# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# 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 
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data_2
_database_code_depnum_ccdc_archive 'CCDC 1485682'
_audit_update_record             
;
2016-06-15 deposited with the CCDC.
2016-08-31 downloaded from the CCDC.
;
_audit_creation_date             2016-06-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C88 H70 O'
_chemical_formula_sum            'C88 H70 O'
_chemical_formula_weight         1143.44
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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        P2(1)/c
_space_group_name_Hall           '-P 2ybc'
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                   15.5050(5)
_cell_length_b                   34.4906(10)
_cell_length_c                   17.2521(5)
_cell_angle_alpha                90
_cell_angle_beta                 112.9897(17)
_cell_angle_gamma                90
_cell_volume                     8493.2(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.399
_cell_measurement_theta_min      2.562
_shelx_estimated_absorpt_T_max   0.970
_shelx_estimated_absorpt_T_min   0.962
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0993 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.8324.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.894
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.1057
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26449
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        39.966
_diffrn_reflns_theta_max         39.966
_diffrn_reflns_theta_min         2.562
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'high brilliance microfocus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2939
_reflns_number_total             4676
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker Apex3, 2016'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         4676
_refine_ls_number_restraints     864
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0843
_refine_ls_restrained_S_all      1.050
_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)+(0.0970P)²+16.4197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2232
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C18(H18), C20(H20), C21(H21), C26(H26), C31(H31), C32(H32),
 C34(H34), C35(H35), C44(H44), C45(H45), C46(H46), C47(H47), C56(H56), C57(H57),
  C58(H58), C59(H59), C62(H62), C66(H66), C67(H67), C69(H69), C70(H70),
 C79(H79), C80(H80), C82(H82), C87(H87), C88(H88)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C84(H84A,
 H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C)
;
_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
C1 C 0.3364(7) 0.4971(3) 0.2658(6) 0.055(2) Uani 1 1 d . U . . .
C2 C 0.2393(6) 0.5129(3) 0.2500(5) 0.075(3) Uani 1 1 d . U . . .
H2A H 0.2346 0.5397 0.2298 0.113 Uiso 1 1 calc GR . . . .
H2B H 0.2290 0.5123 0.3026 0.113 Uiso 1 1 calc GR . . . .
H2C H 0.1918 0.4969 0.2076 0.113 Uiso 1 1 calc GR . . . .
C3 C 0.3461(7) 0.4553(3) 0.2976(5) 0.077(3) Uani 1 1 d . U . . .
H3A H 0.3034 0.4386 0.2532 0.116 Uiso 1 1 calc GR . . . .
H3B H 0.3303 0.4540 0.3472 0.116 Uiso 1 1 calc GR . . . .
H3C H 0.4107 0.4466 0.3126 0.116 Uiso 1 1 calc GR . . . .
C4 C 0.3558(6) 0.4997(3) 0.1858(5) 0.039(2) Uani 1 1 d . U . . .
C5 C 0.4294(6) 0.5246(3) 0.1977(5) 0.042(2) Uani 1 1 d . U . . .
C6 C 0.4719(6) 0.5348(3) 0.2859(5) 0.043(2) Uani 1 1 d . U . . .
C7 C 0.4147(6) 0.5213(3) 0.3246(5) 0.053(3) Uani 1 1 d . U . . .
C007 C 0.6092(6) 0.5763(3) 0.2970(5) 0.042(2) Uani 1 1 d . U . . .
C8 C 0.4251(7) 0.5314(3) 0.4096(6) 0.067(3) Uani 1 1 d . U . . .
H8 H 0.4746 0.5483 0.4417 0.080 Uiso 1 1 calc R . . . .
O9 O 0.3728(5) 0.51893(19) 0.4415(4) 0.069(2) Uani 1 1 d . U . . .
C10 C 0.3108(6) 0.4807(3) 0.1111(5) 0.046(3) Uani 1 1 d . U . . .
H10 H 0.2622 0.4627 0.1052 0.055 Uiso 1 1 calc R . . . .
C11 C 0.3364(6) 0.4878(3) 0.0449(5) 0.042(2) Uani 1 1 d . U . . .
C12 C 0.4012(6) 0.5185(3) 0.0496(5) 0.034(2) Uani 1 1 d . U . . .
C13 C 0.4506(6) 0.5373(3) 0.1285(5) 0.043(2) Uani 1 1 d . U . . .
C14 C 0.2924(6) 0.4672(3) -0.0364(5) 0.042(2) Uani 1 1 d . U . . .
C15 C 0.3085(6) 0.4792(3) -0.1061(5) 0.039(2) Uani 1 1 d . U . . .
C16 C 0.3643(6) 0.5129(3) -0.1018(6) 0.042(2) Uani 1 1 d . U . . .
C17 C 0.4124(6) 0.5316(3) -0.0241(5) 0.044(2) Uani 1 1 d . U . . .
C18 C 0.2319(6) 0.4356(3) -0.0425(6) 0.051(3) Uani 1 1 d . U . . .
H18 H 0.2224 0.4273 0.0061 0.062 Uiso 1 1 calc R . . . .
C19 C 0.1864(6) 0.4165(3) -0.1179(6) 0.048(2) Uani 1 1 d . U . . .
C20 C 0.2033(6) 0.4272(3) -0.1881(5) 0.047(3) Uani 1 1 d . U . . .
H20 H 0.1736 0.4138 -0.2399 0.056 Uiso 1 1 calc R . . . .
C21 C 0.2637(6) 0.4575(3) -0.1820(5) 0.041(2) Uani 1 1 d . U . . .
H21 H 0.2760 0.4643 -0.2301 0.049 Uiso 1 1 calc R . . . .
C22 C 0.1142(7) 0.3844(3) -0.1298(6) 0.066(3) Uani 1 1 d . U . . .
C23 C 0.1033(7) 0.3727(3) -0.0485(5) 0.077(3) Uani 1 1 d . U . . .
H23A H 0.1616 0.3608 -0.0097 0.116 Uiso 1 1 calc GR . . . .
H23B H 0.0518 0.3541 -0.0615 0.116 Uiso 1 1 calc GR . . . .
H23C H 0.0894 0.3958 -0.0222 0.116 Uiso 1 1 calc GR . . . .
C24 C 0.0182(6) 0.3979(3) -0.1915(6) 0.076(3) Uani 1 1 d . U . . .
H24A H 0.0096 0.4253 -0.1813 0.114 Uiso 1 1 calc GR . . . .
H24B H -0.0308 0.3824 -0.1835 0.114 Uiso 1 1 calc GR . . . .
H24C H 0.0141 0.3946 -0.2493 0.114 Uiso 1 1 calc GR . . . .
C25 C 0.1404(7) 0.3478(3) -0.1661(6) 0.080(3) Uani 1 1 d . U . . .
H25A H 0.1383 0.3534 -0.2226 0.121 Uiso 1 1 calc GR . . . .
H25B H 0.0960 0.3270 -0.1696 0.121 Uiso 1 1 calc GR . . . .
H25C H 0.2039 0.3396 -0.1295 0.121 Uiso 1 1 calc GR . . . .
C26 C 0.3657(6) 0.5295(3) -0.1744(6) 0.057(3) Uani 1 1 d . U . . .
H26 H 0.3337 0.5166 -0.2265 0.068 Uiso 1 1 calc R . . . .
C27 C 0.4109(6) 0.5634(3) -0.1748(6) 0.051(3) Uani 1 1 d . U . . .
C28 C 0.4668(6) 0.5813(3) -0.0973(5) 0.045(2) Uani 1 1 d . U . . .
C29 C 0.4646(6) 0.5654(3) -0.0207(5) 0.043(2) Uani 1 1 d . U . . .
C30 C 0.3862(6) 0.5826(3) -0.2593(5) 0.048(3) Uani 1 1 d . U . . .
C31 C 0.3930(6) 0.5638(3) -0.3277(5) 0.055(3) Uani 1 1 d . U . . .
H31 H 0.4221 0.5390 -0.3194 0.066 Uiso 1 1 calc R . . . .
C32 C 0.3588(7) 0.5798(3) -0.4084(6) 0.063(3) Uani 1 1 d . U . . .
H32 H 0.3648 0.5662 -0.4539 0.076 Uiso 1 1 calc R . . . .
C33 C 0.3165(7) 0.6152(3) -0.4210(6) 0.073(3) Uani 1 1 d . U . . .
C34 C 0.3096(7) 0.6356(3) -0.3531(6) 0.074(3) Uani 1 1 d . U . . .
H34 H 0.2813 0.6606 -0.3622 0.089 Uiso 1 1 calc R . . . .
C35 C 0.3434(7) 0.6197(3) -0.2733(6) 0.065(3) Uani 1 1 d . U . . .
H35 H 0.3381 0.6336 -0.2278 0.077 Uiso 1 1 calc R . . . .
C36 C 0.2752(11) 0.6319(4) -0.5098(7) 0.117(4) Uani 1 1 d . U . . .
C37 C 0.2109(13) 0.6053(5) -0.5707(8) 0.209(7) Uani 1 1 d . U . . .
H37A H 0.2350 0.5989 -0.6139 0.313 Uiso 1 1 calc GR . . . .
H37B H 0.1493 0.6175 -0.5973 0.313 Uiso 1 1 calc GR . . . .
H37C H 0.2052 0.5815 -0.5419 0.313 Uiso 1 1 calc GR . . . .
C38 C 0.3533(13) 0.6397(5) -0.5414(9) 0.214(7) Uani 1 1 d . U . . .
H38A H 0.4105 0.6475 -0.4939 0.320 Uiso 1 1 calc GR . . . .
H38B H 0.3339 0.6606 -0.5833 0.320 Uiso 1 1 calc GR . . . .
H38C H 0.3655 0.6161 -0.5671 0.320 Uiso 1 1 calc GR . . . .
C39 C 0.2306(14) 0.6697(5) -0.5166(8) 0.210(7) Uani 1 1 d . U . . .
H39A H 0.1709 0.6667 -0.5102 0.315 Uiso 1 1 calc GR . . . .
H39B H 0.2192 0.6810 -0.5719 0.315 Uiso 1 1 calc GR . . . .
H39C H 0.2718 0.6869 -0.4724 0.315 Uiso 1 1 calc GR . . . .
C40 C 0.5288(6) 0.6134(3) -0.0933(6) 0.048(2) Uani 1 1 d . U . . .
C41 C 0.5599(6) 0.6371(3) -0.0230(6) 0.053(3) Uani 1 1 d . U . . .
C42 C 0.5409(6) 0.6245(3) 0.0516(6) 0.052(3) Uani 1 1 d . U . . .
C43 C 0.5071(6) 0.5877(3) 0.0562(5) 0.044(2) Uani 1 1 d . U . . .
C44 C 0.5660(6) 0.6193(3) -0.1552(5) 0.053(3) Uani 1 1 d . U . . .
H44 H 0.5496 0.6018 -0.2012 0.064 Uiso 1 1 calc R . . . .
C45 C 0.6249(7) 0.6495(3) -0.1513(6) 0.062(3) Uani 1 1 d . U . . .
H45 H 0.6462 0.6536 -0.1953 0.074 Uiso 1 1 calc R . . . .
C46 C 0.6529(7) 0.6739(3) -0.0827(6) 0.065(3) Uani 1 1 d . U . . .
H46 H 0.6936 0.6951 -0.0789 0.078 Uiso 1 1 calc R . . . .
C47 C 0.6208(7) 0.6672(3) -0.0192(6) 0.066(3) Uani 1 1 d . U . . .
H47 H 0.6413 0.6838 0.0286 0.079 Uiso 1 1 calc R . . . .
C48 C 0.5660(6) 0.6488(3) 0.1227(6) 0.051(3) Uani 1 1 d . U . . .
C49 C 0.5960(6) 0.6305(3) 0.2019(5) 0.042(2) Uani 1 1 d . U . . .
C50 C 0.5686(6) 0.5922(3) 0.2100(5) 0.042(2) Uani 1 1 d . U . . .
C51 C 0.5076(6) 0.5723(3) 0.1335(5) 0.041(2) Uani 1 1 d . U . . .
C52 C 0.5602(7) 0.6905(3) 0.1231(6) 0.050(2) Uani 1 1 d . U . . .
C53 C 0.6197(7) 0.7118(3) 0.1928(6) 0.056(3) Uani 1 1 d . U . . .
C55 C 0.6712(6) 0.6503(3) 0.2693(5) 0.040(2) Uani 1 1 d . U . . .
C56 C 0.4919(7) 0.7113(3) 0.0576(6) 0.056(3) Uani 1 1 d . U . . .
H56 H 0.4548 0.6983 0.0070 0.067 Uiso 1 1 calc R . . . .
C57 C 0.4780(8) 0.7500(3) 0.0656(6) 0.073(3) Uani 1 1 d . U . . .
H57 H 0.4287 0.7629 0.0217 0.087 Uiso 1 1 calc R . . . .
C58 C 0.5318(8) 0.7702(3) 0.1335(6) 0.076(3) Uani 1 1 d . U . . .
H58 H 0.5212 0.7972 0.1371 0.091 Uiso 1 1 calc R . . . .
C59 C 0.6021(7) 0.7519(3) 0.1977(6) 0.070(3) Uani 1 1 d . U . . .
H59 H 0.6396 0.7662 0.2462 0.084 Uiso 1 1 calc R . . . .
C60 C 0.6902(6) 0.6893(3) 0.2608(5) 0.045(2) Uani 1 1 d . U . . .
C61 C 0.7782(7) 0.7046(3) 0.3168(6) 0.051(2) Uani 1 1 d . U . . .
C62 C 0.8372(6) 0.6814(3) 0.3814(5) 0.050(3) Uani 1 1 d . U . . .
H62 H 0.8951 0.6919 0.4189 0.060 Uiso 1 1 calc R . . . .
C63 C 0.8150(7) 0.6432(3) 0.3938(5) 0.048(3) Uani 1 1 d . U . . .
C64 C 0.7302(6) 0.6293(3) 0.3384(5) 0.040(2) Uani 1 1 d . U . . .
C65 C 0.8098(7) 0.7433(3) 0.3050(6) 0.061(3) Uani 1 1 d . U . . .
C66 C 0.8138(7) 0.7540(3) 0.2297(6) 0.076(3) Uani 1 1 d . U . . .
H66 H 0.7970 0.7357 0.1850 0.091 Uiso 1 1 calc R . . . .
