# 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_190112my
_audit_block_doi                 10.5517/ccdc.csd.cc23kw3p
_database_code_depnum_ccdc_archive 'CCDC 1953592'
loop_
_audit_author_name
_audit_author_address
'Yusuke Matsuo'
;Kyoto University
Japan
;
_audit_update_record             
;
2019-09-14 deposited with the CCDC.	2019-10-30 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 H15 N3 O , 3(C3 H6 O)'
_chemical_formula_sum            'C41 H33 N3 O4'
_chemical_formula_weight         631.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.5647(16)
_cell_length_b                   21.451(4)
_cell_length_c                   13.969(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.911(5)
_cell_angle_gamma                90
_cell_volume                     3163.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    3673
_cell_measurement_theta_min      25.3
_cell_measurement_theta_max      75.0

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_F_000             1328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.680
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.688
_shelx_estimated_absorpt_T_min   0.652
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.8140
_diffrn_reflns_number            20964
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.778
_diffrn_reflns_theta_max         66.978
_diffrn_reflns_theta_full        66.978
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             5570
_reflns_number_gt                4849
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0681P)²+0.5567P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5570
_refine_ls_number_parameters     439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.1070
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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 0.22359(10) 0.73997(5) 0.58310(8) 0.0191(2) Uani 1 1 d . . . . .
C2 C 0.09935(11) 0.75763(6) 0.56019(8) 0.0227(3) Uani 1 1 d . . . . .
C3 C 0.05836(11) 0.81944(6) 0.55567(9) 0.0269(3) Uani 1 1 d . . . . .
H1 H -0.0274 0.8292 0.5392 0.032 Uiso 1 1 calc R U . . .
C4 C 0.14525(11) 0.86613(6) 0.57564(8) 0.0247(3) Uani 1 1 d . . . . .
H2 H 0.1203 0.9087 0.5735 0.030 Uiso 1 1 calc R U . . .
C5 C 0.27133(11) 0.84959(5) 0.59924(8) 0.0200(2) Uani 1 1 d . . . . .
C6 C 0.31317(11) 0.78711(5) 0.60359(8) 0.0176(2) Uani 1 1 d . . . . .
C7 C 0.44389(11) 0.78807(5) 0.63181(8) 0.0159(2) Uani 1 1 d . . . . .
C8 C 0.47699(10) 0.85066(5) 0.64323(8) 0.0168(2) Uani 1 1 d . . . . .
C9 C 0.60196(11) 0.87123(5) 0.67121(8) 0.0176(2) Uani 1 1 d . . . . .
C10 C 0.63572(12) 0.93446(5) 0.68204(8) 0.0225(3) Uani 1 1 d . . . . .
H3 H 0.5736 0.9659 0.6708 0.027 Uiso 1 1 calc R U . . .
C11 C 0.75700(12) 0.95113(5) 0.70854(9) 0.0275(3) Uani 1 1 d . . . . .
H4 H 0.7784 0.9939 0.7158 0.033 Uiso 1 1 calc R U . . .
C12 C 0.84953(12) 0.90528(6) 0.72497(9) 0.0266(3) Uani 1 1 d . . . . .
H5 H 0.9336 0.9172 0.7431 0.032 Uiso 1 1 calc R U . . .
C13 C 0.81976(11) 0.84316(5) 0.71509(8) 0.0205(3) Uani 1 1 d . . . . .
H6 H 0.8835 0.8125 0.7264 0.025 Uiso 1 1 calc R U . . .
C14 C 0.69606(10) 0.82454(5) 0.68839(7) 0.0160(2) Uani 1 1 d . . . . .
C15 C 0.65984(10) 0.76048(5) 0.67755(7) 0.0148(2) Uani 1 1 d . . . . .
C16 C 0.53777(10) 0.74112(5) 0.64986(7) 0.0145(2) Uani 1 1 d . . . . .
C17 C 0.54024(10) 0.67449(5) 0.64603(7) 0.0150(2) Uani 1 1 d . . . . .
C18 C 0.66365(10) 0.65620(5) 0.67149(7) 0.0155(2) Uani 1 1 d . . . . .
C19 C 0.70413(11) 0.59238(5) 0.67605(8) 0.0180(2) Uani 1 1 d . . . . .
C20 C 0.82857(11) 0.57461(5) 0.70271(9) 0.0227(3) Uani 1 1 d . . . . .
H7 H 0.8904 0.6056 0.7176 0.027 Uiso 1 1 calc R U . . .
C21 C 0.86102(12) 0.51262(6) 0.70728(10) 0.0295(3) Uani 1 1 d . . . . .
H8 H 0.9452 0.5011 0.7256 0.035 Uiso 1 1 calc R U . . .
C22 C 0.77148(13) 0.46631(6) 0.68527(10) 0.0308(3) Uani 1 1 d . . . . .
H9 H 0.7951 0.4236 0.6889 0.037 Uiso 1 1 calc R U . . .
C23 C 0.65022(13) 0.48231(5) 0.65860(9) 0.0261(3) Uani 1 1 d . . . . .
H10 H 0.5902 0.4505 0.6436 0.031 Uiso 1 1 calc R U . . .
C24 C 0.61285(11) 0.54529(5) 0.65305(8) 0.0199(3) Uani 1 1 d . . . . .
C25 C 0.48731(11) 0.56475(5) 0.62644(8) 0.0192(2) Uani 1 1 d . . . . .
C26 C 0.44928(10) 0.62695(5) 0.62305(8) 0.0172(2) Uani 1 1 d . . . . .
C27 C 0.31839(11) 0.62715(5) 0.59511(8) 0.0187(2) Uani 1 1 d . . . . .
C28 C 0.28112(11) 0.56440(5) 0.58295(8) 0.0222(3) Uani 1 1 d . . . . .
C29 C 0.15629(12) 0.54711(6) 0.55752(9) 0.0286(3) Uani 1 1 d . . . . .
H11 H 0.1343 0.5044 0.5503 0.034 Uiso 1 1 calc R U . . .
C30 C 0.06567(12) 0.59300(6) 0.54304(9) 0.0291(3) Uani 1 1 d . . . . .
H12 H -0.0195 0.5826 0.5257 0.035 Uiso 1 1 calc R U . . .
C31 C 0.10298(11) 0.65495(6) 0.55460(8) 0.0237(3) Uani 1 1 d . . . . .
C32 C 0.22588(10) 0.67336(5) 0.57943(8) 0.0195(3) Uani 1 1 d . . . . .
C33 C 0.23909(15) 1.10884(7) 0.55882(11) 0.0404(4) Uani 1 1 d . . . . .
H34 H 0.1673 1.0799 0.5548 0.061 Uiso 1 1 calc R U . . .
H35 H 0.2482 1.1294 0.4968 0.061 Uiso 1 1 calc R U . . .
H36 H 0.2242 1.1403 0.6081 0.061 Uiso 1 1 calc R U . . .
C34 C 0.35709(13) 1.07367(6) 0.58433(9) 0.0287(3) Uani 1 1 d . . . . .
C35 C 0.47526(16) 1.11013(9) 0.60288(11) 0.0484(4) Uani 1 1 d . . . . .
H37 H 0.4726 1.1297 0.6662 0.073 Uiso 1 1 calc R U . . .
H38 H 0.4823 1.1425 0.5538 0.073 Uiso 1 1 calc R U . . .
H39 H 0.5486 1.0822 0.6009 0.073 Uiso 1 1 calc R U . . .
C36 C 1.13635(14) 0.78687(6) 0.82396(10) 0.0345(3) Uani 1 1 d . . . . .
H40 H 1.1715 0.8047 0.7660 0.052 Uiso 1 1 calc R U . . .
H41 H 1.1995 0.7895 0.8768 0.052 Uiso 1 1 calc R U . . .
H42 H 1.0604 0.8102 0.8406 0.052 Uiso 1 1 calc R U . . .
C37 C 1.10212(12) 0.71971(6) 0.80628(8) 0.0271(3) Uani 1 1 d . . . . .
C38 C 1.20425(14) 0.67294(8) 0.82192(10) 0.0423(4) Uani 1 1 d . . . . .
H43 H 1.1737 0.6319 0.8009 0.063 Uiso 1 1 calc R U . . .
H44 H 1.2287 0.6713 0.8902 0.063 Uiso 1 1 calc R U . . .
H45 H 1.2778 0.6847 0.7850 0.063 Uiso 1 1 calc R U . . .
C39 C 0.50462(12) 0.30990(6) 0.60194(9) 0.0268(3) Uani 1 1 d . . . . .
H46 H 0.5697 0.3424 0.5994 0.040 Uiso 1 1 calc R U . . .
H47 H 0.5219 0.2775 0.5547 0.040 Uiso 1 1 calc R U . . .
H48 H 0.5056 0.2915 0.6662 0.040 Uiso 1 1 calc R U . . .
C40 C 0.37711(11) 0.33803(5) 0.57977(8) 0.0193(2) Uani 1 1 d . . . . .
C41 C 0.27013(13) 0.29349(5) 0.56098(9) 0.0263(3) Uani 1 1 d . . . . .
H49 H 0.1908 0.3168 0.5526 0.039 Uiso 1 1 calc R U . . .
H50 H 0.2640 0.2649 0.6153 0.039 Uiso 1 1 calc R U . . .
H51 H 0.2856 0.2696 0.5027 0.039 Uiso 1 1 calc R U . . .
N1 N 0.37257(9) 0.88738(4) 0.62356(7) 0.0198(2) Uani 1 1 d . . . . .
H31 H 0.3708 0.9284 0.6261 0.024 Uiso 1 1 calc R U . . .
N2 N 0.73523(9) 0.70856(4) 0.69110(7) 0.0158(2) Uani 1 1 d . . . . .
H32 H 0.8158 0.7088 0.7093 0.019 Uiso 1 1 calc R U . . .
N3 N 0.38529(9) 0.52729(5) 0.60162(7) 0.0231(2) Uani 1 1 d . . . . .
H33 H 0.3866 0.4863 0.5983 0.028 Uiso 1 1 calc R U . . .
O1 O 0.02365(8) 0.70601(4) 0.54276(6) 0.0269(2) Uani 1 1 d . . . . .
O2 O 0.35626(12) 1.01752(4) 0.58904(8) 0.0471(3) Uani 1 1 d . . . . .
O3 O 0.99518(9) 0.70532(4) 0.77986(7) 0.0320(2) Uani 1 1 d . . . . .
O4 O 0.36082(9) 0.39396(4) 0.57776(6) 0.0283(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3931(16) . ?
C1 C6 1.4078(16) . ?
C1 C32 1.4302(18) . ?
C2 O1 1.3828(15) . ?
C2 C3 1.3956(19) . ?
C3 C4 1.3808(19) . ?
C3 H1 0.9500 . ?
C4 C5 1.4069(16) . ?
C4 H2 0.9500 . ?
C5 N1 1.3758(15) . ?
C5 C6 1.4120(16) . ?
C6 C7 1.4235(17) . ?
C7 C8 1.3952(15) . ?
C7 C16 1.4301(15) . ?
C8 N1 1.3759(14) . ?
C8 C9 1.4338(16) . ?
C9 C10 1.4095(16) . ?
C9 C14 1.4258(15) . ?
C10 C11 1.3693(18) . ?
C10 H3 0.9500 . ?
C11 C12 1.4003(18) . ?
C11 H4 0.9500 . ?
C12 C13 1.3750(16) . ?
C12 H5 0.9500 . ?
C13 C14 1.4050(16) . ?
C13 H6 0.9500 . ?
C14 C15 1.4331(15) . ?
C15 N2 1.3786(14) . ?
C15 C16 1.3971(15) . ?
C16 C17 1.4305(15) . ?
C17 C18 1.3962(15) . ?
C17 C26 1.4305(15) . ?
C18 N2 1.3765(14) . ?
C18 C19 1.4352(15) . ?
C19 C20 1.4071(17) . ?
C19 C24 1.4257(16) . ?
C20 C21 1.3743(17) . ?
C20 H7 0.9500 . ?
C21 C22 1.3988(19) . ?
C21 H8 0.9500 . ?
C22 C23 1.3660(19) . ?
C22 H9 0.9500 . ?
C23 C24 1.4090(16) . ?
C23 H10 0.9500 . ?
C24 C25 1.4278(17) . ?
C25 N3 1.3795(15) . ?
C25 C26 1.3937(16) . ?
C26 C27 1.4243(16) . ?
C27 C32 1.4040(17) . ?
C27 C28 1.4112(16) . ?
C28 N3 1.3761(16) . ?
C28 C29 1.4041(17) . ?
C29 C30 1.383(2) . ?
C29 H11 0.9500 . ?
C30 C31 1.3940(18) . ?
C30 H12 0.9500 . ?
C31 O1 1.3857(16) . ?
C31 C32 1.3901(16) . ?
C33 C34 1.4902(19) . ?
C33 H34 0.9800 . ?
C33 H35 0.9800 . ?
C33 H36 0.9800 . ?
C34 O2 1.2062(16) . ?
C34 C35 1.489(2) . ?
C35 H37 0.9800 . ?
C35 H38 0.9800 . ?
C35 H39 0.9800 . ?
C36 C37 1.5037(19) . ?
C36 H40 0.9800 . ?
C36 H41 0.9800 . ?
C36 H42 0.9800 . ?
C37 O3 1.2166(16) . ?
C37 C38 1.4842(19) . ?
C38 H43 0.9800 . ?
C38 H44 0.9800 . ?
C38 H45 0.9800 . ?
C39 C40 1.4989(17) . ?
C39 H46 0.9800 . ?
C39 H47 0.9800 . ?
C39 H48 0.9800 . ?
C40 O4 1.2122(14) . ?
C40 C41 1.4964(16) . ?
C41 H49 0.9800 . ?
C41 H50 0.9800 . ?
C41 H51 0.9800 . ?
N1 H31 0.8800 . ?
N2 H32 0.8800 . ?
N3 H33 0.8800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 118.25(11) . . ?
C2 C1 C32 106.29(10) . . ?
C6 C1 C32 135.46(10) . . ?
O1 C2 C1 110.95(11) . . ?
O1 C2 C3 125.18(11) . . ?
C1 C2 C3 123.87(11) . . ?
C4 C3 C2 118.48(11) . . ?
C4 C3 H1 120.8 . . ?
C2 C3 H1 120.8 . . ?
C3 C4 C5 118.82(11) . . ?
C3 C4 H2 120.6 . . ?
C5 C4 H2 120.6 . . ?
N1 C5 C4 129.15(11) . . ?
N1 C5 C6 108.00(10) . . ?
C4 C5 C6 122.84(11) . . ?
C1 C6 C5 117.74(10) . . ?
C1 C6 C7 134.92(10) . . ?
C5 C6 C7 107.31(10) . . ?
C8 C7 C6 106.43(9) . . ?
C8 C7 C16 119.19(10) . . ?
C6 C7 C16 134.37(10) . . ?
N1 C8 C7 109.38(10) . . ?
N1 C8 C9 127.09(10) . . ?
C7 C8 C9 123.53(10) . . ?
C10 C9 C14 119.04(10) . . ?
C10 C9 C8 123.56(10) . . ?
C14 C9 C8 117.40(10) . . ?
C11 C10 C9 120.77(11) . . ?
C11 C10 H3 119.6 . . ?
C9 C10 H3 119.6 . . ?
C10 C11 C12 120.18(11) . . ?
C10 C11 H4 119.9 . . ?
C12 C11 H4 119.9 . . ?
C13 C12 C11 120.55(11) . . ?
C13 C12 H5 119.7 . . ?
C11 C12 H5 119.7 . . ?
C12 C13 C14 120.65(11) . . ?
C12 C13 H6 119.7 . . ?
C14 C13 H6 119.7 . . ?
C13 C14 C9 118.83(10) . . ?
C13 C14 C15 122.91(10) . . ?
C9 C14 C15 118.26(10) . . ?
N2 C15 C16 108.76(9) . . ?
N2 C15 C14 127.53(10) . . ?
C16 C15 C14 123.71(10) . . ?
C15 C16 C7 117.89(10) . . ?
C15 C16 C17 106.83(9) . . ?
C7 C16 C17 135.27(10) . . ?
C18 C17 C16 106.81(9) . . ?
C18 C17 C26 118.13(10) . . ?
C16 C17 C26 135.06(10) . . ?
N2 C18 C17 108.88(9) . . ?
N2 C18 C19 127.50(10) . . ?
C17 C18 C19 123.62(10) . . ?
C20 C19 C24 119.13(10) . . ?
C20 C19 C18 122.99(10) . . ?
C24 C19 C18 117.88(10) . . ?
C21 C20 C19 120.25(12) . . ?
C21 C20 H7 119.9 . . ?
C19 C20 H7 119.9 . . ?
C20 C21 C22 120.74(12) . . ?
C20 C21 H8 119.6 . . ?
C22 C21 H8 119.6 . . ?
C23 C22 C21 120.19(11) . . ?
C23 C22 H9 119.9 . . ?
C21 C22 H9 119.9 . . ?
C22 C23 C24 120.96(12) . . ?
C22 C23 H10 119.5 . . ?
C24 C23 H10 119.5 . . ?
C23 C24 C19 118.73(11) . . ?
C23 C24 C25 123.42(11) . . ?
C19 C24 C25 117.84(10) . . ?
N3 C25 C26 109.10(10) . . ?
N3 C25 C24 127.32(10) . . ?
C26 C25 C24 123.57(10) . . ?
C25 C26 C27 106.76(9) . . ?
C25 C26 C17 118.96(10) . . ?
C27 C26 C17 134.28(10) . . ?
C32 C27 C28 117.69(10) . . ?
C32 C27 C26 135.18(10) . . ?
C28 C27 C26 107.13(10) . . ?
N3 C28 C29 129.31(11) . . ?
N3 C28 C27 108.11(10) . . ?
C29 C28 C27 122.57(12) . . ?
C30 C29 C28 119.26(12) . . ?
C30 C29 H11 120.4 . . ?
C28 C29 H11 120.4 . . ?
C29 C30 C31 118.02(11) . . ?
C29 C30 H12 121.0 . . ?
C31 C30 H12 121.0 . . ?
O1 C31 C32 111.19(11) . . ?
O1 C31 C30 124.91(11) . . ?
C32 C31 C30 123.91(12) . . ?
C31 C32 C27 118.55(11) . . ?
C31 C32 C1 106.02(10) . . ?
C27 C32 C1 135.43(10) . . ?
C34 C33 H34 109.5 . . ?
C34 C33 H35 109.5 . . ?
H34 C33 H35 109.5 . . ?
C34 C33 H36 109.5 . . ?
H34 C33 H36 109.5 . . ?
H35 C33 H36 109.5 . . ?
O2 C34 C35 121.52(14) . . ?
O2 C34 C33 120.73(14) . . ?
C35 C34 C33 117.75(13) . . ?
C34 C35 H37 109.5 . . ?
C34 C35 H38 109.5 . . ?
H37 C35 H38 109.5 . . ?
C34 C35 H39 109.5 . . ?
H37 C35 H39 109.5 . . ?
H38 C35 H39 109.5 . . ?
C37 C36 H40 109.5 . . ?
C37 C36 H41 109.5 . . ?
H40 C36 H41 109.5 . . ?
C37 C36 H42 109.5 . . ?
H40 C36 H42 109.5 . . ?
H41 C36 H42 109.5 . . ?
O3 C37 C38 122.43(13) . . ?
O3 C37 C36 120.58(12) . . ?
C38 C37 C36 116.99(12) . . ?
C37 C38 H43 109.5 . . ?
C37 C38 H44 109.5 . . ?
H43 C38 H44 109.5 . . ?
C37 C38 H45 109.5 . . ?
H43 C38 H45 109.5 . . ?
H44 C38 H45 109.5 . . ?
C40 C39 H46 109.5 . . ?
C40 C39 H47 109.5 . . ?
H46 C39 H47 109.5 . . ?
C40 C39 H48 109.5 . . ?
H46 C39 H48 109.5 . . ?
H47 C39 H48 109.5 . . ?
O4 C40 C41 121.47(11) . . ?
O4 C40 C39 121.95(11) . . ?
C41 C40 C39 116.59(10) . . ?
C40 C41 H49 109.5 . . ?
C40 C41 H50 109.5 . . ?
H49 C41 H50 109.5 . . ?
C40 C41 H51 109.5 . . ?
H49 C41 H51 109.5 . . ?
H50 C41 H51 109.5 . . ?
C8 N1 C5 108.87(9) . . ?
C8 N1 H31 125.6 . . ?
C5 N1 H31 125.6 . . ?
C18 N2 C15 108.72(9) . . ?
C18 N2 H32 125.6 . . ?
C15 N2 H32 125.6 . . ?
C28 N3 C25 108.89(10) . . ?
C28 N3 H33 125.6 . . ?
C25 N3 H33 125.6 . . ?
C2 O1 C31 105.55(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
C6 C1 C2 O1 -179.59(9) . . . . ?
C32 C1 C2 O1 0.23(12) . . . . ?
C6 C1 C2 C3 0.46(17) . . . . ?
C32 C1 C2 C3 -179.72(10) . . . . ?
O1 C2 C3 C4 179.58(11) . . . . ?
C1 C2 C3 C4 -0.48(18) . . . . ?
C2 C3 C4 C5 0.29(17) . . . . ?
C3 C4 C5 N1 -178.45(11) . . . . ?
C3 C4 C5 C6 -0.11(17) . . . . ?
C2 C1 C6 C5 -0.25(16) . . . . ?
C32 C1 C6 C5 180.00(11) . . . . ?
C2 C1 C6 C7 177.82(12) . . . . ?
C32 C1 C6 C7 -1.9(2) . . . . ?
N1 C5 C6 C1 178.74(9) . . . . ?
C4 C5 C6 C1 0.09(17) . . . . ?
N1 C5 C6 C7 0.17(12) . . . . ?
C4 C5 C6 C7 -178.48(10) . . . . ?
C1 C6 C7 C8 -178.42(12) . . . . ?
C5 C6 C7 C8 -0.21(12) . . . . ?
C1 C6 C7 C16 0.8(2) . . . . ?
C5 C6 C7 C16 178.99(11) . . . . ?
C6 C7 C8 N1 0.18(12) . . . . ?
C16 C7 C8 N1 -179.17(9) . . . . ?
C6 C7 C8 C9 -179.78(10) . . . . ?
C16 C7 C8 C9 0.88(16) . . . . ?
N1 C8 C9 C10 -0.46(18) . . . . ?
C7 C8 C9 C10 179.48(10) . . . . ?
N1 C8 C9 C14 179.77(10) . . . . ?
C7 C8 C9 C14 -0.29(16) . . . . ?
C14 C9 C10 C11 0.08(17) . . . . ?
C8 C9 C10 C11 -179.69(11) . . . . ?
C9 C10 C11 C12 0.22(18) . . . . ?
C10 C11 C12 C13 -0.25(19) . . . . ?
C11 C12 C13 C14 -0.02(18) . . . . ?
C12 C13 C14 C9 0.31(16) . . . . ?
C12 C13 C14 C15 -179.68(11) . . . . ?
C10 C9 C14 C13 -0.34(15) . . . . ?
C8 C9 C14 C13 179.44(9) . . . . ?
C10 C9 C14 C15 179.66(10) . . . . ?
C8 C9 C14 C15 -0.56(14) . . . . ?
C13 C14 C15 N2 0.38(17) . . . . ?
C9 C14 C15 N2 -179.62(10) . . . . ?
C13 C14 C15 C16 -179.14(10) . . . . ?
C9 C14 C15 C16 0.87(15) . . . . ?
N2 C15 C16 C7 -179.88(9) . . . . ?
C14 C15 C16 C7 -0.29(15) . . . . ?
N2 C15 C16 C17 -0.37(11) . . . . ?
C14 C15 C16 C17 179.22(9) . . . . ?
C8 C7 C16 C15 -0.57(15) . . . . ?
C6 C7 C16 C15 -179.70(11) . . . . ?
C8 C7 C16 C17 -179.91(11) . . . . ?
C6 C7 C16 C17 1.0(2) . . . . ?
C15 C16 C17 C18 -0.04(11) . . . . ?
C7 C16 C17 C18 179.35(11) . . . . ?
C15 C16 C17 C26 -179.86(11) . . . . ?
C7 C16 C17 C26 -0.5(2) . . . . ?
C16 C17 C18 N2 0.44(11) . . . . ?
C26 C17 C18 N2 -179.71(9) . . . . ?
C16 C17 C18 C19 -179.99(10) . . . . ?
C26 C17 C18 C19 -0.14(16) . . . . ?
N2 C18 C19 C20 0.11(18) . . . . ?
C17 C18 C19 C20 -179.38(10) . . . . ?
N2 C18 C19 C24 179.61(10) . . . . ?
C17 C18 C19 C24 0.12(16) . . . . ?
C24 C19 C20 C21 -0.59(17) . . . . ?
C18 C19 C20 C21 178.90(11) . . . . ?
C19 C20 C21 C22 0.24(19) . . . . ?
C20 C21 C22 C23 0.2(2) . . . . ?
C21 C22 C23 C24 -0.23(19) . . . . ?
C22 C23 C24 C19 -0.12(17) . . . . ?
C22 C23 C24 C25 -179.43(11) . . . . ?
C20 C19 C24 C23 0.53(16) . . . . ?
C18 C19 C24 C23 -178.99(10) . . . . ?
C20 C19 C24 C25 179.88(10) . . . . ?
C18 C19 C24 C25 0.36(15) . . . . ?
C23 C24 C25 N3 -0.70(18) . . . . ?
C19 C24 C25 N3 179.98(10) . . . . ?
C23 C24 C25 C26 178.44(11) . . . . ?
C19 C24 C25 C26 -0.87(16) . . . . ?
N3 C25 C26 C27 0.11(12) . . . . ?
C24 C25 C26 C27 -179.17(10) . . . . ?
N3 C25 C26 C17 -179.86(9) . . . . ?
C24 C25 C26 C17 0.86(16) . . . . ?
C18 C17 C26 C25 -0.34(15) . . . . ?
C16 C17 C26 C25 179.47(11) . . . . ?
C18 C17 C26 C27 179.71(11) . . . . ?
C16 C17 C26 C27 -0.5(2) . . . . ?
C25 C26 C27 C32 179.55(12) . . . . ?
C17 C26 C27 C32 -0.5(2) . . . . ?
C25 C26 C27 C28 0.33(12) . . . . ?
C17 C26 C27 C28 -179.71(11) . . . . ?
C32 C27 C28 N3 179.97(9) . . . . ?
C26 C27 C28 N3 -0.65(12) . . . . ?
C32 C27 C28 C29 -0.95(17) . . . . ?
C26 C27 C28 C29 178.43(11) . . . . ?
N3 C28 C29 C30 179.30(11) . . . . ?
C27 C28 C29 C30 0.43(18) . . . . ?
C28 C29 C30 C31 -0.06(18) . . . . ?
C29 C30 C31 O1 -179.94(11) . . . . ?
C29 C30 C31 C32 0.27(18) . . . . ?
O1 C31 C32 C27 179.37(9) . . . . ?
C30 C31 C32 C27 -0.80(17) . . . . ?
O1 C31 C32 C1 -0.19(12) . . . . ?
C30 C31 C32 C1 179.63(11) . . . . ?
C28 C27 C32 C31 1.10(16) . . . . ?
C26 C27 C32 C31 -178.07(12) . . . . ?
C28 C27 C32 C1 -179.50(11) . . . . ?
C26 C27 C32 C1 1.3(2) . . . . ?
C2 C1 C32 C31 -0.02(12) . . . . ?
C6 C1 C32 C31 179.75(12) . . . . ?
C2 C1 C32 C27 -179.47(12) . . . . ?
C6 C1 C32 C27 0.3(2) . . . . ?
C7 C8 N1 C5 -0.07(12) . . . . ?
C9 C8 N1 C5 179.88(10) . . . . ?
C4 C5 N1 C8 178.47(11) . . . . ?
C6 C5 N1 C8 -0.06(12) . . . . ?
C17 C18 N2 C15 -0.68(12) . . . . ?
C19 C18 N2 C15 179.77(10) . . . . ?
C16 C15 N2 C18 0.65(12) . . . . ?
C14 C15 N2 C18 -178.92(10) . . . . ?
C29 C28 N3 C25 -178.27(12) . . . . ?
C27 C28 N3 C25 0.73(12) . . . . ?
C26 C25 N3 C28 -0.52(12) . . . . ?
C24 C25 N3 C28 178.72(11) . . . . ?
C1 C2 O1 C31 -0.34(12) . . . . ?
C3 C2 O1 C31 179.61(11) . . . . ?
C32 C31 O1 C2 0.32(12) . . . . ?
C30 C31 O1 C2 -179.50(11) . . . . ?

