(5) . . ?
N2 C9 C8 107.3(5) . . ?
C10 C9 C8 128.3(5) . . ?
C9 C10 C9 129.1(6) 7_564 . ?
C9 C10 N5 115.5(3) 7_564 . ?
C9 C10 N5 115.5(3) . . ?
C1 C11 C1 128.3(6) 7_564 . ?
C1 C11 N3 115.8(3) 7_564 . ?
C1 C11 N3 115.8(3) . . ?
C17 C12 N3 130.6(5) . . ?
C17 C12 C13 121.3(4) . . ?
N3 C12 C13 108.1(4) . . ?
C14 C13 C12 119.3(4) . . ?
C14 C13 C13 133.3(3) . 7_564 ?
C12 C13 C13 107.2(3) . 7_564 ?
C13 C14 C15 120.0(5) . . ?
C13 C14 H8 120.0 . . ?
C15 C14 H8 120.0 . . ?
O2 C15 C14 125.6(5) . . ?
O2 C15 C16 115.4(4) . . ?
C14 C15 C16 119.0(5) . . ?
C17 C16 C15 120.9(5) . . ?
C17 C16 H9 119.5 . . ?
C15 C16 H9 119.5 . . ?
C12 C17 C16 119.3(5) . . ?
C12 C17 H10 120.4 . . ?
C16 C17 H10 120.4 . . ?
N5 C18 C23 131.7(8) . . ?
N5 C18 C19 108.6(8) . . ?
C23 C18 C19 119.4(9) . . ?
C20 C19 C18 118.1(11) . . ?
C20 C19 C19 135.8(7) . 7_564 ?
C18 C19 C19 106.2(6) . 7_564 ?
C21 C20 C19 122.0(13) . . ?
C21 C20 H5 119.0 . . ?
C19 C20 H5 119.0 . . ?
C20 C21 C22 123.8(15) . . ?
C20 C21 O11 131.6(15) . . ?
C22 C21 O11 104.5(13) . . ?
C23 C22 C21 117.2(12) . . ?
C23 C22 H6 121.4 . . ?
C21 C22 H6 121.4 . . ?
C22 C23 C18 118.4(10) . . ?
C22 C23 H7 120.8 . . ?
C18 C23 H7 120.8 . . ?
C25 C24 C29 122.3(5) . . ?
C25 C24 N4 129.4(5) . . ?
C29 C24 N4 108.2(4) . . ?
C26 C25 C24 116.4(5) . . ?
C26 C25 H15 121.8 . . ?
C24 C25 H15 121.8 . . ?
C25 C26 C27 122.1(6) . . ?
C25 C26 H16 119.0 . . ?
C27 C26 H16 119.0 . . ?
O5 C27 C28 123.7(6) . . ?
O5 C27 C26 114.7(6) . . ?
C28 C27 C26 121.6(6) . . ?
C27 C28 C29 117.3(5) . . ?
C27 C28 H17 121.4 . . ?
C29 C28 H17 121.4 . . ?
C28 C29 C24 120.3(5) . . ?
C28 C29 C30 132.6(5) . . ?
C24 C29 C30 107.0(5) . . ?
C35 C30 C31 123.2(5) . . ?
C35 C30 C29 107.3(4) . . ?
C31 C30 C29 129.3(6) . . ?
C32 C31 C30 116.0(6) . . ?
C32 C31 H18 122.0 . . ?
C30 C31 H18 122.0 . . ?
O3 C32 C31 124.5(6) . . ?
O3 C32 C33 114.3(5) . . ?
C31 C32 C33 121.2(5) . . ?
C34 C33 C32 120.8(6) . . ?
C34 C33 H19 119.6 . . ?
C32 C33 H19 119.6 . . ?
C33 C34 C35 118.1(6) . . ?
C33 C34 H20 121.0 . . ?
C35 C34 H20 121.0 . . ?
C30 C35 C34 120.6(5) . . ?
C30 C35 N4 109.8(5) . . ?
C34 C35 N4 129.5(5) . . ?
O2 C36 C37 106.3(6) . . ?
O2 C36 H11 110.5 . . ?
C37 C36 H11 110.5 . . ?
O2 C36 H12 110.5 . . ?
