# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# 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_aeh75
_database_code_depnum_ccdc_archive 'CCDC 1823109'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H31 N O5'
_chemical_formula_weight         533.60

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   10.3357(5)
_cell_length_b                   23.6593(11)
_cell_length_c                   11.6006(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.704(2)
_cell_angle_gamma                90.00
_cell_volume                     2743.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9628
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      29.63

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8388
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'high brilliance microfocus sealed tube'
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'omega + phi scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            102868
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         29.67
_reflns_number_total             7754
_reflns_number_gt                6323
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2013.2 (Bruker AXS Inc.)'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2011)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2011)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0499P)²+1.6390P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7754
_refine_ls_number_parameters     365
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1145
_refine_ls_wR_factor_gt          0.1065
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.20264(9) 0.26709(4) 0.54984(8) 0.01308(18) Uani 1 1 d . . .
O2 O 0.06573(9) 0.35750(4) 0.70591(8) 0.01752(19) Uani 1 1 d . . .
O3 O 0.25735(9) 0.30914(4) 0.77351(8) 0.01522(19) Uani 1 1 d . . .
O4 O 0.07126(9) 0.39176(4) 0.41307(9) 0.0199(2) Uani 1 1 d . . .
O5 O -0.03796(9) 0.31522(4) 0.45340(9) 0.0197(2) Uani 1 1 d . . .
N1 N 0.35428(10) 0.31239(4) 0.46916(9) 0.0111(2) Uani 1 1 d . . .
C1 C 0.28070(12) 0.25902(5) 0.46560(11) 0.0111(2) Uani 1 1 d . . .
H1 H 0.2204 0.2532 0.3842 0.013 Uiso 1 1 calc R . .
C2 C 0.31957(11) 0.34991(5) 0.55079(10) 0.0100(2) Uani 1 1 d . . .
C3 C 0.18794(11) 0.32639(5) 0.56574(11) 0.0108(2) Uani 1 1 d . . .
C4 C 0.16194(12) 0.33367(5) 0.68952(11) 0.0114(2) Uani 1 1 d . . .
C5 C 0.23930(15) 0.31437(6) 0.89314(12) 0.0211(3) Uani 1 1 d . . .
H5A H 0.2395 0.3544 0.9146 0.032 Uiso 1 1 calc R . .
H5B H 0.3125 0.2949 0.9495 0.032 Uiso 1 1 calc R . .
H5C H 0.1538 0.2973 0.8960 0.032 Uiso 1 1 calc R . .
C6 C 0.06741(12) 0.34940(5) 0.46881(11) 0.0126(2) Uani 1 1 d . . .
C7 C -0.15688(14) 0.33375(7) 0.36461(13) 0.0250(3) Uani 1 1 d . . .
H7A H -0.1821 0.3717 0.3850 0.038 Uiso 1 1 calc R . .
H7B H -0.2305 0.3074 0.3631 0.038 Uiso 1 1 calc R . .
H7C H -0.1381 0.3346 0.2860 0.038 Uiso 1 1 calc R . .
C11 C 0.36761(12) 0.20759(5) 0.50235(11) 0.0113(2) Uani 1 1 d . . .
C12 C 0.34447(13) 0.15905(5) 0.43324(11) 0.0142(2) Uani 1 1 d . . .
H12 H 0.2727 0.1581 0.3633 0.017 Uiso 1 1 calc R . .
C13 C 0.42566(14) 0.11168(5) 0.46558(12) 0.0169(3) Uani 1 1 d . . .
H13 H 0.4088 0.0787 0.4173 0.020 Uiso 1 1 calc R . .
C14 C 0.53077(13) 0.11197(5) 0.56740(12) 0.0161(2) Uani 1 1 d . . .
C15 C 0.55331(13) 0.16109(6) 0.63673(12) 0.0176(3) Uani 1 1 d . . .
H15 H 0.6251 0.1621 0.7066 0.021 Uiso 1 1 calc R . .
C16 C 0.47267(13) 0.20828(5) 0.60524(11) 0.0152(2) Uani 1 1 d . . .
H16 H 0.4889 0.2412 0.6538 0.018 Uiso 1 1 calc R . .
C17 C 0.61828(15) 0.06073(6) 0.60346(15) 0.0259(3) Uani 1 1 d . . .
H17A H 0.5853 0.0385 0.6614 0.039 Uiso 1 1 calc R . .
H17B H 0.7104 0.0728 0.6395 0.039 Uiso 1 1 calc R . .
H17C H 0.6161 0.0376 0.5330 0.039 Uiso 1 1 calc R . .
C21 C 0.40672(11) 0.32681(5) 0.37178(10) 0.0107(2) Uani 1 1 d . . .
C22 C 0.43156(12) 0.28419(5) 0.29626(11) 0.0133(2) Uani 1 1 d . . .
H22 H 0.4120 0.2460 0.3103 0.016 Uiso 1 1 calc R . .
C23 C 0.48463(12) 0.29748(5) 0.20102(11) 0.0142(2) Uani 1 1 d . . .
H23 H 0.4992 0.2681 0.1500 0.017 Uiso 1 1 calc R . .
C24 C 0.51707(12) 0.35270(5) 0.17834(11) 0.0131(2) Uani 1 1 d . . .
C25 C 0.48922(13) 0.39494(5) 0.25246(11) 0.0143(2) Uani 1 1 d . . .
H25 H 0.5083 0.4332 0.2377 0.017 Uiso 1 1 calc R . .
C26 C 0.43430(12) 0.38268(5) 0.34728(11) 0.0128(2) Uani 1 1 d . . .
H26 H 0.4155 0.4124 0.3956 0.015 Uiso 1 1 calc R . .
C27 C 0.58284(14) 0.36600(6) 0.07965(12) 0.0178(3) Uani 1 1 d . . .
H27A H 0.6798 0.3610 0.1087 0.027 Uiso 1 1 calc R . .
H27B H 0.5632 0.4052 0.0537 0.027 Uiso 1 1 calc R . .
H27C H 0.5483 0.3405 0.0124 0.027 Uiso 1 1 calc R . .
C30 C 0.39160(11) 0.39297(5) 0.61180(10) 0.0101(2) Uani 1 1 d . . .
C31 C 0.53414(11) 0.40426(5) 0.61585(10) 0.0107(2) Uani 1 1 d . . .
C32 C 0.62500(12) 0.36070(5) 0.61390(11) 0.0133(2) Uani 1 1 d . . .
H32 H 0.5948 0.3226 0.6061 0.016 Uiso 1 1 calc R . .
C33 C 0.75899(12) 0.37254(6) 0.62321(11) 0.0158(2) Uani 1 1 d . . .
H33 H 0.8199 0.3424 0.6233 0.019 Uiso 1 1 calc R . .
C34 C 0.80458(13) 0.42796(6) 0.63238(12) 0.0175(3) Uani 1 1 d . . .
H34 H 0.8961 0.4359 0.6383 0.021 Uiso 1 1 calc R . .
C35 C 0.71495(13) 0.47173(6) 0.63277(12) 0.0162(2) Uani 1 1 d . . .
H35 H 0.7450 0.5098 0.6377 0.019 Uiso 1 1 calc R . .
C36 C 0.58135(12) 0.45996(5) 0.62598(11) 0.0133(2) Uani 1 1 d . . .
H36 H 0.5214 0.4901 0.6283 0.016 Uiso 1 1 calc R . .
C41 C 0.33046(12) 0.43212(5) 0.68452(11) 0.0114(2) Uani 1 1 d . . .
C42 C 0.21971(12) 0.46568(5) 0.63394(12) 0.0148(2) Uani 1 1 d . . .
