# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

####################################################################### 
# 
# 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_SRG160317
_audit_block_doi                 10.5517/ccdc.csd.cc1mcj5p
_database_code_depnum_ccdc_archive 'CCDC 1500622'
_audit_update_record             
;
2016-08-23 deposited with the CCDC.
2016-12-12 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         'C23 H14 Br N O4'
_chemical_formula_sum            'C23 H14 Br N O4'
_chemical_formula_weight         448.26

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'
Br Br -0.2901 2.4595 '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                   18.294(5)
_cell_length_b                   7.120(5)
_cell_length_c                   15.904(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 111.529(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     1927.0(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9874
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      26.40

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    2.164
_shelx_estimated_absorpt_T_min   0.544
_shelx_estimated_absorpt_T_max   0.625
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_T_max  0.595
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27483
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.197
_diffrn_reflns_theta_max         27.633
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4443
_reflns_number_gt                3466
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0554P)²+0.5559P] 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         4443
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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
Br1 Br 0.6043(2) 0.4547(2) 0.8349(2) 0.0505(6) Uani 0.65(3) 1 d . . P A 1
Br1' Br 0.5938(6) 0.4650(8) 0.8256(5) 0.0791(16) Uani 0.35(3) 1 d . . P A 2
C1 C 0.22512(13) 0.1603(3) 0.77221(13) 0.0340(5) Uani 1 1 d . . . . .
C2 C 0.14549(13) 0.2360(3) 0.72123(14) 0.0374(5) Uani 1 1 d . . . . .
C3 C 0.10566(16) 0.2446(4) 0.62851(16) 0.0507(6) Uani 1 1 d . . . . .
H3 H 0.1280 0.1999 0.5885 0.061 Uiso 1 1 calc R U . . .
C4 C 0.03112(18) 0.3226(4) 0.59805(19) 0.0667(8) Uani 1 1 d . . . . .
H4 H 0.0027 0.3297 0.5362 0.080 Uiso 1 1 calc R U . . .
C5 C -0.00200(18) 0.3898(5) 0.6570(2) 0.0711(9) Uani 1 1 d . . . . .
H5 H -0.0522 0.4411 0.6340 0.085 Uiso 1 1 calc R U . . .
C6 C 0.03722(16) 0.3831(4) 0.7493(2) 0.0565(7) Uani 1 1 d . . . . .
H6 H 0.0147 0.4294 0.7889 0.068 Uiso 1 1 calc R U . . .
C7 C 0.11188(13) 0.3042(3) 0.78069(15) 0.0394(5) Uani 1 1 d . . . . .
C8 C 0.16771(13) 0.2810(3) 0.87541(14) 0.0381(5) Uani 1 1 d . . . . .
C9 C 0.23962(13) 0.1898(3) 0.87000(13) 0.0336(4) Uani 1 1 d . . . . .
C10 C 0.29048(13) 0.0467(3) 0.93902(14) 0.0350(5) Uani 1 1 d . . . . .
H10 H 0.3157 -0.0468 0.9134 0.042 Uiso 1 1 calc R U . . .
C11 C 0.32094(13) 0.2393(3) 0.94082(13) 0.0362(5) Uani 1 1 d . . . . .
H11 H 0.3182 0.3154 0.9909 0.043 Uiso 1 1 calc R U . . .
C12 C 0.38934(13) 0.2883(3) 0.91410(13) 0.0367(5) Uani 1 1 d . . . . .
C13 C 0.40178(15) 0.4744(3) 0.89795(16) 0.0457(6) Uani 1 1 d . . . . .
H13 H 0.3678 0.5664 0.9037 0.055 Uiso 1 1 calc R U . . .
C14 C 0.46450(16) 0.5254(4) 0.87319(17) 0.0497(6) Uani 1 1 d . . . . .
H14 H 0.4719 0.6505 0.8615 0.060 Uiso 1 1 calc R U . . .
C15 C 0.51524(14) 0.3907(4) 0.86611(15) 0.0433(5) Uani 1 1 d . . . . .
C16 C 0.50534(15) 0.2057(4) 0.88380(19) 0.0549(6) Uani 1 1 d . . . . .
H16 H 0.5407 0.1151 0.8801 0.066 Uiso 1 1 calc R U . . .
C17 C 0.44177(16) 0.1551(4) 0.90738(18) 0.0518(6) Uani 1 1 d . . . . .
H17 H 0.4346 0.0297 0.9188 0.062 Uiso 1 1 calc R U . . .
C18 C 0.26437(13) -0.0287(3) 1.01145(14) 0.0353(5) Uani 1 1 d . . . . .
C19 C 0.29534(14) 0.0416(3) 1.09882(14) 0.0405(5) Uani 1 1 d . . . . .
H19 H 0.3333 0.1355 1.1132 0.049 Uiso 1 1 calc R U . . .
C20 C 0.26987(16) -0.0275(3) 1.16461(15) 0.0429(5) Uani 1 1 d . . . . .
H20 H 0.2911 0.0176 1.2235 0.052 Uiso 1 1 calc R U . . .
C21 C 0.21304(14) -0.1633(3) 1.14183(15) 0.0405(5) Uani 1 1 d . . . . .
C22 C 0.18291(15) -0.2414(3) 1.05637(16) 0.0453(5) Uani 1 1 d . . . . .
H22 H 0.1455 -0.3365 1.0427 0.054 Uiso 1 1 calc R U . . .
C23 C 0.21033(14) -0.1733(3) 0.99185(14) 0.0422(5) Uani 1 1 d . . . . .
H23 H 0.1920 -0.2259 0.9343 0.051 Uiso 1 1 calc R U . . .
N1 N 0.18128(16) -0.2231(3) 1.21050(16) 0.0549(6) Uani 1 1 d . . . . .
O1 O 0.26936(10) 0.0855(2) 0.74139(10) 0.0448(4) Uani 1 1 d . . . . .
O2 O 0.15754(11) 0.3297(3) 0.94310(11) 0.0572(5) Uani 1 1 d . . . . .
O3 O 0.12049(14) -0.3096(3) 1.18590(16) 0.0748(6) Uani 1 1 d . . . . .
O4 O 0.21765(15) -0.1779(3) 1.28915(13) 0.0749(6) 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
Br1 C15 1.923(3) . ?
Br1' C15 1.854(6) . ?
C1 O1 1.212(3) . ?
C1 C2 1.484(3) . ?
C1 C9 1.493(3) . ?
C2 C3 1.386(3) . ?
C2 C7 1.391(3) . ?
C3 C4 1.385(4) . ?
C4 C5 1.376(5) . ?
C5 C6 1.378(4) . ?
C6 C7 1.389(3) . ?
C7 C8 1.487(3) . ?
C8 O2 1.209(3) . ?
C8 C9 1.498(3) . ?
C9 C10 1.535(3) . ?
C9 C11 1.542(3) . ?
C10 C11 1.476(3) . ?
C10 C18 1.499(3) . ?
C11 C12 1.503(3) . ?
C12 C17 1.381(3) . ?
C12 C13 1.384(3) . ?
C13 C14 1.391(4) . ?
C14 C15 1.367(4) . ?
C15 C16 1.373(4) . ?
C16 C17 1.394(4) . ?
C18 C23 1.382(3) . ?
C18 C19 1.387(3) . ?
C19 C20 1.383(3) . ?
C20 C21 1.367(3) . ?
C21 C22 1.382(3) . ?
C21 N1 1.476(3) . ?
C22 C23 1.385(3) . ?
N1 O3 1.204(3) . ?
N1 O4 1.225(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 127.27(19) . . ?
O1 C1 C9 126.4(2) . . ?
C2 C1 C9 106.35(18) . . ?
C3 C2 C7 121.1(2) . . ?
C3 C2 C1 128.7(2) . . ?
C7 C2 C1 110.22(18) . . ?
C4 C3 C2 117.1(3) . . ?
C5 C4 C3 121.6(3) . . ?
C4 C5 C6 121.8(3) . . ?
C5 C6 C7 117.1(3) . . ?
C6 C7 C2 121.2(2) . . ?
C6 C7 C8 128.9(2) . . ?
C2 C7 C8 109.83(19) . . ?
O2 C8 C7 126.7(2) . . ?
O2 C8 C9 127.0(2) . . ?
C7 C8 C9 106.34(17) . . ?
C1 C9 C8 107.26(17) . . ?
C1 C9 C10 118.73(18) . . ?
C8 C9 C10 124.13(18) . . ?
C1 C9 C11 123.23(18) . . ?
C8 C9 C11 119.42(18) . . ?
C10 C9 C11 57.34(14) . . ?
C11 C10 C18 122.84(18) . . ?
C11 C10 C9 61.53(14) . . ?
C18 C10 C9 120.44(19) . . ?
C10 C11 C12 123.9(2) . . ?
C10 C11 C9 61.12(14) . . ?
C12 C11 C9 121.80(17) . . ?
C17 C12 C13 118.5(2) . . ?
C17 C12 C11 122.5(2) . . ?
C13 C12 C11 119.0(2) . . ?
C12 C13 C14 120.7(2) . . ?
C15 C14 C13 119.7(2) . . ?
C14 C15 C16 120.8(2) . . ?
C14 C15 Br1' 117.7(3) . . ?
C16 C15 Br1' 121.5(3) . . ?
C14 C15 Br1 121.3(2) . . ?
C16 C15 Br1 117.9(2) . . ?
C15 C16 C17 119.3(2) . . ?
C12 C17 C16 121.0(2) . . ?
C23 C18 C19 119.4(2) . . ?
C23 C18 C10 119.80(19) . . ?
C19 C18 C10 120.8(2) . . ?
C20 C19 C18 120.1(2) . . ?
C21 C20 C19 119.1(2) . . ?
C20 C21 C22 122.4(2) . . ?
C20 C21 N1 118.4(2) . . ?
C22 C21 N1 119.2(2) . . ?
C21 C22 C23 117.7(2) . . ?
C18 C23 C22 121.2(2) . . ?
O3 N1 O4 123.9(2) . . ?
O3 N1 C21 118.4(2) . . ?
O4 N1 C21 117.8(2) . . ?

_refine_diff_density_max         0.258
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.063



####################################################################### 
# 
# 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_1o
_audit_block_doi                 10.5517/ccdc.csd.cc1ly3rd
_database_code_depnum_ccdc_archive 'CCDC 1487744'
_audit_update_record             
;
2016-06-27 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H44 Cl2 N2 O8, C H2 Cl2'
_chemical_formula_sum            'C59 H46 Cl4 N2 O8'
_chemical_formula_weight         1052.78

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.1561(12)
_cell_length_b                   12.5142(14)
_cell_length_c                   18.372(2)
_cell_angle_alpha                72.952(4)
_cell_angle_beta                 80.265(3)
_cell_angle_gamma                86.171(4)
_cell_volume                     2633.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9990
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.33

