# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

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

data_1_acetone
_database_code_depnum_ccdc_archive 'CCDC 1556028'
_audit_update_record             
;
2017-06-14 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_1_acetone           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          21 Note  
RESPONSE: The reason here causing 21 missing FCF reflections below
Theta-min is beamstop theta-min limit set at too high angle.
;
# end Validation Reply Form
_audit_creation_date             2017-05-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H68 Br4 O8, C3 H6 O'
_chemical_formula_sum            'C67 H74 Br4 O9'
_chemical_formula_weight         1342.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H50 O8 Br4 N2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.1022(10)
_cell_length_b                   24.4684(11)
_cell_length_c                   18.3507(13)
_cell_angle_alpha                90
_cell_angle_beta                 98.970(7)
_cell_angle_gamma                90
_cell_volume                     6254.6(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3816
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      21.8800
_cell_measurement_theta_min      3.3890
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.629
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.1151
_exptl_crystal_size_min          0.1043
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0906
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21217
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         3.041
_diffrn_ambient_temperature      '170.00 (10)'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9654
_diffrn_measured_fraction_theta_max 0.8367
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -87.00   53.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6023    0.0000  -60.0000 140

#__ type_ start__ end____ width___ exp.time_
  2 omega   43.00   94.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8523  178.0000   90.0000 51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0373866000
_diffrn_orient_matrix_UB_12      -0.0085280000
_diffrn_orient_matrix_UB_13      0.0281414000
_diffrn_orient_matrix_UB_21      -0.0331149000
_diffrn_orient_matrix_UB_22      -0.0163918000
_diffrn_orient_matrix_UB_23      0.0156482000
_diffrn_orient_matrix_UB_31      0.0100239000
_diffrn_orient_matrix_UB_32      -0.0223331000
_diffrn_orient_matrix_UB_33      -0.0222177000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6181
_reflns_number_total             11207
_reflns_odcompleteness_completeness 96.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.906
_refine_diff_density_min         -1.811
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         11207
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.1594
_refine_ls_R_factor_gt           0.0890
_refine_ls_restrained_S_all      1.022
_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)+(0.1202P)²+30.3108P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2722
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C50-C49 \\sim C51-C50 \\sim C51-C52
 with sigma of 0.01
 C57-C56 \\sim C57B-C56 \\sim C58B-C57B \\sim C58-C57
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C57) \\sim Ueq, Uanis(C58B) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(Br2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H56C)=Sof(H56D)=Sof(C57B)=Sof(H57C)=Sof(H57D)=Sof(C58B)=Sof(H58D)=
 Sof(H58E)=Sof(H58F)=1-FVAR(1)
 Sof(H56A)=Sof(H56B)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(C58)=Sof(H58A)=Sof(H58B)=
 Sof(H58C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C19(H19), C29(H29), C39(H39)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C30(H30A,H30B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
  C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C56(H56C,
 H56D), C57(H57A,H57B), C57B(H57C,H57D), C59(H59A,H59B), C60(H60A,H60B),
 C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C22(H22), C32(H32)
5.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C58(H58A,H58B,H58C), C58B(H58D,H58E,
 H58F), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.03384(7) 0.07072(4) 0.35616(7) 0.0697(4) Uani 1 1 d . . . . .
Br2 Br 0.36668(11) -0.01622(5) 0.01774(8) 0.1008(6) Uani 1 1 d . U . . .
Br3 Br 0.80211(9) -0.14977(4) 0.33900(9) 0.0883(5) Uani 1 1 d . . . . .
Br4 Br 0.47522(8) -0.08013(4) 0.64199(6) 0.0605(3) Uani 1 1 d . . . . .
C1 C 0.4315(6) 0.2146(3) 0.4513(5) 0.044(2) Uani 1 1 d . . . . .
C2 C 0.4596(6) 0.2358(3) 0.3886(5) 0.045(2) Uani 1 1 d . . . . .
H2 H 0.5175 0.2562 0.3932 0.054 Uiso 1 1 calc R . . . .
C3 C 0.4070(6) 0.2287(3) 0.3190(5) 0.044(2) Uani 1 1 d . . . . .
C4 C 0.3236(6) 0.1976(3) 0.3128(5) 0.043(2) Uani 1 1 d . . . . .
C5 C 0.2925(6) 0.1743(3) 0.3747(6) 0.047(2) Uani 1 1 d . . . . .
C6 C 0.3490(6) 0.1837(4) 0.4433(5) 0.046(2) Uani 1 1 d . . . . .
C7 C 0.2088(7) 0.1413(4) 0.3684(6) 0.053(2) Uani 1 1 d . . . . .
C8 C 0.1394(7) 0.1130(4) 0.3631(6) 0.057(3) Uani 1 1 d . . . . .
C9 C 0.4387(6) 0.2497(3) 0.2482(5) 0.042(2) Uani 1 1 d . . . . .
H9 H 0.3795 0.2541 0.2108 0.050 Uiso 1 1 calc R . . . .
C10 C 0.2933(7) 0.1482(3) 0.2003(5) 0.049(2) Uani 1 1 d . . . . .
H10A H 0.2353 0.1317 0.1712 0.058 Uiso 1 1 calc R . . . .
H10B H 0.3265 0.1192 0.2322 0.058 Uiso 1 1 calc R . . . .
C11 C 0.4995(6) 0.2062(3) 0.2198(4) 0.038(2) Uani 1 1 d . . . . .
C12 C 0.5971(6) 0.2032(3) 0.2372(4) 0.0361(19) Uani 1 1 d . . . . .
H12 H 0.6294 0.2309 0.2676 0.043 Uiso 1 1 calc R . . . .
C13 C 0.6519(6) 0.1616(3) 0.2126(4) 0.0357(19) Uani 1 1 d . . . . .
C14 C 0.6032(6) 0.1207(3) 0.1684(4) 0.0363(19) Uani 1 1 d . . . . .
C15 C 0.5034(6) 0.1213(3) 0.1503(4) 0.040(2) Uani 1 1 d . . . . .
C16 C 0.4533(6) 0.1642(3) 0.1756(5) 0.040(2) Uani 1 1 d . . . . .
C17 C 0.4555(7) 0.0775(3) 0.1064(5) 0.048(2) Uani 1 1 d . . . . .
C18 C 0.4198(8) 0.0399(4) 0.0737(6) 0.065(3) Uani 1 1 d . . . . .
C19 C 0.7600(6) 0.1573(3) 0.2343(4) 0.0335(18) Uani 1 1 d . . . . .
H19 H 0.7839 0.1369 0.1936 0.040 Uiso 1 1 calc R . . . .
C20 C 0.6808(6) 0.0345(3) 0.1869(5) 0.043(2) Uani 1 1 d . . . . .
H20A H 0.6772 0.0006 0.1572 0.052 Uiso 1 1 calc R . . . .
H20B H 0.6357 0.0308 0.2229 0.052 Uiso 1 1 calc R . . . .
C21 C 0.7804(5) 0.1216(3) 0.3021(4) 0.0314(17) Uani 1 1 d . . . . .
C22 C 0.7904(6) 0.1427(3) 0.3724(5) 0.040(2) Uani 1 1 d . . . . .
H22 H 0.7850 0.1811 0.3783 0.049 Uiso 1 1 calc R . . . .
C23 C 0.8083(6) 0.1096(3) 0.4360(5) 0.039(2) Uani 1 1 d . . . . .
C24 C 0.8139(6) 0.0538(3) 0.4265(5) 0.0371(19) Uani 1 1 d . . . . .
C25 C 0.8012(6) 0.0301(3) 0.3567(5) 0.039(2) Uani 1 1 d . . . . .
C26 C 0.7839(6) 0.0650(3) 0.2944(4) 0.0345(18) Uani 1 1 d . . . . .
C27 C 0.8031(6) -0.0279(3) 0.3477(5) 0.0380(19) Uani 1 1 d . . . . .
C28 C 0.8041(7) -0.0755(4) 0.3425(5) 0.051(2) Uani 1 1 d . . . . .
C29 C 0.8174(7) 0.1328(4) 0.5140(5) 0.045(2) Uani 1 1 d . . . . .
H29 H 0.8591 0.1072 0.5474 0.054 Uiso 1 1 calc R . . . .
C30 C 0.7574(7) 0.0039(4) 0.5218(5) 0.051(2) Uani 1 1 d . . . . .
H30A H 0.6978 0.0041 0.4852 0.061 Uiso 1 1 calc R . . . .
H30B H 0.7676 -0.0339 0.5408 0.061 Uiso 1 1 calc R . . . .
C31 C 0.7183(6) 0.1306(4) 0.5356(4) 0.042(2) Uani 1 1 d . . . . .
C32 C 0.6545(7) 0.1744(4) 0.5253(4) 0.043(2) Uani 1 1 d . . . . .
H32 H 0.6759 0.2074 0.5060 0.052 Uiso 1 1 calc R . . . .
C33 C 0.5610(7) 0.1728(4) 0.5416(5) 0.046(2) Uani 1 1 d . . . . .
C34 C 0.5313(7) 0.1238(4) 0.5682(5) 0.048(2) Uani 1 1 d . . . . .
C35 C 0.5906(7) 0.0780(4) 0.5790(5) 0.047(2) Uani 1 1 d . . . . .
C36 C 0.6853(7) 0.0827(4) 0.5648(5) 0.047(2) Uani 1 1 d . . . . .
C37 C 0.5544(7) 0.0267(4) 0.6027(5) 0.053(2) Uani 1 1 d . . . . .
C38 C 0.5237(7) -0.0153(4) 0.6179(5) 0.051(2) Uani 1 1 d . . . . .
C39 C 0.4936(7) 0.2203(4) 0.5283(5) 0.051(2) Uani 1 1 d . . . . .
H39 H 0.4484 0.2166 0.5650 0.062 Uiso 1 1 calc R . . . .
C40 C 0.3613(7) 0.1120(4) 0.5326(6) 0.055(3) Uani 1 1 d . . . . .
H40A H 0.3832 0.0919 0.4915 0.066 Uiso 1 1 calc R . . . .
H40B H 0.3129 0.0890 0.5518 0.066 Uiso 1 1 calc R . . . .
C41 C 0.4889(7) 0.3061(3) 0.2572(5) 0.046(2) Uani 1 1 d . . . . .
H41A H 0.5486 0.3027 0.2932 0.056 Uiso 1 1 calc R . . . .
H41B H 0.5070 0.3171 0.2093 0.056 Uiso 1 1 calc R . . . .
C42 C 0.4257(7) 0.3507(4) 0.2832(7) 0.065(3) Uani 1 1 d . . . . .
H42A H 0.4147 0.3412 0.3336 0.078 Uiso 1 1 calc R . . . .
H42B H 0.4626 0.3853 0.2869 0.078 Uiso 1 1 calc R . . . .
C43 C 0.3367(11) 0.3607(5) 0.2407(7) 0.090(4) Uani 1 1 d . . . . .
H43A H 0.2971 0.3274 0.2417 0.108 Uiso 1 1 calc R . . . .
H43B H 0.3469 0.3662 0.1890 0.108 Uiso 1 1 calc R . . . .
C44 C 0.2759(11) 0.4116(5) 0.2634(9) 0.105(5) Uani 1 1 d . . . . .
H44A H 0.2152 0.4150 0.2284 0.126 Uiso 1 1 calc R . . . .
H44B H 0.2599 0.4059 0.3135 0.126 Uiso 1 1 calc R . . . .
C45 C 0.3334(11) 0.4618(4) 0.2618(8) 0.099(5) Uani 1 1 d . . . . .
H45A H 0.3518 0.4667 0.2123 0.119 Uiso 1 1 calc R . . . .
H45B H 0.3927 0.4592 0.2984 0.119 Uiso 1 1 calc R . . . .
C46 C 0.2699(11) 0.5123(6) 0.2809(11) 0.135(6) Uani 1 1 d . U . . .
H46A H 0.2102 0.5137 0.2455 0.202 Uiso 1 1 calc GR . . . .
H46B H 0.3058 0.5463 0.2781 0.202 Uiso 1 1 calc GR . . . .
H46C H 0.2547 0.5079 0.3309 0.202 Uiso 1 1 calc GR . . . .
C47 C 0.8142(6) 0.2125(3) 0.2416(5) 0.043(2) Uani 1 1 d . . . . .
H47A H 0.7991 0.2327 0.1944 0.051 Uiso 1 1 calc R . . . .
H47B H 0.7908 0.2346 0.2803 0.051 Uiso 1 1 calc R . . . .
C48 C 0.9216(6) 0.2063(4) 0.2605(5) 0.051(2) Uani 1 1 d . . . . .
H48A H 0.9417 0.1752 0.2320 0.061 Uiso 1 1 calc R . . . .
H48B H 0.9375 0.1968 0.3135 0.061 Uiso 1 1 calc R . . . .
C49 C 0.9806(9) 0.2563(4) 0.2459(6) 0.069(3) Uani 1 1 d D . . . .
H49A H 1.0493 0.2473 0.2609 0.083 Uiso 1 1 calc R . . . .
H49B H 0.9704 0.2629 0.1920 0.083 Uiso 1 1 calc R . . . .
C50 C 0.9600(10) 0.3086(4) 0.2836(8) 0.096(4) Uani 1 1 d D . . . .
H50A H 0.9623 0.3017 0.3370 0.115 Uiso 1 1 calc R . . . .
H50B H 0.8945 0.3214 0.2634 0.115 Uiso 1 1 calc R . . . .
C51 C 1.0328(11) 0.3535(5) 0.2727(8) 0.103(4) Uani 1 1 d D U . . .
H51A H 1.0960 0.3446 0.3020 0.124 Uiso 1 1 calc R . . . .
H51B H 1.0406 0.3552 0.2201 0.124 Uiso 1 1 calc R . . . .
C52 C 0.9982(12) 0.4086(6) 0.2970(11) 0.148(7) Uani 1 1 d D . . . .
H52A H 0.9308 0.4139 0.2754 0.222 Uiso 1 1 calc GR . . . .
H52B H 1.0373 0.4378 0.2804 0.222 Uiso 1 1 calc GR . . . .
H52C H 1.0043 0.4095 0.3509 0.222 Uiso 1 1 calc GR . . . .
C53 C 0.8651(7) 0.1893(4) 0.5225(5) 0.049(2) Uani 1 1 d . . . . .
H53A H 0.8263 0.2152 0.4887 0.059 Uiso 1 1 calc R . . . .
H53B H 0.8649 0.2024 0.5735 0.059 Uiso 1 1 calc R . . . .
C54 C 0.9664(7) 0.1900(4) 0.5067(6) 0.061(3) Uani 1 1 d . . . . .
H54A H 0.9665 0.1764 0.4559 0.073 Uiso 1 1 calc R . . . .
H54B H 1.0052 0.1643 0.5409 0.073 Uiso 1 1 calc R . . . .
C55 C 1.0148(9) 0.2459(5) 0.5140(6) 0.076(3) Uani 1 1 d . . . . .
H55A H 0.9698 0.2728 0.4873 0.091 Uiso 1 1 calc R . . . .
H55B H 1.0247 0.2562 0.5668 0.091 Uiso 1 1 calc R . . . .
C56 C 1.1067(9) 0.2511(5) 0.4873(7) 0.093(4) Uani 1 1 d D . . . .
H56A H 1.1008 0.2364 0.4365 0.111 Uiso 0.61(2) 1 calc R . P A 1
H56B H 1.1562 0.2295 0.5191 0.111 Uiso 0.61(2) 1 calc R . P A 1
H56C H 1.0905 0.2649 0.4362 0.111 Uiso 0.39(2) 1 calc R . P A 2
H56D H 1.1297 0.2132 0.4830 0.111 Uiso 0.39(2) 1 calc R . P A 2
C57 C 1.1374(15) 0.3107(7) 0.4877(14) 0.070(7) Uani 0.61(2) 1 d D U P A 1
H57A H 1.0848 0.3323 0.4595 0.084 Uiso 0.61(2) 1 calc R . P A 1
H57B H 1.1471 0.3241 0.5392 0.084 Uiso 0.61(2) 1 calc R . P A 1
C57B C 1.1941(15) 0.2831(9) 0.5208(17) 0.087(13) Uani 0.39(2) 1 d D . P A 2
H57C H 1.2050 0.2826 0.5754 0.105 Uiso 0.39(2) 1 calc R . P A 2
H57D H 1.2532 0.2721 0.5016 0.105 Uiso 0.39(2) 1 calc R . P A 2
C58 C 1.2282(13) 0.3206(7) 0.4555(13) 0.090(8) Uani 0.61(2) 1 d D U P A 1
H58A H 1.2167 0.3122 0.4026 0.135 Uiso 0.61(2) 1 calc GR . P A 1
H58B H 1.2796 0.2971 0.4803 0.135 Uiso 0.61(2) 1 calc GR . P A 1
H58C H 1.2473 0.3590 0.4626 0.135 Uiso 0.61(2) 1 calc GR . P A 1
C58B C 1.152(3) 0.3363(13) 0.4889(19) 0.070(10) Uani 0.39(2) 1 d D U P A 2
H58D H 1.1536 0.3368 0.4356 0.106 Uiso 0.39(2) 1 calc GR . P A 2
H58E H 1.1906 0.3668 0.5123 0.106 Uiso 0.39(2) 1 calc GR . P A 2
H58F H 1.0861 0.3397 0.4979 0.106 Uiso 0.39(2) 1 calc GR . P A 2
C59 C 0.5419(8) 0.2765(4) 0.5428(6) 0.062(3) Uani 1 1 d . . . . .
H59A H 0.5853 0.2756 0.5908 0.075 Uiso 1 1 calc R . . . .
H59B H 0.5814 0.2842 0.5039 0.075 Uiso 1 1 calc R . . . .
C60 C 0.4711(8) 0.3210(4) 0.5440(7) 0.071(3) Uani 1 1 d . . . . .
H60A H 0.4224 0.3093 0.5742 0.086 Uiso 1 1 calc R . . . .
H60B H 0.4378 0.3273 0.4931 0.086 Uiso 1 1 calc R . . . .
C61 C 0.5147(10) 0.3740(5) 0.5744(9) 0.100(5) Uani 1 1 d . . . . .
H61A H 0.5656 0.3850 0.5458 0.119 Uiso 1 1 calc R . . . .
H61B H 0.5451 0.3684 0.6262 0.119 Uiso 1 1 calc R . . . .
C62 C 0.4378(11) 0.4220(5) 0.5714(9) 0.107(5) Uani 1 1 d . . . . .
H62A H 0.4062 0.4272 0.5198 0.128 Uiso 1 1 calc R . . . .
H62B H 0.3879 0.4116 0.6012 0.128 Uiso 1 1 calc R . . . .
C63 C 0.4829(13) 0.4730(6) 0.5994(10) 0.129(6) Uani 1 1 d . . . . .
H63A H 0.5337 0.4832 0.5703 0.155 Uiso 1 1 calc R . . . .
H63B H 0.5131 0.4682 0.6514 0.155 Uiso 1 1 calc R . . . .
C64 C 0.4094(12) 0.5177(7) 0.5944(11) 0.131(6) Uani 1 1 d . . . . .
H64A H 0.3642 0.5139 0.5484 0.196 Uiso 1 1 calc GR . . . .
H64B H 0.4415 0.5533 0.5950 0.196 Uiso 1 1 calc GR . . . .
H64C H 0.3746 0.5153 0.6365 0.196 Uiso 1 1 calc GR . . . .
O O 0.2647(4) 0.1893(2) 0.2453(4) 0.0501(16) Uani 1 1 d . . . . .
O1 O 0.3176(5) 0.1607(3) 0.5052(4) 0.0587(18) Uani 1 1 d . . . . .
O2 O 0.6527(4) 0.0793(2) 0.1401(3) 0.0441(15) Uani 1 1 d . . . . .
O3 O 0.3546(4) 0.1662(2) 0.1512(3) 0.0479(15) Uani 1 1 d . . . . .
O4 O 0.8352(4) 0.0189(2) 0.4863(3) 0.0445(14) Uani 1 1 d . . . . .
O5 O 0.7758(4) 0.0408(2) 0.2257(3) 0.0403(14) Uani 1 1 d . . . . .
O6 O 0.4410(5) 0.1197(3) 0.5897(3) 0.0562(17) Uani 1 1 d . . . . .
O7 O 0.7455(4) 0.0386(3) 0.5802(3) 0.0509(16) Uani 1 1 d . . . . .
C65 C 0.7714(13) 0.3458(7) 0.4865(9) 0.131(6) Uani 1 1 d . U . . .
H65A H 0.7637 0.3148 0.5189 0.196 Uiso 1 1 calc GR . . . .
H65B H 0.7329 0.3767 0.4992 0.196 Uiso 1 1 calc GR . . . .
H65C H 0.8392 0.3564 0.4927 0.196 Uiso 1 1 calc GR . . . .
C66 C 0.7398(8) 0.3301(4) 0.4108(5) 0.060(3) Uani 1 1 d . . . . .
C67 C 0.7484(16) 0.3724(8) 0.3577(12) 0.167(8) Uani 1 1 d . U . . .
H67A H 0.7372 0.3568 0.3079 0.251 Uiso 1 1 calc GR . . . .
H67B H 0.8131 0.3881 0.3675 0.251 Uiso 1 1 calc GR . . . .
H67C H 0.7009 0.4011 0.3617 0.251 Uiso 1 1 calc GR . . . .
O8 O 0.7107(6) 0.2867(3) 0.3926(4) 0.072(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C8 1.801(10) . ?
Br2 C18 1.805(9) . ?
Br3 C28 1.818(9) . ?
Br4 C38 1.808(10) . ?
C1 C2 1.377(12) . ?
C1 C6 1.375(12) . ?
C1 C39 1.549(13) . ?
C2 H2 0.9500 . ?
C2 C3 1.383(12) . ?
C3 C4 1.391(12) . ?
C3 C9 1.527(12) . ?
C4 C5 1.401(12) . ?
C4 O 1.395(10) . ?
C5 C6 1.399(13) . ?
C5 C7 1.420(13) . ?
C6 O1 1.400(11) . ?
C7 C8 1.191(12) . ?
C9 H9 1.0000 . ?
C9 C11 1.510(12) . ?
C9 C41 1.546(11) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 O 1.399(11) . ?
C10 O3 1.413(11) . ?
C11 C12 1.365(11) . ?
C11 C16 1.405(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.394(11) . ?
C13 C14 1.398(11) . ?
C13 C19 1.517(11) . ?
C14 C15 1.395(12) . ?
C14 O2 1.377(10) . ?
C15 C16 1.387(12) . ?
C15 C17 1.443(11) . ?
C16 O3 1.394(10) . ?
C17 C18 1.170(12) . ?
C19 H19 1.0000 . ?
C19 C21 1.512(10) . ?
C19 C47 1.546(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 O2 1.412(9) . ?
C20 O5 1.423(10) . ?
C21 C22 1.377(11) . ?
C21 C26 1.391(11) . ?
C22 H22 0.9500 . ?
C22 C23 1.412(11) . ?
C23 C24 1.379(11) . ?
C23 C29 1.526(12) . ?
C24 C25 1.392(12) . ?
C24 O4 1.387(9) . ?
C25 C26 1.417(11) . ?
C25 C27 1.428(11) . ?
C26 O5 1.383(9) . ?
C27 C28 1.170(11) . ?
C29 H29 1.0000 . ?
C29 C31 1.511(12) . ?
C29 C53 1.535(12) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 O4 1.409(10) . ?
C30 O7 1.400(11) . ?
C31 C32 1.393(12) . ?
C31 C36 1.400(12) . ?
C32 H32 0.9500 . ?
C32 C33 1.397(12) . ?
C33 C34 1.383(13) . ?
C33 C39 1.498(13) . ?
C34 C35 1.395(13) . ?
C34 O6 1.394(11) . ?
C35 C36 1.405(13) . ?
C35 C37 1.447(13) . ?
C36 O7 1.374(11) . ?
C37 C38 1.166(12) . ?
C39 H39 1.0000 . ?
C39 C59 1.539(12) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 O1 1.400(11) . ?
C40 O6 1.425(11) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.532(12) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.393(15) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.603(18) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.474(18) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.598(17) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.509(12) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.526(12) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.506(11) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.536(11) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.525(12) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.502(13) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C55 1.524(13) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.462(16) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 H56C 0.9900 . ?
C56 H56D 0.9900 . ?
C56 C57 1.520(14) . ?
C56 C57B 1.508(15) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.512(15) . ?
C57B H57C 0.9900 . ?
C57B H57D 0.9900 . ?
C57B C58B 1.508(15) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C58B H58D 0.9800 . ?
C58B H58E 0.9800 . ?
C58B H58F 0.9800 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.480(14) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.504(15) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.593(18) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.459(18) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.50(2) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C65 C66 1.442(17) . ?
C66 C67 1.44(2) . ?
C66 O8 1.169(11) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C39 122.3(8) . . ?
C6 C1 C2 117.8(8) . . ?
C6 C1 C39 119.7(8) . . ?
C1 C2 H2 118.6 . . ?
C1 C2 C3 122.8(8) . . ?
C3 C2 H2 118.6 . . ?
C2 C3 C4 118.0(9) . . ?
C2 C3 C9 123.8(8) . . ?
C4 C3 C9 118.1(8) . . ?
C3 C4 C5 121.6(9) . . ?
C3 C4 O 122.1(8) . . ?
O C4 C5 116.2(8) . . ?
C4 C5 C7 121.7(9) . . ?
C6 C5 C4 117.1(8) . . ?
C6 C5 C7 121.1(9) . . ?
C1 C6 C5 122.7(9) . . ?
C1 C6 O1 120.2(8) . . ?
C5 C6 O1 117.0(8) . . ?
C8 C7 C5 179.0(10) . . ?
C7 C8 Br1 179.1(10) . . ?
C3 C9 H9 107.3 . . ?
C3 C9 C41 113.6(7) . . ?
C11 C9 C3 108.2(6) . . ?
C11 C9 H9 107.3 . . ?
C11 C9 C41 113.0(7) . . ?
C41 C9 H9 107.3 . . ?
H10A C10 H10B 107.6 . . ?
O C10 H10A 108.6 . . ?
O C10 H10B 108.6 . . ?
O C10 O3 114.5(7) . . ?
O3 C10 H10A 108.6 . . ?
O3 C10 H10B 108.6 . . ?
C12 C11 C9 124.3(7) . . ?
C12 C11 C16 117.1(8) . . ?
C16 C11 C9 118.5(8) . . ?
C11 C12 H12 118.2 . . ?
C11 C12 C13 123.6(7) . . ?
C13 C12 H12 118.2 . . ?
C12 C13 C14 117.5(8) . . ?
C12 C13 C19 123.4(7) . . ?
C14 C13 C19 119.0(7) . . ?
C15 C14 C13 121.2(8) . . ?
O2 C14 C13 120.9(7) . . ?
O2 C14 C15 117.9(7) . . ?
C14 C15 C17 119.6(8) . . ?
C16 C15 C14 118.4(7) . . ?
C16 C15 C17 122.0(8) . . ?
C15 C16 C11 122.2(8) . . ?
C15 C16 O3 117.0(7) . . ?
O3 C16 C11 120.7(7) . . ?
C18 C17 C15 176.0(10) . . ?
C17 C18 Br2 176.3(10) . . ?
C13 C19 H19 106.3 . . ?
C13 C19 C47 115.2(7) . . ?
C21 C19 C13 108.0(6) . . ?
C21 C19 H19 106.3 . . ?
C21 C19 C47 113.9(6) . . ?
C47 C19 H19 106.3 . . ?
H20A C20 H20B 107.9 . . ?
O2 C20 H20A 109.2 . . ?
O2 C20 H20B 109.2 . . ?
O2 C20 O5 111.9(7) . . ?
O5 C20 H20A 109.2 . . ?
O5 C20 H20B 109.2 . . ?
C22 C21 C19 122.1(7) . . ?
C22 C21 C26 117.9(7) . . ?
C26 C21 C19 119.9(7) . . ?
C21 C22 H22 118.7 . . ?
C21 C22 C23 122.6(7) . . ?
C23 C22 H22 118.7 . . ?
C22 C23 C29 122.6(7) . . ?
C24 C23 C22 118.0(8) . . ?
C24 C23 C29 119.3(7) . . ?
C23 C24 C25 121.9(7) . . ?
C23 C24 O4 121.2(7) . . ?
O4 C24 C25 116.9(7) . . ?
C24 C25 C26 118.1(7) . . ?
C24 C25 C27 121.3(7) . . ?
C26 C25 C27 120.6(8) . . ?
C21 C26 C25 121.6(7) . . ?
O5 C26 C21 121.2(7) . . ?
O5 C26 C25 117.1(7) . . ?
C28 C27 C25 177.8(10) . . ?
C27 C28 Br3 176.8(9) . . ?
C23 C29 H29 107.2 . . ?
C23 C29 C53 113.8(7) . . ?
C31 C29 C23 106.6(7) . . ?
C31 C29 H29 107.2 . . ?
C31 C29 C53 114.4(8) . . ?
C53 C29 H29 107.2 . . ?
H30A C30 H30B 107.8 . . ?
O4 C30 H30A 109.0 . . ?
O4 C30 H30B 109.0 . . ?
O7 C30 H30A 109.0 . . ?
O7 C30 H30B 109.0 . . ?
O7 C30 O4 112.9(7) . . ?
C32 C31 C29 122.8(8) . . ?
C32 C31 C36 116.7(8) . . ?
C36 C31 C29 120.4(8) . . ?
C31 C32 H32 117.9 . . ?
C31 C32 C33 124.2(8) . . ?
C33 C32 H32 117.9 . . ?
C32 C33 C39 122.7(8) . . ?
C34 C33 C32 116.6(9) . . ?
C34 C33 C39 120.7(9) . . ?
C33 C34 C35 122.7(9) . . ?
C33 C34 O6 120.2(9) . . ?
O6 C34 C35 117.0(8) . . ?
C34 C35 C36 118.2(8) . . ?
C34 C35 C37 120.6(9) . . ?
C36 C35 C37 121.1(9) . . ?
C31 C36 C35 121.5(9) . . ?
O7 C36 C31 120.3(8) . . ?
O7 C36 C35 118.2(8) . . ?
C38 C37 C35 176.4(11) . . ?
C37 C38 Br4 179.4(10) . . ?
C1 C39 H39 106.0 . . ?
C33 C39 C1 109.4(7) . . ?
C33 C39 H39 106.0 . . ?
C33 C39 C59 114.3(8) . . ?
C59 C39 C1 114.2(8) . . ?
C59 C39 H39 106.0 . . ?
H40A C40 H40B 107.7 . . ?
O1 C40 H40A 108.8 . . ?
O1 C40 H40B 108.8 . . ?
O1 C40 O6 113.8(8) . . ?
O6 C40 H40A 108.8 . . ?
O6 C40 H40B 108.8 . . ?
C9 C41 H41A 109.0 . . ?
C9 C41 H41B 109.0 . . ?
H41A C41 H41B 107.8 . . ?
C42 C41 C9 113.0(8) . . ?
C42 C41 H41A 109.0 . . ?
C42 C41 H41B 109.0 . . ?
C41 C42 H42A 107.8 . . ?
C41 C42 H42B 107.8 . . ?
H42A C42 H42B 107.2 . . ?
C43 C42 C41 117.9(10) . . ?
C43 C42 H42A 107.8 . . ?
C43 C42 H42B 107.8 . . ?
C42 C43 H43A 107.9 . . ?
C42 C43 H43B 107.9 . . ?
C42 C43 C44 117.6(10) . . ?
H43A C43 H43B 107.2 . . ?
C44 C43 H43A 107.9 . . ?
C44 C43 H43B 107.9 . . ?
C43 C44 H44A 109.9 . . ?
C43 C44 H44B 109.9 . . ?
H44A C44 H44B 108.3 . . ?
C45 C44 C43 108.9(12) . . ?
C45 C44 H44A 109.9 . . ?
C45 C44 H44B 109.9 . . ?
C44 C45 H45A 110.1 . . ?
C44 C45 H45B 110.1 . . ?
C44 C45 C46 108.1(13) . . ?
H45A C45 H45B 108.4 . . ?
C46 C45 H45A 110.1 . . ?
C46 C45 H45B 110.1 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C19 C47 H47A 108.9 . . ?
C19 C47 H47B 108.9 . . ?
H47A C47 H47B 107.7 . . ?
C48 C47 C19 113.4(7) . . ?
C48 C47 H47A 108.9 . . ?
C48 C47 H47B 108.9 . . ?
C47 C48 H48A 108.4 . . ?
C47 C48 H48B 108.4 . . ?
C47 C48 C49 115.7(8) . . ?
H48A C48 H48B 107.4 . . ?
C49 C48 H48A 108.4 . . ?
C49 C48 H48B 108.4 . . ?
C48 C49 H49A 108.1 . . ?
C48 C49 H49B 108.1 . . ?
H49A C49 H49B 107.3 . . ?
C50 C49 C48 116.9(10) . . ?
C50 C49 H49A 108.1 . . ?
C50 C49 H49B 108.1 . . ?
C49 C50 H50A 109.3 . . ?
C49 C50 H50B 109.3 . . ?
C49 C50 C51 111.5(12) . . ?
H50A C50 H50B 108.0 . . ?
C51 C50 H50A 109.3 . . ?
C51 C50 H50B 109.3 . . ?
C50 C51 H51A 109.7 . . ?
C50 C51 H51B 109.7 . . ?
H51A C51 H51B 108.2 . . ?
C52 C51 C50 110.0(13) . . ?
C52 C51 H51A 109.7 . . ?
C52 C51 H51B 109.7 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C29 C53 H53A 108.8 . . ?
C29 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
C54 C53 C29 113.9(8) . . ?
C54 C53 H53A 108.8 . . ?
C54 C53 H53B 108.8 . . ?
C53 C54 H54A 108.6 . . ?
C53 C54 H54B 108.6 . . ?
C53 C54 C55 114.8(9) . . ?
H54A C54 H54B 107.5 . . ?
C55 C54 H54A 108.6 . . ?
C55 C54 H54B 108.6 . . ?
C54 C55 H55A 108.0 . . ?
C54 C55 H55B 108.0 . . ?
H55A C55 H55B 107.2 . . ?
C56 C55 C54 117.2(10) . . ?
C56 C55 H55A 108.0 . . ?
C56 C55 H55B 108.0 . . ?
C55 C56 H56A 109.6 . . ?
C55 C56 H56B 109.6 . . ?
C55 C56 H56C 105.2 . . ?
C55 C56 H56D 105.2 . . ?
C55 C56 C57 110.4(13) . . ?
C55 C56 C57B 128.3(17) . . ?
H56A C56 H56B 108.1 . . ?
H56C C56 H56D 105.9 . . ?
C57 C56 H56A 109.6 . . ?
C57 C56 H56B 109.6 . . ?
C57B C56 H56C 105.2 . . ?
C57B C56 H56D 105.2 . . ?
C56 C57 H57A 108.7 . . ?
C56 C57 H57B 108.7 . . ?
H57A C57 H57B 107.6 . . ?
C58 C57 C56 114.2(16) . . ?
C58 C57 H57A 108.7 . . ?
C58 C57 H57B 108.7 . . ?
C56 C57B H57C 113.2 . . ?
C56 C57B H57D 113.2 . . ?
H57C C57B H57D 110.5 . . ?
C58B C57B C56 92.6(18) . . ?
C58B C57B H57C 113.2 . . ?
C58B C57B H57D 113.2 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57B C58B H58D 109.5 . . ?
C57B C58B H58E 109.5 . . ?
C57B C58B H58F 109.5 . . ?
H58D C58B H58E 109.5 . . ?
H58D C58B H58F 109.5 . . ?
H58E C58B H58F 109.5 . . ?
C39 C59 H59A 109.2 . . ?
C39 C59 H59B 109.2 . . ?
H59A C59 H59B 107.9 . . ?
C60 C59 C39 112.2(9) . . ?
C60 C59 H59A 109.2 . . ?
C60 C59 H59B 109.2 . . ?
C59 C60 H60A 108.8 . . ?
C59 C60 H60B 108.8 . . ?
C59 C60 C61 113.7(10) . . ?
H60A C60 H60B 107.7 . . ?
C61 C60 H60A 108.8 . . ?
C61 C60 H60B 108.8 . . ?
C60 C61 H61A 109.1 . . ?
C60 C61 H61B 109.1 . . ?
C60 C61 C62 112.7(11) . . ?
H61A C61 H61B 107.8 . . ?
C62 C61 H61A 109.1 . . ?
C62 C61 H61B 109.1 . . ?
C61 C62 H62A 109.4 . . ?
C61 C62 H62B 109.4 . . ?
H62A C62 H62B 108.0 . . ?
C63 C62 C61 111.2(13) . . ?
C63 C62 H62A 109.4 . . ?
C63 C62 H62B 109.4 . . ?
C62 C63 H63A 109.6 . . ?
C62 C63 H63B 109.6 . . ?
C62 C63 C64 110.1(15) . . ?
H63A C63 H63B 108.1 . . ?
C64 C63 H63A 109.6 . . ?
C64 C63 H63B 109.6 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C4 O C10 116.3(7) . . ?
C40 O1 C6 117.2(7) . . ?
C14 O2 C20 116.9(6) . . ?
C16 O3 C10 117.7(6) . . ?
C24 O4 C30 116.0(6) . . ?
C26 O5 C20 116.1(6) . . ?
C34 O6 C40 116.9(7) . . ?
C36 O7 C30 117.6(7) . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C66 C65 H65A 109.5 . . ?
C66 C65 H65B 109.5 . . ?
C66 C65 H65C 109.5 . . ?
C67 C66 C65 114.5(13) . . ?
O8 C66 C65 123.9(11) . . ?
O8 C66 C67 121.5(12) . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.5(12) . . . . ?
C1 C2 C3 C9 -177.3(8) . . . . ?
C1 C6 O1 C40 -81.1(10) . . . . ?
C1 C39 C59 C60 64.6(11) . . . . ?
C2 C1 C6 C5 -1.4(13) . . . . ?
C2 C1 C6 O1 179.4(8) . . . . ?
C2 C1 C39 C33 -89.5(10) . . . . ?
C2 C1 C39 C59 40.2(12) . . . . ?
C2 C3 C4 C5 0.4(12) . . . . ?
C2 C3 C4 O 178.4(7) . . . . ?
C2 C3 C9 C11 88.7(9) . . . . ?
C2 C3 C9 C41 -37.6(11) . . . . ?
C3 C4 C5 C6 0.2(12) . . . . ?
C3 C4 C5 C7 -178.2(8) . . . . ?
C3 C4 O C10 81.4(9) . . . . ?
C3 C9 C11 C12 -91.8(9) . . . . ?
C3 C9 C11 C16 84.8(9) . . . . ?
C3 C9 C41 C42 -58.4(11) . . . . ?
C4 C3 C9 C11 -87.1(9) . . . . ?
C4 C3 C9 C41 146.6(8) . . . . ?
C4 C5 C6 C1 0.4(13) . . . . ?
C4 C5 C6 O1 179.6(7) . . . . ?
C5 C4 O C10 -100.5(9) . . . . ?
C5 C6 O1 C40 99.6(10) . . . . ?
C6 C1 C2 C3 2.0(13) . . . . ?
C6 C1 C39 C33 85.2(10) . . . . ?
C6 C1 C39 C59 -145.2(9) . . . . ?
C7 C5 C6 C1 178.7(8) . . . . ?
C7 C5 C6 O1 -2.0(12) . . . . ?
C9 C3 C4 C5 176.5(7) . . . . ?
C9 C3 C4 O -5.5(12) . . . . ?
C9 C11 C12 C13 177.6(7) . . . . ?
C9 C11 C16 C15 -176.8(7) . . . . ?
C9 C11 C16 O3 7.5(11) . . . . ?
C9 C41 C42 C43 -57.0(13) . . . . ?
C11 C9 C41 C42 177.8(8) . . . . ?
C11 C12 C13 C14 -0.6(12) . . . . ?
C11 C12 C13 C19 -177.8(7) . . . . ?
C11 C16 O3 C10 -82.3(9) . . . . ?
C12 C11 C16 C15 0.1(12) . . . . ?
C12 C11 C16 O3 -175.6(7) . . . . ?
C12 C13 C14 C15 -0.7(11) . . . . ?
C12 C13 C14 O2 177.8(7) . . . . ?
C12 C13 C19 C21 92.2(8) . . . . ?
C12 C13 C19 C47 -36.5(11) . . . . ?
C13 C14 C15 C16 1.6(12) . . . . ?
C13 C14 C15 C17 -178.1(8) . . . . ?
C13 C14 O2 C20 82.8(9) . . . . ?
C13 C19 C21 C22 -90.4(9) . . . . ?
C13 C19 C21 C26 85.6(9) . . . . ?
C13 C19 C47 C48 -178.0(7) . . . . ?
C14 C13 C19 C21 -84.9(8) . . . . ?
C14 C13 C19 C47 146.4(7) . . . . ?
C14 C15 C16 C11 -1.3(12) . . . . ?
C14 C15 C16 O3 174.6(7) . . . . ?
C15 C14 O2 C20 -98.7(8) . . . . ?
C15 C16 O3 C10 101.8(9) . . . . ?
C16 C11 C12 C13 0.9(12) . . . . ?
C17 C15 C16 C11 178.4(8) . . . . ?
C17 C15 C16 O3 -5.8(12) . . . . ?
C19 C13 C14 C15 176.6(7) . . . . ?
C19 C13 C14 O2 -4.9(11) . . . . ?
C19 C21 C22 C23 179.2(7) . . . . ?
C19 C21 C26 C25 -178.9(7) . . . . ?
C19 C21 C26 O5 4.7(11) . . . . ?
C19 C47 C48 C49 162.2(8) . . . . ?
C21 C19 C47 C48 56.3(10) . . . . ?
C21 C22 C23 C24 -1.4(12) . . . . ?
C21 C22 C23 C29 -178.8(8) . . . . ?
C21 C26 O5 C20 -81.3(9) . . . . ?
C22 C21 C26 C25 -2.6(12) . . . . ?
C22 C21 C26 O5 -179.1(7) . . . . ?
C22 C23 C24 C25 -0.8(12) . . . . ?
C22 C23 C24 O4 177.3(7) . . . . ?
C22 C23 C29 C31 92.1(9) . . . . ?
C22 C23 C29 C53 -35.0(12) . . . . ?
C23 C24 C25 C26 1.2(12) . . . . ?
C23 C24 C25 C27 -177.3(8) . . . . ?
C23 C24 O4 C30 83.2(9) . . . . ?
C23 C29 C31 C32 -93.3(9) . . . . ?
C23 C29 C31 C36 84.3(9) . . . . ?
C23 C29 C53 C54 -61.7(10) . . . . ?
C24 C23 C29 C31 -85.3(9) . . . . ?
C24 C23 C29 C53 147.6(8) . . . . ?
C24 C25 C26 C21 0.6(12) . . . . ?
C24 C25 C26 O5 177.2(7) . . . . ?
C25 C24 O4 C30 -98.6(9) . . . . ?
C25 C26 O5 C20 102.0(8) . . . . ?
C26 C21 C22 C23 3.0(12) . . . . ?
C27 C25 C26 C21 179.1(8) . . . . ?
C27 C25 C26 O5 -4.3(11) . . . . ?
C29 C23 C24 C25 176.7(7) . . . . ?
C29 C23 C24 O4 -5.2(12) . . . . ?
C29 C31 C32 C33 177.0(8) . . . . ?
C29 C31 C36 C35 -174.1(8) . . . . ?
C29 C31 C36 O7 5.6(12) . . . . ?
C29 C53 C54 C55 179.4(8) . . . . ?
C31 C29 C53 C54 175.4(8) . . . . ?
C31 C32 C33 C34 -1.3(12) . . . . ?
C31 C32 C33 C39 -178.6(8) . . . . ?
C31 C36 O7 C30 -82.1(10) . . . . ?
C32 C31 C36 C35 3.7(12) . . . . ?
C32 C31 C36 O7 -176.6(7) . . . . ?
C32 C33 C34 C35 0.4(13) . . . . ?
C32 C33 C34 O6 176.4(7) . . . . ?
C32 C33 C39 C1 93.3(9) . . . . ?
C32 C33 C39 C59 -36.3(12) . . . . ?
C33 C34 C35 C36 2.4(13) . . . . ?
C33 C34 C35 C37 -176.3(8) . . . . ?
C33 C34 O6 C40 80.7(10) . . . . ?
C33 C39 C59 C60 -168.2(9) . . . . ?
C34 C33 C39 C1 -84.0(10) . . . . ?
C34 C33 C39 C59 146.5(9) . . . . ?
C34 C35 C36 C31 -4.5(13) . . . . ?
C34 C35 C36 O7 175.7(7) . . . . ?
C35 C34 O6 C40 -103.0(9) . . . . ?
C35 C36 O7 C30 97.6(9) . . . . ?
C36 C31 C32 C33 -0.7(12) . . . . ?
C37 C35 C36 C31 174.1(8) . . . . ?
C37 C35 C36 O7 -5.6(13) . . . . ?
C39 C1 C2 C3 176.8(8) . . . . ?
C39 C1 C6 C5 -176.3(8) . . . . ?
C39 C1 C6 O1 4.5(12) . . . . ?
C39 C33 C34 C35 177.8(8) . . . . ?
C39 C33 C34 O6 -6.2(12) . . . . ?
C39 C59 C60 C61 167.1(10) . . . . ?
C41 C9 C11 C12 34.8(11) . . . . ?
C41 C9 C11 C16 -148.5(8) . . . . ?
C41 C42 C43 C44 -173.7(10) . . . . ?
C42 C43 C44 C45 58.1(17) . . . . ?
C43 C44 C45 C46 177.5(12) . . . . ?
C47 C19 C21 C22 39.0(11) . . . . ?
C47 C19 C21 C26 -145.0(8) . . . . ?
C47 C48 C49 C50 57.3(13) . . . . ?
C48 C49 C50 C51 172.4(10) . . . . ?
C49 C50 C51 C52 168.0(12) . . . . ?
C53 C29 C31 C32 33.3(11) . . . . ?
C53 C29 C31 C36 -149.0(8) . . . . ?
C53 C54 C55 C56 -169.8(10) . . . . ?
C54 C55 C56 C57 171.3(14) . . . . ?
C54 C55 C56 C57B -141.2(16) . . . . ?
C55 C56 C57 C58 -175.6(17) . . . . ?
C55 C56 C57B C58B -80(3) . . . . ?
C59 C60 C61 C62 177.2(12) . . . . ?
C60 C61 C62 C63 -178.5(14) . . . . ?
C61 C62 C63 C64 178.7(14) . . . . ?
O C4 C5 C6 -178.0(7) . . . . ?
O C4 C5 C7 3.6(12) . . . . ?
O C10 O3 C16 90.6(9) . . . . ?
O1 C40 O6 C34 -91.7(10) . . . . ?
O2 C14 C15 C16 -176.9(7) . . . . ?
O2 C14 C15 C17 3.4(11) . . . . ?
O2 C20 O5 C26 92.3(8) . . . . ?
O3 C10 O C4 -89.9(9) . . . . ?
O4 C24 C25 C26 -177.0(7) . . . . ?
O4 C24 C25 C27 4.5(11) . . . . ?
O4 C30 O7 C36 91.4(9) . . . . ?
O5 C20 O2 C14 -93.8(8) . . . . ?
O6 C34 C35 C36 -173.7(7) . . . . ?
O6 C34 C35 C37 7.6(12) . . . . ?
O6 C40 O1 C6 93.2(10) . . . . ?
O7 C30 O4 C24 -91.7(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-19 1 -5 0.0460 -19.0000 0.9999 -5.0000 -0.8596 0.5346 -0.1017
12 -24 -12 0.0807 12.0000 -23.9999 -12.0000 0.3156 -0.1918 0.9229
19 -9 0 0.0588 19.0000 -8.9999 0.0000 0.7871 -0.4817 0.3914
14 13 13 0.0440 14.0000 13.0001 13.0000 0.7784 -0.4733 -0.4388
8 7 -25 0.0374 8.0000 6.9998 -25.0000 -0.4641 -0.7709 0.4793
-6 25 17 0.0509 -6.0000 25.0000 17.0000 0.0409 0.0549 -0.9962
-6 -20 20 0.0657 -6.0000 -19.9998 20.0000 0.5091 0.8395 -0.0578
-17 -13 12 0.0566 -17.0000 -12.9999 12.0000 -0.1870 0.9638 -0.1467
16 -6 -18 0.0498 16.0000 -6.0001 -18.0000 0.1428 -0.7132 0.6943
17 9 -14 0.0513 17.0000 8.9999 -14.0000 0.1648 -0.9296 0.2805
12 27 -3 0.0682 12.0000 26.9999 -3.0000 0.1340 -0.8869 -0.4161
12 -17 13 0.0708 11.9999 -16.9998 13.0000 0.9594 0.0847 0.2111
3 13 23 0.0594 3.0000 13.0001 23.0000 0.6485 0.0475 -0.7713
-10 14 -18 0.0590 -9.9999 13.9998 -18.0000 -0.9998 -0.1800 -0.0130
-4 16 -21 0.0493 -3.9999 15.9998 -21.0000 -0.8770 -0.4584 0.0692