H42 H 0.1801 0.4636 0.5507 0.018 Uiso 1 1 calc R . .
C43 C 0.16646(13) 0.50223(5) 0.70442(13) 0.0188(3) Uani 1 1 d . . .
H43 H 0.0911 0.5250 0.6689 0.023 Uiso 1 1 calc R . .
C44 C 0.22319(14) 0.50540(6) 0.82599(13) 0.0213(3) Uani 1 1 d . . .
H44 H 0.1859 0.5298 0.8742 0.026 Uiso 1 1 calc R . .
C45 C 0.33494(14) 0.47275(6) 0.87719(12) 0.0206(3) Uani 1 1 d . . .
H45 H 0.3745 0.4751 0.9604 0.025 Uiso 1 1 calc R . .
C46 C 0.38874(13) 0.43679(5) 0.80693(11) 0.0156(2) Uani 1 1 d . . .
H46 H 0.4660 0.4151 0.8424 0.019 Uiso 1 1 calc R . .


_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 C3 1.4283(14) . ?
O1 C1 1.4292(14) . ?
O2 C4 1.1995(15) . ?
O3 C4 1.3307(15) . ?
O3 C5 1.4517(16) . ?
O4 C6 1.1989(15) . ?
O5 C6 1.3316(15) . ?
O5 C7 1.4564(16) . ?
N1 C2 1.4093(15) . ?
N1 C21 1.4131(15) . ?
N1 C1 1.4693(15) . ?
C1 C11 1.5082(16) . ?
C1 H1 1.0000 . ?
C2 C30 1.3511(17) . ?
C2 C3 1.5201(16) . ?
C3 C4 1.5360(16) . ?
C3 C6 1.5497(16) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 C12 1.3862(17) . ?
C11 C16 1.3950(17) . ?
C12 C13 1.3933(18) . ?
C12 H12 0.9500 . ?
C13 C14 1.3871(19) . ?
C13 H13 0.9500 . ?
C14 C15 1.3990(19) . ?
C14 C17 1.5069(18) . ?
C15 C16 1.3856(18) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 C26 1.3966(17) . ?
C21 C22 1.4016(16) . ?
C22 C23 1.3886(17) . ?
C22 H22 0.9500 . ?
C23 C24 1.3905(17) . ?
C23 H23 0.9500 . ?
C24 C25 1.3951(17) . ?
C24 C27 1.5055(17) . ?
C25 C26 1.3904(17) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C30 C31 1.4862(16) . ?
C30 C41 1.4965(16) . ?
C31 C32 1.3984(16) . ?
C31 C36 1.3998(17) . ?
C32 C33 1.3899(17) . ?
C32 H32 0.9500 . ?
C33 C34 1.3884(19) . ?
C33 H33 0.9500 . ?
C34 C35 1.3902(18) . ?
C34 H34 0.9500 . ?
C35 C36 1.3911(17) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.3944(17) . ?
C41 C46 1.3990(17) . ?
C42 C43 1.3955(18) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.391(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.3883(18) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?

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
C3 O1 C1 108.46(9) . . ?
C4 O3 C5 114.31(10) . . ?
C6 O5 C7 115.26(11) . . ?
C2 N1 C21 126.85(10) . . ?
C2 N1 C1 110.00(9) . . ?
C21 N1 C1 119.07(10) . . ?
O1 C1 N1 104.12(9) . . ?
O1 C1 C11 108.27(9) . . ?
N1 C1 C11 114.74(10) . . ?
O1 C1 H1 109.8 . . ?
N1 C1 H1 109.8 . . ?
C11 C1 H1 109.8 . . ?
C30 C2 N1 128.79(11) . . ?
C30 C2 C3 127.33(10) . . ?
N1 C2 C3 103.53(9) . . ?
O1 C3 C2 102.54(9) . . ?
O1 C3 C4 106.29(9) . . ?
C2 C3 C4 116.08(10) . . ?
O1 C3 C6 110.10(9) . . ?
C2 C3 C6 111.50(10) . . ?
C4 C3 C6 109.86(9) . . ?
O2 C4 O3 125.37(11) . . ?
O2 C4 C3 123.35(11) . . ?
O3 C4 C3 111.26(10) . . ?
O3 C5 H5A 109.5 . . ?
O3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O4 C6 O5 124.98(11) . . ?
O4 C6 C3 123.67(11) . . ?
O5 C6 C3 111.32(10) . . ?
O5 C7 H7A 109.5 . . ?
O5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C12 C11 C16 119.15(11) . . ?
C12 C11 C1 120.12(11) . . ?
C16 C11 C1 120.72(11) . . ?
C11 C12 C13 120.46(12) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 120.89(12) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 118.28(12) . . ?
C13 C14 C17 121.18(12) . . ?
C15 C14 C17 120.54(12) . . ?
C16 C15 C14 121.10(12) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C11 120.11(12) . . ?
C15 C16 H16 119.9 . . ?
C11 C16 H16 119.9 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C26 C21 C22 118.33(11) . . ?
C26 C21 N1 122.05(11) . . ?
C22 C21 N1 119.62(11) . . ?
C23 C22 C21 120.43(11) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 121.75(11) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 H23 119.1 . . ?
C23 C24 C25 117.33(11) . . ?
C23 C24 C27 121.15(11) . . ?
C25 C24 C27 121.51(11) . . ?
C26 C25 C24 121.85(11) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C25 C26 C21 120.25(11) . . ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C2 C30 C31 124.20(11) . . ?
C2 C30 C41 120.44(10) . . ?
C31 C30 C41 115.33(10) . . ?
C32 C31 C36 118.29(11) . . ?
C32 C31 C30 122.10(11) . . ?
C36 C31 C30 119.58(10) . . ?
C33 C32 C31 120.68(11) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 120.55(12) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C33 C34 C35 119.36(12) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C36 120.23(12) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 120.87(11) . . ?
C35 C36 H36 119.6 . . ?
C31 C36 H36 119.6 . . ?
C42 C41 C46 118.56(11) . . ?
C42 C41 C30 122.29(11) . . ?
C46 C41 C30 119.11(11) . . ?
C41 C42 C43 120.67(12) . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
C44 C43 C42 120.14(12) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 119.71(12) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C46 C45 C44 120.16(13) . . ?
C46 C45 H45 119.9 . . ?
C44 C45 H45 119.9 . . ?
C45 C46 C41 120.73(12) . . ?
C45 C46 H46 119.6 . . ?
C41 C46 H46 119.6 . . ?

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
C3 O1 C1 N1 21.84(11) . . . . ?
C3 O1 C1 C11 144.36(10) . . . . ?
C2 N1 C1 O1 -0.55(12) . . . . ?
C21 N1 C1 O1 -159.39(10) . . . . ?
C2 N1 C1 C11 -118.71(11) . . . . ?
C21 N1 C1 C11 82.45(13) . . . . ?
C21 N1 C2 C30 -48.75(19) . . . . ?
C1 N1 C2 C30 154.48(12) . . . . ?
C21 N1 C2 C3 137.68(11) . . . . ?
C1 N1 C2 C3 -19.09(12) . . . . ?
C1 O1 C3 C2 -33.19(11) . . . . ?
C1 O1 C3 C4 -155.48(9) . . . . ?
C1 O1 C3 C6 85.58(11) . . . . ?
C30 C2 C3 O1 -142.29(12) . . . . ?
N1 C2 C3 O1 31.40(11) . . . . ?
C30 C2 C3 C4 -26.90(17) . . . . ?
N1 C2 C3 C4 146.80(10) . . . . ?
