# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2017

####################################################################### 
# 
# 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. 
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#######################################################################

data_exp_6568-sr
_database_code_depnum_ccdc_archive 'CCDC 1522610'
_audit_update_record             
;
2016-12-14 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_audit_creation_date             2016-01-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C76 H38 Br N O8'
_chemical_formula_sum            'C76 H38 Br N O8'
_chemical_formula_weight         1172.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C76 N1 O8 Br1'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.8397(9)
_cell_length_b                   24.2642(13)
_cell_length_c                   16.7166(13)
_cell_angle_alpha                90
_cell_angle_beta                 109.444(8)
_cell_angle_gamma                90
_cell_volume                     5293.4(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2689
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      24.1730
_cell_measurement_theta_min      3.3940
_shelx_estimated_absorpt_T_max   0.959
_shelx_estimated_absorpt_T_min   0.920
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1648
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            ?
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.072
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -20.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454  -99.0000   90.0000 72

#__ type_ start__ end____ width___ exp.time_
  2 omega  -12.00   77.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454   57.0000  -90.0000 89
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0127320000
_diffrn_orient_matrix_UB_12      -0.0271233000
_diffrn_orient_matrix_UB_13      -0.0158553000
_diffrn_orient_matrix_UB_21      0.0376119000
_diffrn_orient_matrix_UB_22      -0.0107809000
_diffrn_orient_matrix_UB_23      0.0366887000
_diffrn_orient_matrix_UB_31      -0.0370718000
_diffrn_orient_matrix_UB_32      -0.0016185000
_diffrn_orient_matrix_UB_33      0.0207163000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5220
_reflns_number_total             10314
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         10314
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0699
_refine_ls_restrained_S_all      0.925
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0705P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1714
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(C49) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(C57) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C63) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 1.02349(4) 0.03795(2) 0.61157(4) 0.03887(19) Uani 1 1 d . . . . .
C1 C 0.9703(3) 0.11220(18) 0.6111(3) 0.0281(12) Uani 1 1 d . . . . .
H1A H 0.9599 0.1196 0.6659 0.034 Uiso 1 1 calc R . . . .
H1B H 1.0205 0.1392 0.6043 0.034 Uiso 1 1 calc R . . . .
C2 C 1.0929(4) 0.2789(2) 0.3967(4) 0.0396(15) Uani 1 1 d . . . . .
C3 C 1.1869(5) 0.2738(3) 0.4758(5) 0.077(2) Uani 1 1 d . . . . .
H3A H 1.1701 0.2864 0.5253 0.116 Uiso 1 1 calc GR . . . .
H3B H 1.2424 0.2965 0.4693 0.116 Uiso 1 1 calc GR . . . .
H3C H 1.2090 0.2352 0.4837 0.116 Uiso 1 1 calc GR . . . .
C4 C 1.1213(5) 0.2680(3) 0.3185(4) 0.0604(19) Uani 1 1 d . . . . .
H4A H 1.1539 0.2318 0.3232 0.091 Uiso 1 1 calc GR . . . .
H4B H 1.1691 0.2965 0.3132 0.091 Uiso 1 1 calc GR . . . .
H4C H 1.0594 0.2688 0.2682 0.091 Uiso 1 1 calc GR . . . .
C5 C 1.0369(6) 0.3324(3) 0.3911(6) 0.090(3) Uani 1 1 d . U . . .
H5A H 0.9810 0.3344 0.3367 0.136 Uiso 1 1 calc GR . . . .
H5B H 1.0844 0.3630 0.3954 0.136 Uiso 1 1 calc GR . . . .
H5C H 1.0088 0.3347 0.4376 0.136 Uiso 1 1 calc GR . . . .
C6 C 0.7758(4) 0.44597(18) 0.4309(3) 0.0287(12) Uani 1 1 d . . . . .
C7 C 0.7140(4) 0.4816(2) 0.3574(4) 0.0401(15) Uani 1 1 d . . . . .
H7A H 0.7093 0.4635 0.3038 0.060 Uiso 1 1 calc GR . . . .
H7B H 0.7476 0.5175 0.3606 0.060 Uiso 1 1 calc GR . . . .
H7C H 0.6450 0.4870 0.3602 0.060 Uiso 1 1 calc GR . . . .
C8 C 0.8840(4) 0.4401(2) 0.4334(5) 0.0572(19) Uani 1 1 d . . . . .
H8A H 0.9218 0.4169 0.4817 0.086 Uiso 1 1 calc GR . . . .
H8B H 0.9162 0.4765 0.4396 0.086 Uiso 1 1 calc GR . . . .
H8C H 0.8852 0.4230 0.3806 0.086 Uiso 1 1 calc GR . . . .
C9 C 0.7695(5) 0.4684(2) 0.5131(4) 0.0553(18) Uani 1 1 d . . . . .
H9A H 0.6974 0.4712 0.5093 0.083 Uiso 1 1 calc GR . . . .
H9B H 0.8012 0.5050 0.5237 0.083 Uiso 1 1 calc GR . . . .
H9C H 0.8056 0.4436 0.5597 0.083 Uiso 1 1 calc GR . . . .
C10 C 0.5154(3) 0.36421(18) 0.6361(3) 0.0262(12) Uani 1 1 d . . . . .
C11 C 0.5700(4) 0.3730(2) 0.7311(4) 0.0422(15) Uani 1 1 d . . . . .
H11A H 0.5389 0.3493 0.7633 0.063 Uiso 1 1 calc GR . . . .
H11B H 0.5632 0.4117 0.7455 0.063 Uiso 1 1 calc GR . . . .
H11C H 0.6427 0.3638 0.7455 0.063 Uiso 1 1 calc GR . . . .
C12 C 0.4024(4) 0.3743(2) 0.6140(4) 0.0466(16) Uani 1 1 d . . . . .
H12A H 0.3686 0.3695 0.5528 0.070 Uiso 1 1 calc GR . . . .
H12B H 0.3910 0.4119 0.6302 0.070 Uiso 1 1 calc GR . . . .
H12C H 0.3738 0.3480 0.6446 0.070 Uiso 1 1 calc GR . . . .
C13 C 0.5613(4) 0.3988(2) 0.5825(4) 0.0424(15) Uani 1 1 d . . . . .
H13A H 0.6339 0.3895 0.5963 0.064 Uiso 1 1 calc GR . . . .
H13B H 0.5547 0.4379 0.5943 0.064 Uiso 1 1 calc GR . . . .
H13C H 0.5250 0.3914 0.5223 0.064 Uiso 1 1 calc GR . . . .
C14 C 0.8349(3) 0.07335(18) 0.7974(3) 0.0233(11) Uani 1 1 d . . . . .
C15 C 0.8051(4) 0.0972(2) 0.8682(4) 0.0440(15) Uani 1 1 d . . . . .
H15A H 0.8477 0.1295 0.8912 0.066 Uiso 1 1 calc GR . . . .
H15B H 0.8152 0.0696 0.9130 0.066 Uiso 1 1 calc GR . . . .
H15C H 0.7329 0.1082 0.8468 0.066 Uiso 1 1 calc GR . . . .
C16 C 0.7686(4) 0.0246(2) 0.7556(4) 0.0414(15) Uani 1 1 d . . . . .
H16A H 0.6965 0.0357 0.7355 0.062 Uiso 1 1 calc GR . . . .
H16B H 0.7785 -0.0054 0.7969 0.062 Uiso 1 1 calc GR . . . .
H16C H 0.7882 0.0119 0.7075 0.062 Uiso 1 1 calc GR . . . .
C17 C 0.9474(4) 0.0593(2) 0.8255(4) 0.0383(14) Uani 1 1 d . . . . .
H17A H 0.9642 0.0440 0.7775 0.057 Uiso 1 1 calc GR . . . .
H17B H 0.9631 0.0321 0.8713 0.057 Uiso 1 1 calc GR . . . .
H17C H 0.9879 0.0927 0.8458 0.057 Uiso 1 1 calc GR . . . .
C18 C 0.8381(3) 0.21980(17) 0.5006(3) 0.0178(10) Uani 1 1 d . . . . .
C19 C 0.7688(3) 0.25889(17) 0.5069(3) 0.0171(10) Uani 1 1 d . . . . .