C67 C 0.8421(8) 0.7912(3) 0.2178(7) 0.087(4) Uani 1 1 d . U . . .
H67 H 0.8452 0.7977 0.1654 0.104 Uiso 1 1 calc R . . . .
C68 C 0.8656(8) 0.8186(4) 0.2805(8) 0.084(3) Uani 1 1 d . U . . .
C69 C 0.8635(7) 0.8082(3) 0.3554(7) 0.079(3) Uani 1 1 d . U . . .
H69 H 0.8809 0.8264 0.4003 0.094 Uiso 1 1 calc R . . . .
C70 C 0.8364(6) 0.7716(3) 0.3663(6) 0.061(3) Uani 1 1 d . U . . .
H70 H 0.8359 0.7652 0.4197 0.074 Uiso 1 1 calc R . . . .
C71 C 0.8938(13) 0.8592(4) 0.2592(11) 0.145(5) Uani 1 1 d . U . . .
C72 C 0.8156(14) 0.8750(4) 0.1724(10) 0.196(7) Uani 1 1 d . U . . .
H72A H 0.8020 0.8550 0.1289 0.293 Uiso 1 1 calc GR . . . .
H72B H 0.8389 0.8983 0.1546 0.293 Uiso 1 1 calc GR . . . .
H72C H 0.7582 0.8812 0.1809 0.293 Uiso 1 1 calc GR . . . .
C73 C 0.9812(13) 0.8563(4) 0.2416(12) 0.210(7) Uani 1 1 d . U . . .
H73A H 1.0363 0.8583 0.2945 0.314 Uiso 1 1 calc GR . . . .
H73B H 0.9821 0.8774 0.2038 0.314 Uiso 1 1 calc GR . . . .
H73C H 0.9821 0.8313 0.2148 0.314 Uiso 1 1 calc GR . . . .
C74 C 0.8966(12) 0.8872(4) 0.3262(9) 0.172(6) Uani 1 1 d . U . . .
H74A H 0.8472 0.8808 0.3461 0.258 Uiso 1 1 calc GR . . . .
H74B H 0.8867 0.9136 0.3031 0.258 Uiso 1 1 calc GR . . . .
H74C H 0.9578 0.8857 0.3733 0.258 Uiso 1 1 calc GR . . . .
C75 C 0.8786(7) 0.6187(3) 0.4607(5) 0.045(2) Uani 1 1 d . U . . .
C76 C 0.8457(7) 0.5823(3) 0.4755(5) 0.050(3) Uani 1 1 d . U . . .
C77 C 0.7509(7) 0.5712(3) 0.4274(5) 0.046(2) Uani 1 1 d . U . . .
C78 C 0.6988(6) 0.5919(3) 0.3520(5) 0.039(2) Uani 1 1 d . U . . .
C79 C 0.9738(7) 0.6285(3) 0.5084(6) 0.072(3) Uani 1 1 d . U . . .
H79 H 0.9975 0.6526 0.4987 0.086 Uiso 1 1 calc R . . . .
C80 C 1.0326(7) 0.6036(3) 0.5686(6) 0.064(3) Uani 1 1 d . U . . .
H80 H 1.0958 0.6110 0.5999 0.077 Uiso 1 1 calc R . . . .
C81 C 1.0011(7) 0.5681(3) 0.5841(6) 0.064(3) Uani 1 1 d . U . . .
C82 C 0.9096(7) 0.5581(3) 0.5387(5) 0.053(3) Uani 1 1 d . U . . .
H82 H 0.8878 0.5338 0.5500 0.064 Uiso 1 1 calc R . . . .
C83 C 1.0700(8) 0.5398(3) 0.6441(6) 0.080(3) Uani 1 1 d . U . . .
C84 C 1.1207(7) 0.5582(3) 0.7323(6) 0.092(4) Uani 1 1 d . U . . .
H84A H 1.1597 0.5799 0.7282 0.137 Uiso 1 1 calc GR . . . .
H84B H 1.1604 0.5387 0.7713 0.137 Uiso 1 1 calc GR . . . .
H84C H 1.0742 0.5678 0.7531 0.137 Uiso 1 1 calc GR . . . .
C85 C 1.0232(8) 0.5025(4) 0.6535(8) 0.130(5) Uani 1 1 d . U . . .
H85A H 0.9659 0.5086 0.6622 0.194 Uiso 1 1 calc GR . . . .
H85B H 1.0661 0.4879 0.7019 0.194 Uiso 1 1 calc GR . . . .
H85C H 1.0073 0.4869 0.6023 0.194 Uiso 1 1 calc GR . . . .
C86 C 1.1438(7) 0.5283(3) 0.6097(6) 0.094(4) Uani 1 1 d . U . . .
H86A H 1.1125 0.5199 0.5510 0.142 Uiso 1 1 calc GR . . . .
H86B H 1.1821 0.5070 0.6434 0.142 Uiso 1 1 calc GR . . . .
H86C H 1.1840 0.5506 0.6125 0.142 Uiso 1 1 calc GR . . . .
C87 C 0.7099(6) 0.5395(3) 0.4522(5) 0.047(3) Uani 1 1 d . U . . .
H87 H 0.7459 0.5251 0.5011 0.056 Uiso 1 1 calc R . . . .
C88 C 0.6188(6) 0.5294(3) 0.4066(5) 0.046(2) Uani 1 1 d . U . . .
H88 H 0.5896 0.5102 0.4275 0.055 Uiso 1 1 calc R . . . .
C89 C 0.5674(6) 0.5476(3) 0.3278(5) 0.046(2) 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 C2 1.522(12) . ?
C1 C3 1.526(12) . ?
C1 C4 1.526(11) . ?
C1 C7 1.497(12) . ?
C4 C5 1.380(11) . ?
C4 C10 1.370(11) . ?
C5 C6 1.446(11) . ?
C5 C13 1.423(11) . ?
C6 C7 1.383(11) . ?
C6 C89 1.440(11) . ?
C7 C8 1.453(12) . ?
C007 C50 1.488(11) . ?
C007 C78 1.447(11) . ?
C007 C89 1.396(11) . ?
C8 O9 1.222(10) . ?
C10 C11 1.369(10) . ?
C11 C12 1.440(11) . ?
C11 C14 1.480(11) . ?
C12 C13 1.432(11) . ?
C12 C17 1.423(11) . ?
C13 C51 1.479(11) . ?
C14 C15 1.385(11) . ?
C14 C18 1.414(11) . ?
C15 C16 1.434(11) . ?
C15 C21 1.429(11) . ?
C16 C17 1.410(11) . ?
C16 C26 1.385(11) . ?
C17 C29 1.406(11) . ?
C18 C19 1.380(11) . ?
C19 C20 1.387(11) . ?
C19 C22 1.531(12) . ?
C20 C21 1.380(10) . ?
C22 C23 1.530(12) . ?
C22 C24 1.527(12) . ?
C22 C25 1.533(12) . ?
C26 C27 1.366(12) . ?
C27 C28 1.420(12) . ?
C27 C30 1.507(12) . ?
C28 C29 1.443(11) . ?
C28 C40 1.450(12) . ?
C29 C43 1.451(11) . ?
C30 C31 1.386(11) . ?
C30 C35 1.418(12) . ?
C31 C32 1.395(11) . ?
C32 C33 1.363(12) . ?
C33 C34 1.405(12) . ?
C33 C36 1.524(14) . ?
C34 C35 1.381(11) . ?
C36 C37 1.458(18) . ?
C36 C38 1.533(19) . ?
C36 C39 1.460(16) . ?
C40 C41 1.385(12) . ?
C40 C44 1.413(11) . ?
C41 C42 1.493(12) . ?
C41 C47 1.387(12) . ?
C42 C43 1.389(12) . ?
C42 C48 1.409(12) . ?
C43 C51 1.433(11) . ?
C44 C45 1.368(11) . ?
C45 C46 1.378(12) . ?
C46 C47 1.388(11) . ?
C48 C49 1.411(11) . ?
C48 C52 1.440(12) . ?
C49 C50 1.409(11) . ?
C49 C55 1.456(11) . ?
C50 C51 1.461(11) . ?
C52 C53 1.402(12) . ?
C52 C56 1.407(11) . ?
C53 C59 1.418(12) . ?
C53 C60 1.473(12) . ?
C55 C60 1.398(11) . ?
C55 C64 1.391(11) . ?
C56 C57 1.367(12) . ?
C57 C58 1.338(12) . ?
C58 C59 1.368(12) . ?
C60 C61 1.429(11) . ?
C61 C62 1.387(11) . ?
C61 C65 1.464(13) . ?
C62 C63 1.401(11) . ?
C63 C64 1.376(11) . ?
C63 C75 1.457(12) . ?
C64 C78 1.428(11) . ?
C65 C66 1.374(12) . ?
C65 C70 1.377(12) . ?
C66 C67 1.397(13) . ?
C67 C68 1.375(13) . ?
C68 C69 1.352(13) . ?
C68 C71 1.554(16) . ?
C69 C70 1.369(12) . ?
C71 C72 1.61(2) . ?
C71 C73 1.504(19) . ?
C71 C74 1.494(16) . ?
C75 C76 1.417(12) . ?
C75 C79 1.422(12) . ?
C76 C77 1.430(11) . ?
C76 C82 1.423(11) . ?
C77 C78 1.427(11) . ?
C77 C87 1.411(11) . ?
C79 C80 1.382(12) . ?
C80 C81 1.383(13) . ?
C81 C82 1.370(12) . ?
C81 C83 1.518(13) . ?
C83 C84 1.550(13) . ?
C83 C85 1.516(14) . ?
C83 C86 1.533(13) . ?
C87 C88 1.367(11) . ?
C88 C89 1.426(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C3 110.8(8) . . ?
C2 C1 C4 110.3(7) . . ?
C4 C1 C3 110.7(8) . . ?
C7 C1 C2 113.8(8) . . ?
C7 C1 C3 110.1(8) . . ?
C7 C1 C4 100.7(7) . . ?
C5 C4 C1 110.3(8) . . ?
C10 C4 C1 128.0(8) . . ?
C10 C4 C5 121.7(8) . . ?
C4 C5 C6 108.5(8) . . ?
C4 C5 C13 121.0(8) . . ?
C13 C5 C6 130.4(9) . . ?
C7 C6 C5 108.2(8) . . ?
C7 C6 C89 126.1(8) . . ?
C89 C6 C5 124.0(8) . . ?
C6 C7 C1 111.4(8) . . ?
C6 C7 C8 124.6(9) . . ?
C8 C7 C1 123.9(8) . . ?
C78 C007 C50 116.3(8) . . ?
C89 C007 C50 124.7(8) . . ?
C89 C007 C78 119.0(8) . . ?
O9 C8 C7 122.6(10) . . ?
C11 C10 C4 119.5(8) . . ?
C10 C11 C12 120.6(8) . . ?
C10 C11 C14 121.9(8) . . ?
C12 C11 C14 117.3(8) . . ?
C13 C12 C11 119.2(8) . . ?
C17 C12 C11 120.7(8) . . ?
C17 C12 C13 120.0(8) . . ?
C5 C13 C12 116.5(8) . . ?
C5 C13 C51 122.0(8) . . ?
C12 C13 C51 120.7(8) . . ?
C15 C14 C11 120.5(9) . . ?
C15 C14 C18 120.3(8) . . ?
C18 C14 C11 119.2(8) . . ?
C14 C15 C16 120.5(8) . . ?
C14 C15 C21 116.8(9) . . ?
C21 C15 C16 122.6(8) . . ?
C17 C16 C15 120.3(8) . . ?
C26 C16 C15 120.7(9) . . ?
C26 C16 C17 118.8(9) . . ?
C16 C17 C12 120.0(9) . . ?
C29 C17 C12 119.8(8) . . ?
C29 C17 C16 120.0(8) . . ?
C19 C18 C14 121.2(9) . . ?
C18 C19 C20 119.6(9) . . ?
C18 C19 C22 123.4(9) . . ?
C20 C19 C22 117.0(8) . . ?
C21 C20 C19 119.3(9) . . ?
C20 C21 C15 122.6(8) . . ?
C19 C22 C25 110.7(8) . . ?
C23 C22 C19 113.8(8) . . ?
C23 C22 C25 107.5(8) . . ?
C24 C22 C19 109.6(8) . . ?
C24 C22 C23 107.0(8) . . ?
C24 C22 C25 108.0(8) . . ?
C27 C26 C16 123.2(9) . . ?
C26 C27 C28 119.6(9) . . ?
C26 C27 C30 116.4(9) . . ?
C28 C27 C30 123.5(9) . . ?
C27 C28 C29 118.2(9) . . ?
C27 C28 C40 121.7(8) . . ?
C29 C28 C40 120.0(8) . . ?
C17 C29 C28 119.8(8) . . ?
C17 C29 C43 121.7(8) . . ?
C28 C29 C43 118.0(9) . . ?
C31 C30 C27 122.9(9) . . ?
C31 C30 C35 117.6(9) . . ?
C35 C30 C27 119.1(8) . . ?
C30 C31 C32 122.5(9) . . ?
C33 C32 C31 119.1(9) . . ?
C32 C33 C34 120.3(10) . . ?
C32 C33 C36 119.0(10) . . ?
C34 C33 C36 120.7(10) . . ?
C35 C34 C33 120.6(10) . . ?
C34 C35 C30 119.9(9) . . ?
C33 C36 C38 110.1(12) . . ?
C37 C36 C33 112.8(12) . . ?
C37 C36 C38 105.5(13) . . ?
C37 C36 C39 109.6(14) . . ?
C39 C36 C33 114.7(11) . . ?
C39 C36 C38 103.2(14) . . ?
C41 C40 C28 119.4(9) . . ?
C41 C40 C44 118.1(9) . . ?
C44 C40 C28 122.3(9) . . ?
C40 C41 C42 117.7(9) . . ?
C40 C41 C47 118.8(9) . . ?
C47 C41 C42 122.5(9) . . ?
C43 C42 C41 121.5(9) . . ?
C43 C42 C48 118.5(9) . . ?
C48 C42 C41 119.8(9) . . ?
C42 C43 C29 118.7(8) . . ?
C42 C43 C51 121.8(8) . . ?
C51 C43 C29 119.3(9) . . ?
C45 C44 C40 122.3(9) . . ?
C44 C45 C46 119.2(9) . . ?