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
C36 H42 O1 0.98 2.88 3.3204(17) 108.0 4_676
C41 H51 N2 0.98 2.75 3.5201(17) 136.0 3_666
N1 H31 O2 0.88 1.99 2.8373(14) 162.3 .
N2 H32 O3 0.88 2.11 2.9761(14) 168.6 .
N3 H33 O4 0.88 2.02 2.8901(14) 170.1 .
C36 H42 O1 0.98 2.88 3.3204(17) 108.0 4_676
C41 H51 N2 0.98 2.75 3.5201(17) 136.0 3_666
C41 H49 O1 0.98 2.64 3.3814(16) 133.1 3_566

_refine_diff_density_max         0.325
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.041

####################################################################### 
# 
# 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_160618ch
_audit_block_doi                 10.5517/ccdc.csd.cc23kw4q
_database_code_depnum_ccdc_archive 'CCDC 1953593'
loop_
_audit_author_name
_audit_author_address
'Yusuke Matsuo'
;Kyoto University
Japan
;
_audit_update_record             
;
2019-09-14 deposited with the CCDC.	2019-10-30 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         'C44 H41 Cl0 N3'
_chemical_formula_sum            'C44 H41 Cl0 N3'
_chemical_formula_weight         611.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/a'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_Int_Tables_number      14

_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                   8.191(3)
_cell_length_b                   35.062(11)
_cell_length_c                   11.513(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.607(5)
_cell_angle_gamma                90
_cell_volume                     3151.6(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    1980
_cell_measurement_theta_min      31.3
_cell_measurement_theta_max      68.2

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   0.866
_exptl_transmission_factor_max   0.977
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.571
_shelx_estimated_absorpt_T_min   0.847
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.8140
_diffrn_reflns_number            19620
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         6.820
_diffrn_reflns_theta_max         65.994
_diffrn_reflns_theta_full        65.994
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             5392
_reflns_number_gt                4225
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1286P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5392
_refine_ls_number_parameters     427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0610
_refine_ls_wR_factor_ref         0.1769
_refine_ls_wR_factor_gt          0.1700
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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 0.2389(3) 0.59489(6) 0.21699(16) 0.0314(4) Uani 1 1 d . . . . .
C2 C 0.1724(3) 0.57998(6) 0.30619(17) 0.0347(5) Uani 1 1 d . . . . .
H1 H 0.1501 0.5973 0.3631 0.042 Uiso 1 1 calc R U . . .
C3 C 0.1370(3) 0.54157(6) 0.31700(17) 0.0371(5) Uani 1 1 d . . . . .
H2 H 0.0895 0.5335 0.3787 0.045 Uiso 1 1 calc R U . . .
C4 C 0.1703(3) 0.51513(6) 0.23861(17) 0.0354(5) Uani 1 1 d . . . . .
H3 H 0.1586 0.4885 0.2497 0.043 Uiso 1 1 calc R U . . .
C5 C 0.2220(2) 0.52938(6) 0.14219(17) 0.0316(4) Uani 1 1 d . . . . .
C6 C 0.2472(2) 0.56855(5) 0.12376(17) 0.0299(4) Uani 1 1 d . . . . .
C7 C 0.2678(2) 0.57090(5) 0.00418(16) 0.0292(4) Uani 1 1 d . . . . .
C8 C 0.2660(2) 0.53384(5) -0.03925(17) 0.0308(4) Uani 1 1 d . . . . .
C9 C 0.2880(3) 0.52424(6) -0.15507(17) 0.0322(5) Uani 1 1 d . . . . .
C10 C 0.3347(3) 0.48783(6) -0.18565(18) 0.0356(5) Uani 1 1 d . . . . .
H4 H 0.3447 0.4675 -0.1294 0.043 Uiso 1 1 calc R U . . .
C11 C 0.3661(3) 0.48087(6) -0.29372(18) 0.0387(5) Uani 1 1 d . . . . .
H5 H 0.3930 0.4558 -0.3133 0.046 Uiso 1 1 calc R U . . .
C12 C 0.3584(3) 0.51078(6) -0.37536(19) 0.0397(5) Uani 1 1 d . . . . .
H6 H 0.3808 0.5060 -0.4503 0.048 Uiso 1 1 calc R U . . .
C13 C 0.3191(3) 0.54691(6) -0.34811(18) 0.0377(5) Uani 1 1 d . . . . .
H7 H 0.3185 0.5671 -0.4034 0.045 Uiso 1 1 calc R U . . .
C14 C 0.2789(3) 0.55500(6) -0.23881(17) 0.0328(5) Uani 1 1 d . . . . .
C15 C 0.2488(3) 0.59251(6) -0.20063(17) 0.0321(5) Uani 1 1 d . . . . .
C16 C 0.2573(3) 0.60165(5) -0.08089(17) 0.0303(4) Uani 1 1 d . . . . .
C17 C 0.2440(3) 0.64208(5) -0.07479(17) 0.0311(4) Uani 1 1 d . . . . .
C18 C 0.2281(3) 0.65631(6) -0.19125(17) 0.0339(5) Uani 1 1 d . . . . .
C19 C 0.2314(3) 0.69595(6) -0.21914(18) 0.0376(5) Uani 1 1 d . . . . .
C20 C 0.2336(3) 0.71101(6) -0.33265(19) 0.0435(6) Uani 1 1 d . . . . .
H8 H 0.2384 0.6939 -0.3955 0.052 Uiso 1 1 calc R U . . .
C21 C 0.2292(4) 0.74907(6) -0.3550(2) 0.0528(7) Uani 1 1 d . . . . .
H9 H 0.2344 0.7582 -0.4315 0.063 Uiso 1 1 calc R U . . .
C22 C 0.2170(4) 0.77472(7) -0.2656(2) 0.0557(7) Uani 1 1 d . . . . .
H10 H 0.2050 0.8012 -0.2831 0.067 Uiso 1 1 calc R U . . .
C23 C 0.2225(4) 0.76158(6) -0.1521(2) 0.0479(6) Uani 1 1 d . . . . .
H11 H 0.2139 0.7793 -0.0918 0.057 Uiso 1 1 calc R U . . .
C24 C 0.2403(3) 0.72264(6) -0.12300(19) 0.0387(5) Uani 1 1 d . . . . .
C25 C 0.2687(3) 0.70729(6) -0.00191(18) 0.0346(5) Uani 1 1 d . . . . .
C26 C 0.2616(3) 0.66863(5) 0.02406(17) 0.0313(4) Uani 1 1 d . . . . .
C27 C 0.2992(3) 0.66479(6) 0.15430(17) 0.0322(5) Uani 1 1 d . . . . .
C28 C 0.3393(3) 0.70219(6) 0.20075(18) 0.0343(5) Uani 1 1 d . . . . .
C29 C 0.4005(3) 0.71090(6) 0.32496(18) 0.0398(5) Uani 1 1 d . . . . .
H12 H 0.4240 0.7364 0.3529 0.048 Uiso 1 1 calc R U . . .
C30 C 0.4248(3) 0.68072(6) 0.40468(18) 0.0404(5) Uani 1 1 d . . . . .
H13 H 0.4739 0.6850 0.4896 0.049 Uiso 1 1 calc R U . . .
C31 C 0.3784(3) 0.64417(6) 0.36232(17) 0.0371(5) Uani 1 1 d . . . . .
H14 H 0.3969 0.6242 0.4205 0.044 Uiso 1 1 calc R U . . .
C32 C 0.3056(3) 0.63468(6) 0.23880(17) 0.0317(4) Uani 1 1 d . . . . .
C33 C 0.1748(3) 0.46930(5) 0.02331(18) 0.0341(5) Uani 1 1 d . . . . .
H15 H 0.1374 0.4649 -0.0658 0.041 Uiso 1 1 calc R U . . .
H16 H 0.0722 0.4672 0.0514 0.041 Uiso 1 1 calc R U . . .
C34 C 0.2989(3) 0.43782(6) 0.08359(17) 0.0353(5) Uani 1 1 d . . . . .
H17 H 0.3942 0.4367 0.0475 0.042 Uiso 1 1 calc R U . . .
H18 H 0.3475 0.4431 0.1718 0.042 Uiso 1 1 calc R U . . .
C35 C 0.2045(3) 0.40013(6) 0.06474(19) 0.0391(5) Uani 1 1 d . . . . .
H19 H 0.1496 0.3962 -0.0236 0.047 Uiso 1 1 calc R U . . .
H20 H 0.1126 0.4013 0.1041 0.047 Uiso 1 1 calc R U . . .
C36 C 0.3191(3) 0.36620(6) 0.1157(2) 0.0466(6) Uani 1 1 d . . . . .
H33 H 0.4041 0.3634 0.0720 0.070 Uiso 1 1 calc R U . . .
H34 H 0.2493 0.3430 0.1055 0.070 Uiso 1 1 calc R U . . .
H35 H 0.3778 0.3703 0.2025 0.070 Uiso 1 1 calc R U . . .
N1 N 0.2407(2) 0.50826(4) 0.04608(14) 0.0324(4) Uani 1 1 d . . . . .
N2 N 0.2256(2) 0.62584(5) -0.27043(14) 0.0339(4) Uani 1 1 d . . . . .
C37 C 0.1247(3) 0.62585(6) -0.40114(17) 0.0402(5) Uani 1 1 d . . . . .
H21 H 0.1123 0.5992 -0.4308 0.048 Uiso 1 1 calc R U . . .
H22 H 0.1901 0.6399 -0.4471 0.048 Uiso 1 1 calc R U . . .
C38 C -0.0529(3) 0.64352(6) -0.42983(19) 0.0478(6) Uani 1 1 d . . . . .
H23 H -0.0414 0.6700 -0.3985 0.057 Uiso 1 1 calc R U . . .
H24 H -0.1048 0.6447 -0.5194 0.057 Uiso 1 1 calc R U . . .
C39 C -0.1715(3) 0.62182(7) -0.3756(2) 0.0519(6) Uani 1 1 d . . . . .
H25 H -0.1183 0.6206 -0.2861 0.062 Uiso 1 1 calc R U . . .
H26 H -0.2796 0.6364 -0.3912 0.062 Uiso 1 1 calc R U . . .
C40 C -0.2143(4) 0.58199(8) -0.4226(3) 0.0677(8) Uani 1 1 d . . . . .
H36 H -0.2580 0.5825 -0.5118 0.102 Uiso 1 1 calc R U . . .
H37 H -0.3018 0.5713 -0.3897 0.102 Uiso 1 1 calc R U . . .
H38 H -0.1111 0.5661 -0.3970 0.102 Uiso 1 1 calc R U . . .
N3 N 0.3161(2) 0.72792(5) 0.10670(15) 0.0360(4) Uani 1 1 d . . . . .
C41 C 0.3880(3) 0.76650(6) 0.12973(19) 0.0380(5) Uani 1 1 d . . . . .
H27 H 0.4195 0.7751 0.0574 0.046 Uiso 1 1 calc R U . . .
H28 H 0.4944 0.7655 0.1993 0.046 Uiso 1 1 calc R U . . .
C42 C 0.2681(3) 0.79597(6) 0.15754(19) 0.0380(5) Uani 1 1 d . . . . .
H29 H 0.1700 0.8003 0.0836 0.046 Uiso 1 1 calc R U . . .
H30 H 0.2227 0.7860 0.2221 0.046 Uiso 1 1 calc R U . . .
C43 C 0.3592(3) 0.83354(6) 0.19900(19) 0.0381(5) Uani 1 1 d . . . . .
H31 H 0.4115 0.8424 0.1368 0.046 Uiso 1 1 calc R U . . .
H32 H 0.4527 0.8293 0.2758 0.046 Uiso 1 1 calc R U . . .
C44 C 0.2404(3) 0.86451(6) 0.2197(2) 0.0421(5) Uani 1 1 d . . . . .
H39 H 0.1523 0.8702 0.1426 0.063 Uiso 1 1 calc R U . . .
H40 H 0.3069 0.8876 0.2501 0.063 Uiso 1 1 calc R U . . .
H41 H 0.1858 0.8556 0.2796 0.063 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
C1 C2 1.401(3) . ?
C1 C6 1.433(3) . ?
C1 C32 1.492(3) . ?
C2 C3 1.391(3) . ?
C2 H1 0.9500 . ?
C3 C4 1.378(3) . ?
C3 H2 0.9500 . ?
C4 C5 1.395(3) . ?
C4 H3 0.9500 . ?
C5 N1 1.378(3) . ?
C5 C6 1.414(3) . ?
C6 C7 1.439(3) . ?
C7 C8 1.391(3) . ?
C7 C16 1.442(3) . ?
C8 N1 1.391(3) . ?
C8 C9 1.438(3) . ?
C9 C10 1.407(3) . ?
C9 C14 1.433(3) . ?
C10 C11 1.367(3) . ?
C10 H4 0.9500 . ?
C11 C12 1.397(3) . ?
C11 H5 0.9500 . ?
C12 C13 1.367(3) . ?
C12 H6 0.9500 . ?
C13 C14 1.422(3) . ?
C13 H7 0.9500 . ?
C14 C15 1.432(3) . ?
C15 C16 1.396(3) . ?
C15 N2 1.398(3) . ?
C16 C17 1.425(3) . ?
C17 C18 1.399(3) . ?
C17 C26 1.443(3) . ?
C18 N2 1.400(2) . ?
C18 C19 1.429(3) . ?
C19 C20 1.415(3) . ?
C19 C24 1.434(3) . ?
C20 C21 1.358(3) . ?
C20 H8 0.9500 . ?
C21 C22 1.393(3) . ?
C21 H9 0.9500 . ?
C22 C23 1.374(3) . ?
C22 H10 0.9500 . ?
C23 C24 1.403(3) . ?
C23 H11 0.9500 . ?
C24 C25 1.446(3) . ?
C25 N3 1.394(3) . ?
C25 C26 1.393(3) . ?
C26 C27 1.443(3) . ?
C27 C28 1.417(3) . ?
C27 C32 1.426(3) . ?
C28 N3 1.378(3) . ?
C28 C29 1.398(3) . ?
C29 C30 1.375(3) . ?
C29 H12 0.9500 . ?
C30 C31 1.383(3) . ?
C30 H13 0.9500 . ?
C31 C32 1.406(3) . ?
C31 H14 0.9500 . ?
C33 N1 1.463(3) . ?
C33 C34 1.519(3) . ?
C33 H15 0.9900 . ?
C33 H16 0.9900 . ?
C34 C35 1.513(3) . ?
C34 H17 0.9900 . ?
C34 H18 0.9900 . ?
C35 C36 1.519(3) . ?
C35 H19 0.9900 . ?
C35 H20 0.9900 . ?
C36 H33 0.9800 . ?
C36 H34 0.9800 . ?
C36 H35 0.9800 . ?
N2 C37 1.481(3) . ?
C37 C38 1.523(3) . ?
C37 H21 0.9900 . ?
C37 H22 0.9900 . ?
C38 C39 1.510(4) . ?
C38 H23 0.9900 . ?
C38 H24 0.9900 . ?
C39 C40 1.501(4) . ?
C39 H25 0.9900 . ?
C39 H26 0.9900 . ?
C40 H36 0.9800 . ?
C40 H37 0.9800 . ?
C40 H38 0.9800 . ?
N3 C41 1.467(3) . ?
C41 C42 1.525(3) . ?
C41 H27 0.9900 . ?
C41 H28 0.9900 . ?
C42 C43 1.518(3) . ?
C42 H29 0.9900 . ?
C42 H30 0.9900 . ?
C43 C44 1.524(3) . ?
C43 H31 0.9900 . ?
C43 H32 0.9900 . ?
C44 H39 0.9800 . ?
C44 H40 0.9800 . ?
C44 H41 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
C2 C1 C6 115.18(18) . . ?
C2 C1 C32 115.43(17) . . ?
C6 C1 C32 129.12(18) . . ?
C3 C2 C1 124.40(19) . . ?
C3 C2 H1 117.8 . . ?
C1 C2 H1 117.8 . . ?
C4 C3 C2 120.32(19) . . ?
C4 C3 H2 119.8 . . ?
C2 C3 H2 119.8 . . ?
C3 C4 C5 116.63(19) . . ?
C3 C4 H3 121.7 . . ?
C5 C4 H3 121.7 . . ?
N1 C5 C4 125.51(18) . . ?
N1 C5 C6 110.16(17) . . ?
C4 C5 C6 124.09(19) . . ?
C5 C6 C1 118.12(18) . . ?
C5 C6 C7 105.30(17) . . ?
C1 C6 C7 136.50(18) . . ?
C8 C7 C6 107.39(17) . . ?
C8 C7 C16 117.55(17) . . ?
C6 C7 C16 133.84(18) . . ?
C7 C8 N1 109.63(17) . . ?
C7 C8 C9 124.14(18) . . ?
N1 C8 C9 126.22(17) . . ?
C10 C9 C14 118.48(18) . . ?
C10 C9 C8 124.32(18) . . ?
C14 C9 C8 116.86(17) . . ?
C11 C10 C9 122.01(19) . . ?
C11 C10 H4 119.0 . . ?
C9 C10 H4 119.0 . . ?
C10 C11 C12 119.72(19) . . ?
C10 C11 H5 120.1 . . ?
C12 C11 H5 120.1 . . ?
C13 C12 C11 120.5(2) . . ?
C13 C12 H6 119.8 . . ?
C11 C12 H6 119.8 . . ?
C12 C13 C14 121.4(2) . . ?
C12 C13 H7 119.3 . . ?
C14 C13 H7 119.3 . . ?
C13 C14 C9 117.79(18) . . ?
C13 C14 C15 124.22(19) . . ?
C9 C14 C15 117.61(18) . . ?
C16 C15 N2 109.47(17) . . ?
C16 C15 C14 123.51(18) . . ?
N2 C15 C14 126.69(18) . . ?
C15 C16 C17 107.17(17) . . ?
C15 C16 C7 118.30(17) . . ?
C17 C16 C7 134.44(18) . . ?
C18 C17 C16 107.08(17) . . ?
C18 C17 C26 118.94(18) . . ?
C16 C17 C26 133.58(17) . . ?
C17 C18 N2 109.31(17) . . ?
C17 C18 C19 124.02(18) . . ?
N2 C18 C19 126.40(18) . . ?
C20 C19 C18 125.24(19) . . ?
C20 C19 C24 117.22(19) . . ?
C18 C19 C24 117.48(18) . . ?
C21 C20 C19 122.4(2) . . ?
C21 C20 H8 118.8 . . ?
C19 C20 H8 118.8 . . ?
C20 C21 C22 119.9(2) . . ?
C20 C21 H9 120.1 . . ?
C22 C21 H9 120.1 . . ?
C23 C22 C21 119.8(2) . . ?
C23 C22 H10 120.1 . . ?
C21 C22 H10 120.1 . . ?
C22 C23 C24 121.7(2) . . ?
C22 C23 H11 119.2 . . ?
C24 C23 H11 119.2 . . ?
C23 C24 C19 118.25(19) . . ?
C23 C24 C25 124.57(19) . . ?
C19 C24 C25 117.19(18) . . ?
N3 C25 C26 109.32(17) . . ?
N3 C25 C24 126.25(19) . . ?
C26 C25 C24 124.34(18) . . ?
C25 C26 C17 117.33(17) . . ?
C25 C26 C27 107.71(16) . . ?
C17 C26 C27 134.29(18) . . ?
C28 C27 C32 118.12(17) . . ?
C28 C27 C26 104.96(17) . . ?
C32 C27 C26 136.93(18) . . ?
N3 C28 C29 125.61(19) . . ?
N3 C28 C27 110.39(17) . . ?
C29 C28 C27 123.95(19) . . ?
C30 C29 C28 116.70(19) . . ?
C30 C29 H12 121.7 . . ?
C28 C29 H12 121.7 . . ?
C29 C30 C31 120.58(19) . . ?
C29 C30 H13 119.7 . . ?
C31 C30 H13 119.7 . . ?
C30 C31 C32 124.27(19) . . ?
C30 C31 H14 117.9 . . ?
C32 C31 H14 117.9 . . ?
C31 C32 C27 115.60(18) . . ?
C31 C32 C1 114.40(17) . . ?
C27 C32 C1 129.92(17) . . ?
N1 C33 C34 115.91(17) . . ?
N1 C33 H15 108.3 . . ?
C34 C33 H15 108.3 . . ?
N1 C33 H16 108.3 . . ?
C34 C33 H16 108.3 . . ?
H15 C33 H16 107.4 . . ?
C35 C34 C33 109.10(18) . . ?
C35 C34 H17 109.9 . . ?
C33 C34 H17 109.9 . . ?
C35 C34 H18 109.9 . . ?
C33 C34 H18 109.9 . . ?
H17 C34 H18 108.3 . . ?
C34 C35 C36 113.56(19) . . ?
C34 C35 H19 108.9 . . ?
C36 C35 H19 108.9 . . ?
C34 C35 H20 108.9 . . ?
C36 C35 H20 108.9 . . ?
H19 C35 H20 107.7 . . ?
C35 C36 H33 109.5 . . ?
C35 C36 H34 109.5 . . ?
H33 C36 H34 109.5 . . ?
C35 C36 H35 109.5 . . ?
H33 C36 H35 109.5 . . ?
H34 C36 H35 109.5 . . ?
C5 N1 C8 107.29(16) . . ?
C5 N1 C33 121.40(17) . . ?
C8 N1 C33 126.95(16) . . ?
C15 N2 C18 106.90(16) . . ?
C15 N2 C37 121.40(16) . . ?
C18 N2 C37 123.72(16) . . ?
N2 C37 C38 115.01(17) . . ?
N2 C37 H21 108.5 . . ?
C38 C37 H21 108.5 . . ?
N2 C37 H22 108.5 . . ?
C38 C37 H22 108.5 . . ?
H21 C37 H22 107.5 . . ?
C39 C38 C37 113.41(19) . . ?
C39 C38 H23 108.9 . . ?
C37 C38 H23 108.9 . . ?
C39 C38 H24 108.9 . . ?
C37 C38 H24 108.9 . . ?
H23 C38 H24 107.7 . . ?
C40 C39 C38 115.4(2) . . ?
C40 C39 H25 108.4 . . ?
C38 C39 H25 108.4 . . ?
C40 C39 H26 108.4 . . ?
C38 C39 H26 108.4 . . ?
H25 C39 H26 107.5 . . ?
C39 C40 H36 109.5 . . ?
C39 C40 H37 109.5 . . ?
H36 C40 H37 109.5 . . ?
C39 C40 H38 109.5 . . ?
H36 C40 H38 109.5 . . ?
H37 C40 H38 109.5 . . ?
C28 N3 C25 107.44(16) . . ?
C28 N3 C41 120.62(16) . . ?
C25 N3 C41 128.90(17) . . ?
N3 C41 C42 114.41(19) . . ?
N3 C41 H27 108.7 . . ?
C42 C41 H27 108.7 . . ?
N3 C41 H28 108.7 . . ?
C42 C41 H28 108.7 . . ?
H27 C41 H28 107.6 . . ?
C43 C42 C41 111.54(19) . . ?
C43 C42 H29 109.3 . . ?
C41 C42 H29 109.3 . . ?
C43 C42 H30 109.3 . . ?
C41 C42 H30 109.3 . . ?
H29 C42 H30 108.0 . . ?
C42 C43 C44 113.02(19) . . ?
C42 C43 H31 109.0 . . ?
C44 C43 H31 109.0 . . ?
C42 C43 H32 109.0 . . ?
C44 C43 H32 109.0 . . ?
H31 C43 H32 107.8 . . ?
C43 C44 H39 109.5 . . ?
C43 C44 H40 109.5 . . ?
H39 C44 H40 109.5 . . ?
C43 C44 H41 109.5 . . ?
H39 C44 H41 109.5 . . ?
H40 C44 H41 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 8.4(3) . . . . ?
C32 C1 C2 C3 -166.16(19) . . . . ?
C1 C2 C3 C4 1.4(3) . . . . ?
C2 C3 C4 C5 -6.8(3) . . . . ?
C3 C4 C5 N1 -171.45(19) . . . . ?
C3 C4 C5 C6 2.3(3) . . . . ?
N1 C5 C6 C1 -177.77(16) . . . . ?
C4 C5 C6 C1 7.7(3) . . . . ?
N1 C5 C6 C7 5.0(2) . . . . ?
C4 C5 C6 C7 -169.55(19) . . . . ?
C2 C1 C6 C5 -12.4(3) . . . . ?
C32 C1 C6 C5 161.34(19) . . . . ?
C2 C1 C6 C7 163.7(2) . . . . ?
C32 C1 C6 C7 -22.6(4) . . . . ?
C5 C6 C7 C8 -3.9(2) . . . . ?
C1 C6 C7 C8 179.6(2) . . . . ?
C5 C6 C7 C16 162.7(2) . . . . ?
C1 C6 C7 C16 -13.8(4) . . . . ?
C6 C7 C8 N1 1.6(2) . . . . ?
C16 C7 C8 N1 -167.57(17) . . . . ?
C6 C7 C8 C9 -178.21(18) . . . . ?
C16 C7 C8 C9 12.7(3) . . . . ?
C7 C8 C9 C10 161.1(2) . . . . ?
N1 C8 C9 C10 -18.6(3) . . . . ?
C7 C8 C9 C14 -12.1(3) . . . . ?
N1 C8 C9 C14 168.18(19) . . . . ?
C14 C9 C10 C11 -2.1(3) . . . . ?
C8 C9 C10 C11 -175.1(2) . . . . ?
C9 C10 C11 C12 2.5(3) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C11 C12 C13 C14 -2.2(3) . . . . ?
C12 C13 C14 C9 2.6(3) . . . . ?
C12 C13 C14 C15 175.3(2) . . . . ?
C10 C9 C14 C13 -0.4(3) . . . . ?
C8 C9 C14 C13 173.16(19) . . . . ?
C10 C9 C14 C15 -173.62(19) . . . . ?
C8 C9 C14 C15 0.0(3) . . . . ?
C13 C14 C15 C16 -161.3(2) . . . . ?
C9 C14 C15 C16 11.4(3) . . . . ?
C13 C14 C15 N2 11.3(3) . . . . ?
C9 C14 C15 N2 -175.96(18) . . . . ?
N2 C15 C16 C17 -1.7(2) . . . . ?
C14 C15 C16 C17 172.00(19) . . . . ?
N2 C15 C16 C7 175.28(17) . . . . ?
C14 C15 C16 C7 -11.0(3) . . . . ?
C8 C7 C16 C15 -1.0(3) . . . . ?
C6 C7 C16 C15 -166.5(2) . . . . ?
C8 C7 C16 C17 175.0(2) . . . . ?
C6 C7 C16 C17 9.4(4) . . . . ?
C15 C16 C17 C18 -0.1(2) . . . . ?
C7 C16 C17 C18 -176.4(2) . . . . ?
C15 C16 C17 C26 -172.5(2) . . . . ?
C7 C16 C17 C26 11.2(4) . . . . ?
C16 C17 C18 N2 1.9(2) . . . . ?
C26 C17 C18 N2 175.62(18) . . . . ?
C16 C17 C18 C19 -172.5(2) . . . . ?
C26 C17 C18 C19 1.3(3) . . . . ?
C17 C18 C19 C20 173.0(2) . . . . ?
N2 C18 C19 C20 -0.4(4) . . . . ?
C17 C18 C19 C24 -4.2(3) . . . . ?
N2 C18 C19 C24 -177.6(2) . . . . ?
C18 C19 C20 C21 177.1(2) . . . . ?
C24 C19 C20 C21 -5.7(4) . . . . ?
C19 C20 C21 C22 -1.9(4) . . . . ?
C20 C21 C22 C23 4.9(4) . . . . ?
C21 C22 C23 C24 0.1(4) . . . . ?
C22 C23 C24 C19 -7.7(4) . . . . ?
C22 C23 C24 C25 171.8(3) . . . . ?
C20 C19 C24 C23 10.3(3) . . . . ?
C18 C19 C24 C23 -172.3(2) . . . . ?
C20 C19 C24 C25 -169.3(2) . . . . ?
C18 C19 C24 C25 8.1(3) . . . . ?
C23 C24 C25 N3 -13.6(4) . . . . ?
C19 C24 C25 N3 165.9(2) . . . . ?
C23 C24 C25 C26 170.3(2) . . . . ?
C19 C24 C25 C26 -10.2(3) . . . . ?
N3 C25 C26 C17 -169.47(18) . . . . ?
C24 C25 C26 C17 7.3(3) . . . . ?
N3 C25 C26 C27 2.5(2) . . . . ?
C24 C25 C26 C27 179.2(2) . . . . ?
C18 C17 C26 C25 -2.5(3) . . . . ?
C16 C17 C26 C25 169.2(2) . . . . ?
C18 C17 C26 C27 -171.7(2) . . . . ?
C16 C17 C26 C27 0.0(4) . . . . ?
C25 C26 C27 C28 -4.0(2) . . . . ?
C17 C26 C27 C28 165.9(2) . . . . ?
C25 C26 C27 C32 176.5(2) . . . . ?
C17 C26 C27 C32 -13.6(4) . . . . ?
C32 C27 C28 N3 -176.10(18) . . . . ?
C26 C27 C28 N3 4.3(2) . . . . ?
C32 C27 C28 C29 6.3(3) . . . . ?
C26 C27 C28 C29 -173.3(2) . . . . ?
N3 C28 C29 C30 -176.0(2) . . . . ?
C27 C28 C29 C30 1.2(3) . . . . ?
C28 C29 C30 C31 -4.5(3) . . . . ?
C29 C30 C31 C32 0.3(4) . . . . ?
C30 C31 C32 C27 7.2(3) . . . . ?
C30 C31 C32 C1 -170.0(2) . . . . ?
C28 C27 C32 C31 -9.9(3) . . . . ?
C26 C27 C32 C31 169.5(2) . . . . ?
C28 C27 C32 C1 166.6(2) . . . . ?
C26 C27 C32 C1 -13.9(4) . . . . ?
C2 C1 C32 C31 32.9(3) . . . . ?
C6 C1 C32 C31 -140.8(2) . . . . ?
C2 C1 C32 C27 -143.8(2) . . . . ?
C6 C1 C32 C27 42.5(3) . . . . ?
N1 C33 C34 C35 172.67(17) . . . . ?
C33 C34 C35 C36 176.87(18) . . . . ?
C4 C5 N1 C8 170.32(19) . . . . ?
C6 C5 N1 C8 -4.2(2) . . . . ?
C4 C5 N1 C33 12.3(3) . . . . ?
C6 C5 N1 C33 -162.20(17) . . . . ?
C7 C8 N1 C5 1.6(2) . . . . ?
C9 C8 N1 C5 -178.69(18) . . . . ?
C7 C8 N1 C33 158.02(19) . . . . ?
C9 C8 N1 C33 -22.2(3) . . . . ?
C34 C33 N1 C5 -91.3(2) . . . . ?
C34 C33 N1 C8 115.2(2) . . . . ?
C16 C15 N2 C18 2.8(2) . . . . ?
C14 C15 N2 C18 -170.6(2) . . . . ?
C16 C15 N2 C37 -147.05(19) . . . . ?
C14 C15 N2 C37 39.5(3) . . . . ?
C17 C18 N2 C15 -2.9(2) . . . . ?
C19 C18 N2 C15 171.3(2) . . . . ?
C17 C18 N2 C37 146.1(2) . . . . ?
C19 C18 N2 C37 -39.7(3) . . . . ?
C15 N2 C37 C38 104.9(2) . . . . ?
C18 N2 C37 C38 -39.8(3) . . . . ?
N2 C37 C38 C39 -64.5(3) . . . . ?
C37 C38 C39 C40 -63.7(3) . . . . ?
C29 C28 N3 C25 174.7(2) . . . . ?
C27 C28 N3 C25 -2.9(2) . . . . ?
C29 C28 N3 C41 12.7(3) . . . . ?
C27 C28 N3 C41 -164.85(19) . . . . ?
C26 C25 N3 C28 0.2(2) . . . . ?
C24 C25 N3 C28 -176.4(2) . . . . ?
C26 C25 N3 C41 160.2(2) . . . . ?
C24 C25 N3 C41 -16.5(4) . . . . ?
C28 N3 C41 C42 -90.9(2) . . . . ?
C25 N3 C41 C42 111.3(2) . . . . ?
N3 C41 C42 C43 171.38(16) . . . . ?
C41 C42 C43 C44 176.25(17) . . . . ?