C20 C 0.7161(3) 0.23650(16) 0.5576(3) 0.0151(10) Uani 1 1 d . . . . .
C21 C 0.7536(3) 0.18478(16) 0.5824(3) 0.0152(10) Uani 1 1 d . . . . .
C22 C 0.6987(3) 0.14053(17) 0.6127(3) 0.0173(10) Uani 1 1 d . . . . .
C23 C 0.7066(3) 0.08773(17) 0.5678(3) 0.0182(10) Uani 1 1 d . . . . .
C24 C 0.7825(3) 0.07796(16) 0.5348(3) 0.0186(10) Uani 1 1 d . . . . .
C25 C 0.8681(3) 0.11893(17) 0.5384(3) 0.0201(11) Uani 1 1 d . . . . .
C26 C 0.8722(3) 0.11423(18) 0.4484(3) 0.0179(10) Uani 1 1 d . . . . .
C27 C 0.8813(3) 0.15867(18) 0.4015(3) 0.0222(11) Uani 1 1 d . . . . .
C28 C 0.8857(3) 0.21752(19) 0.4331(3) 0.0243(11) Uani 1 1 d . . . . .
C29 C 0.8126(3) 0.24723(18) 0.3535(3) 0.0219(11) Uani 1 1 d . . . . .
C30 C 0.7415(3) 0.28578(17) 0.3587(3) 0.0208(11) Uani 1 1 d . . . . .
C31 C 0.7271(3) 0.30300(17) 0.4424(3) 0.0189(11) Uani 1 1 d . . . . .
C32 C 0.6104(3) 0.30263(16) 0.4170(3) 0.0205(11) Uani 1 1 d . . . . .
C33 C 0.5588(3) 0.28129(17) 0.4676(3) 0.0194(11) Uani 1 1 d . . . . .
C34 C 0.6103(3) 0.25511(17) 0.5543(3) 0.0192(11) Uani 1 1 d . . . . .
C35 C 0.5440(3) 0.20360(18) 0.5494(3) 0.0197(11) Uani 1 1 d . . . . .
C36 C 0.5835(3) 0.15289(18) 0.5769(3) 0.0206(11) Uani 1 1 d . . . . .
C37 C 0.5327(3) 0.10450(17) 0.5334(3) 0.0212(11) Uani 1 1 d . . . . .
C38 C 0.6074(3) 0.06489(17) 0.5282(3) 0.0193(11) Uani 1 1 d . . . . .
C39 C 0.5871(3) 0.03040(17) 0.4582(3) 0.0205(11) Uani 1 1 d . . . . .
C40 C 0.6667(4) 0.02029(17) 0.4236(3) 0.0219(11) Uani 1 1 d . . . . .
C41 C 0.7621(3) 0.04368(18) 0.4611(3) 0.0216(11) Uani 1 1 d . . . . .
C42 C 0.8166(3) 0.06663(18) 0.4080(3) 0.0205(11) Uani 1 1 d . . . . .
C43 C 0.7738(3) 0.06401(19) 0.3207(3) 0.0260(12) Uani 1 1 d . . . . .
C44 C 0.7815(3) 0.11125(19) 0.2697(3) 0.0240(11) Uani 1 1 d . . . . .
C45 C 0.8319(3) 0.15778(18) 0.3103(3) 0.0200(11) Uani 1 1 d . . . . .
C46 C 0.7909(3) 0.21156(19) 0.2821(3) 0.0219(11) Uani 1 1 d . . . . .
C47 C 0.7000(4) 0.21655(18) 0.2149(3) 0.0232(11) Uani 1 1 d . . . . .
C48 C 0.6252(4) 0.25652(18) 0.2188(3) 0.0255(12) Uani 1 1 d . . . . .
C49 C 0.6462(3) 0.28859(18) 0.2908(3) 0.0203(11) Uani 1 1 d . U . . .
C50 C 0.5655(4) 0.29915(17) 0.3258(3) 0.0230(11) Uani 1 1 d . . . . .
C51 C 0.4677(3) 0.27697(18) 0.2891(3) 0.0259(12) Uani 1 1 d . . . . .
C52 C 0.4143(3) 0.25455(18) 0.3408(3) 0.0237(11) Uani 1 1 d . . . . .
C53 C 0.4593(3) 0.25650(18) 0.4284(3) 0.0224(11) Uani 1 1 d . . . . .
C54 C 0.4518(3) 0.20872(18) 0.4793(3) 0.0206(11) Uani 1 1 d . . . . .
C55 C 0.3976(3) 0.16262(19) 0.4379(3) 0.0242(12) Uani 1 1 d . . . . .
C56 C 0.4392(3) 0.10893(18) 0.4660(3) 0.0214(11) Uani 1 1 d . . . . .
C57 C 0.4188(3) 0.07434(18) 0.3932(3) 0.0225(11) Uani 1 1 d . U . . .
C58 C 0.4911(3) 0.03554(17) 0.3885(3) 0.0227(11) Uani 1 1 d . . . . .
C59 C 0.5127(3) 0.02756(17) 0.3107(3) 0.0223(11) Uani 1 1 d . . . . .
C60 C 0.6210(3) 0.01775(17) 0.3315(3) 0.0222(11) Uani 1 1 d . . . . .
C61 C 0.6742(3) 0.03975(18) 0.2820(3) 0.0233(11) Uani 1 1 d . . . . .
C62 C 0.6195(4) 0.07205(18) 0.2072(3) 0.0239(11) Uani 1 1 d . . . . .
C63 C 0.6862(4) 0.11634(19) 0.2001(3) 0.0241(11) Uani 1 1 d . U . . .
C64 C 0.6462(4) 0.16769(19) 0.1727(3) 0.0236(11) Uani 1 1 d . . . . .
C65 C 0.5376(3) 0.17757(19) 0.1516(3) 0.0250(11) Uani 1 1 d . . . . .
C66 C 0.5251(3) 0.23232(18) 0.1805(3) 0.0230(11) Uani 1 1 d . . . . .
C67 C 0.4471(3) 0.24241(18) 0.2136(3) 0.0252(11) Uani 1 1 d . . . . .
C68 C 0.3802(3) 0.19860(19) 0.2220(3) 0.0274(12) Uani 1 1 d . . . . .
C69 C 0.3937(3) 0.14605(19) 0.1932(3) 0.0270(12) Uani 1 1 d . . . . .
C70 C 0.4740(3) 0.13522(19) 0.1582(3) 0.0247(12) Uani 1 1 d . . . . .
C71 C 0.5151(4) 0.08147(19) 0.1867(3) 0.0262(12) Uani 1 1 d . . . . .
C72 C 0.4611(3) 0.05841(19) 0.2393(3) 0.0259(12) Uani 1 1 d . . . . .
C73 C 0.3846(3) 0.09923(19) 0.2438(3) 0.0234(11) Uani 1 1 d . . . . .
C74 C 0.3651(3) 0.10661(19) 0.3183(3) 0.0252(12) Uani 1 1 d . . . . .
C75 C 0.3518(3) 0.16150(19) 0.3473(3) 0.0240(11) Uani 1 1 d . . . . .
C76 C 0.3602(3) 0.20665(19) 0.2997(3) 0.0239(12) Uani 1 1 d . . . . .
N1 N 0.8288(2) 0.17480(14) 0.5480(2) 0.0166(8) Uani 1 1 d . . . . .
O1 O 0.9876(2) 0.23933(13) 0.4665(2) 0.0279(8) Uani 1 1 d . . . . .
O2 O 1.0274(2) 0.23316(14) 0.3949(2) 0.0358(9) Uani 1 1 d . . . . .
O3 O 0.7741(2) 0.35427(11) 0.4770(2) 0.0254(8) Uani 1 1 d . . . . .
O4 O 0.7215(3) 0.39488(13) 0.4110(2) 0.0375(9) Uani 1 1 d . . . . .
O5 O 0.6219(2) 0.29051(12) 0.6260(2) 0.0218(7) Uani 1 1 d . . . . .
O6 O 0.5166(2) 0.30646(12) 0.6164(2) 0.0275(8) Uani 1 1 d . . . . .
O7 O 0.7238(2) 0.13631(12) 0.7025(2) 0.0223(7) Uani 1 1 d . . . . .