C30 C2 C3 C6 99.93(14) . . . . ?
N1 C2 C3 C6 -86.37(11) . . . . ?
C5 O3 C4 O2 -1.59(18) . . . . ?
C5 O3 C4 C3 179.98(10) . . . . ?
O1 C3 C4 O2 -123.94(12) . . . . ?
C2 C3 C4 O2 122.80(13) . . . . ?
C6 C3 C4 O2 -4.84(16) . . . . ?
O1 C3 C4 O3 54.54(12) . . . . ?
C2 C3 C4 O3 -58.73(13) . . . . ?
C6 C3 C4 O3 173.63(10) . . . . ?
C7 O5 C6 O4 -2.69(19) . . . . ?
C7 O5 C6 C3 179.38(11) . . . . ?
O1 C3 C6 O4 -133.89(12) . . . . ?
C2 C3 C6 O4 -20.77(16) . . . . ?
C4 C3 C6 O4 109.37(13) . . . . ?
O1 C3 C6 O5 44.07(13) . . . . ?
C2 C3 C6 O5 157.19(10) . . . . ?
C4 C3 C6 O5 -72.66(12) . . . . ?
O1 C1 C11 C12 111.75(12) . . . . ?
N1 C1 C11 C12 -132.46(12) . . . . ?
O1 C1 C11 C16 -68.82(14) . . . . ?
N1 C1 C11 C16 46.96(15) . . . . ?
C16 C11 C12 C13 -0.47(18) . . . . ?
C1 C11 C12 C13 178.97(11) . . . . ?
C11 C12 C13 C14 0.2(2) . . . . ?
C12 C13 C14 C15 -0.09(19) . . . . ?
C12 C13 C14 C17 179.50(13) . . . . ?
C13 C14 C15 C16 0.29(19) . . . . ?
C17 C14 C15 C16 -179.30(13) . . . . ?
C14 C15 C16 C11 -0.58(19) . . . . ?
C12 C11 C16 C15 0.67(18) . . . . ?
C1 C11 C16 C15 -178.77(11) . . . . ?
C2 N1 C21 C26 1.88(18) . . . . ?
C1 N1 C21 C26 156.79(11) . . . . ?
C2 N1 C21 C22 -177.73(11) . . . . ?
C1 N1 C21 C22 -22.82(16) . . . . ?
C26 C21 C22 C23 1.19(18) . . . . ?
N1 C21 C22 C23 -179.19(11) . . . . ?
C21 C22 C23 C24 1.17(19) . . . . ?
C22 C23 C24 C25 -2.51(18) . . . . ?
C22 C23 C24 C27 175.96(12) . . . . ?
C23 C24 C25 C26 1.55(18) . . . . ?
C27 C24 C25 C26 -176.91(12) . . . . ?
C24 C25 C26 C21 0.75(19) . . . . ?
C22 C21 C26 C25 -2.12(18) . . . . ?
N1 C21 C26 C25 178.27(11) . . . . ?
N1 C2 C30 C31 -8.8(2) . . . . ?
C3 C2 C30 C31 163.36(11) . . . . ?
N1 C2 C30 C41 173.19(11) . . . . ?
C3 C2 C30 C41 -14.68(18) . . . . ?
C2 C30 C31 C32 -34.15(18) . . . . ?
C41 C30 C31 C32 143.98(12) . . . . ?
C2 C30 C31 C36 148.05(12) . . . . ?
C41 C30 C31 C36 -33.82(15) . . . . ?
C36 C31 C32 C33 0.74(18) . . . . ?
C30 C31 C32 C33 -177.09(11) . . . . ?
C31 C32 C33 C34 -1.21(19) . . . . ?
C32 C33 C34 C35 0.3(2) . . . . ?
C33 C34 C35 C36 1.0(2) . . . . ?
C34 C35 C36 C31 -1.51(19) . . . . ?
C32 C31 C36 C35 0.61(18) . . . . ?
C30 C31 C36 C35 178.50(11) . . . . ?
C2 C30 C41 C42 -61.65(16) . . . . ?
C31 C30 C41 C42 120.14(12) . . . . ?
C2 C30 C41 C46 120.55(13) . . . . ?
C31 C30 C41 C46 -57.65(15) . . . . ?
C46 C41 C42 C43 -1.37(18) . . . . ?
C30 C41 C42 C43 -179.18(11) . . . . ?
C41 C42 C43 C44 -0.20(19) . . . . ?
C42 C43 C44 C45 1.2(2) . . . . ?
C43 C44 C45 C46 -0.5(2) . . . . ?
C44 C45 C46 C41 -1.1(2) . . . . ?
C42 C41 C46 C45 2.01(19) . . . . ?
C30 C41 C46 C45 179.88(12) . . . . ?

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
C33 H33 O2 0.95 2.50 3.0910(15) 120.1 1_655
C34 H34 O2 0.95 2.54 3.1022(16) 118.4 1_655
C42 H42 O4 0.95 2.41 3.1593(16) 135.9 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        29.67
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.057
####################################################################### 
# 
# 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_aeh165_0msp
_database_code_depnum_ccdc_archive 'CCDC 1823110'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H36 N2 O4'
_chemical_formula_weight         560.67

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   10.9629(5)
_cell_length_b                   9.8209(4)
_cell_length_c                   27.4846(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.3970(10)
_cell_angle_gamma                90.00
_cell_volume                     2958.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      72.19

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8136
_exptl_absorpt_correction_T_max  0.9085
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'high brilliance microfocus sealed tube'
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'omega + phi scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            49584
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         72.25
_reflns_number_total             5834
_reflns_number_gt                5375
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2013.2 (Bruker AXS Inc.)'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2011)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0521P)²+1.1158P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    Riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5834
_refine_ls_number_parameters     383
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0965
_refine_ls_wR_factor_gt          0.0937
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.63771(8) 0.39553(9) 0.09081(3) 0.01794(19) Uani 1 1 d . . .
N2 N 0.83562(8) 0.33639(9) 0.10623(3) 0.01724(19) Uani 1 1 d . . .
O1 O 0.62100(8) 0.10348(9) 0.06652(3) 0.02731(19) Uani 1 1 d . . .
O2 O 0.48017(7) 0.11354(8) 0.12467(3) 0.02041(17) Uani 1 1 d . . .
O3 O 0.73217(9) 0.59602(10) 0.15543(3) 0.0358(2) Uani 1 1 d . . .
O4 O 0.87608(8) 0.64538(9) 0.10061(4) 0.0316(2) Uani 1 1 d . . .
C1 C 0.76667(9) 0.26351(11) 0.13991(4) 0.0167(2) Uani 1 1 d . . .
C2 C 0.63243(9) 0.28543(11) 0.12599(4) 0.0166(2) Uani 1 1 d . . .
H2 H 0.5844 0.3125 0.1549 0.020 Uiso 1 1 calc R . .
C3 C 0.76086(9) 0.44601(11) 0.08653(4) 0.0168(2) Uani 1 1 d . . .
H3 H 0.7803 0.4648 0.0518 0.020 Uiso 1 1 calc R . .
C4 C 0.57864(10) 0.15727(11) 0.10157(4) 0.0179(2) Uani 1 1 d . . .
C5 C 0.43119(11) -0.01712(12) 0.10834(4) 0.0252(2) Uani 1 1 d . . .
H5A H 0.4942 -0.0889 0.1116 0.030 Uiso 1 1 calc R . .
H5B H 0.4038 -0.0117 0.0738 0.030 Uiso 1 1 calc R . .
C6 C 0.32514(12) -0.04874(15) 0.14023(5) 0.0333(3) Uani 1 1 d . . .