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40795
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         27.62
_reflns_number_total             12063
_reflns_number_gt                7323
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.1196P)²+0.7902P] 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         12063
_refine_ls_number_parameters     738
_refine_ls_number_restraints     232
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_ref         0.2212
_refine_ls_wR_factor_gt          0.2002
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.110
_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
C1 C 0.1970(2) 0.7210(2) 0.79413(15) 0.0211(6) Uani 1 1 d . . .
H1 H 0.2281 0.7960 0.7795 0.025 Uiso 1 1 calc R . .
C2 C 0.0682(2) 0.7329(2) 0.79810(16) 0.0240(6) Uani 1 1 d . . .
H2 H 0.0519 0.8130 0.7780 0.029 Uiso 1 1 calc R . .
C3 C -0.0016(2) 0.6948(2) 0.87693(16) 0.0227(6) Uani 1 1 d . . .
C4 C -0.1185(2) 0.6950(2) 0.88422(17) 0.0269(7) Uani 1 1 d . . .
H4 H -0.1519 0.7182 0.8400 0.032 Uiso 1 1 calc R . .
C5 C -0.1848(3) 0.6620(3) 0.95500(19) 0.0312(7) Uani 1 1 d . . .
H5 H -0.2621 0.6629 0.9583 0.037 Uiso 1 1 calc R . .
C6 C -0.1366(2) 0.6273(2) 1.02132(18) 0.0286(7) Uani 1 1 d . . .
H6 H -0.1813 0.6042 1.0693 0.034 Uiso 1 1 calc R . .
C7 C -0.0226(2) 0.6270(2) 1.01618(17) 0.0259(6) Uani 1 1 d . . .
H7 H 0.0097 0.6032 1.0608 0.031 Uiso 1 1 calc R . .
C8 C 0.0459(2) 0.6624(2) 0.94383(16) 0.0208(6) Uani 1 1 d . . .
C9 C 0.1696(2) 0.6559(2) 0.94146(15) 0.0180(6) Uani 1 1 d . . .
H9 H 0.1848 0.5834 0.9773 0.022 Uiso 1 1 calc R . .
C10 C 0.3500(2) 0.6814(2) 0.86897(16) 0.0201(6) Uani 1 1 d . . .
H10 H 0.3742 0.7470 0.8258 0.024 Uiso 1 1 calc R . .
C11 C 0.4295(2) 0.5836(3) 0.86520(18) 0.0270(7) Uani 1 1 d . . .
C12 C 0.6011(4) 0.5314(4) 0.7997(3) 0.0740(15) Uani 1 1 d . . .
H12A H 0.5743 0.4758 0.7799 0.089 Uiso 1 1 calc R . .
H12B H 0.6239 0.4940 0.8492 0.089 Uiso 1 1 calc R . .
C13 C 0.6960(3) 0.5925(4) 0.7449(3) 0.0692(13) Uani 1 1 d . . .
H13A H 0.6716 0.6308 0.6967 0.104 Uiso 1 1 calc R . .
H13B H 0.7551 0.5404 0.7366 0.104 Uiso 1 1 calc R . .
H13C H 0.7228 0.6459 0.7658 0.104 Uiso 1 1 calc R . .
C14 C 0.1998(2) 0.8674(2) 0.92726(16) 0.0226(6) Uani 1 1 d . . .
C15 C 0.1641(2) 0.9243(2) 0.98721(16) 0.0216(6) Uani 1 1 d . . .
C16 C 0.1341(2) 1.0363(2) 0.97797(19) 0.0267(7) Uani 1 1 d . . .
H16 H 0.1347 1.0863 0.9292 0.032 Uiso 1 1 calc R . .
C17 C 0.1036(2) 1.0708(3) 1.0431(2) 0.0337(8) Uani 1 1 d . . .
H17 H 0.0837 1.1454 1.0382 0.040 Uiso 1 1 calc R . .
C18 C 0.1020(3) 0.9956(3) 1.1170(2) 0.0362(8) Uani 1 1 d . . .
H18 H 0.0808 1.0208 1.1603 0.043 Uiso 1 1 calc R . .
C19 C 0.1317(3) 0.8845(3) 1.12613(18) 0.0311(7) Uani 1 1 d . . .
H19 H 0.1311 0.8346 1.1750 0.037 Uiso 1 1 calc R . .
C20 C 0.1625(2) 0.8493(2) 1.06047(16) 0.0233(6) Uani 1 1 d . . .
C21 C 0.1995(2) 0.7365(2) 1.05334(16) 0.0215(6) Uani 1 1 d . . .
C22 C 0.2269(2) 0.7446(2) 0.96732(15) 0.0194(6) Uani 1 1 d . . .
C23 C 0.3497(2) 0.7080(2) 0.94609(16) 0.0210(6) Uani 1 1 d . . .
H23 H 0.3614 0.6366 0.9843 0.025 Uiso 1 1 calc R . .
C24 C 0.4386(2) 0.7850(2) 0.94830(16) 0.0231(6) Uani 1 1 d . . .
C25 C 0.4827(2) 0.7646(2) 1.01593(17) 0.0266(7) Uani 1 1 d . . .
H25 H 0.4594 0.7033 1.0576 0.032 Uiso 1 1 calc R . .
C26 C 0.5617(2) 0.8359(3) 1.02133(18) 0.0301(7) Uani 1 1 d . . .
C27 C 0.5992(3) 0.9257(3) 0.9607(2) 0.0346(8) Uani 1 1 d . . .
H27 H 0.6523 0.9726 0.9652 0.042 Uiso 1 1 calc R . .
C28 C 0.5570(3) 0.9452(3) 0.8930(2) 0.0379(8) Uani 1 1 d . . .
H28 H 0.5830 1.0051 0.8512 0.046 Uiso 1 1 calc R . .
C29 C 0.4763(3) 0.8772(3) 0.88584(18) 0.0313(7) Uani 1 1 d . . .
H29 H 0.4473 0.8926 0.8400 0.038 Uiso 1 1 calc R . .
C30 C 0.0347(2) 0.6767(3) 0.74033(16) 0.0271(7) Uani 1 1 d . . .
H30 H -0.0467 0.6784 0.7435 0.033 Uiso 1 1 calc R . .
C31 C 0.0787(2) 0.5580(3) 0.75674(15) 0.0252(6) Uani 1 1 d . . .
C32 C 0.0176(3) 0.4617(3) 0.77412(16) 0.0330(8) Uani 1 1 d . . .
H32 H -0.0598 0.4658 0.7783 0.040 Uiso 1 1 calc R . .
C33 C 0.0727(3) 0.3595(3) 0.78507(18) 0.0413(9) Uani 1 1 d . . .
H33 H 0.0322 0.2947 0.7960 0.050 Uiso 1 1 calc R . .
C34 C 0.1870(3) 0.3524(3) 0.78004(19) 0.0393(8) Uani 1 1 d . . .
H34 H 0.2232 0.2831 0.7870 0.047 Uiso 1 1 calc R . .
C35 C 0.2489(3) 0.4483(3) 0.76463(17) 0.0298(7) Uani 1 1 d . . .
H35 H 0.3259 0.4433 0.7633 0.036 Uiso 1 1 calc R . .
C36 C 0.1944(2) 0.5514(2) 0.75136(15) 0.0226(6) Uani 1 1 d . . .
C37 C 0.2456(2) 0.6639(2) 0.73072(16) 0.0222(6) Uani 1 1 d . . .
H37 H 0.3271 0.6572 0.7258 0.027 Uiso 1 1 calc R . .
C38 C 0.2094(2) 0.7397(3) 0.65499(16) 0.0264(6) Uani 1 1 d . . .
H38 H 0.2354 0.8152 0.6476 0.032 Uiso 1 1 calc R . .
C39 C 0.0495(3) 0.7277(4) 0.59715(19) 0.0496(10) Uani 1 1 d D . .
H39A H 0.0167 0.6546 0.6059 0.060 Uiso 0.435(7) 1 calc PR A 1
H39B H 0.0389 0.6470 0.6093 0.060 Uiso 0.565(7) 1 d PR A 2
C40 C -0.0361(11) 0.8392(12) 0.5698(9) 0.078(3) Uani 0.435(7) 1 d PDU A 1
O5 O -0.1242(8) 0.7997(10) 0.6096(6) 0.102(3) Uani 0.435(7) 1 d PDU A 1
O6 O -0.0128(6) 0.9248(7) 0.5223(4) 0.091(3) Uani 0.435(7) 1 d PDU A 1
C41 C -0.2049(12) 0.8951(14) 0.5898(9) 0.096(3) Uani 0.435(7) 1 d PDU A 1
H41A H -0.2748 0.8701 0.5821 0.115 Uiso 0.435(7) 1 calc PR A 1
H41B H -0.1742 0.9522 0.5437 0.115 Uiso 0.435(7) 1 calc PR A 1
C42 C -0.2212(15) 0.9387(14) 0.6607(11) 0.096(4) Uani 0.435(7) 1 d PDU A 1
H42A H -0.2261 0.8766 0.7065 0.144 Uiso 0.435(7) 1 calc PR A 1
H42B H -0.2888 0.9828 0.6620 0.144 Uiso 0.435(7) 1 calc PR A 1
H42C H -0.1591 0.9838 0.6581 0.144 Uiso 0.435(7) 1 calc PR A 1
C40' C -0.0597(8) 0.7936(11) 0.5805(6) 0.080(2) Uani 0.565(7) 1 d PDU A 2
O5' O -0.1064(5) 0.8443(6) 0.6341(3) 0.0665(17) Uani 0.565(7) 1 d PDU A 2
O6' O -0.1171(6) 0.7836(10) 0.5366(5) 0.146(3) Uani 0.565(7) 1 d PDU A 2
C41' C -0.2061(7) 0.9188(9) 0.6250(4) 0.055(2) Uani 0.565(7) 1 d PDU A 2
H41C H -0.2658 0.8822 0.6131 0.066 Uiso 0.565(7) 1 calc PR A 2
H41D H -0.1884 0.9875 0.5842 0.066 Uiso 0.565(7) 1 calc PR A 2
C42' C -0.2394(9) 0.9423(9) 0.7029(5) 0.073(3) Uani 0.565(7) 1 d PDU A 2
H42D H -0.2646 0.8747 0.7415 0.109 Uiso 0.565(7) 1 calc PR A 2
H42E H -0.2985 0.9976 0.6996 0.109 Uiso 0.565(7) 1 calc PR A 2
H42F H -0.1762 0.9695 0.7167 0.109 Uiso 0.565(7) 1 calc PR A 2
C43 C 0.2734(3) 0.5855(3) 0.58630(18) 0.0392(8) Uani 1 1 d . . .
C44 C 0.3829(4) 0.5502(9) 0.5890(6) 0.053(3) Uani 0.455(12) 1 d PGU B 1
C45 C 0.4341(6) 0.4452(8) 0.6087(5) 0.061(3) Uani 0.455(12) 1 d PGU B 1
H45 H 0.3910 0.3813 0.6263 0.073 Uiso 0.455(12) 1 calc PR B 1
C46 C 0.5497(6) 0.4357(10) 0.6021(5) 0.076(3) Uani 0.455(12) 1 d PGU B 1
H46 H 0.5839 0.3655 0.6153 0.091 Uiso 0.455(12) 1 calc PR B 1
C47 C 0.6141(4) 0.5312(11) 0.5758(6) 0.078(4) Uani 0.455(12) 1 d PGU B 1
H47 H 0.6914 0.5248 0.5714 0.094 Uiso 0.455(12) 1 calc PR B 1