C45 C46 C47 119.1(10) . . ?
C41 C47 C46 122.3(9) . . ?
C42 C48 C49 116.8(9) . . ?
C42 C48 C52 127.0(9) . . ?
C49 C48 C52 116.2(8) . . ?
C48 C49 C55 114.9(8) . . ?
C50 C49 C48 121.2(8) . . ?
C50 C49 C55 122.7(8) . . ?
C49 C50 C007 114.9(8) . . ?
C49 C50 C51 117.8(8) . . ?
C51 C50 C007 127.3(8) . . ?
C43 C51 C13 117.6(8) . . ?
C43 C51 C50 115.6(8) . . ?
C50 C51 C13 126.7(8) . . ?
C53 C52 C48 120.3(9) . . ?
C53 C52 C56 117.3(9) . . ?
C56 C52 C48 122.2(9) . . ?
C52 C53 C59 118.9(9) . . ?
C52 C53 C60 116.3(9) . . ?
C59 C53 C60 124.4(9) . . ?
C60 C55 C49 120.4(8) . . ?
C64 C55 C49 119.5(9) . . ?
C64 C55 C60 119.8(9) . . ?
C57 C56 C52 121.1(9) . . ?
C58 C57 C56 121.8(10) . . ?
C57 C58 C59 119.7(11) . . ?
C58 C59 C53 120.9(10) . . ?
C55 C60 C53 117.9(9) . . ?
C55 C60 C61 118.0(9) . . ?
C61 C60 C53 124.1(9) . . ?
C60 C61 C65 121.7(9) . . ?
C62 C61 C60 119.1(9) . . ?
C62 C61 C65 119.2(9) . . ?
C61 C62 C63 122.9(9) . . ?
C62 C63 C75 122.4(9) . . ?
C64 C63 C62 116.6(9) . . ?
C64 C63 C75 121.1(9) . . ?
C55 C64 C78 117.4(8) . . ?
C63 C64 C55 123.0(9) . . ?
C63 C64 C78 119.6(8) . . ?
C66 C65 C61 121.1(9) . . ?
C66 C65 C70 115.2(10) . . ?
C70 C65 C61 123.7(9) . . ?
C65 C66 C67 121.2(10) . . ?
C68 C67 C66 121.1(11) . . ?
C67 C68 C71 116.5(11) . . ?
C69 C68 C67 118.2(12) . . ?
C69 C68 C71 125.3(12) . . ?
C68 C69 C70 119.9(10) . . ?
C69 C70 C65 124.3(10) . . ?
C68 C71 C72 110.2(13) . . ?
C73 C71 C68 110.3(13) . . ?
C73 C71 C72 104.2(13) . . ?
C74 C71 C68 109.0(12) . . ?
C74 C71 C72 106.5(14) . . ?
C74 C71 C73 116.3(15) . . ?
C76 C75 C63 118.5(9) . . ?
C76 C75 C79 118.1(9) . . ?
C79 C75 C63 123.3(9) . . ?
C75 C76 C77 119.6(9) . . ?
C75 C76 C82 117.9(9) . . ?
C82 C76 C77 122.5(9) . . ?
C78 C77 C76 118.8(9) . . ?
C87 C77 C76 121.0(9) . . ?
C87 C77 C78 120.1(9) . . ?
C64 C78 C007 122.0(8) . . ?
C77 C78 C007 117.9(8) . . ?
C77 C78 C64 119.6(8) . . ?
C80 C79 C75 121.3(10) . . ?
C79 C80 C81 121.1(10) . . ?
C80 C81 C83 119.6(10) . . ?
C82 C81 C80 118.5(10) . . ?
C82 C81 C83 121.6(11) . . ?
C81 C82 C76 123.1(10) . . ?
C81 C83 C84 110.9(9) . . ?
C81 C83 C86 109.5(9) . . ?
C85 C83 C81 112.3(10) . . ?
C85 C83 C84 109.0(10) . . ?
C85 C83 C86 106.4(10) . . ?
C86 C83 C84 108.5(9) . . ?
C88 C87 C77 120.7(9) . . ?
C87 C88 C89 120.2(9) . . ?
C007 C89 C6 124.5(8) . . ?
C007 C89 C88 120.4(9) . . ?
C88 C89 C6 115.2(8) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.431 -0.354 -0.301 3192.3 824.9 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_REFNR01_2                   
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: The sample diffracted very weakly, and at high angles the
reflections were completely absent. Despite the quality of the data,
the connectivity and conformation are not in doubt.
;
_vrf_THETM01_2                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A full set of data was collected, however the very high 
angle data was dominated by noise [I/sigma(I) < 1.0] and was omitted.
;
_vrf_PLAT029_2                   
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.909 Note  
RESPONSE: See _vrf_THETM01_2
;
_vrf_PLAT088_2                   
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.31 Note  
RESPONSE: See _vrf_REFNR01_2
;
_vrf_PLAT220_2                   
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        6.3 Ratio 
RESPONSE: This is due to the t-butyl groups in the molecule
;
_vrf_PLAT242_2                   
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C36 Check 
RESPONSE: this is due to the t-butyl moiety.
;
_vrf_PLAT340_2                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01451 Ang.  
RESPONSE: See _vrf_REFNR01_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_6a
_database_code_depnum_ccdc_archive 'CCDC 1485683'
_audit_update_record             
;
2016-06-15 deposited with the CCDC.
2016-08-31 downloaded from the CCDC.
;
_audit_creation_date             2016-06-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C47 H28 O5'
_chemical_formula_sum            'C47 H28 O5'
_chemical_formula_weight         672.69
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   7.5395(5)
_cell_length_b                   34.5192(18)
_cell_length_c                   11.7823(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.084(3)
_cell_angle_gamma                90
_cell_volume                     3019.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.622
_cell_measurement_theta_min      4.595
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0927 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.8874.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21377
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        66.584
_diffrn_reflns_theta_max         66.584
_diffrn_reflns_theta_min         2.560
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2999
_reflns_number_total             5048
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker Apex3, 2016'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         5048
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0613
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0480P)²+1.9942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1404
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C19(H19), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C39(H39), C48(H48), C49(H49), C50(H50), C51(H51)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C38(H38A,H38B,H38C)
;
_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
O1 O 0.0128(3) 0.59280(7) 0.5539(2) 0.0423(7) Uani 1 1 d . . . . .
C1 C 0.7391(5) 0.40855(10) 0.7988(3) 0.0376(10) Uani 1 1 d . . . . .
H1A H 0.7272 0.3898 0.7354 0.056 Uiso 1 1 calc GR . . . .
H1B H 0.6794 0.3984 0.8601 0.056 Uiso 1 1 calc GR . . . .
H1C H 0.8670 0.4129 0.8294 0.056 Uiso 1 1 calc GR . . . .
C2 C 0.1693(5) 0.59339(11) 0.5410(3) 0.0305(9) Uani 1 1 d . . . . .
C3 C 0.2492(5) 0.62889(10) 0.5019(3) 0.0314(9) Uani 1 1 d . . . . .
C4 C 0.4346(5) 0.63941(10) 0.5291(3) 0.0284(8) Uani 1 1 d . . . . .
C5 C 0.5608(5) 0.62230(9) 0.6244(3) 0.0267(8) Uani 1 1 d . . . . .
C6 C 0.5369(5) 0.58661(10) 0.6821(3) 0.0270(8) Uani 1 1 d . . . . .
C7 C 0.4296(5) 0.55336(10) 0.6321(3) 0.0270(8) Uani 1 1 d . . . . .
C8 C 0.2699(5) 0.55669(10) 0.5502(3) 0.0282(8) Uani 1 1 d . . . . .
C9 C 0.1259(5) 0.65021(11) 0.4265(3) 0.0364(9) Uani 1 1 d . . . . .
H9 H 0.0029 0.6426 0.4119 0.044 Uiso 1 1 calc R . . . .
C10 C 0.1801(5) 0.68250(11) 0.3719(3) 0.0404(10) Uani 1 1 d . . . . .
H10 H 0.0950 0.6969 0.3195 0.048 Uiso 1 1 calc R . . . .
C11 C 0.3565(5) 0.69345(11) 0.3939(3) 0.0366(10) Uani 1 1 d . . . . .
H11 H 0.3929 0.7157 0.3563 0.044 Uiso 1 1 calc R . . . .
C12 C 0.4868(5) 0.67260(10) 0.4712(3) 0.0321(9) Uani 1 1 d . . . . .
C13 C 0.6694(5) 0.68720(10) 0.4989(3) 0.0297(9) Uani 1 1 d . . . . .
C14 C 0.7820(5) 0.67500(10) 0.6010(3) 0.0296(9) Uani 1 1 d . . . . .
C15 C 0.7199(5) 0.64411(9) 0.6686(3) 0.0266(8) Uani 1 1 d . . . . .
C16 C 0.7398(5) 0.71605(10) 0.4331(3) 0.0362(10) Uani 1 1 d . . . . .
O17 O 0.6462(4) 0.72286(7) 0.3234(2) 0.0424(7) Uani 1 1 d . . . . .
C18 C 0.7109(6) 0.75169(11) 0.2571(3) 0.0447(11) Uani 1 1 d . . . . .
H18A H 0.6352 0.7526 0.1805 0.067 Uiso 1 1 calc GR . . . .
H18B H 0.8352 0.7457 0.2493 0.067 Uiso 1 1 calc GR . . . .
H18C H 0.7074 0.7768 0.2951 0.067 Uiso 1 1 calc GR . . . .
C19 C 0.8937(5) 0.73684(11) 0.4773(3) 0.0353(9) Uani 1 1 d . . . . .
H19 H 0.9286 0.7584 0.4362 0.042 Uiso 1 1 calc R . . . .
C20 C 0.9953(5) 0.72614(10) 0.5806(3) 0.0357(9) Uani 1 1 d . . . . .
O21 O 1.1422(4) 0.74732(7) 0.6314(2) 0.0441(7) Uani 1 1 d . . . . .
C22 C 1.1953(6) 0.77968(11) 0.5688(4) 0.0477(11) Uani 1 1 d . . . . .
H22A H 1.2215 0.7708 0.4945 0.071 Uiso 1 1 calc GR . . . .
H22B H 1.3032 0.7917 0.6135 0.071 Uiso 1 1 calc GR . . . .
H22C H 1.0973 0.7987 0.5557 0.071 Uiso 1 1 calc GR . . . .
C23 C 0.9519(5) 0.69319(10) 0.6415(3) 0.0313(9) Uani 1 1 d . . . . .
C24 C 1.0733(5) 0.67728(10) 0.7407(3) 0.0302(9) Uani 1 1 d . . . . .
C25 C 1.0049(4) 0.65078(9) 0.8126(3) 0.0256(8) Uani 1 1 d . . . . .
C26 C 0.8204(5) 0.63680(9) 0.7805(3) 0.0276(8) Uani 1 1 d . . . . .
C27 C 1.2602(5) 0.68511(11) 0.7606(3) 0.0358(10) Uani 1 1 d . . . . .
H27 H 1.3082 0.7025 0.7114 0.043 Uiso 1 1 calc R . . . .
C28 C 1.3727(5) 0.66780(10) 0.8503(3) 0.0351(9) Uani 1 1 d . . . . .
H28 H 1.4977 0.6737 0.8635 0.042 Uiso 1 1 calc R . . . .
C29 C 1.3070(5) 0.64215(10) 0.9210(3) 0.0326(9) Uani 1 1 d . . . . .
H29 H 1.3862 0.6301 0.9824 0.039 Uiso 1 1 calc R . . . .
C30 C 1.1254(5) 0.63389(10) 0.9028(3) 0.0303(9) Uani 1 1 d . . . . .
H30 H 1.0808 0.6162 0.9529 0.036 Uiso 1 1 calc R . . . .
C31 C 0.1886(5) 0.52523(10) 0.4927(3) 0.0324(9) Uani 1 1 d . . . . .
H31 H 0.0832 0.5286 0.4362 0.039 Uiso 1 1 calc R . . . .
C32 C 0.2597(5) 0.48815(10) 0.5166(3) 0.0343(9) Uani 1 1 d . . . . .
H32 H 0.2132 0.4667 0.4704 0.041 Uiso 1 1 calc R . . . .
C33 C 0.3985(5) 0.48329(10) 0.6085(3) 0.0298(9) Uani 1 1 d . . . . .
H33 H 0.4385 0.4578 0.6300 0.036 Uiso 1 1 calc R . . . .
C34 C 0.4835(5) 0.51513(10) 0.6718(3) 0.0286(8) Uani 1 1 d . . . . .
C35 C 0.6020(4) 0.50997(10) 0.7826(3) 0.0259(8) Uani 1 1 d . . . . .
C36 C 0.6690(5) 0.47478(10) 0.8312(3) 0.0296(9) Uani 1 1 d . . . . .
O37 O 0.6591(3) 0.44341(7) 0.7584(2) 0.0348(6) Uani 1 1 d . . . . .
C38 C 0.8847(5) 0.46543(10) 1.1838(3) 0.0344(9) Uani 1 1 d . . . . .
H38A H 0.9821 0.4548 1.1481 0.052 Uiso 1 1 calc GR . . . .
H38B H 0.7817 0.4477 1.1711 0.052 Uiso 1 1 calc GR . . . .
H38C H 0.9270 0.4686 1.2667 0.052 Uiso 1 1 calc GR . . . .
C39 C 0.7446(4) 0.47166(10) 0.9478(3) 0.0286(8) Uani 1 1 d . . . . .
H39 H 0.7849 0.4472 0.9794 0.034 Uiso 1 1 calc R . . . .
C40 C 0.7608(5) 0.50409(10) 1.0170(3) 0.0294(9) Uani 1 1 d . . . . .
O41 O 0.8309(3) 0.50244(7) 1.1330(2) 0.0349(6) Uani 1 1 d . . . . .
C42 C 0.7158(4) 0.54091(10) 0.9724(3) 0.0276(8) Uani 1 1 d . . . . .
C43 C 0.6436(4) 0.54349(10) 0.8533(3) 0.0257(8) Uani 1 1 d . . . . .
C44 C 0.6340(4) 0.58081(10) 0.7944(3) 0.0261(8) Uani 1 1 d . . . . .
C45 C 0.7460(4) 0.61000(9) 0.8514(3) 0.0255(8) Uani 1 1 d . . . . .