_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_1_chcl3
_database_code_depnum_ccdc_archive 'CCDC 1556027'
_audit_update_record             
;
2017-06-14 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_1_chcl3             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          16 Note  
RESPONSE: The reason here causing 16 missing FCF reflections below
Theta-min is beamstop theta-min limit set at too high angle.
;
# end Validation Reply Form
_audit_creation_date             2017-05-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H68 Br4 O8, C H Cl3'
_chemical_formula_sum            'C65 H69 Br4 Cl3 O8'
_chemical_formula_weight         1404.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C70 H60 O8 Br4 Cl3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.4249(2)
_cell_length_b                   25.2475(3)
_cell_length_c                   17.8123(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.8364(16)
_cell_angle_gamma                90
_cell_volume                     6371.46(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11017
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      24.6640
_cell_measurement_theta_min      3.0020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.705
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.3132
_exptl_crystal_size_mid          0.1081
_exptl_crystal_size_min          0.094
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40713
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.249
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.833
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.8668
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -85.00  -18.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.4618  -19.0000   90.0000 134

#__ type_ start__ end____ width___ exp.time_
  2 omega  -90.00  -35.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.4618 -178.0000  -30.0000 110

#__ type_ start__ end____ width___ exp.time_
  3 omega  -35.00   52.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.4618   57.0000 -150.0000 174

#__ type_ start__ end____ width___ exp.time_
  4 omega   17.00   44.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431  -99.0000  -90.0000 54

#__ type_ start__ end____ width___ exp.time_
  5 omega   -4.00   23.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431   77.0000  -90.0000 54

#__ type_ start__ end____ width___ exp.time_
  6 omega  -47.00    1.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431  -77.0000  -90.0000 96