C48 C 0.5629(5) 0.6361(10) 0.5561(5) 0.072(3) Uani 0.455(12) 1 d PGU B 1
H48 H 0.6059 0.7000 0.5385 0.086 Uiso 0.455(12) 1 calc PR B 1
C49 C 0.4473(6) 0.6456(9) 0.5627(5) 0.055(3) Uani 0.455(12) 1 d PGU B 1
C44' C 0.4043(4) 0.5892(5) 0.5772(5) 0.047(2) Uani 0.545(12) 1 d PGU B 2
C45' C 0.4791(6) 0.4992(5) 0.5905(4) 0.059(2) Uani 0.545(12) 1 d PGU B 2
H45' H 0.4527 0.4267 0.6104 0.071 Uiso 0.545(12) 1 calc PR B 2
C46' C 0.5933(6) 0.5176(6) 0.5742(4) 0.065(3) Uani 0.545(12) 1 d PGU B 2
H46' H 0.6433 0.4574 0.5831 0.078 Uiso 0.545(12) 1 calc PR B 2
C47' C 0.6327(4) 0.6260(8) 0.5445(4) 0.063(3) Uani 0.545(12) 1 d PGU B 2
H47' H 0.7092 0.6383 0.5335 0.075 Uiso 0.545(12) 1 calc PR B 2
C48' C 0.5580(4) 0.7160(6) 0.5311(4) 0.051(2) Uani 0.545(12) 1 d PGU B 2
H48' H 0.5843 0.7885 0.5113 0.062 Uiso 0.545(12) 1 calc PR B 2
C49' C 0.4437(4) 0.6976(5) 0.5475(4) 0.0419(19) Uani 0.545(12) 1 d PGU B 2
C50 C 0.3602(3) 0.7652(4) 0.5421(2) 0.0536(11) Uani 1 1 d . . .
C51 C 0.2479(3) 0.7098(3) 0.57748(16) 0.0293(7) Uani 1 1 d . A .
C52 C 0.1507(3) 0.7563(3) 0.53281(17) 0.0358(8) Uani 1 1 d . A .
H52 H 0.1565 0.8379 0.5162 0.043 Uiso 1 1 calc R . .
C53 C 0.1491(3) 0.7204(3) 0.46134(18) 0.0351(8) Uani 1 1 d . . .
C54 C 0.2333(3) 0.7570(3) 0.39854(17) 0.0378(8) Uani 1 1 d . A .
H54 H 0.2888 0.8027 0.4013 0.045 Uiso 1 1 calc R . .
C55 C 0.2348(3) 0.7260(3) 0.33235(18) 0.0392(8) Uani 1 1 d . . .
C56 C 0.1536(3) 0.6597(3) 0.32540(19) 0.0416(9) Uani 1 1 d . A .
H56 H 0.1555 0.6399 0.2802 0.050 Uiso 1 1 calc R . .
C57 C 0.0697(3) 0.6235(3) 0.38668(19) 0.0446(9) Uani 1 1 d . . .
H57 H 0.0134 0.5795 0.3829 0.053 Uiso 1 1 calc R A .
C58 C 0.0687(3) 0.6525(3) 0.4544(2) 0.0451(9) Uani 1 1 d . A .
H58 H 0.0127 0.6255 0.4960 0.054 Uiso 1 1 calc R . .
C59 C 0.5603(6) 0.9997(5) 0.3734(3) 0.097(2) Uani 1 1 d . . .
H59A H 0.6396 0.9987 0.3753 0.116 Uiso 1 1 calc R . .
H59B H 0.5211 0.9770 0.4259 0.116 Uiso 1 1 calc R . .
Cl1 Cl 0.61313(8) 0.80799(8) 1.10818(6) 0.0537(3) Uani 1 1 d . . .
Cl2 Cl 0.34355(10) 0.76833(10) 0.25555(5) 0.0656(3) Uani 1 1 d . A .
Cl3 Cl 0.51718(10) 1.13656(12) 0.32685(6) 0.0732(4) Uani 1 1 d . . .
Cl4 Cl 0.53351(13) 0.90533(13) 0.32525(8) 0.0930(5) Uani 1 1 d . . .
N1 N 0.23446(18) 0.65479(18) 0.86709(13) 0.0195(5) Uani 1 1 d . . .
N2 N 0.0869(2) 0.7458(2) 0.66387(14) 0.0325(6) Uani 1 1 d . A .
O1 O 0.4204(2) 0.4918(2) 0.90740(17) 0.0542(7) Uani 1 1 d . . .
O2 O 0.51388(19) 0.6152(2) 0.80768(15) 0.0490(7) Uani 1 1 d . . .
O3 O 0.2070(2) 0.91143(17) 0.85853(12) 0.0349(5) Uani 1 1 d . . .
O4 O 0.20885(17) 0.65224(17) 1.10581(11) 0.0289(5) Uani 1 1 d . . .
O7 O 0.2069(3) 0.5164(2) 0.58917(13) 0.0563(8) Uani 1 1 d . B .
O8 O 0.3721(3) 0.8650(3) 0.51220(16) 0.0910(13) Uani 1 1 d . B .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.482(3) . ?
C1 C2 1.554(4) . ?
C1 C37 1.555(4) . ?
C1 H1 0.9800 . ?
C2 C3 1.509(4) . ?
C2 C30 1.552(4) . ?
C2 H2 0.9800 . ?
C3 C8 1.388(4) . ?
C3 C4 1.405(4) . ?
C4 C5 1.373(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.374(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.409(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.494(4) . ?
C9 N1 1.461(3) . ?
C9 C22 1.571(4) . ?
C9 H9 0.9800 . ?
C10 N1 1.474(3) . ?
C10 C11 1.518(4) . ?
C10 C23 1.547(4) . ?
C10 H10 0.9800 . ?
C11 O1 1.182(4) . ?
C11 O2 1.330(4) . ?
C12 O2 1.461(4) . ?
C12 C13 1.485(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 O3 1.211(3) . ?
C14 C15 1.471(4) . ?
C14 C22 1.537(4) . ?
C15 C16 1.393(4) . ?
C15 C20 1.395(4) . ?
C16 C17 1.374(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.405(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.381(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.388(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.488(4) . ?
C21 O4 1.216(3) . ?
C21 C22 1.534(4) . ?
C22 C23 1.552(4) . ?
C23 C24 1.507(4) . ?
C23 H23 0.9800 . ?
C24 C25 1.384(4) . ?
C24 C29 1.406(4) . ?
C25 C26 1.388(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.369(4) . ?
C26 Cl1 1.744(3) . ?
C27 C28 1.375(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.387(4) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 N2 1.477(4) . ?
C30 C31 1.507(4) . ?
C30 H30 0.9800 . ?
C31 C32 1.386(4) . ?
C31 C36 1.391(4) . ?
C32 C33 1.380(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.375(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.392(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.385(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.495(4) . ?
C37 C38 1.551(4) . ?
C37 H37 0.9800 . ?
C38 N2 1.469(4) . ?
C38 C51 1.566(4) . ?
C38 H38 0.9800 . ?
C39 N2 1.459(4) . ?
C39 C52 1.536(5) . ?
C39 C40' 1.543(10) . ?
C39 C40 1.690(13) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C40 O6 1.182(12) . ?
C40 O5 1.233(14) . ?
O5 C41 1.493(13) . ?
C41 C42 1.533(15) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C40' O6' 1.190(11) . ?
C40' O5' 1.350(12) . ?
O5' C41' 1.480(9) . ?
C41' C42' 1.528(9) . ?
C41' H41C 0.9700 . ?
C41' H41D 0.9700 . ?
C42' H42D 0.9600 . ?
C42' H42E 0.9600 . ?
C42' H42F 0.9600 . ?
C43 O7 1.207(4) . ?
C43 C44 1.378(6) . ?
C43 C51 1.532(5) . ?
C43 C44' 1.574(6) . ?
C44 C45 1.3900 . ?
C44 C49 1.3900 . ?
C45 C46 1.3900 . ?
C45 H45 0.9300 . ?
C46 C47 1.3900 . ?
C46 H46 0.9300 . ?
C47 C48 1.3900 . ?
C47 H47 0.9300 . ?
C48 C49 1.3900 . ?
C48 H48 0.9300 . ?
C49 C50 1.759(10) . ?
C44' C45' 1.3900 . ?
C44' C49' 1.3900 . ?
C45' C46' 1.3900 . ?
C45' H45' 0.9300 . ?
C46' C47' 1.3900 . ?
C46' H46' 0.9300 . ?
C47' C48' 1.3900 . ?
C47' H47' 0.9300 . ?
C48' C49' 1.3900 . ?
C48' H48' 0.9300 . ?
C49' C50 1.275(6) . ?
C50 O8 1.216(6) . ?
C50 C51 1.526(5) . ?
C51 C52 1.538(4) . ?
C52 C53 1.511(5) . ?
C52 H52 0.9800 . ?
C53 C58 1.382(5) . ?
C53 C54 1.393(5) . ?
C54 C55 1.378(4) . ?
C54 H54 0.9300 . ?
C55 C56 1.375(5) . ?
C55 Cl2 1.745(3) . ?
C56 C57 1.374(5) . ?
C56 H56 0.9300 . ?
C57 C58 1.393(5) . ?
C57 H57 0.9300 . ?
C58 H58 0.9300 . ?
C59 Cl4 1.744(5) . ?
C59 Cl3 1.764(6) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 114.5(2) . . ?
N1 C1 C37 107.9(2) . . ?
C2 C1 C37 109.0(2) . . ?
N1 C1 H1 108.4 . . ?
C2 C1 H1 108.4 . . ?
C37 C1 H1 108.4 . . ?
C3 C2 C30 112.6(2) . . ?
C3 C2 C1 117.0(2) . . ?
C30 C2 C1 107.9(2) . . ?
C3 C2 H2 106.2 . . ?
C30 C2 H2 106.2 . . ?
C1 C2 H2 106.2 . . ?
C8 C3 C4 118.0(3) . . ?
C8 C3 C2 122.0(2) . . ?
C4 C3 C2 120.0(2) . . ?
C5 C4 C3 121.6(3) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 119.8(3) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C6 C7 C8 120.5(3) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C3 C8 C7 120.0(3) . . ?
C3 C8 C9 121.6(2) . . ?
C7 C8 C9 118.2(2) . . ?
N1 C9 C8 114.9(2) . . ?
N1 C9 C22 105.2(2) . . ?
C8 C9 C22 118.9(2) . . ?
N1 C9 H9 105.6 . . ?
C8 C9 H9 105.6 . . ?
C22 C9 H9 105.6 . . ?
N1 C10 C11 111.6(2) . . ?