O8 O 0.8298(2) 0.11592(12) 0.7341(2) 0.0266(8) 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 C1 1.945(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C25 1.536(6) . ?
C2 C3 1.520(9) . ?
C2 C4 1.509(8) . ?
C2 C5 1.498(8) . ?
C2 O2 1.426(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.514(7) . ?
C6 C8 1.491(7) . ?
C6 C9 1.506(8) . ?
C6 O4 1.431(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.530(7) . ?
C10 C12 1.503(7) . ?
C10 C13 1.512(7) . ?
C10 O6 1.441(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.493(7) . ?
C14 C16 1.517(6) . ?
C14 C17 1.508(7) . ?
C14 O8 1.463(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.376(6) . ?
C18 C28 1.486(6) . ?
C18 N1 1.380(5) . ?
C19 C20 1.400(6) . ?
C19 C31 1.492(6) . ?
C20 C21 1.369(5) . ?
C20 C34 1.516(6) . ?
C21 C22 1.498(6) . ?
C21 N1 1.367(5) . ?
C22 C23 1.507(6) . ?
C22 C36 1.534(6) . ?
C22 O7 1.428(5) . ?
C23 C24 1.360(6) . ?
C23 C38 1.423(6) . ?
C24 C25 1.533(6) . ?
C24 C41 1.435(6) . ?
C25 C26 1.527(7) . ?
C25 N1 1.489(5) . ?
C26 C27 1.364(6) . ?
C26 C42 1.427(6) . ?
C27 C28 1.517(6) . ?
C27 C45 1.448(7) . ?
C28 C29 1.555(7) . ?
C28 O1 1.434(5) . ?
C29 C30 1.381(6) . ?
C29 C46 1.422(6) . ?
C30 C31 1.534(7) . ?
C30 C49 1.427(6) . ?
C31 C32 1.527(6) . ?
C31 O3 1.434(5) . ?
C32 C33 1.377(6) . ?
C32 C50 1.444(7) . ?
C33 C34 1.525(7) . ?
C33 C53 1.445(6) . ?
C34 C35 1.537(6) . ?
C34 O5 1.438(5) . ?
C35 C36 1.362(6) . ?
C35 C54 1.423(6) . ?
C36 C37 1.436(6) . ?
C37 C38 1.435(6) . ?
C37 C56 1.409(6) . ?
C38 C39 1.389(6) . ?
C39 C40 1.427(6) . ?
C39 C58 1.452(6) . ?
C40 C41 1.381(6) . ?
C40 C60 1.458(7) . ?
C41 C42 1.453(6) . ?
C42 C43 1.382(7) . ?
C43 C44 1.453(7) . ?
C43 C61 1.439(6) . ?
C44 C45 1.381(6) . ?
C44 C63 1.445(6) . ?
C45 C46 1.439(6) . ?
C46 C47 1.384(6) . ?
C47 C48 1.436(6) . ?
C47 C64 1.452(6) . ?
C48 C49 1.380(7) . ?
C48 C66 1.443(6) . ?
C49 C50 1.446(6) . ?
C50 C51 1.394(6) . ?
C51 C52 1.420(7) . ?
C51 C67 1.461(7) . ?
C52 C53 1.387(7) . ?
C52 C76 1.429(6) . ?
C53 C54 1.462(6) . ?
C54 C55 1.395(6) . ?
C55 C56 1.438(6) . ?
C55 C75 1.434(7) . ?
C56 C57 1.427(7) . ?
C57 C58 1.395(6) . ?
C57 C74 1.455(7) . ?
C58 C59 1.441(7) . ?
C59 C60 1.441(6) . ?
C59 C72 1.388(7) . ?
C60 C61 1.384(7) . ?
C61 C62 1.456(7) . ?
C62 C63 1.447(6) . ?
C62 C71 1.388(6) . ?
C63 C64 1.378(6) . ?
C64 C65 1.444(6) . ?
C65 C66 1.444(6) . ?
C65 C70 1.382(6) . ?
C66 C67 1.390(6) . ?
C67 C68 1.446(6) . ?
C68 C69 1.397(6) . ?
C68 C76 1.428(7) . ?
C69 C70 1.442(7) . ?
C69 C73 1.446(7) . ?
C70 C71 1.439(6) . ?
C71 C72 1.443(7) . ?
C72 C73 1.470(6) . ?
C73 C74 1.371(7) . ?
C74 C75 1.450(6) . ?
C75 C76 1.382(7) . ?
O1 O2 1.482(4) . ?
O3 O4 1.478(4) . ?
O5 O6 1.465(4) . ?
O7 O8 1.469(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 C1 H1A 109.6 . . ?
Br1 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C25 C1 Br1 110.4(3) . . ?
C25 C1 H1A 109.6 . . ?
C25 C1 H1B 109.6 . . ?
C4 C2 C3 110.1(5) . . ?
C5 C2 C3 113.6(6) . . ?
C5 C2 C4 112.0(6) . . ?
O2 C2 C3 108.0(5) . . ?
O2 C2 C4 101.2(4) . . ?
O2 C2 C5 111.1(5) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C8 C6 C7 111.6(5) . . ?
C8 C6 C9 111.8(5) . . ?
C9 C6 C7 110.2(4) . . ?
O4 C6 C7 101.2(4) . . ?
O4 C6 C8 111.6(4) . . ?
O4 C6 C9 109.9(4) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C11 110.2(4) . . ?
C12 C10 C13 111.8(4) . . ?
C13 C10 C11 112.2(4) . . ?
O6 C10 C11 109.5(4) . . ?
O6 C10 C12 101.0(4) . . ?
O6 C10 C13 111.5(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C16 112.6(4) . . ?
C15 C14 C17 111.7(4) . . ?
C17 C14 C16 111.7(4) . . ?
O8 C14 C15 109.8(4) . . ?
O8 C14 C16 110.0(4) . . ?
O8 C14 C17 100.4(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C28 125.4(4) . . ?
C19 C18 N1 107.6(4) . . ?
N1 C18 C28 123.8(4) . . ?
C18 C19 C20 107.1(4) . . ?
C18 C19 C31 123.5(4) . . ?
C20 C19 C31 124.2(4) . . ?
C19 C20 C34 123.7(4) . . ?
C21 C20 C19 108.5(4) . . ?
C21 C20 C34 123.3(4) . . ?
C20 C21 C22 125.1(4) . . ?
N1 C21 C20 107.5(4) . . ?
N1 C21 C22 123.9(3) . . ?
C21 C22 C23 108.1(4) . . ?
C21 C22 C36 107.9(3) . . ?
C23 C22 C36 102.1(4) . . ?
O7 C22 C21 115.7(4) . . ?
O7 C22 C23 115.5(4) . . ?
O7 C22 C36 106.4(3) . . ?
C24 C23 C22 123.0(4) . . ?
C24 C23 C38 120.0(4) . . ?
C38 C23 C22 110.1(4) . . ?
C23 C24 C25 124.3(4) . . ?
C23 C24 C41 119.4(4) . . ?
C41 C24 C25 109.7(4) . . ?
C24 C25 C1 117.2(4) . . ?
C26 C25 C1 116.5(4) . . ?
C26 C25 C24 101.2(4) . . ?
N1 C25 C1 106.5(3) . . ?
N1 C25 C24 106.8(3) . . ?
N1 C25 C26 108.0(4) . . ?
C27 C26 C25 123.2(4) . . ?
C27 C26 C42 120.4(4) . . ?
C42 C26 C25 109.6(4) . . ?
C26 C27 C28 123.0(4) . . ?
C26 C27 C45 119.5(4) . . ?
C45 C27 C28 109.3(4) . . ?
C18 C28 C27 108.8(4) . . ?
C18 C28 C29 107.8(4) . . ?
C27 C28 C29 101.5(4) . . ?
O1 C28 C18 108.5(4) . . ?
O1 C28 C27 113.8(3) . . ?
O1 C28 C29 116.0(4) . . ?
C30 C29 C28 122.2(4) . . ?
C30 C29 C46 120.6(4) . . ?
C46 C29 C28 109.3(4) . . ?
C29 C30 C31 123.6(4) . . ?
C29 C30 C49 118.1(4) . . ?
C49 C30 C31 110.3(4) . . ?