#__ type_ start__ end____ width___ exp.time_
  7 omega   45.00   71.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431   37.0000   30.0000 52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0400610000
_diffrn_orient_matrix_UB_12      0.0119319000
_diffrn_orient_matrix_UB_13      -0.0229699000
_diffrn_orient_matrix_UB_21      0.0290531000
_diffrn_orient_matrix_UB_22      0.0103525000
_diffrn_orient_matrix_UB_23      -0.0244973000
_diffrn_orient_matrix_UB_31      -0.0076224000
_diffrn_orient_matrix_UB_32      -0.0232330000
_diffrn_orient_matrix_UB_33      -0.0227054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8282
_reflns_number_total             11503
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         11503
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0505
_refine_ls_restrained_S_all      1.030
_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)+(0.0763P)²+6.2156P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1495
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C46B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3. Others
 Fixed Sof: H29A(0.6) H29B(0.6) H29C(0.4) H29D(0.4) C30(0.6) H30A(0.6)
 H30B(0.6) C30B(0.4) H30C(0.4) H30D(0.4) C31(0.6) H31A(0.6) H31B(0.6) C31B(0.4)
 H31C(0.4) H31D(0.4) H32A(0.6) H32B(0.6) H32C(0.6) H32D(0.4) H32E(0.4)
 H32F(0.4) H45A(0.6) H45B(0.6) H45C(0.4) H45D(0.4) C46(0.6) H46A(0.6) H46B(0.6)
 C46B(0.4) H46C(0.4) H46D(0.4) C47(0.6) H47A(0.6) H47B(0.6) C47B(0.4) H47C(0.4)
 H47D(0.4) H48D(0.4) H48E(0.4) H48F(0.4) H48A(0.6) H48B(0.6) H48C(0.6)
 H62C(0.4) H62D(0.4) H62A(0.6) H62B(0.6) C63(0.6) H63A(0.6) H63B(0.6) C63B(0.4)
 H63C(0.4) H63D(0.4) C64(0.6) H64A(0.6) H64B(0.6) H64C(0.6) C64B(0.4) H64D(0.4)
 H64E(0.4) H64F(0.4)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C26(H26), C42(H42), C58(H58), C65(H65)
4.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
  C29(H29C,H29D), C30(H30A,H30B), C30B(H30C,H30D), C31(H31A,H31B), C31B(H31C,
 H31D), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C45(H45C,H45D), C46(H46A,H46B), C46B(H46C,H46D), C47(H47A,H47B), C47B(H47C,
 H47D), C57(H57A,H57B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B),
 C62(H62C,H62D), C62(H62A,H62B), C63(H63A,H63B), C63B(H63C,H63D)
4.c Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C32(H32D,H32E,H32F), C48(H48D,H48E,H48F), C48(H48A,H48B,
 H48C)
4.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C22(H22), C38(H38), C54(H54)
4.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C64(H64A,H64B,H64C), C64B(H64D,H64E,H64F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.77295(4) -0.14190(2) 0.30019(3) 0.06537(18) Uani 1 1 d . . . . .
Br2 Br 0.46766(3) -0.07965(2) 0.63984(3) 0.05418(15) Uani 1 1 d . . . . .
Br3 Br 0.04166(3) 0.07768(2) 0.35457(3) 0.05848(17) Uani 1 1 d . . . . .
Br4 Br 0.38312(4) -0.02670(2) 0.03362(3) 0.06745(19) Uani 1 1 d . . . . .
C1 C 0.7865(2) 0.11841(15) 0.3065(2) 0.0296(8) Uani 1 1 d . . . . .
C2 C 0.7906(3) 0.06435(16) 0.2946(2) 0.0329(9) Uani 1 1 d . . . . .
C3 C 0.8056(3) 0.02845(16) 0.3556(2) 0.0353(9) Uani 1 1 d . . . . .
C4 C 0.8183(3) 0.04850(15) 0.4302(2) 0.0336(9) Uani 1 1 d . . . . .
C5 C 0.8144(2) 0.10236(15) 0.4447(2) 0.0316(9) Uani 1 1 d . . . . .
C6 C 0.7984(2) 0.13647(15) 0.3817(2) 0.0317(9) Uani 1 1 d . . . . .
H6 H 0.7954 0.1735 0.3905 0.038 Uiso 1 1 calc R . . . .
C7 C 0.8014(3) -0.02789(16) 0.3409(2) 0.0361(9) Uani 1 1 d . . . . .
C8 C 0.7922(3) -0.07298(17) 0.3253(3) 0.0437(10) Uani 1 1 d . . . . .
C9 C 0.7560(3) -0.00212(16) 0.5210(3) 0.0423(10) Uani 1 1 d . . . . .
H9A H 0.7618 -0.0398 0.5365 0.051 Uiso 1 1 calc R . . . .
H9B H 0.6985 0.0015 0.4811 0.051 Uiso 1 1 calc R . . . .
C10 C 0.8234(3) 0.12173(16) 0.5266(2) 0.0340(9) Uani 1 1 d . . . . .
H10 H 0.8633 0.0957 0.5606 0.041 Uiso 1 1 calc R . . . .
C11 C 0.8714(3) 0.17638(16) 0.5399(2) 0.0370(9) Uani 1 1 d . . . . .
H11A H 0.8345 0.2023 0.5046 0.044 Uiso 1 1 calc R . . . .
H11B H 0.8698 0.1880 0.5927 0.044 Uiso 1 1 calc R . . . .
C12 C 0.9735(3) 0.17737(18) 0.5282(3) 0.0434(10) Uani 1 1 d . . . . .
H12A H 1.0137 0.1579 0.5704 0.052 Uiso 1 1 calc R . . . .
H12B H 0.9778 0.1592 0.4797 0.052 Uiso 1 1 calc R . . . .
C13 C 1.0098(3) 0.23376(18) 0.5259(3) 0.0499(12) Uani 1 1 d . . . . .
H13A H 0.9691 0.2527 0.4834 0.060 Uiso 1 1 calc R . . . .
H13B H 1.0032 0.2517 0.5740 0.060 Uiso 1 1 calc R . . . .
C14 C 1.1115(3) 0.23891(19) 0.5158(3) 0.0503(12) Uani 1 1 d . . . . .
H14A H 1.1199 0.2187 0.4699 0.060 Uiso 1 1 calc R . . . .
H14B H 1.1532 0.2230 0.5606 0.060 Uiso 1 1 calc R . . . .
C15 C 1.1413(3) 0.2963(2) 0.5073(3) 0.0592(14) Uani 1 1 d . . . . .
H15A H 1.1000 0.3119 0.4620 0.071 Uiso 1 1 calc R . . . .
H15B H 1.1312 0.3165 0.5527 0.071 Uiso 1 1 calc R . . . .
C16 C 1.2420(4) 0.3028(3) 0.4989(4) 0.089(2) Uani 1 1 d . . . . .
H16A H 1.2505 0.2878 0.4499 0.133 Uiso 1 1 calc GR . . . .
H16B H 1.2832 0.2843 0.5407 0.133 Uiso 1 1 calc GR . . . .
H16C H 1.2581 0.3405 0.5005 0.133 Uiso 1 1 calc GR . . . .
C17 C 0.7244(3) 0.12045(16) 0.5459(2) 0.0341(9) Uani 1 1 d . . . . .
C18 C 0.6905(3) 0.07341(16) 0.5711(2) 0.0370(9) Uani 1 1 d . . . . .
C19 C 0.5974(3) 0.07088(17) 0.5855(2) 0.0397(10) Uani 1 1 d . . . . .
C20 C 0.5430(3) 0.11651(17) 0.5776(2) 0.0369(10) Uani 1 1 d . . . . .
C21 C 0.5737(3) 0.16391(16) 0.5515(2) 0.0336(9) Uani 1 1 d . . . . .
C22 C 0.6652(3) 0.16434(16) 0.5358(2) 0.0336(9) Uani 1 1 d . . . . .
H22 H 0.6880 0.1962 0.5174 0.040 Uiso 1 1 calc R . . . .
C23 C 0.5592(3) 0.02155(18) 0.6068(2) 0.0409(10) Uani 1 1 d . . . . .
C24 C 0.5231(3) -0.01854(18) 0.6199(2) 0.0433(10) Uani 1 1 d . . . . .
C25 C 0.3733(3) 0.10895(17) 0.5431(2) 0.0422(10) Uani 1 1 d . . . . .
H25A H 0.3898 0.0890 0.4997 0.051 Uiso 1 1 calc R . . . .
H25B H 0.3258 0.0880 0.5638 0.051 Uiso 1 1 calc R . . . .
C26 C 0.5106(3) 0.21144(16) 0.5400(2) 0.0362(9) Uani 1 1 d . . . . .
H26 H 0.4682 0.2084 0.5783 0.043 Uiso 1 1 calc R . . . .
C27 C 0.5635(3) 0.26424(16) 0.5566(3) 0.0422(10) Uani 1 1 d . . . . .
H27A H 0.6076 0.2615 0.6062 0.051 Uiso 1 1 calc R . . . .
H27B H 0.6016 0.2705 0.5166 0.051 Uiso 1 1 calc R . . . .
C28 C 0.4987(3) 0.31134(18) 0.5591(3) 0.0534(12) Uani 1 1 d . . . . .
H28A H 0.4496 0.3017 0.5888 0.064 Uiso 1 1 calc R . . . .
H28B H 0.4666 0.3201 0.5064 0.064 Uiso 1 1 calc R . . . .
C29 C 0.5520(4) 0.3597(2) 0.5950(4) 0.085(2) Uani 1 1 d . . . . .
H29A H 0.5922 0.3738 0.5603 0.102 Uiso 0.6 1 calc R . P A 1
H29B H 0.5935 0.3495 0.6437 0.102 Uiso 0.6 1 calc R . P A 1
H29C H 0.6192 0.3564 0.5905 0.102 Uiso 0.4 1 calc R . P B 2
H29D H 0.5493 0.3606 0.6501 0.102 Uiso 0.4 1 calc R . P B 2
C30 C 0.4791(8) 0.4043(4) 0.6109(6) 0.056(2) Uani 0.6 1 d . . P C 1
H30A H 0.4268 0.3881 0.6318 0.068 Uiso 0.6 1 calc R . P C 1
H30B H 0.5113 0.4305 0.6483 0.068 Uiso 0.6 1 calc R . P C 1
C30B C 0.5115(11) 0.4138(5) 0.5569(11) 0.065(4) Uani 0.4 1 d . . P C 2
H30C H 0.5584 0.4427 0.5685 0.079 Uiso 0.4 1 calc R . P C 2
H30D H 0.4924 0.4102 0.5008 0.079 Uiso 0.4 1 calc R . P C 2
C31 C 0.4427(8) 0.4300(4) 0.5383(7) 0.069(3) Uani 0.6 1 d . . P C 1
H31A H 0.4054 0.4046 0.5024 0.082 Uiso 0.6 1 calc R . P C 1
H31B H 0.4953 0.4434 0.5150 0.082 Uiso 0.6 1 calc R . P C 1
C31B C 0.4268(14) 0.4236(7) 0.5942(13) 0.078(5) Uani 0.4 1 d . . P C 2
H31C H 0.4467 0.4285 0.6501 0.093 Uiso 0.4 1 calc R . P C 2
H31D H 0.3820 0.3936 0.5847 0.093 Uiso 0.4 1 calc R . P C 2
C32 C 0.3796(5) 0.4764(3) 0.5553(5) 0.109(3) Uani 1 1 d . . . . .
H32A H 0.3535 0.4948 0.5076 0.163 Uiso 0.6 1 calc R . P C 1
H32B H 0.3279 0.4625 0.5782 0.163 Uiso 0.6 1 calc R . P C 1
H32C H 0.4174 0.5012 0.5908 0.163 Uiso 0.6 1 calc R . P C 1
H32D H 0.3238 0.4852 0.5769 0.163 Uiso 0.4 1 calc R . P C 2
H32E H 0.4251 0.5055 0.5650 0.163 Uiso 0.4 1 calc R . P C 2
H32F H 0.3607 0.4709 0.5000 0.163 Uiso 0.4 1 calc R . P C 2
C33 C 0.4466(3) 0.20786(15) 0.4613(2) 0.0359(9) Uani 1 1 d . . . . .
C34 C 0.3630(3) 0.17880(16) 0.4523(2) 0.0367(9) Uani 1 1 d . . . . .
C35 C 0.3057(3) 0.17100(16) 0.3810(3) 0.0376(10) Uani 1 1 d . . . . .
C36 C 0.3338(3) 0.19268(16) 0.3165(2) 0.0364(9) Uani 1 1 d . . . . .
C37 C 0.4160(3) 0.22251(15) 0.3231(2) 0.0348(9) Uani 1 1 d . . . . .
C38 C 0.4709(3) 0.22942(15) 0.3955(2) 0.0346(9) Uani 1 1 d . . . . .
H38 H 0.5273 0.2496 0.4003 0.041 Uiso 1 1 calc R . . . .
C39 C 0.2204(3) 0.14059(17) 0.3728(2) 0.0394(10) Uani 1 1 d . . . . .
C40 C 0.1496(3) 0.11557(17) 0.3646(3) 0.0433(11) Uani 1 1 d . . . . .
C41 C 0.3037(3) 0.14246(18) 0.2025(3) 0.0445(11) Uani 1 1 d . . . . .
H41A H 0.2464 0.1251 0.1735 0.053 Uiso 1 1 calc R . . . .
H41B H 0.3389 0.1158 0.2374 0.053 Uiso 1 1 calc R . . . .
C42 C 0.4460(3) 0.24313(16) 0.2506(2) 0.0372(9) Uani 1 1 d . . . . .
H42 H 0.3870 0.2475 0.2114 0.045 Uiso 1 1 calc R . . . .
C43 C 0.4951(3) 0.29753(15) 0.2599(3) 0.0403(10) Uani 1 1 d . . . . .
H43A H 0.5492 0.2958 0.3033 0.048 Uiso 1 1 calc R . . . .
H43B H 0.5203 0.3055 0.2132 0.048 Uiso 1 1 calc R . . . .
C44 C 0.4302(4) 0.34233(18) 0.2741(3) 0.0568(13) Uani 1 1 d . . . . .
H44A H 0.4082 0.3357 0.3227 0.068 Uiso 1 1 calc R . . . .
H44B H 0.3741 0.3428 0.2324 0.068 Uiso 1 1 calc R . . . .
C45 C 0.4785(5) 0.3965(2) 0.2783(4) 0.085(2) Uani 1 1 d . . . . .
H45A H 0.5232 0.3964 0.2424 0.102 Uiso 0.6 1 calc R . P D 1
H45B H 0.5161 0.4010 0.3304 0.102 Uiso 0.6 1 calc R . P D 1
H45C H 0.4868 0.4069 0.2264 0.102 Uiso 0.4 1 calc R . P E 2
H45D H 0.5420 0.3936 0.3108 0.102 Uiso 0.4 1 calc R . P E 2
C46 C 0.4123(12) 0.4454(4) 0.2598(8) 0.078(3) Uani 0.6 1 d . . P F 1
H46A H 0.4509 0.4776 0.2576 0.094 Uiso 0.6 1 calc R . P F 1
H46B H 0.3714 0.4406 0.2090 0.094 Uiso 0.6 1 calc R . P F 1
C46B C 0.4210(19) 0.4411(8) 0.3117(18) 0.101(7) Uani 0.4 1 d . U P F 2
H46C H 0.4052 0.4287 0.3605 0.121 Uiso 0.4 1 calc R . P F 2
H46D H 0.4609 0.4731 0.3226 0.121 Uiso 0.4 1 calc R . P F 2
C47 C 0.3526(12) 0.4526(5) 0.3184(10) 0.095(4) Uani 0.6 1 d . . P F 1
H47A H 0.3926 0.4590 0.3691 0.114 Uiso 0.6 1 calc R . P F 1
H47B H 0.3142 0.4205 0.3217 0.114 Uiso 0.6 1 calc R . P F 1
C47B C 0.3374(14) 0.4544(9) 0.2608(12) 0.094(6) Uani 0.4 1 d . . P F 2
H47C H 0.2949 0.4233 0.2532 0.113 Uiso 0.4 1 calc R . P F 2
H47D H 0.3524 0.4643 0.2107 0.113 Uiso 0.4 1 calc R . P F 2
C48 C 0.2857(5) 0.5023(3) 0.2932(5) 0.114(3) Uani 1 1 d . . . . .
H48D H 0.2277 0.5110 0.2570 0.171 Uiso 0.4 1 calc R . P F 2
H48E H 0.2700 0.4924 0.3425 0.171 Uiso 0.4 1 calc R . P F 2
H48F H 0.3275 0.5333 0.3000 0.171 Uiso 0.4 1 calc R . P F 2
H48A H 0.2452 0.5082 0.3308 0.171 Uiso 0.6 1 calc R . P F 1
H48B H 0.3245 0.5339 0.2902 0.171 Uiso 0.6 1 calc R . P F 1
H48C H 0.2464 0.4954 0.2430 0.171 Uiso 0.6 1 calc R . P F 1
C49 C 0.5033(3) 0.19966(15) 0.2218(2) 0.0336(9) Uani 1 1 d . . . . .
C50 C 0.4580(3) 0.15895(17) 0.1762(2) 0.0362(9) Uani 1 1 d . . . . .
C51 C 0.5085(3) 0.11732(16) 0.1516(2) 0.0355(9) Uani 1 1 d . . . . .
C52 C 0.6066(3) 0.11828(16) 0.1697(2) 0.0342(9) Uani 1 1 d . . . . .
C53 C 0.6553(3) 0.15800(15) 0.2153(2) 0.0325(9) Uani 1 1 d . . . . .
C54 C 0.6012(3) 0.19767(15) 0.2406(2) 0.0314(9) Uani 1 1 d . . . . .
H54 H 0.6330 0.2248 0.2724 0.038 Uiso 1 1 calc R . . . .
C55 C 0.4613(3) 0.07272(18) 0.1111(3) 0.0416(10) Uani 1 1 d . . . . .
C56 C 0.4283(3) 0.03301(19) 0.0824(3) 0.0471(11) Uani 1 1 d . . . . .
C57 C 0.6893(3) 0.03549(16) 0.1817(2) 0.0392(10) Uani 1 1 d . . . . .
H57A H 0.6879 0.0041 0.1481 0.047 Uiso 1 1 calc R . . . .
H57B H 0.6473 0.0283 0.2185 0.047 Uiso 1 1 calc R . . . .
C58 C 0.7625(3) 0.15560(15) 0.2376(2) 0.0322(9) Uani 1 1 d . . . . .
H58 H 0.7859 0.1382 0.1944 0.039 Uiso 1 1 calc R . . . .
C59 C 0.8092(3) 0.21009(15) 0.2487(2) 0.0365(9) Uani 1 1 d . . . . .
H59A H 0.7885 0.2312 0.2016 0.044 Uiso 1 1 calc R . . . .
H59B H 0.7867 0.2285 0.2910 0.044 Uiso 1 1 calc R . . . .
C60 C 0.9167(3) 0.20875(16) 0.2663(3) 0.0384(10) Uani 1 1 d . . . . .
H60A H 0.9393 0.1849 0.2294 0.046 Uiso 1 1 calc R . . . .
H60B H 0.9381 0.1940 0.3181 0.046 Uiso 1 1 calc R . . . .
C61 C 0.9602(3) 0.26344(18) 0.2620(3) 0.0487(11) Uani 1 1 d . . . . .
H61A H 0.9396 0.2777 0.2098 0.058 Uiso 1 1 calc R . . . .
H61B H 0.9357 0.2874 0.2978 0.058 Uiso 1 1 calc R . . . .
C62 C 1.0668(3) 0.2639(2) 0.2811(3) 0.0584(13) Uani 1 1 d . . . . .
H62C H 1.0942 0.2427 0.2439 0.070 Uiso 0.4 1 calc R . P G 2
H62D H 1.0904 0.2501 0.3332 0.070 Uiso 0.4 1 calc R . P G 2
H62A H 1.0887 0.2331 0.2548 0.070 Uiso 0.6 1 calc R . P H 1
H62B H 1.0850 0.2570 0.3366 0.070 Uiso 0.6 1 calc R . P H 1
C63 C 1.1247(9) 0.3122(7) 0.2634(8) 0.053(3) Uani 0.6 1 d . . P I 1
H63A H 1.1919 0.3067 0.2866 0.063 Uiso 0.6 1 calc R . P I 1
H63B H 1.1201 0.3152 0.2074 0.063 Uiso 0.6 1 calc R . P I 1
C63B C 1.0896(15) 0.3238(13) 0.2753(15) 0.068(8) Uani 0.4 1 d . . P I 2
H63C H 1.0510 0.3389 0.2283 0.081 Uiso 0.4 1 calc R . P I 2
H63D H 1.0743 0.3429 0.3199 0.081 Uiso 0.4 1 calc R . P I 2
C64 C 1.0908(8) 0.3630(4) 0.2935(6) 0.072(3) Uani 0.6 1 d . . P I 1
H64A H 1.0251 0.3694 0.2689 0.109 Uiso 0.6 1 calc GR . P I 1
H64B H 1.1303 0.3924 0.2823 0.109 Uiso 0.6 1 calc GR . P I 1
H64C H 1.0949 0.3601 0.3489 0.109 Uiso 0.6 1 calc GR . P I 1
C64B C 1.1936(11) 0.3298(8) 0.2731(11) 0.098(6) Uani 0.4 1 d . . P I 2
H64D H 1.2077 0.3119 0.2278 0.147 Uiso 0.4 1 calc GR . P I 2
H64E H 1.2313 0.3140 0.3192 0.147 Uiso 0.4 1 calc GR . P I 2
H64F H 1.2091 0.3675 0.2710 0.147 Uiso 0.4 1 calc GR . P I 2
O1 O 0.78228(19) 0.04328(11) 0.22209(15) 0.0368(6) Uani 1 1 d . . . . .
O2 O 0.83542(19) 0.01229(11) 0.48977(16) 0.0386(7) Uani 1 1 d . . . . .
O3 O 0.74577(19) 0.02900(11) 0.58484(16) 0.0420(7) Uani 1 1 d . . . . .
O4 O 0.45522(19) 0.11434(12) 0.60066(16) 0.0417(7) Uani 1 1 d . . . . .
O5 O 0.33307(19) 0.15780(12) 0.51619(16) 0.0411(7) Uani 1 1 d . . . . .
O6 O 0.27649(18) 0.18437(12) 0.24617(17) 0.0427(7) Uani 1 1 d . . . . .
O7 O 0.36103(19) 0.15968(12) 0.15033(16) 0.0420(7) Uani 1 1 d . . . . .
O8 O 0.65532(19) 0.07989(11) 0.13681(15) 0.0378(7) Uani 1 1 d . . . . .
C65 C 0.8052(3) 0.35656(18) 0.4581(3) 0.0521(12) Uani 1 1 d . . . . .
H65 H 0.8313 0.3500 0.5134 0.062 Uiso 1 1 calc R . . . .
Cl1 Cl 0.72389(11) 0.40713(6) 0.45145(13) 0.1018(6) Uani 1 1 d . . . . .
Cl2 Cl 0.89810(11) 0.37405(7) 0.41303(10) 0.0843(5) Uani 1 1 d . . . . .
Cl3 Cl 0.75077(10) 0.29761(5) 0.41796(8) 0.0658(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C8 1.805(4) . ?
Br2 C24 1.804(4) . ?
Br3 C40 1.807(4) . ?
Br4 C56 1.800(5) . ?
C1 C2 1.384(5) . ?
C1 C6 1.394(5) . ?
C1 C58 1.532(5) . ?
C2 C3 1.400(6) . ?
C2 O1 1.381(5) . ?
C3 C4 1.402(6) . ?
C3 C7 1.445(6) . ?
C4 C5 1.387(5) . ?
C4 O2 1.387(5) . ?
C5 C6 1.398(5) . ?
C5 C10 1.521(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.174(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 O2 1.412(5) . ?
C9 O3 1.413(5) . ?
C10 H10 1.0000 . ?
C10 C11 1.542(5) . ?
C10 C17 1.530(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.526(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.520(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.516(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.527(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.496(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.391(6) . ?
C17 C22 1.390(6) . ?
C18 C19 1.416(6) . ?
C18 O3 1.371(5) . ?
C19 C20 1.386(6) . ?
C19 C23 1.441(6) . ?
C20 C21 1.387(6) . ?
C20 O4 1.404(5) . ?
C21 C22 1.399(5) . ?
C21 C26 1.497(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.181(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 O4 1.417(5) . ?
C25 O5 1.408(5) . ?
C26 H26 1.0000 . ?
C26 C27 1.537(6) . ?
C26 C33 1.529(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.519(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.519(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 H29C 0.9900 . ?
C29 H29D 0.9900 . ?
C29 C30 1.603(12) . ?
C29 C30B 1.588(17) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.454(15) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C30B C31B 1.52(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.548(12) . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?
C31B C32 1.59(2) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32 H32D 0.9800 . ?
C32 H32E 0.9800 . ?
C32 H32F 0.9800 . ?
C33 C34 1.395(6) . ?
C33 C38 1.396(6) . ?
C34 C35 1.394(6) . ?
C34 O5 1.395(5) . ?
C35 C36 1.400(6) . ?
C35 C39 1.434(6) . ?
C36 C37 1.392(6) . ?
C36 O6 1.380(5) . ?
C37 C38 1.392(6) . ?
C37 C42 1.528(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.186(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 O6 1.412(5) . ?
C41 O7 1.423(5) . ?
C42 H42 1.0000 . ?
C42 C43 1.540(6) . ?
C42 C49 1.520(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.519(6) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.530(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 H45C 0.9900 . ?