_refine_diff_density_max         0.707
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.059

####################################################################### 
# 
# 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_my0420
_audit_block_doi                 10.5517/ccdc.csd.cc23kw5r
_database_code_depnum_ccdc_archive 'CCDC 1953594'
loop_
_audit_author_name
_audit_author_address
'Yusuke Matsuo'
;Kyoto University
Japan
;
_audit_update_record             
;
2019-09-14 deposited with the CCDC.	2019-10-30 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         'C44 H39 N3 O, C Cl2'
_chemical_formula_sum            'C45 H39 Cl2 N3 O'
_chemical_formula_weight         708.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.881(4)
_cell_length_b                   13.068(7)
_cell_length_c                   13.624(7)
_cell_angle_alpha                114.604(18)
_cell_angle_beta                 92.906(5)
_cell_angle_gamma                97.348(10)
_cell_volume                     1735.2(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    972
_cell_measurement_theta_min      25.3
_cell_measurement_theta_max      74.0


_exptl_crystal_description       Prism
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_F_000             744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    2.003
_shelx_estimated_absorpt_T_min   0.428
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
;
Rigaku Pilatus 200K
;
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            22539
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.592
_diffrn_reflns_theta_max         67.000
_diffrn_reflns_theta_full        67.000
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             6044
_reflns_number_gt                3585
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0950P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6044
_refine_ls_number_parameters     516
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.1754
_refine_ls_wR_factor_gt          0.1619
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4687(2) 0.6462(2) 0.3607(2) 0.0363(6) Uani 1 1 d . . . . .
C2 C 0.4451(3) 0.5798(3) 0.2491(2) 0.0435(7) Uani 1 1 d . . . . .
C3 C 0.4935(3) 0.4806(3) 0.1932(2) 0.0518(8) Uani 1 1 d . . . . .
H1 H 0.4755 0.4388 0.1166 0.062 Uiso 1 1 calc R U . . .
C4 C 0.5698(3) 0.4447(3) 0.2540(2) 0.0480(8) Uani 1 1 d . . . . .
H2 H 0.6032 0.3763 0.2195 0.058 Uiso 1 1 calc R U . . .
C5 C 0.5968(2) 0.5104(2) 0.3667(2) 0.0386(6) Uani 1 1 d . . . . .
C6 C 0.5481(2) 0.6124(2) 0.4231(2) 0.0343(6) Uani 1 1 d . . . . .
C7 C 0.5985(2) 0.6569(2) 0.5346(2) 0.0329(6) Uani 1 1 d . . . . .
C8 C 0.6743(2) 0.5802(2) 0.5425(2) 0.0357(6) Uani 1 1 d . . . . .
C9 C 0.7432(2) 0.5989(2) 0.6438(2) 0.0384(6) Uani 1 1 d . . . . .
C10 C 0.8209(3) 0.5247(3) 0.6564(2) 0.0450(7) Uani 1 1 d . . . . .
H3 H 0.8341 0.4602 0.5939 0.054 Uiso 1 1 calc R U . . .
C11 C 0.8776(3) 0.5430(3) 0.7562(2) 0.0549(8) Uani 1 1 d . . . . .
H4 H 0.9286 0.4916 0.7621 0.066 Uiso 1 1 calc R U . . .
C12 C 0.8595(3) 0.6380(3) 0.8488(3) 0.0703(11) Uani 1 1 d . . . . .
H5 H 0.8969 0.6503 0.9181 0.084 Uiso 1 1 calc R U . . .
C13 C 0.7874(3) 0.7138(3) 0.8398(2) 0.0663(10) Uani 1 1 d . . . . .
H6 H 0.7760 0.7778 0.9036 0.080 Uiso 1 1 calc R U . . .
C14 C 0.7303(2) 0.6988(3) 0.7386(2) 0.0451(7) Uani 1 1 d . . . . .
C15 C 0.6575(2) 0.7786(2) 0.7268(2) 0.0408(7) Uani 1 1 d . . . . .
C16 C 0.5897(2) 0.7586(2) 0.6285(2) 0.0351(6) Uani 1 1 d . . . . .
C17 C 0.5249(2) 0.8554(2) 0.6512(2) 0.0358(6) Uani 1 1 d . . . . .
C18 C 0.5574(2) 0.9283(2) 0.7612(2) 0.0394(7) Uani 1 1 d . . . . .
N1 N 0.6719(2) 0.49092(19) 0.44022(17) 0.0381(5) Uani 1 1 d . . . . .
N2 N 0.6406(2) 0.8837(2) 0.80892(18) 0.0456(6) Uani 1 1 d . . . . .
N3 N 0.3282(2) 1.0121(2) 0.55980(19) 0.0424(6) Uani 1 1 d . . . . .
C19 C 0.5034(3) 1.0299(2) 0.8165(2) 0.0440(7) Uani 1 1 d . . . . .
C20 C 0.5171(3) 1.0917(3) 0.9308(2) 0.0527(8) Uani 1 1 d . . . . .
H7 H 0.5660 1.0671 0.9740 0.063 Uiso 1 1 calc R U . . .
C21 C 0.4617(4) 1.1864(3) 0.9811(3) 0.0663(10) Uani 1 1 d . . . . .
H8 H 0.4732 1.2269 1.0580 0.080 Uiso 1 1 calc R U . . .
C22 C 0.3881(4) 1.2229(3) 0.9184(3) 0.0747(11) Uani 1 1 d . . . . .
H9 H 0.3520 1.2898 0.9529 0.090 Uiso 1 1 calc R U . . .
C23 C 0.3681(3) 1.1628(3) 0.8079(3) 0.0585(9) Uani 1 1 d . . . . .
H10 H 0.3155 1.1871 0.7670 0.070 Uiso 1 1 calc R U . . .
C24 C 0.4239(3) 1.0651(2) 0.7528(2) 0.0424(7) Uani 1 1 d . . . . .
C25 C 0.4002(2) 0.9944(2) 0.6377(2) 0.0394(7) Uani 1 1 d . . . . .
C26 C 0.4430(2) 0.8896(2) 0.5883(2) 0.0353(6) Uani 1 1 d . . . . .
C27 C 0.3936(2) 0.8402(2) 0.4755(2) 0.0367(6) Uani 1 1 d . . . . .
C28 C 0.3246(2) 0.9180(2) 0.4602(2) 0.0397(7) Uani 1 1 d . . . . .
C29 C 0.2669(3) 0.9007(3) 0.3589(2) 0.0458(7) Uani 1 1 d . . . . .
H11 H 0.2217 0.9556 0.3526 0.055 Uiso 1 1 calc R U . . .
C30 C 0.2769(3) 0.8031(3) 0.2690(2) 0.0481(8) Uani 1 1 d . . . . .
H12 H 0.2385 0.7887 0.1994 0.058 Uiso 1 1 calc R U . . .
C31 C 0.3451(3) 0.7257(3) 0.2829(2) 0.0432(7) Uani 1 1 d . . . . .
C32 C 0.4040(2) 0.7417(2) 0.3836(2) 0.0372(6) Uani 1 1 d . . . . .
C33 C 0.7154(3) 0.3801(3) 0.4066(2) 0.0461(7) Uani 1 1 d . . . . .
H13 H 0.6538 0.3204 0.3488 0.055 Uiso 1 1 calc R U . . .
H14 H 0.7201 0.3605 0.4693 0.055 Uiso 1 1 calc R U . . .
C34 C 0.8420(3) 0.3801(3) 0.3649(3) 0.0536(8) Uani 1 1 d . . . . .
H15 H 0.9070 0.4271 0.4265 0.064 Uiso 1 1 calc R U . . .
H16 H 0.8431 0.4150 0.3128 0.064 Uiso 1 1 calc R U . . .
C35 C 0.8723(3) 0.2576(3) 0.3082(3) 0.0655(10) Uani 1 1 d . . . . .
H17 H 0.9614 0.2620 0.2963 0.079 Uiso 1 1 calc R U . . .
H18 H 0.8588 0.2191 0.3568 0.079 Uiso 1 1 calc R U . . .
C36 C 0.7932(4) 0.1865(3) 0.2001(3) 0.0777(11) Uani 1 1 d . . . . .
H19 H 0.8161 0.1101 0.1679 0.117 Uiso 1 1 calc R U . . .
H20 H 0.7048 0.1802 0.2115 0.117 Uiso 1 1 calc R U . . .
H21 H 0.8075 0.2232 0.1509 0.117 Uiso 1 1 calc R U . . .
C37 C 0.7483(8) 0.9711(7) 0.8848(6) 0.0463(19) Uani 0.701(8) 1 d . . P A 4
H22 H 0.7220 1.0471 0.9135 0.056 Uiso 0.701(8) 1 calc R U P A 4
H23 H 0.7657 0.9529 0.9473 0.056 Uiso 0.701(8) 1 calc R U P A 4
C38 C 0.8655(6) 0.9786(5) 0.8359(5) 0.0476(16) Uani 0.701(8) 1 d . . P A 4
H24 H 0.8467 0.9828 0.7660 0.057 Uiso 0.701(8) 1 calc R U P A 4
H25 H 0.9019 0.9086 0.8206 0.057 Uiso 0.701(8) 1 calc R U P A 4
C39 C 0.9604(4) 1.0822(4) 0.9099(3) 0.0546(16) Uani 0.701(8) 1 d . . P A 4
H26 H 0.9185 1.1501 0.9384 0.066 Uiso 0.701(8) 1 calc R U P A 4
H27 H 0.9934 1.0699 0.9725 0.066 Uiso 0.701(8) 1 calc R U P A 4
C40 C 1.0658(6) 1.1042(6) 0.8524(6) 0.0767(18) Uani 0.701(8) 1 d . . P A 4
H28 H 1.1245 1.1713 0.9027 0.115 Uiso 0.701(8) 1 calc R U P A 4
H29 H 1.1086 1.0378 0.8252 0.115 Uiso 0.701(8) 1 calc R U P A 4
H30 H 1.0337 1.1179 0.7911 0.115 Uiso 0.701(8) 1 calc R U P A 4
C41 C 0.2934(3) 1.1188(2) 0.5626(2) 0.0448(7) Uani 1 1 d . . . . .
H31 H 0.3160 1.1255 0.4958 0.054 Uiso 1 1 calc R U . . .
H32 H 0.3435 1.1839 0.6253 0.054 Uiso 1 1 calc R U . . .
C42 C 0.1570(3) 1.1287(3) 0.5712(2) 0.0481(7) Uani 1 1 d . . . . .
H33 H 0.1358 1.1324 0.6423 0.058 Uiso 1 1 calc R U . . .
H34 H 0.1053 1.0600 0.5134 0.058 Uiso 1 1 calc R U . . .
C43 C 0.1272(3) 1.2351(3) 0.5603(3) 0.0544(8) Uani 1 1 d . . . . .
H35 H 0.1826 1.3029 0.6160 0.065 Uiso 1 1 calc R U . . .
H36 H 0.1462 1.2294 0.4881 0.065 Uiso 1 1 calc R U . . .
C44 C -0.0071(3) 1.2530(3) 0.5729(3) 0.0677(10) Uani 1 1 d . . . . .
H37 H -0.0191 1.3224 0.5650 0.101 Uiso 1 1 calc R U . . .
H38 H -0.0628 1.1873 0.5169 0.101 Uiso 1 1 calc R U . . .
H39 H -0.0264 1.2609 0.6449 0.101 Uiso 1 1 calc R U . . .
C45 C 0.2271(5) 0.5097(5) -0.0423(4) 0.1110(17) Uani 1 1 d . . . . .
O1 O 0.36905(19) 0.62685(17) 0.19971(15) 0.0499(5) Uani 1 1 d . . . . .
Cl1 Cl 0.1887(2) 0.6271(2) -0.04730(16) 0.0662(7) Uani 0.608(7) 1 d . . P B 1
Cl2 Cl 0.1025(5) 0.3802(2) -0.1285(2) 0.0982(12) Uani 0.608(7) 1 d . . P B 1
Cl3 Cl 0.1327(11) 0.6151(7) -0.0029(9) 0.255(7) Uani 0.392(7) 1 d . . P B 2
Cl4 Cl 0.1873(7) 0.4047(4) -0.1477(3) 0.0922(15) Uani 0.392(7) 1 d . . P B 2
C46 C 0.9028(15) 0.9547(14) 0.7913(12) 0.058(4) Uani 0.299(8) 1 d . U P A 3
H40 H 0.8476 0.9215 0.7218 0.069 Uiso 0.299(8) 1 calc R U P A 3
H41 H 0.9377 0.8931 0.8017 0.069 Uiso 0.299(8) 1 calc R U P A 3
C47 C 0.8328(17) 1.0217(14) 0.8881(13) 0.062(4) Uani 0.299(8) 1 d . U P A 3
H42 H 0.8926 1.0656 0.9543 0.075 Uiso 0.299(8) 1 calc R U P A 3
H43 H 0.7893 1.0759 0.8718 0.075 Uiso 0.299(8) 1 calc R U P A 3
C48 C 1.0081(16) 1.0497(14) 0.7953(14) 0.086(5) Uani 0.299(8) 1 d . U P A 3
H44 H 1.0598 1.0169 0.7367 0.129 Uiso 0.299(8) 1 calc R U P A 3
H45 H 0.9708 1.1101 0.7863 0.129 Uiso 0.299(8) 1 calc R U P A 3
H46 H 1.0601 1.0819 0.8655 0.129 Uiso 0.299(8) 1 calc R U P A 3
C49 C 0.742(2) 0.9390(17) 0.9056(15) 0.056(5) Uani 0.299(8) 1 d . U P A 3
H47 H 0.7037 0.9783 0.9731 0.067 Uiso 0.299(8) 1 calc R U P A 3
H48 H 0.7842 0.8797 0.9135 0.067 Uiso 0.299(8) 1 calc R U P A 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.392(4) . ?
C1 C6 1.414(3) . ?
C1 C32 1.439(4) . ?
C2 O1 1.390(3) . ?
C2 C3 1.390(4) . ?
C3 C4 1.396(4) . ?
C3 H1 0.9500 . ?
C4 C5 1.404(4) . ?
C4 H2 0.9500 . ?
C5 N1 1.385(3) . ?
C5 C6 1.420(4) . ?
C6 C7 1.430(4) . ?
C7 C8 1.410(3) . ?
C7 C16 1.429(4) . ?
C8 N1 1.393(3) . ?
C8 C9 1.446(4) . ?
C9 C10 1.422(4) . ?
C9 C14 1.433(4) . ?
C10 C11 1.375(4) . ?
C10 H3 0.9500 . ?
C11 C12 1.398(5) . ?
C11 H4 0.9500 . ?
C12 C13 1.379(4) . ?
C12 H5 0.9500 . ?
C13 C14 1.409(4) . ?
C13 H6 0.9500 . ?
C14 C15 1.442(4) . ?
C15 C16 1.401(4) . ?
C15 N2 1.406(4) . ?
C16 C17 1.455(4) . ?
C17 C18 1.397(4) . ?
C17 C26 1.440(4) . ?
C18 N2 1.404(3) . ?
C18 C19 1.445(4) . ?
N1 C33 1.475(3) . ?
N2 C49 1.52(2) . ?
N2 C37 1.516(9) . ?
N3 C28 1.396(4) . ?
N3 C25 1.400(3) . ?
N3 C41 1.477(3) . ?
C19 C20 1.413(4) . ?
C19 C24 1.439(4) . ?
C20 C21 1.376(4) . ?
C20 H7 0.9500 . ?
C21 C22 1.402(5) . ?
C21 H8 0.9500 . ?
C22 C23 1.367(5) . ?
C22 H9 0.9500 . ?
C23 C24 1.416(4) . ?
C23 H10 0.9500 . ?
C24 C25 1.439(4) . ?
C25 C26 1.404(4) . ?
C26 C27 1.438(4) . ?
C27 C32 1.396(4) . ?
C27 C28 1.413(4) . ?
C28 C29 1.402(4) . ?
C29 C30 1.374(4) . ?
C29 H11 0.9500 . ?
C30 C31 1.395(4) . ?
C30 H12 0.9500 . ?
C31 O1 1.385(3) . ?
C31 C32 1.406(4) . ?
C33 C34 1.516(4) . ?
C33 H13 0.9900 . ?
C33 H14 0.9900 . ?
C34 C35 1.550(4) . ?
C34 H15 0.9900 . ?
C34 H16 0.9900 . ?
C35 C36 1.517(5) . ?
C35 H17 0.9900 . ?
C35 H18 0.9900 . ?
C36 H19 0.9800 . ?
C36 H20 0.9800 . ?
C36 H21 0.9800 . ?
C37 C38 1.478(10) . ?
C37 H22 0.9900 . ?
C37 H23 0.9900 . ?
C38 C39 1.522(7) . ?
C38 H24 0.9900 . ?
C38 H25 0.9900 . ?
C39 C40 1.485(7) . ?
C39 H26 0.9900 . ?
C39 H27 0.9900 . ?
C40 H28 0.9800 . ?
C40 H29 0.9800 . ?
C40 H30 0.9800 . ?
C41 C42 1.512(4) . ?
C41 H31 0.9900 . ?
C41 H32 0.9900 . ?
C42 C43 1.531(4) . ?
C42 H33 0.9900 . ?
C42 H34 0.9900 . ?
C43 C44 1.517(4) . ?
C43 H35 0.9900 . ?
C43 H36 0.9900 . ?
C44 H37 0.9800 . ?
C44 H38 0.9800 . ?
C44 H39 0.9800 . ?
C45 Cl4 1.509(6) . ?
C45 Cl1 1.668(6) . ?
C45 Cl3 1.745(7) . ?
C45 Cl2 1.918(7) . ?
C46 C47 1.55(2) . ?
C46 C48 1.56(2) . ?
C46 H40 0.9900 . ?
C46 H41 0.9900 . ?
C47 C49 1.47(3) . ?
C47 H42 0.9900 . ?
C47 H43 0.9900 . ?
C48 H44 0.9800 . ?
C48 H45 0.9800 . ?
C48 H46 0.9800 . ?
C49 H47 0.9900 . ?
C49 H48 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
C2 C1 C6 118.7(2) . . ?
C2 C1 C32 106.2(2) . . ?
C6 C1 C32 135.0(2) . . ?
O1 C2 C3 124.1(2) . . ?
O1 C2 C1 111.4(2) . . ?
C3 C2 C1 124.5(2) . . ?
C2 C3 C4 117.4(3) . . ?
C2 C3 H1 121.3 . . ?
C4 C3 H1 121.3 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H2 120.2 . . ?
C5 C4 H2 120.2 . . ?
N1 C5 C4 128.3(2) . . ?
N1 C5 C6 108.9(2) . . ?
C4 C5 C6 122.8(2) . . ?
C1 C6 C5 117.0(2) . . ?
C1 C6 C7 136.1(2) . . ?
C5 C6 C7 106.9(2) . . ?
C8 C7 C16 119.8(2) . . ?
C8 C7 C6 106.8(2) . . ?
C16 C7 C6 133.3(2) . . ?
N1 C8 C7 109.2(2) . . ?
N1 C8 C9 128.3(2) . . ?
C7 C8 C9 122.5(2) . . ?
C10 C9 C14 117.7(2) . . ?
C10 C9 C8 124.9(3) . . ?
C14 C9 C8 117.4(2) . . ?
C11 C10 C9 122.2(3) . . ?
C11 C10 H3 118.9 . . ?
C9 C10 H3 118.9 . . ?
C10 C11 C12 119.4(3) . . ?
C10 C11 H4 120.3 . . ?
C12 C11 H4 120.3 . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H5 119.9 . . ?
C11 C12 H5 119.9 . . ?
C12 C13 C14 121.7(3) . . ?
C12 C13 H6 119.1 . . ?
C14 C13 H6 119.1 . . ?
C13 C14 C9 118.5(3) . . ?
C13 C14 C15 122.7(3) . . ?
C9 C14 C15 118.7(2) . . ?
C16 C15 N2 110.2(2) . . ?
C16 C15 C14 123.0(3) . . ?
N2 C15 C14 126.7(2) . . ?
C15 C16 C7 118.2(2) . . ?
C15 C16 C17 106.3(2) . . ?
C7 C16 C17 135.4(2) . . ?
C18 C17 C26 117.9(2) . . ?
C18 C17 C16 106.7(2) . . ?
C26 C17 C16 135.4(2) . . ?
C17 C18 N2 110.3(2) . . ?
C17 C18 C19 123.0(2) . . ?
N2 C18 C19 126.5(2) . . ?
C5 N1 C8 108.2(2) . . ?
C5 N1 C33 119.7(2) . . ?
C8 N1 C33 131.1(2) . . ?
C18 N2 C15 106.4(2) . . ?
C18 N2 C49 132.9(7) . . ?
C15 N2 C49 116.2(8) . . ?
C18 N2 C37 114.4(3) . . ?
C15 N2 C37 122.7(4) . . ?
C28 N3 C25 107.7(2) . . ?
C28 N3 C41 119.8(2) . . ?
C25 N3 C41 129.8(2) . . ?
C20 C19 C24 118.1(2) . . ?
C20 C19 C18 123.2(3) . . ?
C24 C19 C18 118.5(2) . . ?
C21 C20 C19 121.8(3) . . ?
C21 C20 H7 119.1 . . ?
C19 C20 H7 119.1 . . ?
C20 C21 C22 119.8(3) . . ?
C20 C21 H8 120.1 . . ?
C22 C21 H8 120.1 . . ?
C23 C22 C21 120.3(3) . . ?
C23 C22 H9 119.9 . . ?
C21 C22 H9 119.9 . . ?
C22 C23 C24 121.8(3) . . ?
C22 C23 H10 119.1 . . ?
C24 C23 H10 119.1 . . ?
C23 C24 C19 118.2(3) . . ?
C23 C24 C25 124.2(3) . . ?
C19 C24 C25 117.5(2) . . ?
N3 C25 C26 109.6(2) . . ?
N3 C25 C24 127.8(2) . . ?
C26 C25 C24 122.5(2) . . ?
C25 C26 C27 106.5(2) . . ?
C25 C26 C17 119.8(2) . . ?
C27 C26 C17 133.6(2) . . ?
C32 C27 C28 117.1(2) . . ?
C32 C27 C26 135.4(2) . . ?
C28 C27 C26 107.3(2) . . ?
N3 C28 C29 127.6(2) . . ?
N3 C28 C27 108.8(2) . . ?
C29 C28 C27 123.6(3) . . ?
C30 C29 C28 118.9(3) . . ?
C30 C29 H11 120.6 . . ?
C28 C29 H11 120.6 . . ?
C29 C30 C31 118.2(3) . . ?
C29 C30 H12 120.9 . . ?
C31 C30 H12 120.9 . . ?
O1 C31 C30 125.0(2) . . ?
O1 C31 C32 111.2(2) . . ?
C30 C31 C32 123.8(3) . . ?
C27 C32 C31 118.5(2) . . ?
C27 C32 C1 135.8(2) . . ?
C31 C32 C1 105.7(2) . . ?
N1 C33 C34 112.9(2) . . ?
N1 C33 H13 109.0 . . ?
C34 C33 H13 109.0 . . ?
N1 C33 H14 109.0 . . ?
C34 C33 H14 109.0 . . ?
H13 C33 H14 107.8 . . ?
C33 C34 C35 111.5(3) . . ?
C33 C34 H15 109.3 . . ?
C35 C34 H15 109.3 . . ?
C33 C34 H16 109.3 . . ?
C35 C34 H16 109.3 . . ?
H15 C34 H16 108.0 . . ?
C36 C35 C34 112.9(3) . . ?
C36 C35 H17 109.0 . . ?
C34 C35 H17 109.0 . . ?
C36 C35 H18 109.0 . . ?
C34 C35 H18 109.0 . . ?
H17 C35 H18 107.8 . . ?
C35 C36 H19 109.5 . . ?
C35 C36 H20 109.5 . . ?
H19 C36 H20 109.5 . . ?
C35 C36 H21 109.5 . . ?
H19 C36 H21 109.5 . . ?
H20 C36 H21 109.5 . . ?
C38 C37 N2 115.5(5) . . ?
C38 C37 H22 108.4 . . ?
N2 C37 H22 108.4 . . ?
C38 C37 H23 108.4 . . ?
N2 C37 H23 108.4 . . ?
H22 C37 H23 107.5 . . ?
C37 C38 C39 112.2(6) . . ?
C37 C38 H24 109.2 . . ?
C39 C38 H24 109.2 . . ?
C37 C38 H25 109.2 . . ?
C39 C38 H25 109.2 . . ?
H24 C38 H25 107.9 . . ?
C40 C39 C38 112.1(5) . . ?
C40 C39 H26 109.2 . . ?
C38 C39 H26 109.2 . . ?
C40 C39 H27 109.2 . . ?
C38 C39 H27 109.2 . . ?
H26 C39 H27 107.9 . . ?
C39 C40 H28 109.5 . . ?
C39 C40 H29 109.5 . . ?
H28 C40 H29 109.5 . . ?
C39 C40 H30 109.5 . . ?
H28 C40 H30 109.5 . . ?
H29 C40 H30 109.5 . . ?
N3 C41 C42 115.3(2) . . ?
N3 C41 H31 108.5 . . ?
C42 C41 H31 108.5 . . ?
N3 C41 H32 108.5 . . ?
C42 C41 H32 108.5 . . ?
H31 C41 H32 107.5 . . ?
C41 C42 C43 111.4(2) . . ?
C41 C42 H33 109.3 . . ?
C43 C42 H33 109.3 . . ?
C41 C42 H34 109.3 . . ?
C43 C42 H34 109.3 . . ?
H33 C42 H34 108.0 . . ?
C44 C43 C42 114.2(3) . . ?
C44 C43 H35 108.7 . . ?
C42 C43 H35 108.7 . . ?
C44 C43 H36 108.7 . . ?
C42 C43 H36 108.7 . . ?
H35 C43 H36 107.6 . . ?
C43 C44 H37 109.5 . . ?
C43 C44 H38 109.5 . . ?
H37 C44 H38 109.5 . . ?
C43 C44 H39 109.5 . . ?
H37 C44 H39 109.5 . . ?
H38 C44 H39 109.5 . . ?
Cl4 C45 Cl3 118.4(4) . . ?
Cl1 C45 Cl2 110.2(3) . . ?
C31 O1 C2 105.50(19) . . ?
C47 C46 C48 101.9(14) . . ?
C47 C46 H40 111.4 . . ?
C48 C46 H40 111.4 . . ?
C47 C46 H41 111.4 . . ?
C48 C46 H41 111.4 . . ?
H40 C46 H41 109.3 . . ?
C49 C47 C46 108.2(15) . . ?
C49 C47 H42 110.1 . . ?
C46 C47 H42 110.1 . . ?
C49 C47 H43 110.1 . . ?
C46 C47 H43 110.1 . . ?
H42 C47 H43 108.4 . . ?
C46 C48 H44 109.5 . . ?
C46 C48 H45 109.5 . . ?
H44 C48 H45 109.5 . . ?
C46 C48 H46 109.5 . . ?
H44 C48 H46 109.5 . . ?
H45 C48 H46 109.5 . . ?
C47 C49 N2 109.2(13) . . ?
C47 C49 H47 109.8 . . ?
N2 C49 H47 109.8 . . ?
C47 C49 H48 109.8 . . ?
N2 C49 H48 109.8 . . ?
H47 C49 H48 108.3 . . ?

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
C6 C1 C2 O1 -178.0(2) . . . . ?
C32 C1 C2 O1 -0.2(3) . . . . ?
C6 C1 C2 C3 0.5(4) . . . . ?
C32 C1 C2 C3 178.3(3) . . . . ?
O1 C2 C3 C4 179.2(3) . . . . ?
C1 C2 C3 C4 0.9(5) . . . . ?
C2 C3 C4 C5 -1.6(4) . . . . ?
C3 C4 C5 N1 -178.5(3) . . . . ?
C3 C4 C5 C6 1.0(4) . . . . ?
C2 C1 C6 C5 -1.2(4) . . . . ?
C32 C1 C6 C5 -178.1(3) . . . . ?
C2 C1 C6 C7 177.0(3) . . . . ?
C32 C1 C6 C7 0.1(5) . . . . ?
N1 C5 C6 C1 -180.0(2) . . . . ?
C4 C5 C6 C1 0.4(4) . . . . ?
N1 C5 C6 C7 1.3(3) . . . . ?
C4 C5 C6 C7 -178.2(3) . . . . ?
C1 C6 C7 C8 -179.1(3) . . . . ?
C5 C6 C7 C8 -0.8(3) . . . . ?
C1 C6 C7 C16 -2.0(5) . . . . ?
C5 C6 C7 C16 176.3(3) . . . . ?
C16 C7 C8 N1 -177.5(2) . . . . ?
C6 C7 C8 N1 0.0(3) . . . . ?
C16 C7 C8 C9 1.1(4) . . . . ?
C6 C7 C8 C9 178.7(2) . . . . ?
N1 C8 C9 C10 -1.5(4) . . . . ?
C7 C8 C9 C10 -179.9(3) . . . . ?
N1 C8 C9 C14 179.5(3) . . . . ?
C7 C8 C9 C14 1.1(4) . . . . ?
C14 C9 C10 C11 3.4(4) . . . . ?
C8 C9 C10 C11 -175.6(3) . . . . ?
C9 C10 C11 C12 -0.4(5) . . . . ?
C10 C11 C12 C13 -1.3(6) . . . . ?
C11 C12 C13 C14 -0.1(6) . . . . ?
C12 C13 C14 C9 3.1(5) . . . . ?
C12 C13 C14 C15 -178.2(3) . . . . ?
C10 C9 C14 C13 -4.6(4) . . . . ?
C8 C9 C14 C13 174.4(3) . . . . ?
C10 C9 C14 C15 176.7(3) . . . . ?
C8 C9 C14 C15 -4.3(4) . . . . ?
C13 C14 C15 C16 -173.1(3) . . . . ?
C9 C14 C15 C16 5.6(4) . . . . ?
C13 C14 C15 N2 5.2(5) . . . . ?
C9 C14 C15 N2 -176.1(3) . . . . ?
N2 C15 C16 C7 178.1(2) . . . . ?
C14 C15 C16 C7 -3.3(4) . . . . ?
N2 C15 C16 C17 -1.2(3) . . . . ?
C14 C15 C16 C17 177.3(3) . . . . ?
C8 C7 C16 C15 -0.1(4) . . . . ?
C6 C7 C16 C15 -176.9(3) . . . . ?
C8 C7 C16 C17 179.0(3) . . . . ?
C6 C7 C16 C17 2.2(5) . . . . ?
C15 C16 C17 C18 0.2(3) . . . . ?
C7 C16 C17 C18 -179.0(3) . . . . ?
C15 C16 C17 C26 178.9(3) . . . . ?
C7 C16 C17 C26 -0.3(5) . . . . ?
C26 C17 C18 N2 -178.1(2) . . . . ?
C16 C17 C18 N2 0.9(3) . . . . ?
C26 C17 C18 C19 6.1(4) . . . . ?
C16 C17 C18 C19 -174.9(3) . . . . ?
C4 C5 N1 C8 178.2(3) . . . . ?
C6 C5 N1 C8 -1.3(3) . . . . ?
C4 C5 N1 C33 -11.6(4) . . . . ?
C6 C5 N1 C33 168.9(2) . . . . ?
C7 C8 N1 C5 0.8(3) . . . . ?
C9 C8 N1 C5 -177.8(3) . . . . ?
C7 C8 N1 C33 -167.9(3) . . . . ?
C9 C8 N1 C33 13.6(5) . . . . ?
C17 C18 N2 C15 -1.7(3) . . . . ?
C19 C18 N2 C15 174.0(3) . . . . ?
C17 C18 N2 C49 152.8(12) . . . . ?
C19 C18 N2 C49 -31.6(12) . . . . ?
C17 C18 N2 C37 137.0(4) . . . . ?
C19 C18 N2 C37 -47.4(5) . . . . ?
C16 C15 N2 C18 1.8(3) . . . . ?
C14 C15 N2 C18 -176.7(3) . . . . ?
C16 C15 N2 C49 -157.6(9) . . . . ?
C14 C15 N2 C49 23.9(10) . . . . ?
C16 C15 N2 C37 -132.6(4) . . . . ?
C14 C15 N2 C37 48.9(5) . . . . ?
C17 C18 C19 C20 167.4(3) . . . . ?
N2 C18 C19 C20 -7.7(5) . . . . ?
C17 C18 C19 C24 -7.6(4) . . . . ?
N2 C18 C19 C24 177.3(3) . . . . ?
C24 C19 C20 C21 -3.1(5) . . . . ?
C18 C19 C20 C21 -178.2(3) . . . . ?
C19 C20 C21 C22 0.7(6) . . . . ?
C20 C21 C22 C23 2.1(6) . . . . ?
C21 C22 C23 C24 -2.4(6) . . . . ?
C22 C23 C24 C19 -0.1(5) . . . . ?
C22 C23 C24 C25 175.9(3) . . . . ?
C20 C19 C24 C23 2.7(4) . . . . ?
C18 C19 C24 C23 178.1(3) . . . . ?
C20 C19 C24 C25 -173.6(3) . . . . ?
C18 C19 C24 C25 1.8(4) . . . . ?
C28 N3 C25 C26 0.2(3) . . . . ?
C41 N3 C25 C26 -160.7(3) . . . . ?
C28 N3 C25 C24 -176.0(3) . . . . ?
C41 N3 C25 C24 23.1(4) . . . . ?
C23 C24 C25 N3 5.1(5) . . . . ?
C19 C24 C25 N3 -178.9(3) . . . . ?
C23 C24 C25 C26 -170.7(3) . . . . ?
C19 C24 C25 C26 5.3(4) . . . . ?
N3 C25 C26 C27 -0.8(3) . . . . ?
C24 C25 C26 C27 175.6(2) . . . . ?
N3 C25 C26 C17 176.6(2) . . . . ?
C24 C25 C26 C17 -6.9(4) . . . . ?
C18 C17 C26 C25 1.1(4) . . . . ?
C16 C17 C26 C25 -177.5(3) . . . . ?
C18 C17 C26 C27 177.8(3) . . . . ?
C16 C17 C26 C27 -0.9(5) . . . . ?
C25 C26 C27 C32 177.2(3) . . . . ?
C17 C26 C27 C32 0.3(6) . . . . ?
C25 C26 C27 C28 1.2(3) . . . . ?
C17 C26 C27 C28 -175.8(3) . . . . ?
C25 N3 C28 C29 -177.6(3) . . . . ?
C41 N3 C28 C29 -14.5(4) . . . . ?
C25 N3 C28 C27 0.6(3) . . . . ?
C41 N3 C28 C27 163.7(2) . . . . ?
C32 C27 C28 N3 -178.0(2) . . . . ?
C26 C27 C28 N3 -1.1(3) . . . . ?
C32 C27 C28 C29 0.3(4) . . . . ?
C26 C27 C28 C29 177.2(3) . . . . ?
N3 C28 C29 C30 178.1(3) . . . . ?
C27 C28 C29 C30 0.2(4) . . . . ?
C28 C29 C30 C31 -0.4(4) . . . . ?
C29 C30 C31 O1 -176.5(3) . . . . ?
C29 C30 C31 C32 0.1(5) . . . . ?
C28 C27 C32 C31 -0.6(4) . . . . ?
C26 C27 C32 C31 -176.3(3) . . . . ?
C28 C27 C32 C1 175.7(3) . . . . ?
C26 C27 C32 C1 -0.1(6) . . . . ?
O1 C31 C32 C27 177.4(2) . . . . ?
C30 C31 C32 C27 0.4(4) . . . . ?
O1 C31 C32 C1 0.1(3) . . . . ?
C30 C31 C32 C1 -176.9(3) . . . . ?
C2 C1 C32 C27 -176.5(3) . . . . ?
C6 C1 C32 C27 0.7(6) . . . . ?
C2 C1 C32 C31 0.1(3) . . . . ?
C6 C1 C32 C31 177.3(3) . . . . ?
C5 N1 C33 C34 93.0(3) . . . . ?
C8 N1 C33 C34 -99.4(3) . . . . ?
N1 C33 C34 C35 -168.0(2) . . . . ?
C33 C34 C35 C36 70.6(4) . . . . ?
C18 N2 C37 C38 -96.1(5) . . . . ?
C15 N2 C37 C38 35.1(6) . . . . ?
N2 C37 C38 C39 169.2(4) . . . . ?
C37 C38 C39 C40 -167.5(5) . . . . ?
C28 N3 C41 C42 90.5(3) . . . . ?
C25 N3 C41 C42 -110.6(3) . . . . ?
N3 C41 C42 C43 -173.4(2) . . . . ?
C41 C42 C43 C44 -177.6(3) . . . . ?
C30 C31 O1 C2 176.7(3) . . . . ?
C32 C31 O1 C2 -0.2(3) . . . . ?
C3 C2 O1 C31 -178.2(3) . . . . ?
C1 C2 O1 C31 0.3(3) . . . . ?
C48 C46 C47 C49 -171.1(11) . . . . ?
C46 C47 C49 N2 -67.2(17) . . . . ?
C18 N2 C49 C47 -57.3(19) . . . . ?
C15 N2 C49 C47 95.2(14) . . . . ?