C19 C31 C30 109.1(3) . . ?
C19 C31 C32 108.4(4) . . ?
C32 C31 C30 101.0(4) . . ?
O3 C31 C19 108.4(4) . . ?
O3 C31 C30 115.2(3) . . ?
O3 C31 C32 114.4(3) . . ?
C33 C32 C31 123.3(4) . . ?
C33 C32 C50 119.8(4) . . ?
C50 C32 C31 109.8(4) . . ?
C32 C33 C34 124.5(4) . . ?
C32 C33 C53 119.3(4) . . ?
C53 C33 C34 109.3(4) . . ?
C20 C34 C33 107.4(4) . . ?
C20 C34 C35 108.2(3) . . ?
C33 C34 C35 101.9(4) . . ?
O5 C34 C20 108.0(3) . . ?
O5 C34 C33 115.5(3) . . ?
O5 C34 C35 115.4(4) . . ?
C36 C35 C34 123.5(4) . . ?
C36 C35 C54 120.4(4) . . ?
C54 C35 C34 109.2(4) . . ?
C35 C36 C22 123.8(4) . . ?
C35 C36 C37 119.6(4) . . ?
C37 C36 C22 107.9(4) . . ?
C38 C37 C36 109.7(4) . . ?
C56 C37 C36 120.5(4) . . ?
C56 C37 C38 119.4(4) . . ?
C23 C38 C37 108.3(4) . . ?
C39 C38 C23 121.3(4) . . ?
C39 C38 C37 120.5(4) . . ?
C38 C39 C40 118.6(4) . . ?
C38 C39 C58 119.9(4) . . ?
C40 C39 C58 108.2(4) . . ?
C39 C40 C60 108.3(4) . . ?
C41 C40 C39 119.7(4) . . ?
C41 C40 C60 120.7(4) . . ?
C24 C41 C42 108.0(4) . . ?
C40 C41 C24 120.9(4) . . ?
C40 C41 C42 119.5(4) . . ?
C26 C42 C41 109.2(4) . . ?
C43 C42 C26 120.7(4) . . ?
C43 C42 C41 120.0(4) . . ?
C42 C43 C44 119.6(4) . . ?
C42 C43 C61 120.2(4) . . ?
C61 C43 C44 107.8(4) . . ?
C45 C44 C43 118.7(4) . . ?
C45 C44 C63 120.2(4) . . ?
C63 C44 C43 108.3(4) . . ?
C44 C45 C27 120.9(4) . . ?
C44 C45 C46 120.1(4) . . ?
C46 C45 C27 109.2(4) . . ?
C29 C46 C45 109.1(4) . . ?
C47 C46 C29 120.5(4) . . ?
C47 C46 C45 119.9(4) . . ?
C46 C47 C48 119.8(4) . . ?
C46 C47 C64 120.2(4) . . ?
C48 C47 C64 108.2(4) . . ?
C47 C48 C66 107.8(4) . . ?
C49 C48 C47 118.3(4) . . ?
C49 C48 C66 120.6(4) . . ?
C30 C49 C50 108.7(4) . . ?
C48 C49 C30 122.5(4) . . ?
C48 C49 C50 119.0(4) . . ?
C32 C50 C49 108.5(4) . . ?
C51 C50 C32 120.1(4) . . ?
C51 C50 C49 121.4(4) . . ?
C50 C51 C52 120.3(4) . . ?
C50 C51 C67 119.0(4) . . ?
C52 C51 C67 108.3(4) . . ?
C51 C52 C76 108.3(4) . . ?
C53 C52 C51 119.2(4) . . ?
C53 C52 C76 121.0(4) . . ?
C33 C53 C54 107.9(4) . . ?
C52 C53 C33 121.2(4) . . ?
C52 C53 C54 119.5(4) . . ?
C35 C54 C53 109.3(4) . . ?
C55 C54 C35 121.7(4) . . ?
C55 C54 C53 118.6(4) . . ?
C54 C55 C56 118.3(4) . . ?
C54 C55 C75 120.9(4) . . ?
C75 C55 C56 108.4(4) . . ?
C37 C56 C55 119.4(4) . . ?
C37 C56 C57 120.4(4) . . ?
C57 C56 C55 108.1(4) . . ?
C56 C57 C74 108.5(4) . . ?
C58 C57 C56 120.2(4) . . ?
C58 C57 C74 119.0(5) . . ?
C57 C58 C39 119.6(4) . . ?
C57 C58 C59 120.6(4) . . ?
C59 C58 C39 107.7(4) . . ?
C60 C59 C58 108.4(4) . . ?
C72 C59 C58 120.1(4) . . ?
C72 C59 C60 119.5(4) . . ?
C59 C60 C40 107.4(4) . . ?
C61 C60 C40 118.9(4) . . ?
C61 C60 C59 120.7(4) . . ?
C43 C61 C62 108.2(4) . . ?
C60 C61 C43 120.7(4) . . ?
C60 C61 C62 119.5(4) . . ?
C63 C62 C61 107.9(4) . . ?
C71 C62 C61 120.1(4) . . ?
C71 C62 C63 119.8(4) . . ?
C44 C63 C62 107.8(4) . . ?
C64 C63 C44 120.2(4) . . ?
C64 C63 C62 120.1(4) . . ?
C63 C64 C47 119.5(4) . . ?
C63 C64 C65 120.1(4) . . ?
C65 C64 C47 107.9(4) . . ?
C66 C65 C64 107.6(4) . . ?
C70 C65 C64 119.7(4) . . ?
C70 C65 C66 120.4(4) . . ?
C48 C66 C65 108.6(4) . . ?
C67 C66 C48 120.6(4) . . ?
C67 C66 C65 119.4(4) . . ?
C66 C67 C51 119.4(4) . . ?
C66 C67 C68 121.1(4) . . ?
C68 C67 C51 106.6(4) . . ?
C69 C68 C67 118.3(4) . . ?
C69 C68 C76 121.8(5) . . ?
C76 C68 C67 108.2(4) . . ?
C68 C69 C70 121.0(4) . . ?
C68 C69 C73 117.9(5) . . ?
C70 C69 C73 108.8(4) . . ?
C65 C70 C69 119.7(4) . . ?
C65 C70 C71 120.6(4) . . ?
C71 C70 C69 107.7(4) . . ?
C62 C71 C70 119.7(4) . . ?
C62 C71 C72 119.5(5) . . ?
C70 C71 C72 109.0(4) . . ?
C59 C72 C71 120.7(4) . . ?
C59 C72 C73 119.5(5) . . ?
C71 C72 C73 107.3(4) . . ?
C69 C73 C72 107.2(4) . . ?
C74 C73 C69 120.7(4) . . ?
C74 C73 C72 119.8(4) . . ?
C73 C74 C57 120.9(4) . . ?
C73 C74 C75 120.6(4) . . ?
C75 C74 C57 106.9(4) . . ?
C55 C75 C74 108.1(4) . . ?
C76 C75 C55 120.1(4) . . ?
C76 C75 C74 119.4(5) . . ?
C68 C76 C52 108.6(4) . . ?
C75 C76 C52 119.8(5) . . ?
C75 C76 C68 119.6(4) . . ?
C18 N1 C25 123.4(4) . . ?
C21 N1 C18 109.3(3) . . ?
C21 N1 C25 124.3(3) . . ?
C28 O1 O2 103.2(3) . . ?
C2 O2 O1 108.0(3) . . ?
C31 O3 O4 103.4(3) . . ?
C6 O4 O3 108.2(3) . . ?
C34 O5 O6 103.6(3) . . ?
C10 O6 O5 108.6(3) . . ?
C22 O7 O8 105.5(3) . . ?