N1 C10 C23 106.9(2) . . ?
C11 C10 C23 109.2(2) . . ?
N1 C10 H10 109.7 . . ?
C11 C10 H10 109.7 . . ?
C23 C10 H10 109.7 . . ?
O1 C11 O2 123.5(3) . . ?
O1 C11 C10 125.9(3) . . ?
O2 C11 C10 110.5(2) . . ?
O2 C12 C13 106.3(4) . . ?
O2 C12 H12A 110.5 . . ?
C13 C12 H12A 110.5 . . ?
O2 C12 H12B 110.5 . . ?
C13 C12 H12B 110.5 . . ?
H12A C12 H12B 108.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O3 C14 C15 125.1(3) . . ?
O3 C14 C22 126.8(3) . . ?
C15 C14 C22 108.0(2) . . ?
C16 C15 C20 120.9(3) . . ?
C16 C15 C14 128.4(3) . . ?
C20 C15 C14 110.7(2) . . ?
C17 C16 C15 118.0(3) . . ?
C17 C16 H16 121.0 . . ?
C15 C16 H16 121.0 . . ?
C16 C17 C18 121.2(3) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C19 C18 C17 120.7(3) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 118.2(3) . . ?
C18 C19 H19 120.9 . . ?
C20 C19 H19 120.9 . . ?
C19 C20 C15 120.9(3) . . ?
C19 C20 C21 129.6(3) . . ?
C15 C20 C21 109.6(2) . . ?
O4 C21 C20 126.8(3) . . ?
O4 C21 C22 125.2(3) . . ?
C20 C21 C22 108.1(2) . . ?
C21 C22 C14 103.6(2) . . ?
C21 C22 C23 110.8(2) . . ?
C14 C22 C23 114.4(2) . . ?
C21 C22 C9 115.5(2) . . ?
C14 C22 C9 115.4(2) . . ?
C23 C22 C9 97.5(2) . . ?
C24 C23 C10 117.1(2) . . ?
C24 C23 C22 116.5(2) . . ?
C10 C23 C22 103.2(2) . . ?
C24 C23 H23 106.4 . . ?
C10 C23 H23 106.4 . . ?
C22 C23 H23 106.4 . . ?
C25 C24 C29 119.0(3) . . ?
C25 C24 C23 117.9(2) . . ?
C29 C24 C23 123.0(3) . . ?
C24 C25 C26 119.7(3) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C27 C26 C25 121.7(3) . . ?
C27 C26 Cl1 120.2(2) . . ?
C25 C26 Cl1 118.1(2) . . ?
C26 C27 C28 118.7(3) . . ?
C26 C27 H27 120.7 . . ?
C28 C27 H27 120.7 . . ?
C27 C28 C29 121.4(3) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C28 C29 C24 119.5(3) . . ?
C28 C29 H29 120.3 . . ?
C24 C29 H29 120.3 . . ?
N2 C30 C31 111.2(2) . . ?
N2 C30 C2 104.5(2) . . ?
C31 C30 C2 110.1(2) . . ?
N2 C30 H30 110.3 . . ?
C31 C30 H30 110.3 . . ?
C2 C30 H30 110.3 . . ?
C32 C31 C36 120.2(3) . . ?
C32 C31 C30 127.3(3) . . ?
C36 C31 C30 112.5(2) . . ?
C33 C32 C31 119.3(3) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C34 C33 C32 120.7(3) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C33 C34 C35 120.4(3) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C36 C35 C34 119.1(3) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C35 C36 C31 120.1(3) . . ?
C35 C36 C37 127.4(3) . . ?
C31 C36 C37 112.4(3) . . ?
C36 C37 C38 109.9(2) . . ?
C36 C37 C1 108.4(2) . . ?
C38 C37 C1 105.8(2) . . ?
C36 C37 H37 110.9 . . ?
C38 C37 H37 110.9 . . ?
C1 C37 H37 110.9 . . ?
N2 C38 C37 109.4(2) . . ?
N2 C38 C51 105.0(2) . . ?
C37 C38 C51 120.0(2) . . ?
N2 C38 H38 107.3 . . ?
C37 C38 H38 107.3 . . ?
C51 C38 H38 107.3 . . ?
N2 C39 C52 104.6(3) . . ?
N2 C39 C40' 111.1(5) . . ?
C52 C39 C40' 116.5(5) . . ?
N2 C39 C40 102.5(7) . . ?
C52 C39 C40 101.8(5) . . ?
C40' C39 C40 21.5(7) . . ?
N2 C39 H39A 115.4 . . ?
C52 C39 H39A 115.4 . . ?
C40' C39 H39A 94.2 . . ?
C40 C39 H39A 115.4 . . ?
N2 C39 H39B 106.4 . . ?
C52 C39 H39B 106.4 . . ?
C40' C39 H39B 111.2 . . ?
C40 C39 H39B 132.5 . . ?
H39A C39 H39B 17.1 . . ?
O6 C40 O5 133.7(13) . . ?
O6 C40 C39 127.1(10) . . ?
O5 C40 C39 99.0(10) . . ?
C40 O5 C41 102.4(11) . . ?
O5 C41 C42 103.0(10) . . ?
O5 C41 H41A 111.2 . . ?
C42 C41 H41A 111.2 . . ?
O5 C41 H41B 111.2 . . ?
C42 C41 H41B 111.2 . . ?
H41A C41 H41B 109.1 . . ?
O6' C40' O5' 117.0(8) . . ?
O6' C40' C39 125.8(10) . . ?
O5' C40' C39 114.9(7) . . ?
C40' O5' C41' 122.7(6) . . ?
O5' C41' C42' 104.7(6) . . ?
O5' C41' H41C 110.8 . . ?
C42' C41' H41C 110.8 . . ?
O5' C41' H41D 110.8 . . ?
C42' C41' H41D 110.8 . . ?
H41C C41' H41D 108.9 . . ?
C41' C42' H42D 109.5 . . ?
C41' C42' H42E 109.5 . . ?
H42D C42' H42E 109.5 . . ?
C41' C42' H42F 109.5 . . ?
H42D C42' H42F 109.5 . . ?
H42E C42' H42F 109.5 . . ?
O7 C43 C44 117.1(5) . . ?
O7 C43 C51 126.0(3) . . ?
C44 C43 C51 116.9(5) . . ?
O7 C43 C44' 135.2(4) . . ?
C44 C43 C44' 19.6(5) . . ?
C51 C43 C44' 98.2(3) . . ?
C43 C44 C45 133.3(6) . . ?
C43 C44 C49 106.7(6) . . ?
C45 C44 C49 120.0 . . ?
C44 C45 C46 120.0 . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C47 120.0 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 H46 120.0 . . ?
C48 C47 C46 120.0 . . ?
C48 C47 H47 120.0 . . ?
C46 C47 H47 120.0 . . ?
C49 C48 C47 120.0 . . ?
C49 C48 H48 120.0 . . ?
C47 C48 H48 120.0 . . ?
C48 C49 C44 120.0 . . ?
C48 C49 C50 130.2(4) . . ?
C44 C49 C50 109.8(4) . . ?
C45' C44' C49' 120.0 . . ?
C45' C44' C43 127.6(4) . . ?
C49' C44' C43 112.2(4) . . ?
C46' C45' C44' 120.0 . . ?
C46' C45' H45' 120.0 . . ?
C44' C45' H45' 120.0 . . ?
C47' C46' C45' 120.0 . . ?
C47' C46' H46' 120.0 . . ?
C45' C46' H46' 120.0 . . ?
C46' C47' C48' 120.0 . . ?
C46' C47' H47' 120.0 . . ?
C48' C47' H47' 120.0 . . ?
C47' C48' C49' 120.0 . . ?
C47' C48' H48' 120.0 . . ?
C49' C48' H48' 120.0 . . ?
C50 C49' C48' 131.6(4) . . ?
C50 C49' C44' 108.4(4) . . ?
C48' C49' C44' 120.0 . . ?
O8 C50 C49' 121.4(5) . . ?
O8 C50 C51 124.4(4) . . ?
C49' C50 C51 114.2(5) . . ?
O8 C50 C49 136.8(4) . . ?
C49' C50 C49 15.5(4) . . ?
C51 C50 C49 98.7(4) . . ?
C50 C51 C43 103.8(3) . . ?
C50 C51 C52 115.6(3) . . ?
C43 C51 C52 113.6(3) . . ?
C50 C51 C38 106.9(2) . . ?
C43 C51 C38 114.9(2) . . ?
C52 C51 C38 102.3(2) . . ?
C53 C52 C39 117.7(3) . . ?
C53 C52 C51 116.1(3) . . ?
C39 C52 C51 101.7(2) . . ?
C53 C52 H52 106.9 . . ?
C39 C52 H52 106.9 . . ?
C51 C52 H52 106.9 . . ?
C58 C53 C54 117.6(3) . . ?
C58 C53 C52 123.7(3) . . ?
C54 C53 C52 118.7(3) . . ?
C55 C54 C53 120.4(3) . . ?
C55 C54 H54 119.8 . . ?
C53 C54 H54 119.8 . . ?
C56 C55 C54 121.7(3) . . ?
C56 C55 Cl2 118.4(3) . . ?
C54 C55 Cl2 119.8(3) . . ?
C57 C56 C55 118.5(3) . . ?
C57 C56 H56 120.7 . . ?
C55 C56 H56 120.7 . . ?
C56 C57 C58 120.2(3) . . ?
C56 C57 H57 119.9 . . ?
C58 C57 H57 119.9 . . ?
C53 C58 C57 121.5(3) . . ?
C53 C58 H58 119.2 . . ?
C57 C58 H58 119.2 . . ?
Cl4 C59 Cl3 111.3(3) . . ?
Cl4 C59 H59A 109.4 . . ?
Cl3 C59 H59A 109.4 . . ?
Cl4 C59 H59B 109.4 . . ?
Cl3 C59 H59B 109.4 . . ?
H59A C59 H59B 108.0 . . ?
C9 N1 C10 106.7(2) . . ?
C9 N1 C1 120.7(2) . . ?
C10 N1 C1 111.1(2) . . ?
C39 N2 C38 110.2(2) . . ?
C39 N2 C30 116.5(3) . . ?
C38 N2 C30 111.9(2) . . ?
C11 O2 C12 116.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.655
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.110
####################################################################### 
# 
# 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_1p
_audit_block_doi                 10.5517/ccdc.csd.cc1ly3sf
_database_code_depnum_ccdc_archive 'CCDC 1487745'
_audit_update_record             
;
2016-06-27 deposited with the CCDC.
2016-12-12 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         'C60 H50 N2 O8'
_chemical_formula_sum            'C60 H50 N2 O8'
_chemical_formula_weight         927.02