C37 C36 H12 110.5 . . ?
H11 C36 H12 108.7 . . ?
O1 C37 C36 105.0(6) . . ?
O1 C37 H13 110.7 . . ?
C36 C37 H13 110.7 . . ?
O1 C37 H14 110.7 . . ?
C36 C37 H14 110.7 . . ?
H13 C37 H14 108.8 . . ?
O1 C38 H21 109.5 . . ?
O1 C38 H22 109.5 . . ?
H21 C38 H22 109.5 . . ?
O1 C38 H23 109.5 . . ?
H21 C38 H23 109.5 . . ?
H22 C38 H23 109.5 . . ?
C40 C39 O11 108(2) . . ?
C40 C39 H41 110.1 . . ?
O11 C39 H41 110.1 . . ?
C40 C39 H42 110.1 . . ?
O11 C39 H42 110.1 . . ?
H41 C39 H42 108.4 . . ?
O16 C40 C39 90(2) . . ?
O16 C40 H51 113.7 . . ?
C39 C40 H51 113.7 . . ?
O16 C40 H52 113.7 . . ?
C39 C40 H52 113.7 . . ?
H51 C40 H52 110.9 . . ?
O16 C41 H56 109.5 . . ?
O16 C41 H57 109.5 . . ?
H56 C41 H57 109.5 . . ?
O16 C41 H58 109.5 . . ?
H56 C41 H58 109.5 . . ?
H57 C41 H58 109.5 . . ?
C43 C42 O3 113.9(7) . . ?
C43 C42 H54 108.8 . . ?
O3 C42 H54 108.8 . . ?
C43 C42 H55 108.8 . . ?
O3 C42 H55 108.8 . . ?
H54 C42 H55 107.7 . . ?
O4 C43 C42 110.5(10) . . ?
O4 C43 H33 109.6 . . ?
C42 C43 H33 109.6 . . ?
O4 C43 H34 109.6 . . ?
C42 C43 H34 109.6 . . ?
H33 C43 H34 108.1 . . ?
O4 C44 H48 109.5 . . ?
O4 C44 H49 109.5 . . ?
H48 C44 H49 109.5 . . ?
O4 C44 H50 109.5 . . ?
H48 C44 H50 109.5 . . ?
H49 C44 H50 109.5 . . ?
C46 C45 O5 108.8(9) . . ?
C46 C45 H24 109.9 . . ?
O5 C45 H24 109.9 . . ?
C46 C45 H25 109.9 . . ?
O5 C45 H25 109.9 . . ?
H24 C45 H25 108.3 . . ?
C45 C46 O6 103.2(13) . . ?
C45 C46 H26 111.1 . . ?
O6 C46 H26 111.1 . . ?
C45 C46 H27 111.1 . . ?
O6 C46 H27 111.1 . . ?
H26 C46 H27 109.1 . . ?
O6 C47 H28 109.5 . . ?
O6 C47 H29 109.5 . . ?
H28 C47 H29 109.5 . . ?
O6 C47 H30 109.5 . . ?
H28 C47 H30 109.5 . . ?
H29 C47 H30 109.5 . . ?
F3 C48 F1 112.3(8) . . ?
F3 C48 F2 106.9(11) . . ?
F1 C48 F2 109.0(8) . . ?
F3 C48 S1 113.0(6) . . ?
F1 C48 S1 111.0(8) . . ?
F2 C48 S1 104.2(6) . . ?
F5 C49 F6 111.2(14) . . ?
F5 C49 F4 107.5(13) . . ?
F6 C49 F4 102.4(12) . . ?
F5 C49 S2 113.1(12) . . ?
F6 C49 S2 107.7(11) . . ?
F4 C49 S2 114.5(16) . . ?
C37 O1 C38 110.9(6) . . ?
C4 N1 C1 108.6(4) . . ?
C4 N1 H39 125.7 . . ?
C1 N1 H39 125.7 . . ?
C6 N2 C9 108.8(4) . . ?
C6 N2 H40 125.6 . . ?
C9 N2 H40 125.6 . . ?
C12 N3 C12 109.4(5) . 7_564 ?
C12 N3 C11 125.3(3) . . ?
C12 N3 C11 125.3(3) 7_564 . ?