C14 O8 O7 107.5(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_details          
;
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.207 0.381 0.105 160 30 ' '
2 0.207 0.619 0.895 160 30 ' '
3 0.293 0.119 0.605 160 30 ' '
4 0.114 0.339 0.874 23 2 ' '
5 0.385 0.839 0.625 23 2 ' '
6 0.707 0.881 0.395 160 30 ' '
7 0.614 0.161 0.374 23 2 ' '
8 0.885 0.661 0.125 23 2 ' '

####################################################################### 
# 
# 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_test31
_database_code_depnum_ccdc_archive 'CCDC 1522611'
_audit_update_record             
;
2016-12-14 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H39 N O9'
_chemical_formula_weight         1110.08

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           orthorhombic
_symmetry_space_group_name_H-M   Pna21

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

_cell_length_a                   21.489(4)
_cell_length_b                   10.179(2)
_cell_length_c                   22.215(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4859.2(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    300
_cell_measurement_theta_min      2
_cell_measurement_theta_max      30

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2296
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_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  synchrotron
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27095
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         31.26
_reflns_number_total             14273
_reflns_number_gt                11323
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1172P)²+2.1081P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2.6(16)
_refine_ls_number_reflns         14273
_refine_ls_number_parameters     817
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1998
_refine_ls_wR_factor_gt          0.1822
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.005

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 0.36028(16) -0.1297(4) 0.15531(16) 0.0259(7) Uani 1 1 d . . .
C2 C 0.39178(19) -0.2179(4) 0.10750(18) 0.0401(7) Uani 1 1 d . . .
H2A H 0.3606 -0.2556 0.0819 0.060 Uiso 1 1 calc R . .
H2B H 0.4144 -0.2869 0.1272 0.060 Uiso 1 1 calc R . .
H2C H 0.4199 -0.1661 0.0838 0.060 Uiso 1 1 calc R . .
C3 C 0.3217(3) -0.2237(5) 0.1911(2) 0.0622(15) Uani 1 1 d . . .
H3A H 0.3046 -0.1793 0.2255 0.093 Uiso 1 1 calc R . .
H3B H 0.3473 -0.2955 0.2044 0.093 Uiso 1 1 calc R . .
H3C H 0.2885 -0.2568 0.1665 0.093 Uiso 1 1 calc R . .
C4 C 0.40850(16) -0.0628(4) 0.1952(2) 0.0321(8) Uani 1 1 d . . .
H4A H 0.4380 -0.0170 0.1705 0.048 Uiso 1 1 calc R . .
H4B H 0.4297 -0.1279 0.2188 0.048 Uiso 1 1 calc R . .
H4C H 0.3881 -0.0015 0.2215 0.048 Uiso 1 1 calc R . .
C5 C 0.36039(16) -0.1316(4) -0.14408(17) 0.0271(7) Uani 1 1 d . . .
C6 C 0.31609(15) -0.2160(4) -0.18298(15) 0.0318(7) Uani 1 1 d . . .
H6A H 0.2890 -0.2657 -0.1573 0.048 Uiso 1 1 calc R . .
H6B H 0.3401 -0.2749 -0.2075 0.048 Uiso 1 1 calc R . .
H6C H 0.2917 -0.1597 -0.2084 0.048 Uiso 1 1 calc R . .
C7 C 0.40849(17) -0.0602(4) -0.18380(19) 0.0296(8) Uani 1 1 d . . .
H7A H 0.3882 -0.0255 -0.2189 0.044 Uiso 1 1 calc R . .
H7B H 0.4403 -0.1209 -0.1959 0.044 Uiso 1 1 calc R . .
H7C H 0.4269 0.0104 -0.1614 0.044 Uiso 1 1 calc R . .
C8 C 0.3882(2) -0.1956(8) -0.0899(3) 0.109(3) Uani 1 1 d . . .
H8A H 0.3997 -0.1294 -0.0611 0.163 Uiso 1 1 calc R . .
H8B H 0.4244 -0.2445 -0.1015 0.163 Uiso 1 1 calc R . .
H8C H 0.3582 -0.2539 -0.0721 0.163 Uiso 1 1 calc R . .
C9 C 0.09294(16) -0.1287(4) -0.24144(14) 0.0240(6) Uani 1 1 d . . .
C10 C 0.04092(16) -0.2272(4) -0.22796(18) 0.0284(7) Uani 1 1 d . . .
H10A H 0.0417 -0.2498 -0.1860 0.043 Uiso 1 1 calc R . .
H10B H 0.0470 -0.3050 -0.2517 0.043 Uiso 1 1 calc R . .
H10C H 0.0014 -0.1887 -0.2377 0.043 Uiso 1 1 calc R . .
C11 C 0.0868(2) -0.0706(4) -0.30406(16) 0.0307(8) Uani 1 1 d . . .
H11A H 0.0481 -0.0240 -0.3071 0.046 Uiso 1 1 calc R . .
H11B H 0.0878 -0.1398 -0.3334 0.046 Uiso 1 1 calc R . .
H11C H 0.1206 -0.0111 -0.3113 0.046 Uiso 1 1 calc R . .
C12 C 0.15743(19) -0.1943(6) -0.2330(2) 0.0532(15) Uani 1 1 d . . .
H12A H 0.1894 -0.1287 -0.2357 0.080 Uiso 1 1 calc R . .
H12B H 0.1636 -0.2589 -0.2640 0.080 Uiso 1 1 calc R . .
H12C H 0.1592 -0.2360 -0.1943 0.080 Uiso 1 1 calc R . .
C13 C 0.09278(16) -0.1298(4) 0.25345(15) 0.0252(7) Uani 1 1 d . . .
C14 C 0.04132(16) -0.2260(4) 0.24058(16) 0.0253(6) Uani 1 1 d . . .
H14A H 0.0020 -0.1812 0.2413 0.038 Uiso 1 1 calc R . .
H14B H 0.0415 -0.2938 0.2706 0.038 Uiso 1 1 calc R . .
H14C H 0.0476 -0.2645 0.2016 0.038 Uiso 1 1 calc R . .
C15 C 0.08590(19) -0.0689(4) 0.31657(15) 0.0299(8) Uani 1 1 d . . .
H15A H 0.1165 -0.0012 0.3218 0.045 Uiso 1 1 calc R . .
H15B H 0.0918 -0.1357 0.3465 0.045 Uiso 1 1 calc R . .
H15C H 0.0451 -0.0318 0.3207 0.045 Uiso 1 1 calc R . .
C16 C 0.15697(18) -0.1875(5) 0.2457(2) 0.0466(12) Uani 1 1 d . . .
H16A H 0.1625 -0.2148 0.2047 0.070 Uiso 1 1 calc R . .
H16B H 0.1616 -0.2620 0.2718 0.070 Uiso 1 1 calc R . .
H16C H 0.1877 -0.1225 0.2556 0.070 Uiso 1 1 calc R . .
C17 C 0.12913(18) 0.0102(3) -0.04494(13) 0.0228(7) Uani 1 1 d . A .
C18 C 0.18982(15) 0.0064(3) -0.02627(14) 0.0189(5) Uani 1 1 d . . .
C19 C 0.18967(16) 0.0047(3) 0.03712(16) 0.0209(6) Uani 1 1 d . . .
C20 C 0.12869(18) 0.0109(3) 0.05600(14) 0.0236(7) Uani 1 1 d . A .
C21 C 0.1085(3) 0.0558(4) 0.11820(16) 0.0388(11) Uani 1 1 d . . .
C22 C 0.1635(3) 0.1442(4) 0.14334(16) 0.0423(11) Uani 1 1 d . . .
C23 C 0.2225(3) 0.1399(4) 0.12338(18) 0.0399(11) Uani 1 1 d . . .
C24 C 0.2454(2) 0.0428(4) 0.0752(2) 0.0319(8) Uani 1 1 d . . .
C25 C 0.28723(17) 0.1342(4) 0.0373(2) 0.0309(8) Uani 1 1 d . . .
C26 C 0.28735(16) 0.1324(4) -0.0244(2) 0.0356(9) Uani 1 1 d . . .
C27 C 0.2441(2) 0.0454(4) -0.0638(2) 0.0352(10) Uani 1 1 d . . .
C28 C 0.2223(2) 0.1393(4) -0.11291(17) 0.0370(10) Uani 1 1 d . . .
C29 C 0.1609(3) 0.1460(4) -0.13235(15) 0.0402(11) Uani 1 1 d . . .
C30 C 0.1089(2) 0.0561(4) -0.10768(15) 0.0375(10) Uani 1 1 d . . .
C31 C 0.0554(3) 0.1572(5) -0.10313(19) 0.0420(11) Uani 1 1 d . A .
C32 C 0.0743(3) 0.2738(5) -0.1312(2) 0.0529(15) Uani 1 1 d . . .