H6A H 0.3518 -0.0440 0.1745 0.050 Uiso 1 1 calc R . .
H6B H 0.2947 -0.1405 0.1329 0.050 Uiso 1 1 calc R . .
H6C H 0.2599 0.0177 0.1341 0.050 Uiso 1 1 calc R . .
C7 C 0.78464(10) 0.57247(11) 0.11873(4) 0.0219(2) Uani 1 1 d . . .
C8 C 0.92357(14) 0.75819(14) 0.12998(7) 0.0484(4) Uani 1 1 d . . .
H8A H 0.8615 0.7866 0.1535 0.058 Uiso 1 1 calc R . .
H8B H 0.9406 0.8367 0.1086 0.058 Uiso 1 1 calc R . .
C9 C 1.03717(12) 0.71799(15) 0.15677(5) 0.0352(3) Uani 1 1 d . . .
H9A H 1.0185 0.6470 0.1805 0.053 Uiso 1 1 calc R . .
H9B H 1.0716 0.7974 0.1738 0.053 Uiso 1 1 calc R . .
H9C H 1.0964 0.6830 0.1337 0.053 Uiso 1 1 calc R . .
C10 C 0.80982(10) 0.19446(11) 0.17901(4) 0.0184(2) Uani 1 1 d . . .
C11 C 0.53720(9) 0.47839(11) 0.07941(4) 0.0170(2) Uani 1 1 d . . .
C12 C 0.42014(10) 0.44543(11) 0.09463(4) 0.0193(2) Uani 1 1 d . . .
H12 H 0.4081 0.3677 0.1145 0.023 Uiso 1 1 calc R . .
C13 C 0.32112(10) 0.52644(12) 0.08066(4) 0.0209(2) Uani 1 1 d . . .
H13 H 0.2422 0.5030 0.0915 0.025 Uiso 1 1 calc R . .
C14 C 0.33425(10) 0.64083(11) 0.05131(4) 0.0202(2) Uani 1 1 d . . .
C15 C 0.45167(10) 0.67302(11) 0.03671(4) 0.0210(2) Uani 1 1 d . . .
H15 H 0.4634 0.7508 0.0168 0.025 Uiso 1 1 calc R . .
C16 C 0.55164(10) 0.59459(11) 0.05049(4) 0.0197(2) Uani 1 1 d . . .
H16 H 0.6307 0.6197 0.0403 0.024 Uiso 1 1 calc R . .
C17 C 0.22624(11) 0.72644(13) 0.03511(4) 0.0258(3) Uani 1 1 d . . .
H17A H 0.1525 0.6700 0.0342 0.039 Uiso 1 1 calc R . .
H17B H 0.2403 0.7631 0.0026 0.039 Uiso 1 1 calc R . .
H17C H 0.2158 0.8017 0.0580 0.039 Uiso 1 1 calc R . .
C21 C 0.93402(9) 0.28223(11) 0.07985(4) 0.0160(2) Uani 1 1 d . . .
C22 C 1.00958(10) 0.36967(11) 0.05449(4) 0.0193(2) Uani 1 1 d . . .
H22 H 0.9967 0.4653 0.0558 0.023 Uiso 1 1 calc R . .
C23 C 1.10385(10) 0.31704(12) 0.02726(4) 0.0209(2) Uani 1 1 d . . .
H23 H 1.1536 0.3778 0.0096 0.025 Uiso 1 1 calc R . .
C24 C 1.12736(10) 0.17820(12) 0.02518(4) 0.0205(2) Uani 1 1 d . . .
C25 C 1.05165(10) 0.09288(11) 0.05130(4) 0.0221(2) Uani 1 1 d . . .
H25 H 1.0658 -0.0025 0.0507 0.027 Uiso 1 1 calc R . .
C26 C 0.95614(10) 0.14296(11) 0.07827(4) 0.0198(2) Uani 1 1 d . . .
H26 H 0.9059 0.0821 0.0957 0.024 Uiso 1 1 calc R . .
C27 C 1.23195(11) 0.12347(13) -0.00375(5) 0.0287(3) Uani 1 1 d . . .
H27A H 1.2279 0.1615 -0.0367 0.043 Uiso 1 1 calc R . .
H27B H 1.2264 0.0240 -0.0055 0.043 Uiso 1 1 calc R . .
H27C H 1.3094 0.1494 0.0122 0.043 Uiso 1 1 calc R . .
C31 C 0.94063(10) 0.19011(12) 0.19483(4) 0.0193(2) Uani 1 1 d . . .
C32 C 1.01839(11) 0.30197(12) 0.18972(4) 0.0240(2) Uani 1 1 d . . .
H32 H 0.9883 0.3829 0.1748 0.029 Uiso 1 1 calc R . .
C33 C 1.13933(11) 0.29605(13) 0.20623(4) 0.0283(3) Uani 1 1 d . . .
H33 H 1.1909 0.3729 0.2026 0.034 Uiso 1 1 calc R . .
C34 C 1.18488(11) 0.17844(14) 0.22792(4) 0.0287(3) Uani 1 1 d . . .
H34 H 1.2675 0.1745 0.2391 0.034 Uiso 1 1 calc R . .
C35 C 1.10937(11) 0.06703(13) 0.23312(4) 0.0273(3) Uani 1 1 d . . .
H35 H 1.1404 -0.0138 0.2478 0.033 Uiso 1 1 calc R . .
C36 C 0.98792(10) 0.07258(12) 0.21696(4) 0.0231(2) Uani 1 1 d . . .
H36 H 0.9367 -0.0044 0.2210 0.028 Uiso 1 1 calc R . .
C41 C 0.72219(10) 0.11445(12) 0.20850(4) 0.0221(2) Uani 1 1 d . . .
C42 C 0.67822(11) -0.01072(13) 0.19227(5) 0.0290(3) Uani 1 1 d . . .
H42 H 0.7044 -0.0460 0.1621 0.035 Uiso 1 1 calc R . .
C43 C 0.59671(13) -0.08481(17) 0.21957(6) 0.0441(4) Uani 1 1 d . . .
H43 H 0.5677 -0.1705 0.2081 0.053 Uiso 1 1 calc R . .
C44 C 0.55772(13) -0.0341(2) 0.26332(6) 0.0542(5) Uani 1 1 d . . .
H44 H 0.5004 -0.0838 0.2817 0.065 Uiso 1 1 calc R . .
C45 C 0.60231(14) 0.0894(2) 0.28045(6) 0.0502(5) Uani 1 1 d . . .
H45 H 0.5762 0.1236 0.3108 0.060 Uiso 1 1 calc R . .
C46 C 0.68488(12) 0.16354(15) 0.25354(5) 0.0335(3) Uani 1 1 d . . .
H46 H 0.7160 0.2475 0.2657 0.040 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C11 1.3992(13) . ?
N1 C3 1.4457(13) . ?
N1 C2 1.4527(13) . ?
N2 C1 1.4054(14) . ?
N2 C21 1.4178(13) . ?
N2 C3 1.4499(13) . ?
O1 C4 1.2019(14) . ?
O2 C4 1.3365(13) . ?
O2 C5 1.4576(13) . ?
O3 C7 1.1959(15) . ?
O4 C7 1.3379(15) . ?
O4 C8 1.4594(16) . ?
C1 C10 1.3467(15) . ?
C1 C2 1.5268(14) . ?
C2 C4 1.5372(15) . ?
C3 C7 1.5436(15) . ?
C5 C6 1.5054(17) . ?
C8 C9 1.485(2) . ?
C10 C31 1.4890(15) . ?
C10 C41 1.4950(15) . ?