C35 N4 C5 123.5(4) . . ?
C35 N4 C24 107.5(4) . . ?
C5 N4 C24 127.1(4) . . ?
C18 N5 C18 110.5(9) 7_564 . ?
C18 N5 C10 124.8(4) 7_564 . ?
C18 N5 C10 124.8(4) . . ?
O12 S1 O7 112.3(7) . . ?
O12 S1 O9 116.9(4) . . ?
O7 S1 O9 114.8(5) . . ?
O12 S1 C48 107.5(5) . . ?
O7 S1 C48 100.6(5) . . ?
O9 S1 C48 102.5(4) . . ?
C15 O2 C36 117.9(5) . . ?
C32 O3 C42 116.3(6) . . ?
C44 O4 C43 116.9(10) . . ?
C27 O5 C45 116.7(6) . . ?
C46 O6 C47 106.9(10) . . ?
C21 O11 C39 104.9(14) . . ?
C40 O16 C41 113.2(14) . . ?
O17 S2 O19 118(2) . . ?
O17 S2 O18 98.1(16) . . ?
O19 S2 O18 128(2) . . ?
O17 S2 C49 102.3(14) . . ?
O19 S2 C49 105.2(10) . . ?
O18 S2 C49 101.5(9) . . ?

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
N1 C1 C2 C3 2.1(5) . . . . ?
C11 C1 C2 C3 -174.5(4) . . . . ?
C1 C2 C3 C4 -1.9(6) . . . . ?
C2 C3 C4 N1 1.1(5) . . . . ?
C2 C3 C4 C5 178.1(5) . . . . ?
N1 C4 C5 C6 16.8(8) . . . . ?
C3 C4 C5 C6 -159.8(5) . . . . ?
N1 C4 C5 N4 -168.6(4) . . . . ?
C3 C4 C5 N4 14.8(7) . . . . ?
C4 C5 C6 N2 16.3(8) . . . . ?
N4 C5 C6 N2 -158.3(5) . . . . ?
C4 C5 C6 C7 -167.0(5) . . . . ?
N4 C5 C6 C7 18.4(8) . . . . ?
N2 C6 C7 C8 1.4(6) . . . . ?
C5 C6 C7 C8 -175.7(5) . . . . ?
C6 C7 C8 C9 -0.7(6) . . . . ?
C7 C8 C9 N2 -0.4(6) . . . . ?
C7 C8 C9 C10 179.8(5) . . . . ?
N2 C9 C10 C9 -11.4(4) . . . 7_564 ?
C8 C9 C10 C9 168.4(6) . . . 7_564 ?
N2 C9 C10 N5 168.6(4) . . . . ?
C8 C9 C10 N5 -11.6(6) . . . . ?
N1 C1 C11 C1 -19.0(3) . . . 7_564 ?
C2 C1 C11 C1 157.1(5) . . . 7_564 ?
N1 C1 C11 N3 161.0(3) . . . . ?
C2 C1 C11 N3 -22.9(5) . . . . ?
C17 C12 C13 C14 -2.7(9) . . . . ?
N3 C12 C13 C14 176.5(5) . . . . ?
C17 C12 C13 C13 -178.6(6) . . . 7_564 ?
N3 C12 C13 C13 0.6(7) . . . 7_564 ?
C12 C13 C14 C15 0.7(9) . . . . ?
C13 C13 C14 C15 175.3(8) 7_564 . . . ?
C13 C14 C15 O2 179.7(6) . . . . ?
C13 C14 C15 C16 1.8(10) . . . . ?
O2 C15 C16 C17 179.4(6) . . . . ?
C14 C15 C16 C17 -2.5(10) . . . . ?
N3 C12 C17 C16 -177.0(5) . . . . ?
C13 C12 C17 C16 2.1(9) . . . . ?
C15 C16 C17 C12 0.5(10) . . . . ?
N5 C18 C19 C20 -179.8(10) . . . . ?
C23 C18 C19 C20 6.0(16) . . . . ?
N5 C18 C19 C19 -0.4(15) . . . 7_564 ?
C23 C18 C19 C19 -174.6(12) . . . 7_564 ?
C18 C19 C20 C21 4(2) . . . . ?