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

_space_group_crystal_system      triclinic
_space_group_IT_number           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                   13.2141(7)
_cell_length_b                   14.5785(8)
_cell_length_c                   15.5709(9)
_cell_angle_alpha                86.9983(16)
_cell_angle_beta                 65.9210(15)
_cell_angle_gamma                64.2557(15)
_cell_volume                     2438.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7258
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      25.50

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.084
_shelx_estimated_absorpt_T_min   0.979
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30746
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.292
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             8483
_reflns_number_gt                5210
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0811P)²+1.3839P] 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         8483
_refine_ls_number_parameters     682
_refine_ls_number_restraints     156
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.1754
_refine_ls_wR_factor_gt          0.1570
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.072
_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 0.07564(19) 0.12972(16) 0.52630(18) 0.0256(6) Uani 1 1 d . . . . .
C2 C 0.0775(2) 0.10491(17) 0.61927(18) 0.0278(6) Uani 1 1 d . . . . .
C3 C 0.0176(2) 0.05566(19) 0.68423(19) 0.0382(7) Uani 1 1 d . . . . .
H3 H -0.0320 0.0330 0.6724 0.046 Uiso 1 1 calc R U . . .
C4 C 0.0339(3) 0.0414(2) 0.7668(2) 0.0463(9) Uani 1 1 d . . . . .
H4 H -0.0048 0.0080 0.8109 0.056 Uiso 1 1 calc R U . . .
C5 C 0.1074(3) 0.07613(19) 0.78538(19) 0.0416(8) Uani 1 1 d . . . . .
H5 H 0.1160 0.0664 0.8420 0.050 Uiso 1 1 calc R U . . .
C6 C 0.1673(2) 0.12464(18) 0.72058(17) 0.0323(7) Uani 1 1 d . . . . .
H6 H 0.2162 0.1479 0.7327 0.039 Uiso 1 1 calc R U . . .
C7 C 0.1526(2) 0.13776(17) 0.63678(17) 0.0251(6) Uani 1 1 d . . . . .
C8 C 0.21065(19) 0.18121(17) 0.55388(16) 0.0226(6) Uani 1 1 d . . . . .
C9 C 0.17083(18) 0.17008(16) 0.47720(16) 0.0208(6) Uani 1 1 d . . . . .
C10 C 0.28717(19) 0.09929(17) 0.38582(16) 0.0233(6) Uani 1 1 d . . . . .
H10 H 0.3556 0.1130 0.3808 0.028 Uiso 1 1 calc R U . . .
C11 C 0.33268(19) -0.01582(17) 0.38296(17) 0.0240(6) Uani 1 1 d . . . . .
C12 C 0.44258(19) -0.07630(17) 0.39027(16) 0.0233(6) Uani 1 1 d . . . . .
H12 H 0.4879 -0.0454 0.3971 0.028 Uiso 1 1 calc R U . . .
C13 C 0.4869(2) -0.18220(18) 0.38763(18) 0.0314(7) Uani 1 1 d . . . . .
H13 H 0.5619 -0.2209 0.3917 0.038 Uiso 1 1 calc R U . . .
C14 C 0.4215(2) -0.23104(18) 0.37907(19) 0.0341(7) Uani 1 1 d . . . . .
C15 C 0.4687(3) -0.34577(19) 0.3760(2) 0.0552(9) Uani 1 1 d . . . . .
H15A H 0.5531 -0.3802 0.3284 0.083 Uiso 1 1 calc R U . . .
H15B H 0.4178 -0.3667 0.3606 0.083 Uiso 1 1 calc R U . . .
H15C H 0.4655 -0.3635 0.4370 0.083 Uiso 1 1 calc R U . . .
C16 C 0.3111(2) -0.1706(2) 0.3726(2) 0.0475(8) Uani 1 1 d . . . . .
H16 H 0.2651 -0.2013 0.3668 0.057 Uiso 1 1 calc R U . . .
C17 C 0.2678(2) -0.06581(19) 0.3747(2) 0.0430(8) Uani 1 1 d . . . . .
H17 H 0.1930 -0.0274 0.3704 0.052 Uiso 1 1 calc R U . . .
C18 C 0.12164(18) 0.27177(16) 0.43508(16) 0.0196(6) Uani 1 1 d . . . . .
H18 H 0.1788 0.3014 0.4251 0.024 Uiso 1 1 calc R U . . .
C19 C -0.00610(18) 0.35435(16) 0.49709(16) 0.0205(6) Uani 1 1 d . . . . .
C20 C -0.0212(2) 0.41403(17) 0.57273(17) 0.0261(6) Uani 1 1 d . . . . .
H20 H 0.0477 0.4015 0.5834 0.031 Uiso 1 1 calc R U . . .
C21 C -0.1357(2) 0.49105(18) 0.63185(18) 0.0312(7) Uani 1 1 d . . . . .
H21 H -0.1448 0.5297 0.6825 0.037 Uiso 1 1 calc R U . . .
C22 C -0.2371(2) 0.50977(18) 0.61448(18) 0.0317(7) Uani 1 1 d . . . . .
H22 H -0.3151 0.5616 0.6539 0.038 Uiso 1 1 calc R U . . .
C23 C -0.2242(2) 0.45276(17) 0.53957(17) 0.0261(6) Uani 1 1 d . . . . .
H23 H -0.2935 0.4668 0.5289 0.031 Uiso 1 1 calc R U . . .
C24 C -0.10785(18) 0.37364(16) 0.47895(16) 0.0199(6) Uani 1 1 d . . . . .
C25 C -0.09690(18) 0.30917(16) 0.39948(16) 0.0199(6) Uani 1 1 d . . . . .
H25 H -0.1357 0.2649 0.4297 0.024 Uiso 1 1 calc R U . . .
C26 C 0.03767(18) 0.23665(16) 0.32654(16) 0.0203(6) Uani 1 1 d . . . . .
H26 H 0.0485 0.1658 0.3286 0.024 Uiso 1 1 calc R U . . .
C27 C 0.25357(19) 0.14353(18) 0.30219(17) 0.0282(6) Uani 1 1 d D . . . .
H27A H 0.2330 0.0953 0.2796 0.034 Uiso 0.402(2) 1 calc R U P A 1
H27B H 0.2394 0.0946 0.2735 0.034 Uiso 0.598(2) 1 calc R U P A 2
O3 O 0.4098(6) 0.0928(5) 0.1434(5) 0.103(2) Uani 0.402(2) 1 d . U P A 1
O4 O 0.3905(5) 0.2085(4) 0.2382(4) 0.0710(12) Uani 0.402(2) 1 d D U P A 1
C28 C 0.3589(7) 0.1482(7) 0.2186(6) 0.0655(15) Uani 0.402(2) 1 d D U P A 1
C29 C 0.4892(6) 0.2213(6) 0.1565(7) 0.0814(17) Uani 0.402(2) 1 d D U P A 1
H29A H 0.5276 0.1656 0.1049 0.098 Uiso 0.402(2) 1 calc R U P A 1
H29B H 0.5528 0.2166 0.1751 0.098 Uiso 0.402(2) 1 calc R U P A 1
C30 C 0.4409(8) 0.3227(7) 0.1214(7) 0.100(3) Uani 0.402(2) 1 d D U P A 1
H30A H 0.3857 0.3771 0.1748 0.150 Uiso 0.402(2) 1 calc R U P A 1
H30B H 0.3967 0.3202 0.0863 0.150 Uiso 0.402(2) 1 calc R U P A 1
H30C H 0.5093 0.3356 0.0809 0.150 Uiso 0.402(2) 1 calc R U P A 1
O3' O 0.4697(3) 0.0951(3) 0.2027(3) 0.0916(16) Uani 0.598(2) 1 d . U P A 2
O4' O 0.3425(3) 0.2501(3) 0.2078(3) 0.0805(11) Uani 0.598(2) 1 d D U P A 2
C28' C 0.3639(4) 0.1550(4) 0.2288(4) 0.0528(13) Uani 0.598(2) 1 d D U P A 2
C29' C 0.4456(6) 0.2729(5) 0.1375(5) 0.0939(15) Uani 0.598(2) 1 d D U P A 2
H29C H 0.4202 0.3464 0.1420 0.113 Uiso 0.598(2) 1 calc R U P A 2
H29D H 0.5205 0.2387 0.1474 0.113 Uiso 0.598(2) 1 calc R U P A 2
C30' C 0.4639(6) 0.2302(6) 0.0453(5) 0.115(2) Uani 0.598(2) 1 d D U P A 2
H30D H 0.5017 0.1564 0.0386 0.172 Uiso 0.598(2) 1 calc R U P A 2
H30E H 0.5171 0.2512 -0.0056 0.172 Uiso 0.598(2) 1 calc R U P A 2
H30F H 0.3850 0.2553 0.0429 0.172 Uiso 0.598(2) 1 calc R U P A 2
C31 C -0.01626(19) 0.33293(17) 0.05822(16) 0.0222(6) Uani 1 1 d . . . . .
C32 C 0.1130(2) 0.28405(17) -0.01642(16) 0.0246(6) Uani 1 1 d . . . . .
C33 C 0.1860(2) 0.3293(2) -0.07050(18) 0.0359(7) Uani 1 1 d . . . . .
H33 H 0.1548 0.4006 -0.0645 0.043 Uiso 1 1 calc R U . . .
C34 C 0.3065(3) 0.2656(2) -0.1336(2) 0.0495(9) Uani 1 1 d . . . . .
H34 H 0.3577 0.2943 -0.1703 0.059 Uiso 1 1 calc R U . . .
C35 C 0.3532(3) 0.1586(2) -0.1433(2) 0.0553(10) Uani 1 1 d . . . . .
H35 H 0.4352 0.1173 -0.1858 0.066 Uiso 1 1 calc R U . . .
C36 C 0.2795(2) 0.1132(2) -0.09087(18) 0.0404(8) Uani 1 1 d . . . . .
H36 H 0.3101 0.0420 -0.0982 0.049 Uiso 1 1 calc R U . . .
C37 C 0.1587(2) 0.17713(17) -0.02699(16) 0.0270(6) Uani 1 1 d . . . . .
C38 C 0.0607(2) 0.15108(17) 0.03833(16) 0.0247(6) Uani 1 1 d . . . . .
C39 C -0.04498(18) 0.24776(16) 0.10848(16) 0.0200(6) Uani 1 1 d . . . . .
C40 C -0.17976(18) 0.26630(17) 0.13891(16) 0.0227(6) Uani 1 1 d . . . . .
H40 H -0.1818 0.2010 0.1547 0.027 Uiso 1 1 calc R U . . .
C41 C -0.22867(19) 0.29749(18) 0.06347(17) 0.0270(6) Uani 1 1 d . . . . .
C42 C -0.2012(2) 0.2220(2) -0.0037(2) 0.0510(9) Uani 1 1 d . . . . .
H42 H -0.1577 0.1532 0.0005 0.061 Uiso 1 1 calc R U . . .
C43 C -0.2372(3) 0.2467(3) -0.0773(2) 0.0696(11) Uani 1 1 d . . . . .
H43 H -0.2167 0.1940 -0.1218 0.084 Uiso 1 1 calc R U . . .
C44 C -0.3029(2) 0.3479(3) -0.0859(2) 0.0582(10) Uani 1 1 d . . . . .
C45 C -0.3386(3) 0.3734(4) -0.1688(2) 0.0989(16) Uani 1 1 d . . . . .
H45A H -0.3918 0.3438 -0.1662 0.148 Uiso 1 1 calc R U . . .
H45B H -0.2649 0.3456 -0.2277 0.148 Uiso 1 1 calc R U . . .
H45C H -0.3816 0.4468 -0.1647 0.148 Uiso 1 1 calc R U . . .
C46 C -0.3331(2) 0.4226(2) -0.0180(2) 0.0541(8) Uani 1 1 d . . . . .
H46 H -0.3791 0.4912 -0.0212 0.065 Uiso 1 1 calc R U . . .
C47 C -0.2969(2) 0.3986(2) 0.0560(2) 0.0423(7) Uani 1 1 d . . . . .
H47 H -0.3190 0.4514 0.1011 0.051 Uiso 1 1 calc R U . . .
C48 C -0.16840(18) 0.37419(16) 0.34276(16) 0.0210(6) Uani 1 1 d . . . . .
H48 H -0.2547 0.4201 0.3862 0.025 Uiso 1 1 calc R U . . .
C49 C -0.10420(19) 0.43606(16) 0.28757(16) 0.0210(6) Uani 1 1 d . . . . .
C50 C -0.1524(2) 0.54220(17) 0.29558(18) 0.0322(6) Uani 1 1 d . . . . .
H50 H -0.2340 0.5840 0.3385 0.039 Uiso 1 1 calc R U . . .
C51 C -0.0779(2) 0.58551(19) 0.23902(19) 0.0429(7) Uani 1 1 d . . . . .
H51 H -0.1099 0.6568 0.2439 0.051 Uiso 1 1 calc R U . . .
C52 C 0.0430(2) 0.5240(2) 0.17575(19) 0.0437(7) Uani 1 1 d . . . . .
H52 H 0.0918 0.5540 0.1377 0.052 Uiso 1 1 calc R U . . .
C53 C 0.0925(2) 0.41771(19) 0.16827(17) 0.0317(6) Uani 1 1 d . . . . .
H53 H 0.1747 0.3764 0.1260 0.038 Uiso 1 1 calc R U . . .
C54 C 0.01860(18) 0.37336(16) 0.22444(16) 0.0218(6) Uani 1 1 d . . . . .
C55 C 0.05341(18) 0.26114(16) 0.22454(15) 0.0201(6) Uani 1 1 d . . . . .
H55 H 0.1389 0.2190 0.1774 0.024 Uiso 1 1 calc R U . . .
C56 C -0.03800(18) 0.23613(16) 0.20655(16) 0.0200(6) Uani 1 1 d . . . . .
H56 H -0.0177 0.1643 0.2157 0.024 Uiso 1 1 calc R U . . .
C57 C -0.24945(18) 0.33956(17) 0.23251(16) 0.0222(6) Uani 1 1 d . . . . .
H57 H -0.2633 0.4096 0.2199 0.027 Uiso 1 1 calc R U . . .
C58 C -0.37154(19) 0.34041(17) 0.30083(17) 0.0260(6) Uani 1 1 d . . . . .
C59 C -0.4661(2) 0.23335(18) 0.3731(2) 0.0348(7) Uani 1 1 d . . . . .
H59A H -0.5381 0.2600 0.3593 0.042 Uiso 1 1 calc R U . . .
H59B H -0.4898 0.2690 0.4342 0.042 Uiso 1 1 calc R U . . .
C60 C -0.4180(2) 0.11996(18) 0.3746(2) 0.0382(7) Uani 1 1 d . . . . .
H60A H -0.3982 0.0861 0.3146 0.057 Uiso 1 1 calc R U . . .
H60B H -0.4803 0.1067 0.4247 0.057 Uiso 1 1 calc R U . . .
H60C H -0.3445 0.0942 0.3854 0.057 Uiso 1 1 calc R U . . .
N1 N 0.13912(15) 0.24056(13) 0.34126(13) 0.0206(5) Uani 1 1 d . . . . .
N2 N -0.16433(14) 0.29968(13) 0.27913(13) 0.0194(5) Uani 1 1 d . . . . .