_refine_diff_density_max         0.315
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.054

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_181030matsuo
_audit_block_doi                 10.5517/ccdc.csd.cc23kw8v
_database_code_depnum_ccdc_archive 'CCDC 1953597'
loop_
_audit_author_name
_audit_author_address
'Yusuke Matsuo'
;Kyoto University
Japan
;
_audit_update_record             
;
2019-09-14 deposited with the CCDC.	2019-10-30 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_sum            'C42 H37 N3 O4'
_chemical_formula_moiety         'C34 H21 N3 O2, 2(C4 H8 O)'
_chemical_formula_weight         647.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.5709(4)
_cell_length_b                   24.7927(5)
_cell_length_c                   11.9563(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.905(3)
_cell_angle_gamma                90
_cell_volume                     3126.25(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    16785
_cell_measurement_theta_min      3.5410
_cell_measurement_theta_max      69.3700

_exptl_crystal_description       Prism
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_F_000             1368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.708
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_reflns_number            56541
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.565
_diffrn_reflns_theta_max         66.979
_diffrn_reflns_theta_full        66.979
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             5407
_reflns_number_gt                4138
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²+9.4715P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5407
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0887
_refine_ls_wR_factor_ref         0.3301
_refine_ls_wR_factor_gt          0.3067
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1963(3) 0.76145(14) 0.3777(3) 0.0316(8) Uani 1 1 d . . . . .
O2 O 0.2160(3) 0.73668(13) 0.5944(3) 0.0293(8) Uani 1 1 d . . . . .
C1 C 0.3992(5) 0.72613(18) 0.4422(4) 0.0243(10) Uani 1 1 d . . . . .
C2 C 0.2844(5) 0.72028(19) 0.3769(4) 0.0281(11) Uani 1 1 d . . . . .
C3 C 0.2532(5) 0.67295(19) 0.3161(4) 0.0280(11) Uani 1 1 d . . . . .
H1 H 0.1743 0.6708 0.2732 0.034 Uiso 1 1 calc R U . . .
C4 C 0.3354(5) 0.62936(19) 0.3177(4) 0.0289(11) Uani 1 1 d . . . . .
H2 H 0.3111 0.5958 0.2843 0.035 Uiso 1 1 calc R U . . .
C5 C 0.4547(5) 0.63705(18) 0.3705(4) 0.0270(11) Uani 1 1 d . . . . .
C6 C 0.4919(5) 0.68524(17) 0.4264(4) 0.0243(10) Uani 1 1 d . . . . .
C7 C 0.6269(5) 0.68040(18) 0.4528(4) 0.0247(10) Uani 1 1 d . . . . .
C8 C 0.6617(5) 0.62827(18) 0.4211(4) 0.0255(10) Uani 1 1 d . . . . .
C9 C 0.7902(5) 0.60907(18) 0.4265(4) 0.0262(10) Uani 1 1 d . . . . .
C10 C 0.8226(5) 0.55557(18) 0.4008(4) 0.0293(11) Uani 1 1 d . . . . .
H3 H 0.7574 0.5299 0.3840 0.035 Uiso 1 1 calc R U . . .
C11 C 0.9471(5) 0.54016(19) 0.3999(4) 0.0304(11) Uani 1 1 d . . . . .
H4 H 0.9674 0.5043 0.3796 0.036 Uiso 1 1 calc R U . . .
C12 C 1.0443(5) 0.5769(2) 0.4285(4) 0.0330(12) Uani 1 1 d . . . . .
H5 H 1.1302 0.5657 0.4289 0.040 Uiso 1 1 calc R U . . .
C13 C 1.0164(5) 0.62963(19) 0.4562(4) 0.0288(11) Uani 1 1 d . . . . .
H6 H 1.0831 0.6541 0.4770 0.035 Uiso 1 1 calc R U . . .
C14 C 0.8889(5) 0.64694(18) 0.4538(4) 0.0256(10) Uani 1 1 d . . . . .
C15 C 0.8525(5) 0.70156(18) 0.4719(4) 0.0253(10) Uani 1 1 d . . . . .
C16 C 0.7264(5) 0.71851(18) 0.4758(4) 0.0245(10) Uani 1 1 d . . . . .
C17 C 0.7296(5) 0.77564(18) 0.4886(4) 0.0243(10) Uani 1 1 d . . . . .
C18 C 0.8566(5) 0.79123(18) 0.4922(4) 0.0255(10) Uani 1 1 d . . . . .
C19 C 0.8999(5) 0.84522(19) 0.5133(4) 0.0269(11) Uani 1 1 d . . . . .
C20 C 1.0282(5) 0.8608(2) 0.5158(4) 0.0308(11) Uani 1 1 d . . . . .
H7 H 1.0904 0.8358 0.4949 0.037 Uiso 1 1 calc R U . . .
O3 O 0.5831(4) 0.47776(14) 0.3058(3) 0.0339(9) Uani 1 1 d . . . . .
O4 O 0.6328(4) 1.00628(14) 0.7042(3) 0.0376(9) Uani 1 1 d . . . . .
C21 C 1.0639(5) 0.9120(2) 0.5484(4) 0.0342(12) Uani 1 1 d . . . . .
H8 H 1.1508 0.9221 0.5515 0.041 Uiso 1 1 calc R U . . .
C22 C 0.9719(5) 0.9498(2) 0.5773(4) 0.0335(12) Uani 1 1 d . . . . .
H9 H 0.9976 0.9849 0.6014 0.040 Uiso 1 1 calc R U . . .
C23 C 0.8469(5) 0.93651(19) 0.5709(4) 0.0301(11) Uani 1 1 d . . . . .
H10 H 0.7857 0.9630 0.5869 0.036 Uiso 1 1 calc R U . . .
C24 C 0.8070(5) 0.88378(18) 0.5407(4) 0.0261(10) Uani 1 1 d . . . . .
C25 C 0.6785(5) 0.86626(18) 0.5436(4) 0.0255(10) Uani 1 1 d . . . . .
C26 C 0.6350(5) 0.81489(18) 0.5119(4) 0.0231(10) Uani 1 1 d . . . . .
C27 C 0.5047(5) 0.81072(18) 0.5404(4) 0.0244(10) Uani 1 1 d . . . . .
C28 C 0.4818(5) 0.85945(18) 0.5996(4) 0.0256(10) Uani 1 1 d . . . . .
C29 C 0.3761(5) 0.86612(19) 0.6596(4) 0.0282(11) Uani 1 1 d . . . . .
H11 H 0.3618 0.8989 0.6981 0.034 Uiso 1 1 calc R U . . .
C30 C 0.2916(5) 0.82373(19) 0.6620(4) 0.0296(11) Uani 1 1 d . . . . .
H12 H 0.2229 0.8259 0.7091 0.036 Uiso 1 1 calc R U . . .
C31 C 0.3056(5) 0.77727(19) 0.5957(4) 0.0272(10) Uani 1 1 d . . . . .
C32 C 0.4082(5) 0.77102(18) 0.5267(4) 0.0246(10) Uani 1 1 d . . . . .
C33 C 0.1263(6) 0.7722(2) 0.2737(5) 0.0411(14) Uani 1 1 d . . . . .
H13 H 0.0670 0.8020 0.2836 0.062 Uiso 1 1 calc R U . . .
H14 H 0.1849 0.7822 0.2171 0.062 Uiso 1 1 calc R U . . .
H15 H 0.0789 0.7399 0.2490 0.062 Uiso 1 1 calc R U . . .
C34 C 0.1489(5) 0.7307(2) 0.6931(4) 0.0350(12) Uani 1 1 d . . . . .
H16 H 0.0882 0.7009 0.6829 0.052 Uiso 1 1 calc R U . . .
H17 H 0.2092 0.7228 0.7570 0.052 Uiso 1 1 calc R U . . .
H18 H 0.1033 0.7641 0.7074 0.052 Uiso 1 1 calc R U . . .
C35 C 0.5786(6) 0.4403(2) 0.3977(5) 0.0379(13) Uani 1 1 d . . . . .
H19 H 0.4896 0.4326 0.4131 0.045 Uiso 1 1 calc R U . . .
H20 H 0.6227 0.4555 0.4663 0.045 Uiso 1 1 calc R U . . .
C36 C 0.6446(6) 0.3891(2) 0.3623(5) 0.0425(14) Uani 1 1 d . . . . .
H21 H 0.6894 0.3710 0.4273 0.051 Uiso 1 1 calc R U . . .
H22 H 0.5836 0.3635 0.3247 0.051 Uiso 1 1 calc R U . . .
C37 C 0.7369(6) 0.4105(2) 0.2817(5) 0.0383(13) Uani 1 1 d . . . . .
H23 H 0.8142 0.4252 0.3220 0.046 Uiso 1 1 calc R U . . .
H24 H 0.7612 0.3822 0.2288 0.046 Uiso 1 1 calc R U . . .
C38 C 0.6596(6) 0.4545(2) 0.2222(5) 0.0404(14) Uani 1 1 d . . . . .
H25 H 0.7157 0.4821 0.1921 0.049 Uiso 1 1 calc R U . . .
H26 H 0.6049 0.4393 0.1594 0.049 Uiso 1 1 calc R U . . .
C39 C 0.5664(7) 1.0486(3) 0.6449(6) 0.0547(17) Uani 1 1 d . . . . .
H27 H 0.4738 1.0426 0.6438 0.066 Uiso 1 1 calc R U . . .
H28 H 0.5913 1.0504 0.5667 0.066 Uiso 1 1 calc R U . . .
C40 C 0.6024(9) 1.1001(3) 0.7067(7) 0.072(2) Uani 1 1 d . . . . .
H29 H 0.5463 1.1070 0.7682 0.086 Uiso 1 1 calc R U . . .
H30 H 0.5994 1.1315 0.6554 0.086 Uiso 1 1 calc R U . . .
C41 C 0.7379(7) 1.0879(2) 0.7519(5) 0.0496(16) Uani 1 1 d . . . . .
H31 H 0.7991 1.0935 0.6940 0.060 Uiso 1 1 calc R U . . .
H32 H 0.7629 1.1102 0.8184 0.060 Uiso 1 1 calc R U . . .
C42 C 0.7275(6) 1.0295(2) 0.7822(5) 0.0398(13) Uani 1 1 d . . . . .
H33 H 0.8100 1.0112 0.7765 0.048 Uiso 1 1 calc R U . . .
H34 H 0.7020 1.0258 0.8600 0.048 Uiso 1 1 calc R U . . .
N1 N 0.5573(4) 0.60196(15) 0.3743(3) 0.0269(9) Uani 1 1 d . . . . .
H35 H 0.5555 0.5684 0.3506 0.032 Uiso 1 1 calc R U . . .
N2 N 0.9307(4) 0.74578(15) 0.4818(3) 0.0274(9) Uani 1 1 d . . . . .
H36 H 1.0139 0.7453 0.4815 0.033 Uiso 1 1 calc R U . . .
N3 N 0.5840(4) 0.89369(15) 0.5935(3) 0.0273(9) Uani 1 1 d . . . . .
H37 H 0.5880 0.9273 0.6174 0.033 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
O1 C2 1.382(6) . ?
O1 C33 1.429(6) . ?
O2 C31 1.382(6) . ?
O2 C34 1.426(6) . ?
C1 C2 1.405(7) . ?
C1 C6 1.431(6) . ?
C1 C32 1.502(6) . ?
C2 C3 1.408(7) . ?
C3 C4 1.386(7) . ?
C3 H1 0.9500 . ?
C4 C5 1.385(7) . ?
C4 H2 0.9500 . ?
C5 N1 1.389(6) . ?
C5 C6 1.411(6) . ?
C6 C7 1.445(7) . ?
C7 C8 1.403(6) . ?
C7 C16 1.427(7) . ?
C8 N1 1.368(6) . ?
C8 C9 1.437(7) . ?
C9 C10 1.409(6) . ?
C9 C14 1.425(7) . ?
C10 C11 1.371(7) . ?
C10 H3 0.9500 . ?
C11 C12 1.399(7) . ?
C11 H4 0.9500 . ?
C12 C13 1.384(7) . ?
C12 H5 0.9500 . ?
C13 C14 1.413(7) . ?
C13 H6 0.9500 . ?
C14 C15 1.428(6) . ?
C15 N2 1.374(6) . ?
C15 C16 1.401(7) . ?
C16 C17 1.425(6) . ?
C17 C18 1.395(7) . ?
C17 C26 1.436(6) . ?
C18 N2 1.383(6) . ?
C18 C19 1.431(6) . ?
C19 C20 1.409(7) . ?
C19 C24 1.425(7) . ?
C20 C21 1.374(7) . ?
C20 H7 0.9500 . ?
O3 C35 1.442(6) . ?
O3 C38 1.447(6) . ?
O4 C39 1.424(7) . ?
O4 C42 1.441(7) . ?
C21 C22 1.409(8) . ?
C21 H8 0.9500 . ?
C22 C23 1.359(8) . ?
C22 H9 0.9500 . ?
C23 C24 1.413(7) . ?
C23 H10 0.9500 . ?
C24 C25 1.428(7) . ?
C25 N3 1.378(6) . ?
C25 C26 1.398(6) . ?
C26 C27 1.445(7) . ?
C27 C32 1.419(7) . ?
C27 C28 1.430(6) . ?
C28 C29 1.379(7) . ?
C28 N3 1.379(6) . ?
C29 C30 1.381(7) . ?
C29 H11 0.9500 . ?
C30 C31 1.412(7) . ?
C30 H12 0.9500 . ?
C31 C32 1.415(7) . ?
C33 H13 0.9800 . ?
C33 H14 0.9800 . ?
C33 H15 0.9800 . ?
C34 H16 0.9800 . ?
C34 H17 0.9800 . ?
C34 H18 0.9800 . ?
C35 C36 1.523(8) . ?
C35 H19 0.9900 . ?
C35 H20 0.9900 . ?
C36 C37 1.513(8) . ?
C36 H21 0.9900 . ?
C36 H22 0.9900 . ?
C37 C38 1.512(8) . ?
C37 H23 0.9900 . ?
C37 H24 0.9900 . ?
C38 H25 0.9900 . ?
C38 H26 0.9900 . ?
C39 C40 1.510(10) . ?
C39 H27 0.9900 . ?
C39 H28 0.9900 . ?
C40 C41 1.527(11) . ?
C40 H29 0.9900 . ?
C40 H30 0.9900 . ?
C41 C42 1.496(8) . ?
C41 H31 0.9900 . ?
C41 H32 0.9900 . ?
C42 H33 0.9900 . ?
C42 H34 0.9900 . ?
N1 H35 0.8800 . ?
N2 H36 0.8800 . ?
N3 H37 0.8800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 C33 116.2(4) . . ?
C31 O2 C34 116.5(4) . . ?
C2 C1 C6 115.3(4) . . ?
C2 C1 C32 117.6(4) . . ?
C6 C1 C32 127.0(4) . . ?
O1 C2 C1 118.5(4) . . ?
O1 C2 C3 119.0(5) . . ?
C1 C2 C3 122.4(5) . . ?
C4 C3 C2 121.2(5) . . ?
C4 C3 H1 119.4 . . ?
C2 C3 H1 119.4 . . ?
C5 C4 C3 116.7(4) . . ?
C5 C4 H2 121.6 . . ?
C3 C4 H2 121.6 . . ?
C4 C5 N1 127.9(4) . . ?
C4 C5 C6 123.2(5) . . ?
N1 C5 C6 108.9(4) . . ?
C5 C6 C1 119.4(5) . . ?
C5 C6 C7 105.8(4) . . ?
C1 C6 C7 134.8(4) . . ?
C8 C7 C16 117.3(4) . . ?
C8 C7 C6 106.9(4) . . ?
C16 C7 C6 133.7(4) . . ?
N1 C8 C7 109.3(4) . . ?
N1 C8 C9 126.5(4) . . ?
C7 C8 C9 123.9(4) . . ?
C10 C9 C14 119.0(4) . . ?
C10 C9 C8 123.0(4) . . ?
C14 C9 C8 117.9(4) . . ?
C11 C10 C9 120.8(5) . . ?
C11 C10 H3 119.6 . . ?
C9 C10 H3 119.6 . . ?
C10 C11 C12 120.4(5) . . ?
C10 C11 H4 119.8 . . ?
C12 C11 H4 119.8 . . ?
C13 C12 C11 120.6(5) . . ?
C13 C12 H5 119.7 . . ?
C11 C12 H5 119.7 . . ?
C12 C13 C14 120.0(5) . . ?
C12 C13 H6 120.0 . . ?
C14 C13 H6 120.0 . . ?
C13 C14 C9 119.2(4) . . ?
C13 C14 C15 123.5(5) . . ?
C9 C14 C15 117.3(4) . . ?
N2 C15 C16 109.0(4) . . ?
N2 C15 C14 127.1(4) . . ?
C16 C15 C14 123.8(4) . . ?
C15 C16 C17 106.6(4) . . ?
C15 C16 C7 119.0(4) . . ?
C17 C16 C7 133.7(4) . . ?
C18 C17 C16 107.1(4) . . ?
C18 C17 C26 119.2(4) . . ?
C16 C17 C26 133.1(4) . . ?
N2 C18 C17 108.8(4) . . ?
N2 C18 C19 127.0(5) . . ?
C17 C18 C19 124.1(4) . . ?
C20 C19 C24 119.2(4) . . ?
C20 C19 C18 123.8(5) . . ?
C24 C19 C18 116.8(4) . . ?
C21 C20 C19 120.3(5) . . ?
C21 C20 H7 119.8 . . ?
C19 C20 H7 119.8 . . ?
C35 O3 C38 108.6(4) . . ?
C39 O4 C42 108.9(4) . . ?
C20 C21 C22 120.2(5) . . ?
C20 C21 H8 119.9 . . ?
C22 C21 H8 119.9 . . ?
C23 C22 C21 120.6(5) . . ?
C23 C22 H9 119.7 . . ?
C21 C22 H9 119.7 . . ?
C22 C23 C24 120.7(5) . . ?
C22 C23 H10 119.6 . . ?
C24 C23 H10 119.6 . . ?
C23 C24 C19 118.7(5) . . ?
C23 C24 C25 122.9(4) . . ?
C19 C24 C25 118.2(4) . . ?
N3 C25 C26 109.4(4) . . ?
N3 C25 C24 125.4(4) . . ?
C26 C25 C24 124.5(4) . . ?
C25 C26 C17 116.7(4) . . ?
C25 C26 C27 107.6(4) . . ?
C17 C26 C27 133.2(4) . . ?
C32 C27 C28 119.9(4) . . ?
C32 C27 C26 135.4(4) . . ?
C28 C27 C26 104.6(4) . . ?
C29 C28 N3 128.2(4) . . ?
C29 C28 C27 122.0(4) . . ?
N3 C28 C27 109.5(4) . . ?
C28 C29 C30 117.9(4) . . ?
C28 C29 H11 121.0 . . ?
C30 C29 H11 121.0 . . ?
C29 C30 C31 121.1(4) . . ?
C29 C30 H12 119.5 . . ?
C31 C30 H12 119.5 . . ?
O2 C31 C30 120.1(4) . . ?
O2 C31 C32 117.8(4) . . ?
C30 C31 C32 122.0(4) . . ?
C31 C32 C27 115.5(4) . . ?
C31 C32 C1 117.2(4) . . ?
C27 C32 C1 127.1(4) . . ?
O1 C33 H13 109.5 . . ?
O1 C33 H14 109.5 . . ?
H13 C33 H14 109.5 . . ?
O1 C33 H15 109.5 . . ?
H13 C33 H15 109.5 . . ?
H14 C33 H15 109.5 . . ?
O2 C34 H16 109.5 . . ?
O2 C34 H17 109.5 . . ?
H16 C34 H17 109.5 . . ?
O2 C34 H18 109.5 . . ?
H16 C34 H18 109.5 . . ?
H17 C34 H18 109.5 . . ?
O3 C35 C36 106.6(4) . . ?
O3 C35 H19 110.4 . . ?
C36 C35 H19 110.4 . . ?
O3 C35 H20 110.4 . . ?
C36 C35 H20 110.4 . . ?
H19 C35 H20 108.6 . . ?
C37 C36 C35 102.3(4) . . ?
C37 C36 H21 111.3 . . ?
C35 C36 H21 111.3 . . ?
C37 C36 H22 111.3 . . ?
C35 C36 H22 111.3 . . ?
H21 C36 H22 109.2 . . ?
C38 C37 C36 101.6(5) . . ?
C38 C37 H23 111.5 . . ?
C36 C37 H23 111.5 . . ?
C38 C37 H24 111.5 . . ?
C36 C37 H24 111.5 . . ?
H23 C37 H24 109.3 . . ?
O3 C38 C37 105.8(4) . . ?
O3 C38 H25 110.6 . . ?
C37 C38 H25 110.6 . . ?
O3 C38 H26 110.6 . . ?
C37 C38 H26 110.6 . . ?
H25 C38 H26 108.7 . . ?
O4 C39 C40 106.3(6) . . ?
O4 C39 H27 110.5 . . ?
C40 C39 H27 110.5 . . ?
O4 C39 H28 110.5 . . ?
C40 C39 H28 110.5 . . ?
H27 C39 H28 108.7 . . ?
C39 C40 C41 101.8(6) . . ?
C39 C40 H29 111.4 . . ?
C41 C40 H29 111.4 . . ?
C39 C40 H30 111.4 . . ?
C41 C40 H30 111.4 . . ?
H29 C40 H30 109.3 . . ?
C42 C41 C40 101.3(5) . . ?
C42 C41 H31 111.5 . . ?
C40 C41 H31 111.5 . . ?
C42 C41 H32 111.5 . . ?
C40 C41 H32 111.5 . . ?
H31 C41 H32 109.3 . . ?
O4 C42 C41 106.8(5) . . ?
O4 C42 H33 110.4 . . ?
C41 C42 H33 110.4 . . ?
O4 C42 H34 110.4 . . ?
C41 C42 H34 110.4 . . ?
H33 C42 H34 108.6 . . ?
C8 N1 C5 108.7(4) . . ?
C8 N1 H35 125.6 . . ?
C5 N1 H35 125.6 . . ?
C15 N2 C18 108.5(4) . . ?
C15 N2 H36 125.8 . . ?
C18 N2 H36 125.8 . . ?
C25 N3 C28 108.2(4) . . ?
C25 N3 H37 125.9 . . ?
C28 N3 H37 125.9 . . ?

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
C33 O1 C2 C1 143.1(5) . . . . ?
C33 O1 C2 C3 -40.4(6) . . . . ?
C6 C1 C2 O1 -172.5(4) . . . . ?
C32 C1 C2 O1 12.5(6) . . . . ?
C6 C1 C2 C3 11.2(7) . . . . ?
C32 C1 C2 C3 -163.9(4) . . . . ?
O1 C2 C3 C4 -176.4(4) . . . . ?
C1 C2 C3 C4 0.0(7) . . . . ?
C2 C3 C4 C5 -7.5(7) . . . . ?
C3 C4 C5 N1 -173.3(4) . . . . ?
C3 C4 C5 C6 3.5(7) . . . . ?
C4 C5 C6 C1 7.9(7) . . . . ?
N1 C5 C6 C1 -174.7(4) . . . . ?
C4 C5 C6 C7 -170.7(4) . . . . ?
N1 C5 C6 C7 6.7(5) . . . . ?
C2 C1 C6 C5 -14.7(6) . . . . ?
C32 C1 C6 C5 159.8(4) . . . . ?
C2 C1 C6 C7 163.4(5) . . . . ?
C32 C1 C6 C7 -22.1(8) . . . . ?
C5 C6 C7 C8 -5.2(5) . . . . ?
C1 C6 C7 C8 176.6(5) . . . . ?
C5 C6 C7 C16 157.3(5) . . . . ?
C1 C6 C7 C16 -21.0(9) . . . . ?
C16 C7 C8 N1 -164.1(4) . . . . ?
C6 C7 C8 N1 1.7(5) . . . . ?
C16 C7 C8 C9 9.5(7) . . . . ?
C6 C7 C8 C9 175.4(4) . . . . ?
N1 C8 C9 C10 -11.5(7) . . . . ?
C7 C8 C9 C10 176.0(4) . . . . ?
N1 C8 C9 C14 165.3(4) . . . . ?
C7 C8 C9 C14 -7.3(7) . . . . ?
C14 C9 C10 C11 -1.2(7) . . . . ?
C8 C9 C10 C11 175.5(4) . . . . ?
C9 C10 C11 C12 2.4(7) . . . . ?
C10 C11 C12 C13 -1.1(8) . . . . ?
C11 C12 C13 C14 -1.2(7) . . . . ?
C12 C13 C14 C9 2.3(7) . . . . ?
C12 C13 C14 C15 -174.5(5) . . . . ?
C10 C9 C14 C13 -1.1(7) . . . . ?
C8 C9 C14 C13 -178.0(4) . . . . ?
C10 C9 C14 C15 175.9(4) . . . . ?
C8 C9 C14 C15 -1.0(6) . . . . ?
C13 C14 C15 N2 7.6(8) . . . . ?
C9 C14 C15 N2 -169.2(4) . . . . ?
C13 C14 C15 C16 -176.3(4) . . . . ?
C9 C14 C15 C16 6.9(7) . . . . ?
N2 C15 C16 C17 0.0(5) . . . . ?
C14 C15 C16 C17 -176.7(4) . . . . ?
N2 C15 C16 C7 172.1(4) . . . . ?
C14 C15 C16 C7 -4.6(7) . . . . ?
C8 C7 C16 C15 -3.5(6) . . . . ?
C6 C7 C16 C15 -164.6(5) . . . . ?
C8 C7 C16 C17 165.9(5) . . . . ?
C6 C7 C16 C17 4.9(9) . . . . ?
C15 C16 C17 C18 -0.1(5) . . . . ?
C7 C16 C17 C18 -170.5(5) . . . . ?
C15 C16 C17 C26 -170.7(5) . . . . ?
C7 C16 C17 C26 18.9(9) . . . . ?
C16 C17 C18 N2 0.2(5) . . . . ?
C26 C17 C18 N2 172.3(4) . . . . ?
C16 C17 C18 C19 -174.9(4) . . . . ?
C26 C17 C18 C19 -2.8(7) . . . . ?
N2 C18 C19 C20 6.4(8) . . . . ?
C17 C18 C19 C20 -179.4(5) . . . . ?
N2 C18 C19 C24 -169.0(4) . . . . ?
C17 C18 C19 C24 5.1(7) . . . . ?
C24 C19 C20 C21 2.4(7) . . . . ?
C18 C19 C20 C21 -173.0(5) . . . . ?
C19 C20 C21 C22 -1.4(8) . . . . ?
C20 C21 C22 C23 -1.5(8) . . . . ?
C21 C22 C23 C24 3.2(8) . . . . ?
C22 C23 C24 C19 -2.1(7) . . . . ?
C22 C23 C24 C25 173.6(5) . . . . ?
C20 C19 C24 C23 -0.7(7) . . . . ?
C18 C19 C24 C23 175.0(4) . . . . ?
C20 C19 C24 C25 -176.6(4) . . . . ?
C18 C19 C24 C25 -0.9(7) . . . . ?
C23 C24 C25 N3 -12.2(8) . . . . ?
C19 C24 C25 N3 163.5(4) . . . . ?
C23 C24 C25 C26 178.4(5) . . . . ?
C19 C24 C25 C26 -5.9(7) . . . . ?
N3 C25 C26 C17 -162.6(4) . . . . ?
C24 C25 C26 C17 8.2(7) . . . . ?
N3 C25 C26 C27 1.9(5) . . . . ?
C24 C25 C26 C27 172.7(4) . . . . ?
C18 C17 C26 C25 -3.7(6) . . . . ?
C16 C17 C26 C25 165.9(5) . . . . ?
C18 C17 C26 C27 -163.3(5) . . . . ?
C16 C17 C26 C27 6.3(9) . . . . ?
C25 C26 C27 C32 177.2(5) . . . . ?
C17 C26 C27 C32 -21.8(9) . . . . ?
C25 C26 C27 C28 -5.9(5) . . . . ?
C17 C26 C27 C28 155.0(5) . . . . ?
C32 C27 C28 C29 10.3(7) . . . . ?
C26 C27 C28 C29 -167.1(5) . . . . ?
C32 C27 C28 N3 -174.6(4) . . . . ?
C26 C27 C28 N3 7.9(5) . . . . ?
N3 C28 C29 C30 -173.5(5) . . . . ?
C27 C28 C29 C30 0.5(7) . . . . ?
C28 C29 C30 C31 -6.7(8) . . . . ?
C34 O2 C31 C30 -28.4(7) . . . . ?
C34 O2 C31 C32 153.3(5) . . . . ?
C29 C30 C31 O2 -176.2(5) . . . . ?
C29 C30 C31 C32 2.1(8) . . . . ?
O2 C31 C32 C27 -173.3(4) . . . . ?
C30 C31 C32 C27 8.4(7) . . . . ?
O2 C31 C32 C1 11.0(7) . . . . ?
C30 C31 C32 C1 -167.4(5) . . . . ?
C28 C27 C32 C31 -14.2(7) . . . . ?
C26 C27 C32 C31 162.3(5) . . . . ?
C28 C27 C32 C1 161.0(5) . . . . ?
C26 C27 C32 C1 -22.5(9) . . . . ?
C2 C1 C32 C31 46.3(6) . . . . ?
C6 C1 C32 C31 -128.1(5) . . . . ?
C2 C1 C32 C27 -128.9(5) . . . . ?
C6 C1 C32 C27 56.8(7) . . . . ?
C38 O3 C35 C36 -6.1(6) . . . . ?
O3 C35 C36 C37 27.9(6) . . . . ?
C35 C36 C37 C38 -37.8(6) . . . . ?
C35 O3 C38 C37 -18.5(6) . . . . ?
C36 C37 C38 O3 35.3(6) . . . . ?
C42 O4 C39 C40 -12.6(7) . . . . ?
O4 C39 C40 C41 31.8(8) . . . . ?
C39 C40 C41 C42 -37.8(7) . . . . ?
C39 O4 C42 C41 -12.4(6) . . . . ?
C40 C41 C42 O4 31.6(6) . . . . ?
C7 C8 N1 C5 2.5(5) . . . . ?
C9 C8 N1 C5 -170.9(4) . . . . ?
C4 C5 N1 C8 171.4(5) . . . . ?
C6 C5 N1 C8 -5.9(5) . . . . ?
C16 C15 N2 C18 0.1(5) . . . . ?
C14 C15 N2 C18 176.7(5) . . . . ?
C17 C18 N2 C15 -0.1(5) . . . . ?
C19 C18 N2 C15 174.7(5) . . . . ?
C26 C25 N3 C28 3.1(5) . . . . ?
C24 C25 N3 C28 -167.6(4) . . . . ?
C29 C28 N3 C25 167.7(5) . . . . ?
C27 C28 N3 C25 -7.0(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
N1 H35 O3 0.88 2.33 3.203(5) 170.3 .
N2 H36 O1 0.88 2.40 3.171(6) 147.0 1_655
N2 H36 O2 0.88 2.46 3.225(6) 146.2 1_655
N3 H37 O4 0.88 2.25 3.117(5) 167.5 .
N1 H35 O3 0.88 2.33 3.203(5) 170.3 .
N2 H36 O1 0.88 2.40 3.171(6) 147.0 1_655