C45 H45D 0.9900 . ?
C45 C46 1.558(15) . ?
C45 C46B 1.58(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.485(18) . ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C46B C47B 1.41(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.596(16) . ?
C47B H47C 0.9900 . ?
C47B H47D 0.9900 . ?
C47B C48 1.58(2) . ?
C48 H48D 0.9800 . ?
C48 H48E 0.9800 . ?
C48 H48F 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.394(6) . ?
C49 C54 1.390(5) . ?
C50 C51 1.395(6) . ?
C50 O7 1.389(5) . ?
C51 C52 1.392(6) . ?
C51 C55 1.438(6) . ?
C52 C53 1.394(6) . ?
C52 O8 1.389(5) . ?
C53 C54 1.395(5) . ?
C53 C58 1.524(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.184(6) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 O1 1.411(5) . ?
C57 O8 1.410(5) . ?
C58 H58 1.0000 . ?
C58 C59 1.528(5) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.523(6) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.524(6) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.512(7) . ?
C62 H62C 0.9900 . ?
C62 H62D 0.9900 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.544(16) . ?
C62 C63B 1.55(3) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.51(2) . ?
C63B H63C 0.9900 . ?
C63B H63D 0.9900 . ?
C63B C64B 1.52(2) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C64B H64D 0.9800 . ?
C64B H64E 0.9800 . ?
C64B H64F 0.9800 . ?
C65 H65 1.0000 . ?
C65 Cl1 1.723(5) . ?
C65 Cl2 1.744(5) . ?
C65 Cl3 1.770(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 118.0(4) . . ?
C2 C1 C58 119.4(3) . . ?
C6 C1 C58 122.5(3) . . ?
C1 C2 C3 121.6(4) . . ?
O1 C2 C1 121.6(4) . . ?
O1 C2 C3 116.7(3) . . ?
C2 C3 C4 118.4(4) . . ?
C2 C3 C7 120.1(4) . . ?
C4 C3 C7 121.3(4) . . ?
C5 C4 C3 121.8(4) . . ?
C5 C4 O2 120.8(4) . . ?
O2 C4 C3 117.4(3) . . ?
C4 C5 C6 117.5(4) . . ?
C4 C5 C10 119.6(4) . . ?
C6 C5 C10 122.9(4) . . ?
C1 C6 C5 122.7(4) . . ?
C1 C6 H6 118.6 . . ?
C5 C6 H6 118.6 . . ?
C8 C7 C3 175.2(5) . . ?
C7 C8 Br1 177.7(4) . . ?
H9A C9 H9B 107.8 . . ?
O2 C9 H9A 109.0 . . ?
O2 C9 H9B 109.0 . . ?
O2 C9 O3 112.9(3) . . ?
O3 C9 H9A 109.0 . . ?
O3 C9 H9B 109.0 . . ?
C5 C10 H10 107.7 . . ?
C5 C10 C11 112.9(3) . . ?
C5 C10 C17 107.1(3) . . ?
C11 C10 H10 107.7 . . ?
C17 C10 H10 107.7 . . ?
C17 C10 C11 113.3(3) . . ?
C10 C11 H11A 108.7 . . ?
C10 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 C10 114.3(3) . . ?
C12 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
C11 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
C13 C12 C11 111.4(4) . . ?
C13 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C12 C13 H13A 108.4 . . ?
C12 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 C12 115.4(4) . . ?
C14 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C13 C14 C15 113.0(4) . . ?
H14A C14 H14B 107.8 . . ?
C15 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
C14 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C16 C15 C14 114.3(5) . . ?
C16 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C10 119.4(4) . . ?
C22 C17 C10 122.1(4) . . ?
C22 C17 C18 118.5(4) . . ?
C17 C18 C19 120.0(4) . . ?
O3 C18 C17 121.9(4) . . ?
O3 C18 C19 118.1(4) . . ?
C18 C19 C23 120.6(4) . . ?
C20 C19 C18 118.8(4) . . ?
C20 C19 C23 120.6(4) . . ?
C19 C20 C21 122.8(4) . . ?
C19 C20 O4 117.5(4) . . ?
C21 C20 O4 119.7(4) . . ?
C20 C21 C22 116.5(4) . . ?
C20 C21 C26 120.8(3) . . ?
C22 C21 C26 122.6(4) . . ?
C17 C22 C21 123.3(4) . . ?
C17 C22 H22 118.4 . . ?
C21 C22 H22 118.4 . . ?
C24 C23 C19 175.4(5) . . ?
C23 C24 Br2 179.8(5) . . ?
H25A C25 H25B 107.7 . . ?
O4 C25 H25A 108.9 . . ?
O4 C25 H25B 108.9 . . ?
O5 C25 H25A 108.9 . . ?
O5 C25 H25B 108.9 . . ?
O5 C25 O4 113.4(3) . . ?
C21 C26 H26 106.3 . . ?
C21 C26 C27 113.6(3) . . ?
C21 C26 C33 108.9(3) . . ?
C27 C26 H26 106.3 . . ?
C33 C26 H26 106.3 . . ?
C33 C26 C27 114.8(3) . . ?
C26 C27 H27A 108.9 . . ?
C26 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 C26 113.5(3) . . ?
C28 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C27 C28 H28A 109.2 . . ?
C27 C28 H28B 109.2 . . ?
C27 C28 C29 112.1(4) . . ?
H28A C28 H28B 107.9 . . ?
C29 C28 H28A 109.2 . . ?
C29 C28 H28B 109.2 . . ?
C28 C29 H29A 109.7 . . ?
C28 C29 H29B 109.7 . . ?
C28 C29 H29C 108.9 . . ?
C28 C29 H29D 108.9 . . ?
C28 C29 C30 110.0(5) . . ?
C28 C29 C30B 113.2(7) . . ?
H29A C29 H29B 108.2 . . ?
H29C C29 H29D 107.7 . . ?
C30 C29 H29A 109.7 . . ?
C30 C29 H29B 109.7 . . ?
C30B C29 H29C 108.9 . . ?
C30B C29 H29D 108.9 . . ?
C29 C30 H30A 110.3 . . ?
C29 C30 H30B 110.3 . . ?
H30A C30 H30B 108.5 . . ?
C31 C30 C29 107.2(9) . . ?
C31 C30 H30A 110.3 . . ?
C31 C30 H30B 110.3 . . ?
C29 C30B H30C 111.3 . . ?
C29 C30B H30D 111.3 . . ?
H30C C30B H30D 109.2 . . ?
C31B C30B C29 102.4(14) . . ?
C31B C30B H30C 111.3 . . ?
C31B C30B H30D 111.3 . . ?
C30 C31 H31A 110.3 . . ?
C30 C31 H31B 110.3 . . ?
C30 C31 C32 106.9(10) . . ?
H31A C31 H31B 108.6 . . ?
C32 C31 H31A 110.3 . . ?
C32 C31 H31B 110.3 . . ?
C30B C31B H31C 110.7 . . ?
C30B C31B H31D 110.7 . . ?
C30B C31B C32 105.0(14) . . ?
H31C C31B H31D 108.8 . . ?
C32 C31B H31C 110.7 . . ?
C32 C31B H31D 110.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
C31B C32 H32D 109.5 . . ?
C31B C32 H32E 109.5 . . ?
C31B C32 H32F 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
H32D C32 H32E 109.5 . . ?
H32D C32 H32F 109.5 . . ?
H32E C32 H32F 109.5 . . ?
C34 C33 C26 119.7(4) . . ?
C34 C33 C38 117.2(4) . . ?
C38 C33 C26 122.9(3) . . ?
C35 C34 C33 122.0(4) . . ?
C35 C34 O5 117.9(4) . . ?
O5 C34 C33 120.0(4) . . ?
C34 C35 C36 118.7(4) . . ?
C34 C35 C39 121.2(4) . . ?
C36 C35 C39 120.1(4) . . ?
C37 C36 C35 121.1(4) . . ?
O6 C36 C35 118.0(4) . . ?
O6 C36 C37 121.0(4) . . ?
C36 C37 C38 118.3(4) . . ?
C36 C37 C42 119.0(4) . . ?
C38 C37 C42 122.6(4) . . ?
C33 C38 H38 118.6 . . ?
C37 C38 C33 122.7(4) . . ?
C37 C38 H38 118.6 . . ?
C40 C39 C35 178.7(5) . . ?
C39 C40 Br3 178.5(4) . . ?
H41A C41 H41B 107.8 . . ?
O6 C41 H41A 109.0 . . ?
O6 C41 H41B 109.0 . . ?
O6 C41 O7 112.8(4) . . ?
O7 C41 H41A 109.0 . . ?
O7 C41 H41B 109.0 . . ?
C37 C42 H42 106.8 . . ?
C37 C42 C43 114.2(3) . . ?
C43 C42 H42 106.8 . . ?
C49 C42 C37 107.3(3) . . ?
C49 C42 H42 106.8 . . ?
C49 C42 C43 114.4(3) . . ?
C42 C43 H43A 108.9 . . ?
C42 C43 H43B 108.9 . . ?
H43A C43 H43B 107.7 . . ?
C44 C43 C42 113.4(4) . . ?
C44 C43 H43A 108.9 . . ?
C44 C43 H43B 108.9 . . ?
C43 C44 H44A 109.1 . . ?
C43 C44 H44B 109.1 . . ?
C43 C44 C45 112.6(4) . . ?
H44A C44 H44B 107.8 . . ?
C45 C44 H44A 109.1 . . ?
C45 C44 H44B 109.1 . . ?
C44 C45 H45A 108.2 . . ?
C44 C45 H45B 108.2 . . ?
C44 C45 H45C 109.0 . . ?
C44 C45 H45D 109.0 . . ?
C44 C45 C46 116.3(7) . . ?
C44 C45 C46B 112.9(12) . . ?
H45A C45 H45B 107.4 . . ?
H45C C45 H45D 107.8 . . ?
C46 C45 H45A 108.2 . . ?
C46 C45 H45B 108.2 . . ?
C46B C45 H45C 109.0 . . ?
C46B C45 H45D 109.0 . . ?
C45 C46 H46A 109.4 . . ?
C45 C46 H46B 109.4 . . ?
H46A C46 H46B 108.0 . . ?
C47 C46 C45 111.2(12) . . ?
C47 C46 H46A 109.4 . . ?
C47 C46 H46B 109.4 . . ?
C45 C46B H46C 109.2 . . ?
C45 C46B H46D 109.2 . . ?
H46C C46B H46D 107.9 . . ?
C47B C46B C45 112(2) . . ?
C47B C46B H46C 109.2 . . ?
C47B C46B H46D 109.2 . . ?
C46 C47 H47A 110.2 . . ?
C46 C47 H47B 110.2 . . ?
C46 C47 C48 107.3(13) . . ?
H47A C47 H47B 108.5 . . ?
C48 C47 H47A 110.2 . . ?
C48 C47 H47B 110.2 . . ?
C46B C47B H47C 109.5 . . ?
C46B C47B H47D 109.5 . . ?
C46B C47B C48 111(2) . . ?
H47C C47B H47D 108.1 . . ?
C48 C47B H47C 109.5 . . ?
C48 C47B H47D 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
C47B C48 H48D 109.5 . . ?
C47B C48 H48E 109.5 . . ?
C47B C48 H48F 109.5 . . ?
H48D C48 H48E 109.5 . . ?
H48D C48 H48F 109.5 . . ?
H48E C48 H48F 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 C42 120.3(4) . . ?
C54 C49 C42 122.5(4) . . ?
C54 C49 C50 117.2(4) . . ?
C49 C50 C51 121.6(4) . . ?
O7 C50 C49 121.0(4) . . ?
O7 C50 C51 117.3(4) . . ?
C50 C51 C55 121.5(4) . . ?
C52 C51 C50 118.8(4) . . ?
C52 C51 C55 119.6(4) . . ?
C51 C52 C53 121.7(4) . . ?
O8 C52 C51 117.6(3) . . ?
O8 C52 C53 120.6(3) . . ?
C52 C53 C54 117.0(4) . . ?
C52 C53 C58 119.9(3) . . ?
C54 C53 C58 123.1(3) . . ?
C49 C54 C53 123.6(4) . . ?
C49 C54 H54 118.2 . . ?
C53 C54 H54 118.2 . . ?
C56 C55 C51 173.7(5) . . ?
C55 C56 Br4 175.9(5) . . ?
H57A C57 H57B 107.9 . . ?
O1 C57 H57A 109.2 . . ?
O1 C57 H57B 109.2 . . ?
O8 C57 H57A 109.2 . . ?
O8 C57 H57B 109.2 . . ?
O8 C57 O1 112.0(3) . . ?
C1 C58 H58 106.9 . . ?
C53 C58 C1 107.4(3) . . ?
C53 C58 H58 106.9 . . ?
C53 C58 C59 113.5(3) . . ?
C59 C58 C1 114.9(3) . . ?
C59 C58 H58 106.9 . . ?
C58 C59 H59A 108.7 . . ?
C58 C59 H59B 108.7 . . ?
H59A C59 H59B 107.6 . . ?
C60 C59 C58 114.4(3) . . ?
C60 C59 H59A 108.7 . . ?
C60 C59 H59B 108.7 . . ?
C59 C60 H60A 109.1 . . ?
C59 C60 H60B 109.1 . . ?
C59 C60 C61 112.5(3) . . ?
H60A C60 H60B 107.8 . . ?
C61 C60 H60A 109.1 . . ?
C61 C60 H60B 109.1 . . ?
C60 C61 H61A 108.8 . . ?
C60 C61 H61B 108.8 . . ?
H61A C61 H61B 107.7 . . ?
C62 C61 C60 114.0(4) . . ?
C62 C61 H61A 108.8 . . ?
C62 C61 H61B 108.8 . . ?
C61 C62 H62C 111.3 . . ?
C61 C62 H62D 111.3 . . ?
C61 C62 H62A 106.9 . . ?
C61 C62 H62B 106.9 . . ?
C61 C62 C63 121.8(7) . . ?
C61 C62 C63B 102.2(9) . . ?
H62C C62 H62D 109.2 . . ?
H62A C62 H62B 106.7 . . ?
C63 C62 H62A 106.9 . . ?
C63 C62 H62B 106.9 . . ?
C63B C62 H62C 111.3 . . ?
C63B C62 H62D 111.3 . . ?
C62 C63 H63A 109.2 . . ?
C62 C63 H63B 109.2 . . ?
H63A C63 H63B 107.9 . . ?
C64 C63 C62 112.1(9) . . ?
C64 C63 H63A 109.2 . . ?
C64 C63 H63B 109.2 . . ?
C62 C63B H63C 109.9 . . ?
C62 C63B H63D 109.9 . . ?
H63C C63B H63D 108.3 . . ?
C64B C63B C62 108.8(18) . . ?
C64B C63B H63C 109.9 . . ?
C64B C63B H63D 109.9 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63B C64B H64D 109.5 . . ?
C63B C64B H64E 109.5 . . ?
C63B C64B H64F 109.5 . . ?
H64D C64B H64E 109.5 . . ?
H64D C64B H64F 109.5 . . ?
H64E C64B H64F 109.5 . . ?
C2 O1 C57 116.0(3) . . ?
C4 O2 C9 115.5(3) . . ?
C18 O3 C9 117.2(3) . . ?
C20 O4 C25 117.9(3) . . ?
C34 O5 C25 116.1(3) . . ?
C36 O6 C41 115.6(3) . . ?
C50 O7 C41 116.9(3) . . ?
C52 O8 C57 117.7(3) . . ?
Cl1 C65 H65 108.4 . . ?
Cl1 C65 Cl2 110.7(3) . . ?
Cl1 C65 Cl3 110.5(3) . . ?
Cl2 C65 H65 108.4 . . ?
Cl2 C65 Cl3 110.3(3) . . ?
Cl3 C65 H65 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.0(5) . . . . ?
C1 C2 C3 C7 174.7(3) . . . . ?
C1 C2 O1 C57 -84.2(4) . . . . ?
C1 C58 C59 C60 59.4(5) . . . . ?
C2 C1 C6 C5 0.4(5) . . . . ?
C2 C1 C58 C53 84.6(4) . . . . ?
C2 C1 C58 C59 -148.1(3) . . . . ?
C2 C3 C4 C5 1.3(5) . . . . ?
C2 C3 C4 O2 -178.5(3) . . . . ?
C3 C2 O1 C57 97.4(4) . . . . ?
C3 C4 C5 C6 -0.7(5) . . . . ?
C3 C4 C5 C10 176.7(3) . . . . ?
C3 C4 O2 C9 -98.0(4) . . . . ?
C4 C5 C6 C1 -0.1(5) . . . . ?
C4 C5 C10 C11 148.2(4) . . . . ?
C4 C5 C10 C17 -86.4(4) . . . . ?
C5 C4 O2 C9 82.3(4) . . . . ?
C5 C10 C11 C12 -63.4(5) . . . . ?
C5 C10 C17 C18 84.5(4) . . . . ?
C5 C10 C17 C22 -92.6(4) . . . . ?
C6 C1 C2 C3 0.2(5) . . . . ?
C6 C1 C2 O1 -178.1(3) . . . . ?
C6 C1 C58 C53 -90.9(4) . . . . ?
C6 C1 C58 C59 36.5(5) . . . . ?
C6 C5 C10 C11 -34.6(5) . . . . ?
C6 C5 C10 C17 90.9(4) . . . . ?
C7 C3 C4 C5 -174.4(4) . . . . ?
C7 C3 C4 O2 5.8(5) . . . . ?
C10 C5 C6 C1 -177.4(3) . . . . ?
C10 C11 C12 C13 168.2(4) . . . . ?
C10 C17 C18 C19 -176.8(4) . . . . ?
C10 C17 C18 O3 5.1(6) . . . . ?
C10 C17 C22 C21 178.6(4) . . . . ?
C11 C10 C17 C18 -150.3(4) . . . . ?
C11 C10 C17 C22 32.6(5) . . . . ?
C11 C12 C13 C14 179.0(4) . . . . ?
C12 C13 C14 C15 175.3(4) . . . . ?
C13 C14 C15 C16 178.8(5) . . . . ?
C17 C10 C11 C12 174.5(3) . . . . ?
C17 C18 C19 C20 -3.1(6) . . . . ?
C17 C18 C19 C23 175.9(4) . . . . ?
C17 C18 O3 C9 -80.6(5) . . . . ?
C18 C17 C22 C21 1.5(6) . . . . ?
C18 C19 C20 C21 4.1(6) . . . . ?
C18 C19 C20 O4 -172.8(4) . . . . ?
C19 C18 O3 C9 101.2(4) . . . . ?
C19 C20 C21 C22 -2.3(6) . . . . ?
C19 C20 C21 C26 176.8(4) . . . . ?
C19 C20 O4 C25 -101.6(4) . . . . ?
C20 C21 C22 C17 -0.5(6) . . . . ?
C20 C21 C26 C27 146.7(4) . . . . ?
C20 C21 C26 C33 -83.9(4) . . . . ?
C21 C20 O4 C25 81.4(5) . . . . ?
C21 C26 C27 C28 -169.4(4) . . . . ?
C21 C26 C33 C34 84.7(4) . . . . ?
C21 C26 C33 C38 -90.6(4) . . . . ?
C22 C17 C18 C19 0.4(6) . . . . ?
C22 C17 C18 O3 -177.7(3) . . . . ?
C22 C21 C26 C27 -34.2(5) . . . . ?
C22 C21 C26 C33 95.2(4) . . . . ?
C23 C19 C20 C21 -174.8(4) . . . . ?
C23 C19 C20 O4 8.2(6) . . . . ?
C26 C21 C22 C17 -179.7(4) . . . . ?
C26 C27 C28 C29 165.3(5) . . . . ?
C26 C33 C34 C35 -175.2(4) . . . . ?
C26 C33 C34 O5 6.7(6) . . . . ?
C26 C33 C38 C37 174.8(4) . . . . ?
C27 C26 C33 C34 -146.6(4) . . . . ?
C27 C26 C33 C38 38.2(5) . . . . ?
C27 C28 C29 C30 -169.3(6) . . . . ?
C27 C28 C29 C30B 144.4(8) . . . . ?
C28 C29 C30 C31 -77.9(9) . . . . ?
C28 C29 C30B C31B 80.0(14) . . . . ?
C29 C30 C31 C32 -174.8(6) . . . . ?
C29 C30B C31B C32 -177.4(11) . . . . ?
C33 C26 C27 C28 64.2(5) . . . . ?
C33 C34 C35 C36 0.6(6) . . . . ?
C33 C34 C35 C39 179.4(4) . . . . ?
C33 C34 O5 C25 -83.3(5) . . . . ?
C34 C33 C38 C37 -0.6(6) . . . . ?
C34 C35 C36 C37 -1.5(6) . . . . ?
C34 C35 C36 O6 179.7(3) . . . . ?
C35 C34 O5 C25 98.5(4) . . . . ?
C35 C36 C37 C38 1.3(6) . . . . ?
C35 C36 C37 C42 177.2(4) . . . . ?
C35 C36 O6 C41 -97.9(4) . . . . ?
C36 C37 C38 C33 -0.2(6) . . . . ?
C36 C37 C42 C43 145.9(4) . . . . ?
C36 C37 C42 C49 -86.3(4) . . . . ?
C37 C36 O6 C41 83.2(5) . . . . ?
C37 C42 C43 C44 -66.8(5) . . . . ?
C37 C42 C49 C50 84.1(4) . . . . ?
C37 C42 C49 C54 -94.3(4) . . . . ?
C38 C33 C34 C35 0.4(6) . . . . ?
C38 C33 C34 O5 -177.8(3) . . . . ?
C38 C37 C42 C43 -38.4(5) . . . . ?
C38 C37 C42 C49 89.5(4) . . . . ?
C39 C35 C36 C37 179.7(4) . . . . ?
C39 C35 C36 O6 0.9(6) . . . . ?
C42 C37 C38 C33 -176.0(4) . . . . ?
C42 C43 C44 C45 -176.5(4) . . . . ?
C42 C49 C50 C51 -177.2(4) . . . . ?
C42 C49 C50 O7 5.9(6) . . . . ?
C42 C49 C54 C53 179.5(4) . . . . ?
C43 C42 C49 C50 -148.1(4) . . . . ?
C43 C42 C49 C54 33.4(5) . . . . ?
C43 C44 C45 C46 156.2(7) . . . . ?
C43 C44 C45 C46B -166.6(11) . . . . ?
C44 C45 C46 C47 66.3(15) . . . . ?
C44 C45 C46B C47B -70(3) . . . . ?
C45 C46 C47 C48 -178.4(9) . . . . ?
C45 C46B C47B C48 -175.5(14) . . . . ?
C49 C42 C43 C44 169.1(4) . . . . ?
C49 C50 C51 C52 -3.7(6) . . . . ?
C49 C50 C51 C55 173.7(4) . . . . ?
C49 C50 O7 C41 -80.7(5) . . . . ?
C50 C49 C54 C53 1.1(6) . . . . ?
C50 C51 C52 C53 3.8(6) . . . . ?
C50 C51 C52 O8 -172.3(3) . . . . ?
C51 C50 O7 C41 102.3(4) . . . . ?
C51 C52 C53 C54 -1.6(6) . . . . ?
C51 C52 C53 C58 176.3(3) . . . . ?
C51 C52 O8 C57 -99.7(4) . . . . ?
C52 C53 C54 C49 -0.9(6) . . . . ?
C52 C53 C58 C1 -82.4(4) . . . . ?
C52 C53 C58 C59 149.5(4) . . . . ?
C53 C52 O8 C57 84.1(5) . . . . ?
C53 C58 C59 C60 -176.5(3) . . . . ?
C54 C49 C50 C51 1.3(6) . . . . ?
C54 C49 C50 O7 -175.6(3) . . . . ?
C54 C53 C58 C1 95.4(4) . . . . ?
C54 C53 C58 C59 -32.8(5) . . . . ?
C55 C51 C52 C53 -173.6(4) . . . . ?
C55 C51 C52 O8 10.3(6) . . . . ?
C58 C1 C2 C3 -175.5(3) . . . . ?
C58 C1 C2 O1 6.2(5) . . . . ?
C58 C1 C6 C5 175.9(3) . . . . ?
C58 C53 C54 C49 -178.7(3) . . . . ?
C58 C59 C60 C61 169.3(4) . . . . ?
C59 C60 C61 C62 178.6(4) . . . . ?
C60 C61 C62 C63 166.5(7) . . . . ?
C60 C61 C62 C63B -177.8(10) . . . . ?
C61 C62 C63 C64 50.9(12) . . . . ?
C61 C62 C63B C64B -165.9(14) . . . . ?
O1 C2 C3 C4 177.4(3) . . . . ?
O1 C2 C3 C7 -6.9(5) . . . . ?
O1 C57 O8 C52 -91.4(4) . . . . ?
O2 C4 C5 C6 179.0(3) . . . . ?
O2 C4 C5 C10 -3.6(5) . . . . ?
O2 C9 O3 C18 92.0(4) . . . . ?
O3 C9 O2 C4 -93.6(4) . . . . ?
O3 C18 C19 C20 175.1(4) . . . . ?
O3 C18 C19 C23 -5.9(6) . . . . ?
O4 C20 C21 C22 174.6(3) . . . . ?
O4 C20 C21 C26 -6.3(6) . . . . ?
O4 C25 O5 C34 92.4(4) . . . . ?
O5 C25 O4 C20 -91.2(4) . . . . ?
O5 C34 C35 C36 178.8(3) . . . . ?
O5 C34 C35 C39 -2.4(6) . . . . ?
O6 C36 C37 C38 -179.9(3) . . . . ?
O6 C36 C37 C42 -4.0(6) . . . . ?
O6 C41 O7 C50 91.3(4) . . . . ?
O7 C41 O6 C36 -93.9(4) . . . . ?
O7 C50 C51 C52 173.3(3) . . . . ?
O7 C50 C51 C55 -9.4(6) . . . . ?
O8 C52 C53 C54 174.5(3) . . . . ?
O8 C52 C53 C58 -7.7(6) . . . . ?
O8 C57 O1 C2 91.3(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5 26 -17 0.0489 4.9904 26.0123 -16.9870 0.5006 0.8304 -0.2567
1 -21 -20 0.0591 0.9708 -21.0197 -19.9907 0.1695 0.3003 0.9348
-1 21 20 0.0420 -0.9708 21.0197 19.9907 -0.1695 -0.3003 -0.9348
-5 -25 17 0.0437 -4.9900 -25.0116 16.9871 -0.4887 -0.8200 0.2334
1 29 14 0.0558 1.0253 29.0232 13.9952 -0.0162 -0.0126 -0.9999
-19 10 8 0.1432 -18.9806 10.0108 7.9953 0.6962 -0.6437 -0.2694
-20 -7 0 0.1415 -19.9951 -7.0027 -0.0020 0.7175 -0.6534 0.3152
19 11 2 0.1158 18.9991 11.0061 2.0012 -0.6758 0.6169 -0.4460
13 -23 -13 0.1114 12.9727 -23.0203 -12.9942 -0.4959 0.4569 0.7310
-4 -3 25 0.0352 -3.9736 -2.9947 24.9850 -0.4504 -0.7585 -0.4674
-3 -34 -6 0.0612 -3.0181 -34.0242 -6.0005 -0.1472 -0.2929 0.9497
4 35 -2 0.0561 4.0098 35.0225 -1.9948 0.3031 0.5279 -0.7990
3 -4 -25 0.0604 2.9713 -4.0099 -24.9858 0.4070 0.6569 0.6378