O1 O 0.00835(13) 0.12061(12) 0.49617(12) 0.0334(4) Uani 1 1 d . . . . .
O2 O 0.28075(13) 0.21732(12) 0.54636(11) 0.0318(4) Uani 1 1 d . . . . .
O5 O -0.08995(13) 0.42392(11) 0.07402(11) 0.0278(4) Uani 1 1 d . . . . .
O6 O 0.06344(15) 0.06605(12) 0.04012(12) 0.0345(5) Uani 1 1 d . . . . .
O7 O -0.45948(16) 0.41404(13) 0.35507(18) 0.0690(8) Uani 1 1 d . . . . .
O8 O -0.36567(14) 0.24731(12) 0.29929(13) 0.0376(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.216(3) . ?
C1 C2 1.481(4) . ?
C1 C9 1.525(3) . ?
C2 C3 1.389(4) . ?
C2 C7 1.391(4) . ?
C3 C4 1.378(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.478(3) . ?
C8 O2 1.216(3) . ?
C8 C9 1.528(3) . ?
C9 C10 1.563(3) . ?
C9 C18 1.568(3) . ?
C10 C11 1.513(3) . ?
C10 C27 1.563(3) . ?
C10 H10 0.9800 . ?
C11 C12 1.382(3) . ?
C11 C17 1.388(4) . ?
C12 C13 1.389(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(4) . ?
C13 H13 0.9300 . ?
C14 C16 1.381(4) . ?
C14 C15 1.505(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.375(4) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 N1 1.448(3) . ?
C18 C19 1.502(3) . ?
C18 H18 0.9800 . ?
C19 C24 1.393(3) . ?
C19 C20 1.396(3) . ?
C20 C21 1.376(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.383(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.377(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.405(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.514(3) . ?
C25 C48 1.545(3) . ?
C25 C26 1.554(3) . ?
C25 H25 0.9800 . ?
C26 N1 1.474(3) . ?
C26 C55 1.558(3) . ?
C26 H26 0.9800 . ?
C27 N1 1.463(3) . ?
C27 C28 1.493(7) . ?
C27 C28' 1.514(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
O3 C28 1.210(11) . ?
O4 C28 1.221(11) . ?
O4 C29 1.479(8) . ?
C29 C30 1.508(10) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
O3' C28' 1.181(6) . ?
O4' C28' 1.340(7) . ?
O4' C29' 1.518(7) . ?
C29' C30' 1.479(10) . ?
C29' H29C 0.9700 . ?
C29' H29D 0.9700 . ?
C30' H30D 0.9600 . ?
C30' H30E 0.9600 . ?
C30' H30F 0.9600 . ?
C31 O5 1.219(2) . ?
C31 C32 1.479(3) . ?
C31 C39 1.537(3) . ?
C32 C33 1.381(4) . ?
C32 C37 1.396(3) . ?
C33 C34 1.378(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.396(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.381(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.384(3) . ?
C36 H36 0.9300 . ?
C37 C38 1.472(3) . ?
C38 O6 1.224(3) . ?
C38 C39 1.529(3) . ?
C39 C40 1.542(3) . ?
C39 C56 1.563(3) . ?
C40 C41 1.521(3) . ?
C40 C57 1.525(3) . ?
C40 H40 0.9800 . ?
C41 C42 1.378(4) . ?
C41 C47 1.383(3) . ?
C42 C43 1.386(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.383(5) . ?
C43 H43 0.9300 . ?
C44 C46 1.364(4) . ?
C44 C45 1.523(5) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 C47 1.394(4) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 N2 1.477(3) . ?
C48 C49 1.503(3) . ?
C48 H48 0.9800 . ?
C49 C50 1.384(3) . ?
C49 C54 1.392(3) . ?
C50 C51 1.385(4) . ?
C50 H50 0.9300 . ?
C51 C52 1.375(3) . ?
C51 H51 0.9300 . ?
C52 C53 1.386(3) . ?
C52 H52 0.9300 . ?
C53 C54 1.389(3) . ?
C53 H53 0.9300 . ?
C54 C55 1.495(3) . ?
C55 C56 1.530(3) . ?
C55 H55 0.9800 . ?
C56 N2 1.466(2) . ?
C56 H56 0.9800 . ?
C57 N2 1.478(3) . ?
C57 C58 1.523(3) . ?
C57 H57 0.9800 . ?
C58 O7 1.194(3) . ?
C58 O8 1.326(3) . ?
C59 O8 1.445(3) . ?
C59 C60 1.494(3) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 125.5(2) . . ?
O1 C1 C9 126.8(2) . . ?
C2 C1 C9 107.7(2) . . ?
C3 C2 C7 120.9(3) . . ?
C3 C2 C1 128.8(3) . . ?
C7 C2 C1 110.3(2) . . ?
C4 C3 C2 118.0(3) . . ?
C4 C3 H3 121.0 . . ?
C2 C3 H3 121.0 . . ?
C3 C4 C5 121.3(3) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 120.7(3) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 118.2(3) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 H6 120.9 . . ?
C6 C7 C2 121.0(2) . . ?
C6 C7 C8 129.5(2) . . ?
C2 C7 C8 109.4(2) . . ?
O2 C8 C7 126.2(2) . . ?
O2 C8 C9 125.4(2) . . ?
C7 C8 C9 108.4(2) . . ?
C1 C9 C8 103.57(19) . . ?
C1 C9 C10 115.63(19) . . ?
C8 C9 C10 110.03(17) . . ?
C1 C9 C18 114.37(17) . . ?
C8 C9 C18 113.67(19) . . ?
C10 C9 C18 99.95(17) . . ?
C11 C10 C9 117.17(19) . . ?
C11 C10 C27 115.0(2) . . ?
C9 C10 C27 104.16(16) . . ?
C11 C10 H10 106.6 . . ?
C9 C10 H10 106.6 . . ?
C27 C10 H10 106.6 . . ?
C12 C11 C17 116.7(2) . . ?
C12 C11 C10 120.2(2) . . ?
C17 C11 C10 123.0(2) . . ?
C11 C12 C13 121.6(2) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C14 C13 C12 121.1(2) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C16 C14 C13 117.4(2) . . ?
C16 C14 C15 121.1(3) . . ?
C13 C14 C15 121.5(2) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C14 121.4(3) . . ?
C17 C16 H16 119.3 . . ?
C14 C16 H16 119.3 . . ?
C16 C17 C11 121.8(2) . . ?
C16 C17 H17 119.1 . . ?
C11 C17 H17 119.1 . . ?
N1 C18 C19 114.77(18) . . ?
N1 C18 C9 106.33(17) . . ?
C19 C18 C9 116.49(18) . . ?
N1 C18 H18 106.2 . . ?
C19 C18 H18 106.2 . . ?
C9 C18 H18 106.2 . . ?
C24 C19 C20 119.96(18) . . ?
C24 C19 C18 121.3(2) . . ?
C20 C19 C18 118.7(2) . . ?
C21 C20 C19 121.5(2) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C20 C21 C22 118.7(2) . . ?
C20 C21 H21 120.7 . . ?
C22 C21 H21 120.7 . . ?
C23 C22 C21 120.9(2) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 121.0(2) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C19 C24 C23 118.0(2) . . ?
C19 C24 C25 121.91(17) . . ?
C23 C24 C25 120.0(2) . . ?
C24 C25 C48 113.09(17) . . ?
C24 C25 C26 115.79(18) . . ?
C48 C25 C26 107.54(17) . . ?
C24 C25 H25 106.6 . . ?
C48 C25 H25 106.6 . . ?
C26 C25 H25 106.6 . . ?
N1 C26 C25 116.47(19) . . ?
N1 C26 C55 107.78(17) . . ?
C25 C26 C55 109.16(17) . . ?
N1 C26 H26 107.7 . . ?
C25 C26 H26 107.7 . . ?
C55 C26 H26 107.7 . . ?
N1 C27 C28 115.3(4) . . ?
N1 C27 C28' 113.7(3) . . ?
N1 C27 C10 108.16(17) . . ?
C28 C27 C10 113.9(4) . . ?
C28' C27 C10 107.4(3) . . ?
N1 C27 H27A 106.3 . . ?
C28 C27 H27A 106.3 . . ?
C10 C27 H27A 106.3 . . ?
N1 C27 H27B 109.2 . . ?
C28' C27 H27B 109.2 . . ?
C10 C27 H27B 109.2 . . ?
C28 O4 C29 114.3(7) . . ?
O3 C28 O4 125.6(7) . . ?
O3 C28 C27 122.3(8) . . ?
O4 C28 C27 111.9(7) . . ?
O4 C29 C30 112.7(6) . . ?
O4 C29 H29A 109.1 . . ?
C30 C29 H29A 109.1 . . ?
O4 C29 H29B 109.1 . . ?
C30 C29 H29B 109.1 . . ?
H29A C29 H29B 107.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28' O4' C29' 121.8(4) . . ?
O3' C28' O4' 115.4(5) . . ?
O3' C28' C27 126.4(5) . . ?
O4' C28' C27 116.4(3) . . ?
C30' C29' O4' 102.0(6) . . ?
C30' C29' H29C 111.4 . . ?
O4' C29' H29C 111.4 . . ?
C30' C29' H29D 111.4 . . ?
O4' C29' H29D 111.4 . . ?
H29C C29' H29D 109.2 . . ?
C29' C30' H30D 109.5 . . ?
C29' C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C29' C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
O5 C31 C32 126.3(2) . . ?
O5 C31 C39 125.55(19) . . ?
C32 C31 C39 108.08(17) . . ?
C33 C32 C37 121.1(2) . . ?
C33 C32 C31 129.4(2) . . ?
C37 C32 C31 109.5(2) . . ?
C34 C33 C32 117.9(2) . . ?
C34 C33 H33 121.0 . . ?
C32 C33 H33 121.0 . . ?
C33 C34 C35 121.1(3) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
C36 C35 C34 121.1(2) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C35 C36 C37 117.8(2) . . ?
C35 C36 H36 121.1 . . ?
C37 C36 H36 121.1 . . ?
C36 C37 C32 120.9(2) . . ?
C36 C37 C38 129.9(2) . . ?
C32 C37 C38 109.27(18) . . ?
O6 C38 C37 126.75(19) . . ?
O6 C38 C39 124.6(2) . . ?
C37 C38 C39 108.6(2) . . ?
C38 C39 C31 101.60(17) . . ?
C38 C39 C40 118.3(2) . . ?
C31 C39 C40 114.04(17) . . ?
C38 C39 C56 107.87(17) . . ?
C31 C39 C56 115.53(19) . . ?
C40 C39 C56 100.01(17) . . ?
C41 C40 C57 117.94(17) . . ?
C41 C40 C39 115.60(18) . . ?
C57 C40 C39 102.15(19) . . ?
C41 C40 H40 106.8 . . ?
C57 C40 H40 106.8 . . ?
C39 C40 H40 106.8 . . ?
C42 C41 C47 117.2(3) . . ?
C42 C41 C40 119.1(2) . . ?
C47 C41 C40 123.7(2) . . ?
C41 C42 C43 121.4(3) . . ?
C41 C42 H42 119.3 . . ?
C43 C42 H42 119.3 . . ?
C44 C43 C42 121.3(3) . . ?
C44 C43 H43 119.3 . . ?
C42 C43 H43 119.3 . . ?
C46 C44 C43 117.4(3) . . ?
C46 C44 C45 122.2(3) . . ?
C43 C44 C45 120.5(3) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 C47 121.7(3) . . ?
C44 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C41 C47 C46 121.0(3) . . ?
C41 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
N2 C48 C49 111.71(18) . . ?
N2 C48 C25 105.92(17) . . ?
C49 C48 C25 108.39(18) . . ?
N2 C48 H48 110.2 . . ?
C49 C48 H48 110.2 . . ?
C25 C48 H48 110.2 . . ?
C50 C49 C54 120.4(2) . . ?
C50 C49 C48 127.68(19) . . ?
C54 C49 C48 111.91(18) . . ?
C49 C50 C51 119.3(2) . . ?
C49 C50 H50 120.3 . . ?
C51 C50 H50 120.3 . . ?
C52 C51 C50 120.6(2) . . ?
C52 C51 H51 119.7 . . ?
C50 C51 H51 119.7 . . ?
C51 C52 C53 120.5(2) . . ?
C51 C52 H52 119.8 . . ?
C53 C52 H52 119.8 . . ?
C52 C53 C54 119.5(2) . . ?
C52 C53 H53 120.3 . . ?
C54 C53 H53 120.3 . . ?
C53 C54 C49 119.7(2) . . ?
C53 C54 C55 127.48(19) . . ?
C49 C54 C55 112.76(19) . . ?
C54 C55 C56 110.39(17) . . ?
C54 C55 C26 108.24(18) . . ?
C56 C55 C26 105.25(18) . . ?
C54 C55 H55 110.9 . . ?
C56 C55 H55 110.9 . . ?
C26 C55 H55 110.9 . . ?
N2 C56 C55 109.24(18) . . ?
N2 C56 C39 106.25(16) . . ?
C55 C56 C39 119.92(18) . . ?
N2 C56 H56 106.9 . . ?
C55 C56 H56 106.9 . . ?
C39 C56 H56 106.9 . . ?
N2 C57 C58 107.00(18) . . ?
N2 C57 C40 104.07(15) . . ?
C58 C57 C40 115.4(2) . . ?
N2 C57 H57 110.0 . . ?
C58 C57 H57 110.0 . . ?
C40 C57 H57 110.0 . . ?
O7 C58 O8 123.3(2) . . ?
O7 C58 C57 124.4(2) . . ?
O8 C58 C57 112.04(17) . . ?
O8 C59 C60 106.18(18) . . ?
O8 C59 H59A 110.5 . . ?
C60 C59 H59A 110.5 . . ?
O8 C59 H59B 110.5 . . ?
C60 C59 H59B 110.5 . . ?
H59A C59 H59B 108.7 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C18 N1 C27 106.59(17) . . ?
C18 N1 C26 120.95(16) . . ?
C27 N1 C26 112.11(18) . . ?
C56 N2 C48 112.23(17) . . ?
C56 N2 C57 108.76(17) . . ?
C48 N2 C57 117.89(16) . . ?
C58 O8 C59 117.63(17) . . ?