_refine_diff_density_max         0.721
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.135

####################################################################### 
# 
# 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_my
_audit_block_doi                 10.5517/ccdc.csd.cc23kw6s
_database_code_depnum_ccdc_archive 'CCDC 1953595'
loop_
_audit_author_name
_audit_author_address
'Yusuke Matsuo'
;Kyoto University
Japan
;
_audit_update_record             
;
2019-09-14 deposited with the CCDC.	2019-10-30 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         'C46 H45 N3 O2, C2 H6 O S'
_chemical_formula_sum            'C96 H102 N6 O6 S2'
_chemical_formula_weight         1499.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.877(2)
_cell_length_b                   15.0887(14)
_cell_length_c                   17.9227(12)
_cell_angle_alpha                71.320(5)
_cell_angle_beta                 89.990(11)
_cell_angle_gamma                89.980(12)
_cell_volume                     3811.3(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    4108
_cell_measurement_theta_min      24.7
_cell_measurement_theta_max      74.2

_exptl_crystal_description       Prism
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    1.128
_shelx_estimated_absorpt_T_min   0.541
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.8140
_diffrn_reflns_number            50031
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.602
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_full        66.998
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             13284
_reflns_number_gt                11581
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+4.7946P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13284
_refine_ls_number_parameters     1017
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0638
_refine_ls_wR_factor_ref         0.1747
_refine_ls_wR_factor_gt          0.1699
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.016
_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
C15 C 0.53805(13) 1.03659(14) 0.72609(12) 0.0115(4) Uani 1 1 d . . . . .
C6 C 0.39495(13) 1.11336(14) 0.53877(12) 0.0116(4) Uani 1 1 d . . . . .
C8 C 0.42722(13) 0.97136(14) 0.63063(12) 0.0119(4) Uani 1 1 d . . . . .
C9 C 0.46174(14) 0.90430(14) 0.70127(13) 0.0130(4) Uani 1 1 d . . . . .
C10 C 0.44036(15) 0.80786(15) 0.72583(13) 0.0155(4) Uani 1 1 d . . . . .
H1 H 0.3957 0.7861 0.6980 0.019 Uiso 1 1 calc R U . . .
C11 C 0.48273(15) 0.74462(15) 0.78912(13) 0.0176(5) Uani 1 1 d . . . . .
H2 H 0.4667 0.6803 0.8050 0.021 Uiso 1 1 calc R U . . .
C12 C 0.54966(15) 0.77580(15) 0.82989(13) 0.0179(5) Uani 1 1 d . . . . .
H3 H 0.5819 0.7320 0.8713 0.021 Uiso 1 1 calc R U . . .
C13 C 0.56880(15) 0.86976(15) 0.81012(13) 0.0155(4) Uani 1 1 d . . . . .
H4 H 0.6135 0.8898 0.8390 0.019 Uiso 1 1 calc R U . . .
C14 C 0.52344(14) 0.93753(14) 0.74772(12) 0.0126(4) Uani 1 1 d . . . . .
C16 C 0.49232(13) 1.10166(14) 0.66388(12) 0.0102(4) Uani 1 1 d . . . . .
C18 C 0.59524(13) 1.17890(14) 0.71295(12) 0.0104(4) Uani 1 1 d . . . . .
C19 C 0.65120(14) 1.25333(14) 0.71981(12) 0.0125(4) Uani 1 1 d . . . . .
C20 C 0.73467(14) 1.23808(15) 0.75986(13) 0.0162(4) Uani 1 1 d . . . . .
H5 H 0.7557 1.1759 0.7832 0.019 Uiso 1 1 calc R U . . .
C21 C 0.78600(15) 1.31157(16) 0.76570(14) 0.0206(5) Uani 1 1 d . . . . .
H6 H 0.8414 1.2999 0.7936 0.025 Uiso 1 1 calc R U . . .
C22 C 0.75627(16) 1.40356(16) 0.73040(15) 0.0227(5) Uani 1 1 d . . . . .
H7 H 0.7908 1.4542 0.7356 0.027 Uiso 1 1 calc R U . . .
C23 C 0.67721(15) 1.42125(15) 0.68813(13) 0.0178(5) Uani 1 1 d . . . . .
H8 H 0.6591 1.4842 0.6632 0.021 Uiso 1 1 calc R U . . .
C24 C 0.62234(14) 1.34773(14) 0.68099(12) 0.0124(4) Uani 1 1 d . . . . .
C25 C 0.54115(13) 1.35998(14) 0.63454(12) 0.0109(4) Uani 1 1 d . . . . .
C26 C 0.50138(13) 1.28646(14) 0.61387(12) 0.0098(4) Uani 1 1 d . . . . .
C27 C 0.42452(13) 1.32383(14) 0.56543(12) 0.0100(4) Uani 1 1 d . . . . .
C28 C 0.41615(14) 1.41740(14) 0.56580(12) 0.0118(4) Uani 1 1 d . . . . .
C29 C 0.34206(14) 1.47292(14) 0.53292(13) 0.0139(4) Uani 1 1 d . . . . .
H9 H 0.3382 1.5362 0.5318 0.017 Uiso 1 1 calc R U . . .
C30 C 0.27439(14) 1.43237(15) 0.50199(13) 0.0140(4) Uani 1 1 d . . . . .
H10 H 0.2207 1.4664 0.4837 0.017 Uiso 1 1 calc R U . . .
C32 C 0.36220(13) 1.28830(14) 0.52196(12) 0.0105(4) Uani 1 1 d . . . . .
C33 C 0.30950(16) 1.33200(16) 0.29005(13) 0.0188(5) Uani 1 1 d . . . . .
H11 H 0.3100 1.3995 0.2621 0.028 Uiso 1 1 calc R U . . .
H12 H 0.3414 1.2994 0.2587 0.028 Uiso 1 1 calc R U . . .
H13 H 0.2472 1.3098 0.2983 0.028 Uiso 1 1 calc R U . . .
C34 C 0.14678(15) 1.35896(16) 0.42353(14) 0.0196(5) Uani 1 1 d . . . . .
H14 H 0.1036 1.3211 0.4056 0.029 Uiso 1 1 calc R U . . .
H15 H 0.1160 1.3894 0.4571 0.029 Uiso 1 1 calc R U . . .
H16 H 0.1727 1.4067 0.3778 0.029 Uiso 1 1 calc R U . . .
C40 C 0.53848(15) 1.03279(16) 0.89526(13) 0.0176(5) Uani 1 1 d . . . . .
H17 H 0.5567 1.0218 0.9506 0.021 Uiso 1 1 calc R U . . .
H18 H 0.5134 0.9735 0.8917 0.021 Uiso 1 1 calc R U . . .
C41 C 0.46491(17) 1.1074(2) 0.87385(15) 0.0298(6) Uani 1 1 d . . . . .
H19 H 0.4484 1.1199 0.8179 0.036 Uiso 1 1 calc R U . . .
H20 H 0.4110 1.0821 0.9060 0.036 Uiso 1 1 calc R U . . .
C42 C 0.4903(2) 1.1992(2) 0.88579(18) 0.0439(8) Uani 1 1 d . . . . .
H21 H 0.4396 1.2428 0.8707 0.066 Uiso 1 1 calc R U . . .
H22 H 0.5051 1.1881 0.9413 0.066 Uiso 1 1 calc R U . . .
H23 H 0.5426 1.2259 0.8530 0.066 Uiso 1 1 calc R U . . .
C43 C 0.49638(14) 1.53052(14) 0.61836(13) 0.0156(4) Uani 1 1 d . . . . .
H24 H 0.4570 1.5764 0.5806 0.019 Uiso 1 1 calc R U . . .
H25 H 0.5590 1.5534 0.6081 0.019 Uiso 1 1 calc R U . . .
C44 C 0.47066(18) 1.52612(19) 0.70144(16) 0.0292(6) Uani 1 1 d . . . . .
H26 H 0.4774 1.5891 0.7066 0.035 Uiso 1 1 calc R U . . .
H27 H 0.5126 1.4835 0.7391 0.035 Uiso 1 1 calc R U . . .
C45 C 0.3750(2) 1.4924(3) 0.7230(2) 0.0575(10) Uani 1 1 d . . . . .
H28 H 0.3340 1.5331 0.6831 0.069 Uiso 1 1 calc R U . . .
H29 H 0.3697 1.4283 0.7199 0.069 Uiso 1 1 calc R U . . .
C46 C 0.3438(3) 1.4911(4) 0.8024(3) 0.0701(13) Uani 1 1 d . . . . .
H30 H 0.2817 1.4684 0.8105 0.105 Uiso 1 1 calc R U . . .
H31 H 0.3825 1.4494 0.8429 0.105 Uiso 1 1 calc R U . . .
H32 H 0.3467 1.5544 0.8060 0.105 Uiso 1 1 calc R U . . .
C67 C 1.28599(15) 0.18842(16) 0.73424(14) 0.0211(5) Uani 1 1 d . . . . .
H33 H 1.3413 0.2002 0.7062 0.025 Uiso 1 1 calc R U . . .
C68 C 1.25632(16) 0.09641(16) 0.76966(15) 0.0229(5) Uani 1 1 d . . . . .
H34 H 1.2909 0.0457 0.7646 0.027 Uiso 1 1 calc R U . . .
C69 C 1.17724(15) 0.07895(15) 0.81181(14) 0.0179(5) Uani 1 1 d . . . . .
H35 H 1.1591 0.0160 0.8367 0.021 Uiso 1 1 calc R U . . .
C79 C 0.80946(16) 0.16790(16) 1.21008(13) 0.0188(5) Uani 1 1 d . . . . .
H36 H 0.8099 0.1004 1.2380 0.028 Uiso 1 1 calc R U . . .
H37 H 0.8414 0.2004 1.2415 0.028 Uiso 1 1 calc R U . . .
H38 H 0.7472 0.1902 1.2019 0.028 Uiso 1 1 calc R U . . .
C80 C 0.64691(15) 0.14108(16) 1.07642(14) 0.0194(5) Uani 1 1 d . . . . .
H39 H 0.6037 0.1790 1.0944 0.029 Uiso 1 1 calc R U . . .
H40 H 0.6161 0.1106 1.0428 0.029 Uiso 1 1 calc R U . . .
H41 H 0.6729 0.0933 1.1221 0.029 Uiso 1 1 calc R U . . .
C82 C 0.80153(15) 0.67645(16) 0.95484(16) 0.0219(5) Uani 1 1 d . . . . .
H42 H 0.7588 0.6277 0.9847 0.026 Uiso 1 1 calc R U . . .
H43 H 0.7796 0.7018 0.8999 0.026 Uiso 1 1 calc R U . . .
C83 C 0.80463(19) 0.7545(2) 0.9913(2) 0.0398(7) Uani 1 1 d . . . . .
H44 H 0.8368 0.7311 1.0423 0.048 Uiso 1 1 calc R U . . .
H45 H 0.8403 0.8068 0.9565 0.048 Uiso 1 1 calc R U . . .
C84 C 0.71545(19) 0.7919(2) 1.00545(18) 0.0340(6) Uani 1 1 d . . . . .
H46 H 0.7245 0.8416 1.0290 0.051 Uiso 1 1 calc R U . . .
H47 H 0.6835 0.8173 0.9553 0.051 Uiso 1 1 calc R U . . .
H48 H 0.6799 0.7414 1.0413 0.051 Uiso 1 1 calc R U . . .
C86 C 1.03833(15) 0.46727(16) 0.60450(13) 0.0176(5) Uani 1 1 d . . . . .
H49 H 1.0131 0.5266 0.6079 0.021 Uiso 1 1 calc R U . . .
H50 H 1.0566 0.4780 0.5492 0.021 Uiso 1 1 calc R U . . .
C87 C 0.96508(17) 0.3926(2) 0.62621(15) 0.0299(6) Uani 1 1 d . . . . .
H51 H 0.9487 0.3802 0.6822 0.036 Uiso 1 1 calc R U . . .
H52 H 0.9110 0.4177 0.5942 0.036 Uiso 1 1 calc R U . . .
C88 C 0.9904(2) 0.3007(2) 0.61441(18) 0.0439(8) Uani 1 1 d . . . . .
H53 H 0.9398 0.2571 0.6297 0.066 Uiso 1 1 calc R U . . .
H54 H 1.0050 0.3117 0.5589 0.066 Uiso 1 1 calc R U . . .
H55 H 1.0428 0.2741 0.6470 0.066 Uiso 1 1 calc R U . . .
C90 C 0.97086(18) -0.02586(19) 0.79835(16) 0.0294(6) Uani 1 1 d . . . . .
H56 H 0.9777 -0.0888 0.7930 0.035 Uiso 1 1 calc R U . . .
H57 H 1.0129 0.0168 0.7608 0.035 Uiso 1 1 calc R U . . .
C91 C 0.8751(2) 0.0080(3) 0.7766(2) 0.0558(10) Uani 1 1 d . . . . .
H58 H 0.8340 -0.0324 0.8167 0.067 Uiso 1 1 calc R U . . .
H59 H 0.8698 0.0722 0.7794 0.067 Uiso 1 1 calc R U . . .
C92 C 0.8435(3) 0.0090(4) 0.6973(2) 0.0694(13) Uani 1 1 d . . . . .
H60 H 0.7814 0.0318 0.6893 0.104 Uiso 1 1 calc R U . . .
H61 H 0.8821 0.0504 0.6566 0.104 Uiso 1 1 calc R U . . .
H62 H 0.8462 -0.0545 0.6940 0.104 Uiso 1 1 calc R U . . .
N3 N 0.48935(11) 1.44018(12) 0.60394(10) 0.0119(4) Uani 1 1 d . . . . .
N6 N 0.98935(11) 0.05984(12) 0.89613(10) 0.0117(4) Uani 1 1 d . . . . .
O1 O 0.35286(10) 1.31364(10) 0.36425(9) 0.0165(3) Uani 1 1 d . . . . .
O2 O 0.21630(10) 1.30058(10) 0.46704(9) 0.0167(3) Uani 1 1 d . . . . .
O3 O 0.85288(10) 0.18637(10) 1.13569(9) 0.0163(3) Uani 1 1 d . . . . .
O4 O 0.71635(10) 0.19943(10) 1.03290(9) 0.0165(3) Uani 1 1 d . . . . .
C1 C 0.37518(13) 1.20697(14) 0.49270(12) 0.0112(4) Uani 1 1 d . . . . .
C3 C 0.34897(14) 1.14822(16) 0.38113(13) 0.0164(4) Uani 1 1 d . . . . .
H63 H 0.3386 1.1617 0.3263 0.020 Uiso 1 1 calc R U . . .
C4 C 0.35438(14) 1.05589(15) 0.42918(13) 0.0167(5) Uani 1 1 d . . . . .
H64 H 0.3430 1.0057 0.4092 0.020 Uiso 1 1 calc R U . . .
C2 C 0.35847(13) 1.22172(15) 0.41197(13) 0.0135(4) Uani 1 1 d . . . . .
C5 C 0.37714(13) 1.03949(14) 0.50775(13) 0.0133(4) Uani 1 1 d . . . . .
C7 C 0.43331(13) 1.06861(14) 0.61517(12) 0.0109(4) Uani 1 1 d . . . . .
C39 C 0.62161(14) 1.05826(14) 0.84296(12) 0.0134(4) Uani 1 1 d . . . . .
H65 H 0.6525 1.1113 0.8531 0.016 Uiso 1 1 calc R U . . .
H66 H 0.6634 1.0044 0.8576 0.016 Uiso 1 1 calc R U . . .
C47 C 0.87534(13) 0.29319(14) 1.00725(12) 0.0112(4) Uani 1 1 d . . . . .
C56 C 0.94037(15) 0.69222(15) 0.77406(13) 0.0159(4) Uani 1 1 d . . . . .
H67 H 0.8957 0.7140 0.8018 0.019 Uiso 1 1 calc R U . . .
C57 C 0.98271(15) 0.75519(15) 0.71087(13) 0.0174(5) Uani 1 1 d . . . . .
H68 H 0.9667 0.8195 0.6950 0.021 Uiso 1 1 calc R U . . .
C58 C 1.04951(15) 0.72430(15) 0.67002(13) 0.0180(5) Uani 1 1 d . . . . .
H69 H 1.0816 0.7681 0.6286 0.022 Uiso 1 1 calc R U . . .
C59 C 1.06871(15) 0.63018(15) 0.69004(13) 0.0153(4) Uani 1 1 d . . . . .
H70 H 1.1136 0.6101 0.6613 0.018 Uiso 1 1 calc R U . . .
C61 C 1.03794(13) 0.46336(14) 0.77393(12) 0.0107(4) Uani 1 1 d . . . . .
C78 C 0.86231(13) 0.21172(14) 0.97801(12) 0.0107(4) Uani 1 1 d . . . . .
C81 C 0.89372(14) 0.63281(14) 0.95526(13) 0.0148(4) Uani 1 1 d . . . . .
H71 H 0.9329 0.6786 0.9173 0.018 Uiso 1 1 calc R U . . .
H72 H 0.9206 0.6196 1.0082 0.018 Uiso 1 1 calc R U . . .
C85 C 1.12161(14) 0.44184(14) 0.65705(12) 0.0127(4) Uani 1 1 d . . . . .
H73 H 1.1527 0.3888 0.6469 0.015 Uiso 1 1 calc R U . . .
H74 H 1.1633 0.4958 0.6425 0.015 Uiso 1 1 calc R U . . .
C89 C 0.99639(14) -0.03054(14) 0.88166(13) 0.0155(4) Uani 1 1 d . . . . .
H75 H 0.9569 -0.0764 0.9193 0.019 Uiso 1 1 calc R U . . .
H76 H 1.0590 -0.0536 0.8920 0.019 Uiso 1 1 calc R U . . .
N1 N 0.39186(12) 0.95400(12) 0.56492(11) 0.0139(4) Uani 1 1 d . . . . .
N2 N 0.60139(11) 1.08413(12) 0.75771(10) 0.0108(4) Uani 1 1 d . . . . .
N4 N 0.89197(12) 0.54596(12) 0.93507(11) 0.0137(4) Uani 1 1 d . . . . .
N5 N 1.10134(11) 0.41588(12) 0.74228(10) 0.0105(3) Uani 1 1 d . . . . .
C48 C 0.85857(13) 0.27817(14) 1.08804(13) 0.0131(4) Uani 1 1 d . . . . .
C49 C 0.84893(14) 0.35197(16) 1.11879(13) 0.0168(4) Uani 1 1 d . . . . .
H77 H 0.8385 0.3385 1.1736 0.020 Uiso 1 1 calc R U . . .
C50 C 0.85425(14) 0.44405(15) 1.07096(13) 0.0164(4) Uani 1 1 d . . . . .
H78 H 0.8428 0.4942 1.0909 0.020 Uiso 1 1 calc R U . . .
C52 C 0.89514(13) 0.38675(14) 0.96124(12) 0.0110(4) Uani 1 1 d . . . . .
C53 C 0.93336(13) 0.43131(14) 0.88472(12) 0.0109(4) Uani 1 1 d . . . . .
C17 C 0.52775(13) 1.19230(14) 0.65673(12) 0.0103(4) Uani 1 1 d . . . . .
C31 C 0.28366(13) 1.34217(15) 0.49725(12) 0.0125(4) Uani 1 1 d . . . . .
C51 C 0.87699(13) 0.46041(14) 0.99244(13) 0.0128(4) Uani 1 1 d . . . . .
C54 C 0.92731(13) 0.52863(14) 0.86937(12) 0.0122(4) Uani 1 1 d . . . . .
C55 C 0.96181(14) 0.59553(14) 0.79884(13) 0.0129(4) Uani 1 1 d . . . . .
C60 C 1.02342(14) 0.56243(14) 0.75236(12) 0.0124(4) Uani 1 1 d . . . . .
C62 C 0.99213(13) 0.39844(14) 0.83617(12) 0.0104(4) Uani 1 1 d . . . . .
C63 C 1.02780(13) 0.30766(14) 0.84323(12) 0.0105(4) Uani 1 1 d . . . . .
C64 C 1.09522(13) 0.32105(14) 0.78720(12) 0.0105(4) Uani 1 1 d . . . . .
C65 C 1.15122(13) 0.24666(14) 0.78021(12) 0.0125(4) Uani 1 1 d . . . . .
C66 C 1.23454(14) 0.26184(15) 0.74020(13) 0.0157(4) Uani 1 1 d . . . . .
H79 H 1.2556 0.3241 0.7169 0.019 Uiso 1 1 calc R U . . .
C70 C 1.12241(14) 0.15236(14) 0.81894(12) 0.0124(4) Uani 1 1 d . . . . .
C71 C 1.04117(13) 0.13998(14) 0.86536(12) 0.0108(4) Uani 1 1 d . . . . .
C72 C 1.00144(13) 0.21364(14) 0.88611(12) 0.0101(4) Uani 1 1 d . . . . .
C73 C 0.92454(13) 0.17627(14) 0.93458(12) 0.0104(4) Uani 1 1 d . . . . .
C74 C 0.91619(13) 0.08252(14) 0.93423(12) 0.0115(4) Uani 1 1 d . . . . .
C75 C 0.84214(14) 0.02727(15) 0.96714(13) 0.0140(4) Uani 1 1 d . . . . .
H80 H 0.8384 -0.0360 0.9683 0.017 Uiso 1 1 calc R U . . .
C76 C 0.77459(14) 0.06746(15) 0.99795(13) 0.0139(4) Uani 1 1 d . . . . .
H81 H 0.7210 0.0332 1.0163 0.017 Uiso 1 1 calc R U . . .
C77 C 0.78356(13) 0.15793(14) 1.00278(12) 0.0122(4) Uani 1 1 d . . . . .
C97 C 0.39356(14) 0.86731(14) 0.54452(13) 0.0154(4) Uani 1 1 d . . . . .
H82 H 0.4331 0.8216 0.5822 0.018 Uiso 1 1 calc R U . . .
H83 H 0.4201 0.8807 0.4914 0.018 Uiso 1 1 calc R U . . .
C98 C 0.30154(15) 0.82347(16) 0.54531(16) 0.0226(5) Uani 1 1 d . . . . .
H84 H 0.2586 0.8721 0.5155 0.027 Uiso 1 1 calc R U . . .
H85 H 0.2798 0.7983 0.6003 0.027 Uiso 1 1 calc R U . . .
C100 C 0.21548(18) 0.7081(2) 0.49453(18) 0.0339(6) Uani 1 1 d . . . . .
H86 H 0.2246 0.6582 0.4713 0.051 Uiso 1 1 calc R U . . .
H87 H 0.1830 0.6831 0.5445 0.051 Uiso 1 1 calc R U . . .
H88 H 0.1803 0.7587 0.4583 0.051 Uiso 1 1 calc R U . . .
C99 C 0.30456(19) 0.7452(2) 0.5091(2) 0.0403(8) Uani 1 1 d . . . . .
H89 H 0.3372 0.7682 0.4584 0.048 Uiso 1 1 calc R U . . .
H90 H 0.3399 0.6928 0.5444 0.048 Uiso 1 1 calc R U . . .
S5 S 0.84661(8) 0.97329(9) 0.41684(7) 0.0117(3) Uiso 0.4 1 d . . P A 1
O7 O 0.9366(4) 1.0476(4) 0.3925(4) 0.0309(14) Uiso 0.4 1 d . . P A 1
C102 C 0.8580(5) 0.9298(4) 0.5222(4) 0.0131(14) Uiso 0.4 1 d . . P A 1
H91 H 0.8095 0.8853 0.5446 0.020 Uiso 0.4 1 calc R U P A 1
H92 H 0.9161 0.8984 0.5360 0.020 Uiso 0.4 1 calc R U P A 1
H93 H 0.8544 0.9821 0.5433 0.020 Uiso 0.4 1 calc R U P A 1
C101 C 0.8952(4) 0.8732(4) 0.4004(3) 0.0178(11) Uiso 0.4 1 d . . P A 1
H94 H 0.8508 0.8226 0.4121 0.027 Uiso 0.4 1 calc R U P A 1
H95 H 0.9141 0.8892 0.3453 0.027 Uiso 0.4 1 calc R U P A 1
H96 H 0.9476 0.8525 0.4348 0.027 Uiso 0.4 1 calc R U P A 1
S6 S 0.93178(14) 0.94606(15) 0.43406(12) 0.0259(4) Uiso 0.3 1 d . . P B 2
C103 C 0.8373(8) 0.9064(9) 0.3925(7) 0.042(3) Uiso 0.3 1 d . . P B 2
H97 H 0.8345 0.8380 0.4127 0.063 Uiso 0.3 1 calc R U P B 2
H98 H 0.7821 0.9326 0.4068 0.063 Uiso 0.3 1 calc R U P B 2
H99 H 0.8432 0.9269 0.3350 0.063 Uiso 0.3 1 calc R U P B 2
O9 O 0.9059(5) 1.0533(4) 0.3850(4) 0.0160(14) Uiso 0.3 1 d . . P B 2
C104 C 0.8859(9) 0.9254(8) 0.5293(7) 0.030(3) Uiso 0.3 1 d . . P B 2
H100 H 0.8994 0.8611 0.5620 0.045 Uiso 0.3 1 calc R U P B 2
H101 H 0.9123 0.9692 0.5533 0.045 Uiso 0.3 1 calc R U P B 2
H102 H 0.8206 0.9343 0.5252 0.045 Uiso 0.3 1 calc R U P B 2
O6 O 0.4138(3) 0.4476(3) 0.1134(3) 0.0314(12) Uiso 0.5 1 d . . P C 3
S3 S 0.34651(8) 0.52678(9) 0.08300(7) 0.0249(3) Uiso 0.5 1 d . . P C 3
C95 C 0.3950(4) 0.6272(4) 0.0998(3) 0.0316(12) Uiso 0.5 1 d . . P C 3
H103 H 0.3538 0.6804 0.0810 0.047 Uiso 0.5 1 calc R U P C 3
H104 H 0.4058 0.6138 0.1563 0.047 Uiso 0.5 1 calc R U P C 3
H105 H 0.4521 0.6425 0.0713 0.047 Uiso 0.5 1 calc R U P C 3
C96 C 0.3650(3) 0.5699(3) -0.0234(3) 0.0142(8) Uiso 0.5 1 d . . P C 3
H106 H 0.3236 0.6217 -0.0475 0.021 Uiso 0.5 1 calc R U P C 3
H107 H 0.4271 0.5919 -0.0342 0.021 Uiso 0.5 1 calc R U P C 3
H108 H 0.3542 0.5192 -0.0454 0.021 Uiso 0.5 1 calc R U P C 3
S8 S 0.43154(14) 0.55393(15) 0.06592(12) 0.0209(7) Uiso 0.273(2) 1 d . . P D 4
O12 O 0.3349(7) 0.5898(8) 0.1073(6) 0.052(3) Uiso 0.273(2) 1 d . . P D 4
C201 C 0.4212(7) 0.4347(6) 0.0775(6) 0.0199(19) Uiso 0.273(2) 1 d . . P D 4
H109 H 0.3982 0.4015 0.1303 0.030 Uiso 0.273(2) 1 calc R U P D 4
H110 H 0.3795 0.4265 0.0379 0.030 Uiso 0.273(2) 1 calc R U P D 4
H111 H 0.4802 0.4094 0.0708 0.030 Uiso 0.273(2) 1 calc R U P D 4
C202 C 0.4582(11) 0.6109(11) 0.0070(9) 0.066(4) Uiso 0.273(2) 1 d . . P D 4
H112 H 0.4583 0.6727 0.0139 0.099 Uiso 0.273(2) 1 calc R U P D 4
H113 H 0.5194 0.5947 -0.0041 0.099 Uiso 0.273(2) 1 calc R U P D 4
H114 H 0.4187 0.6118 -0.0370 0.099 Uiso 0.273(2) 1 calc R U P D 4
C200 C 0.8228(7) 0.9373(9) 0.3951(6) 0.037(3) Uiso 0.3 1 d D . P E 5
H115 H 0.7888 0.8800 0.4209 0.055 Uiso 0.3 1 calc R U P E 5
H116 H 0.7818 0.9856 0.3633 0.055 Uiso 0.3 1 calc R U P E 5
H117 H 0.8690 0.9243 0.3610 0.055 Uiso 0.3 1 calc R U P E 5
S7 S 0.8743(2) 0.9768(2) 0.46718(19) 0.0513(7) Uiso 0.3 1 d D . P E 5
C107 C 0.9577(10) 0.8871(10) 0.4947(9) 0.068(4) Uiso 0.3 1 d . . P E 5
H118 H 0.9300 0.8283 0.5267 0.102 Uiso 0.3 1 calc R U P E 5
H119 H 0.9841 0.8789 0.4472 0.102 Uiso 0.3 1 calc R U P E 5
H120 H 1.0049 0.9049 0.5253 0.102 Uiso 0.3 1 calc R U P E 5
O11 O 0.9223(6) 1.0627(6) 0.4192(5) 0.0421(18) Uiso 0.3 1 d . . P E 5
S9 S 0.3745(2) 0.5225(2) 0.03292(18) 0.0315(9) Uiso 0.227(2) 1 d D U P D 6
O13 O 0.4411(6) 0.4543(5) 0.0988(5) 0.0152(19) Uiso 0.227(2) 1 d D U P D 6
C203 C 0.402(3) 0.599(2) -0.0628(11) 0.154(12) Uiso 0.227(2) 1 d D U P D 6
H121 H 0.3471 0.6305 -0.0885 0.230 Uiso 0.227(2) 1 calc R U P D 6
H122 H 0.4456 0.6452 -0.0585 0.230 Uiso 0.227(2) 1 calc R U P D 6
H123 H 0.4273 0.5623 -0.0942 0.230 Uiso 0.227(2) 1 calc R U P D 6
C204 C 0.3158(9) 0.5610(11) 0.1064(7) 0.032(3) Uiso 0.227(2) 1 d D . P D 6
H124 H 0.2687 0.6058 0.0807 0.048 Uiso 0.227(2) 1 calc R U P D 6
H125 H 0.2885 0.5069 0.1458 0.048 Uiso 0.227(2) 1 calc R U P D 6
H126 H 0.3585 0.5911 0.1323 0.048 Uiso 0.227(2) 1 calc R U P D 6