C11 C12 1.3976(15) . ?
C11 C16 1.4019(15) . ?
C12 C13 1.3922(15) . ?
C13 C14 1.3926(16) . ?
C14 C15 1.3940(16) . ?
C14 C17 1.5105(15) . ?
C15 C16 1.3848(15) . ?
C21 C26 1.3900(15) . ?
C21 C22 1.3920(15) . ?
C22 C23 1.3903(16) . ?
C23 C24 1.3892(16) . ?
C24 C25 1.3912(16) . ?
C24 C27 1.5099(15) . ?
C25 C26 1.3876(15) . ?
C31 C36 1.3984(16) . ?
C31 C32 1.3996(16) . ?
C32 C33 1.3920(17) . ?
C33 C34 1.3871(19) . ?
C34 C35 1.3816(19) . ?
C35 C36 1.3943(16) . ?
C41 C42 1.3900(18) . ?
C41 C46 1.3988(18) . ?
C42 C43 1.3870(18) . ?
C43 C44 1.379(3) . ?
C44 C45 1.386(3) . ?
C45 C46 1.389(2) . ?

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
C11 N1 C3 120.94(9) . . ?
C11 N1 C2 122.55(9) . . ?
C3 N1 C2 111.22(8) . . ?
C1 N2 C21 125.03(9) . . ?
C1 N2 C3 108.42(8) . . ?
C21 N2 C3 121.18(8) . . ?
C4 O2 C5 115.62(9) . . ?
C7 O4 C8 117.43(11) . . ?
C10 C1 N2 126.73(10) . . ?
C10 C1 C2 126.06(10) . . ?
N2 C1 C2 107.08(8) . . ?
N1 C2 C1 102.59(8) . . ?
N1 C2 C4 109.87(8) . . ?
C1 C2 C4 110.56(8) . . ?
N1 C3 N2 103.62(8) . . ?
N1 C3 C7 111.97(9) . . ?
N2 C3 C7 107.29(8) . . ?
O1 C4 O2 124.88(10) . . ?
O1 C4 C2 123.93(10) . . ?
O2 C4 C2 111.19(9) . . ?
O2 C5 C6 106.63(10) . . ?
O3 C7 O4 126.21(11) . . ?
O3 C7 C3 124.14(11) . . ?
O4 C7 C3 109.55(9) . . ?
O4 C8 C9 110.86(11) . . ?
C1 C10 C31 124.37(10) . . ?
C1 C10 C41 118.64(10) . . ?
C31 C10 C41 116.98(9) . . ?
C12 C11 N1 121.47(10) . . ?
C12 C11 C16 118.39(10) . . ?
N1 C11 C16 120.09(10) . . ?
C13 C12 C11 120.04(10) . . ?
C12 C13 C14 121.99(10) . . ?
C13 C14 C15 117.32(10) . . ?
C13 C14 C17 121.90(10) . . ?
C15 C14 C17 120.78(10) . . ?
C16 C15 C14 121.70(10) . . ?
C15 C16 C11 120.55(10) . . ?
C26 C21 C22 119.01(10) . . ?
C26 C21 N2 121.37(10) . . ?
C22 C21 N2 119.61(9) . . ?
C23 C22 C21 119.96(10) . . ?
C24 C23 C22 121.89(10) . . ?
C23 C24 C25 117.14(10) . . ?
C23 C24 C27 121.01(10) . . ?
C25 C24 C27 121.84(10) . . ?
C26 C25 C24 121.98(10) . . ?
C25 C26 C21 120.00(10) . . ?
C36 C31 C32 118.11(10) . . ?
C36 C31 C10 119.66(10) . . ?
C32 C31 C10 122.20(10) . . ?
C33 C32 C31 120.81(11) . . ?
C34 C33 C32 120.32(12) . . ?
C35 C34 C33 119.58(11) . . ?
C34 C35 C36 120.40(11) . . ?
C35 C36 C31 120.79(11) . . ?
C42 C41 C46 118.83(12) . . ?
C42 C41 C10 120.88(11) . . ?
C46 C41 C10 120.28(11) . . ?
C43 C42 C41 120.88(14) . . ?
C44 C43 C42 120.00(16) . . ?
C43 C44 C45 119.86(13) . . ?
C44 C45 C46 120.47(15) . . ?
C45 C46 C41 119.93(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 N2 C1 C10 54.52(16) . . . . ?
C3 N2 C1 C10 -151.34(11) . . . . ?
C21 N2 C1 C2 -129.40(10) . . . . ?
C3 N2 C1 C2 24.74(11) . . . . ?
C11 N1 C2 C1 -159.37(9) . . . . ?
C3 N1 C2 C1 -4.91(11) . . . . ?
C11 N1 C2 C4 83.03(12) . . . . ?
C3 N1 C2 C4 -122.51(9) . . . . ?
C10 C1 C2 N1 164.09(10) . . . . ?
N2 C1 C2 N1 -12.03(11) . . . . ?
C10 C1 C2 C4 -78.80(13) . . . . ?
N2 C1 C2 C4 105.08(9) . . . . ?
C11 N1 C3 N2 174.22(9) . . . . ?
C2 N1 C3 N2 19.29(11) . . . . ?
C11 N1 C3 C7 58.90(12) . . . . ?
C2 N1 C3 C7 -96.02(10) . . . . ?
C1 N2 C3 N1 -27.08(11) . . . . ?
C21 N2 C3 N1 128.25(10) . . . . ?
C1 N2 C3 C7 91.52(10) . . . . ?
C21 N2 C3 C7 -113.15(10) . . . . ?
C5 O2 C4 O1 6.91(15) . . . . ?
C5 O2 C4 C2 -172.46(8) . . . . ?
N1 C2 C4 O1 57.57(14) . . . . ?
C1 C2 C4 O1 -54.95(14) . . . . ?
N1 C2 C4 O2 -123.06(9) . . . . ?
C1 C2 C4 O2 124.42(9) . . . . ?
C4 O2 C5 C6 177.80(10) . . . . ?
C8 O4 C7 O3 5.25(18) . . . . ?
C8 O4 C7 C3 -171.34(10) . . . . ?
N1 C3 C7 O3 27.33(15) . . . . ?
N2 C3 C7 O3 -85.72(13) . . . . ?
N1 C3 C7 O4 -155.98(9) . . . . ?
N2 C3 C7 O4 90.96(10) . . . . ?
C7 O4 C8 C9 99.43(15) . . . . ?
N2 C1 C10 C31 3.51(18) . . . . ?
C2 C1 C10 C31 -171.85(10) . . . . ?
N2 C1 C10 C41 -175.48(10) . . . . ?
C2 C1 C10 C41 9.16(16) . . . . ?
C3 N1 C11 C12 -163.55(10) . . . . ?
C2 N1 C11 C12 -11.50(16) . . . . ?
C3 N1 C11 C16 19.01(15) . . . . ?
C2 N1 C11 C16 171.06(10) . . . . ?
N1 C11 C12 C13 -176.85(10) . . . . ?
C16 C11 C12 C13 0.63(16) . . . . ?
C11 C12 C13 C14 0.38(17) . . . . ?
C12 C13 C14 C15 -0.85(16) . . . . ?
C12 C13 C14 C17 178.36(10) . . . . ?
C13 C14 C15 C16 0.31(16) . . . . ?
C17 C14 C15 C16 -178.91(10) . . . . ?
C14 C15 C16 C11 0.70(17) . . . . ?
C12 C11 C16 C15 -1.16(16) . . . . ?
N1 C11 C16 C15 176.35(10) . . . . ?