_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_3_dmso
_database_code_depnum_ccdc_archive 'CCDC 1556033'
_audit_update_record             
;
2017-06-14 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_3_dmso              
;
PROBLEM: Check Calcd Residual Density  0.14A From      I1       3.18 eA-3  
RESPONSE: The relatively large residual density is very close to the
heavy atom, which might be caused by the unsuitable absorption 
correction.
;
_vrf_PLAT972_3_dmso              
;
PROBLEM: Check Calcd Residual Density  0.85A From      I2      -2.51 eA-3  
RESPONSE: The density hole is close to the heavy atom, which might be
caused by the unsuitable absorption correction, same reason inducing
high residual density.
;
# end Validation Reply Form

_audit_creation_date             2017-05-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H76 I4 O8, 4(C2 H6 O S)'
_chemical_formula_sum            'C76 H100 I4 O12 S4'
_chemical_formula_weight         1841.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C80 H80 O8 I4 Br2'
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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   12.8712(5)
_cell_length_b                   16.8782(7)
_cell_length_c                   20.3485(12)
_cell_angle_alpha                111.180(5)
_cell_angle_beta                 95.315(4)
_cell_angle_gamma                99.321(3)
_cell_volume                     4012.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4360
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.5590
_cell_measurement_theta_min      3.5100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.619
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.284
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.2087
_exptl_crystal_size_mid          0.0234
_exptl_crystal_size_min          0.0209
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.1573
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25862
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         76.770
_diffrn_reflns_theta_min         2.938
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9906
_diffrn_measured_fraction_theta_max 0.9509
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -96.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  125.0000  120.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega -113.00  -13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -57.0000  -30.0000 100

#__ type_ start__ end____ width___ exp.time_
  3 omega  -48.00   30.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   37.0000  -90.0000 78

#__ type_ start__ end____ width___ exp.time_
  4 omega  -49.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   37.0000  120.0000 82

#__ type_ start__ end____ width___ exp.time_
  5 omega   29.00   99.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   60.0000 70

#__ type_ start__ end____ width___ exp.time_
  6 omega   39.00   98.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -60.0000 59

#__ type_ start__ end____ width___ exp.time_
  7 omega   36.00  145.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  150.0000 109

#__ type_ start__ end____ width___ exp.time_
  8 omega   36.00   91.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -120.0000 55

#__ type_ start__ end____ width___ exp.time_
  9 omega   49.00   91.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000    0.0000 42

#__ type_ start__ end____ width___ exp.time_
 10 omega   36.00   87.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 51

#__ type_ start__ end____ width___ exp.time_
 11 omega   37.00  116.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  150.0000 79

#__ type_ start__ end____ width___ exp.time_
 12 omega  104.00  177.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  -90.0000 73

#__ type_ start__ end____ width___ exp.time_
 13 omega   30.00  109.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -30.0000 79