C33 C 0.1359(3) 0.2714(5) -0.14914(17) 0.0496(14) Uani 1 1 d . . .
C34 C 0.1734(3) 0.3829(5) -0.15069(17) 0.0497(14) Uani 1 1 d . . .
C35 C 0.2373(2) 0.3780(4) -0.12974(16) 0.0379(10) Uani 1 1 d . . .
C36 C 0.2597(2) 0.2595(4) -0.11006(17) 0.0389(10) Uani 1 1 d . . .
C37 C 0.2494(2) 0.4982(4) -0.09732(18) 0.0372(10) Uani 1 1 d . . .
C38 C 0.2883(2) 0.4946(4) -0.0474(2) 0.0335(9) Uani 1 1 d . . .
C39 C 0.31354(18) 0.3709(4) -0.0271(2) 0.0353(9) Uani 1 1 d . . .
C40 C 0.29833(19) 0.2547(4) -0.0581(2) 0.0396(10) Uani 1 1 d . . .
C41 C 0.31357(18) 0.3693(4) 0.0377(2) 0.0315(8) Uani 1 1 d . . .
C42 C 0.29978(17) 0.2526(4) 0.0682(2) 0.0328(8) Uani 1 1 d . . .
C43 C 0.2601(2) 0.2564(4) 0.12135(19) 0.0402(10) Uani 1 1 d . . .
C44 C 0.2349(3) 0.3777(4) 0.14171(17) 0.0457(12) Uani 1 1 d . A .
C45 C 0.2505(2) 0.4990(4) 0.10894(19) 0.0342(9) Uani 1 1 d . A .
C46 C 0.2877(2) 0.4950(4) 0.05793(18) 0.0294(8) Uani 1 1 d . . .
C47 C 0.27182(9) 0.57215(16) 0.0059(3) 0.0293(3) Uani 1 1 d . . .
C48 C 0.21817(10) 0.64978(16) 0.0055(3) 0.0315(4) Uani 1 1 d . . .
C49 C 0.1782(2) 0.6534(4) -0.0469(2) 0.0378(10) Uani 1 1 d . . .
C50 C 0.1952(2) 0.5789(4) -0.09768(19) 0.0362(9) Uani 1 1 d . . .
C51 C 0.1470(3) 0.5074(4) -0.1309(2) 0.0437(12) Uani 1 1 d . . .
C52 C 0.0863(3) 0.5120(5) -0.1123(3) 0.0567(16) Uani 1 1 d . A .
C53 C 0.0485(3) 0.3939(6) -0.1119(2) 0.0521(14) Uani 1 1 d . . .
C54 C 0.0087(2) 0.3945(5) -0.0586(3) 0.0568(17) Uani 1 1 d . . .
C55 C -0.00551(18) 0.2762(5) -0.0282(3) 0.0421(10) Uani 1 1 d . A .
C56 C 0.0132(3) 0.1510(5) -0.0558(2) 0.0528(14) Uani 1 1 d . . .
C57 C -0.0056(2) 0.2754(5) 0.0378(3) 0.0484(12) Uani 1 1 d . . .
C58 C 0.0125(3) 0.1580(5) 0.0677(3) 0.0553(14) Uani 1 1 d . A .
C59 C 0.0088(3) 0.3940(5) 0.0685(3) 0.0570(16) Uani 1 1 d . A .
C60 C 0.0213(2) 0.5144(5) 0.0348(4) 0.0584(17) Uani 1 1 d . . .
C61 C 0.0221(3) 0.5170(6) -0.0279(4) 0.0583(16) Uani 1 1 d . A .
C62 C 0.0692(2) 0.5903(5) -0.0594(3) 0.0561(16) Uani 1 1 d . . .
C63 C 0.1145(3) 0.6589(4) -0.0270(3) 0.0453(12) Uani 1 1 d . A .
C64 C 0.1141(3) 0.6588(4) 0.0390(3) 0.0490(13) Uani 1 1 d . . .
C65 C 0.0680(3) 0.5885(4) 0.0691(3) 0.0542(15) Uani 1 1 d . A .
C66 C 0.1786(2) 0.6535(4) 0.0594(2) 0.0355(9) Uani 1 1 d . A .
C67 C 0.1938(3) 0.5793(4) 0.10924(18) 0.0414(11) Uani 1 1 d . . .
C68 C 0.1461(3) 0.5077(5) 0.1419(2) 0.0529(15) Uani 1 1 d . A .
C69 C 0.1734(3) 0.3854(5) 0.16170(16) 0.0475(14) Uani 1 1 d . . .
C70 C 0.1375(3) 0.2681(5) 0.16194(16) 0.0472(13) Uani 1 1 d . A .
C71 C 0.0728(3) 0.2784(5) 0.1413(2) 0.0491(14) Uani 1 1 d . . .
C72 C 0.0466(3) 0.3945(5) 0.1219(3) 0.0598(18) Uani 1 1 d . A .
C73 C 0.0844(3) 0.5148(5) 0.1222(3) 0.0535(15) Uani 1 1 d . . .
C74 C 0.0549(3) 0.1551(5) 0.1137(2) 0.0460(13) Uani 1 1 d . A .
C75 C 0.0249(3) 0.0207(7) -0.0160(3) 0.0217(16) Uani 0.495(10) 1 d P A 1
C76 C -0.0137(3) 0.0318(8) 0.0395(5) 0.037(2) Uani 0.495(10) 1 d P A 1
H76C H -0.0080 -0.0434 0.0657 0.045 Uiso 0.495(10) 1 calc PR A 1
H76D H -0.0576 0.0408 0.0299 0.045 Uiso 0.495(10) 1 calc PR A 1
C75B C 0.0228(4) 0.0213(9) 0.0268(4) 0.033(2) Uani 0.505(10) 1 d P A 2
C76B C -0.0154(3) 0.0354(10) -0.0278(4) 0.037(2) Uani 0.505(10) 1 d P A 2
H76A H -0.0122 -0.0413 -0.0535 0.044 Uiso 0.505(10) 1 calc PR A 2
H76B H -0.0588 0.0510 -0.0180 0.044 Uiso 0.505(10) 1 calc PR A 2
N1 N 0.09134(6) 0.00845(13) 0.0056(2) 0.0219(2) Uani 1 1 d . . .
O1 O 0.2728(2) -0.0724(3) 0.0973(2) 0.0588(13) Uani 1 1 d . . .
O2 O 0.3256(2) -0.0219(3) 0.1335(3) 0.0719(17) Uani 1 1 d . . .
O3 O 0.2729(2) -0.0735(3) -0.0860(2) 0.0587(13) Uani 1 1 d . . .
O4 O 0.3239(2) -0.0208(3) -0.1255(2) 0.0686(15) Uani 1 1 d . . .
O5 O 0.08508(17) -0.0147(3) -0.20305(11) 0.0346(7) Uani 1 1 d . . .
O6 O 0.09590(19) -0.0630(3) -0.14049(12) 0.0443(9) Uani 1 1 d . . .
O7 O 0.09554(19) -0.0588(3) 0.15240(12) 0.0437(9) Uani 1 1 d . . .
O8 O 0.08447(17) -0.0138(3) 0.21485(12) 0.0350(7) Uani 1 1 d . . .
O9 O 0.0040(3) -0.0921(6) -0.0472(3) 0.0326(16) Uani 0.495(10) 1 d P A 1
H9 H 0.0278 -0.1082 -0.0751 0.049 Uiso 0.495(10) 1 calc PR A 1
O9B O 0.0051(3) -0.0905(6) 0.0593(3) 0.0381(18) Uani 0.505(10) 1 d P A 2
H9B H 0.0203 -0.0873 0.0931 0.057 Uiso 0.505(10) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.412(4) . ?
C1 C3 1.496(6) . ?
C1 C4 1.524(5) . ?
C1 C2 1.547(5) . ?
C5 O4 1.435(5) . ?
C5 C8 1.493(6) . ?
C5 C7 1.541(5) . ?
C5 C6 1.546(5) . ?
C9 O5 1.450(5) . ?
C9 C11 1.518(5) . ?
C9 C10 1.532(5) . ?
C9 C12 1.550(6) . ?