_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
C15 C16 1.403(3) . ?
C15 N2 1.409(3) . ?
C15 C14 1.435(3) . ?
C6 C1 1.420(3) . ?
C6 C5 1.421(3) . ?
C6 C7 1.437(3) . ?
C8 N1 1.389(3) . ?
C8 C7 1.406(3) . ?
C8 C9 1.439(3) . ?
C9 C10 1.415(3) . ?
C9 C14 1.434(3) . ?
C10 C11 1.379(3) . ?
C10 H1 0.9500 . ?
C11 C12 1.403(3) . ?
C11 H2 0.9500 . ?
C12 C13 1.377(3) . ?
C12 H3 0.9500 . ?
C13 C14 1.421(3) . ?
C13 H4 0.9500 . ?
C16 C17 1.433(3) . ?
C16 C7 1.436(3) . ?
C18 C17 1.391(3) . ?
C18 N2 1.401(3) . ?
C18 C19 1.435(3) . ?
C19 C20 1.416(3) . ?
C19 C24 1.436(3) . ?
C20 C21 1.378(3) . ?
C20 H5 0.9500 . ?
C21 C22 1.400(3) . ?
C21 H6 0.9500 . ?
C22 C23 1.378(3) . ?
C22 H7 0.9500 . ?
C23 C24 1.416(3) . ?
C23 H8 0.9500 . ?
C24 C25 1.445(3) . ?
C25 N3 1.390(3) . ?
C25 C26 1.408(3) . ?
C26 C17 1.436(3) . ?
C26 C27 1.437(3) . ?
C27 C28 1.419(3) . ?
C27 C32 1.422(3) . ?
C28 N3 1.386(3) . ?
C28 C29 1.395(3) . ?
C29 C30 1.383(3) . ?
C29 H9 0.9500 . ?
C30 C31 1.397(3) . ?
C30 H10 0.9500 . ?
C32 C31 1.411(3) . ?
C32 C1 1.493(3) . ?
C33 O1 1.423(3) . ?
C33 H11 0.9800 . ?
C33 H12 0.9800 . ?
C33 H13 0.9800 . ?
C34 O2 1.419(2) . ?
C34 H14 0.9800 . ?
C34 H15 0.9800 . ?
C34 H16 0.9800 . ?
C40 C39 1.525(3) . ?
C40 C41 1.528(3) . ?
C40 H17 0.9900 . ?
C40 H18 0.9900 . ?
C41 C42 1.516(4) . ?
C41 H19 0.9900 . ?
C41 H20 0.9900 . ?
C42 H21 0.9800 . ?
C42 H22 0.9800 . ?
C42 H23 0.9800 . ?
C43 N3 1.470(3) . ?
C43 C44 1.518(3) . ?
C43 H24 0.9900 . ?
C43 H25 0.9900 . ?
C44 C45 1.519(4) . ?
C44 H26 0.9900 . ?
C44 H27 0.9900 . ?
C45 C46 1.490(5) . ?
C45 H28 0.9900 . ?
C45 H29 0.9900 . ?
C46 H30 0.9800 . ?
C46 H31 0.9800 . ?
C46 H32 0.9800 . ?
C67 C66 1.378(3) . ?
C67 C68 1.400(3) . ?
C67 H33 0.9500 . ?
C68 C69 1.377(3) . ?
C68 H34 0.9500 . ?
C69 C70 1.414(3) . ?
C69 H35 0.9500 . ?
C79 O3 1.426(3) . ?
C79 H36 0.9800 . ?
C79 H37 0.9800 . ?
C79 H38 0.9800 . ?
C80 O4 1.418(3) . ?
C80 H39 0.9800 . ?
C80 H40 0.9800 . ?
C80 H41 0.9800 . ?
C82 C81 1.520(3) . ?
C82 C83 1.520(3) . ?
C82 H42 0.9900 . ?
C82 H43 0.9900 . ?
C83 C84 1.495(4) . ?
C83 H44 0.9900 . ?
C83 H45 0.9900 . ?
C84 H46 0.9800 . ?
C84 H47 0.9800 . ?
C84 H48 0.9800 . ?
C86 C87 1.526(3) . ?
C86 C85 1.529(3) . ?
C86 H49 0.9900 . ?
C86 H50 0.9900 . ?
C87 C88 1.514(4) . ?
C87 H51 0.9900 . ?
C87 H52 0.9900 . ?
C88 H53 0.9800 . ?
C88 H54 0.9800 . ?
C88 H55 0.9800 . ?
C90 C89 1.520(3) . ?
C90 C91 1.522(4) . ?
C90 H56 0.9900 . ?
C90 H57 0.9900 . ?
C91 C92 1.492(5) . ?
C91 H58 0.9900 . ?
C91 H59 0.9900 . ?
C92 H60 0.9800 . ?
C92 H61 0.9800 . ?
C92 H62 0.9800 . ?
N6 C74 1.385(3) . ?
N6 C71 1.391(3) . ?
N6 C89 1.471(3) . ?
O1 C2 1.379(3) . ?
O2 C31 1.382(2) . ?
O3 C48 1.378(3) . ?
O4 C77 1.378(2) . ?
C1 C2 1.414(3) . ?
C3 C4 1.386(3) . ?
C3 C2 1.396(3) . ?
C3 H63 0.9500 . ?
C4 C5 1.391(3) . ?
C4 H64 0.9500 . ?
C5 N1 1.384(3) . ?
C39 N2 1.482(3) . ?
C39 H65 0.9900 . ?
C39 H66 0.9900 . ?
C47 C48 1.414(3) . ?
C47 C52 1.419(3) . ?
C47 C78 1.495(3) . ?
C56 C57 1.376(3) . ?
C56 C55 1.418(3) . ?
C56 H67 0.9500 . ?
C57 C58 1.400(3) . ?
C57 H68 0.9500 . ?
C58 C59 1.378(3) . ?
C58 H69 0.9500 . ?
C59 C60 1.420(3) . ?
C59 H70 0.9500 . ?
C61 C62 1.403(3) . ?
C61 N5 1.409(3) . ?
C61 C60 1.435(3) . ?
C78 C77 1.413(3) . ?
C78 C73 1.420(3) . ?
C81 N4 1.467(3) . ?
C81 H71 0.9900 . ?
C81 H72 0.9900 . ?
C85 N5 1.481(3) . ?
C85 H73 0.9900 . ?
C85 H74 0.9900 . ?
C89 H75 0.9900 . ?
C89 H76 0.9900 . ?
N1 C97 1.467(3) . ?
N4 C51 1.387(3) . ?
N4 C54 1.389(3) . ?
N5 C64 1.402(3) . ?
C48 C49 1.399(3) . ?
C49 C50 1.382(3) . ?
C49 H77 0.9500 . ?
C50 C51 1.390(3) . ?
C50 H78 0.9500 . ?
C52 C51 1.421(3) . ?
C52 C53 1.437(3) . ?
C53 C54 1.408(3) . ?
C53 C62 1.430(3) . ?
C54 C55 1.436(3) . ?
C55 C60 1.432(3) . ?
C62 C63 1.436(3) . ?
C63 C64 1.387(3) . ?
C63 C72 1.435(3) . ?
C64 C65 1.435(3) . ?
C65 C66 1.414(3) . ?
C65 C70 1.435(3) . ?
C66 H79 0.9500 . ?
C70 C71 1.445(3) . ?
C71 C72 1.410(3) . ?
C72 C73 1.438(3) . ?
C73 C74 1.422(3) . ?
C74 C75 1.394(3) . ?
C75 C76 1.377(3) . ?
C75 H80 0.9500 . ?
C76 C77 1.402(3) . ?
C76 H81 0.9500 . ?
C97 C98 1.519(3) . ?
C97 H82 0.9900 . ?
C97 H83 0.9900 . ?
C98 C99 1.520(3) . ?
C98 H84 0.9900 . ?
C98 H85 0.9900 . ?
C100 C99 1.494(4) . ?
C100 H86 0.9800 . ?
C100 H87 0.9800 . ?
C100 H88 0.9800 . ?
C99 H89 0.9900 . ?
C99 H90 0.9900 . ?
S5 O7 1.712(6) . ?
S5 C101 1.783(6) . ?
S5 C102 1.797(6) . ?
C102 H91 0.9800 . ?
C102 H92 0.9800 . ?
C102 H93 0.9800 . ?
C101 H94 0.9800 . ?
C101 H95 0.9800 . ?
C101 H96 0.9800 . ?
S6 O9 1.621(6) . ?
S6 C104 1.771(11) . ?
S6 C103 1.782(11) . ?
C103 H97 0.9800 . ?
C103 H98 0.9800 . ?
C103 H99 0.9800 . ?
C104 H100 0.9800 . ?
C104 H101 0.9800 . ?
C104 H102 0.9800 . ?
O6 S3 1.519(5) . ?
S3 C95 1.789(6) . ?
S3 C96 1.827(5) . ?
C95 H103 0.9800 . ?
C95 H104 0.9800 . ?
C95 H105 0.9800 . ?
C96 H106 0.9800 . ?
C96 H107 0.9800 . ?
C96 H108 0.9800 . ?
S8 C202 1.195(16) . ?
S8 C201 1.750(10) . ?
S8 O12 1.780(10) . ?
C201 H109 0.9800 . ?
C201 H110 0.9800 . ?
C201 H111 0.9800 . ?
C202 H112 0.9800 . ?
C202 H113 0.9800 . ?
C202 H114 0.9800 . ?
C200 S7 1.763(8) . ?
C200 H115 0.9800 . ?
C200 H116 0.9800 . ?
C200 H117 0.9800 . ?
S7 O11 1.488(8) . ?
S7 C107 1.786(15) . ?
C107 H118 0.9800 . ?
C107 H119 0.9800 . ?
C107 H120 0.9800 . ?
S9 O13 1.629(6) . ?
S9 C203 1.779(10) . ?
S9 C204 1.825(9) . ?
C203 H121 0.9800 . ?
C203 H122 0.9800 . ?
C203 H123 0.9800 . ?
C204 H124 0.9800 . ?
C204 H125 0.9800 . ?
C204 H126 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
C16 C15 N2 109.10(18) . . ?
C16 C15 C14 122.97(18) . . ?
N2 C15 C14 127.81(18) . . ?
C1 C6 C5 119.52(18) . . ?
C1 C6 C7 135.46(19) . . ?
C5 C6 C7 105.01(18) . . ?
N1 C8 C7 109.00(18) . . ?
N1 C8 C9 127.65(18) . . ?
C7 C8 C9 123.07(19) . . ?
C10 C9 C14 118.66(19) . . ?
C10 C9 C8 123.83(19) . . ?
C14 C9 C8 117.48(19) . . ?
C11 C10 C9 121.7(2) . . ?
C11 C10 H1 119.2 . . ?
C9 C10 H1 119.2 . . ?
C10 C11 C12 119.6(2) . . ?
C10 C11 H2 120.2 . . ?
C12 C11 H2 120.2 . . ?
C13 C12 C11 120.2(2) . . ?
C13 C12 H3 119.9 . . ?
C11 C12 H3 119.9 . . ?
C12 C13 C14 121.8(2) . . ?
C12 C13 H4 119.1 . . ?
C14 C13 H4 119.1 . . ?
C13 C14 C9 117.63(19) . . ?
C13 C14 C15 124.42(19) . . ?
C9 C14 C15 117.90(18) . . ?
C15 C16 C17 107.32(17) . . ?
C15 C16 C7 119.26(18) . . ?
C17 C16 C7 132.71(19) . . ?
C17 C18 N2 110.29(17) . . ?
C17 C18 C19 123.04(19) . . ?
N2 C18 C19 126.62(18) . . ?
C20 C19 C18 123.24(19) . . ?
C20 C19 C24 118.86(19) . . ?
C18 C19 C24 117.85(18) . . ?
C21 C20 C19 121.4(2) . . ?
C21 C20 H5 119.3 . . ?
C19 C20 H5 119.3 . . ?
C20 C21 C22 119.7(2) . . ?
C20 C21 H6 120.1 . . ?
C22 C21 H6 120.1 . . ?
C23 C22 C21 120.5(2) . . ?
C23 C22 H7 119.8 . . ?
C21 C22 H7 119.8 . . ?
C22 C23 C24 121.5(2) . . ?
C22 C23 H8 119.2 . . ?
C24 C23 H8 119.2 . . ?
C23 C24 C19 117.91(18) . . ?
C23 C24 C25 125.10(19) . . ?
C19 C24 C25 116.93(18) . . ?
N3 C25 C26 108.83(17) . . ?
N3 C25 C24 128.68(18) . . ?
C26 C25 C24 122.49(18) . . ?
C25 C26 C17 118.19(18) . . ?
C25 C26 C27 107.69(17) . . ?
C17 C26 C27 132.04(18) . . ?
C28 C27 C32 119.71(18) . . ?
C28 C27 C26 105.37(17) . . ?
C32 C27 C26 134.92(18) . . ?
N3 C28 C29 128.21(19) . . ?
N3 C28 C27 109.74(17) . . ?
C29 C28 C27 122.03(18) . . ?
C30 C29 C28 117.49(19) . . ?
C30 C29 H9 121.3 . . ?
C28 C29 H9 121.3 . . ?
C29 C30 C31 121.15(18) . . ?
C29 C30 H10 119.4 . . ?
C31 C30 H10 119.4 . . ?
C31 C32 C27 115.57(18) . . ?
C31 C32 C1 116.87(17) . . ?
C27 C32 C1 127.20(17) . . ?
O1 C33 H11 109.5 . . ?
O1 C33 H12 109.5 . . ?
H11 C33 H12 109.5 . . ?
O1 C33 H13 109.5 . . ?
H11 C33 H13 109.5 . . ?
H12 C33 H13 109.5 . . ?
O2 C34 H14 109.5 . . ?
O2 C34 H15 109.5 . . ?
H14 C34 H15 109.5 . . ?
O2 C34 H16 109.5 . . ?
H14 C34 H16 109.5 . . ?
H15 C34 H16 109.5 . . ?
C39 C40 C41 114.0(2) . . ?
C39 C40 H17 108.8 . . ?
C41 C40 H17 108.8 . . ?
C39 C40 H18 108.8 . . ?
C41 C40 H18 108.8 . . ?
H17 C40 H18 107.7 . . ?
C42 C41 C40 114.7(2) . . ?
C42 C41 H19 108.6 . . ?
C40 C41 H19 108.6 . . ?
C42 C41 H20 108.6 . . ?
C40 C41 H20 108.6 . . ?
H19 C41 H20 107.6 . . ?
C41 C42 H21 109.5 . . ?
C41 C42 H22 109.5 . . ?
H21 C42 H22 109.5 . . ?
C41 C42 H23 109.5 . . ?
H21 C42 H23 109.5 . . ?
H22 C42 H23 109.5 . . ?
N3 C43 C44 113.75(19) . . ?
N3 C43 H24 108.8 . . ?
C44 C43 H24 108.8 . . ?
N3 C43 H25 108.8 . . ?
C44 C43 H25 108.8 . . ?
H24 C43 H25 107.7 . . ?
C43 C44 C45 113.1(2) . . ?
C43 C44 H26 109.0 . . ?
C45 C44 H26 109.0 . . ?
C43 C44 H27 109.0 . . ?
C45 C44 H27 109.0 . . ?
H26 C44 H27 107.8 . . ?
C46 C45 C44 115.9(3) . . ?
C46 C45 H28 108.3 . . ?
C44 C45 H28 108.3 . . ?
C46 C45 H29 108.3 . . ?
C44 C45 H29 108.3 . . ?
H28 C45 H29 107.4 . . ?
C45 C46 H30 109.5 . . ?
C45 C46 H31 109.5 . . ?
H30 C46 H31 109.5 . . ?
C45 C46 H32 109.5 . . ?
H30 C46 H32 109.5 . . ?
H31 C46 H32 109.5 . . ?
C66 C67 C68 119.6(2) . . ?
C66 C67 H33 120.2 . . ?
C68 C67 H33 120.2 . . ?
C69 C68 C67 120.4(2) . . ?
C69 C68 H34 119.8 . . ?
C67 C68 H34 119.8 . . ?
C68 C69 C70 121.6(2) . . ?
C68 C69 H35 119.2 . . ?
C70 C69 H35 119.2 . . ?
O3 C79 H36 109.5 . . ?
O3 C79 H37 109.5 . . ?
H36 C79 H37 109.5 . . ?
O3 C79 H38 109.5 . . ?
H36 C79 H38 109.5 . . ?
H37 C79 H38 109.5 . . ?
O4 C80 H39 109.5 . . ?
O4 C80 H40 109.5 . . ?
H39 C80 H40 109.5 . . ?
O4 C80 H41 109.5 . . ?
H39 C80 H41 109.5 . . ?
H40 C80 H41 109.5 . . ?
C81 C82 C83 111.4(2) . . ?
C81 C82 H42 109.4 . . ?
C83 C82 H42 109.4 . . ?
C81 C82 H43 109.4 . . ?
C83 C82 H43 109.4 . . ?
H42 C82 H43 108.0 . . ?
C84 C83 C82 115.6(2) . . ?
C84 C83 H44 108.4 . . ?
C82 C83 H44 108.4 . . ?
C84 C83 H45 108.4 . . ?
C82 C83 H45 108.4 . . ?
H44 C83 H45 107.4 . . ?
C83 C84 H46 109.5 . . ?
C83 C84 H47 109.5 . . ?
H46 C84 H47 109.5 . . ?
C83 C84 H48 109.5 . . ?
H46 C84 H48 109.5 . . ?
H47 C84 H48 109.5 . . ?
C87 C86 C85 113.74(19) . . ?
C87 C86 H49 108.8 . . ?
C85 C86 H49 108.8 . . ?
C87 C86 H50 108.8 . . ?
C85 C86 H50 108.8 . . ?
H49 C86 H50 107.7 . . ?
C88 C87 C86 114.9(2) . . ?
C88 C87 H51 108.5 . . ?
C86 C87 H51 108.5 . . ?
C88 C87 H52 108.5 . . ?
C86 C87 H52 108.5 . . ?
H51 C87 H52 107.5 . . ?
C87 C88 H53 109.5 . . ?
C87 C88 H54 109.5 . . ?
H53 C88 H54 109.5 . . ?
C87 C88 H55 109.5 . . ?
H53 C88 H55 109.5 . . ?
H54 C88 H55 109.5 . . ?
C89 C90 C91 113.1(2) . . ?
C89 C90 H56 109.0 . . ?
C91 C90 H56 109.0 . . ?
C89 C90 H57 109.0 . . ?
C91 C90 H57 109.0 . . ?
H56 C90 H57 107.8 . . ?
C92 C91 C90 116.1(3) . . ?
C92 C91 H58 108.3 . . ?
C90 C91 H58 108.3 . . ?
C92 C91 H59 108.3 . . ?
C90 C91 H59 108.3 . . ?
H58 C91 H59 107.4 . . ?
C91 C92 H60 109.5 . . ?
C91 C92 H61 109.5 . . ?
H60 C92 H61 109.5 . . ?
C91 C92 H62 109.5 . . ?
H60 C92 H62 109.5 . . ?
H61 C92 H62 109.5 . . ?
C28 N3 C25 107.93(16) . . ?
C28 N3 C43 122.22(16) . . ?
C25 N3 C43 129.03(17) . . ?
C74 N6 C71 108.09(16) . . ?
C74 N6 C89 122.15(17) . . ?
C71 N6 C89 128.91(17) . . ?
C2 O1 C33 117.58(16) . . ?
C31 O2 C34 117.66(16) . . ?
C48 O3 C79 117.64(16) . . ?
C77 O4 C80 117.64(16) . . ?
C2 C1 C6 115.65(18) . . ?
C2 C1 C32 117.32(18) . . ?
C6 C1 C32 126.78(19) . . ?
C4 C3 C2 121.1(2) . . ?
C4 C3 H63 119.5 . . ?
C2 C3 H63 119.5 . . ?
C3 C4 C5 117.43(19) . . ?
C3 C4 H64 121.3 . . ?
C5 C4 H64 121.3 . . ?
O1 C2 C3 121.13(19) . . ?
O1 C2 C1 116.28(18) . . ?
C3 C2 C1 122.59(19) . . ?
N1 C5 C4 127.54(19) . . ?
N1 C5 C6 110.04(18) . . ?
C4 C5 C6 122.27(19) . . ?
C8 C7 C16 117.61(18) . . ?
C8 C7 C6 107.72(17) . . ?
C16 C7 C6 132.36(19) . . ?
N2 C39 C40 113.61(17) . . ?
N2 C39 H65 108.8 . . ?
C40 C39 H65 108.8 . . ?
N2 C39 H66 108.8 . . ?
C40 C39 H66 108.8 . . ?
H65 C39 H66 107.7 . . ?
C48 C47 C52 115.78(18) . . ?
C48 C47 C78 117.11(18) . . ?
C52 C47 C78 126.85(18) . . ?
C57 C56 C55 121.6(2) . . ?
C57 C56 H67 119.2 . . ?
C55 C56 H67 119.2 . . ?
C56 C57 C58 119.9(2) . . ?
C56 C57 H68 120.1 . . ?
C58 C57 H68 120.1 . . ?
C59 C58 C57 119.9(2) . . ?
C59 C58 H69 120.0 . . ?
C57 C58 H69 120.0 . . ?
C58 C59 C60 121.9(2) . . ?
C58 C59 H70 119.0 . . ?
C60 C59 H70 119.0 . . ?
C62 C61 N5 109.26(17) . . ?
C62 C61 C60 122.88(19) . . ?
N5 C61 C60 127.74(19) . . ?
C77 C78 C73 115.68(18) . . ?
C77 C78 C47 116.84(18) . . ?
C73 C78 C47 127.14(18) . . ?
N4 C81 C82 113.71(17) . . ?
N4 C81 H71 108.8 . . ?
C82 C81 H71 108.8 . . ?
N4 C81 H72 108.8 . . ?
C82 C81 H72 108.8 . . ?
H71 C81 H72 107.7 . . ?
N5 C85 C86 113.68(17) . . ?
N5 C85 H73 108.8 . . ?
C86 C85 H73 108.8 . . ?
N5 C85 H74 108.8 . . ?
C86 C85 H74 108.8 . . ?
H73 C85 H74 107.7 . . ?
N6 C89 C90 113.66(18) . . ?
N6 C89 H75 108.8 . . ?
C90 C89 H75 108.8 . . ?
N6 C89 H76 108.8 . . ?
C90 C89 H76 108.8 . . ?
H75 C89 H76 107.7 . . ?
C5 N1 C8 107.67(17) . . ?
C5 N1 C97 120.81(18) . . ?
C8 N1 C97 129.06(17) . . ?
C18 N2 C15 106.50(16) . . ?
C18 N2 C39 119.17(16) . . ?
C15 N2 C39 123.42(17) . . ?
C51 N4 C54 107.83(17) . . ?
C51 N4 C81 120.85(18) . . ?
C54 N4 C81 128.90(18) . . ?
C64 N5 C61 106.39(16) . . ?
C64 N5 C85 119.31(16) . . ?
C61 N5 C85 123.42(16) . . ?
O3 C48 C49 121.24(19) . . ?
O3 C48 C47 116.43(18) . . ?
C49 C48 C47 122.3(2) . . ?
C50 C49 C48 121.3(2) . . ?
C50 C49 H77 119.4 . . ?
C48 C49 H77 119.4 . . ?
C49 C50 C51 117.33(19) . . ?
C49 C50 H78 121.3 . . ?
C51 C50 H78 121.3 . . ?
C47 C52 C51 119.32(19) . . ?
C47 C52 C53 135.32(19) . . ?
C51 C52 C53 105.35(18) . . ?
C54 C53 C62 117.61(19) . . ?
C54 C53 C52 107.54(18) . . ?
C62 C53 C52 132.48(18) . . ?
C18 C17 C16 106.73(17) . . ?
C18 C17 C26 118.28(18) . . ?
C16 C17 C26 134.41(18) . . ?
O2 C31 C30 121.72(18) . . ?
O2 C31 C32 115.82(18) . . ?
C30 C31 C32 122.45(18) . . ?
N4 C51 C50 127.65(19) . . ?
N4 C51 C52 109.71(18) . . ?
C50 C51 C52 122.47(19) . . ?
N4 C54 C53 109.05(18) . . ?
N4 C54 C55 127.69(18) . . ?
C53 C54 C55 122.99(19) . . ?
C56 C55 C60 118.5(2) . . ?
C56 C55 C54 123.9(2) . . ?
C60 C55 C54 117.58(18) . . ?
C59 C60 C55 117.65(19) . . ?
C59 C60 C61 124.48(19) . . ?
C55 C60 C61 117.82(19) . . ?
C61 C62 C53 119.41(18) . . ?
C61 C62 C63 107.10(18) . . ?
C53 C62 C63 132.78(19) . . ?
C64 C63 C72 118.37(18) . . ?
C64 C63 C62 106.83(18) . . ?
C72 C63 C62 134.24(19) . . ?
C63 C64 N5 110.36(17) . . ?
C63 C64 C65 123.09(19) . . ?
N5 C64 C65 126.51(19) . . ?
C66 C65 C70 118.83(18) . . ?
C66 C65 C64 123.3(2) . . ?
C70 C65 C64 117.81(19) . . ?
C67 C66 C65 121.5(2) . . ?
C67 C66 H79 119.3 . . ?
C65 C66 H79 119.3 . . ?
C69 C70 C65 117.92(19) . . ?
C69 C70 C71 125.0(2) . . ?
C65 C70 C71 117.00(18) . . ?
N6 C71 C72 108.78(18) . . ?
N6 C71 C70 128.88(18) . . ?
C72 C71 C70 122.34(19) . . ?
C71 C72 C63 118.15(19) . . ?
C71 C72 C73 107.63(18) . . ?
C63 C72 C73 132.10(18) . . ?
C78 C73 C74 119.69(19) . . ?
C78 C73 C72 134.93(19) . . ?
C74 C73 C72 105.38(17) . . ?
N6 C74 C75 128.41(19) . . ?
N6 C74 C73 109.67(18) . . ?
C75 C74 C73 121.90(19) . . ?
C76 C75 C74 117.78(19) . . ?
C76 C75 H80 121.1 . . ?
C74 C75 H80 121.1 . . ?
C75 C76 C77 121.17(19) . . ?
C75 C76 H81 119.4 . . ?
C77 C76 H81 119.4 . . ?
O4 C77 C76 121.91(18) . . ?
O4 C77 C78 115.92(18) . . ?
C76 C77 C78 122.17(19) . . ?
N1 C97 C98 113.75(18) . . ?
N1 C97 H82 108.8 . . ?
C98 C97 H82 108.8 . . ?
N1 C97 H83 108.8 . . ?
C98 C97 H83 108.8 . . ?
H82 C97 H83 107.7 . . ?
C97 C98 C99 111.4(2) . . ?
C97 C98 H84 109.3 . . ?
C99 C98 H84 109.3 . . ?
C97 C98 H85 109.3 . . ?
C99 C98 H85 109.3 . . ?
H84 C98 H85 108.0 . . ?
C99 C100 H86 109.5 . . ?
C99 C100 H87 109.5 . . ?
H86 C100 H87 109.5 . . ?
C99 C100 H88 109.5 . . ?
H86 C100 H88 109.5 . . ?
H87 C100 H88 109.5 . . ?
C100 C99 C98 115.8(2) . . ?
C100 C99 H89 108.3 . . ?
C98 C99 H89 108.3 . . ?
C100 C99 H90 108.3 . . ?
C98 C99 H90 108.3 . . ?
H89 C99 H90 107.4 . . ?
O7 S5 C101 99.3(3) . . ?
O7 S5 C102 100.5(3) . . ?
C101 S5 C102 95.3(3) . . ?
S5 C102 H91 109.5 . . ?
S5 C102 H92 109.5 . . ?
H91 C102 H92 109.5 . . ?
S5 C102 H93 109.5 . . ?
H91 C102 H93 109.5 . . ?
H92 C102 H93 109.5 . . ?
S5 C101 H94 109.5 . . ?
S5 C101 H95 109.5 . . ?
H94 C101 H95 109.5 . . ?
S5 C101 H96 109.5 . . ?
H94 C101 H96 109.5 . . ?
H95 C101 H96 109.5 . . ?
O9 S6 C104 105.6(4) . . ?
O9 S6 C103 89.8(5) . . ?
C104 S6 C103 96.9(6) . . ?
S6 C103 H97 109.5 . . ?
S6 C103 H98 109.5 . . ?
H97 C103 H98 109.5 . . ?
S6 C103 H99 109.5 . . ?
H97 C103 H99 109.5 . . ?
H98 C103 H99 109.5 . . ?
S6 C104 H100 109.5 . . ?
S6 C104 H101 109.5 . . ?
H100 C104 H101 109.5 . . ?
S6 C104 H102 109.5 . . ?
H100 C104 H102 109.5 . . ?
H101 C104 H102 109.5 . . ?
O6 S3 C95 106.5(3) . . ?
O6 S3 C96 104.5(2) . . ?
C95 S3 C96 94.4(2) . . ?
S3 C95 H103 109.5 . . ?
S3 C95 H104 109.5 . . ?
H103 C95 H104 109.5 . . ?
S3 C95 H105 109.5 . . ?
H103 C95 H105 109.5 . . ?
H104 C95 H105 109.5 . . ?
S3 C96 H106 109.5 . . ?
S3 C96 H107 109.5 . . ?
H106 C96 H107 109.5 . . ?
S3 C96 H108 109.5 . . ?
H106 C96 H108 109.5 . . ?
H107 C96 H108 109.5 . . ?
C202 S8 C201 123.7(9) . . ?
C202 S8 O12 114.0(9) . . ?
C201 S8 O12 108.5(5) . . ?
S8 C201 H109 109.5 . . ?
S8 C201 H110 109.5 . . ?
H109 C201 H110 109.5 . . ?
S8 C201 H111 109.5 . . ?
H109 C201 H111 109.5 . . ?
H110 C201 H111 109.5 . . ?
S8 C202 H112 109.5 . . ?
S8 C202 H113 109.5 . . ?
H112 C202 H113 109.5 . . ?
S8 C202 H114 109.5 . . ?
H112 C202 H114 109.5 . . ?
H113 C202 H114 109.5 . . ?
S7 C200 H115 109.5 . . ?
S7 C200 H116 109.5 . . ?
H115 C200 H116 109.5 . . ?
S7 C200 H117 109.5 . . ?
H115 C200 H117 109.5 . . ?
H116 C200 H117 109.5 . . ?
O11 S7 C200 102.8(5) . . ?
O11 S7 C107 105.6(6) . . ?
C200 S7 C107 95.7(7) . . ?
S7 C107 H118 109.5 . . ?
S7 C107 H119 109.5 . . ?
H118 C107 H119 109.5 . . ?
S7 C107 H120 109.5 . . ?
H118 C107 H120 109.5 . . ?
H119 C107 H120 109.5 . . ?
O13 S9 C203 128.6(14) . . ?
O13 S9 C204 92.3(6) . . ?
C203 S9 C204 123.2(14) . . ?
S9 C203 H121 109.5 . . ?
S9 C203 H122 109.5 . . ?
H121 C203 H122 109.5 . . ?
S9 C203 H123 109.5 . . ?
H121 C203 H123 109.5 . . ?
H122 C203 H123 109.5 . . ?
S9 C204 H124 109.5 . . ?
S9 C204 H125 109.5 . . ?
H124 C204 H125 109.5 . . ?
S9 C204 H126 109.5 . . ?
H124 C204 H126 109.5 . . ?
H125 C204 H126 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C8 C9 C10 -20.5(3) . . . . ?
C7 C8 C9 C10 166.3(2) . . . . ?
N1 C8 C9 C14 157.5(2) . . . . ?
C7 C8 C9 C14 -15.7(3) . . . . ?
C14 C9 C10 C11 -5.4(3) . . . . ?
C8 C9 C10 C11 172.7(2) . . . . ?
C9 C10 C11 C12 -0.9(3) . . . . ?
C10 C11 C12 C13 4.2(3) . . . . ?
C11 C12 C13 C14 -1.2(3) . . . . ?
C12 C13 C14 C9 -5.0(3) . . . . ?
C12 C13 C14 C15 177.7(2) . . . . ?
C10 C9 C14 C13 8.1(3) . . . . ?
C8 C9 C14 C13 -170.01(19) . . . . ?
C10 C9 C14 C15 -174.41(19) . . . . ?
C8 C9 C14 C15 7.4(3) . . . . ?
C16 C15 C14 C13 179.7(2) . . . . ?
N2 C15 C14 C13 4.1(3) . . . . ?
C16 C15 C14 C9 2.5(3) . . . . ?
N2 C15 C14 C9 -173.15(19) . . . . ?
N2 C15 C16 C17 -0.3(2) . . . . ?
C14 C15 C16 C17 -176.64(19) . . . . ?
N2 C15 C16 C7 171.27(17) . . . . ?
C14 C15 C16 C7 -5.1(3) . . . . ?
C17 C18 C19 C20 -161.3(2) . . . . ?
N2 C18 C19 C20 16.1(3) . . . . ?
C17 C18 C19 C24 15.9(3) . . . . ?
N2 C18 C19 C24 -166.68(19) . . . . ?
C18 C19 C20 C21 -179.4(2) . . . . ?
C24 C19 C20 C21 3.4(3) . . . . ?
C19 C20 C21 C22 -1.1(4) . . . . ?
C20 C21 C22 C23 -1.7(4) . . . . ?
C21 C22 C23 C24 2.0(4) . . . . ?
C22 C23 C24 C19 0.4(3) . . . . ?
C22 C23 C24 C25 -176.6(2) . . . . ?
C20 C19 C24 C23 -3.1(3) . . . . ?
C18 C19 C24 C23 179.61(19) . . . . ?
C20 C19 C24 C25 174.2(2) . . . . ?
C18 C19 C24 C25 -3.1(3) . . . . ?
C23 C24 C25 N3 -16.6(4) . . . . ?
C19 C24 C25 N3 166.4(2) . . . . ?
C23 C24 C25 C26 164.1(2) . . . . ?
C19 C24 C25 C26 -12.9(3) . . . . ?
N3 C25 C26 C17 -162.69(18) . . . . ?
C24 C25 C26 C17 16.7(3) . . . . ?
N3 C25 C26 C27 2.9(2) . . . . ?
C24 C25 C26 C27 -177.73(19) . . . . ?
C25 C26 C27 C28 -5.8(2) . . . . ?
C17 C26 C27 C28 156.9(2) . . . . ?
C25 C26 C27 C32 174.1(2) . . . . ?
C17 C26 C27 C32 -23.1(4) . . . . ?
C32 C27 C28 N3 -173.12(18) . . . . ?
C26 C27 C28 N3 6.8(2) . . . . ?
C32 C27 C28 C29 8.2(3) . . . . ?
C26 C27 C28 C29 -171.8(2) . . . . ?
N3 C28 C29 C30 -176.1(2) . . . . ?
C27 C28 C29 C30 2.3(3) . . . . ?
C28 C29 C30 C31 -5.8(3) . . . . ?
C28 C27 C32 C31 -14.5(3) . . . . ?
C26 C27 C32 C31 165.6(2) . . . . ?
C28 C27 C32 C1 158.5(2) . . . . ?
C26 C27 C32 C1 -21.5(4) . . . . ?
C39 C40 C41 C42 -65.3(3) . . . . ?
N3 C43 C44 C45 -59.0(3) . . . . ?
C43 C44 C45 C46 -177.0(3) . . . . ?
C66 C67 C68 C69 -1.5(4) . . . . ?
C67 C68 C69 C70 1.8(4) . . . . ?
C81 C82 C83 C84 -170.7(3) . . . . ?
C85 C86 C87 C88 -65.4(3) . . . . ?
C89 C90 C91 C92 -176.5(3) . . . . ?
C29 C28 N3 C25 173.3(2) . . . . ?
C27 C28 N3 C25 -5.2(2) . . . . ?
C29 C28 N3 C43 2.9(3) . . . . ?
C27 C28 N3 C43 -175.71(18) . . . . ?
C26 C25 N3 C28 1.4(2) . . . . ?
C24 C25 N3 C28 -178.0(2) . . . . ?
C26 C25 N3 C43 171.0(2) . . . . ?
C24 C25 N3 C43 -8.4(4) . . . . ?
C44 C43 N3 C28 99.8(2) . . . . ?
C44 C43 N3 C25 -68.5(3) . . . . ?
C5 C6 C1 C2 -14.2(3) . . . . ?
C7 C6 C1 C2 164.3(2) . . . . ?
C5 C6 C1 C32 159.8(2) . . . . ?
C7 C6 C1 C32 -21.7(4) . . . . ?
C31 C32 C1 C2 45.0(3) . . . . ?
C27 C32 C1 C2 -127.9(2) . . . . ?
C31 C32 C1 C6 -128.9(2) . . . . ?
C27 C32 C1 C6 58.2(3) . . . . ?
C2 C3 C4 C5 -5.3(3) . . . . ?
C33 O1 C2 C3 19.8(3) . . . . ?
C33 O1 C2 C1 -160.86(19) . . . . ?
C4 C3 C2 O1 -179.82(19) . . . . ?
C4 C3 C2 C1 0.9(3) . . . . ?
C6 C1 C2 O1 -170.38(17) . . . . ?
C32 C1 C2 O1 15.0(3) . . . . ?
C6 C1 C2 C3 8.9(3) . . . . ?
C32 C1 C2 C3 -165.65(19) . . . . ?
C3 C4 C5 N1 -175.7(2) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . . ?
C1 C6 C5 N1 -173.45(18) . . . . ?
C7 C6 C5 N1 7.6(2) . . . . ?
C1 C6 C5 C4 10.5(3) . . . . ?
C7 C6 C5 C4 -168.4(2) . . . . ?
N1 C8 C7 C16 -161.15(18) . . . . ?
C9 C8 C7 C16 13.2(3) . . . . ?
N1 C8 C7 C6 3.7(2) . . . . ?
C9 C8 C7 C6 178.05(19) . . . . ?
C15 C16 C7 C8 -2.6(3) . . . . ?
C17 C16 C7 C8 166.4(2) . . . . ?
C15 C16 C7 C6 -162.9(2) . . . . ?
C17 C16 C7 C6 6.1(4) . . . . ?
C1 C6 C7 C8 174.5(2) . . . . ?
C5 C6 C7 C8 -6.8(2) . . . . ?
C1 C6 C7 C16 -23.7(4) . . . . ?
C5 C6 C7 C16 154.9(2) . . . . ?
C41 C40 C39 N2 -53.6(3) . . . . ?
C55 C56 C57 C58 -0.8(3) . . . . ?
C56 C57 C58 C59 4.1(3) . . . . ?
C57 C58 C59 C60 -1.0(3) . . . . ?
C48 C47 C78 C77 45.1(3) . . . . ?
C52 C47 C78 C77 -128.9(2) . . . . ?
C48 C47 C78 C73 -127.9(2) . . . . ?
C52 C47 C78 C73 58.1(3) . . . . ?
C83 C82 C81 N4 168.8(2) . . . . ?
C87 C86 C85 N5 -53.4(3) . . . . ?
C74 N6 C89 C90 99.9(2) . . . . ?
C71 N6 C89 C90 -68.3(3) . . . . ?
C91 C90 C89 N6 -59.1(3) . . . . ?
C4 C5 N1 C8 170.2(2) . . . . ?
C6 C5 N1 C8 -5.5(2) . . . . ?
C4 C5 N1 C97 6.5(3) . . . . ?
C6 C5 N1 C97 -169.27(18) . . . . ?
C7 C8 N1 C5 1.0(2) . . . . ?
C9 C8 N1 C5 -172.9(2) . . . . ?
C7 C8 N1 C97 163.0(2) . . . . ?
C9 C8 N1 C97 -11.0(4) . . . . ?
C17 C18 N2 C15 2.4(2) . . . . ?
C19 C18 N2 C15 -175.3(2) . . . . ?
C17 C18 N2 C39 -142.98(18) . . . . ?
C19 C18 N2 C39 39.3(3) . . . . ?
C16 C15 N2 C18 -1.3(2) . . . . ?
C14 C15 N2 C18 174.9(2) . . . . ?
C16 C15 N2 C39 142.29(18) . . . . ?
C14 C15 N2 C39 -41.6(3) . . . . ?
C40 C39 N2 C18 98.2(2) . . . . ?
C40 C39 N2 C15 -41.1(3) . . . . ?
C82 C81 N4 C51 -86.4(2) . . . . ?
C82 C81 N4 C54 113.4(2) . . . . ?
C62 C61 N5 C64 -1.3(2) . . . . ?
C60 C61 N5 C64 174.67(19) . . . . ?
C62 C61 N5 C85 142.34(18) . . . . ?
C60 C61 N5 C85 -41.7(3) . . . . ?
C86 C85 N5 C64 98.1(2) . . . . ?
C86 C85 N5 C61 -41.2(3) . . . . ?
C79 O3 C48 C49 19.6(3) . . . . ?
C79 O3 C48 C47 -160.92(18) . . . . ?
C52 C47 C48 O3 -170.40(17) . . . . ?
C78 C47 C48 O3 15.0(3) . . . . ?
C52 C47 C48 C49 9.0(3) . . . . ?
C78 C47 C48 C49 -165.56(19) . . . . ?
O3 C48 C49 C50 -179.72(19) . . . . ?
C47 C48 C49 C50 0.9(3) . . . . ?
C48 C49 C50 C51 -5.3(3) . . . . ?
C48 C47 C52 C51 -14.4(3) . . . . ?
C78 C47 C52 C51 159.62(19) . . . . ?
C48 C47 C52 C53 164.5(2) . . . . ?
C78 C47 C52 C53 -21.5(4) . . . . ?
C47 C52 C53 C54 174.5(2) . . . . ?
C51 C52 C53 C54 -6.5(2) . . . . ?
C47 C52 C53 C62 -24.0(4) . . . . ?
C51 C52 C53 C62 155.0(2) . . . . ?
N2 C18 C17 C16 -2.6(2) . . . . ?
C19 C18 C17 C16 175.20(19) . . . . ?
N2 C18 C17 C26 169.93(18) . . . . ?
C19 C18 C17 C26 -12.3(3) . . . . ?
C15 C16 C17 C18 1.7(2) . . . . ?
C7 C16 C17 C18 -168.2(2) . . . . ?
C15 C16 C17 C26 -169.0(2) . . . . ?
C7 C16 C17 C26 21.0(4) . . . . ?
C25 C26 C17 C18 -4.0(3) . . . . ?
C27 C26 C17 C18 -165.3(2) . . . . ?
C25 C26 C17 C16 166.0(2) . . . . ?
C27 C26 C17 C16 4.6(4) . . . . ?
C34 O2 C31 C30 15.0(3) . . . . ?
C34 O2 C31 C32 -164.3(2) . . . . ?
C29 C30 C31 O2 179.5(2) . . . . ?
C29 C30 C31 C32 -1.2(3) . . . . ?
C27 C32 C31 O2 -169.35(18) . . . . ?
C1 C32 C31 O2 16.9(3) . . . . ?
C27 C32 C31 C30 11.3(3) . . . . ?
C1 C32 C31 C30 -162.4(2) . . . . ?
C54 N4 C51 C50 170.2(2) . . . . ?
C81 N4 C51 C50 6.3(3) . . . . ?
C54 N4 C51 C52 -5.3(2) . . . . ?
C81 N4 C51 C52 -169.14(17) . . . . ?
C49 C50 C51 N4 -175.5(2) . . . . ?
C49 C50 C51 C52 -0.5(3) . . . . ?
C47 C52 C51 N4 -173.51(17) . . . . ?
C53 C52 C51 N4 7.3(2) . . . . ?
C47 C52 C51 C50 10.7(3) . . . . ?
C53 C52 C51 C50 -168.43(19) . . . . ?
C51 N4 C54 C53 1.0(2) . . . . ?
C81 N4 C54 C53 163.13(19) . . . . ?
C51 N4 C54 C55 -173.01(19) . . . . ?
C81 N4 C54 C55 -10.9(3) . . . . ?
C62 C53 C54 N4 -161.13(17) . . . . ?
C52 C53 C54 N4 3.6(2) . . . . ?
C62 C53 C54 C55 13.2(3) . . . . ?
C52 C53 C54 C55 177.91(18) . . . . ?
C57 C56 C55 C60 -5.5(3) . . . . ?
C57 C56 C55 C54 172.7(2) . . . . ?
N4 C54 C55 C56 -20.7(3) . . . . ?
C53 C54 C55 C56 166.10(19) . . . . ?
N4 C54 C55 C60 157.51(19) . . . . ?
C53 C54 C55 C60 -15.7(3) . . . . ?
C58 C59 C60 C55 -5.2(3) . . . . ?
C58 C59 C60 C61 177.5(2) . . . . ?
C56 C55 C60 C59 8.3(3) . . . . ?
C54 C55 C60 C59 -170.01(18) . . . . ?
C56 C55 C60 C61 -174.25(18) . . . . ?
C54 C55 C60 C61 7.5(3) . . . . ?
C62 C61 C60 C59 179.73(19) . . . . ?
N5 C61 C60 C59 4.2(3) . . . . ?
C62 C61 C60 C55 2.4(3) . . . . ?
N5 C61 C60 C55 -173.07(18) . . . . ?
N5 C61 C62 C53 171.22(17) . . . . ?
C60 C61 C62 C53 -5.0(3) . . . . ?
N5 C61 C62 C63 -0.3(2) . . . . ?
C60 C61 C62 C63 -176.52(17) . . . . ?
C54 C53 C62 C61 -2.6(3) . . . . ?
C52 C53 C62 C61 -162.7(2) . . . . ?
C54 C53 C62 C63 166.3(2) . . . . ?
C52 C53 C62 C63 6.2(4) . . . . ?
C61 C62 C63 C64 1.8(2) . . . . ?
C53 C62 C63 C64 -168.1(2) . . . . ?
C61 C62 C63 C72 -169.1(2) . . . . ?
C53 C62 C63 C72 21.0(4) . . . . ?
C72 C63 C64 N5 169.90(16) . . . . ?
C62 C63 C64 N5 -2.7(2) . . . . ?
C72 C63 C64 C65 -12.1(3) . . . . ?
C62 C63 C64 C65 175.28(18) . . . . ?
C61 N5 C64 C63 2.5(2) . . . . ?
C85 N5 C64 C63 -142.92(17) . . . . ?
C61 N5 C64 C65 -175.39(19) . . . . ?
C85 N5 C64 C65 39.2(3) . . . . ?
C63 C64 C65 C66 -161.4(2) . . . . ?
N5 C64 C65 C66 16.3(3) . . . . ?
C63 C64 C65 C70 15.8(3) . . . . ?
N5 C64 C65 C70 -166.55(18) . . . . ?
C68 C67 C66 C65 -1.2(4) . . . . ?
C70 C65 C66 C67 3.4(3) . . . . ?
C64 C65 C66 C67 -179.4(2) . . . . ?
C68 C69 C70 C65 0.4(3) . . . . ?
C68 C69 C70 C71 -176.6(2) . . . . ?
C66 C65 C70 C69 -3.0(3) . . . . ?
C64 C65 C70 C69 179.69(19) . . . . ?
C66 C65 C70 C71 174.26(18) . . . . ?
C64 C65 C70 C71 -3.1(3) . . . . ?
C74 N6 C71 C72 1.6(2) . . . . ?
C89 N6 C71 C72 171.03(18) . . . . ?
C74 N6 C71 C70 -178.0(2) . . . . ?
C89 N6 C71 C70 -8.6(3) . . . . ?
C69 C70 C71 N6 -16.4(3) . . . . ?
C65 C70 C71 N6 166.53(19) . . . . ?
C69 C70 C71 C72 164.0(2) . . . . ?
C65 C70 C71 C72 -13.0(3) . . . . ?
N6 C71 C72 C63 -162.74(17) . . . . ?
C70 C71 C72 C63 16.9(3) . . . . ?
N6 C71 C72 C73 2.7(2) . . . . ?
C70 C71 C72 C73 -177.66(17) . . . . ?
C64 C63 C72 C71 -4.2(3) . . . . ?
C62 C63 C72 C71 165.9(2) . . . . ?
C64 C63 C72 C73 -165.4(2) . . . . ?
C62 C63 C72 C73 4.7(4) . . . . ?
C77 C78 C73 C74 -14.5(3) . . . . ?
C47 C78 C73 C74 158.52(19) . . . . ?
C77 C78 C73 C72 165.5(2) . . . . ?
C47 C78 C73 C72 -21.4(4) . . . . ?
C71 C72 C73 C78 174.2(2) . . . . ?
C63 C72 C73 C78 -23.2(4) . . . . ?
C71 C72 C73 C74 -5.8(2) . . . . ?
C63 C72 C73 C74 156.9(2) . . . . ?
C71 N6 C74 C75 173.3(2) . . . . ?
C89 N6 C74 C75 2.9(3) . . . . ?
C71 N6 C74 C73 -5.3(2) . . . . ?
C89 N6 C74 C73 -175.66(17) . . . . ?
C78 C73 C74 N6 -173.10(17) . . . . ?
C72 C73 C74 N6 6.8(2) . . . . ?
C78 C73 C74 C75 8.2(3) . . . . ?
C72 C73 C74 C75 -171.86(19) . . . . ?
N6 C74 C75 C76 -176.1(2) . . . . ?
C73 C74 C75 C76 2.3(3) . . . . ?
C74 C75 C76 C77 -5.8(3) . . . . ?
C80 O4 C77 C76 15.0(3) . . . . ?
C80 O4 C77 C78 -164.23(19) . . . . ?
C75 C76 C77 O4 179.51(19) . . . . ?
C75 C76 C77 C78 -1.3(3) . . . . ?
C73 C78 C77 O4 -169.32(17) . . . . ?
C47 C78 C77 O4 16.9(3) . . . . ?
C73 C78 C77 C76 11.4(3) . . . . ?
C47 C78 C77 C76 -162.38(19) . . . . ?
C5 N1 C97 C98 -86.9(3) . . . . ?
C8 N1 C97 C98 113.2(2) . . . . ?
N1 C97 C98 C99 169.2(2) . . . . ?
C97 C98 C99 C100 -170.1(3) . . . . ?