C46 C 0.7718(4) 0.61114(10) 0.9783(3) 0.0269(8) Uani 1 1 d . . . . .
C47 C 0.7433(4) 0.57701(10) 1.0376(3) 0.0273(8) Uani 1 1 d . . . . .
C48 C 0.7353(5) 0.57971(11) 1.1562(3) 0.0322(9) Uani 1 1 d . . . . .
H48 H 0.7187 0.5569 1.1983 0.039 Uiso 1 1 calc R . . . .
C49 C 0.7512(5) 0.61493(11) 1.2113(3) 0.0361(10) Uani 1 1 d . . . . .
H49 H 0.7409 0.6164 1.2904 0.043 Uiso 1 1 calc R . . . .
C50 C 0.7825(5) 0.64865(10) 1.1517(3) 0.0323(9) Uani 1 1 d . . . . .
H50 H 0.7961 0.6729 1.1905 0.039 Uiso 1 1 calc R . . . .
C51 C 0.7931(4) 0.64638(11) 1.0370(3) 0.0308(9) Uani 1 1 d . . . . .
H51 H 0.8154 0.6692 0.9967 0.037 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.216(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 O37 1.392(4) . ?
C2 C3 1.474(5) . ?
C2 C8 1.471(5) . ?
C3 C4 1.425(5) . ?
C3 C9 1.381(5) . ?
C4 C5 1.463(5) . ?
C4 C12 1.424(5) . ?
C5 C6 1.434(5) . ?
C5 C15 1.434(5) . ?
C6 C7 1.467(4) . ?
C6 C44 1.410(5) . ?
C7 C8 1.410(5) . ?
C7 C34 1.435(4) . ?
C8 C31 1.367(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.384(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.363(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.414(5) . ?
C12 C13 1.449(5) . ?
C13 C14 1.410(5) . ?
C13 C16 1.421(5) . ?
C14 C15 1.457(5) . ?
C14 C23 1.431(5) . ?
C15 C26 1.424(5) . ?
C16 O17 1.379(4) . ?
C16 C19 1.386(5) . ?
O17 C18 1.405(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 0.9500 . ?
C19 C20 1.370(5) . ?
C20 O21 1.374(4) . ?
C20 C23 1.414(5) . ?
O21 C22 1.433(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.460(5) . ?
C24 C25 1.404(5) . ?
C24 C27 1.413(5) . ?
C25 C26 1.458(5) . ?
C25 C30 1.399(5) . ?
C26 C45 1.426(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.371(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.366(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.378(5) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C31 C32 1.397(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.378(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.417(4) . ?
C34 C35 1.458(5) . ?
C35 C36 1.399(5) . ?
C35 C43 1.428(4) . ?
C36 O37 1.375(4) . ?
C36 C39 1.396(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C38 O41 1.439(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.377(5) . ?
C40 O41 1.378(4) . ?
C40 C42 1.394(5) . ?
C42 C43 1.417(5) . ?
C42 C47 1.459(5) . ?
C43 C44 1.459(4) . ?
C44 C45 1.407(5) . ?
C45 C46 1.474(5) . ?
C46 C47 1.406(5) . ?
C46 C51 1.395(5) . ?
C47 C48 1.412(5) . ?
C48 H48 0.9500 . ?
C48 C49 1.374(5) . ?
C49 H49 0.9500 . ?
C49 C50 1.400(5) . ?
C50 H50 0.9500 . ?
C50 C51 1.370(5) . ?
C51 H51 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O37 C1 H1A 109.5 . . ?
O37 C1 H1B 109.5 . . ?
O37 C1 H1C 109.5 . . ?
O1 C2 C3 120.8(3) . . ?
O1 C2 C8 118.4(3) . . ?
C8 C2 C3 120.4(3) . . ?
C4 C3 C2 125.5(3) . . ?
C9 C3 C2 112.2(3) . . ?
C9 C3 C4 122.1(3) . . ?
C3 C4 C5 123.4(3) . . ?
C12 C4 C3 116.1(3) . . ?
C12 C4 C5 119.7(3) . . ?
C6 C5 C4 126.3(3) . . ?
C6 C5 C15 116.5(3) . . ?
C15 C5 C4 117.2(3) . . ?
C5 C6 C7 126.0(3) . . ?
C44 C6 C5 118.6(3) . . ?
C44 C6 C7 115.2(3) . . ?
C8 C7 C6 123.8(3) . . ?
C8 C7 C34 117.2(3) . . ?
C34 C7 C6 118.9(3) . . ?
C7 C8 C2 119.2(3) . . ?
C31 C8 C2 117.8(3) . . ?
C31 C8 C7 122.0(3) . . ?
C3 C9 H9 119.7 . . ?
C3 C9 C10 120.6(4) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.5(4) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 119.1 . . ?
C10 C11 C12 121.7(4) . . ?
C12 C11 H11 119.1 . . ?
C4 C12 C13 120.2(3) . . ?
C11 C12 C4 119.9(3) . . ?
C11 C12 C13 119.6(3) . . ?
C14 C13 C12 119.7(3) . . ?
C14 C13 C16 116.6(3) . . ?
C16 C13 C12 123.5(3) . . ?
C13 C14 C15 118.8(3) . . ?
C13 C14 C23 121.6(3) . . ?
C23 C14 C15 119.6(3) . . ?
C5 C15 C14 120.9(3) . . ?
C26 C15 C5 121.3(3) . . ?
C26 C15 C14 117.8(3) . . ?
O17 C16 C13 116.9(3) . . ?
O17 C16 C19 121.4(3) . . ?
C19 C16 C13 121.7(4) . . ?
C16 O17 C18 118.2(3) . . ?
O17 C18 H18A 109.5 . . ?
O17 C18 H18B 109.5 . . ?
O17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19 120.2 . . ?
C20 C19 C16 119.7(4) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 O21 121.8(3) . . ?
C19 C20 C23 121.7(4) . . ?
O21 C20 C23 116.6(3) . . ?
C20 O21 C22 117.8(3) . . ?
O21 C22 H22A 109.5 . . ?
O21 C22 H22B 109.5 . . ?
O21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C14 C23 C24 120.1(3) . . ?
C20 C23 C14 117.2(3) . . ?
C20 C23 C24 122.7(3) . . ?
C25 C24 C23 118.9(3) . . ?
C25 C24 C27 119.0(3) . . ?
C27 C24 C23 121.9(3) . . ?
C24 C25 C26 119.6(3) . . ?
C30 C25 C24 118.1(3) . . ?
C30 C25 C26 121.5(3) . . ?
C15 C26 C25 120.7(3) . . ?
C15 C26 C45 117.2(3) . . ?
C45 C26 C25 121.2(3) . . ?
C24 C27 H27 119.7 . . ?
C28 C27 C24 120.6(4) . . ?
C28 C27 H27 119.7 . . ?
C27 C28 H28 119.6 . . ?
C29 C28 C27 120.7(4) . . ?
C29 C28 H28 119.6 . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.7(4) . . ?
C30 C29 H29 120.2 . . ?
C25 C30 H30 119.1 . . ?
C29 C30 C25 121.8(3) . . ?
C29 C30 H30 119.1 . . ?
C8 C31 H31 119.8 . . ?
C8 C31 C32 120.3(4) . . ?
C32 C31 H31 119.8 . . ?
C31 C32 H32 120.6 . . ?
C33 C32 C31 118.8(3) . . ?
C33 C32 H32 120.6 . . ?
C32 C33 H33 119.0 . . ?
C32 C33 C34 122.1(3) . . ?
C34 C33 H33 119.0 . . ?
C7 C34 C35 119.9(3) . . ?
C33 C34 C7 117.7(3) . . ?
C33 C34 C35 121.8(3) . . ?
C36 C35 C34 126.4(3) . . ?
C36 C35 C43 116.0(3) . . ?
C43 C35 C34 117.4(3) . . ?
O37 C36 C35 116.9(3) . . ?
O37 C36 C39 121.4(3) . . ?
C39 C36 C35 121.7(3) . . ?
C36 O37 C1 119.6(3) . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O41 C38 H38A 109.5 . . ?
O41 C38 H38B 109.5 . . ?
O41 C38 H38C 109.5 . . ?
C36 C39 H39 120.1 . . ?
C40 C39 C36 119.9(3) . . ?
C40 C39 H39 120.1 . . ?
C39 C40 O41 122.1(3) . . ?
C39 C40 C42 121.9(3) . . ?
O41 C40 C42 115.9(3) . . ?
C40 O41 C38 118.7(3) . . ?
C40 C42 C43 117.1(3) . . ?
C40 C42 C47 125.3(3) . . ?
C43 C42 C47 117.5(3) . . ?
C35 C43 C44 116.8(3) . . ?
C42 C43 C35 122.3(3) . . ?
C42 C43 C44 120.3(3) . . ?
C6 C44 C43 123.1(3) . . ?
C45 C44 C6 121.1(3) . . ?
C45 C44 C43 115.4(3) . . ?
C26 C45 C46 125.5(3) . . ?
C44 C45 C26 116.7(3) . . ?
C44 C45 C46 117.7(3) . . ?
C47 C46 C45 118.6(3) . . ?
C51 C46 C45 120.6(3) . . ?
C51 C46 C47 119.9(3) . . ?
C46 C47 C42 118.3(3) . . ?
C46 C47 C48 118.3(3) . . ?
C48 C47 C42 123.4(3) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 C47 120.7(3) . . ?
C49 C48 H48 119.6 . . ?
C48 C49 H49 119.8 . . ?
C48 C49 C50 120.5(3) . . ?
C50 C49 H49 119.8 . . ?
C49 C50 H50 120.3 . . ?
C51 C50 C49 119.4(3) . . ?
C51 C50 H50 120.3 . . ?
C46 C51 H51 119.4 . . ?
C50 C51 C46 121.2(3) . . ?
C50 C51 H51 119.4 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_6b
_database_code_depnum_ccdc_archive 'CCDC 1485684'
_audit_update_record             
;
2016-06-15 deposited with the CCDC.
2016-08-31 downloaded from the CCDC.
;
_audit_creation_date             2016-06-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H24 O5'
_chemical_formula_sum            'C46 H22 Cl2 O5'
_chemical_formula_weight         725.53
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.664(2)
_cell_length_b                   12.471(2)
_cell_length_c                   13.809(3)
_cell_angle_alpha                116.004(15)
_cell_angle_beta                 114.439(13)
_cell_angle_gamma                91.219(14)
_cell_volume                     1592.3(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1303
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.00
_cell_measurement_theta_min      4.04
_shelx_estimated_absorpt_T_max   0.875
_shelx_estimated_absorpt_T_min   0.804
_exptl_absorpt_coefficient_mu    2.280
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1003 before and 0.0814 after correction.
The Ratio of minimum to maximum transmission is 0.8233.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1897
_diffrn_reflns_av_unetI/netI     0.1312
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31508
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         4.037
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2607
_reflns_number_total             5577
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker Apex3, 2016'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         5577
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0718
_refine_ls_restrained_S_all      0.925
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0826P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1814
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18),
 C25(H25), C34(H34), C40(H40), C41(H41), C42(H42), C43(H43), C48(H48), C49(H49),
  C50(H50), C51(H51)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C33(H33A,H33B,H33C)
;
_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
O1 O 0.1354(3) 0.0472(3) 0.4205(3) 0.0547(9) Uani 1 1 d . . . . .
C2 C 0.0955(4) 0.1354(4) 0.4155(4) 0.0461(12) Uani 1 1 d . . . . .
C3 C 0.0494(4) 0.2167(4) 0.4998(4) 0.0374(11) Uani 1 1 d . . . . .
C4 C 0.0769(4) 0.3462(3) 0.5478(4) 0.0362(11) Uani 1 1 d . . . . .
C5 C 0.1752(4) 0.4154(3) 0.5412(4) 0.0358(10) Uani 1 1 d . . . . .
C6 C 0.1852(4) 0.3795(4) 0.4355(4) 0.0360(11) Uani 1 1 d . . . . .
C8 C 0.0621(4) 0.1526(4) 0.3077(4) 0.0436(12) Uani 1 1 d . . . . .
C9 C -0.0330(5) 0.1615(4) 0.5225(4) 0.0438(12) Uani 1 1 d . . . . .
H9 H -0.0494 0.0749 0.4905 0.053 Uiso 1 1 calc R . . . .
C10 C -0.0925(5) 0.2271(4) 0.5898(4) 0.0460(12) Uani 1 1 d . . . . .
H10 H -0.1457 0.1876 0.6074 0.055 Uiso 1 1 calc R . . . .
C11 C -0.0719(4) 0.3533(4) 0.6311(4) 0.0417(11) Uani 1 1 d . . . . .
H11 H -0.1149 0.4003 0.6742 0.050 Uiso 1 1 calc R . . . .
C12 C 0.0107(4) 0.4106(4) 0.6098(4) 0.0364(11) Uani 1 1 d . . . . .
H12 H 0.0226 0.4966 0.6383 0.044 Uiso 1 1 calc R . . . .
C13 C 0.2531(4) 0.5344(3) 0.6461(4) 0.0325(10) Uani 1 1 d . . . . .
C14 C 0.2809(4) 0.5709(4) 0.7699(4) 0.0354(10) Uani 1 1 d . . . . .
C15 C 0.2850(4) 0.4827(4) 0.8097(4) 0.0389(11) Uani 1 1 d . . . . .
H15 H 0.2622 0.3977 0.7518 0.047 Uiso 1 1 calc R . . . .
C16 C 0.3207(5) 0.5166(4) 0.9281(4) 0.0462(12) Uani 1 1 d . . . . .
H16 H 0.3233 0.4558 0.9523 0.055 Uiso 1 1 calc R . . . .
C17 C 0.3536(5) 0.6420(4) 1.0146(4) 0.0452(12) Uani 1 1 d . . . . .
H17 H 0.3770 0.6661 1.0971 0.054 Uiso 1 1 calc R . . . .
C18 C 0.3520(4) 0.7300(4) 0.9794(4) 0.0387(11) Uani 1 1 d . . . . .
H18 H 0.3740 0.8143 1.0388 0.046 Uiso 1 1 calc R . . . .
C19 C 0.3185(4) 0.6988(4) 0.8581(4) 0.0369(11) Uani 1 1 d . . . . .
C20 C 0.3300(4) 0.7878(3) 0.8212(4) 0.0350(10) Uani 1 1 d . . . . .