C1 N2 C21 C26 12.59(15) . . . . ?
C3 N2 C21 C26 -138.48(10) . . . . ?
C1 N2 C21 C22 -168.12(10) . . . . ?
C3 N2 C21 C22 40.81(14) . . . . ?
C26 C21 C22 C23 1.37(15) . . . . ?
N2 C21 C22 C23 -177.94(9) . . . . ?
C21 C22 C23 C24 -1.34(17) . . . . ?
C22 C23 C24 C25 0.51(17) . . . . ?
C22 C23 C24 C27 -178.65(10) . . . . ?
C23 C24 C25 C26 0.25(17) . . . . ?
C27 C24 C25 C26 179.41(11) . . . . ?
C24 C25 C26 C21 -0.19(17) . . . . ?
C22 C21 C26 C25 -0.63(16) . . . . ?
N2 C21 C26 C25 178.66(10) . . . . ?
C1 C10 C31 C36 -147.14(11) . . . . ?
C41 C10 C31 C36 31.86(14) . . . . ?
C1 C10 C31 C32 34.86(16) . . . . ?
C41 C10 C31 C32 -146.13(11) . . . . ?
C36 C31 C32 C33 0.00(17) . . . . ?
C10 C31 C32 C33 178.02(10) . . . . ?
C31 C32 C33 C34 0.27(18) . . . . ?
C32 C33 C34 C35 -0.10(18) . . . . ?
C33 C34 C35 C36 -0.34(19) . . . . ?
C34 C35 C36 C31 0.61(18) . . . . ?
C32 C31 C36 C35 -0.43(17) . . . . ?
C10 C31 C36 C35 -178.51(10) . . . . ?
C1 C10 C41 C42 77.03(14) . . . . ?
C31 C10 C41 C42 -102.04(12) . . . . ?
C1 C10 C41 C46 -104.23(13) . . . . ?
C31 C10 C41 C46 76.70(14) . . . . ?
C46 C41 C42 C43 1.39(17) . . . . ?
C10 C41 C42 C43 -179.85(11) . . . . ?
C41 C42 C43 C44 0.35(19) . . . . ?
C42 C43 C44 C45 -1.5(2) . . . . ?
C43 C44 C45 C46 0.9(2) . . . . ?
C44 C45 C46 C41 0.9(2) . . . . ?
C42 C41 C46 C45 -2.01(18) . . . . ?
C10 C41 C46 C45 179.23(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
C27 H27B O1 0.98 2.71 3.2679(15) 116.9 3_755
C22 H22 O4 0.95 2.54 3.3423(14) 141.7 .
C32 H32 N2 0.95 2.53 3.0285(14) 112.8 .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        72.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.043
####################################################################### 
# 
# 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_DBG_dicloro2
_database_code_depnum_ccdc_archive 'CCDC 1823111'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H44 Cl2 N2 O6 S'
_chemical_formula_weight         799.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

_cell_length_a                   18.1688(9)
_cell_length_b                   18.3501(10)
_cell_length_c                   11.8464(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3949.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9986
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      30.09

_exptl_crystal_description       lath
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_F_000             1680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.269
_shelx_estimated_absorpt_T_min   0.914
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7164
_exptl_absorpt_correction_T_max  0.7406
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'omega + phi scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            210453
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.220
_diffrn_reflns_theta_max         30.587
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12107
_reflns_number_gt                10316
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'APEX 2013.2 (Bruker AXS Inc.)'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2011)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2011)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0612P)²+3.2446P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4219 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         12107
_refine_ls_number_parameters     510
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1119
_refine_ls_wR_factor_gt          0.1027
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_restrained_S_all      0.918
_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
S1 S 0.52891(3) 0.71353(3) 0.51506(6) 0.01054(12) Uani 1 1 d . . . . .
N1 N 0.52930(12) 0.76959(12) 0.62356(19) 0.0103(4) Uani 1 1 d . . . . .
N2 N 0.53931(12) 0.83121(12) 0.9046(2) 0.0124(4) Uani 1 1 d . . . . .
O1 O 0.57165(11) 0.74488(11) 0.42527(17) 0.0151(4) Uani 1 1 d . . . . .
O2 O 0.54763(11) 0.64338(10) 0.56006(17) 0.0147(4) Uani 1 1 d . . . . .
O3 O 0.67786(11) 0.71423(11) 0.64476(17) 0.0155(4) Uani 1 1 d . . . . .
O4 O 0.67660(10) 0.75407(11) 0.82476(17) 0.0149(4) Uani 1 1 d . . . . .
O5 O 0.45613(11) 0.67563(10) 0.77656(17) 0.0150(4) Uani 1 1 d . . . . .
O6 O 0.56899(11) 0.63551(10) 0.82487(17) 0.0144(4) Uani 1 1 d . . . . .
C1 C 0.50941(13) 0.84758(13) 0.6094(2) 0.0093(4) Uani 1 1 d . . . . .
H1 H 0.5331 0.8663 0.5389 0.011 Uiso 1 1 calc R U . . .
C2 C 0.54766(13) 0.88384(13) 0.7133(2) 0.0088(4) Uani 1 1 d . . . . .
C3 C 0.54681(13) 0.82180(13) 0.8004(2) 0.0092(4) Uani 1 1 d . . . . .
C4 C 0.56139(14) 0.75067(13) 0.7322(2) 0.0102(5) Uani 1 1 d . . . . .
C5 C 0.52169(14) 0.68272(14) 0.7806(2) 0.0117(5) Uani 1 1 d . . . . .
C6 C 0.53536(17) 0.57002(15) 0.8719(3) 0.0201(6) Uani 1 1 d . . . . .
H6A H 0.5121 0.5410 0.8111 0.024 Uiso 1 1 calc R U . . .
H6B H 0.4970 0.5834 0.9274 0.024 Uiso 1 1 calc R U . . .
C7 C 0.5948(2) 0.52638(18) 0.9284(3) 0.0317(8) Uani 1 1 d . . . . .
H7A H 0.6313 0.5115 0.8721 0.048 Uiso 1 1 calc R U . . .
H7B H 0.5732 0.4830 0.9634 0.048 Uiso 1 1 calc R U . . .
H7C H 0.6187 0.5562 0.9864 0.048 Uiso 1 1 calc R U . . .
C8 C 0.64646(14) 0.73664(14) 0.7263(2) 0.0112(5) Uani 1 1 d . . . . .
C9 C 0.75526(15) 0.73875(15) 0.8383(3) 0.0198(6) Uani 1 1 d . . . . .
H9A H 0.7759 0.7704 0.8982 0.024 Uiso 1 1 calc R U . . .
H9B H 0.7814 0.7497 0.7670 0.024 Uiso 1 1 calc R U . . .
C10 C 0.76691(17) 0.66044(18) 0.8690(3) 0.0256(7) Uani 1 1 d . . . . .
H10A H 0.7382 0.6488 0.9367 0.038 Uiso 1 1 calc R U . . .
H10B H 0.8193 0.6520 0.8840 0.038 Uiso 1 1 calc R U . . .
H10C H 0.7509 0.6293 0.8064 0.038 Uiso 1 1 calc R U . . .
C11 C 0.43702(14) 0.70940(14) 0.4668(2) 0.0115(5) Uani 1 1 d . . . . .
C12 C 0.38475(16) 0.67251(16) 0.5301(2) 0.0186(6) Uani 1 1 d . . . . .
H12 H 0.3971 0.6532 0.6021 0.022 Uiso 1 1 calc R U . . .
C13 C 0.31419(16) 0.66419(18) 0.4871(3) 0.0214(6) Uani 1 1 d . . . . .