_refine_diff_density_max         0.775
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.055




#====================================================
####################################################################### 
# 
# 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_1e
_audit_block_doi                 10.5517/ccdc.csd.cc1ly3qc
_database_code_depnum_ccdc_archive 'CCDC 1487743'
_audit_update_record             
;
2016-06-27 deposited with the CCDC.
2016-12-12 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         'C58 H46 N2 O8, 2(C H2 Cl2)'
_chemical_formula_sum            'C60 H50 Cl4 N2 O8'
_chemical_formula_weight         1068.82

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'
Cl Cl 0.1484 0.1585 '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                   10.7475(5)
_cell_length_b                   15.2939(6)
_cell_length_c                   18.4528(8)
_cell_angle_alpha                106.4990(12)
_cell_angle_beta                 91.8576(13)
_cell_angle_gamma                101.3248(13)
_cell_volume                     2839.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9914
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      27.61

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.263
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39184
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.156
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             11054
_reflns_number_gt                8347
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1845P)²+4.9046P] 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         11054
_refine_ls_number_parameters     671
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.1027
_refine_ls_wR_factor_ref         0.3119
_refine_ls_wR_factor_gt          0.2952
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.108
_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 0.9081(3) 1.2519(2) 0.4057(2) 0.0246(8) Uani 1 1 d . . . . .
C2 C 0.9406(4) 1.3307(2) 0.4767(2) 0.0306(9) Uani 1 1 d . . . . .
C3 C 0.8699(5) 1.3958(3) 0.5100(3) 0.0448(12) Uani 1 1 d . . . . .
H3 H 0.7887 1.3932 0.4892 0.054 Uiso 1 1 calc R U . . .
C4 C 0.9261(7) 1.4656(3) 0.5760(3) 0.0618(18) Uani 1 1 d . . . . .
H4 H 0.8813 1.5103 0.5998 0.074 Uiso 1 1 calc R U . . .
C5 C 1.0468(7) 1.4697(3) 0.6069(3) 0.0588(16) Uani 1 1 d . . . . .
H5 H 1.0811 1.5169 0.6511 0.071 Uiso 1 1 calc R U . . .
C6 C 1.1166(6) 1.4062(3) 0.5740(2) 0.0464(12) Uani 1 1 d . . . . .
H6 H 1.1981 1.4099 0.5947 0.056 Uiso 1 1 calc R U . . .
C7 C 1.0621(4) 1.3354(2) 0.5081(2) 0.0311(9) Uani 1 1 d . . . . .
C8 C 1.1164(4) 1.2589(2) 0.4609(2) 0.0268(8) Uani 1 1 d . . . . .
C9 C 1.0167(3) 1.2008(2) 0.39530(19) 0.0204(7) Uani 1 1 d . . . . .
C10 C 1.0751(3) 1.1875(2) 0.31815(18) 0.0192(7) Uani 1 1 d . . . . .
H10 H 1.1591 1.1739 0.3257 0.023 Uiso 1 1 calc R U . . .
C11 C 1.0958(3) 1.2701(2) 0.28730(19) 0.0210(7) Uani 1 1 d . . . . .
C12 C 1.0006(4) 1.2895(3) 0.2442(2) 0.0296(8) Uani 1 1 d . . . . .
H12 H 0.9195 1.2511 0.2348 0.035 Uiso 1 1 calc R U . . .
C13 C 1.0258(5) 1.3650(3) 0.2154(2) 0.0375(10) Uani 1 1 d . . . . .
H13 H 0.9612 1.3760 0.1866 0.045 Uiso 1 1 calc R U . . .
C14 C 1.1453(5) 1.4247(3) 0.2286(2) 0.0405(11) Uani 1 1 d . . . . .
C15 C 1.1712(7) 1.5053(4) 0.1955(4) 0.0709(18) Uani 1 1 d . . . . .
H15A H 1.2615 1.5269 0.1966 0.106 Uiso 1 1 calc R U . . .
H15B H 1.1350 1.5551 0.2249 0.106 Uiso 1 1 calc R U . . .
H15C H 1.1335 1.4852 0.1440 0.106 Uiso 1 1 calc R U . . .
C16 C 1.2373(4) 1.4067(3) 0.2724(2) 0.0395(10) Uani 1 1 d . . . . .
H16 H 1.3173 1.4465 0.2831 0.047 Uiso 1 1 calc R U . . .
C17 C 1.2150(4) 1.3312(3) 0.3012(2) 0.0280(8) Uani 1 1 d . . . . .
H17 H 1.2802 1.3211 0.3302 0.034 Uiso 1 1 calc R U . . .
C18 C 0.9758(3) 1.0945(2) 0.39279(18) 0.0199(7) Uani 1 1 d . . . . .
H18 H 1.0550 1.0741 0.4000 0.024 Uiso 1 1 calc R U . . .
C19 C 0.8944(3) 1.0732(2) 0.45280(19) 0.0235(7) Uani 1 1 d . . . . .
C20 C 0.9480(4) 1.1038(3) 0.5283(2) 0.0316(9) Uani 1 1 d . . . . .
H20 H 1.0317 1.1376 0.5400 0.038 Uiso 1 1 calc R U . . .
C21 C 0.8779(5) 1.0843(3) 0.5857(2) 0.0412(11) Uani 1 1 d . . . . .
H21 H 0.9139 1.1056 0.6358 0.049 Uiso 1 1 calc R U . . .
C22 C 0.7541(5) 1.0330(3) 0.5679(2) 0.0462(12) Uani 1 1 d . . . . .
H22 H 0.7064 1.0192 0.6059 0.055 Uiso 1 1 calc R U . . .
C23 C 0.7016(4) 1.0021(3) 0.4934(2) 0.0360(10) Uani 1 1 d . . . . .
H23 H 0.6180 0.9681 0.4820 0.043 Uiso 1 1 calc R U . . .
C24 C 0.7711(4) 1.0208(2) 0.43471(19) 0.0241(7) Uani 1 1 d . . . . .
C25 C 0.7077(3) 0.9843(2) 0.35504(19) 0.0222(7) Uani 1 1 d . . . . .
H25 H 0.6312 1.0105 0.3562 0.027 Uiso 1 1 calc R U . . .
C26 C 0.7857(3) 1.0155(2) 0.29353(18) 0.0182(7) Uani 1 1 d . . . . .
H26 H 0.7546 1.0671 0.2829 0.022 Uiso 1 1 calc R U . . .
C27 C 0.9894(3) 1.0958(2) 0.26561(18) 0.0190(7) Uani 1 1 d . . . . .
H27 H 0.9261 1.1113 0.2346 0.023 Uiso 1 1 calc R U . . .
C28 C 1.0698(3) 1.0380(2) 0.2139(2) 0.0242(8) Uani 1 1 d . . . . .
C29 C 1.2299(4) 0.9508(3) 0.2095(3) 0.0422(11) Uani 1 1 d . . . . .
H29A H 1.1776 0.9035 0.1681 0.063 Uiso 1 1 calc R U . . .
H29B H 1.2677 0.9218 0.2419 0.063 Uiso 1 1 calc R U . . .
H29C H 1.2959 0.9874 0.1900 0.063 Uiso 1 1 calc R U . . .
C30 C 0.6377(3) 0.7636(2) 0.08547(18) 0.0182(7) Uani 1 1 d . . . . .
C31 C 0.6582(3) 0.7831(2) 0.0124(2) 0.0229(7) Uani 1 1 d . . . . .
C32 C 0.7344(4) 0.7470(3) -0.0430(2) 0.0317(9) Uani 1 1 d . . . . .
H32 H 0.7818 0.7044 -0.0367 0.038 Uiso 1 1 calc R U . . .
C33 C 0.7379(5) 0.7754(3) -0.1067(2) 0.0438(11) Uani 1 1 d . . . . .
H33 H 0.7905 0.7535 -0.1436 0.053 Uiso 1 1 calc R U . . .
C34 C 0.6635(5) 0.8370(3) -0.1175(2) 0.0437(11) Uani 1 1 d . . . . .
H34 H 0.6661 0.8538 -0.1621 0.052 Uiso 1 1 calc R U . . .
C35 C 0.5866(4) 0.8733(3) -0.0638(2) 0.0353(9) Uani 1 1 d . . . . .
H35 H 0.5374 0.9143 -0.0711 0.042 Uiso 1 1 calc R U . . .
C36 C 0.5855(3) 0.8458(2) 0.0024(2) 0.0236(7) Uani 1 1 d . . . . .
C37 C 0.5164(3) 0.8745(2) 0.0702(2) 0.0229(7) Uani 1 1 d . . . . .
C38 C 0.5534(3) 0.8272(2) 0.12822(19) 0.0195(7) Uani 1 1 d . . . . .
C39 C 0.4349(3) 0.7717(2) 0.1537(2) 0.0254(8) Uani 1 1 d . . . . .
H39 H 0.3761 0.8141 0.1673 0.031 Uiso 1 1 calc R U . . .
C40 C 0.3612(3) 0.6855(3) 0.0950(2) 0.0270(8) Uani 1 1 d . . . . .
C41 C 0.3942(4) 0.5990(3) 0.0765(2) 0.0300(8) Uani 1 1 d . . . . .
H41 H 0.4650 0.5913 0.1024 0.036 Uiso 1 1 calc R U . . .
C42 C 0.3223(4) 0.5240(3) 0.0196(2) 0.0359(9) Uani 1 1 d . . . . .
H42 H 0.3466 0.4668 0.0078 0.043 Uiso 1 1 calc R U . . .
C43 C 0.2155(4) 0.5321(3) -0.0198(3) 0.0427(11) Uani 1 1 d . . . . .
C44 C 0.1380(5) 0.4505(4) -0.0808(4) 0.0676(18) Uani 1 1 d . . . . .
H44A H 0.0490 0.4498 -0.0767 0.101 Uiso 1 1 calc R U . . .
H44B H 0.1559 0.3937 -0.0750 0.101 Uiso 1 1 calc R U . . .
H44C H 0.1595 0.4559 -0.1296 0.101 Uiso 1 1 calc R U . . .
C45 C 0.1840(5) 0.6179(4) -0.0016(3) 0.0565(15) Uani 1 1 d . . . . .
H45 H 0.1133 0.6253 -0.0279 0.068 Uiso 1 1 calc R U . . .
C46 C 0.2542(4) 0.6937(3) 0.0547(3) 0.0453(12) Uani 1 1 d . . . . .
H46 H 0.2297 0.7508 0.0658 0.054 Uiso 1 1 calc R U . . .
C47 C 0.6138(3) 0.9004(2) 0.20467(18) 0.0201(7) Uani 1 1 d . . . . .
H47 H 0.5815 0.9570 0.2083 0.024 Uiso 1 1 calc R U . . .
C48 C 0.7605(3) 0.9303(2) 0.21967(18) 0.0177(7) Uani 1 1 d . . . . .
H48 H 0.7984 0.9481 0.1769 0.021 Uiso 1 1 calc R U . . .
C49 C 0.8178(3) 0.8562(2) 0.23779(18) 0.0198(7) Uani 1 1 d . . . . .
C50 C 0.9137(3) 0.8175(2) 0.2027(2) 0.0238(7) Uani 1 1 d . . . . .
H50 H 0.9491 0.8362 0.1628 0.029 Uiso 1 1 calc R U . . .
C51 C 0.9571(4) 0.7497(3) 0.2276(2) 0.0317(9) Uani 1 1 d . . . . .
H51 H 1.0227 0.7239 0.2048 0.038 Uiso 1 1 calc R U . . .
C52 C 0.9024(4) 0.7209(3) 0.2863(2) 0.0369(10) Uani 1 1 d . . . . .
H52 H 0.9311 0.6752 0.3022 0.044 Uiso 1 1 calc R U . . .
C53 C 0.8054(4) 0.7594(3) 0.3217(2) 0.0319(9) Uani 1 1 d . . . . .
H53 H 0.7685 0.7395 0.3608 0.038 Uiso 1 1 calc R U . . .
C54 C 0.7644(4) 0.8281(2) 0.29791(19) 0.0250(8) Uani 1 1 d . . . . .
C55 C 0.6594(4) 0.8765(2) 0.32733(19) 0.0250(8) Uani 1 1 d . . . . .
H55 H 0.6227 0.8541 0.3684 0.030 Uiso 1 1 calc R U . . .
C56 C 0.4910(4) 0.7645(3) 0.2287(2) 0.0330(9) Uani 1 1 d . . . . .
H56 H 0.5470 0.7199 0.2212 0.040 Uiso 1 1 calc R U . . .
C57 C 0.3838(8) 0.7436(6) 0.2773(5) 0.0933(12) Uani 1 1 d . U . . .
C58 C 0.3156(8) 0.7017(6) 0.3811(5) 0.1014(15) Uani 1 1 d . U . . .
H58A H 0.3415 0.7496 0.4286 0.152 Uiso 1 1 calc R U . . .
H58B H 0.3022 0.6415 0.3895 0.152 Uiso 1 1 calc R U . . .
H58C H 0.2377 0.7093 0.3591 0.152 Uiso 1 1 calc R U . . .
C59 C 0.5027(9) 0.2180(9) 0.3956(6) 0.121(3) Uani 1 1 d . . . . .
H59A H 0.5671 0.2701 0.3914 0.145 Uiso 1 1 calc R U . . .
H59B H 0.4274 0.2415 0.4117 0.145 Uiso 1 1 calc R U . . .
C60 C 0.8473(7) 0.0680(4) 0.0263(4) 0.0685(16) Uani 1 1 d . . . . .
H60A H 0.8996 0.0279 0.0381 0.082 Uiso 1 1 calc R U . . .
H60B H 0.7961 0.0337 -0.0212 0.082 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5565(3) 0.1760(3) 0.4617(2) 0.1471(11) Uani 1 1 d . . . . .
Cl2 Cl 0.4656(4) 0.1377(3) 0.3091(2) 0.1735(16) Uani 1 1 d . . . . .
Cl3 Cl 0.74575(13) 0.09375(11) 0.09830(8) 0.0598(4) Uani 1 1 d . . . . .
Cl4 Cl 0.94548(16) 0.16619(13) 0.01494(10) 0.0794(5) Uani 1 1 d . . . . .
N1 N 0.9238(3) 1.04508(19) 0.31494(15) 0.0187(6) Uani 1 1 d . . . . .
N2 N 0.5594(3) 0.8611(2) 0.26514(16) 0.0251(7) Uani 1 1 d . . . . .
O1 O 0.8116(3) 1.23194(19) 0.36314(17) 0.0354(7) Uani 1 1 d . . . . .