C13 O8 1.470(5) . ?
C13 C14 1.505(5) . ?
C13 C16 1.509(5) . ?
C13 C15 1.540(5) . ?
C17 C18 1.369(5) . ?
C17 N1 1.386(5) . ?
C17 C30 1.533(5) . ?
C18 C19 1.408(2) . ?
C18 C27 1.487(4) . ?
C19 C20 1.377(5) . ?
C19 C24 1.517(5) . ?
C20 N1 1.377(5) . ?
C20 C21 1.518(5) . ?
C21 O7 1.420(4) . ?
C21 C74 1.537(8) . ?
C21 C22 1.587(6) . ?
C22 C23 1.343(8) . ?
C22 C70 1.440(7) . ?
C23 C43 1.435(5) . ?
C23 C24 1.538(7) . ?
C24 O1 1.400(5) . ?
C24 C25 1.544(6) . ?
C25 C26 1.370(3) . ?
C25 C42 1.412(6) . ?
C26 C40 1.472(6) . ?
C26 C27 1.553(6) . ?
C27 O3 1.446(4) . ?
C27 C28 1.525(7) . ?
C28 C29 1.389(8) . ?
C28 C36 1.465(5) . ?
C29 C33 1.434(7) . ?
C29 C30 1.545(6) . ?
C30 O6 1.442(4) . ?
C30 C31 1.547(8) . ?
C31 C56 1.390(8) . ?
C31 C32 1.401(6) . ?
C32 C33 1.382(9) . ?
C32 C53 1.410(9) . ?
C33 C34 1.392(6) . ?
C34 C35 1.450(8) . ?
C34 C51 1.456(8) . ?
C35 C36 1.370(7) . ?
C35 C37 1.444(6) . ?
C36 C40 1.423(8) . ?
C37 C38 1.390(7) . ?
C37 C50 1.427(7) . ?
C38 C39 1.443(6) . ?
C38 C47 1.465(6) . ?
C39 C40 1.407(6) . ?
C39 C41 1.441(3) . ?
C41 C42 1.398(6) . ?
C41 C46 1.465(6) . ?
C42 C43 1.458(7) . ?
C43 C44 1.422(7) . ?
C44 C69 1.398(8) . ?
C44 C45 1.472(5) . ?
C45 C46 1.388(7) . ?
C45 C67 1.468(7) . ?
C46 C47 1.439(6) . ?
C47 C48 1.398(3) . ?
C48 C49 1.447(7) . ?
C48 C66 1.467(7) . ?
C49 C50 1.408(7) . ?
C49 C63 1.437(8) . ?
C50 C51 1.465(6) . ?
C51 C52 1.369(9) . ?
C52 C53 1.450(7) . ?
C52 C62 1.466(10) . ?
C53 C54 1.460(10) . ?
C54 C55 1.414(7) . ?
C54 C61 1.450(9) . ?
C55 C57 1.468(4) . ?
C55 C56 1.470(8) . ?
C56 C76B 1.466(11) . ?
C56 C75 1.613(9) . ?
C57 C59 1.420(8) . ?
C57 C58 1.421(8) . ?
C58 C74 1.368(9) . ?
C58 C76 1.537(10) . ?
C58 C75B 1.678(10) . ?
C59 C72 1.439(11) . ?
C59 C60 1.461(9) . ?
C60 C61 1.394(5) . ?
C60 C65 1.470(9) . ?
C61 C62 1.439(9) . ?
C62 C63 1.398(8) . ?
C63 C64 1.465(4) . ?
C64 C65 1.393(8) . ?
C64 C66 1.460(8) . ?
C65 C73 1.441(10) . ?
C66 C67 1.380(7) . ?
C67 C68 1.452(6) . ?
C68 C73 1.398(9) . ?
C68 C69 1.444(9) . ?
C69 C70 1.421(6) . ?
C70 C71 1.469(9) . ?
C71 C72 1.378(9) . ?
C71 C74 1.449(6) . ?
C72 C73 1.469(7) . ?
C75 O9 1.415(9) . ?
C75 C76 1.491(12) . ?
C75 N1 1.511(7) . ?
C75B O9B 1.400(10) . ?
C75B C76B 1.471(12) . ?
C75B N1 1.552(8) . ?
O1 O2 1.483(4) . ?
O3 O4 1.504(4) . ?
O5 O6 1.492(3) . ?
O7 O8 1.480(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 C3 112.8(4) . . ?
O2 C1 C4 102.2(3) . . ?
C3 C1 C4 110.7(3) . . ?
O2 C1 C2 116.5(4) . . ?
C3 C1 C2 103.6(3) . . ?
C4 C1 C2 111.2(3) . . ?
O4 C5 C8 109.2(5) . . ?
O4 C5 C7 99.2(3) . . ?
C8 C5 C7 113.5(3) . . ?
O4 C5 C6 105.2(4) . . ?
C8 C5 C6 117.0(4) . . ?
C7 C5 C6 110.8(3) . . ?
O5 C9 C11 102.5(3) . . ?
O5 C9 C10 108.9(3) . . ?
C11 C9 C10 111.8(3) . . ?
O5 C9 C12 112.2(4) . . ?
C11 C9 C12 110.9(3) . . ?
C10 C9 C12 110.3(3) . . ?
O8 C13 C14 108.8(3) . . ?
O8 C13 C16 110.9(4) . . ?
C14 C13 C16 113.3(4) . . ?
O8 C13 C15 101.3(3) . . ?
C14 C13 C15 111.4(3) . . ?
C16 C13 C15 110.4(3) . . ?
C18 C17 N1 108.2(3) . . ?
C18 C17 C30 123.6(3) . . ?
N1 C17 C30 125.1(4) . . ?
C17 C18 C19 107.5(3) . . ?
C17 C18 C27 124.8(3) . . ?
C19 C18 C27 124.4(4) . . ?
C20 C19 C18 107.8(3) . . ?
C20 C19 C24 124.7(3) . . ?
C18 C19 C24 123.6(4) . . ?
C19 C20 N1 107.8(3) . . ?
C19 C20 C21 124.2(4) . . ?
N1 C20 C21 125.4(4) . . ?
O7 C21 C20 107.2(3) . . ?
O7 C21 C74 115.3(4) . . ?
C20 C21 C74 110.6(4) . . ?
O7 C21 C22 115.1(4) . . ?
C20 C21 C22 106.2(3) . . ?
C74 C21 C22 102.1(4) . . ?
C23 C22 C70 119.3(4) . . ?
C23 C22 C21 124.6(4) . . ?
C70 C22 C21 108.0(5) . . ?
C22 C23 C43 121.0(5) . . ?
C22 C23 C24 123.5(4) . . ?
C43 C23 C24 109.2(4) . . ?
O1 C24 C19 108.2(3) . . ?
O1 C24 C23 115.5(4) . . ?
C19 C24 C23 107.4(3) . . ?
O1 C24 C25 116.9(4) . . ?
C19 C24 C25 108.0(3) . . ?
C23 C24 C25 100.3(3) . . ?
C26 C25 C42 119.8(5) . . ?
C26 C25 C24 122.6(4) . . ?
C42 C25 C24 111.1(4) . . ?
C25 C26 C40 119.8(5) . . ?
C25 C26 C27 124.8(4) . . ?
C40 C26 C27 106.9(4) . . ?
O3 C27 C18 107.6(3) . . ?
O3 C27 C28 114.3(4) . . ?
C18 C27 C28 109.1(4) . . ?
O3 C27 C26 114.4(4) . . ?
C18 C27 C26 107.8(3) . . ?
C28 C27 C26 103.3(3) . . ?
C29 C28 C36 119.6(4) . . ?
C29 C28 C27 123.0(3) . . ?
C36 C28 C27 108.9(4) . . ?
C28 C29 C33 118.7(4) . . ?
C28 C29 C30 123.2(4) . . ?
C33 C29 C30 110.4(5) . . ?
O6 C30 C17 105.0(3) . . ?
O6 C30 C29 117.3(4) . . ?
C17 C30 C29 107.4(3) . . ?
O6 C30 C31 116.6(4) . . ?
C17 C30 C31 110.7(3) . . ?
C29 C30 C31 99.6(4) . . ?
C56 C31 C32 124.4(5) . . ?