C21 C 0.3336(4) 0.7500(3) 0.7110(4) 0.0353(10) Uani 1 1 d . . . . .
C22 C 0.3036(4) 0.6214(3) 0.6275(4) 0.0334(10) Uani 1 1 d . . . . .
C23 C 0.3461(4) 0.9224(4) 0.8981(4) 0.0392(11) Uani 1 1 d . . . . .
O24 O 0.3527(3) 0.9666(2) 0.9997(3) 0.0431(8) Uani 1 1 d . . . . .
C25 C 0.3453(4) 1.0002(4) 0.8446(4) 0.0383(11) Uani 1 1 d . . . . .
H25 H 0.3346 1.0811 0.8823 0.046 Uiso 1 1 calc R . . . .
C26 C 0.3590(4) 0.9619(4) 0.7440(4) 0.0378(11) Uani 1 1 d . . . . .
O27 O 0.3474(3) 1.0241(2) 0.6816(2) 0.0405(8) Uani 1 1 d . . . . .
C28 C 0.3161(5) 1.1406(3) 0.7275(4) 0.0457(12) Uani 1 1 d . . . . .
H28A H 0.3074 1.1752 0.6741 0.069 Uiso 1 1 calc GR . . . .
H28B H 0.3855 1.1970 0.8102 0.069 Uiso 1 1 calc GR . . . .
H28C H 0.2339 1.1293 0.7297 0.069 Uiso 1 1 calc GR . . . .
C29 C 0.3734(4) 0.8370(3) 0.6827(3) 0.0339(10) Uani 1 1 d . . . . .
C30 C 0.4244(4) 0.8002(3) 0.6026(3) 0.0334(10) Uani 1 1 d . . . . .
C31 C 0.5179(4) 0.8846(3) 0.6054(4) 0.0367(11) Uani 1 1 d . . . . .
O32 O 0.5813(3) 0.9889(2) 0.7153(2) 0.0409(8) Uani 1 1 d . . . . .
C33 C 0.6824(5) 1.0732(4) 0.7299(4) 0.0428(12) Uani 1 1 d . . . . .
H33A H 0.6441 1.1038 0.6722 0.064 Uiso 1 1 calc GR . . . .
H33B H 0.7472 1.0301 0.7140 0.064 Uiso 1 1 calc GR . . . .
H33C H 0.7242 1.1426 0.8135 0.064 Uiso 1 1 calc GR . . . .
C34 C 0.5418(4) 0.8518(4) 0.5109(4) 0.0377(11) Uani 1 1 d . . . . .
H34 H 0.6005 0.9088 0.5141 0.045 Uiso 1 1 calc R . . . .
C35 C 0.4801(5) 0.7311(4) 0.4040(4) 0.0420(11) Uani 1 1 d . . . . .
O36 O 0.4837(4) 0.7122(3) 0.3097(3) 0.0590(10) Uani 1 1 d . . . . .
C37 C 0.4168(4) 0.6335(4) 0.4142(4) 0.0352(10) Uani 1 1 d . . . . .
C38 C 0.3915(4) 0.6704(3) 0.5122(4) 0.0340(10) Uani 1 1 d . . . . .
C39 C 0.3825(4) 0.5031(4) 0.3263(3) 0.0348(10) Uani 1 1 d . . . . .
C40 C 0.4157(4) 0.4598(4) 0.2300(4) 0.0392(11) Uani 1 1 d . . . . .
H40 H 0.4526 0.5169 0.2163 0.047 Uiso 1 1 calc R . . . .
C41 C 0.3946(4) 0.3356(4) 0.1567(4) 0.0406(11) Uani 1 1 d . . . . .
H41 H 0.4141 0.3073 0.0906 0.049 Uiso 1 1 calc R . . . .
C42 C 0.3446(4) 0.2507(4) 0.1783(4) 0.0414(11) Uani 1 1 d . . . . .
H42 H 0.3351 0.1653 0.1299 0.050 Uiso 1 1 calc R . . . .
C43 C 0.3095(4) 0.2896(4) 0.2684(4) 0.0386(11) Uani 1 1 d . . . . .
H43 H 0.2768 0.2307 0.2827 0.046 Uiso 1 1 calc R . . . .
C44 C 0.3204(4) 0.4167(3) 0.3418(4) 0.0343(10) Uani 1 1 d . . . . .
C45 C 0.2769(4) 0.4566(4) 0.4321(4) 0.0342(10) Uani 1 1 d . . . . .
C46 C 0.3224(4) 0.5824(3) 0.5225(3) 0.0313(10) Uani 1 1 d . . . . .
C47 C 0.0906(4) 0.2693(4) 0.3180(4) 0.0373(11) Uani 1 1 d . . . . .
C48 C 0.0345(4) 0.2786(4) 0.2127(4) 0.0417(11) Uani 1 1 d . . . . .
H48 H 0.0505 0.3563 0.2175 0.050 Uiso 1 1 calc R . . . .
C49 C -0.0457(5) 0.1745(4) 0.0988(4) 0.0510(13) Uani 1 1 d . . . . .
H49 H -0.0860 0.1830 0.0279 0.061 Uiso 1 1 calc R . . . .
C50 C -0.0662(5) 0.0612(4) 0.0892(4) 0.0516(14) Uani 1 1 d . . . . .
H50 H -0.1174 -0.0094 0.0115 0.062 Uiso 1 1 calc R . . . .
C51 C -0.0126(5) 0.0495(4) 0.1927(4) 0.0505(13) Uani 1 1 d . . . . .
H51 H -0.0265 -0.0294 0.1857 0.061 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.222(5) . ?
C2 C3 1.476(6) . ?
C2 C8 1.489(6) . ?
C3 C4 1.418(5) . ?
C3 C9 1.381(6) . ?
C4 C5 1.477(6) . ?
C4 C12 1.395(6) . ?
C5 C6 1.384(5) . ?
C5 C13 1.447(5) . ?
C6 C45 1.451(6) . ?
C6 C47 1.496(6) . ?
C8 C47 1.417(6) . ?
C8 C51 1.397(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.380(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.394(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.384(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.445(5) . ?
C13 C22 1.390(5) . ?
C14 C15 1.423(6) . ?
C14 C19 1.430(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.361(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.406(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.378(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.412(5) . ?
C19 C20 1.432(6) . ?
C20 C21 1.403(5) . ?
C20 C23 1.496(5) . ?
C21 C22 1.430(5) . ?
C21 C29 1.430(5) . ?
C22 C46 1.427(5) . ?
C23 O24 1.229(4) . ?
C23 C25 1.453(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.337(6) . ?
C26 O27 1.363(5) . ?
C26 C29 1.465(5) . ?
O27 C28 1.432(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.379(5) . ?
C30 C31 1.475(6) . ?
C30 C38 1.460(5) . ?
C31 O32 1.357(4) . ?
C31 C34 1.337(5) . ?
O32 C33 1.448(5) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34 0.9500 . ?
C34 C35 1.445(6) . ?
C35 O36 1.237(5) . ?
C35 C37 1.499(6) . ?
C37 C38 1.386(5) . ?
C37 C39 1.455(5) . ?
C38 C46 1.438(6) . ?
C39 C40 1.420(5) . ?
C39 C44 1.423(6) . ?
C40 H40 0.9500 . ?
C40 C41 1.373(5) . ?
C41 H41 0.9500 . ?
C41 C42 1.394(6) . ?
C42 H42 0.9500 . ?
C42 C43 1.361(6) . ?
C43 H43 0.9500 . ?
C43 C44 1.425(5) . ?
C44 C45 1.433(5) . ?
C45 C46 1.415(5) . ?
C47 C48 1.386(6) . ?
C48 H48 0.9500 . ?
C48 C49 1.405(6) . ?
C49 H49 0.9500 . ?
C49 C50 1.367(6) . ?
C50 H50 0.9500 . ?
C50 C51 1.378(7) . ?
C51 H51 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C2 C3 123.1(4) . . ?
O1 C2 C8 121.8(4) . . ?
C3 C2 C8 113.8(4) . . ?
C4 C3 C2 122.4(4) . . ?
C9 C3 C2 117.5(4) . . ?
C9 C3 C4 119.8(4) . . ?
C3 C4 C5 123.8(4) . . ?
C12 C4 C3 117.0(4) . . ?
C12 C4 C5 119.1(4) . . ?
C6 C5 C4 123.2(4) . . ?
C6 C5 C13 118.4(4) . . ?
C13 C5 C4 117.8(4) . . ?
C5 C6 C45 120.7(4) . . ?
C5 C6 C47 120.9(4) . . ?
C45 C6 C47 118.0(4) . . ?
C47 C8 C2 122.9(4) . . ?
C51 C8 C2 116.8(4) . . ?
C51 C8 C47 119.9(5) . . ?
C3 C9 H9 118.6 . . ?
C3 C9 C10 122.7(4) . . ?
C10 C9 H9 118.6 . . ?
C9 C10 H10 121.2 . . ?
C9 C10 C11 117.7(4) . . ?
C11 C10 H10 121.2 . . ?
C10 C11 H11 119.7 . . ?
C12 C11 C10 120.5(4) . . ?
C12 C11 H11 119.7 . . ?
C4 C12 H12 119.0 . . ?
C11 C12 C4 122.1(4) . . ?
C11 C12 H12 119.0 . . ?
C14 C13 C5 124.7(4) . . ?
C22 C13 C5 118.4(4) . . ?
C22 C13 C14 116.9(4) . . ?
C15 C14 C13 121.3(4) . . ?
C15 C14 C19 118.7(4) . . ?
C19 C14 C13 119.7(4) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 121.9(4) . . ?
C16 C15 H15 119.0 . . ?
C15 C16 H16 120.1 . . ?
C15 C16 C17 119.7(4) . . ?
C17 C16 H16 120.1 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 119.9(4) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 118.9 . . ?
C17 C18 C19 122.1(4) . . ?
C19 C18 H18 118.9 . . ?
C14 C19 C20 118.7(4) . . ?
C18 C19 C14 117.6(4) . . ?
C18 C19 C20 123.6(4) . . ?
C19 C20 C23 123.4(4) . . ?
C21 C20 C19 119.4(3) . . ?
C21 C20 C23 117.1(4) . . ?
C20 C21 C22 119.4(4) . . ?
C20 C21 C29 121.6(4) . . ?
C29 C21 C22 119.0(4) . . ?
C13 C22 C21 120.6(4) . . ?
C13 C22 C46 119.8(4) . . ?
C46 C22 C21 119.6(4) . . ?
O24 C23 C20 122.6(4) . . ?
O24 C23 C25 120.0(4) . . ?
C25 C23 C20 117.2(4) . . ?
C23 C25 H25 118.9 . . ?
C26 C25 C23 122.3(4) . . ?
C26 C25 H25 118.9 . . ?
C25 C26 O27 126.1(4) . . ?
C25 C26 C29 120.0(4) . . ?
O27 C26 C29 113.5(3) . . ?
C26 O27 C28 116.7(3) . . ?
O27 C28 H28A 109.5 . . ?
O27 C28 H28B 109.5 . . ?
O27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C21 C29 C26 116.8(4) . . ?
C30 C29 C21 119.1(4) . . ?
C30 C29 C26 124.1(4) . . ?
C29 C30 C31 123.7(4) . . ?
C29 C30 C38 120.0(4) . . ?
C38 C30 C31 116.2(4) . . ?
O32 C31 C30 112.6(4) . . ?
C34 C31 C30 121.1(4) . . ?
C34 C31 O32 126.0(4) . . ?
C31 O32 C33 116.6(3) . . ?
O32 C33 H33A 109.5 . . ?
O32 C33 H33B 109.5 . . ?
O32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34 119.4 . . ?
C31 C34 C35 121.2(4) . . ?
C35 C34 H34 119.4 . . ?
C34 C35 C37 117.8(4) . . ?
O36 C35 C34 119.2(4) . . ?
O36 C35 C37 123.0(4) . . ?
C38 C37 C35 117.9(4) . . ?
C38 C37 C39 119.5(4) . . ?
C39 C37 C35 122.6(4) . . ?
C37 C38 C30 121.3(4) . . ?
C37 C38 C46 120.7(4) . . ?
C46 C38 C30 117.8(4) . . ?
C40 C39 C37 121.6(4) . . ?
C40 C39 C44 119.4(4) . . ?
C44 C39 C37 118.9(4) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 C39 120.2(4) . . ?
C41 C40 H40 119.9 . . ?
C40 C41 H41 119.7 . . ?
C40 C41 C42 120.6(4) . . ?
C42 C41 H41 119.7 . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.3(4) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 119.2 . . ?
C42 C43 C44 121.6(4) . . ?
C44 C43 H43 119.2 . . ?
C39 C44 C43 117.4(4) . . ?
C39 C44 C45 121.2(3) . . ?
C43 C44 C45 121.4(4) . . ?
C44 C45 C6 125.3(4) . . ?
C46 C45 C6 117.1(4) . . ?
C46 C45 C44 117.5(4) . . ?
C22 C46 C38 119.7(3) . . ?
C45 C46 C22 119.3(4) . . ?
C45 C46 C38 120.9(4) . . ?
C8 C47 C6 122.7(4) . . ?
C48 C47 C6 119.1(4) . . ?
C48 C47 C8 118.0(4) . . ?
C47 C48 H48 119.6 . . ?
C47 C48 C49 120.8(4) . . ?
C49 C48 H48 119.6 . . ?
C48 C49 H49 119.8 . . ?
C50 C49 C48 120.5(5) . . ?
C50 C49 H49 119.8 . . ?
C49 C50 H50 120.1 . . ?
C49 C50 C51 119.9(4) . . ?
C51 C50 H50 120.1 . . ?
C8 C51 H51 119.7 . . ?
C50 C51 C8 120.7(5) . . ?
C50 C51 H51 119.7 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 1.000 198.2 64.4 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_CHEMW03_6b                  
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: During the structure refinement, a region of electron density 
 was identified as a highly disordered molecule of dichloromethane (DCM). 
 Attempts to model this electron density as the DCM molecule 
 were not successful due to the extent of the disorder. In the 
 final structure model, the contribution of the electron density 
 from the DCM molecule has been removed from the intensity data
 using the solvent mask tool in OLEX2 (Dolomanov, O.V., Bourhis, 
 L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.(2009), J. Appl.