_refine_diff_density_max         1.037
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.080

####################################################################### 
# 
# 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_181122matsuo
_audit_block_doi                 10.5517/ccdc.csd.cc23kw7t
_database_code_depnum_ccdc_archive 'CCDC 1953596'
loop_
_audit_author_name
_audit_author_address
'Yusuke Matsuo'
;Kyoto University
Japan
;
_audit_update_record             
;
2019-09-14 deposited with the CCDC.	2019-10-30 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 H17 Cl2 N3, 3(C4 H8 O)'
_chemical_formula_sum            'C44 H41 Cl2 N3 O3'
_chemical_formula_weight         730.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.02860(10)
_cell_length_b                   12.6096(2)
_cell_length_c                   12.8296(2)
_cell_angle_alpha                74.4620(10)
_cell_angle_beta                 75.3610(10)
_cell_angle_gamma                86.8280(10)
_cell_volume                     1813.80(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    2745
_cell_measurement_theta_min      25.2
_cell_measurement_theta_max      74.3

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.973
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
;
Rigaku Pilatus 200K
;
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            20594
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.639
_diffrn_reflns_theta_max         66.992
_diffrn_reflns_theta_full        66.992
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             6302
_reflns_number_gt                6204
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0760P)²+0.9607P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6302
_refine_ls_number_parameters     607
_refine_ls_number_restraints     360
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1255
_refine_ls_wR_factor_gt          0.1251
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.076
_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
C1 C 0.19442(15) 0.27756(14) 0.50496(14) 0.0246(4) Uani 1 1 d . . . . .
H1 H 0.2751 0.2874 0.4752 0.029 Uiso 1 1 calc R U . . .
C2 C 0.14994(17) 0.20220(14) 0.60462(15) 0.0297(4) Uani 1 1 d . . . . .
C3 C 0.03222(18) 0.18640(15) 0.65276(15) 0.0323(4) Uani 1 1 d . . . . .
H2 H 0.0055 0.1309 0.7203 0.039 Uiso 1 1 calc R U . . .
C4 C -0.04546(16) 0.25192(15) 0.60169(15) 0.0301(4) Uani 1 1 d . . . . .
H3 H -0.1257 0.2442 0.6346 0.036 Uiso 1 1 calc R U . . .
C5 C -0.00258(15) 0.32942(14) 0.50079(15) 0.0249(4) Uani 1 1 d . . . . .
C6 C 0.11661(14) 0.33969(13) 0.44844(14) 0.0215(3) Uani 1 1 d . . . . .
C7 C 0.12897(14) 0.42383(13) 0.34522(14) 0.0206(3) Uani 1 1 d . . . . .
C8 C 0.01923(14) 0.46632(14) 0.34391(14) 0.0232(3) Uani 1 1 d . . . . .
C9 C -0.00359(15) 0.56051(14) 0.26141(15) 0.0247(4) Uani 1 1 d . . . . .
C10 C -0.11488(16) 0.59838(16) 0.25665(17) 0.0307(4) Uani 1 1 d . . . . .
H4 H -0.1797 0.5594 0.3092 0.037 Uiso 1 1 calc R U . . .
N1 N -0.05976(12) 0.40660(12) 0.43625(12) 0.0262(3) Uani 1 1 d . . . . .
H5 H -0.1345 0.4164 0.4513 0.031 Uiso 1 1 calc R U . . .
N2 N 0.30801(12) 0.62144(11) 0.11802(11) 0.0219(3) Uani 1 1 d . . . . .
H6 H 0.3176 0.6861 0.0688 0.026 Uiso 1 1 calc R U . . .
C11 C -0.13091(17) 0.69133(17) 0.17665(18) 0.0358(5) Uani 1 1 d . . . . .
H7 H -0.2066 0.7155 0.1737 0.043 Uiso 1 1 calc R U . . .
C12 C -0.03633(18) 0.75040(17) 0.09972(17) 0.0353(4) Uani 1 1 d . . . . .
H8 H -0.0480 0.8151 0.0454 0.042 Uiso 1 1 calc R U . . .
C13 C 0.07372(17) 0.71538(15) 0.10222(15) 0.0294(4) Uani 1 1 d . . . . .
H9 H 0.1374 0.7561 0.0495 0.035 Uiso 1 1 calc R U . . .
C14 C 0.09276(15) 0.61971(14) 0.18221(14) 0.0238(4) Uani 1 1 d . . . . .
C15 C 0.20480(14) 0.57624(13) 0.18533(13) 0.0217(3) Uani 1 1 d . . . . .
C16 C 0.22442(14) 0.47442(13) 0.25557(13) 0.0201(3) Uani 1 1 d . . . . .
C17 C 0.34493(14) 0.45334(13) 0.22028(13) 0.0196(3) Uani 1 1 d . . . . .
C18 C 0.39396(14) 0.54894(13) 0.14016(13) 0.0202(3) Uani 1 1 d . . . . .
C19 C 0.51477(14) 0.56735(13) 0.09386(13) 0.0204(3) Uani 1 1 d . . . . .
C20 C 0.56315(15) 0.66655(14) 0.01706(13) 0.0236(3) Uani 1 1 d . . . . .
H10 H 0.5145 0.7256 -0.0056 0.028 Uiso 1 1 calc R U . . .
C21 C 0.68015(15) 0.67793(14) -0.02490(14) 0.0263(4) Uani 1 1 d . . . . .
H11 H 0.7116 0.7447 -0.0767 0.032 Uiso 1 1 calc R U . . .
C22 C 0.75361(15) 0.59218(15) 0.00777(15) 0.0268(4) Uani 1 1 d . . . . .
H12 H 0.8343 0.6009 -0.0222 0.032 Uiso 1 1 calc R U . . .
C23 C 0.70907(15) 0.49549(14) 0.08307(14) 0.0242(4) Uani 1 1 d . . . . .
H13 H 0.7593 0.4379 0.1053 0.029 Uiso 1 1 calc R U . . .
C24 C 0.58952(14) 0.48096(13) 0.12762(13) 0.0201(3) Uani 1 1 d . . . . .
C25 C 0.53774(14) 0.37930(13) 0.19975(13) 0.0197(3) Uani 1 1 d . . . . .
C26 C 0.41960(14) 0.36138(13) 0.24197(13) 0.0184(3) Uani 1 1 d . . . . .
C27 C 0.40362(14) 0.24399(13) 0.28856(13) 0.0191(3) Uani 1 1 d . . . . .
C28 C 0.51502(14) 0.19880(13) 0.28169(13) 0.0199(3) Uani 1 1 d . . . . .
C29 C 0.53165(15) 0.08682(14) 0.32426(14) 0.0251(4) Uani 1 1 d . . . . .
H14 H 0.6065 0.0587 0.3245 0.030 Uiso 1 1 calc R U . . .
C30 C 0.43652(15) 0.01790(14) 0.36606(15) 0.0274(4) Uani 1 1 d . . . . .
H15 H 0.4451 -0.0586 0.3967 0.033 Uiso 1 1 calc R U . . .
C31 C 0.32727(15) 0.06115(14) 0.36310(14) 0.0249(4) Uani 1 1 d . . . . .
C32 C 0.30825(14) 0.17218(13) 0.32629(13) 0.0210(3) Uani 1 1 d . . . . .
H16 H 0.2329 0.1992 0.3265 0.025 Uiso 1 1 calc R U . . .
N3 N 0.59500(12) 0.28128(11) 0.22696(11) 0.0210(3) Uani 1 1 d . . . . .
H17 H 0.6700 0.2733 0.2117 0.025 Uiso 1 1 calc R U . . .
Cl1 Cl 0.24700(5) 0.12417(4) 0.67548(4) 0.04613(17) Uani 1 1 d . . . . .
Cl2 Cl 0.20976(4) -0.02996(3) 0.40771(4) 0.03880(15) Uani 1 1 d . . . . .
O1 O -0.309(2) 0.3999(14) 0.5101(17) 0.038(2) Uani 0.477(14) 1 d . U P A 1
C34 C -0.3587(6) 0.3399(11) 0.6195(5) 0.0426(19) Uani 0.477(14) 1 d . U P A 1
H18 H -0.3027 0.2866 0.6477 0.051 Uiso 0.477(14) 1 calc R U P A 1
H19 H -0.3799 0.3904 0.6684 0.051 Uiso 0.477(14) 1 calc R U P A 1
C35 C -0.4412(9) 0.2925(5) 0.6214(6) 0.0415(19) Uani 0.477(14) 1 d . U P A 1
H20 H -0.5084 0.3129 0.6749 0.050 Uiso 0.477(14) 1 calc R U P A 1
H21 H -0.4301 0.2122 0.6466 0.050 Uiso 0.477(14) 1 calc R U P A 1
C36 C -0.4641(11) 0.3225(12) 0.5018(12) 0.041(2) Uani 0.477(14) 1 d . U P A 1
H22 H -0.4910 0.2580 0.4844 0.050 Uiso 0.477(14) 1 calc R U P A 1
H23 H -0.5197 0.3831 0.4919 0.050 Uiso 0.477(14) 1 calc R U P A 1
C37 C -0.3566(8) 0.3544(9) 0.4413(7) 0.0433(18) Uani 0.477(14) 1 d . U P A 1
H24 H -0.3583 0.4099 0.3707 0.052 Uiso 0.477(14) 1 calc R U P A 1
H25 H -0.3114 0.2907 0.4236 0.052 Uiso 0.477(14) 1 calc R U P A 1
O4 O -0.3069(17) 0.4265(12) 0.4951(15) 0.037(2) Uani 0.523(14) 1 d . U P A 2
C50 C -0.4811(6) 0.3340(11) 0.6311(6) 0.067(2) Uani 0.523(14) 1 d . U P A 2
H26 H -0.4785 0.2571 0.6761 0.080 Uiso 0.523(14) 1 calc R U P A 2
H27 H -0.5460 0.3717 0.6706 0.080 Uiso 0.523(14) 1 calc R U P A 2
C49 C -0.3705(5) 0.3931(7) 0.6107(5) 0.0297(13) Uani 0.523(14) 1 d . U P A 2
H28 H -0.3869 0.4594 0.6391 0.036 Uiso 0.523(14) 1 calc R U P A 2
H29 H -0.3214 0.3447 0.6544 0.036 Uiso 0.523(14) 1 calc R U P A 2
C51 C -0.4929(11) 0.3372(12) 0.5189(12) 0.056(3) Uani 0.523(14) 1 d . U P A 2
H30 H -0.5623 0.3782 0.5043 0.067 Uiso 0.523(14) 1 calc R U P A 2
H31 H -0.4989 0.2616 0.5116 0.067 Uiso 0.523(14) 1 calc R U P A 2
C52 C -0.3765(7) 0.3998(9) 0.4314(7) 0.0477(18) Uani 0.523(14) 1 d . U P A 2
H32 H -0.3345 0.3511 0.3861 0.057 Uiso 0.523(14) 1 calc R U P A 2
H33 H -0.3972 0.4676 0.3804 0.057 Uiso 0.523(14) 1 calc R U P A 2
O2 O 0.3450(7) 0.8581(8) 0.0201(7) 0.0300(11) Uani 0.719(11) 1 d . U P B 3
C38 C 0.3414(6) 0.8913(6) 0.1186(7) 0.0418(14) Uani 0.719(11) 1 d . U P B 3
H34 H 0.4136 0.8715 0.1427 0.050 Uiso 0.719(11) 1 calc R U P B 3
H35 H 0.2762 0.8549 0.1800 0.050 Uiso 0.719(11) 1 calc R U P B 3
C40 C 0.3079(8) 0.9502(8) -0.0578(6) 0.0411(16) Uani 0.719(11) 1 d . U P B 3
H36 H 0.3745 0.9839 -0.1190 0.049 Uiso 0.719(11) 1 calc R U P B 3
H37 H 0.2517 0.9247 -0.0909 0.049 Uiso 0.719(11) 1 calc R U P B 3
C41 C 0.2560(6) 1.0293(4) 0.0009(4) 0.0555(15) Uani 0.719(11) 1 d . U P B 3
H38 H 0.1736 1.0122 0.0366 0.067 Uiso 0.719(11) 1 calc R U P B 3
H39 H 0.2641 1.1049 -0.0491 0.067 Uiso 0.719(11) 1 calc R U P B 3
C42 C 0.3269(6) 1.0150(3) 0.0890(4) 0.0509(13) Uani 0.719(11) 1 d . U P B 3
H40 H 0.4018 1.0543 0.0569 0.061 Uiso 0.719(11) 1 calc R U P B 3
H41 H 0.2843 1.0404 0.1545 0.061 Uiso 0.719(11) 1 calc R U P B 3
O5 O 0.326(2) 0.856(3) 0.036(2) 0.052(6) Uani 0.281(11) 1 d . U P B 4
C54 C 0.3287(15) 1.0482(7) -0.0316(9) 0.054(3) Uani 0.281(11) 1 d . U P B 4
H42 H 0.2879 1.1073 -0.0749 0.065 Uiso 0.281(11) 1 calc R U P B 4
H43 H 0.4072 1.0739 -0.0385 0.065 Uiso 0.281(11) 1 calc R U P B 4
C56 C 0.2991(17) 0.896(2) 0.1297(19) 0.051(4) Uani 0.281(11) 1 d . U P B 4
H44 H 0.3680 0.8962 0.1587 0.061 Uiso 0.281(11) 1 calc R U P B 4
H45 H 0.2386 0.8498 0.1892 0.061 Uiso 0.281(11) 1 calc R U P B 4
C53 C 0.330(2) 0.937(2) -0.067(2) 0.056(5) Uani 0.281(11) 1 d . U P B 4
H46 H 0.2625 0.9307 -0.0961 0.067 Uiso 0.281(11) 1 calc R U P B 4
H47 H 0.4012 0.9309 -0.1242 0.067 Uiso 0.281(11) 1 calc R U P B 4
C55 C 0.259(2) 1.0061(11) 0.0950(12) 0.075(4) Uani 0.281(11) 1 d . U P B 4
H48 H 0.2763 1.0526 0.1404 0.090 Uiso 0.281(11) 1 calc R U P B 4
H49 H 0.1755 1.0064 0.1014 0.090 Uiso 0.281(11) 1 calc R U P B 4
O3 O 0.8392(9) 0.2367(8) 0.1995(7) 0.0277(12) Uani 0.579(8) 1 d . U P C 5
C45 C 0.9343(7) 0.3112(10) 0.1743(9) 0.026(2) Uani 0.579(8) 1 d . U P C 5
H50 H 0.9143 0.3681 0.2161 0.031 Uiso 0.579(8) 1 calc R U P C 5
H51 H 0.9570 0.3481 0.0934 0.031 Uiso 0.579(8) 1 calc R U P C 5
C46 C 1.0301(6) 0.2400(4) 0.2103(6) 0.0258(12) Uani 0.579(8) 1 d . U P C 5
H52 H 1.0741 0.2073 0.1503 0.031 Uiso 0.579(8) 1 calc R U P C 5
H53 H 1.0834 0.2823 0.2320 0.031 Uiso 0.579(8) 1 calc R U P C 5
C47 C 0.9654(12) 0.1530(11) 0.3091(13) 0.052(4) Uani 0.579(8) 1 d . U P C 5
H54 H 1.0095 0.0840 0.3216 0.063 Uiso 0.579(8) 1 calc R U P C 5
H55 H 0.9463 0.1787 0.3779 0.063 Uiso 0.579(8) 1 calc R U P C 5
C48 C 0.8607(4) 0.1380(4) 0.2733(4) 0.0510(16) Uani 0.579(8) 1 d . U P C 5
H56 H 0.8720 0.0777 0.2358 0.061 Uiso 0.579(8) 1 calc R U P C 5
H57 H 0.7944 0.1183 0.3392 0.061 Uiso 0.579(8) 1 calc R U P C 5
O6 O 0.8301(14) 0.2440(13) 0.2276(11) 0.047(3) Uani 0.421(8) 1 d . U P C 6
C59 C 1.0234(11) 0.2055(14) 0.2116(10) 0.078(4) Uani 0.421(8) 1 d . U P C 6
H58 H 1.0404 0.1566 0.1609 0.094 Uiso 0.421(8) 1 calc R U P C 6
H59 H 1.0963 0.2384 0.2117 0.094 Uiso 0.421(8) 1 calc R U P C 6
C57 C 0.9384(14) 0.2953(16) 0.1765(12) 0.043(5) Uani 0.421(8) 1 d . U P C 6
H60 H 0.9460 0.3604 0.2036 0.051 Uiso 0.421(8) 1 calc R U P C 6
H61 H 0.9511 0.3186 0.0943 0.051 Uiso 0.421(8) 1 calc R U P C 6
C60 C 0.8362(4) 0.1795(4) 0.3390(4) 0.0296(15) Uani 0.421(8) 1 d . U P C 6
H62 H 0.7846 0.1142 0.3647 0.035 Uiso 0.421(8) 1 calc R U P C 6
H63 H 0.8145 0.2245 0.3934 0.035 Uiso 0.421(8) 1 calc R U P C 6
C61 C 0.9632(11) 0.1448(11) 0.3251(14) 0.027(2) Uani 0.421(8) 1 d . U P C 6
H64 H 0.9958 0.1643 0.3812 0.032 Uiso 0.421(8) 1 calc R U P C 6
H65 H 0.9702 0.0645 0.3341 0.032 Uiso 0.421(8) 1 calc R U P C 6