#__ type_ start__ end____ width___ exp.time_
 14 omega   61.00  178.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000 -150.0000 117
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1006959000
_diffrn_orient_matrix_UB_12      -0.0282701000
_diffrn_orient_matrix_UB_13      0.0282357000
_diffrn_orient_matrix_UB_21      -0.0678316000
_diffrn_orient_matrix_UB_22      -0.0230000000
_diffrn_orient_matrix_UB_23      -0.0733980000
_diffrn_orient_matrix_UB_31      0.0194637000
_diffrn_orient_matrix_UB_32      -0.0932628000
_diffrn_orient_matrix_UB_33      -0.0243023000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8816
_reflns_number_total             16087
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.275
_refine_diff_density_min         -2.621
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       0.00049(7)
_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   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         16087
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_gt           0.0920
_refine_ls_restrained_S_all      1.027
_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)+(0.1202P)²+0.9006P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2372
_refine_ls_wR_factor_ref         0.2885
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C63) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C76) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(I4B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(I4B)=1-FVAR(1)
 Sof(I4A)=FVAR(1)
 Sof(S3B)=Sof(H73D)=Sof(H73E)=Sof(H73F)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(2)
 Sof(S3A)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(2)
 Sof(S4B)=Sof(H76D)=Sof(H76E)=Sof(H76F)=1-FVAR(3)
 Sof(S4A)=Sof(H76A)=Sof(H76B)=Sof(H76C)=FVAR(3)
 Fixed Sof: H75A(0.5) H75B(0.5) H75C(0.5) H75D(0.5) H75E(0.5) H75F(0.5)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C26(H26), C43(H43), C60(H60)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C16(H16A,H16B), C17(H17A,H17B), C27(H27A,H27B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C50(H50A,H50B), C51(H51A,H51B), C61(H61A,H61B), C62(H62A,H62B),
 C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C67(H67A,H67B), C68(H68A,H68B)
4.c Me refined with riding coordinates:
 C73(H73A,H73B,H73C), C73(H73D,H73E,H73F), C74(H74A,H74B,H74C), C74(H74D,H74E,
 H74F), C75(H75A,H75B,H75C), C75(H75D,H75E,H75F), C76(H76A,H76B,H76C), C76(H76D,
 H76E,H76F)
4.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C23(H23), C40(H40), C57(H57)
4.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C32(H32A,H32B,H32C), C49(H49A,H49B,H49C), C66(H66A,H66B,
 H66C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C69(H69A,H69B,H69C), C70(H70A,
 H70B,H70C)
;
_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
I1 I 0.58992(7) 0.58632(6) 1.09936(5) 0.0493(2) Uani 1 1 d . . . . .
I2 I 0.70883(8) 0.86539(5) 0.75606(5) 0.0551(3) Uani 1 1 d . . . . .
I3 I 0.28918(8) 0.23629(10) 0.46488(8) 0.0853(4) Uani 1 1 d . . . . .
I4A I 0.43349(8) -0.06520(6) 0.84650(7) 0.0550(4) Uani 0.917(4) 1 d . . P A 1
I4B I 0.4027(8) -0.0911(6) 0.7945(6) 0.043(3) Uani 0.083(4) 1 d . U P A 2
O1 O 0.8918(6) 0.6192(5) 0.9509(4) 0.0374(17) Uani 1 1 d . . . . .
O2 O 0.9380(6) 0.7042(4) 0.8560(4) 0.0365(17) Uani 1 1 d . . . . .
O3 O 0.8048(6) 0.5619(5) 0.6039(4) 0.0334(15) Uani 1 1 d . . . . .
O4 O 0.6821(6) 0.3867(5) 0.5369(4) 0.0340(16) Uani 1 1 d . . . . .
O5 O 0.6015(6) 0.1089(5) 0.5557(5) 0.0371(17) Uani 1 1 d . . . . .
O6 O 0.6459(6) 0.0122(5) 0.6434(5) 0.0385(17) Uani 1 1 d . . . . .
O7 O 0.7539(6) 0.1582(5) 0.8975(4) 0.0370(17) Uani 1 1 d . . . . .
O8 O 0.7912(6) 0.3419(5) 0.9692(4) 0.0348(16) Uani 1 1 d . . . . .
C1 C 0.9228(8) 0.3617(6) 0.8970(6) 0.0285(19) Uani 1 1 d . . . . .
C2 C 0.8498(8) 0.3939(6) 0.9395(6) 0.030(2) Uani 1 1 d . . . . .
C3 C 0.8373(8) 0.4808(7) 0.9569(6) 0.033(2) Uani 1 1 d . . . . .
C4 C 0.8988(8) 0.5322(6) 0.9299(6) 0.032(2) Uani 1 1 d . . . . .
C5 C 0.9733(8) 0.5019(6) 0.8859(5) 0.029(2) Uani 1 1 d . . . . .
C6 C 0.9829(8) 0.4175(6) 0.8704(6) 0.031(2) Uani 1 1 d . . . . .
H6 H 1.0323 0.3955 0.8402 0.037 Uiso 1 1 calc R . . . .
C7 C 0.7592(8) 0.5122(7) 1.0003(6) 0.034(2) Uani 1 1 d . . . . .
C8 C 0.6927(10) 0.5388(8) 1.0347(8) 0.049(3) Uani 1 1 d . . . . .
C9 C 1.0378(7) 0.5637(6) 0.8591(5) 0.0265(18) Uani 1 1 d . . . . .
H9 H 1.0460 0.6233 0.8965 0.032 Uiso 1 1 calc R . . . .
C10 C 1.1496(8) 0.5493(7) 0.8499(6) 0.033(2) Uani 1 1 d . . . . .
H10A H 1.1451 0.4938 0.8092 0.040 Uiso 1 1 calc R . . . .
H10B H 1.1838 0.5441 0.8934 0.040 Uiso 1 1 calc R . . . .
C11 C 1.2193(8) 0.6224(7) 0.8367(8) 0.043(3) Uani 1 1 d . . . . .
H11A H 1.2002 0.6147 0.7862 0.051 Uiso 1 1 calc R . . . .
H11B H 1.2038 0.6786 0.8670 0.051 Uiso 1 1 calc R . . . .
C12 C 1.3380(10) 0.6259(8) 0.8525(9) 0.055(4) Uani 1 1 d . . . . .
H12A H 1.3567 0.6307 0.9023 0.066 Uiso 1 1 calc R . . . .
H12B H 1.3545 0.5712 0.8203 0.066 Uiso 1 1 calc R . . . .
C13 C 1.4051(12) 0.7020(9) 0.8426(10) 0.063(4) Uani 1 1 d . . . . .
H13A H 1.3794 0.7551 0.8688 0.075 Uiso 1 1 calc R . . . .
H13B H 1.3929 0.6921 0.7912 0.075 Uiso 1 1 calc R . . . .
C14 C 1.5244(11) 0.7187(10) 0.8673(11) 0.073(5) Uani 1 1 d . . . . .
H14A H 1.5605 0.7655 0.8536 0.088 Uiso 1 1 calc R . . . .
H14B H 1.5504 0.6655 0.8419 0.088 Uiso 1 1 calc R . . . .
C15 C 1.5567(14) 0.7450(13) 0.9488(13) 0.091(7) Uani 1 1 d . . . . .
H15A H 1.6346 0.7623 0.9615 0.136 Uiso 1 1 calc GR . . . .
H15B H 1.5310 0.6956 0.9617 0.136 Uiso 1 1 calc GR . . . .
H15C H 1.5249 0.7939 0.9746 0.136 Uiso 1 1 calc GR . . . .
C16 C 0.8072(9) 0.6338(7) 0.9089(7) 0.038(2) Uani 1 1 d . . . . .
H16A H 0.7464 0.6429 0.9352 0.045 Uiso 1 1 calc R . . . .
H16B H 0.7822 0.5826 0.8636 0.045 Uiso 1 1 calc R . . . .
C17 C 0.8482(10) 0.7131(7) 0.8935(7) 0.041(3) Uani 1 1 d . . . . .
H17A H 0.7899 0.7237 0.8645 0.049 Uiso 1 1 calc R . . . .
H17B H 0.8696 0.7643 0.9392 0.049 Uiso 1 1 calc R . . . .
C18 C 0.9752(8) 0.5633(6) 0.7918(5) 0.0277(19) Uani 1 1 d . . . . .
C19 C 0.9237(8) 0.6317(6) 0.7936(6) 0.0284(19) Uani 1 1 d . . . . .
C20 C 0.8637(8) 0.6301(6) 0.7308(6) 0.030(2) Uani 1 1 d . . . . .
C21 C 0.8569(7) 0.5598(6) 0.6657(5) 0.0262(18) Uani 1 1 d . . . . .
C22 C 0.9056(7) 0.4907(6) 0.6625(6) 0.028(2) Uani 1 1 d . . . . .
C23 C 0.9640(8) 0.4937(6) 0.7260(6) 0.030(2) Uani 1 1 d . . . . .
H23 H 0.9969 0.4467 0.7241 0.036 Uiso 1 1 calc R . . . .
C24 C 0.8169(9) 0.7020(7) 0.7340(6) 0.037(2) Uani 1 1 d . . . . .
C25 C 0.7788(10) 0.7632(7) 0.7401(7) 0.042(3) Uani 1 1 d . . . . .
C26 C 0.9017(7) 0.4168(6) 0.5904(5) 0.0241(18) Uani 1 1 d . . . . .
H26 H 0.8719 0.4356 0.5526 0.029 Uiso 1 1 calc R . . . .
C27 C 1.0126(7) 0.4013(6) 0.5761(6) 0.031(2) Uani 1 1 d . . . . .
H27A H 1.0581 0.4571 0.5811 0.038 Uiso 1 1 calc R . . . .
H27B H 1.0443 0.3833 0.6133 0.038 Uiso 1 1 calc R . . . .
C28 C 1.0163(8) 0.3342(6) 0.5040(6) 0.031(2) Uani 1 1 d . . . . .
H28A H 0.9879 0.2759 0.5037 0.037 Uiso 1 1 calc R . . . .
H28B H 1.0918 0.3369 0.4972 0.037 Uiso 1 1 calc R . . . .
C29 C 0.9543(8) 0.3438(6) 0.4411(6) 0.033(2) Uani 1 1 d . . . . .
H29A H 0.9810 0.4024 0.4416 0.039 Uiso 1 1 calc R . . . .
H29B H 0.8781 0.3388 0.4465 0.039 Uiso 1 1 calc R . . . .
C30 C 0.9634(9) 0.2755(7) 0.3691(6) 0.037(2) Uani 1 1 d . . . . .
H30A H 1.0382 0.2856 0.3610 0.044 Uiso 1 1 calc R . . . .
H30B H 0.9461 0.2172 0.3712 0.044 Uiso 1 1 calc R . . . .
C31 C 0.8908(10) 0.2765(8) 0.3066(6) 0.041(2) Uani 1 1 d . . . . .
H31A H 0.9127 0.3326 0.3013 0.049 Uiso 1 1 calc R . . . .
H31B H 0.8167 0.2720 0.3166 0.049 Uiso 1 1 calc R . . . .
C32 C 0.8938(11) 0.2027(8) 0.2372(7) 0.051(3) Uani 1 1 d . . . . .
H32A H 0.8460 0.2060 0.1983 0.076 Uiso 1 1 calc GR . . . .
H32B H 0.8705 0.1470 0.2419 0.076 Uiso 1 1 calc GR . . . .
H32C H 0.9668 0.2075 0.2267 0.076 Uiso 1 1 calc GR . . . .
C33 C 0.6894(8) 0.5408(7) 0.5949(6) 0.034(2) Uani 1 1 d . . . . .
H33A H 0.6594 0.5447 0.5498 0.041 Uiso 1 1 calc R . . . .
H33B H 0.6655 0.5845 0.6347 0.041 Uiso 1 1 calc R . . . .
C34 C 0.6458(9) 0.4520(7) 0.5931(7) 0.039(2) Uani 1 1 d . . . . .
H34A H 0.6698 0.4493 0.6398 0.047 Uiso 1 1 calc R . . . .
H34B H 0.5669 0.4405 0.5848 0.047 Uiso 1 1 calc R . . . .
C35 C 0.8226(7) 0.3346(6) 0.5850(5) 0.0255(18) Uani 1 1 d . . . . .
C36 C 0.7150(8) 0.3239(7) 0.5584(7) 0.036(2) Uani 1 1 d . . . . .
C37 C 0.6408(7) 0.2498(6) 0.5499(6) 0.031(2) Uani 1 1 d . . . . .
C38 C 0.6745(8) 0.1850(6) 0.5685(7) 0.034(2) Uani 1 1 d . . . . .
C39 C 0.7826(7) 0.1936(6) 0.5954(5) 0.0258(18) Uani 1 1 d . . . . .
C40 C 0.8531(8) 0.2687(6) 0.6030(5) 0.0274(19) Uani 1 1 d . . . . .
H40 H 0.9260 0.2755 0.6214 0.033 Uiso 1 1 calc R . . . .
C41 C 0.5282(8) 0.2408(7) 0.5231(6) 0.037(2) Uani 1 1 d . . . . .
C42 C 0.4424(11) 0.2364(9) 0.5037(8) 0.054(3) Uani 1 1 d . . . . .
C43 C 0.8155(7) 0.1215(6) 0.6136(6) 0.028(2) Uani 1 1 d . . . . .
H43 H 0.7671 0.0661 0.5801 0.034 Uiso 1 1 calc R . . . .
C44 C 0.9285(8) 0.1124(6) 0.6028(6) 0.031(2) Uani 1 1 d . . . . .
H44A H 0.9782 0.1656 0.6371 0.037 Uiso 1 1 calc R . . . .
H44B H 0.9368 0.1094 0.5541 0.037 Uiso 1 1 calc R . . . .
C45 C 0.9621(8) 0.0333(6) 0.6118(6) 0.036(2) Uani 1 1 d . . . . .
H45A H 0.9524 0.0349 0.6600 0.043 Uiso 1 1 calc R . . . .
H45B H 0.9148 -0.0203 0.5762 0.043 Uiso 1 1 calc R . . . .
C46 C 1.0762(9) 0.0300(7) 0.6028(7) 0.040(3) Uani 1 1 d . . . . .
H46A H 1.1228 0.0837 0.6387 0.048 Uiso 1 1 calc R . . . .
H46B H 1.0855 0.0298 0.5550 0.048 Uiso 1 1 calc R . . . .
C47 C 1.1137(9) -0.0478(7) 0.6101(7) 0.040(3) Uani 1 1 d . . . . .
H47A H 1.1051 -0.0479 0.6579 0.049 Uiso 1 1 calc R . . . .
H47B H 1.0678 -0.1018 0.5740 0.049 Uiso 1 1 calc R . . . .
C48 C 1.2288(9) -0.0481(7) 0.6006(8) 0.047(3) Uani 1 1 d . . . . .
H48A H 1.2742 0.0075 0.6347 0.056 Uiso 1 1 calc R . . . .
H48B H 1.2364 -0.0516 0.5517 0.056 Uiso 1 1 calc R . . . .
C49 C 1.2692(10) -0.1225(8) 0.6121(8) 0.047(3) Uani 1 1 d . . . . .
H49A H 1.2272 -0.1779 0.5769 0.071 Uiso 1 1 calc GR . . . .
H49B H 1.2619 -0.1197 0.6604 0.071 Uiso 1 1 calc GR . . . .
H49C H 1.3444 -0.1180 0.6064 0.071 Uiso 1 1 calc GR . . . .
C50 C 0.5432(9) 0.1086(7) 0.6120(7) 0.041(3) Uani 1 1 d . . . . .
H50A H 0.4696 0.1151 0.5998 0.049 Uiso 1 1 calc R . . . .
H50B H 0.5778 0.1582 0.6567 0.049 Uiso 1 1 calc R . . . .
C51 C 0.5399(8) 0.0240(7) 0.6230(7) 0.040(2) Uani 1 1 d . . . . .
H51A H 0.4967 0.0234 0.6607 0.048 Uiso 1 1 calc R . . . .
H51B H 0.5045 -0.0252 0.5782 0.048 Uiso 1 1 calc R . . . .
C52 C 0.7975(8) 0.1315(6) 0.6891(6) 0.030(2) Uani 1 1 d . . . . .
C53 C 0.7108(8) 0.0783(6) 0.7006(6) 0.031(2) Uani 1 1 d . . . . .
C54 C 0.6933(8) 0.0899(6) 0.7702(6) 0.033(2) Uani 1 1 d . . . . .
C55 C 0.7656(9) 0.1512(6) 0.8289(6) 0.032(2) Uani 1 1 d . . . . .
C56 C 0.8540(8) 0.2045(6) 0.8184(6) 0.030(2) Uani 1 1 d . . . . .
C57 C 0.8662(8) 0.1929(6) 0.7487(6) 0.031(2) Uani 1 1 d . . . . .
H57 H 0.9249 0.2291 0.7414 0.038 Uiso 1 1 calc R . . . .
C58 C 0.6099(8) 0.0349(7) 0.7842(7) 0.039(3) Uani 1 1 d . . . . .
C59A C 0.5400(11) -0.0083(8) 0.8029(8) 0.053(3) Uani 1 1 d . . . . .
C60 C 0.9371(9) 0.2689(6) 0.8820(6) 0.035(2) Uani 1 1 d . . . . .
H60 H 0.9211 0.2559 0.9246 0.042 Uiso 1 1 calc R . . . .
C61 C 1.0509(8) 0.2557(7) 0.8727(7) 0.037(2) Uani 1 1 d . . . . .
H61A H 1.1029 0.3032 0.9112 0.045 Uiso 1 1 calc R . . . .
H61B H 1.0658 0.2572 0.8263 0.045 Uiso 1 1 calc R . . . .
C62 C 1.0626(10) 0.1675(8) 0.8756(9) 0.054(3) Uani 1 1 d . . . . .
H62A H 1.0242 0.1200 0.8307 0.065 Uiso 1 1 calc R . . . .
H62B H 1.0300 0.1600 0.9157 0.065 Uiso 1 1 calc R . . . .
C63 C 1.1833(17) 0.1620(15) 0.8858(14) 0.094(6) Uani 1 1 d . U . . .
H63A H 1.2220 0.2126 0.9286 0.113 Uiso 1 1 calc R . . . .
H63B H 1.1884 0.1089 0.8949 0.113 Uiso 1 1 calc R . . . .
C64 C 1.2344(19) 0.1604(15) 0.8267(14) 0.099(7) Uani 1 1 d . . . . .
H64A H 1.2297 0.2129 0.8164 0.119 Uiso 1 1 calc R . . . .
H64B H 1.1991 0.1085 0.7837 0.119 Uiso 1 1 calc R . . . .
C65 C 1.3534(18) 0.1576(16) 0.8455(15) 0.109(8) Uani 1 1 d . U . . .
H65A H 1.3892 0.2108 0.8870 0.131 Uiso 1 1 calc R . . . .
H65B H 1.3577 0.1068 0.8583 0.131 Uiso 1 1 calc R . . . .
C66 C 1.408(2) 0.1512(18) 0.7831(15) 0.129(12) Uani 1 1 d . . . . .
H66A H 1.3583 0.1151 0.7389 0.193 Uiso 1 1 calc GR . . . .
H66B H 1.4699 0.1249 0.7860 0.193 Uiso 1 1 calc GR . . . .
H66C H 1.4317 0.2095 0.7833 0.193 Uiso 1 1 calc GR . . . .
C67 C 0.6751(9) 0.2023(7) 0.9286(7) 0.042(3) Uani 1 1 d . . . . .
H67A H 0.6778 0.2057 0.9783 0.050 Uiso 1 1 calc R . . . .
H67B H 0.6037 0.1686 0.9016 0.050 Uiso 1 1 calc R . . . .
C68 C 0.6902(8) 0.2933(6) 0.9287(6) 0.034(2) Uani 1 1 d . . . . .
H68A H 0.6863 0.2907 0.8791 0.040 Uiso 1 1 calc R . . . .
H68B H 0.6330 0.3216 0.9500 0.040 Uiso 1 1 calc R . . . .
S3A S 0.4210(3) 0.6278(3) 1.2605(2) 0.0467(13) Uani 0.755(11) 1 d . . P B 1
S3B S 0.3766(12) 0.5829(9) 1.1947(10) 0.064(5) Uani 0.245(11) 1 d . . P B 2
O11 O 0.4729(9) 0.6635(8) 1.2109(8) 0.079(4) Uani 1 1 d . . . . .
C73 C 0.4187(13) 0.5165(11) 1.2215(10) 0.068(4) Uani 1 1 d . . . . .
H73A H 0.3857 0.4872 1.2505 0.103 Uiso 0.755(11) 1 calc R . P B 1
H73B H 0.3771 0.4924 1.1732 0.103 Uiso 0.755(11) 1 calc R . P B 1
H73C H 0.4918 0.5076 1.2190 0.103 Uiso 0.755(11) 1 calc R . P B 1
H73D H 0.3605 0.4665 1.2120 0.103 Uiso 0.245(11) 1 calc R . P B 2
H73E H 0.4769 0.4969 1.1964 0.103 Uiso 0.245(11) 1 calc R . P B 2
H73F H 0.4450 0.5444 1.2730 0.103 Uiso 0.245(11) 1 calc R . P B 2
C74 C 0.2847(11) 0.6256(9) 1.2424(7) 0.050(3) Uani 1 1 d . . . . .
H74A H 0.2466 0.6028 1.2734 0.075 Uiso 0.755(11) 1 calc R . P B 1
H74B H 0.2744 0.6847 1.2513 0.075 Uiso 0.755(11) 1 calc R . P B 1
H74C H 0.2568 0.5882 1.1923 0.075 Uiso 0.755(11) 1 calc R . P B 1
H74D H 0.2594 0.6671 1.2246 0.075 Uiso 0.245(11) 1 calc R . P B 2
H74E H 0.2244 0.5790 1.2373 0.075 Uiso 0.245(11) 1 calc R . P B 2
H74F H 0.3169 0.6556 1.2928 0.075 Uiso 0.245(11) 1 calc R . P B 2
O12 O 0.1078(9) 0.3080(8) 0.7077(7) 0.073(3) Uani 1 1 d . . . . .
S4A S 0.1913(5) 0.3037(4) 0.6591(4) 0.060(2) Uani 0.579(13) 1 d . . P C 1
S4B S 0.2155(9) 0.3324(7) 0.7255(7) 0.073(4) Uani 0.421(13) 1 d . . P C 2
C75 C 0.2747(14) 0.4060(12) 0.6890(12) 0.082(6) Uani 1 1 d . . . . .
H75A H 0.3295 0.4050 0.6585 0.124 Uiso 0.5 1 calc R . P C 1
H75B H 0.2327 0.4488 0.6871 0.124 Uiso 0.5 1 calc R . P C 1
H75C H 0.3091 0.4219 0.7384 0.124 Uiso 0.5 1 calc R . P C 1
H75D H 0.3523 0.4206 0.7042 0.124 Uiso 0.5 1 calc R . P C 2
H75E H 0.2583 0.3791 0.6368 0.124 Uiso 0.5 1 calc R . P C 2
H75F H 0.2464 0.4591 0.7059 0.124 Uiso 0.5 1 calc R . P C 2
C76 C 0.2865(19) 0.2490(14) 0.6737(15) 0.109(8) Uani 1 1 d . U . . .
H76A H 0.3379 0.2484 0.6409 0.163 Uiso 0.579(13) 1 calc R . P C 1
H76B H 0.3238 0.2782 0.7231 0.163 Uiso 0.579(13) 1 calc R . P C 1
H76C H 0.2524 0.1892 0.6653 0.163 Uiso 0.579(13) 1 calc R . P C 1
H76D H 0.3637 0.2706 0.6891 0.163 Uiso 0.421(13) 1 calc R . P C 2
H76E H 0.2647 0.1954 0.6820 0.163 Uiso 0.421(13) 1 calc R . P C 2
H76F H 0.2686 0.2370 0.6227 0.163 Uiso 0.421(13) 1 calc R . P C 2
S2 S 0.4204(3) 0.5757(3) 0.6060(2) 0.0577(9) Uani 1 1 d . . . . .
O10 O 0.4606(9) 0.5526(8) 0.6669(6) 0.068(3) Uani 1 1 d . . . . .
C71 C 0.2784(11) 0.5470(10) 0.5938(9) 0.061(4) Uani 1 1 d . . . . .
H71A H 0.2549 0.5657 0.6404 0.091 Uiso 1 1 calc GR . . . .
H71B H 0.2548 0.4838 0.5692 0.091 Uiso 1 1 calc GR . . . .
H71C H 0.2475 0.5757 0.5650 0.091 Uiso 1 1 calc GR . . . .
C72 C 0.4315(16) 0.6904(10) 0.6407(9) 0.075(5) Uani 1 1 d . . . . .
H72A H 0.5070 0.7194 0.6510 0.112 Uiso 1 1 calc GR . . . .
H72B H 0.4007 0.7080 0.6847 0.112 Uiso 1 1 calc GR . . . .
H72C H 0.3931 0.7068 0.6054 0.112 Uiso 1 1 calc GR . . . .
S1 S 0.2158(4) -0.0591(2) 0.9487(2) 0.0649(10) Uani 1 1 d . . . . .
O9 O 0.2947(9) -0.1175(7) 0.9286(7) 0.070(3) Uani 1 1 d . . . . .
C69 C 0.1069(13) -0.1188(12) 0.9712(9) 0.072(5) Uani 1 1 d . . . . .
H69A H 0.1328 -0.1334 1.0113 0.107 Uiso 1 1 calc GR . . . .
H69B H 0.0749 -0.1724 0.9299 0.107 Uiso 1 1 calc GR . . . .
H69C H 0.0532 -0.0834 0.9848 0.107 Uiso 1 1 calc GR . . . .
C70 C 0.268(2) 0.0206(12) 1.0345(11) 0.106(8) Uani 1 1 d . . . . .
H70A H 0.2969 -0.0067 1.0651 0.159 Uiso 1 1 calc GR . . . .
H70B H 0.2108 0.0484 1.0551 0.159 Uiso 1 1 calc GR . . . .
H70C H 0.3246 0.0644 1.0310 0.159 Uiso 1 1 calc GR . . . .