 Cryst. 42, 339-341.). The contribution from the DCM has been included
 in the empirical formula to give the correct calculated density, absorption 
 coefficient and molecular weight.
;
_vrf_RINTA01_6b                  
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The quality of the data was poor due to the crystal quality. 
The crystal is very weakly diffracting, so that a large proportion of 
essentially "unobserved" reflections were used in the refinement.
;
_vrf_PLAT020_6b                  
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.190 Report
RESPONSE: see response _vrf_RINTA01
;
####################################################################### 
# 
# 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_6h
_database_code_depnum_ccdc_archive 'CCDC 1485685'
_audit_update_record             
;
2016-06-15 deposited with the CCDC.
2016-08-31 downloaded from the CCDC.
;
_audit_creation_date             2016-06-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C47 H26 O5'
_chemical_formula_sum            'C50 H33 O5'
_chemical_formula_weight         713.76
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.1702(8)
_cell_length_b                   17.3964(12)
_cell_length_c                   17.5084(11)
_cell_angle_alpha                63.486(5)
_cell_angle_beta                 70.365(4)
_cell_angle_gamma                81.999(4)
_cell_volume                     3380.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.45
_cell_measurement_theta_min      2.84
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.932
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1092 before and 0.0818 after correction.
The Ratio of minimum to maximum transmission is 0.7802.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2037
_diffrn_reflns_av_unetI/netI     0.1939
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38935
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.592
_diffrn_reflns_theta_max         66.592
_diffrn_reflns_theta_min         2.839
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4541
_reflns_number_total             11864
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker Apex3, 2016'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.849
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         11864
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1842
_refine_ls_R_factor_gt           0.0779
_refine_ls_restrained_S_all      0.849
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0637P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1873
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C16A(H16A), C22A(H22A), C23A(H23A), C24A(H24A),
 C31A(H31A), C32A(H32A), C33A(H33A), C41A(H41A), C49A(H49A), C50A(H50A),
 C51A(H51A), C4B(H4B), C5B(H5B), C6B(H6B), C16B(H16B), C22B(H22B), C23B(H23B),
 C24B(H24B), C31B(H31B), C32B(H32B), C33B(H33B), C41B(H41B), C49B(H49B),
 C50B(H50B), C51B(H51B)
2.b Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C19A(H19A,H19B,H19C), C40A(H40A,H40B,H40C), C44A(H44A,
 H44B,H44C), C15B(H15D,H15E,H15F), C19B(H19D,H19E,H19F), C40B(H40D,H40E,H40F),
 C44B(H44D,H44E,H44F)
;
_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
O1A O 0.3656(3) 0.8124(2) 1.1034(2) 0.0508(10) Uani 1 1 d . . . . .
C2A C 0.3637(5) 0.8231(3) 1.0291(3) 0.0416(14) Uani 1 1 d . . . . .
C3A C 0.4474(4) 0.8743(3) 0.9465(3) 0.0404(13) Uani 1 1 d . . . . .
C4A C 0.4681(5) 0.9536(4) 0.9389(4) 0.0511(16) Uani 1 1 d . . . . .
H4A H 0.4286 0.9709 0.9849 0.061 Uiso 1 1 calc R . . . .
C5A C 0.5450(5) 1.0072(4) 0.8655(4) 0.0562(17) Uani 1 1 d . . . . .
H5A H 0.5536 1.0643 0.8561 0.067 Uiso 1 1 calc R . . . .
C6A C 0.6101(5) 0.9762(4) 0.8050(3) 0.0486(15) Uani 1 1 d . . . . .
H6A H 0.6668 1.0120 0.7560 0.058 Uiso 1 1 calc R . . . .
C7A C 0.5959(4) 0.8950(3) 0.8133(3) 0.0384(13) Uani 1 1 d . . . . .
C8A C 0.5041(4) 0.8442(3) 0.8808(3) 0.0376(13) Uani 1 1 d . . . . .
C9A C 0.4800(4) 0.7619(3) 0.8845(3) 0.0349(12) Uani 1 1 d . . . . .
C10A C 0.5687(4) 0.7220(3) 0.8436(3) 0.0365(13) Uani 1 1 d . . . . .
C11A C 0.6714(4) 0.7661(3) 0.7879(3) 0.0373(13) Uani 1 1 d . . . . .
C12A C 0.6793(4) 0.8558(3) 0.7604(3) 0.0373(13) Uani 1 1 d . . . . .
C13A C 0.7724(4) 0.8990(3) 0.6918(3) 0.0358(13) Uani 1 1 d . . . . .
O14A O 0.7754(3) 0.9872(2) 0.6596(2) 0.0426(9) Uani 1 1 d . . . . .
C15A C 0.8740(5) 1.0321(3) 0.5919(3) 0.0510(16) Uani 1 1 d . . . . .
H15A H 0.8849 1.0251 0.5372 0.076 Uiso 1 1 calc GR . . . .
H15B H 0.9354 1.0080 0.6146 0.076 Uiso 1 1 calc GR . . . .
H15C H 0.8680 1.0933 0.5784 0.076 Uiso 1 1 calc GR . . . .
C16A C 0.8562(4) 0.8561(3) 0.6574(3) 0.0390(13) Uani 1 1 d . . . . .
H16A H 0.9171 0.8871 0.6096 0.047 Uiso 1 1 calc R . . . .
C17A C 0.8525(5) 0.7680(3) 0.6920(3) 0.0426(14) Uani 1 1 d . . . . .
O18A O 0.9412(3) 0.7247(2) 0.6612(2) 0.0442(10) Uani 1 1 d . . . . .
C19A C 1.0406(5) 0.7702(4) 0.6105(4) 0.0569(17) Uani 1 1 d . . . . .
H19A H 1.0371 0.8116 0.5509 0.085 Uiso 1 1 calc GR . . . .
H19B H 1.0989 0.7297 0.6041 0.085 Uiso 1 1 calc GR . . . .
H19C H 1.0547 0.8008 0.6413 0.085 Uiso 1 1 calc GR . . . .
C20A C 0.7623(4) 0.7199(3) 0.7569(3) 0.0348(13) Uani 1 1 d . . . . .
C21A C 0.7544(4) 0.6261(3) 0.7932(3) 0.0336(12) Uani 1 1 d . . . . .
C22A C 0.8442(5) 0.5738(3) 0.7862(3) 0.0428(14) Uani 1 1 d . . . . .
H22A H 0.9145 0.5986 0.7596 0.051 Uiso 1 1 calc R . . . .
C23A C 0.8314(5) 0.4852(3) 0.8180(3) 0.0434(14) Uani 1 1 d . . . . .
H23A H 0.8933 0.4499 0.8156 0.052 Uiso 1 1 calc R . . . .
C24A C 0.7314(5) 0.4486(3) 0.8523(3) 0.0419(14) Uani 1 1 d . . . . .
H24A H 0.7244 0.3890 0.8701 0.050 Uiso 1 1 calc R . . . .
C25A C 0.6388(5) 0.4987(3) 0.8617(3) 0.0399(14) Uani 1 1 d . . . . .
C26A C 0.6511(4) 0.5868(3) 0.8360(3) 0.0363(13) Uani 1 1 d . . . . .
C27A C 0.5587(4) 0.6359(3) 0.8573(3) 0.0361(13) Uani 1 1 d . . . . .
C28A C 0.4549(5) 0.5997(3) 0.8907(3) 0.0379(13) Uani 1 1 d . . . . .
C29A C 0.4424(5) 0.5133(3) 0.9017(3) 0.0400(14) Uani 1 1 d . . . . .
C30A C 0.5325(5) 0.4617(3) 0.8932(3) 0.0403(14) Uani 1 1 d . . . . .
C31A C 0.5199(5) 0.3762(3) 0.9091(3) 0.0422(14) Uani 1 1 d . . . . .
H31A H 0.5811 0.3412 0.9019 0.051 Uiso 1 1 calc R . . . .
C32A C 0.4194(5) 0.3445(3) 0.9350(3) 0.0482(15) Uani 1 1 d . . . . .
H32A H 0.4111 0.2858 0.9494 0.058 Uiso 1 1 calc R . . . .
C33A C 0.3292(5) 0.3945(3) 0.9411(3) 0.0436(14) Uani 1 1 d . . . . .
H33A H 0.2602 0.3702 0.9586 0.052 Uiso 1 1 calc R . . . .
C34A C 0.3385(4) 0.4810(3) 0.9217(3) 0.0391(13) Uani 1 1 d . . . . .
C35A C 0.2505(5) 0.5412(3) 0.9175(3) 0.0399(14) Uani 1 1 d . . . . .
C36A C 0.2576(5) 0.6203(3) 0.9225(3) 0.0411(14) Uani 1 1 d . . . . .
C37A C 0.3620(4) 0.6472(3) 0.9137(3) 0.0346(13) Uani 1 1 d . . . . .
C38A C 0.1567(5) 0.5299(4) 0.9020(3) 0.0458(15) Uani 1 1 d . . . . .
O39A O 0.1507(3) 0.4569(2) 0.8908(2) 0.0531(11) Uani 1 1 d . . . . .
C40A C 0.0635(5) 0.4483(4) 0.8636(4) 0.0596(17) Uani 1 1 d . . . . .
H40A H 0.0672 0.4953 0.8046 0.089 Uiso 1 1 calc GR . . . .
H40B H -0.0052 0.4505 0.9075 0.089 Uiso 1 1 calc GR . . . .
H40C H 0.0687 0.3931 0.8600 0.089 Uiso 1 1 calc GR . . . .
C41A C 0.0738(5) 0.5891(4) 0.8954(3) 0.0430(14) Uani 1 1 d . . . . .
H41A H 0.0139 0.5807 0.8812 0.052 Uiso 1 1 calc R . . . .
C42A C 0.0793(5) 0.6599(4) 0.9097(3) 0.0437(14) Uani 1 1 d . . . . .
O43A O -0.0020(3) 0.7194(2) 0.9071(2) 0.0459(10) Uani 1 1 d . . . . .
C44A C -0.0833(5) 0.7135(4) 0.8717(4) 0.0550(16) Uani 1 1 d . . . . .
H44A H -0.0497 0.7218 0.8094 0.083 Uiso 1 1 calc GR . . . .
H44B H -0.1373 0.7579 0.8740 0.083 Uiso 1 1 calc GR . . . .
H44C H -0.1182 0.6567 0.9077 0.083 Uiso 1 1 calc GR . . . .
C45A C 0.1706(4) 0.6748(3) 0.9278(3) 0.0372(13) Uani 1 1 d . . . . .
C46A C 0.1740(4) 0.7389(3) 0.9610(3) 0.0393(13) Uani 1 1 d . . . . .
C47A C 0.2735(4) 0.7588(3) 0.9630(3) 0.0386(13) Uani 1 1 d . . . . .
C48A C 0.3753(4) 0.7243(3) 0.9196(3) 0.0372(13) Uani 1 1 d . . . . .
C49A C 0.0772(5) 0.7726(3) 1.0006(3) 0.0474(15) Uani 1 1 d . . . . .
H49A H 0.0117 0.7647 0.9933 0.057 Uiso 1 1 calc R . . . .
C50A C 0.0766(5) 0.8166(4) 1.0496(4) 0.0531(16) Uani 1 1 d . . . . .
H50A H 0.0112 0.8391 1.0755 0.064 Uiso 1 1 calc R . . . .
C51A C 0.1717(5) 0.8280(4) 1.0607(3) 0.0501(16) Uani 1 1 d . . . . .
H51A H 0.1707 0.8544 1.0982 0.060 Uiso 1 1 calc R . . . .
C52A C 0.2684(4) 0.8011(3) 1.0174(3) 0.0384(13) Uani 1 1 d . . . . .
O1B O 0.9811(4) 0.9092(3) 0.1888(2) 0.0590(12) Uani 1 1 d . . . . .
C2B C 0.9795(5) 0.9037(3) 0.2621(3) 0.0437(14) Uani 1 1 d . . . . .
C3B C 0.9149(5) 0.9623(3) 0.2993(3) 0.0443(14) Uani 1 1 d . . . . .
C4B C 0.9299(5) 1.0494(3) 0.2398(3) 0.0466(15) Uani 1 1 d . . . . .
H4B H 0.9736 1.0663 0.1792 0.056 Uiso 1 1 calc R . . . .
C5B C 0.8815(4) 1.1097(3) 0.2692(3) 0.0441(14) Uani 1 1 d . . . . .
H5B H 0.8941 1.1690 0.2301 0.053 Uiso 1 1 calc R . . . .
C6B C 0.8142(5) 1.0841(3) 0.3560(3) 0.0448(14) Uani 1 1 d . . . . .
H6B H 0.7825 1.1269 0.3763 0.054 Uiso 1 1 calc R . . . .
C7B C 0.7905(4) 0.9976(3) 0.4157(3) 0.0362(12) Uani 1 1 d . . . . .
C8B C 0.8490(4) 0.9337(3) 0.3899(3) 0.0412(14) Uani 1 1 d . . . . .
C9B C 0.8254(4) 0.8428(3) 0.4521(3) 0.0351(12) Uani 1 1 d . . . . .
C10B C 0.7248(4) 0.8230(3) 0.5166(3) 0.0358(13) Uani 1 1 d . . . . .
C11B C 0.6556(4) 0.8884(3) 0.5386(3) 0.0357(12) Uani 1 1 d . . . . .
C12B C 0.6990(4) 0.9734(3) 0.4983(3) 0.0390(13) Uani 1 1 d . . . . .
C13B C 0.6425(5) 1.0305(3) 0.5346(3) 0.0392(13) Uani 1 1 d . . . . .
O14B O 0.6880(3) 1.1095(2) 0.5027(2) 0.0437(9) Uani 1 1 d . . . . .
C15B C 0.6307(5) 1.1694(3) 0.5377(4) 0.0522(16) Uani 1 1 d . . . . .
H15D H 0.6732 1.2227 0.5082 0.078 Uiso 1 1 calc GR . . . .
H15E H 0.6190 1.1444 0.6025 0.078 Uiso 1 1 calc GR . . . .
H15F H 0.5610 1.1820 0.5262 0.078 Uiso 1 1 calc GR . . . .
C16B C 0.5442(5) 1.0065(4) 0.6033(3) 0.0432(14) Uani 1 1 d . . . . .
H16B H 0.5073 1.0459 0.6270 0.052 Uiso 1 1 calc R . . . .