C19 C19 C20 C21 -176(2) 7_564 . . . ?
C19 C20 C21 C22 -12(3) . . . . ?
C19 C20 C21 O11 172.2(15) . . . . ?
C20 C21 C22 C23 10(2) . . . . ?
O11 C21 C22 C23 -172.9(12) . . . . ?
C21 C22 C23 C18 -0.1(17) . . . . ?
N5 C18 C23 C22 -179.6(10) . . . . ?
C19 C18 C23 C22 -6.9(15) . . . . ?
C29 C24 C25 C26 2.5(10) . . . . ?
N4 C24 C25 C26 177.9(7) . . . . ?
C24 C25 C26 C27 -2.5(12) . . . . ?
C25 C26 C27 O5 -177.4(8) . . . . ?
C25 C26 C27 C28 3.0(15) . . . . ?
O5 C27 C28 C29 177.3(9) . . . . ?
C26 C27 C28 C29 -3.2(14) . . . . ?
C27 C28 C29 C24 3.1(12) . . . . ?
C27 C28 C29 C30 177.5(8) . . . . ?
C25 C24 C29 C28 -2.8(11) . . . . ?
N4 C24 C29 C28 -179.2(7) . . . . ?
C25 C24 C29 C30 -178.6(6) . . . . ?
N4 C24 C29 C30 5.1(7) . . . . ?
C28 C29 C30 C35 -178.6(8) . . . . ?
C24 C29 C30 C35 -3.6(7) . . . . ?
C28 C29 C30 C31 -3.5(14) . . . . ?
C24 C29 C30 C31 171.5(7) . . . . ?
C35 C30 C31 C32 -1.8(10) . . . . ?
C29 C30 C31 C32 -176.3(7) . . . . ?
C30 C31 C32 O3 -178.2(6) . . . . ?
C30 C31 C32 C33 0.0(10) . . . . ?
O3 C32 C33 C34 -178.9(6) . . . . ?
C31 C32 C33 C34 2.8(10) . . . . ?
C32 C33 C34 C35 -3.6(9) . . . . ?
C31 C30 C35 C34 0.9(10) . . . . ?
C29 C30 C35 C34 176.5(6) . . . . ?
C31 C30 C35 N4 -174.8(6) . . . . ?
C29 C30 C35 N4 0.8(7) . . . . ?
C33 C34 C35 C30 1.8(9) . . . . ?
C33 C34 C35 N4 176.6(6) . . . . ?
O2 C36 C37 O1 172.8(8) . . . . ?
O11 C39 C40 O16 -51(2) . . . . ?
O3 C42 C43 O4 -74.0(12) . . . . ?
O5 C45 C46 O6 -71.0(14) . . . . ?
C36 C37 O1 C38 179.5(10) . . . . ?
C5 C4 N1 C1 -176.8(4) . . . . ?
C3 C4 N1 C1 0.2(5) . . . . ?
C11 C1 N1 C4 175.2(4) . . . . ?
C2 C1 N1 C4 -1.4(5) . . . . ?
C7 C6 N2 C9 -1.7(6) . . . . ?
C5 C6 N2 C9 175.6(5) . . . . ?
C10 C9 N2 C6 -178.9(4) . . . . ?
C8 C9 N2 C6 1.3(6) . . . . ?
C17 C12 N3 C12 178.9(7) . . . 7_564 ?
C13 C12 N3 C12 -0.2(3) . . . 7_564 ?
C17 C12 N3 C11 -1.1(7) . . . . ?
C13 C12 N3 C11 179.8(3) . . . . ?
C1 C11 N3 C12 -69.7(3) 7_564 . . . ?
C1 C11 N3 C12 110.3(3) . . . . ?
C1 C11 N3 C12 110.3(3) 7_564 . . 7_564 ?
C1 C11 N3 C12 -69.7(3) . . . 7_564 ?
C30 C35 N4 C5 167.6(5) . . . . ?
C34 C35 N4 C5 -7.6(10) . . . . ?
C30 C35 N4 C24 2.4(7) . . . . ?
C34 C35 N4 C24 -172.8(6) . . . . ?
C4 C5 N4 C35 -108.9(6) . . . . ?
C6 C5 N4 C35 66.2(7) . . . . ?