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.372(3) . ?
C1 C6 1.405(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.396(3) . ?
C2 Cl1 1.7572(19) . ?
C3 C4 1.385(3) . ?
C3 H2 0.9500 . ?
C4 C5 1.392(3) . ?
C4 H3 0.9500 . ?
C5 N1 1.374(2) . ?
C5 C6 1.418(2) . ?
C6 C7 1.437(2) . ?
C7 C8 1.399(2) . ?
C7 C16 1.438(2) . ?
C8 N1 1.380(2) . ?
C8 C9 1.430(3) . ?
C9 C10 1.407(2) . ?
C9 C14 1.424(3) . ?
C10 C11 1.377(3) . ?
C10 H4 0.9500 . ?
N1 H5 0.8800 . ?
N2 C15 1.373(2) . ?
N2 C18 1.375(2) . ?
N2 H6 0.8800 . ?
C11 C12 1.398(3) . ?
C11 H7 0.9500 . ?
C12 C13 1.378(3) . ?
C12 H8 0.9500 . ?
C13 C14 1.409(3) . ?
C13 H9 0.9500 . ?
C14 C15 1.432(2) . ?
C15 C16 1.404(2) . ?
C16 C17 1.438(2) . ?
C17 C18 1.402(2) . ?
C17 C26 1.438(2) . ?
C18 C19 1.430(2) . ?
C19 C20 1.416(2) . ?
C19 C24 1.421(2) . ?
C20 C21 1.374(3) . ?
C20 H10 0.9500 . ?
C21 C22 1.402(3) . ?
C21 H11 0.9500 . ?
C22 C23 1.373(3) . ?
C22 H12 0.9500 . ?
C23 C24 1.409(2) . ?
C23 H13 0.9500 . ?
C24 C25 1.431(2) . ?
C25 N3 1.386(2) . ?
C25 C26 1.395(2) . ?
C26 C27 1.444(2) . ?
C27 C32 1.403(2) . ?
C27 C28 1.418(2) . ?
C28 N3 1.371(2) . ?
C28 C29 1.394(2) . ?
C29 C30 1.379(3) . ?
C29 H14 0.9500 . ?
C30 C31 1.400(3) . ?
C30 H15 0.9500 . ?
C31 C32 1.379(2) . ?
C31 Cl2 1.7504(17) . ?
C32 H16 0.9500 . ?
N3 H17 0.8800 . ?
O1 C34 1.398(19) . ?
O1 C37 1.41(3) . ?
C34 C35 1.177(12) . ?
C34 H18 0.9900 . ?
C34 H19 0.9900 . ?
C35 C36 1.570(15) . ?
C35 H20 0.9900 . ?
C35 H21 0.9900 . ?
C36 C37 1.349(16) . ?
C36 H22 0.9900 . ?
C36 H23 0.9900 . ?
C37 H24 0.9900 . ?
C37 H25 0.9900 . ?
O4 C52 1.42(2) . ?
O4 C49 1.445(18) . ?
C50 C51 1.470(16) . ?
C50 C49 1.490(8) . ?
C50 H26 0.9900 . ?
C50 H27 0.9900 . ?
C49 H28 0.9900 . ?
C49 H29 0.9900 . ?
C51 C52 1.643(16) . ?
C51 H30 0.9900 . ?
C51 H31 0.9900 . ?
C52 H32 0.9900 . ?
C52 H33 0.9900 . ?
O2 C38 1.424(12) . ?
O2 C40 1.447(11) . ?
C38 C42 1.515(9) . ?
C38 H34 0.9900 . ?
C38 H35 0.9900 . ?
C40 C41 1.432(9) . ?
C40 H36 0.9900 . ?
C40 H37 0.9900 . ?
C41 C42 1.548(7) . ?
C41 H38 0.9900 . ?
C41 H39 0.9900 . ?
C42 H40 0.9900 . ?
C42 H41 0.9900 . ?
O5 C56 1.38(4) . ?
O5 C53 1.43(4) . ?
C54 C53 1.58(3) . ?
C54 C55 1.59(2) . ?
C54 H42 0.9900 . ?
C54 H43 0.9900 . ?
C56 C55 1.43(2) . ?
C56 H44 0.9900 . ?
C56 H45 0.9900 . ?
C53 H46 0.9900 . ?
C53 H47 0.9900 . ?
C55 H48 0.9900 . ?
C55 H49 0.9900 . ?
O3 C48 1.403(11) . ?
O3 C45 1.437(12) . ?
C45 C46 1.510(12) . ?
C45 H50 0.9900 . ?
C45 H51 0.9900 . ?
C46 C47 1.506(16) . ?
C46 H52 0.9900 . ?
C46 H53 0.9900 . ?
C47 C48 1.482(13) . ?
C47 H54 0.9900 . ?
C47 H55 0.9900 . ?
C48 H56 0.9900 . ?
C48 H57 0.9900 . ?
O6 C57 1.41(2) . ?
O6 C60 1.460(15) . ?
C59 C61 1.47(2) . ?
C59 C57 1.54(2) . ?
C59 H58 0.9900 . ?
C59 H59 0.9900 . ?
C57 H60 0.9900 . ?
C57 H61 0.9900 . ?
C60 C61 1.546(14) . ?
C60 H62 0.9900 . ?
C60 H63 0.9900 . ?
C61 H64 0.9900 . ?
C61 H65 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
C2 C1 C6 117.70(16) . . ?
C2 C1 H1 121.1 . . ?
C6 C1 H1 121.1 . . ?
C1 C2 C3 123.24(17) . . ?
C1 C2 Cl1 117.84(15) . . ?
C3 C2 Cl1 118.91(14) . . ?
C4 C3 C2 119.75(17) . . ?
C4 C3 H2 120.1 . . ?
C2 C3 H2 120.1 . . ?
C3 C4 C5 118.12(17) . . ?
C3 C4 H3 120.9 . . ?
C5 C4 H3 120.9 . . ?
N1 C5 C4 129.70(16) . . ?
N1 C5 C6 108.51(15) . . ?
C4 C5 C6 121.78(17) . . ?
C1 C6 C5 119.07(15) . . ?
C1 C6 C7 134.12(15) . . ?
C5 C6 C7 106.63(14) . . ?
C8 C7 C6 106.39(15) . . ?
C8 C7 C16 118.36(15) . . ?
C6 C7 C16 135.03(15) . . ?
N1 C8 C7 109.35(15) . . ?
N1 C8 C9 126.58(15) . . ?
C7 C8 C9 124.01(16) . . ?
C10 C9 C14 119.10(17) . . ?
C10 C9 C8 123.56(17) . . ?
C14 C9 C8 117.33(15) . . ?
C11 C10 C9 120.69(19) . . ?
C11 C10 H4 119.7 . . ?
C9 C10 H4 119.7 . . ?
C5 N1 C8 108.89(14) . . ?
C5 N1 H5 125.6 . . ?
C8 N1 H5 125.6 . . ?
C15 N2 C18 108.71(14) . . ?
C15 N2 H6 125.6 . . ?
C18 N2 H6 125.6 . . ?
C10 C11 C12 120.29(17) . . ?
C10 C11 H7 119.9 . . ?
C12 C11 H7 119.9 . . ?
C13 C12 C11 120.38(18) . . ?
C13 C12 H8 119.8 . . ?
C11 C12 H8 119.8 . . ?
C12 C13 C14 120.61(19) . . ?
C12 C13 H9 119.7 . . ?
C14 C13 H9 119.7 . . ?
C13 C14 C9 118.92(16) . . ?
C13 C14 C15 123.10(17) . . ?
C9 C14 C15 117.94(15) . . ?
N2 C15 C16 109.14(14) . . ?
N2 C15 C14 126.96(16) . . ?
C16 C15 C14 123.79(16) . . ?
C15 C16 C17 106.22(14) . . ?
C15 C16 C7 116.96(14) . . ?
C17 C16 C7 136.57(15) . . ?
C18 C17 C16 106.45(14) . . ?
C18 C17 C26 116.99(14) . . ?
C16 C17 C26 136.44(15) . . ?
N2 C18 C17 109.01(14) . . ?
N2 C18 C19 126.64(15) . . ?
C17 C18 C19 124.31(15) . . ?
C20 C19 C24 118.72(15) . . ?
C20 C19 C18 123.57(15) . . ?
C24 C19 C18 117.70(15) . . ?
C21 C20 C19 120.34(16) . . ?
C21 C20 H10 119.8 . . ?
C19 C20 H10 119.8 . . ?
C20 C21 C22 120.81(16) . . ?
C20 C21 H11 119.6 . . ?
C22 C21 H11 119.6 . . ?
C23 C22 C21 120.07(16) . . ?
C23 C22 H12 120.0 . . ?
C21 C22 H12 120.0 . . ?
C22 C23 C24 120.62(16) . . ?
C22 C23 H13 119.7 . . ?
C24 C23 H13 119.7 . . ?
C23 C24 C19 119.43(15) . . ?
C23 C24 C25 123.04(15) . . ?
C19 C24 C25 117.35(15) . . ?
N3 C25 C26 109.77(14) . . ?
N3 C25 C24 125.51(15) . . ?
C26 C25 C24 124.30(15) . . ?
C25 C26 C17 118.15(14) . . ?
C25 C26 C27 106.09(13) . . ?
C17 C26 C27 135.28(15) . . ?
C32 C27 C28 118.77(15) . . ?
C32 C27 C26 134.49(15) . . ?
C28 C27 C26 106.46(14) . . ?
N3 C28 C29 129.23(15) . . ?
N3 C28 C27 108.87(14) . . ?
C29 C28 C27 121.89(15) . . ?
C30 C29 C28 118.25(16) . . ?
C30 C29 H14 120.9 . . ?
C28 C29 H14 120.9 . . ?
C29 C30 C31 119.74(16) . . ?
C29 C30 H15 120.1 . . ?
C31 C30 H15 120.1 . . ?
C32 C31 C30 122.92(16) . . ?
C32 C31 Cl2 118.59(13) . . ?
C30 C31 Cl2 118.48(13) . . ?
C31 C32 C27 117.93(15) . . ?
C31 C32 H16 121.0 . . ?
C27 C32 H16 121.0 . . ?
C28 N3 C25 108.47(13) . . ?
C28 N3 H17 125.8 . . ?
C25 N3 H17 125.8 . . ?
C34 O1 C37 105.5(13) . . ?
C35 C34 O1 109.7(11) . . ?
C35 C34 H18 109.7 . . ?
O1 C34 H18 109.7 . . ?
C35 C34 H19 109.7 . . ?
O1 C34 H19 109.7 . . ?
H18 C34 H19 108.2 . . ?
C34 C35 C36 109.9(7) . . ?
C34 C35 H20 109.7 . . ?
C36 C35 H20 109.7 . . ?
C34 C35 H21 109.7 . . ?
C36 C35 H21 109.7 . . ?
H20 C35 H21 108.2 . . ?
C37 C36 C35 98.6(9) . . ?
C37 C36 H22 112.1 . . ?
C35 C36 H22 112.1 . . ?
C37 C36 H23 112.1 . . ?
C35 C36 H23 112.1 . . ?
H22 C36 H23 109.7 . . ?
C36 C37 O1 104.9(11) . . ?
C36 C37 H24 110.8 . . ?
O1 C37 H24 110.8 . . ?
C36 C37 H25 110.8 . . ?
O1 C37 H25 110.8 . . ?
H24 C37 H25 108.8 . . ?
C52 O4 C49 106.8(13) . . ?
C51 C50 C49 104.5(7) . . ?
C51 C50 H26 110.9 . . ?
C49 C50 H26 110.9 . . ?
C51 C50 H27 110.9 . . ?
C49 C50 H27 110.9 . . ?
H26 C50 H27 108.9 . . ?
O4 C49 C50 115.0(9) . . ?
O4 C49 H28 108.5 . . ?
C50 C49 H28 108.5 . . ?
O4 C49 H29 108.5 . . ?
C50 C49 H29 108.5 . . ?
H28 C49 H29 107.5 . . ?
C50 C51 C52 105.9(9) . . ?
C50 C51 H30 110.6 . . ?
C52 C51 H30 110.6 . . ?
C50 C51 H31 110.6 . . ?
C52 C51 H31 110.6 . . ?
H30 C51 H31 108.7 . . ?
O4 C52 C51 107.7(10) . . ?
O4 C52 H32 110.2 . . ?
C51 C52 H32 110.2 . . ?
O4 C52 H33 110.2 . . ?
C51 C52 H33 110.2 . . ?
H32 C52 H33 108.5 . . ?
C38 O2 C40 107.6(8) . . ?
O2 C38 C42 106.3(6) . . ?
O2 C38 H34 110.5 . . ?
C42 C38 H34 110.5 . . ?
O2 C38 H35 110.5 . . ?
C42 C38 H35 110.5 . . ?
H34 C38 H35 108.7 . . ?
C41 C40 O2 108.5(7) . . ?
C41 C40 H36 110.0 . . ?
O2 C40 H36 110.0 . . ?
C41 C40 H37 110.0 . . ?
O2 C40 H37 110.0 . . ?
H36 C40 H37 108.4 . . ?
C40 C41 C42 101.5(4) . . ?
C40 C41 H38 111.5 . . ?
C42 C41 H38 111.5 . . ?
C40 C41 H39 111.5 . . ?
C42 C41 H39 111.5 . . ?
H38 C41 H39 109.3 . . ?
C38 C42 C41 100.5(4) . . ?
C38 C42 H40 111.7 . . ?
C41 C42 H40 111.7 . . ?
C38 C42 H41 111.7 . . ?
C41 C42 H41 111.7 . . ?
H40 C42 H41 109.4 . . ?
C56 O5 C53 115(3) . . ?
C53 C54 C55 98.8(13) . . ?
C53 C54 H42 112.0 . . ?
C55 C54 H42 112.0 . . ?
C53 C54 H43 112.0 . . ?
C55 C54 H43 112.0 . . ?
H42 C54 H43 109.7 . . ?
O5 C56 C55 106.2(19) . . ?
O5 C56 H44 110.5 . . ?
C55 C56 H44 110.5 . . ?
O5 C56 H45 110.5 . . ?
C55 C56 H45 110.5 . . ?
H44 C56 H45 108.7 . . ?
O5 C53 C54 102(2) . . ?
O5 C53 H46 111.4 . . ?
C54 C53 H46 111.4 . . ?
O5 C53 H47 111.4 . . ?
C54 C53 H47 111.4 . . ?
H46 C53 H47 109.3 . . ?
C56 C55 C54 103.8(12) . . ?
C56 C55 H48 111.0 . . ?
C54 C55 H48 111.0 . . ?
C56 C55 H49 111.0 . . ?
C54 C55 H49 111.0 . . ?
H48 C55 H49 109.0 . . ?
C48 O3 C45 108.7(9) . . ?
O3 C45 C46 105.0(9) . . ?
O3 C45 H50 110.7 . . ?
C46 C45 H50 110.7 . . ?
O3 C45 H51 110.7 . . ?
C46 C45 H51 110.7 . . ?
H50 C45 H51 108.8 . . ?
C47 C46 C45 102.2(8) . . ?
C47 C46 H52 111.3 . . ?
C45 C46 H52 111.3 . . ?
C47 C46 H53 111.3 . . ?
C45 C46 H53 111.3 . . ?
H52 C46 H53 109.2 . . ?
C48 C47 C46 101.6(9) . . ?
C48 C47 H54 111.5 . . ?
C46 C47 H54 111.5 . . ?
C48 C47 H55 111.5 . . ?
C46 C47 H55 111.5 . . ?
H54 C47 H55 109.3 . . ?
O3 C48 C47 108.7(7) . . ?
O3 C48 H56 110.0 . . ?
C47 C48 H56 110.0 . . ?
O3 C48 H57 110.0 . . ?
C47 C48 H57 110.0 . . ?
H56 C48 H57 108.3 . . ?
C57 O6 C60 106.2(13) . . ?
C61 C59 C57 103.9(10) . . ?
C61 C59 H58 111.0 . . ?
C57 C59 H58 111.0 . . ?
C61 C59 H59 111.0 . . ?
C57 C59 H59 111.0 . . ?
H58 C59 H59 109.0 . . ?
O6 C57 C59 103.8(15) . . ?
O6 C57 H60 111.0 . . ?
C59 C57 H60 111.0 . . ?
O6 C57 H61 111.0 . . ?
C59 C57 H61 111.0 . . ?
H60 C57 H61 109.0 . . ?
O6 C60 C61 104.4(9) . . ?
O6 C60 H62 110.9 . . ?
C61 C60 H62 110.9 . . ?
O6 C60 H63 110.9 . . ?
C61 C60 H63 110.9 . . ?
H62 C60 H63 108.9 . . ?
C59 C61 C60 105.8(11) . . ?
C59 C61 H64 110.6 . . ?
C60 C61 H64 110.6 . . ?
C59 C61 H65 110.6 . . ?
C60 C61 H65 110.6 . . ?
H64 C61 H65 108.7 . . ?

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
C6 C1 C2 C3 -1.3(3) . . . . ?
C6 C1 C2 Cl1 179.91(12) . . . . ?
C1 C2 C3 C4 -2.8(3) . . . . ?
Cl1 C2 C3 C4 175.95(13) . . . . ?
C2 C3 C4 C5 2.3(3) . . . . ?
C3 C4 C5 N1 -176.97(16) . . . . ?
C3 C4 C5 C6 2.2(2) . . . . ?
C2 C1 C6 C5 5.7(2) . . . . ?
C2 C1 C6 C7 -179.84(17) . . . . ?
N1 C5 C6 C1 173.02(14) . . . . ?
C4 C5 C6 C1 -6.3(2) . . . . ?
N1 C5 C6 C7 -2.83(17) . . . . ?
C4 C5 C6 C7 177.86(15) . . . . ?
C1 C6 C7 C8 -170.37(17) . . . . ?
C5 C6 C7 C8 4.57(17) . . . . ?
C1 C6 C7 C16 4.0(3) . . . . ?
C5 C6 C7 C16 178.89(17) . . . . ?
C6 C7 C8 N1 -4.71(17) . . . . ?
C16 C7 C8 N1 179.84(13) . . . . ?
C6 C7 C8 C9 172.44(14) . . . . ?
C16 C7 C8 C9 -3.0(2) . . . . ?
N1 C8 C9 C10 -7.6(3) . . . . ?
C7 C8 C9 C10 175.76(15) . . . . ?
N1 C8 C9 C14 170.80(15) . . . . ?
C7 C8 C9 C14 -5.9(2) . . . . ?
C14 C9 C10 C11 0.0(2) . . . . ?
C8 C9 C10 C11 178.38(16) . . . . ?
C4 C5 N1 C8 179.19(16) . . . . ?
C6 C5 N1 C8 -0.05(18) . . . . ?
C7 C8 N1 C5 3.04(18) . . . . ?
C9 C8 N1 C5 -174.03(15) . . . . ?
C9 C10 C11 C12 -0.9(3) . . . . ?
C10 C11 C12 C13 0.9(3) . . . . ?
C11 C12 C13 C14 0.0(3) . . . . ?
C12 C13 C14 C9 -0.8(2) . . . . ?
C12 C13 C14 C15 176.75(16) . . . . ?
C10 C9 C14 C13 0.8(2) . . . . ?
C8 C9 C14 C13 -177.65(14) . . . . ?
C10 C9 C14 C15 -176.87(14) . . . . ?
C8 C9 C14 C15 4.7(2) . . . . ?
C18 N2 C15 C16 2.32(17) . . . . ?
C18 N2 C15 C14 -173.92(15) . . . . ?
C13 C14 C15 N2 3.6(3) . . . . ?
C9 C14 C15 N2 -178.81(15) . . . . ?
C13 C14 C15 C16 -172.11(15) . . . . ?
C9 C14 C15 C16 5.5(2) . . . . ?
N2 C15 C16 C17 -5.77(17) . . . . ?
C14 C15 C16 C17 170.61(14) . . . . ?
N2 C15 C16 C7 169.38(13) . . . . ?
C14 C15 C16 C7 -14.2(2) . . . . ?
C8 C7 C16 C15 12.6(2) . . . . ?
C6 C7 C16 C15 -161.21(17) . . . . ?
C8 C7 C16 C17 -174.18(17) . . . . ?
C6 C7 C16 C17 12.0(3) . . . . ?
C15 C16 C17 C18 6.96(17) . . . . ?
C7 C16 C17 C18 -166.76(18) . . . . ?
C15 C16 C17 C26 -168.78(17) . . . . ?
C7 C16 C17 C26 17.5(3) . . . . ?
C15 N2 C18 C17 2.23(17) . . . . ?
C15 N2 C18 C19 -175.39(14) . . . . ?
C16 C17 C18 N2 -5.73(17) . . . . ?
C26 C17 C18 N2 170.97(13) . . . . ?
C16 C17 C18 C19 171.96(14) . . . . ?
C26 C17 C18 C19 -11.3(2) . . . . ?
N2 C18 C19 C20 0.5(2) . . . . ?
C17 C18 C19 C20 -176.80(15) . . . . ?
N2 C18 C19 C24 -179.73(14) . . . . ?
C17 C18 C19 C24 3.0(2) . . . . ?
C24 C19 C20 C21 0.9(2) . . . . ?
C18 C19 C20 C21 -179.30(15) . . . . ?
C19 C20 C21 C22 -0.3(2) . . . . ?
C20 C21 C22 C23 -0.4(3) . . . . ?
C21 C22 C23 C24 0.5(3) . . . . ?
C22 C23 C24 C19 0.1(2) . . . . ?
C22 C23 C24 C25 175.17(15) . . . . ?
C20 C19 C24 C23 -0.8(2) . . . . ?
C18 C19 C24 C23 179.40(14) . . . . ?
C20 C19 C24 C25 -176.13(14) . . . . ?
C18 C19 C24 C25 4.1(2) . . . . ?
C23 C24 C25 N3 -6.0(2) . . . . ?
C19 C24 C25 N3 169.17(14) . . . . ?
C23 C24 C25 C26 -177.71(15) . . . . ?
C19 C24 C25 C26 -2.6(2) . . . . ?
N3 C25 C26 C17 -178.74(13) . . . . ?
C24 C25 C26 C17 -5.9(2) . . . . ?
N3 C25 C26 C27 -5.46(17) . . . . ?
C24 C25 C26 C27 167.40(14) . . . . ?
C18 C17 C26 C25 12.3(2) . . . . ?
C16 C17 C26 C25 -172.27(17) . . . . ?
C18 C17 C26 C27 -158.47(17) . . . . ?
C16 C17 C26 C27 16.9(3) . . . . ?
C25 C26 C27 C32 -167.70(17) . . . . ?
C17 C26 C27 C32 3.9(3) . . . . ?
C25 C26 C27 C28 5.84(17) . . . . ?
C17 C26 C27 C28 177.40(17) . . . . ?
C32 C27 C28 N3 170.53(14) . . . . ?
C26 C27 C28 N3 -4.21(17) . . . . ?
C32 C27 C28 C29 -8.3(2) . . . . ?
C26 C27 C28 C29 177.00(15) . . . . ?
N3 C28 C29 C30 -173.36(16) . . . . ?
C27 C28 C29 C30 5.2(2) . . . . ?
C28 C29 C30 C31 1.0(3) . . . . ?
C29 C30 C31 C32 -4.2(3) . . . . ?
C29 C30 C31 Cl2 175.54(14) . . . . ?
C30 C31 C32 C27 1.1(3) . . . . ?
Cl2 C31 C32 C27 -178.68(12) . . . . ?
C28 C27 C32 C31 5.0(2) . . . . ?
C26 C27 C32 C31 177.88(17) . . . . ?
C29 C28 N3 C25 179.58(16) . . . . ?
C27 C28 N3 C25 0.90(17) . . . . ?
C26 C25 N3 C28 2.94(17) . . . . ?
C24 C25 N3 C28 -169.81(15) . . . . ?
C37 O1 C34 C35 -17.3(18) . . . . ?
O1 C34 C35 C36 -3.3(13) . . . . ?
C34 C35 C36 C37 23.1(10) . . . . ?
C35 C36 C37 O1 -31.6(12) . . . . ?
C34 O1 C37 C36 32.8(18) . . . . ?
C52 O4 C49 C50 5.0(13) . . . . ?
C51 C50 C49 O4 -4.3(12) . . . . ?
C49 C50 C51 C52 1.9(10) . . . . ?
C49 O4 C52 C51 -3.3(13) . . . . ?
C50 C51 C52 O4 0.8(13) . . . . ?
C40 O2 C38 C42 -12.6(8) . . . . ?
C38 O2 C40 C41 -13.6(10) . . . . ?
O2 C40 C41 C42 32.9(9) . . . . ?
O2 C38 C42 C41 31.5(6) . . . . ?
C40 C41 C42 C38 -38.5(7) . . . . ?
C53 O5 C56 C55 12(3) . . . . ?
C56 O5 C53 C54 12(3) . . . . ?
C55 C54 C53 O5 -29(2) . . . . ?
O5 C56 C55 C54 -31(2) . . . . ?
C53 C54 C55 C56 37(2) . . . . ?
C48 O3 C45 C46 16.3(9) . . . . ?
O3 C45 C46 C47 -32.9(9) . . . . ?
C45 C46 C47 C48 36.1(10) . . . . ?
C45 O3 C48 C47 7.4(10) . . . . ?
C46 C47 C48 O3 -27.8(10) . . . . ?
C60 O6 C57 C59 40.8(13) . . . . ?
C61 C59 C57 O6 -34.5(14) . . . . ?
C57 O6 C60 C61 -31.0(13) . . . . ?
C57 C59 C61 C60 15.1(13) . . . . ?
O6 C60 C61 C59 8.3(11) . . . . ?

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
N1 H5 O1 0.88 2.05 2.91(2) 165.8 .
N1 H5 O4 0.88 2.01 2.89(2) 175.2 .
N2 H6 O2 0.88 2.11 2.921(10) 153.1 .
N2 H6 O5 0.88 2.08 2.87(3) 148.8 .
C29 H14 Cl1 0.95 2.82 3.6583(17) 147.2 2_656
N3 H17 O3 0.88 2.04 2.910(11) 171.1 .
N3 H17 O6 0.88 1.99 2.842(17) 162.5 .
C48 H56 Cl1 0.99 2.80 3.453(4) 123.8 2_656
N1 H5 O1 0.88 2.05 2.91(2) 165.8 .
N1 H5 O4 0.88 2.01 2.89(2) 175.2 .

_refine_diff_density_max         0.456
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.136