O2 O 1.2211(3) 1.2451(2) 0.47142(17) 0.0398(7) Uani 1 1 d . . . . .
O3 O 1.0612(3) 1.0206(2) 0.14591(16) 0.0432(8) Uani 1 1 d . . . . .
O4 O 1.1525(3) 1.0105(2) 0.25266(15) 0.0341(7) Uani 1 1 d . . . . .
O5 O 0.6762(2) 0.70402(17) 0.10532(14) 0.0249(6) Uani 1 1 d . . . . .
O6 O 0.4419(3) 0.9254(2) 0.07941(17) 0.0362(7) Uani 1 1 d . . . . .
O7 O 0.2810(5) 0.7589(4) 0.2735(3) 0.0917(12) Uani 1 1 d . U . . .
O8 O 0.4192(5) 0.7090(4) 0.3272(3) 0.0965(11) Uani 1 1 d . 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 O1 1.213(5) . ?
C1 C2 1.482(5) . ?
C1 C9 1.517(5) . ?
C2 C3 1.388(6) . ?
C2 C7 1.391(6) . ?
C3 C4 1.396(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.362(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.396(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.480(5) . ?
C8 O2 1.205(5) . ?
C8 C9 1.527(5) . ?
C9 C10 1.551(5) . ?
C9 C18 1.585(4) . ?
C10 C11 1.509(5) . ?
C10 C27 1.555(4) . ?
C10 H10 0.9800 . ?
C11 C17 1.397(5) . ?
C11 C12 1.403(5) . ?
C12 C13 1.387(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.392(7) . ?
C13 H13 0.9300 . ?
C14 C16 1.375(7) . ?
C14 C15 1.508(6) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.386(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 N1 1.454(4) . ?
C18 C19 1.501(5) . ?
C18 H18 0.9800 . ?
C19 C24 1.383(5) . ?
C19 C20 1.400(5) . ?
C20 C21 1.387(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.381(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.399(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.502(5) . ?
C25 C55 1.555(5) . ?
C25 C26 1.559(4) . ?
C25 H25 0.9800 . ?
C26 N1 1.470(4) . ?
C26 C48 1.568(4) . ?
C26 H26 0.9800 . ?
C27 N1 1.468(4) . ?
C27 C28 1.522(5) . ?
C27 H27 0.9800 . ?
C28 O3 1.202(5) . ?
C28 O4 1.325(5) . ?
C29 O4 1.445(4) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 O5 1.210(4) . ?
C30 C31 1.476(5) . ?
C30 C38 1.532(4) . ?
C31 C32 1.388(5) . ?
C31 C36 1.396(5) . ?
C32 C33 1.365(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.399(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.376(7) . ?
C34 H34 0.9300 . ?
C35 C36 1.400(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.478(5) . ?
C37 O6 1.205(4) . ?
C37 C38 1.535(5) . ?
C38 C39 1.551(5) . ?
C38 C47 1.557(4) . ?
C39 C40 1.505(5) . ?
C39 C56 1.532(6) . ?
C39 H39 0.9800 . ?
C40 C41 1.388(6) . ?
C40 C46 1.396(6) . ?
C41 C42 1.390(5) . ?
C41 H41 0.9300 . ?
C42 C43 1.385(6) . ?
C42 H42 0.9300 . ?
C43 C45 1.371(7) . ?
C43 C44 1.499(6) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.384(6) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C47 N2 1.495(4) . ?
C47 C48 1.545(4) . ?
C47 H47 0.9800 . ?
C48 C49 1.501(5) . ?
C48 H48 0.9800 . ?
C49 C50 1.377(5) . ?
C49 C54 1.400(5) . ?
C50 C51 1.396(5) . ?
C50 H50 0.9300 . ?
C51 C52 1.388(6) . ?
C51 H51 0.9300 . ?
C52 C53 1.389(6) . ?
C52 H52 0.9300 . ?
C53 C54 1.387(5) . ?
C53 H53 0.9300 . ?
C54 C55 1.502(5) . ?
C55 N2 1.482(5) . ?
C55 H55 0.9800 . ?
C56 N2 1.467(5) . ?
C56 C57 1.524(7) . ?
C56 H56 0.9800 . ?
C57 O7 1.177(11) . ?
C57 O8 1.267(10) . ?
C58 O8 1.526(8) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 Cl1 1.668(11) . ?
C59 Cl2 1.694(11) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 Cl4 1.728(7) . ?
C60 Cl3 1.753(6) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 126.1(3) . . ?
O1 C1 C9 125.8(3) . . ?
C2 C1 C9 108.1(3) . . ?
C3 C2 C7 121.1(4) . . ?
C3 C2 C1 129.0(4) . . ?
C7 C2 C1 109.9(3) . . ?
C2 C3 C4 117.0(5) . . ?
C2 C3 H3 121.5 . . ?
C4 C3 H3 121.5 . . ?
C5 C4 C3 121.5(5) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C6 C5 C4 121.5(5) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C7 118.0(5) . . ?
C5 C6 H6 121.0 . . ?
C7 C6 H6 121.0 . . ?
C2 C7 C6 120.9(4) . . ?
C2 C7 C8 109.9(3) . . ?
C6 C7 C8 129.3(4) . . ?
O2 C8 C7 126.4(3) . . ?
O2 C8 C9 125.7(3) . . ?
C7 C8 C9 107.9(3) . . ?
C1 C9 C8 104.0(3) . . ?
C1 C9 C10 116.2(3) . . ?
C8 C9 C10 110.9(3) . . ?
C1 C9 C18 113.8(3) . . ?
C8 C9 C18 113.5(3) . . ?
C10 C9 C18 98.8(2) . . ?
C11 C10 C9 116.6(3) . . ?
C11 C10 C27 115.9(3) . . ?
C9 C10 C27 103.9(3) . . ?
C11 C10 H10 106.6 . . ?
C9 C10 H10 106.6 . . ?
C27 C10 H10 106.6 . . ?
C17 C11 C12 117.1(3) . . ?
C17 C11 C10 119.6(3) . . ?
C12 C11 C10 123.2(3) . . ?
C13 C12 C11 120.9(4) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 121.6(4) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C16 C14 C13 117.2(4) . . ?
C16 C14 C15 122.1(5) . . ?
C13 C14 C15 120.7(5) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 C17 122.3(4) . . ?
C14 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
C16 C17 C11 120.8(4) . . ?
C16 C17 H17 119.6 . . ?
C11 C17 H17 119.6 . . ?
N1 C18 C19 115.4(3) . . ?
N1 C18 C9 105.2(3) . . ?
C19 C18 C9 116.9(3) . . ?
N1 C18 H18 106.2 . . ?
C19 C18 H18 106.2 . . ?
C9 C18 H18 106.2 . . ?
C24 C19 C20 119.8(3) . . ?
C24 C19 C18 121.6(3) . . ?
C20 C19 C18 118.5(3) . . ?
C21 C20 C19 120.9(4) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C22 C21 C20 119.4(4) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C23 C22 C21 119.8(4) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 121.6(4) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C19 C24 C23 118.5(3) . . ?
C19 C24 C25 123.0(3) . . ?
C23 C24 C25 118.5(3) . . ?
C24 C25 C55 113.8(3) . . ?
C24 C25 C26 115.9(3) . . ?
C55 C25 C26 109.0(3) . . ?
C24 C25 H25 105.8 . . ?
C55 C25 H25 105.8 . . ?
C26 C25 H25 105.8 . . ?
N1 C26 C25 114.1(3) . . ?
N1 C26 C48 108.6(2) . . ?
C25 C26 C48 107.4(2) . . ?
N1 C26 H26 108.9 . . ?
C25 C26 H26 108.9 . . ?
C48 C26 H26 108.9 . . ?
N1 C27 C28 111.4(3) . . ?
N1 C27 C10 107.2(3) . . ?
C28 C27 C10 110.3(3) . . ?
N1 C27 H27 109.3 . . ?
C28 C27 H27 109.3 . . ?
C10 C27 H27 109.3 . . ?
O3 C28 O4 123.8(3) . . ?
O3 C28 C27 124.2(4) . . ?
O4 C28 C27 112.0(3) . . ?
O4 C29 H29A 109.5 . . ?
O4 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O4 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O5 C30 C31 125.0(3) . . ?
O5 C30 C38 126.8(3) . . ?
C31 C30 C38 108.1(3) . . ?
C32 C31 C36 120.8(3) . . ?
C32 C31 C30 128.9(3) . . ?
C36 C31 C30 110.3(3) . . ?
C33 C32 C31 118.3(4) . . ?
C33 C32 H32 120.8 . . ?
C31 C32 H32 120.8 . . ?
C32 C33 C34 121.0(4) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C35 C34 C33 121.8(4) . . ?
C35 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C34 C35 C36 117.1(4) . . ?
C34 C35 H35 121.4 . . ?
C36 C35 H35 121.4 . . ?
C31 C36 C35 120.9(4) . . ?
C31 C36 C37 109.6(3) . . ?
C35 C36 C37 129.5(4) . . ?
O6 C37 C36 127.0(3) . . ?
O6 C37 C38 124.6(3) . . ?
C36 C37 C38 108.4(3) . . ?
C30 C38 C37 103.2(3) . . ?
C30 C38 C39 112.3(3) . . ?
C37 C38 C39 112.0(3) . . ?
C30 C38 C47 116.7(3) . . ?
C37 C38 C47 111.4(3) . . ?
C39 C38 C47 101.6(3) . . ?
C40 C39 C56 119.9(3) . . ?
C40 C39 C38 116.4(3) . . ?
C56 C39 C38 100.8(3) . . ?
C40 C39 H39 106.2 . . ?
C56 C39 H39 106.2 . . ?
C38 C39 H39 106.2 . . ?
C41 C40 C46 117.7(3) . . ?
C41 C40 C39 124.7(3) . . ?
C46 C40 C39 117.6(3) . . ?
C40 C41 C42 120.5(4) . . ?
C40 C41 H41 119.7 . . ?
C42 C41 H41 119.7 . . ?
C43 C42 C41 121.7(4) . . ?
C43 C42 H42 119.1 . . ?
C41 C42 H42 119.1 . . ?
C45 C43 C42 117.4(4) . . ?
C45 C43 C44 121.2(4) . . ?
C42 C43 C44 121.3(4) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 C46 121.9(4) . . ?
C43 C45 H45 119.0 . . ?
C46 C45 H45 119.0 . . ?
C45 C46 C40 120.7(4) . . ?
C45 C46 H46 119.6 . . ?
C40 C46 H46 119.6 . . ?
N2 C47 C48 110.3(3) . . ?
N2 C47 C38 105.3(3) . . ?
C48 C47 C38 119.2(3) . . ?
N2 C47 H47 107.2 . . ?
C48 C47 H47 107.2 . . ?
C38 C47 H47 107.2 . . ?
C49 C48 C47 111.9(3) . . ?
C49 C48 C26 106.5(3) . . ?
C47 C48 C26 104.8(2) . . ?
C49 C48 H48 111.1 . . ?
C47 C48 H48 111.1 . . ?
C26 C48 H48 111.1 . . ?
C50 C49 C54 120.4(3) . . ?
C50 C49 C48 126.9(3) . . ?
C54 C49 C48 112.7(3) . . ?
C49 C50 C51 119.4(4) . . ?
C49 C50 H50 120.3 . . ?
C51 C50 H50 120.3 . . ?
C52 C51 C50 120.1(4) . . ?
C52 C51 H51 120.0 . . ?
C50 C51 H51 120.0 . . ?
C51 C52 C53 120.8(4) . . ?
C51 C52 H52 119.6 . . ?
C53 C52 H52 119.6 . . ?
C54 C53 C52 118.9(4) . . ?
C54 C53 H53 120.5 . . ?
C52 C53 H53 120.5 . . ?
C53 C54 C49 120.4(4) . . ?
C53 C54 C55 127.0(3) . . ?
C49 C54 C55 112.5(3) . . ?
N2 C55 C54 110.4(3) . . ?
N2 C55 C25 103.9(3) . . ?
C54 C55 C25 111.3(3) . . ?
N2 C55 H55 110.4 . . ?
C54 C55 H55 110.4 . . ?
C25 C55 H55 110.4 . . ?
N2 C56 C57 106.8(4) . . ?
N2 C56 C39 101.5(3) . . ?
C57 C56 C39 109.6(5) . . ?
N2 C56 H56 112.7 . . ?
C57 C56 H56 112.7 . . ?
C39 C56 H56 112.7 . . ?
O7 C57 O8 121.5(6) . . ?
O7 C57 C56 127.1(8) . . ?
O8 C57 C56 111.4(8) . . ?
O8 C58 H58A 109.5 . . ?
O8 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
O8 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
Cl1 C59 Cl2 113.3(7) . . ?
Cl1 C59 H59A 108.9 . . ?
Cl2 C59 H59A 108.9 . . ?
Cl1 C59 H59B 108.9 . . ?
Cl2 C59 H59B 108.9 . . ?
H59A C59 H59B 107.7 . . ?
Cl4 C60 Cl3 113.2(3) . . ?
Cl4 C60 H60A 108.9 . . ?
Cl3 C60 H60A 108.9 . . ?
Cl4 C60 H60B 108.9 . . ?
Cl3 C60 H60B 108.9 . . ?
H60A C60 H60B 107.7 . . ?
C18 N1 C27 107.8(2) . . ?
C18 N1 C26 121.7(3) . . ?
C27 N1 C26 112.2(3) . . ?
C56 N2 C55 117.0(3) . . ?
C56 N2 C47 108.0(3) . . ?
C55 N2 C47 110.3(3) . . ?
C28 O4 C29 117.2(3) . . ?
C57 O8 C58 109.4(7) . . ?

_refine_diff_density_max         2.376
_refine_diff_density_min         -1.576
_refine_diff_density_rms         0.119


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 420 159 ' '
_platon_squeeze_details          
; 
;