H13 H 0.2780 0.6397 0.5308 0.026 Uiso 1 1 calc R U . . .
C14 C 0.29551(16) 0.69114(16) 0.3807(3) 0.0179(6) Uani 1 1 d . . . . .
C15 C 0.34893(17) 0.72800(17) 0.3191(3) 0.0208(6) Uani 1 1 d . . . . .
H15 H 0.3368 0.7471 0.2469 0.025 Uiso 1 1 calc R U . . .
C16 C 0.42003(16) 0.73752(16) 0.3612(3) 0.0176(5) Uani 1 1 d . . . . .
H16 H 0.4561 0.7628 0.3184 0.021 Uiso 1 1 calc R U . . .
C17 C 0.21879(17) 0.6805(2) 0.3344(3) 0.0287(7) Uani 1 1 d . . . . .
H17A H 0.2017 0.6312 0.3523 0.043 Uiso 1 1 calc R U . . .
H17B H 0.2194 0.6871 0.2523 0.043 Uiso 1 1 calc R U . . .
H17C H 0.1855 0.7163 0.3685 0.043 Uiso 1 1 calc R U . . .
C21 C 0.42687(13) 0.85991(14) 0.6014(2) 0.0115(5) Uani 1 1 d . . . . .
C22 C 0.37811(15) 0.83607(15) 0.6835(3) 0.0172(5) Uani 1 1 d . . . . .
H22 H 0.3962 0.8111 0.7481 0.021 Uiso 1 1 calc R U . . .
C23 C 0.30298(16) 0.84842(16) 0.6721(3) 0.0216(6) Uani 1 1 d . . . . .
H23 H 0.2704 0.8330 0.7302 0.026 Uiso 1 1 calc R U . . .
C24 C 0.27459(15) 0.88309(15) 0.5768(3) 0.0218(6) Uani 1 1 d . . . . .
C25 C 0.32349(16) 0.90584(17) 0.4944(3) 0.0234(6) Uani 1 1 d . . . . .
H25 H 0.3053 0.9288 0.4282 0.028 Uiso 1 1 calc R U . . .
C26 C 0.39892(14) 0.89564(15) 0.5071(3) 0.0177(5) Uani 1 1 d . . . . .
H26 H 0.4317 0.9132 0.4508 0.021 Uiso 1 1 calc R U . . .
C27 C 0.19240(17) 0.89432(19) 0.5630(4) 0.0348(9) Uani 1 1 d . . . . .
H27A H 0.1794 0.9440 0.5857 0.052 Uiso 1 1 calc R U . . .
H27B H 0.1659 0.8594 0.6105 0.052 Uiso 1 1 calc R U . . .
H27C H 0.1788 0.8868 0.4838 0.052 Uiso 1 1 calc R U . . .
C31 C 0.50969(14) 0.95542(13) 0.7455(2) 0.0099(5) Uani 1 1 d . . . . .
C32 C 0.46080(14) 0.96335(14) 0.8355(2) 0.0130(5) Uani 1 1 d . . . . .
H32 H 0.4498 0.9228 0.8825 0.016 Uiso 1 1 calc R U . . .
C33 C 0.42795(15) 1.03079(15) 0.8567(2) 0.0148(5) Uani 1 1 d . . . . .
H33 H 0.3948 1.0357 0.9183 0.018 Uiso 1 1 calc R U . . .
C34 C 0.44294(15) 1.09070(15) 0.7893(2) 0.0151(5) Uani 1 1 d . . . . .
H34 H 0.4210 1.1366 0.8051 0.018 Uiso 1 1 calc R U . . .
C35 C 0.49040(15) 1.08268(15) 0.6983(3) 0.0160(5) Uani 1 1 d . . . . .
H35 H 0.5004 1.1230 0.6505 0.019 Uiso 1 1 calc R U . . .
C36 C 0.52328(14) 1.01581(14) 0.6770(2) 0.0135(5) Uani 1 1 d . . . . .
H36 H 0.5557 1.0110 0.6146 0.016 Uiso 1 1 calc R U . . .
C41 C 0.63015(14) 0.89923(13) 0.6900(2) 0.0105(5) Uani 1 1 d . . . . .
C42 C 0.66619(13) 0.88042(13) 0.5905(2) 0.0113(5) Uani 1 1 d . . . . .
H42 H 0.6405 0.8548 0.5330 0.014 Uiso 1 1 calc R U . . .
C43 C 0.74007(15) 0.89916(15) 0.5748(2) 0.0153(5) Uani 1 1 d . . . . .
H43 H 0.7641 0.8866 0.5063 0.018 Uiso 1 1 calc R U . . .
C44 C 0.77844(15) 0.93584(16) 0.6579(3) 0.0179(6) Uani 1 1 d . . . . .
H44 H 0.8284 0.9491 0.6464 0.021 Uiso 1 1 calc R U . . .
C45 C 0.74331(16) 0.95309(15) 0.7583(3) 0.0176(5) Uani 1 1 d . . . . .
H45 H 0.7698 0.9771 0.8166 0.021 Uiso 1 1 calc R U . . .
C46 C 0.66965(14) 0.93549(15) 0.7741(2) 0.0148(5) Uani 1 1 d . . . . .
H46 H 0.6459 0.9482 0.8428 0.018 Uiso 1 1 calc R U . . .
C51 C 0.53642(15) 0.77340(14) 0.9852(2) 0.0134(5) Uani 1 1 d . . . . .
C52 C 0.46857(16) 0.74171(15) 1.0089(3) 0.0174(5) Uani 1 1 d . . . . .
H52 H 0.4255 0.7581 0.9711 0.021 Uiso 1 1 calc R U . . .
C53 C 0.46402(19) 0.68585(16) 1.0882(3) 0.0224(6) Uani 1 1 d . . . . .
H53 H 0.4176 0.6641 1.1033 0.027 Uiso 1 1 calc R U . . .
C54 C 0.5258(2) 0.66133(16) 1.1456(3) 0.0249(7) Uani 1 1 d . . . . .
C55 C 0.5924(2) 0.69644(17) 1.1251(3) 0.0235(6) Uani 1 1 d . . . . .
H55 H 0.6349 0.6817 1.1658 0.028 Uiso 1 1 calc R U . . .
C56 C 0.59838(17) 0.75263(16) 1.0463(2) 0.0184(6) Uani 1 1 d . . . . .
H56 H 0.6442 0.7764 1.0346 0.022 Uiso 1 1 calc R U . . .
C57 C 0.5209(3) 0.59777(19) 1.2265(3) 0.0393(10) Uani 1 1 d . . . . .
H57A H 0.4702 0.5931 1.2539 0.059 Uiso 1 1 calc R U . . .
H57B H 0.5539 0.6062 1.2906 0.059 Uiso 1 1 calc R U . . .
H57C H 0.5353 0.5529 1.1875 0.059 Uiso 1 1 calc R U . . .
C99 C 0.8306(2) 0.5352(2) 0.1020(3) 0.0337(8) Uani 1 1 d . . . . .
H99A H 0.8731 0.5353 0.1542 0.040 Uiso 1 1 calc R U . A 1
H99B H 0.8188 0.5865 0.0836 0.040 Uiso 1 1 calc R U . A 1
Cl1A Cl 0.75480(19) 0.49555(16) 0.17033(19) 0.0809(13) Uani 0.875(8) 1 d . . P
B 1
Cl2A Cl 0.85580(15) 0.48950(13) -0.0231(2) 0.0470(5) Uani 0.875(8) 1 d . . P B
1
Cl1B Cl 0.7914(7) 0.4697(5) 0.1832(9) 0.038(3) Uiso 0.125(8) 1 d . . P B 2
Cl2B Cl 0.8391(7) 0.4925(8) -0.0300(12) 0.019(2) Uiso 0.125(8) 1 d . . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.4341(19) . ?