C17B C 0.5014(4) 0.9274(4) 0.6363(3) 0.0431(14) Uani 1 1 d . . . . .
O18B O 0.4059(3) 0.9019(2) 0.7053(2) 0.0481(10) Uani 1 1 d . . . . .
C19B C 0.3517(5) 0.9617(4) 0.7407(4) 0.0514(16) Uani 1 1 d . . . . .
H19D H 0.3295 1.0114 0.6940 0.077 Uiso 1 1 calc GR . . . .
H19E H 0.4005 0.9808 0.7607 0.077 Uiso 1 1 calc GR . . . .
H19F H 0.2879 0.9338 0.7917 0.077 Uiso 1 1 calc GR . . . .
C20B C 0.5534(4) 0.8653(3) 0.6046(3) 0.0366(13) Uani 1 1 d . . . . .
C21B C 0.5068(5) 0.7805(3) 0.6353(3) 0.0419(14) Uani 1 1 d . . . . .
C22B C 0.3973(5) 0.7618(4) 0.6770(3) 0.0440(14) Uani 1 1 d . . . . .
H22B H 0.3499 0.8043 0.6890 0.053 Uiso 1 1 calc R . . . .
C23B C 0.3562(5) 0.6823(4) 0.7012(3) 0.0415(14) Uani 1 1 d . . . . .
H23B H 0.2805 0.6720 0.7261 0.050 Uiso 1 1 calc R . . . .
C24B C 0.4244(5) 0.6177(4) 0.6895(3) 0.0450(15) Uani 1 1 d . . . . .
H24B H 0.3952 0.5630 0.7078 0.054 Uiso 1 1 calc R . . . .
C25B C 0.5351(5) 0.6318(3) 0.6514(3) 0.0406(14) Uani 1 1 d . . . . .
C26B C 0.5759(4) 0.7163(3) 0.6182(3) 0.0376(13) Uani 1 1 d . . . . .
C27B C 0.6881(4) 0.7359(3) 0.5665(3) 0.0349(12) Uani 1 1 d . . . . .
C28B C 0.7605(4) 0.6687(3) 0.5647(3) 0.0345(13) Uani 1 1 d . . . . .
C29B C 0.7224(4) 0.5814(3) 0.6106(3) 0.0379(13) Uani 1 1 d . . . . .
C30B C 0.6104(5) 0.5631(3) 0.6470(3) 0.0417(14) Uani 1 1 d . . . . .
C31B C 0.5768(5) 0.4777(4) 0.6811(3) 0.0475(15) Uani 1 1 d . . . . .
H31B H 0.5018 0.4647 0.7039 0.057 Uiso 1 1 calc R . . . .
C32B C 0.6496(5) 0.4120(4) 0.6825(3) 0.0521(17) Uani 1 1 d . . . . .
H32B H 0.6250 0.3554 0.7024 0.063 Uiso 1 1 calc R . . . .
C33B C 0.7589(5) 0.4295(3) 0.6546(3) 0.0458(15) Uani 1 1 d . . . . .
H33B H 0.8086 0.3837 0.6597 0.055 Uiso 1 1 calc R . . . .
C34B C 0.7977(5) 0.5137(3) 0.6190(3) 0.0410(14) Uani 1 1 d . . . . .
C35B C 0.9126(5) 0.5338(3) 0.5932(3) 0.0397(14) Uani 1 1 d . . . . .
C36B C 0.9501(5) 0.6212(3) 0.5371(3) 0.0381(13) Uani 1 1 d . . . . .
C37B C 0.8713(4) 0.6884(3) 0.5169(3) 0.0353(12) Uani 1 1 d . . . . .
C38B C 0.9887(5) 0.4731(3) 0.6250(3) 0.0402(14) Uani 1 1 d . . . . .
O39B O 0.9564(3) 0.3894(2) 0.6774(2) 0.0513(11) Uani 1 1 d . . . . .
C40B C 1.0321(6) 0.3257(4) 0.7120(4) 0.0614(18) Uani 1 1 d . . . . .
H40D H 1.0950 0.3261 0.6621 0.092 Uiso 1 1 calc GR . . . .
H40E H 0.9975 0.2688 0.7449 0.092 Uiso 1 1 calc GR . . . .
H40F H 1.0552 0.3390 0.7526 0.092 Uiso 1 1 calc GR . . . .
C41B C 1.0939(5) 0.4972(3) 0.6060(3) 0.0462(15) Uani 1 1 d . . . . .
H41B H 1.1427 0.4558 0.6311 0.055 Uiso 1 1 calc R . . . .
C42B C 1.1277(5) 0.5828(3) 0.5496(3) 0.0432(14) Uani 1 1 d . . . . .
O43B O 1.2295(3) 0.6076(2) 0.5355(2) 0.0505(10) Uani 1 1 d . . . . .
C44B C 1.3076(5) 0.5431(4) 0.5633(5) 0.0697(19) Uani 1 1 d . . . . .
H44D H 1.3785 0.5704 0.5400 0.104 Uiso 1 1 calc GR . . . .
H44E H 1.3112 0.5009 0.5397 0.104 Uiso 1 1 calc GR . . . .
H44F H 1.2861 0.5142 0.6290 0.104 Uiso 1 1 calc GR . . . .
C45B C 1.0580(5) 0.6433(3) 0.5093(3) 0.0380(13) Uani 1 1 d . . . . .
C46B C 1.0951(4) 0.7275(3) 0.4325(3) 0.0376(13) Uani 1 1 d . . . . .
C47B C 1.0170(5) 0.7867(3) 0.3978(3) 0.0379(13) Uani 1 1 d . . . . .
C48B C 0.9022(4) 0.7742(3) 0.4540(3) 0.0350(12) Uani 1 1 d . . . . .
C49B C 1.2057(4) 0.7458(3) 0.3819(3) 0.0425(14) Uani 1 1 d . . . . .
H49B H 1.2588 0.7099 0.4064 0.051 Uiso 1 1 calc R . . . .
C50B C 1.2384(5) 0.8134(3) 0.2992(4) 0.0424(14) Uani 1 1 d . . . . .
H50B H 1.3129 0.8263 0.2686 0.051 Uiso 1 1 calc R . . . .
C51B C 1.1625(5) 0.8625(4) 0.2606(3) 0.0454(15) Uani 1 1 d . . . . .
H51B H 1.1845 0.9055 0.2005 0.055 Uiso 1 1 calc R . . . .
C52B C 1.0543(5) 0.8494(3) 0.3090(3) 0.0445(14) 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
O1A C2A 1.238(6) . ?
C2A C3A 1.467(7) . ?
C2A C52A 1.463(8) . ?
C3A C4A 1.382(7) . ?
C3A C8A 1.417(7) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.366(8) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.384(8) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.387(7) . ?
C7A C8A 1.430(7) . ?
C7A C12A 1.484(7) . ?
C8A C9A 1.478(7) . ?
C9A C10A 1.420(7) . ?
C9A C48A 1.425(7) . ?
C10A C11A 1.449(7) . ?
C10A C27A 1.424(7) . ?
C11A C12A 1.422(7) . ?
C11A C20A 1.435(7) . ?
C12A C13A 1.403(7) . ?
C13A O14A 1.380(6) . ?
C13A C16A 1.365(7) . ?
O14A C15A 1.456(6) . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C16A H16A 0.9500 . ?
C16A C17A 1.374(7) . ?
C17A O18A 1.385(6) . ?
C17A C20A 1.387(7) . ?
O18A C19A 1.418(6) . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C20A C21A 1.468(7) . ?
C21A C22A 1.393(8) . ?
C21A C26A 1.413(7) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.400(7) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.363(8) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.403(8) . ?
C25A C26A 1.409(7) . ?
C25A C30A 1.447(8) . ?
C26A C27A 1.428(7) . ?
C27A C28A 1.409(7) . ?
C28A C29A 1.452(7) . ?
C28A C37A 1.423(8) . ?
C29A C30A 1.394(8) . ?
C29A C34A 1.423(7) . ?
C30A C31A 1.408(7) . ?
C31A H31A 0.9500 . ?
C31A C32A 1.356(8) . ?
C32A H32A 0.9500 . ?
C32A C33A 1.373(8) . ?
C33A H33A 0.9500 . ?
C33A C34A 1.402(7) . ?
C34A C35A 1.447(8) . ?
C35A C36A 1.436(7) . ?
C35A C38A 1.405(8) . ?
C36A C37A 1.451(8) . ?
C36A C45A 1.387(8) . ?
C37A C48A 1.430(7) . ?
C38A O39A 1.385(7) . ?
C38A C41A 1.390(8) . ?
O39A C40A 1.432(7) . ?
C40A H40A 0.9800 . ?
C40A H40B 0.9800 . ?
C40A H40C 0.9800 . ?
C41A H41A 0.9500 . ?
C41A C42A 1.378(8) . ?
C42A O43A 1.379(7) . ?
C42A C45A 1.425(8) . ?
O43A C44A 1.440(7) . ?
C44A H44A 0.9800 . ?
C44A H44B 0.9800 . ?
C44A H44C 0.9800 . ?
C45A C46A 1.480(7) . ?
C46A C47A 1.417(8) . ?
C46A C49A 1.419(8) . ?
C47A C48A 1.493(7) . ?
C47A C52A 1.422(7) . ?
C49A H49A 0.9500 . ?
C49A C50A 1.379(8) . ?
C50A H50A 0.9500 . ?
C50A C51A 1.384(8) . ?
C51A H51A 0.9500 . ?
C51A C52A 1.385(7) . ?
O1B C2B 1.236(6) . ?
C2B C3B 1.472(8) . ?
C2B C52B 1.459(8) . ?
C3B C4B 1.398(7) . ?
C3B C8B 1.417(7) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.358(7) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.377(7) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.400(7) . ?
C7B C8B 1.418(7) . ?
C7B C12B 1.466(7) . ?
C8B C9B 1.468(7) . ?
C9B C10B 1.387(7) . ?
C9B C48B 1.448(7) . ?
C10B C11B 1.463(7) . ?
C10B C27B 1.425(7) . ?
C11B C12B 1.430(7) . ?
C11B C20B 1.414(7) . ?
C12B C13B 1.408(7) . ?
C13B O14B 1.370(6) . ?
C13B C16B 1.397(7) . ?
O14B C15B 1.440(6) . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
C16B H16B 0.9500 . ?
C16B C17B 1.354(8) . ?
C17B O18B 1.376(6) . ?
C17B C20B 1.422(7) . ?
O18B C19B 1.430(6) . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
C20B C21B 1.471(7) . ?
C21B C22B 1.388(8) . ?
C21B C26B 1.414(8) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.385(8) . ?
C23B H23B 0.9500 . ?
C23B C24B 1.382(8) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.390(8) . ?
C25B C26B 1.427(7) . ?
C25B C30B 1.455(8) . ?
C26B C27B 1.444(7) . ?
C27B C28B 1.408(7) . ?
C28B C29B 1.433(7) . ?
C28B C37B 1.418(7) . ?
C29B C30B 1.416(8) . ?
C29B C34B 1.418(8) . ?
C30B C31B 1.404(8) . ?
C31B H31B 0.9500 . ?
C31B C32B 1.383(8) . ?
C32B H32B 0.9500 . ?
C32B C33B 1.385(9) . ?
C33B H33B 0.9500 . ?
C33B C34B 1.404(7) . ?
C34B C35B 1.470(8) . ?
C35B C36B 1.440(7) . ?
C35B C38B 1.409(8) . ?
C36B C37B 1.451(7) . ?
C36B C45B 1.387(8) . ?
C37B C48B 1.418(7) . ?
C38B O39B 1.363(6) . ?
C38B C41B 1.391(8) . ?
O39B C40B 1.445(7) . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C41B H41B 0.9500 . ?
C41B C42B 1.402(7) . ?
C42B O43B 1.374(7) . ?
C42B C45B 1.397(8) . ?
O43B C44B 1.442(7) . ?
C44B H44D 0.9800 . ?
C44B H44E 0.9800 . ?
C44B H44F 0.9800 . ?
C45B C46B 1.481(7) . ?
C46B C47B 1.433(8) . ?
C46B C49B 1.420(7) . ?
C47B C48B 1.484(7) . ?
C47B C52B 1.404(7) . ?
C49B H49B 0.9500 . ?
C49B C50B 1.367(7) . ?
C50B H50B 0.9500 . ?
C50B C51B 1.372(8) . ?
C51B H51B 0.9500 . ?
C51B C52B 1.382(8) . ?

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
O1A C2A C3A 121.1(5) . . ?
O1A C2A C52A 121.7(5) . . ?
C52A C2A C3A 116.1(4) . . ?
C4A C3A C2A 114.6(5) . . ?
C4A C3A C8A 122.7(5) . . ?
C8A C3A C2A 122.7(5) . . ?
C3A C4A H4A 119.8 . . ?
C5A C4A C3A 120.3(5) . . ?
C5A C4A H4A 119.8 . . ?
C4A C5A H5A 120.8 . . ?
C4A C5A C6A 118.5(5) . . ?
C6A C5A H5A 120.8 . . ?
C5A C6A H6A 118.7 . . ?
C5A C6A C7A 122.5(5) . . ?
C7A C6A H6A 118.7 . . ?
C6A C7A C8A 119.3(5) . . ?
C6A C7A C12A 121.6(5) . . ?
C8A C7A C12A 118.8(4) . . ?
C3A C8A C7A 115.2(5) . . ?
C3A C8A C9A 124.0(4) . . ?
C7A C8A C9A 120.5(4) . . ?
C10A C9A C8A 115.8(4) . . ?
C10A C9A C48A 119.0(5) . . ?
C48A C9A C8A 125.0(5) . . ?
C9A C10A C11A 121.9(5) . . ?
C9A C10A C27A 120.0(5) . . ?
C27A C10A C11A 118.0(5) . . ?
C12A C11A C10A 119.5(5) . . ?
C12A C11A C20A 120.6(5) . . ?
C20A C11A C10A 119.8(5) . . ?
C11A C12A C7A 117.8(4) . . ?
C13A C12A C7A 124.4(5) . . ?
C13A C12A C11A 117.4(5) . . ?
O14A C13A C12A 117.2(4) . . ?
C16A C13A C12A 121.7(5) . . ?
C16A C13A O14A 121.1(4) . . ?
C13A O14A C15A 117.5(4) . . ?
O14A C15A H15A 109.5 . . ?