C56 C31 C30 120.3(4) . . ?
C32 C31 C30 108.6(5) . . ?
C33 C32 C31 113.1(5) . . ?
C33 C32 C53 118.6(4) . . ?
C31 C32 C53 119.0(6) . . ?
C32 C33 C34 123.2(6) . . ?
C32 C33 C29 107.4(4) . . ?
C34 C33 C29 121.0(5) . . ?
C33 C34 C35 120.7(5) . . ?
C33 C34 C51 118.5(6) . . ?
C35 C34 C51 107.6(4) . . ?
C36 C35 C37 121.5(4) . . ?
C36 C35 C34 117.8(4) . . ?
C37 C35 C34 107.6(4) . . ?
C35 C36 C40 119.6(4) . . ?
C35 C36 C28 121.9(5) . . ?
C40 C36 C28 109.1(4) . . ?
C38 C37 C50 120.7(4) . . ?
C38 C37 C35 119.0(4) . . ?
C50 C37 C35 109.7(4) . . ?
C37 C38 C39 119.9(4) . . ?
C37 C38 C47 119.0(4) . . ?
C39 C38 C47 108.0(4) . . ?
C40 C39 C41 118.7(5) . . ?
C40 C39 C38 119.6(4) . . ?
C41 C39 C38 108.8(5) . . ?
C39 C40 C36 120.2(5) . . ?
C39 C40 C26 120.0(4) . . ?
C36 C40 C26 110.4(4) . . ?
C42 C41 C39 119.5(4) . . ?
C42 C41 C46 120.9(4) . . ?
C39 C41 C46 107.2(4) . . ?
C41 C42 C25 122.0(4) . . ?
C41 C42 C43 119.6(4) . . ?
C25 C42 C43 107.7(4) . . ?
C44 C43 C23 119.6(5) . . ?
C44 C43 C42 120.2(4) . . ?
C23 C43 C42 109.5(4) . . ?
C69 C44 C43 120.7(4) . . ?
C69 C44 C45 109.0(5) . . ?
C43 C44 C45 119.0(5) . . ?
C46 C45 C67 119.9(4) . . ?
C46 C45 C44 120.7(4) . . ?
C67 C45 C44 106.0(4) . . ?
C45 C46 C47 120.2(4) . . ?
C45 C46 C41 119.6(4) . . ?
C47 C46 C41 108.7(4) . . ?
C48 C47 C46 120.6(5) . . ?
C48 C47 C38 120.0(5) . . ?
C46 C47 C38 107.28(16) . . ?
C47 C48 C49 120.6(5) . . ?
C47 C48 C66 119.2(5) . . ?
C49 C48 C66 108.09(19) . . ?
C50 C49 C63 120.9(4) . . ?
C50 C49 C48 118.5(4) . . ?
C63 C49 C48 108.6(4) . . ?
C49 C50 C37 121.2(4) . . ?
C49 C50 C51 119.2(5) . . ?
C37 C50 C51 107.1(4) . . ?
C52 C51 C34 119.5(4) . . ?
C52 C51 C50 120.3(5) . . ?
C34 C51 C50 108.0(5) . . ?
C51 C52 C53 120.5(6) . . ?
C51 C52 C62 119.9(5) . . ?
C53 C52 C62 107.8(6) . . ?
C32 C53 C52 119.8(6) . . ?
C32 C53 C54 118.7(5) . . ?
C52 C53 C54 109.2(6) . . ?
C55 C54 C61 123.4(6) . . ?
C55 C54 C53 120.7(6) . . ?
C61 C54 C53 105.6(5) . . ?
C54 C55 C57 118.9(6) . . ?
C54 C55 C56 118.7(5) . . ?
C57 C55 C56 114.3(5) . . ?
C31 C56 C76B 129.1(6) . . ?
C31 C56 C55 117.0(4) . . ?
C76B C56 C55 113.8(6) . . ?
C31 C56 C75 110.5(5) . . ?
C76B C56 C75 34.3(4) . . ?
C55 C56 C75 121.8(5) . . ?
C59 C57 C58 115.6(6) . . ?
C59 C57 C55 118.3(6) . . ?
C58 C57 C55 118.1(5) . . ?
C74 C58 C57 123.3(5) . . ?
C74 C58 C76 122.0(6) . . ?
C57 C58 C76 114.3(6) . . ?
C74 C58 C75B 107.4(6) . . ?
C57 C58 C75B 118.7(6) . . ?
C76 C58 C75B 29.9(4) . . ?
C57 C59 C72 121.4(6) . . ?
C57 C59 C60 120.5(6) . . ?
C72 C59 C60 108.4(6) . . ?
C61 C60 C59 122.0(6) . . ?
C61 C60 C65 120.0(6) . . ?
C59 C60 C65 106.9(6) . . ?
C60 C61 C62 120.3(7) . . ?
C60 C61 C54 116.9(6) . . ?
C62 C61 C54 110.9(7) . . ?
C63 C62 C61 120.0(6) . . ?
C63 C62 C52 120.6(6) . . ?
C61 C62 C52 106.5(5) . . ?
C62 C63 C49 119.1(5) . . ?
C62 C63 C64 120.6(7) . . ?
C49 C63 C64 108.3(5) . . ?
C65 C64 C66 120.4(6) . . ?
C65 C64 C63 119.1(7) . . ?
C66 C64 C63 107.7(5) . . ?
C64 C65 C73 119.2(6) . . ?
C64 C65 C60 120.0(6) . . ?
C73 C65 C60 108.9(5) . . ?
C67 C66 C64 119.6(4) . . ?
C67 C66 C48 120.2(4) . . ?
C64 C66 C48 107.3(4) . . ?
C66 C67 C68 120.7(5) . . ?
C66 C67 C45 119.8(4) . . ?
C68 C67 C45 108.0(4) . . ?
C73 C68 C69 121.6(4) . . ?
C73 C68 C67 119.1(5) . . ?
C69 C68 C67 107.4(5) . . ?
C44 C69 C70 117.8(5) . . ?
C44 C69 C68 109.6(4) . . ?
C70 C69 C68 120.4(6) . . ?
C69 C70 C22 121.6(5) . . ?
C69 C70 C71 116.9(5) . . ?
C22 C70 C71 109.9(4) . . ?
C72 C71 C74 120.1(6) . . ?
C72 C71 C70 123.0(5) . . ?
C74 C71 C70 108.8(5) . . ?
C71 C72 C59 119.0(5) . . ?
C71 C72 C73 119.2(6) . . ?
C59 C72 C73 108.6(6) . . ?
C68 C73 C65 121.0(5) . . ?
C68 C73 C72 118.9(6) . . ?
C65 C73 C72 107.2(6) . . ?
C58 C74 C71 118.3(6) . . ?
C58 C74 C21 124.2(4) . . ?
C71 C74 C21 110.0(5) . . ?
O9 C75 C76 106.8(6) . . ?
O9 C75 N1 112.9(5) . . ?
C76 C75 N1 105.6(6) . . ?
O9 C75 C56 110.5(5) . . ?
C76 C75 C56 107.7(6) . . ?
N1 C75 C56 112.9(5) . . ?
C75 C76 C58 101.3(6) . . ?
O9B C75B C76B 110.7(7) . . ?
O9B C75B N1 110.2(6) . . ?
C76B C75B N1 106.8(6) . . ?
O9B C75B C58 111.0(6) . . ?
C76B C75B C58 107.0(7) . . ?
N1 C75B C58 111.0(5) . . ?
C56 C76B C75B 101.1(6) . . ?
C20 N1 C17 108.48(12) . . ?
C20 N1 C75 143.8(4) . . ?
C17 N1 C75 107.1(4) . . ?
C20 N1 C75B 107.8(4) . . ?
C17 N1 C75B 143.2(4) . . ?
C75 N1 C75B 36.2(2) . . ?
C24 O1 O2 102.7(3) . . ?
C1 O2 O1 108.7(3) . . ?
C27 O3 O4 102.2(3) . . ?
C5 O4 O3 106.6(3) . . ?
C9 O5 O6 105.4(3) . . ?
C30 O6 O5 103.0(2) . . ?
C21 O7 O8 106.2(3) . . ?
C13 O8 O7 106.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        31.26
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.072