_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
I1 C8 2.007(15) . ?
I2 C25 2.010(10) . ?
I3 C42 2.054(15) . ?
I4A C59A 2.001(15) . ?
I4B C59A 2.019(16) . ?
O1 C4 1.394(12) . ?
O1 C16 1.429(14) . ?
O2 C17 1.442(13) . ?
O2 C19 1.380(12) . ?
O3 C21 1.383(12) . ?
O3 C33 1.450(12) . ?
O4 C34 1.448(12) . ?
O4 C36 1.392(13) . ?
O5 C38 1.387(12) . ?
O5 C50 1.427(14) . ?
O6 C51 1.455(13) . ?
O6 C53 1.370(13) . ?
O7 C55 1.382(13) . ?
O7 C67 1.416(12) . ?
O8 C2 1.400(12) . ?
O8 C68 1.418(13) . ?
C1 C2 1.378(13) . ?
C1 C6 1.410(14) . ?
C1 C60 1.531(13) . ?
C2 C3 1.420(14) . ?
C3 C4 1.373(16) . ?
C3 C7 1.438(13) . ?
C4 C5 1.403(14) . ?
C5 C6 1.373(14) . ?
C5 C9 1.512(13) . ?
C7 C8 1.197(18) . ?
C9 C10 1.515(12) . ?
C9 C18 1.521(13) . ?
C10 C11 1.524(15) . ?
C11 C12 1.518(16) . ?
C12 C13 1.514(16) . ?
C13 C14 1.52(2) . ?
C14 C15 1.55(3) . ?
C16 C17 1.508(15) . ?
C18 C19 1.412(13) . ?
C18 C23 1.402(14) . ?
C19 C20 1.419(15) . ?
C20 C21 1.408(13) . ?
C20 C24 1.425(14) . ?
C21 C22 1.396(13) . ?
C22 C23 1.412(15) . ?
C22 C26 1.534(13) . ?
C24 C25 1.185(16) . ?
C26 C27 1.529(11) . ?
C26 C35 1.543(12) . ?
C27 C28 1.506(14) . ?
C28 C29 1.517(15) . ?
C29 C30 1.531(15) . ?
C30 C31 1.514(15) . ?
C31 C32 1.516(16) . ?
C33 C34 1.499(15) . ?
C35 C36 1.398(13) . ?
C35 C40 1.392(14) . ?
C36 C37 1.390(14) . ?
C37 C38 1.397(15) . ?
C37 C41 1.465(13) . ?
C38 C39 1.411(13) . ?
C39 C40 1.383(13) . ?
C39 C43 1.503(13) . ?
C41 C42 1.119(18) . ?
C43 C44 1.516(12) . ?
C43 C52 1.527(15) . ?
C44 C45 1.534(13) . ?
C45 C46 1.505(14) . ?
C46 C47 1.522(15) . ?
C47 C48 1.512(14) . ?
C48 C49 1.517(16) . ?
C50 C51 1.518(16) . ?
C52 C53 1.408(14) . ?
C52 C57 1.387(15) . ?
C53 C54 1.402(15) . ?
C54 C55 1.398(16) . ?
C54 C58 1.422(14) . ?
C55 C56 1.415(14) . ?
C56 C57 1.388(15) . ?
C56 C60 1.533(15) . ?
C58 C59A 1.239(19) . ?
C60 C61 1.534(14) . ?
C61 C62 1.541(15) . ?
C62 C63 1.57(2) . ?
C63 C64 1.42(3) . ?
C64 C65 1.56(3) . ?
C65 C66 1.48(4) . ?
C67 C68 1.515(14) . ?
S3A O11 1.503(14) . ?
S3A C73 1.749(15) . ?
S3A C74 1.751(14) . ?
S3B O11 1.596(18) . ?
S3B C73 1.56(2) . ?
S3B C74 1.687(19) . ?
O12 S4A 1.519(13) . ?
O12 S4B 1.355(15) . ?
S4A C75 1.739(18) . ?
S4A C76 1.71(2) . ?
S4B C75 1.77(2) . ?
S4B C76 1.86(2) . ?
S2 O10 1.501(11) . ?
S2 C71 1.783(14) . ?
S2 C72 1.780(17) . ?
S1 O9 1.511(12) . ?
S1 C69 1.785(15) . ?
S1 C70 1.760(18) . ?

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
C4 O1 C16 114.0(8) . . ?
C19 O2 C17 116.3(8) . . ?
C21 O3 C33 114.7(8) . . ?
C36 O4 C34 113.0(9) . . ?
C38 O5 C50 116.0(8) . . ?
C53 O6 C51 117.4(8) . . ?
C55 O7 C67 117.2(9) . . ?
C2 O8 C68 115.4(9) . . ?
C2 C1 C6 117.8(9) . . ?
C2 C1 C60 119.4(9) . . ?
C6 C1 C60 122.8(9) . . ?
O8 C2 C3 119.2(9) . . ?
C1 C2 O8 119.7(9) . . ?
C1 C2 C3 121.0(9) . . ?
C2 C3 C7 119.8(10) . . ?
C4 C3 C2 118.5(9) . . ?
C4 C3 C7 121.6(10) . . ?
O1 C4 C5 118.9(9) . . ?
C3 C4 O1 118.5(9) . . ?
C3 C4 C5 122.4(9) . . ?
C4 C5 C9 118.5(9) . . ?
C6 C5 C4 117.2(10) . . ?
C6 C5 C9 124.4(9) . . ?
C5 C6 C1 123.1(9) . . ?
C8 C7 C3 178.0(13) . . ?
C7 C8 I1 175.4(11) . . ?
C5 C9 C10 114.3(8) . . ?
C5 C9 C18 110.1(8) . . ?
C10 C9 C18 112.5(8) . . ?
C9 C10 C11 112.9(9) . . ?
C12 C11 C10 113.4(10) . . ?
C13 C12 C11 112.1(11) . . ?
C12 C13 C14 116.0(14) . . ?
C13 C14 C15 114.2(14) . . ?
O1 C16 C17 108.7(9) . . ?
O2 C17 C16 112.5(8) . . ?
C19 C18 C9 121.3(9) . . ?
C23 C18 C9 121.1(9) . . ?
C23 C18 C19 117.6(9) . . ?
O2 C19 C18 119.7(9) . . ?
O2 C19 C20 119.1(8) . . ?
C18 C19 C20 121.0(9) . . ?
C19 C20 C24 119.5(9) . . ?
C21 C20 C19 119.4(9) . . ?
C21 C20 C24 121.1(10) . . ?
O3 C21 C20 118.9(8) . . ?
O3 C21 C22 120.2(9) . . ?
C22 C21 C20 120.8(9) . . ?
C21 C22 C23 118.5(9) . . ?
C21 C22 C26 120.0(9) . . ?
C23 C22 C26 121.4(8) . . ?
C18 C23 C22 122.7(9) . . ?
C25 C24 C20 176.8(13) . . ?
C24 C25 I2 175.9(12) . . ?
C22 C26 C35 109.8(8) . . ?
C27 C26 C22 112.3(8) . . ?
C27 C26 C35 113.7(7) . . ?
C28 C27 C26 115.6(8) . . ?
C27 C28 C29 115.0(8) . . ?
C28 C29 C30 112.8(8) . . ?
C31 C30 C29 113.5(9) . . ?
C30 C31 C32 112.2(10) . . ?
O3 C33 C34 113.4(8) . . ?
O4 C34 C33 110.4(10) . . ?
C36 C35 C26 118.7(9) . . ?
C40 C35 C26 123.6(8) . . ?
C40 C35 C36 117.7(9) . . ?
O4 C36 C35 119.5(9) . . ?
C37 C36 O4 119.2(9) . . ?
C37 C36 C35 121.2(9) . . ?
C36 C37 C38 119.3(9) . . ?
C36 C37 C41 120.2(9) . . ?
C38 C37 C41 120.5(9) . . ?
O5 C38 C37 119.0(9) . . ?
O5 C38 C39 119.9(9) . . ?
C37 C38 C39 121.0(9) . . ?
C38 C39 C43 119.1(9) . . ?
C40 C39 C38 117.4(9) . . ?
C40 C39 C43 123.5(9) . . ?
C39 C40 C35 123.3(9) . . ?
C42 C41 C37 178.0(14) . . ?
C41 C42 I3 175.2(13) . . ?
C39 C43 C44 113.3(8) . . ?
C39 C43 C52 110.7(8) . . ?
C44 C43 C52 111.8(9) . . ?
C43 C44 C45 115.6(8) . . ?
C46 C45 C44 112.8(9) . . ?
C45 C46 C47 115.2(9) . . ?
C48 C47 C46 113.2(10) . . ?
C47 C48 C49 113.7(11) . . ?
O5 C50 C51 109.8(9) . . ?
O6 C51 C50 112.2(9) . . ?
C53 C52 C43 121.1(9) . . ?
C57 C52 C43 121.3(9) . . ?
C57 C52 C53 117.6(10) . . ?
O6 C53 C52 119.6(10) . . ?
O6 C53 C54 119.7(9) . . ?
C54 C53 C52 120.6(10) . . ?
C53 C54 C58 122.4(11) . . ?
C55 C54 C53 120.1(10) . . ?
C55 C54 C58 117.2(10) . . ?
O7 C55 C54 120.5(9) . . ?
O7 C55 C56 119.4(10) . . ?
C54 C55 C56 120.1(10) . . ?
C55 C56 C60 120.8(10) . . ?
C57 C56 C55 117.9(10) . . ?
C57 C56 C60 121.2(10) . . ?
C52 C57 C56 123.7(10) . . ?
C59A C58 C54 174.3(15) . . ?
C58 C59A I4A 172.0(13) . . ?
C58 C59A I4B 158.4(14) . . ?
C1 C60 C56 110.0(9) . . ?
C1 C60 C61 114.4(9) . . ?
C56 C60 C61 112.1(9) . . ?
C60 C61 C62 109.7(10) . . ?
C61 C62 C63 111.0(12) . . ?
C64 C63 C62 114.2(19) . . ?
C63 C64 C65 108(2) . . ?
C66 C65 C64 110(2) . . ?
O7 C67 C68 112.4(9) . . ?
O8 C68 C67 108.8(9) . . ?
O11 S3A C73 103.4(8) . . ?
O11 S3A C74 105.9(7) . . ?
C73 S3A C74 99.6(7) . . ?
O11 S3B C74 104.8(10) . . ?
C73 S3B O11 108.3(13) . . ?
C73 S3B C74 110.8(14) . . ?
O12 S4A C75 107.8(9) . . ?
O12 S4A C76 113.2(12) . . ?
C76 S4A C75 96.9(11) . . ?
O12 S4B C75 114.3(11) . . ?
O12 S4B C76 113.5(12) . . ?
C75 S4B C76 90.8(12) . . ?
O10 S2 C71 105.9(7) . . ?
O10 S2 C72 106.9(8) . . ?
C72 S2 C71 96.7(8) . . ?
O9 S1 C69 106.3(8) . . ?
O9 S1 C70 107.4(10) . . ?
C70 S1 C69 98.6(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C4 C5 C6 175.7(9) . . . . ?
O1 C4 C5 C9 -4.0(15) . . . . ?
O1 C16 C17 O2 58.8(13) . . . . ?
O2 C19 C20 C21 174.3(9) . . . . ?
O2 C19 C20 C24 -1.8(14) . . . . ?
O3 C21 C22 C23 175.8(9) . . . . ?
O3 C21 C22 C26 0.1(13) . . . . ?
O3 C33 C34 O4 -56.8(12) . . . . ?
O4 C36 C37 C38 177.3(10) . . . . ?
O4 C36 C37 C41 -3.9(17) . . . . ?
O5 C38 C39 C40 176.1(9) . . . . ?
O5 C38 C39 C43 -3.4(15) . . . . ?
O5 C50 C51 O6 61.2(13) . . . . ?
O6 C53 C54 C55 173.3(9) . . . . ?
O6 C53 C54 C58 0.2(15) . . . . ?
O7 C55 C56 C57 176.9(8) . . . . ?
O7 C55 C56 C60 0.6(14) . . . . ?
O7 C67 C68 O8 -60.6(13) . . . . ?
O8 C2 C3 C4 177.2(10) . . . . ?
O8 C2 C3 C7 -4.7(16) . . . . ?
C1 C2 C3 C4 0.8(17) . . . . ?
C1 C2 C3 C7 178.9(10) . . . . ?
C1 C60 C61 C62 166.8(11) . . . . ?
C2 O8 C68 C67 137.1(9) . . . . ?
C2 C1 C6 C5 1.3(17) . . . . ?
C2 C1 C60 C56 85.1(12) . . . . ?
C2 C1 C60 C61 -147.8(11) . . . . ?
C2 C3 C4 O1 -175.7(10) . . . . ?
C2 C3 C4 C5 -0.1(16) . . . . ?
C3 C4 C5 C6 0.1(16) . . . . ?
C3 C4 C5 C9 -179.6(10) . . . . ?
C4 O1 C16 C17 -137.5(9) . . . . ?
C4 C5 C6 C1 -0.7(16) . . . . ?
C4 C5 C9 C10 147.3(10) . . . . ?
C4 C5 C9 C18 -84.9(11) . . . . ?
C5 C9 C10 C11 -169.1(10) . . . . ?
C5 C9 C18 C19 103.0(10) . . . . ?
C5 C9 C18 C23 -75.0(11) . . . . ?
C6 C1 C2 O8 -177.7(9) . . . . ?
C6 C1 C2 C3 -1.3(16) . . . . ?
C6 C1 C60 C56 -96.2(12) . . . . ?
C6 C1 C60 C61 31.0(15) . . . . ?
C6 C5 C9 C10 -32.4(14) . . . . ?
C6 C5 C9 C18 95.4(11) . . . . ?
C7 C3 C4 O1 6.2(16) . . . . ?
C7 C3 C4 C5 -178.2(10) . . . . ?
C9 C5 C6 C1 179.0(10) . . . . ?
C9 C10 C11 C12 160.3(11) . . . . ?
C9 C18 C19 O2 6.0(14) . . . . ?
C9 C18 C19 C20 -178.7(9) . . . . ?
C9 C18 C23 C22 179.3(9) . . . . ?
C10 C9 C18 C19 -128.2(10) . . . . ?
C10 C9 C18 C23 53.7(13) . . . . ?
C10 C11 C12 C13 -177.0(12) . . . . ?
C11 C12 C13 C14 171.5(14) . . . . ?
C12 C13 C14 C15 -64(2) . . . . ?
C16 O1 C4 C3 -85.9(12) . . . . ?
C16 O1 C4 C5 98.3(11) . . . . ?
C17 O2 C19 C18 -107.8(11) . . . . ?
C17 O2 C19 C20 76.9(12) . . . . ?
C18 C9 C10 C11 64.4(12) . . . . ?
C18 C19 C20 C21 -1.0(15) . . . . ?
C18 C19 C20 C24 -177.1(10) . . . . ?
C19 O2 C17 C16 53.9(14) . . . . ?
C19 C18 C23 C22 1.2(15) . . . . ?
C19 C20 C21 O3 -175.3(9) . . . . ?
C19 C20 C21 C22 2.0(15) . . . . ?
C20 C21 C22 C23 -1.4(14) . . . . ?
C20 C21 C22 C26 -177.1(9) . . . . ?
C21 O3 C33 C34 -59.2(12) . . . . ?
C21 C22 C23 C18 -0.2(15) . . . . ?
C21 C22 C26 C27 126.1(9) . . . . ?
C21 C22 C26 C35 -106.3(10) . . . . ?
C22 C26 C27 C28 -175.7(8) . . . . ?
C22 C26 C35 C36 87.7(11) . . . . ?
C22 C26 C35 C40 -94.5(11) . . . . ?
C23 C18 C19 O2 -175.9(9) . . . . ?
C23 C18 C19 C20 -0.6(14) . . . . ?
C23 C22 C26 C27 -49.6(12) . . . . ?
C23 C22 C26 C35 78.1(11) . . . . ?
C24 C20 C21 O3 0.8(15) . . . . ?
C24 C20 C21 C22 178.1(9) . . . . ?
C26 C22 C23 C18 175.4(9) . . . . ?
C26 C27 C28 C29 48.3(12) . . . . ?
C26 C35 C36 O4 0.6(15) . . . . ?
C26 C35 C36 C37 177.7(10) . . . . ?
C26 C35 C40 C39 -177.4(9) . . . . ?
C27 C26 C35 C36 -145.4(10) . . . . ?
C27 C26 C35 C40 32.4(14) . . . . ?
C27 C28 C29 C30 178.3(9) . . . . ?
C28 C29 C30 C31 172.4(9) . . . . ?
C29 C30 C31 C32 -174.4(10) . . . . ?
C33 O3 C21 C20 -77.9(11) . . . . ?
C33 O3 C21 C22 104.8(10) . . . . ?
C34 O4 C36 C35 -93.1(12) . . . . ?
C34 O4 C36 C37 89.7(12) . . . . ?
C35 C26 C27 C28 58.7(12) . . . . ?
C35 C36 C37 C38 0.2(18) . . . . ?
C35 C36 C37 C41 178.9(11) . . . . ?
C36 O4 C34 C33 136.4(9) . . . . ?
C36 C35 C40 C39 0.4(15) . . . . ?
C36 C37 C38 O5 -176.0(10) . . . . ?
C36 C37 C38 C39 -0.3(17) . . . . ?
C37 C38 C39 C40 0.5(15) . . . . ?
C37 C38 C39 C43 -179.0(10) . . . . ?
C38 O5 C50 C51 -135.4(10) . . . . ?
C38 C39 C40 C35 -0.6(14) . . . . ?
C38 C39 C43 C44 148.7(10) . . . . ?
C38 C39 C43 C52 -84.8(11) . . . . ?
C39 C43 C44 C45 -172.9(9) . . . . ?
C39 C43 C52 C53 104.1(10) . . . . ?
C39 C43 C52 C57 -76.2(11) . . . . ?
C40 C35 C36 O4 -177.3(9) . . . . ?
C40 C35 C36 C37 -0.2(17) . . . . ?
C40 C39 C43 C44 -30.8(13) . . . . ?
C40 C39 C43 C52 95.7(10) . . . . ?
C41 C37 C38 O5 5.3(16) . . . . ?
C41 C37 C38 C39 -179.1(10) . . . . ?
C43 C39 C40 C35 178.9(9) . . . . ?
C43 C44 C45 C46 -178.1(10) . . . . ?
C43 C52 C53 O6 4.9(14) . . . . ?
C43 C52 C53 C54 -178.0(9) . . . . ?
C43 C52 C57 C56 -179.7(9) . . . . ?
C44 C43 C52 C53 -128.6(9) . . . . ?
C44 C43 C52 C57 51.1(12) . . . . ?
C44 C45 C46 C47 -179.2(10) . . . . ?
C45 C46 C47 C48 -180.0(11) . . . . ?
C46 C47 C48 C49 176.6(11) . . . . ?
C50 O5 C38 C37 -89.6(13) . . . . ?
C50 O5 C38 C39 94.7(12) . . . . ?
C51 O6 C53 C52 -106.7(11) . . . . ?
C51 O6 C53 C54 76.3(13) . . . . ?
C52 C43 C44 C45 61.2(12) . . . . ?
C52 C53 C54 C55 -3.7(15) . . . . ?
C52 C53 C54 C58 -176.8(9) . . . . ?
C53 O6 C51 C50 52.8(14) . . . . ?
C53 C52 C57 C56 0.0(15) . . . . ?
C53 C54 C55 O7 -174.6(9) . . . . ?
C53 C54 C55 C56 2.8(15) . . . . ?
C54 C55 C56 C57 -0.6(14) . . . . ?
C54 C55 C56 C60 -176.9(9) . . . . ?
C55 O7 C67 C68 -55.5(14) . . . . ?
C55 C56 C57 C52 -0.9(14) . . . . ?
C55 C56 C60 C1 -105.9(11) . . . . ?
C55 C56 C60 C61 125.8(10) . . . . ?
C56 C60 C61 C62 -67.2(13) . . . . ?
C57 C52 C53 O6 -174.8(9) . . . . ?
C57 C52 C53 C54 2.3(14) . . . . ?
C57 C56 C60 C1 78.0(11) . . . . ?
C57 C56 C60 C61 -50.4(13) . . . . ?
C58 C54 C55 O7 -1.2(14) . . . . ?
C58 C54 C55 C56 176.3(9) . . . . ?
C60 C1 C2 O8 1.1(16) . . . . ?
C60 C1 C2 C3 177.5(10) . . . . ?
C60 C1 C6 C5 -177.4(10) . . . . ?
C60 C56 C57 C52 175.4(9) . . . . ?
C60 C61 C62 C63 -165.7(14) . . . . ?
C61 C62 C63 C64 -67(2) . . . . ?
C62 C63 C64 C65 178.4(17) . . . . ?
C63 C64 C65 C66 177(2) . . . . ?
C67 O7 C55 C54 -77.8(12) . . . . ?
C67 O7 C55 C56 104.7(11) . . . . ?
C68 O8 C2 C1 -93.3(12) . . . . ?
C68 O8 C2 C3 90.2(12) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
8 -3 0 0.1145 8.0008 -3.0021 0.0023 -0.7207 -0.4738 0.4357
-8 2 0 0.0925 -8.0002 2.0027 -0.0022 0.7489 0.4968 -0.3424
0 -10 0 0.0161 0.0060 -9.9948 0.0014 0.2820 0.2294 0.9322
0 10 0 0.0048 -0.0060 9.9948 -0.0014 -0.2820 -0.2294 -0.9322
-1 -2 13 0.0165 -1.0048 -2.0179 13.0094 0.5256 -0.8403 -0.1475
1 4 -13 0.0034 1.0036 4.0168 -13.0097 -0.5820 0.7944 -0.0389

_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_2_mecn
_database_code_depnum_ccdc_archive 'CCDC 1556029'
_audit_update_record             
;
2017-06-14 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_audit_creation_date             2017-05-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H68 I4 O8, C2 H3 N'
_chemical_formula_sum            'C66 H71 I4 N O8'
_chemical_formula_weight         1513.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C80 H80 O8 Br4 N2'
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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.2220(2)
_cell_length_b                   24.9361(3)
_cell_length_c                   18.1166(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.6494(16)
_cell_angle_gamma                90
_cell_volume                     6351.82(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8862
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      75.7550
_cell_measurement_theta_min      3.5320
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.831
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.2143
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.1121
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25434
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.749
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         3.038
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9758
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -42.00  -13.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000   30.0000 29

#__ type_ start__ end____ width___ exp.time_
  2 omega  -49.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000  -60.0000 79

#__ type_ start__ end____ width___ exp.time_
  3 omega  -50.00   -5.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  125.0000  -30.0000 45

#__ type_ start__ end____ width___ exp.time_
  4 omega  -49.00   28.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000 -120.0000 77

#__ type_ start__ end____ width___ exp.time_
  5 omega  -83.00  -56.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  125.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
  6 omega   79.00  170.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -30.0000 91

#__ type_ start__ end____ width___ exp.time_
  7 omega  120.00  170.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000 -150.0000 50

#__ type_ start__ end____ width___ exp.time_
  8 omega  101.00  147.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000 -120.0000 46

#__ type_ start__ end____ width___ exp.time_
  9 omega   61.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 30