S1 O1 1.437(2) . ?
S1 N1 1.646(2) . ?
S1 C11 1.766(3) . ?
N1 C4 1.455(3) . ?
N1 C1 1.486(3) . ?
N2 C3 1.254(3) . ?
N2 C51 1.428(3) . ?
O3 C8 1.195(3) . ?
O4 C8 1.328(3) . ?
O4 C9 1.465(3) . ?
O5 C5 1.199(3) . ?
O6 C5 1.328(3) . ?
O6 C6 1.459(3) . ?
C1 C21 1.520(3) . ?
C1 C2 1.562(4) . ?
C1 H1 1.0000 . ?
C2 C31 1.532(3) . ?
C2 C3 1.536(3) . ?
C2 C41 1.550(3) . ?
C3 C4 1.558(3) . ?
C4 C5 1.550(4) . ?
C4 C8 1.568(3) . ?
C6 C7 1.501(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C9 C10 1.497(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.387(4) . ?
C11 C16 1.387(4) . ?
C12 C13 1.388(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.390(4) . ?
C14 C17 1.511(4) . ?
C15 C16 1.396(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 C22 1.387(4) . ?
C21 C26 1.392(4) . ?
C22 C23 1.390(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.395(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(5) . ?
C24 C27 1.516(4) . ?
C25 C26 1.391(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C31 C32 1.395(4) . ?
C31 C36 1.396(4) . ?
C32 C33 1.397(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.386(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.388(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.388(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.393(4) . ?
C41 C46 1.397(4) . ?
C42 C43 1.398(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.382(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.386(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.389(4) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C52 1.392(4) . ?
C51 C56 1.392(4) . ?
C52 C53 1.393(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.387(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.392(5) . ?
C54 C57 1.512(4) . ?
C55 C56 1.395(4) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C99 Cl1B 1.697(11) . ?
C99 Cl2B 1.756(15) . ?
C99 Cl1A 1.756(4) . ?
C99 Cl2A 1.763(4) . ?
C99 H99A 0.9900 . ?
C99 H99B 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
O2 S1 O1 120.42(12) . . ?
O2 S1 N1 105.64(12) . . ?
O1 S1 N1 108.99(12) . . ?
O2 S1 C11 107.82(12) . . ?
O1 S1 C11 106.75(13) . . ?
N1 S1 C11 106.47(12) . . ?
C4 N1 C1 115.3(2) . . ?
C4 N1 S1 122.90(17) . . ?
C1 N1 S1 120.84(17) . . ?
C3 N2 C51 124.0(2) . . ?
C8 O4 C9 116.9(2) . . ?
C5 O6 C6 114.7(2) . . ?
N1 C1 C21 113.0(2) . . ?
N1 C1 C2 102.30(19) . . ?
C21 C1 C2 115.1(2) . . ?
N1 C1 H1 108.7 . . ?
C21 C1 H1 108.7 . . ?
C2 C1 H1 108.7 . . ?
C31 C2 C3 117.6(2) . . ?
C31 C2 C41 108.9(2) . . ?
C3 C2 C41 105.32(19) . . ?
C31 C2 C1 111.2(2) . . ?
C3 C2 C1 102.08(19) . . ?
C41 C2 C1 111.6(2) . . ?
N2 C3 C2 124.1(2) . . ?
N2 C3 C4 130.1(2) . . ?
C2 C3 C4 105.7(2) . . ?
N1 C4 C5 109.4(2) . . ?
N1 C4 C3 100.99(19) . . ?
C5 C4 C3 113.8(2) . . ?
N1 C4 C8 113.2(2) . . ?
C5 C4 C8 110.1(2) . . ?
C3 C4 C8 109.2(2) . . ?
O5 C5 O6 126.0(2) . . ?
O5 C5 C4 122.3(2) . . ?
O6 C5 C4 111.7(2) . . ?
O6 C6 C7 107.9(3) . . ?
O6 C6 H6A 110.1 . . ?
C7 C6 H6A 110.1 . . ?
O6 C6 H6B 110.1 . . ?
C7 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 O4 126.6(2) . . ?
O3 C8 C4 124.3(2) . . ?
O4 C8 C4 109.1(2) . . ?
O4 C9 C10 110.4(2) . . ?
O4 C9 H9A 109.6 . . ?
C10 C9 H9A 109.6 . . ?
O4 C9 H9B 109.6 . . ?
C10 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 121.1(3) . . ?
C12 C11 S1 119.5(2) . . ?
C16 C11 S1 119.1(2) . . ?
C11 C12 C13 119.2(3) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C14 121.2(3) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 118.5(3) . . ?
C15 C14 C17 121.1(3) . . ?
C13 C14 C17 120.4(3) . . ?
C14 C15 C16 121.3(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C11 C16 C15 118.8(3) . . ?
C11 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C21 C26 118.6(2) . . ?
C22 C21 C1 122.7(2) . . ?
C26 C21 C1 118.7(2) . . ?
C21 C22 C23 120.5(3) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C24 121.1(3) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 118.1(3) . . ?
C25 C24 C27 121.0(3) . . ?
C23 C24 C27 120.9(3) . . ?
C24 C25 C26 121.0(3) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C21 120.6(3) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C32 C31 C36 118.3(2) . . ?
C32 C31 C2 124.5(2) . . ?
C36 C31 C2 117.1(2) . . ?
C31 C32 C33 120.1(2) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C34 C33 C32 121.0(3) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 119.0(2) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C36 C35 C34 120.1(3) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C31 121.4(3) . . ?
C35 C36 H36 119.3 . . ?
C31 C36 H36 119.3 . . ?
C42 C41 C46 118.7(2) . . ?
C42 C41 C2 124.1(2) . . ?
C46 C41 C2 117.2(2) . . ?
C41 C42 C43 120.2(2) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 120.6(3) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C43 C44 C45 119.4(3) . . ?
C43 C44 H44 120.3 . . ?
C45 C44 H44 120.3 . . ?
C44 C45 C46 120.4(3) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C45 C46 C41 120.6(3) . . ?
C45 C46 H46 119.7 . . ?
C41 C46 H46 119.7 . . ?
C52 C51 C56 119.8(3) . . ?
C52 C51 N2 118.5(2) . . ?
C56 C51 N2 121.4(2) . . ?
C51 C52 C53 119.7(3) . . ?
C51 C52 H52 120.1 . . ?
C53 C52 H52 120.1 . . ?
C54 C53 C52 121.4(3) . . ?
C54 C53 H53 119.3 . . ?
C52 C53 H53 119.3 . . ?
C53 C54 C55 117.8(3) . . ?
C53 C54 C57 120.9(3) . . ?
C55 C54 C57 121.3(3) . . ?
C54 C55 C56 121.8(3) . . ?
C54 C55 H55 119.1 . . ?
C56 C55 H55 119.1 . . ?
C51 C56 C55 119.2(3) . . ?
C51 C56 H56 120.4 . . ?
C55 C56 H56 120.4 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
Cl1B C99 Cl2B 103.1(6) . . ?
Cl1A C99 Cl2A 113.2(2) . . ?
Cl1A C99 H99A 108.9 . . ?
Cl2A C99 H99A 108.9 . . ?
Cl1A C99 H99B 108.9 . . ?
Cl2A C99 H99B 108.9 . . ?
H99A C99 H99B 107.8 . . ?

_refine_diff_density_max         0.630
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.065