O14A C15A H15B 109.5 . . ?
O14A C15A H15C 109.5 . . ?
H15A C15A H15B 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C13A C16A H16A 119.9 . . ?
C13A C16A C17A 120.1(5) . . ?
C17A C16A H16A 120.0 . . ?
C16A C17A O18A 119.6(5) . . ?
C16A C17A C20A 122.5(5) . . ?
O18A C17A C20A 117.9(5) . . ?
C17A O18A C19A 118.1(4) . . ?
O18A C19A H19A 109.5 . . ?
O18A C19A H19B 109.5 . . ?
O18A C19A H19C 109.5 . . ?
H19A C19A H19B 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C11A C20A C21A 119.1(4) . . ?
C17A C20A C11A 117.0(5) . . ?
C17A C20A C21A 123.9(5) . . ?
C22A C21A C20A 123.0(5) . . ?
C22A C21A C26A 118.3(5) . . ?
C26A C21A C20A 118.7(5) . . ?
C21A C22A H22A 119.8 . . ?
C21A C22A C23A 120.4(5) . . ?
C23A C22A H22A 119.8 . . ?
C22A C23A H23A 119.5 . . ?
C24A C23A C22A 121.0(6) . . ?
C24A C23A H23A 119.5 . . ?
C23A C24A H24A 119.8 . . ?
C23A C24A C25A 120.4(5) . . ?
C25A C24A H24A 119.8 . . ?
C24A C25A C26A 118.9(5) . . ?
C24A C25A C30A 120.9(5) . . ?
C26A C25A C30A 120.2(5) . . ?
C21A C26A C27A 119.8(5) . . ?
C25A C26A C21A 120.6(5) . . ?
C25A C26A C27A 119.6(5) . . ?
C10A C27A C26A 121.5(5) . . ?
C28A C27A C10A 118.8(5) . . ?
C28A C27A C26A 119.6(5) . . ?
C27A C28A C29A 119.9(5) . . ?
C27A C28A C37A 120.4(5) . . ?
C37A C28A C29A 119.8(5) . . ?
C30A C29A C28A 119.8(5) . . ?
C30A C29A C34A 119.9(5) . . ?
C34A C29A C28A 120.3(5) . . ?
C29A C30A C25A 119.3(5) . . ?
C29A C30A C31A 119.9(5) . . ?
C31A C30A C25A 120.7(5) . . ?
C30A C31A H31A 120.3 . . ?
C32A C31A C30A 119.3(6) . . ?
C32A C31A H31A 120.3 . . ?
C31A C32A H32A 118.9 . . ?
C31A C32A C33A 122.3(5) . . ?
C33A C32A H32A 118.9 . . ?
C32A C33A H33A 119.9 . . ?
C32A C33A C34A 120.3(5) . . ?
C34A C33A H33A 119.9 . . ?
C29A C34A C35A 117.3(5) . . ?
C33A C34A C29A 118.1(5) . . ?
C33A C34A C35A 124.7(5) . . ?
C36A C35A C34A 121.2(5) . . ?
C38A C35A C34A 123.2(5) . . ?
C38A C35A C36A 115.5(5) . . ?
C35A C36A C37A 118.3(5) . . ?
C45A C36A C35A 122.2(5) . . ?
C45A C36A C37A 119.3(5) . . ?
C28A C37A C36A 119.0(4) . . ?
C28A C37A C48A 119.1(5) . . ?
C48A C37A C36A 121.6(5) . . ?
O39A C38A C35A 116.8(5) . . ?
O39A C38A C41A 120.1(5) . . ?
C41A C38A C35A 123.0(5) . . ?
C38A O39A C40A 118.7(5) . . ?
O39A C40A H40A 109.5 . . ?
O39A C40A H40B 109.5 . . ?
O39A C40A H40C 109.5 . . ?
H40A C40A H40B 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C38A C41A H41A 120.3 . . ?
C42A C41A C38A 119.4(6) . . ?
C42A C41A H41A 120.3 . . ?
C41A C42A C45A 120.8(6) . . ?
O43A C42A C41A 122.2(5) . . ?
O43A C42A C45A 116.9(5) . . ?
C42A O43A C44A 116.4(4) . . ?
O43A C44A H44A 109.5 . . ?
O43A C44A H44B 109.5 . . ?
O43A C44A H44C 109.5 . . ?
H44A C44A H44B 109.5 . . ?
H44A C44A H44C 109.5 . . ?
H44B C44A H44C 109.5 . . ?
C36A C45A C42A 117.9(5) . . ?
C36A C45A C46A 117.7(5) . . ?
C42A C45A C46A 124.0(5) . . ?
C47A C46A C45A 119.6(5) . . ?
C49A C46A C45A 120.4(5) . . ?
C49A C46A C47A 119.6(5) . . ?
C46A C47A C48A 119.2(5) . . ?
C46A C47A C52A 116.8(5) . . ?
C52A C47A C48A 123.4(5) . . ?
C9A C48A C37A 119.4(5) . . ?
C9A C48A C47A 125.8(5) . . ?
C37A C48A C47A 114.7(5) . . ?
C46A C49A H49A 119.5 . . ?
C50A C49A C46A 121.1(6) . . ?
C50A C49A H49A 119.5 . . ?
C49A C50A H50A 120.2 . . ?
C49A C50A C51A 119.7(6) . . ?
C51A C50A H50A 120.2 . . ?
C50A C51A H51A 119.9 . . ?
C52A C51A C50A 120.2(5) . . ?
C52A C51A H51A 119.9 . . ?
C47A C52A C2A 123.4(5) . . ?
C51A C52A C2A 114.6(5) . . ?
C51A C52A C47A 121.9(5) . . ?
O1B C2B C3B 121.5(5) . . ?
O1B C2B C52B 122.0(5) . . ?
C52B C2B C3B 115.7(5) . . ?
C4B C3B C2B 114.5(4) . . ?
C4B C3B C8B 122.4(5) . . ?
C8B C3B C2B 122.9(5) . . ?
C3B C4B H4B 120.2 . . ?
C5B C4B C3B 119.6(5) . . ?
C5B C4B H4B 120.2 . . ?
C4B C5B H5B 120.2 . . ?
C4B C5B C6B 119.5(5) . . ?
C6B C5B H5B 120.2 . . ?
C5B C6B H6B 118.7 . . ?
C5B C6B C7B 122.6(5) . . ?
C7B C6B H6B 118.7 . . ?
C6B C7B C8B 118.6(4) . . ?
C6B C7B C12B 120.7(5) . . ?
C8B C7B C12B 120.3(4) . . ?
C3B C8B C7B 116.5(5) . . ?
C3B C8B C9B 123.6(5) . . ?
C7B C8B C9B 119.1(4) . . ?
C10B C9B C8B 117.0(5) . . ?
C10B C9B C48B 118.5(4) . . ?
C48B C9B C8B 124.4(5) . . ?
C9B C10B C11B 122.2(5) . . ?
C9B C10B C27B 119.8(5) . . ?
C27B C10B C11B 117.9(4) . . ?
C12B C11B C10B 117.9(4) . . ?
C20B C11B C10B 120.3(4) . . ?
C20B C11B C12B 121.5(5) . . ?
C11B C12B C7B 117.3(4) . . ?
C13B C12B C7B 124.7(5) . . ?
C13B C12B C11B 117.5(5) . . ?
O14B C13B C12B 118.3(5) . . ?
O14B C13B C16B 120.6(5) . . ?
C16B C13B C12B 121.0(5) . . ?
C13B O14B C15B 119.2(4) . . ?
O14B C15B H15D 109.5 . . ?
O14B C15B H15E 109.5 . . ?
O14B C15B H15F 109.5 . . ?
H15D C15B H15E 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C13B C16B H16B 119.9 . . ?
C17B C16B C13B 120.3(5) . . ?
C17B C16B H16B 119.9 . . ?
C16B C17B O18B 121.2(5) . . ?
C16B C17B C20B 122.5(5) . . ?
O18B C17B C20B 116.3(5) . . ?
C17B O18B C19B 118.3(4) . . ?
O18B C19B H19D 109.5 . . ?
O18B C19B H19E 109.5 . . ?
O18B C19B H19F 109.5 . . ?
H19D C19B H19E 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C11B C20B C17B 116.8(5) . . ?
C11B C20B C21B 119.1(5) . . ?
C17B C20B C21B 124.0(5) . . ?
C22B C21B C20B 123.0(5) . . ?
C22B C21B C26B 118.5(5) . . ?
C26B C21B C20B 118.5(5) . . ?
C21B C22B H22B 119.5 . . ?
C23B C22B C21B 121.1(5) . . ?
C23B C22B H22B 119.5 . . ?
C22B C23B H23B 119.8 . . ?
C24B C23B C22B 120.5(5) . . ?
C24B C23B H23B 119.8 . . ?
C23B C24B H24B 119.6 . . ?
C23B C24B C25B 120.8(5) . . ?
C25B C24B H24B 119.6 . . ?
C24B C25B C26B 118.3(5) . . ?
C24B C25B C30B 122.4(5) . . ?
C26B C25B C30B 119.2(5) . . ?
C21B C26B C25B 120.2(5) . . ?
C21B C26B C27B 120.3(5) . . ?
C25B C26B C27B 119.5(5) . . ?
C10B C27B C26B 120.1(5) . . ?
C28B C27B C10B 120.3(5) . . ?
C28B C27B C26B 119.7(5) . . ?
C27B C28B C29B 120.3(5) . . ?
C27B C28B C37B 119.2(4) . . ?
C37B C28B C29B 120.5(5) . . ?
C30B C29B C28B 120.1(5) . . ?
C30B C29B C34B 120.3(5) . . ?
C34B C29B C28B 119.6(5) . . ?
C29B C30B C25B 119.3(5) . . ?
C31B C30B C25B 122.6(5) . . ?
C31B C30B C29B 118.0(5) . . ?
C30B C31B H31B 119.0 . . ?
C32B C31B C30B 122.0(6) . . ?
C32B C31B H31B 119.0 . . ?
C31B C32B H32B 120.3 . . ?
C31B C32B C33B 119.4(5) . . ?
C33B C32B H32B 120.3 . . ?
C32B C33B H33B 119.3 . . ?
C32B C33B C34B 121.3(6) . . ?
C34B C33B H33B 119.3 . . ?
C29B C34B C35B 118.8(5) . . ?
C33B C34B C29B 118.5(5) . . ?
C33B C34B C35B 122.6(5) . . ?
C36B C35B C34B 119.2(5) . . ?
C38B C35B C34B 123.8(5) . . ?
C38B C35B C36B 116.8(5) . . ?
C35B C36B C37B 118.7(5) . . ?
C45B C36B C35B 121.5(5) . . ?
C45B C36B C37B 119.5(5) . . ?
C28B C37B C36B 119.1(4) . . ?
C48B C37B C28B 118.8(5) . . ?
C48B C37B C36B 121.9(5) . . ?
O39B C38B C35B 118.5(5) . . ?
O39B C38B C41B 120.0(5) . . ?
C41B C38B C35B 121.5(5) . . ?
C38B O39B C40B 119.9(5) . . ?
O39B C40B H40D 109.5 . . ?
O39B C40B H40E 109.5 . . ?
O39B C40B H40F 109.5 . . ?
H40D C40B H40E 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C38B C41B H41B 120.1 . . ?
C38B C41B C42B 119.7(6) . . ?
C42B C41B H41B 120.1 . . ?
O43B C42B C41B 119.6(5) . . ?
O43B C42B C45B 119.8(5) . . ?
C45B C42B C41B 120.6(6) . . ?
C42B O43B C44B 119.6(5) . . ?
O43B C44B H44D 109.5 . . ?
O43B C44B H44E 109.5 . . ?
O43B C44B H44F 109.5 . . ?
H44D C44B H44E 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H44E C44B H44F 109.5 . . ?
C36B C45B C42B 118.8(5) . . ?
C36B C45B C46B 117.8(5) . . ?
C42B C45B C46B 123.1(5) . . ?
C47B C46B C45B 119.0(5) . . ?
C49B C46B C45B 122.0(5) . . ?
C49B C46B C47B 118.0(5) . . ?
C46B C47B C48B 119.0(4) . . ?
C52B C47B C46B 116.7(5) . . ?
C52B C47B C48B 124.2(5) . . ?
C9B C48B C47B 124.8(4) . . ?
C37B C48B C9B 120.0(5) . . ?
C37B C48B C47B 115.1(5) . . ?
C46B C49B H49B 118.9 . . ?
C50B C49B C46B 122.1(6) . . ?
C50B C49B H49B 118.9 . . ?
C49B C50B H50B 120.3 . . ?
C49B C50B C51B 119.5(5) . . ?
C51B C50B H50B 120.3 . . ?
C50B C51B H51B 120.0 . . ?
C50B C51B C52B 120.1(5) . . ?
C52B C51B H51B 120.0 . . ?
C47B C52B C2B 121.2(5) . . ?
C51B C52B C2B 116.2(5) . . ?
C51B C52B C47B 122.5(6) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 591.8 128.4 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_CHEMW03_6h                  
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: During the structure refinement, a region of electron density 
 was identified as a highly disordered molecule of hexane. 
 Attempts to model this electron density as the hexane molecule 
 were not successful due to the extent of the disorder. In the 
 final structure model, the contribution of the electron density 
 from the hexane molecule has been removed from the intensity data
 using the solvent mask tool in OLEX2 (Dolomanov, O.V., Bourhis, 
 L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.(2009), J. Appl.
 Cryst. 42, 339-341.). The contribution from the hexane has been included
 in the empirical formula to give the correct calculated density, absorption 
 coefficient and molecular weight.
;
_vrf_RINTA01_6h                  
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The quality of the data was poor due to the crystal quality. The crystal is very weakly 
diffracting, so that a large proportion of essentially "unobserved" reflections were used in the 
refinement.
;
_vrf_PLAT020_6h                  
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.204 Report
RESPONSE: The quality of the data was poor due to the crystal quality. The crystal is very weakly 
diffracting, so that a large proportion of essentially "unobserved" reflections were used in the 
refinement.
;
_vrf_PLAT026_6h                  
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         38 %     
RESPONSE: The quality of the data was poor due to the crystal quality. The crystal is very weakly 
diffracting, so that a large proportion of essentially "unobserved" reflections were used in the 
refinement.
;
# end Validation Reply Form