C4 C5 N4 C24 53.3(7) . . . . ?
C6 C5 N4 C24 -131.6(6) . . . . ?
C25 C24 N4 C35 179.3(6) . . . . ?
C29 C24 N4 C35 -4.7(7) . . . . ?
C25 C24 N4 C5 14.8(10) . . . . ?
C29 C24 N4 C5 -169.2(6) . . . . ?
C23 C18 N5 C18 173.4(13) . . . 7_564 ?
C19 C18 N5 C18 0.2(6) . . . 7_564 ?
C23 C18 N5 C10 -6.6(13) . . . . ?
C19 C18 N5 C10 -179.9(6) . . . . ?
C9 C10 N5 C18 -98.2(5) 7_564 . . 7_564 ?
C9 C10 N5 C18 81.8(5) . . . 7_564 ?
C9 C10 N5 C18 81.8(5) 7_564 . . . ?
C9 C10 N5 C18 -98.2(5) . . . . ?
F3 C48 S1 O12 176.5(8) . . . . ?
F1 C48 S1 O12 49.3(8) . . . . ?
F2 C48 S1 O12 -67.8(9) . . . . ?
F3 C48 S1 O7 58.9(10) . . . . ?
F1 C48 S1 O7 -68.4(8) . . . . ?
F2 C48 S1 O7 174.5(8) . . . . ?
F3 C48 S1 O9 -59.7(8) . . . . ?
F1 C48 S1 O9 173.0(6) . . . . ?
F2 C48 S1 O9 55.9(8) . . . . ?
C14 C15 O2 C36 1.7(11) . . . . ?
C16 C15 O2 C36 179.7(7) . . . . ?
C37 C36 O2 C15 175.8(7) . . . . ?
C31 C32 O3 C42 -4.7(11) . . . . ?
C33 C32 O3 C42 177.1(7) . . . . ?
C43 C42 O3 C32 -169.2(8) . . . . ?
C42 C43 O4 C44 83.4(16) . . . . ?
C28 C27 O5 C45 0.1(15) . . . . ?
C26 C27 O5 C45 -179.4(9) . . . . ?
C46 C45 O5 C27 -166.2(11) . . . . ?
C45 C46 O6 C47 169.0(14) . . . . ?
C20 C21 O11 C39 -17(3) . . . . ?
C22 C21 O11 C39 165.9(15) . . . . ?
C40 C39 O11 C21 -179.4(17) . . . . ?
C39 C40 O16 C41 -106(3) . . . . ?
F5 C49 S2 O17 -57(2) . . . . ?
F6 C49 S2 O17 180(2) . . . . ?
F4 C49 S2 O17 67(2) . . . . ?
F5 C49 S2 O19 179(3) . . . . ?
F6 C49 S2 O19 56(3) . . . . ?
F4 C49 S2 O19 -57(3) . . . . ?
F5 C49 S2 O18 44(2) . . . . ?
F6 C49 S2 O18 -79(2) . . . . ?
F4 C49 S2 O18 168(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
C2 H1 O3 0.95 2.39 3.224(7) 146.1 11_645
C3 H2 O2 0.95 2.60 3.513(6) 161.3 14_664
C8 H4 O5 0.95 2.66 3.246(7) 120.7 8_564
C16 H9 F2 0.95 2.36 3.086(8) 132.4 20_566
C23 H7 O12 0.95 2.63 3.487(13) 150.3 .
C31 H18 O18 0.95 2.41 3.26(2) 148.0 .
C42 H54 O18 0.99 2.64 3.47(3) 142.2 .
C44 H48 O3 0.98 2.31 3.03(2) 129.6 .
C45 H24 F6 0.99 2.63 3.32(3) 126.4 .
N1 H39 N2 0.88 2.56 3.003(5) 111.9 .
N1 H39 O9 0.88 1.96 2.803(5) 161.0 7_564
N2 H40 N1 0.88 2.52 3.003(5) 115.7 .
N2 H40 N2 0.88 2.51 3.017(9) 117.3 7_564
N2 H40 S1 0.88 3.01 3.491(5) 116.5 .
N2 H40 O9 0.88 2.11 2.845(6) 140.9 .

_refine_diff_density_max         1.040
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.115