#__ type_ start__ end____ width___ exp.time_
 10 omega  106.00  132.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 11 omega   44.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
 12 omega   37.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 54

#__ type_ start__ end____ width___ exp.time_
 13 omega   36.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 62

#__ type_ start__ end____ width___ exp.time_
 14 omega   27.00   61.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.6513 -125.0000  150.0000 34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0294556000
_diffrn_orient_matrix_UB_12      -0.0167759000
_diffrn_orient_matrix_UB_13      0.0751233000
_diffrn_orient_matrix_UB_21      -0.0532715000
_diffrn_orient_matrix_UB_22      -0.0488277000
_diffrn_orient_matrix_UB_23      -0.0380198000
_diffrn_orient_matrix_UB_31      0.0910559000
_diffrn_orient_matrix_UB_32      -0.0339581000
_diffrn_orient_matrix_UB_33      0.0176625000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8938
_reflns_number_total             11246
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.967
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         11246
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      1.018
_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)+(0.0707P)²+20.7338P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1462
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C10(H10), C20(H20), C30(H30), C40(H40)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C19(H19A,H19B), C29(H29A,H29B), C39(H39A,H39B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C47(H47A,H47B),
  C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
 C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C26(H26), C36(H36)
3.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C58(H58A,H58B,H58C), C64(H64A,H64B,
 H64C), C66(H66A,H66B,H66C)
;
_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 0.3588(4) 0.3325(2) 0.7880(3) 0.0219(12) Uani 1 1 d . . . . .
C2 C 0.4060(4) 0.3723(2) 0.8330(3) 0.0238(12) Uani 1 1 d . . . . .
C3 C 0.5036(5) 0.3724(2) 0.8509(3) 0.0243(12) Uani 1 1 d . . . . .
C4 C 0.5565(4) 0.3309(2) 0.8253(3) 0.0248(13) Uani 1 1 d . . . . .
C5 C 0.5120(4) 0.2899(2) 0.7803(3) 0.0228(12) Uani 1 1 d . . . . .
C6 C 0.4134(4) 0.2922(2) 0.7616(3) 0.0207(12) Uani 1 1 d . . . . .
H6 H 0.3821 0.2654 0.7296 0.025 Uiso 1 1 calc R . . . .
C7 C 0.5515(5) 0.4171(3) 0.8923(4) 0.0304(14) Uani 1 1 d . . . . .
C8 C 0.5862(5) 0.4561(3) 0.9217(4) 0.0349(15) Uani 1 1 d . . . . .
C9 C 0.7136(4) 0.3490(3) 0.7988(4) 0.0285(14) Uani 1 1 d . . . . .
H9A H 0.6792 0.3773 0.7673 0.034 Uiso 1 1 calc R . . . .
H9B H 0.7711 0.3655 0.8276 0.034 Uiso 1 1 calc R . . . .
C10 C 0.5726(4) 0.2474(2) 0.7494(3) 0.0228(12) Uani 1 1 d . . . . .
H10 H 0.6314 0.2427 0.7867 0.027 Uiso 1 1 calc R . . . .
C11 C 0.6034(4) 0.2697(2) 0.6788(3) 0.0220(12) Uani 1 1 d . . . . .
C12 C 0.6838(4) 0.3013(2) 0.6845(4) 0.0250(13) Uani 1 1 d . . . . .
C13 C 0.7124(4) 0.3251(2) 0.6212(4) 0.0233(12) Uani 1 1 d . . . . .
C14 C 0.6585(4) 0.3165(2) 0.5516(3) 0.0225(12) Uani 1 1 d . . . . .
C15 C 0.5765(4) 0.2848(2) 0.5434(3) 0.0222(12) Uani 1 1 d . . . . .
C16 C 0.5495(4) 0.2628(2) 0.6073(3) 0.0236(12) Uani 1 1 d . . . . .
H16 H 0.4925 0.2424 0.6029 0.028 Uiso 1 1 calc R . . . .
C17 C 0.7951(4) 0.3595(2) 0.6292(4) 0.0258(13) Uani 1 1 d . . . . .
C18 C 0.8612(5) 0.3887(3) 0.6345(4) 0.0352(15) Uani 1 1 d . . . . .
C19 C 0.6448(4) 0.3880(2) 0.4637(4) 0.0265(13) Uani 1 1 d . . . . .
H19A H 0.6213 0.4063 0.5058 0.032 Uiso 1 1 calc R . . . .
H19B H 0.6918 0.4118 0.4452 0.032 Uiso 1 1 calc R . . . .
C20 C 0.5184(4) 0.2783(2) 0.4659(3) 0.0232(12) Uani 1 1 d . . . . .
H20 H 0.5638 0.2827 0.4292 0.028 Uiso 1 1 calc R . . . .
C21 C 0.4488(4) 0.3251(2) 0.4531(3) 0.0237(12) Uani 1 1 d . . . . .
C22 C 0.4787(4) 0.3744(2) 0.4271(3) 0.0236(12) Uani 1 1 d . . . . .
C23 C 0.4186(5) 0.4187(2) 0.4174(3) 0.0256(13) Uani 1 1 d . . . . .
C24 C 0.3252(5) 0.4130(2) 0.4326(3) 0.0256(13) Uani 1 1 d . . . . .
C25 C 0.2931(4) 0.3655(2) 0.4596(3) 0.0213(12) Uani 1 1 d . . . . .
C26 C 0.3562(4) 0.3221(2) 0.4696(3) 0.0231(12) Uani 1 1 d . . . . .
H26 H 0.3352 0.2893 0.4883 0.028 Uiso 1 1 calc R . . . .
C27 C 0.4513(4) 0.4701(2) 0.3960(3) 0.0259(13) Uani 1 1 d . . . . .
C28 C 0.4785(4) 0.5137(3) 0.3804(4) 0.0271(13) Uani 1 1 d . . . . .
C29 C 0.2534(4) 0.4908(2) 0.4765(3) 0.0254(13) Uani 1 1 d . . . . .
H29A H 0.2417 0.5277 0.4572 0.030 Uiso 1 1 calc R . . . .
H29B H 0.3129 0.4911 0.5127 0.030 Uiso 1 1 calc R . . . .
C30 C 0.1945(4) 0.3630(2) 0.4827(3) 0.0214(12) Uani 1 1 d . . . . .
H30 H 0.1533 0.3886 0.4498 0.026 Uiso 1 1 calc R . . . .
C31 C 0.2039(4) 0.3852(2) 0.5618(3) 0.0216(12) Uani 1 1 d . . . . .
C32 C 0.1993(4) 0.4402(2) 0.5732(3) 0.0211(12) Uani 1 1 d . . . . .
C33 C 0.2108(4) 0.4620(2) 0.6453(3) 0.0234(12) Uani 1 1 d . . . . .
C34 C 0.2272(4) 0.4274(2) 0.7064(3) 0.0208(12) Uani 1 1 d . . . . .
C35 C 0.2308(4) 0.3724(2) 0.6973(3) 0.0206(11) Uani 1 1 d . . . . .
C36 C 0.2211(4) 0.3521(2) 0.6249(3) 0.0201(11) Uani 1 1 d . . . . .
H36 H 0.2263 0.3145 0.6181 0.024 Uiso 1 1 calc R . . . .
C37 C 0.2045(4) 0.5192(3) 0.6563(4) 0.0283(14) Uani 1 1 d . . . . .
C38 C 0.2003(5) 0.5656(2) 0.6667(4) 0.0286(14) Uani 1 1 d . . . . .
C39 C 0.3263(4) 0.4570(2) 0.8155(3) 0.0258(13) Uani 1 1 d . . . . .
H39A H 0.3286 0.4901 0.8460 0.031 Uiso 1 1 calc R . . . .
H39B H 0.3711 0.4615 0.7791 0.031 Uiso 1 1 calc R . . . .
C40 C 0.2510(4) 0.3361(2) 0.7661(3) 0.0235(12) Uani 1 1 d . . . . .
H40 H 0.2265 0.3555 0.8077 0.028 Uiso 1 1 calc R . . . .
C41 C 0.5248(5) 0.1921(2) 0.7385(4) 0.0288(14) Uani 1 1 d . . . . .
H41A H 0.5084 0.1799 0.7869 0.035 Uiso 1 1 calc R . . . .
H41B H 0.4647 0.1959 0.7034 0.035 Uiso 1 1 calc R . . . .
C42 C 0.5860(5) 0.1489(3) 0.7085(4) 0.0320(14) Uani 1 1 d . . . . .
H42A H 0.5493 0.1150 0.7027 0.038 Uiso 1 1 calc R . . . .
H42B H 0.5985 0.1598 0.6584 0.038 Uiso 1 1 calc R . . . .
C43 C 0.6798(5) 0.1384(3) 0.7573(4) 0.0395(17) Uani 1 1 d . . . . .
H43A H 0.6682 0.1326 0.8092 0.047 Uiso 1 1 calc R . . . .
H43B H 0.7204 0.1706 0.7570 0.047 Uiso 1 1 calc R . . . .
C44 C 0.7336(6) 0.0896(3) 0.7325(5) 0.0413(17) Uani 1 1 d . . . . .
H44A H 0.7465 0.0956 0.6809 0.050 Uiso 1 1 calc R . . . .
H44B H 0.7956 0.0863 0.7654 0.050 Uiso 1 1 calc R . . . .
C45 C 0.6784(6) 0.0378(3) 0.7352(5) 0.0473(19) Uani 1 1 d . . . . .
H45A H 0.6222 0.0387 0.6956 0.057 Uiso 1 1 calc R . . . .
H45B H 0.6551 0.0355 0.7839 0.057 Uiso 1 1 calc R . . . .
C46 C 0.7371(7) -0.0126(3) 0.7246(6) 0.060(2) Uani 1 1 d . . . . .
H46A H 0.7522 -0.0134 0.6736 0.090 Uiso 1 1 calc GR . . . .
H46B H 0.7004 -0.0446 0.7333 0.090 Uiso 1 1 calc GR . . . .
H46C H 0.7963 -0.0120 0.7602 0.090 Uiso 1 1 calc GR . . . .
C47 C 0.4706(5) 0.2235(2) 0.4502(4) 0.0279(13) Uani 1 1 d . . . . .
H47A H 0.4286 0.2165 0.4880 0.033 Uiso 1 1 calc R . . . .
H47B H 0.4303 0.2245 0.4006 0.033 Uiso 1 1 calc R . . . .
C48 C 0.5415(5) 0.1780(3) 0.4515(4) 0.0317(14) Uani 1 1 d . . . . .
H48A H 0.5749 0.1736 0.5032 0.038 Uiso 1 1 calc R . . . .
H48B H 0.5896 0.1878 0.4197 0.038 Uiso 1 1 calc R . . . .
C49 C 0.4973(5) 0.1247(3) 0.4248(5) 0.0388(16) Uani 1 1 d . . . . .
H49A H 0.4661 0.1288 0.3725 0.047 Uiso 1 1 calc R . . . .
H49B H 0.4473 0.1157 0.4553 0.047 Uiso 1 1 calc R . . . .
C50 C 0.5672(5) 0.0784(3) 0.4289(5) 0.0422(18) Uani 1 1 d . . . . .
H50A H 0.5956 0.0727 0.4816 0.051 Uiso 1 1 calc R . . . .
H50B H 0.6192 0.0881 0.4006 0.051 Uiso 1 1 calc R . . . .
C51 C 0.5217(6) 0.0264(3) 0.3977(5) 0.051(2) Uani 1 1 d . . . . .
H51A H 0.4936 0.0321 0.3449 0.061 Uiso 1 1 calc R . . . .
H51B H 0.4695 0.0169 0.4258 0.061 Uiso 1 1 calc R . . . .
C52 C 0.5916(7) -0.0199(3) 0.4022(6) 0.061(3) Uani 1 1 d . . . . .
H52A H 0.6305 -0.0165 0.3621 0.092 Uiso 1 1 calc GR . . . .
H52B H 0.5566 -0.0539 0.3967 0.092 Uiso 1 1 calc GR . . . .
H52C H 0.6329 -0.0192 0.4506 0.092 Uiso 1 1 calc GR . . . .
C53 C 0.1462(4) 0.3076(2) 0.4730(3) 0.0224(12) Uani 1 1 d . . . . .
H53A H 0.1445 0.2956 0.4207 0.027 Uiso 1 1 calc R . . . .
H53B H 0.1845 0.2814 0.5058 0.027 Uiso 1 1 calc R . . . .
C54 C 0.0454(5) 0.3085(3) 0.4916(4) 0.0291(14) Uani 1 1 d . . . . .
H54A H 0.0071 0.3345 0.4583 0.035 Uiso 1 1 calc R . . . .
H54B H 0.0472 0.3212 0.5436 0.035 Uiso 1 1 calc R . . . .
C55 C -0.0034(5) 0.2539(3) 0.4835(4) 0.0350(16) Uani 1 1 d . . . . .
H55A H -0.0160 0.2445 0.4298 0.042 Uiso 1 1 calc R . . . .
H55B H 0.0409 0.2267 0.5089 0.042 Uiso 1 1 calc R . . . .
C56 C -0.0957(6) 0.2507(4) 0.5148(5) 0.052(2) Uani 1 1 d . . . . .
H56A H -0.1432 0.2745 0.4859 0.062 Uiso 1 1 calc R . . . .
H56B H -0.0854 0.2632 0.5673 0.062 Uiso 1 1 calc R . . . .
C57 C -0.1362(7) 0.1903(4) 0.5116(5) 0.060(2) Uani 1 1 d . . . . .
H57A H -0.1598 0.1806 0.4591 0.071 Uiso 1 1 calc R . . . .
H57B H -0.0840 0.1653 0.5306 0.071 Uiso 1 1 calc R . . . .
C58 C -0.2136(7) 0.1845(4) 0.5564(8) 0.080(3) Uani 1 1 d . . . . .
H58A H -0.2628 0.2113 0.5406 0.121 Uiso 1 1 calc GR . . . .
H58B H -0.1885 0.1897 0.6093 0.121 Uiso 1 1 calc GR . . . .
H58C H -0.2412 0.1485 0.5491 0.121 Uiso 1 1 calc GR . . . .
C59 C 0.1980(4) 0.2820(2) 0.7570(3) 0.0261(13) Uani 1 1 d . . . . .
H59A H 0.2213 0.2613 0.7168 0.031 Uiso 1 1 calc R . . . .
H59B H 0.2136 0.2613 0.8039 0.031 Uiso 1 1 calc R . . . .
C60 C 0.0914(5) 0.2873(3) 0.7388(4) 0.0318(14) Uani 1 1 d . . . . .
H60A H 0.0752 0.2997 0.6865 0.038 Uiso 1 1 calc R . . . .
H60B H 0.0701 0.3153 0.7713 0.038 Uiso 1 1 calc R . . . .
C61 C 0.0361(6) 0.2359(3) 0.7482(4) 0.0446(19) Uani 1 1 d . . . . .
H61A H 0.0496 0.2246 0.8011 0.054 Uiso 1 1 calc R . . . .
H61B H -0.0328 0.2439 0.7369 0.054 Uiso 1 1 calc R . . . .
C62 C 0.0572(6) 0.1901(3) 0.7006(5) 0.053(2) Uani 1 1 d . . . . .
H62A H 0.1262 0.1821 0.7107 0.064 Uiso 1 1 calc R . . . .
H62B H 0.0414 0.2004 0.6474 0.064 Uiso 1 1 calc R . . . .
C63 C 0.0007(8) 0.1389(4) 0.7148(6) 0.072(3) Uani 1 1 d . U . . .
H63A H 0.0043 0.1336 0.7693 0.086 Uiso 1 1 calc R . . . .
H63B H -0.0670 0.1441 0.6935 0.086 Uiso 1 1 calc R . . . .
C64 C 0.0378(11) 0.0893(5) 0.6808(10) 0.119(6) Uani 1 1 d . U . . .
H64A H 0.0446 0.0965 0.6287 0.179 Uiso 1 1 calc GR . . . .
H64B H -0.0070 0.0597 0.6828 0.179 Uiso 1 1 calc GR . . . .
H64C H 0.0998 0.0796 0.7089 0.179 Uiso 1 1 calc GR . . . .
I1 I 0.63940(4) 0.52115(2) 0.97751(3) 0.05214(16) Uani 1 1 d . . . . .
I2 I 0.97647(3) 0.43534(2) 0.64310(3) 0.04671(15) Uani 1 1 d . . . . .
I3 I 0.52099(3) 0.58713(2) 0.35828(2) 0.02876(11) Uani 1 1 d . . . . .
I4 I 0.19497(4) 0.64471(2) 0.68196(3) 0.05099(16) Uani 1 1 d . . . . .
O1 O 0.6541(3) 0.32959(17) 0.8495(2) 0.0276(9) Uani 1 1 d . . . . .
O2 O 0.7416(3) 0.30835(17) 0.7523(2) 0.0259(9) Uani 1 1 d . . . . .
O3 O 0.6904(3) 0.33959(17) 0.4898(2) 0.0277(9) Uani 1 1 d . . . . .
O4 O 0.5681(3) 0.37952(17) 0.4060(2) 0.0282(9) Uani 1 1 d . . . . .
O5 O 0.2647(3) 0.45628(17) 0.4167(2) 0.0259(9) Uani 1 1 d . . . . .
O6 O 0.1770(3) 0.47494(16) 0.5137(2) 0.0236(9) Uani 1 1 d . . . . .
O7 O 0.2331(3) 0.45009(16) 0.7766(2) 0.0253(9) Uani 1 1 d . . . . .
O8 O 0.3555(3) 0.41255(16) 0.8629(2) 0.0259(9) Uani 1 1 d . . . . .
C65 C 0.2659(6) 0.1770(4) 0.5773(5) 0.051(2) Uani 1 1 d . . . . .
C66 C 0.2158(11) 0.1326(5) 0.5357(8) 0.102(5) Uani 1 1 d . . . . .
H66A H 0.1864 0.1453 0.4864 0.153 Uiso 1 1 calc GR . . . .
H66B H 0.1664 0.1190 0.5631 0.153 Uiso 1 1 calc GR . . . .
H66C H 0.2610 0.1038 0.5298 0.153 Uiso 1 1 calc GR . . . .
N1 N 0.3039(6) 0.2119(3) 0.6060(4) 0.0579(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.392(8) . ?
C1 C6 1.397(8) . ?
C1 C40 1.527(8) . ?
C2 C3 1.377(9) . ?
C2 O8 1.391(7) . ?
C3 C4 1.400(9) . ?
C3 C7 1.455(8) . ?
C4 C5 1.398(8) . ?
C4 O1 1.392(7) . ?
C5 C6 1.394(8) . ?
C5 C10 1.526(8) . ?
C7 C8 1.180(10) . ?
C8 I1 1.999(7) . ?
C9 O1 1.423(8) . ?
C9 O2 1.414(8) . ?
C10 C11 1.518(8) . ?
C10 C41 1.535(8) . ?
C11 C12 1.381(9) . ?
C11 C16 1.413(8) . ?
C12 C13 1.403(9) . ?
C12 O2 1.383(7) . ?
C13 C14 1.392(9) . ?
C13 C17 1.445(8) . ?
C14 C15 1.397(8) . ?
C14 O3 1.394(7) . ?
C15 C16 1.387(9) . ?
C15 C20 1.527(8) . ?
C17 C18 1.182(10) . ?
C18 I2 1.998(7) . ?
C19 O3 1.417(7) . ?
C19 O4 1.408(8) . ?
C20 C21 1.525(8) . ?
C20 C47 1.533(8) . ?
C21 C22 1.405(8) . ?
C21 C26 1.396(9) . ?
C22 C23 1.392(9) . ?
C22 O4 1.388(7) . ?
C23 C24 1.404(9) . ?
C23 C27 1.436(8) . ?
C24 C25 1.385(8) . ?
C24 O5 1.383(8) . ?
C25 C26 1.401(9) . ?
C25 C30 1.524(8) . ?
C27 C28 1.201(9) . ?
C28 I3 1.989(6) . ?
C29 O5 1.411(8) . ?
C29 O6 1.418(7) . ?
C30 C31 1.523(8) . ?
C30 C53 1.542(8) . ?
C31 C32 1.390(8) . ?
C31 C36 1.400(8) . ?
C32 C33 1.400(8) . ?
C32 O6 1.383(7) . ?
C33 C34 1.397(9) . ?
C33 C37 1.444(9) . ?
C34 C35 1.382(8) . ?
C34 O7 1.383(7) . ?
C35 C36 1.394(8) . ?
C35 C40 1.534(8) . ?
C37 C38 1.175(9) . ?
C38 I4 1.995(6) . ?
C39 O7 1.415(7) . ?
C39 O8 1.426(7) . ?
C40 C59 1.542(8) . ?
C41 C42 1.534(9) . ?
C42 C43 1.508(10) . ?
C43 C44 1.541(10) . ?
C44 C45 1.516(11) . ?
C45 C46 1.538(11) . ?
C47 C48 1.517(9) . ?
C48 C49 1.517(9) . ?
C49 C50 1.518(10) . ?
C50 C51 1.519(10) . ?
C51 C52 1.519(11) . ?
C53 C54 1.522(8) . ?
C54 C55 1.526(9) . ?
C55 C56 1.509(10) . ?
C56 C57 1.610(13) . ?
C57 C58 1.470(14) . ?
C59 C60 1.509(9) . ?
C60 C61 1.526(9) . ?
C61 C62 1.488(12) . ?
C62 C63 1.549(12) . ?
C63 C64 1.512(18) . ?
C65 C66 1.462(13) . ?
C65 N1 1.112(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 C6 118.0(6) . . ?
C2 C1 C40 119.1(5) . . ?
C6 C1 C40 122.8(5) . . ?
C3 C2 C1 121.4(6) . . ?
C3 C2 O8 117.9(5) . . ?
O8 C2 C1 120.7(5) . . ?
C2 C3 C4 119.5(5) . . ?
C2 C3 C7 120.0(6) . . ?
C4 C3 C7 120.3(6) . . ?
C5 C4 C3 121.0(6) . . ?
O1 C4 C3 118.3(5) . . ?
O1 C4 C5 120.6(6) . . ?
C4 C5 C10 119.4(5) . . ?
C6 C5 C4 117.6(6) . . ?
C6 C5 C10 122.8(5) . . ?
C5 C6 C1 122.4(5) . . ?
C8 C7 C3 174.5(7) . . ?
C7 C8 I1 175.7(7) . . ?
O2 C9 O1 112.8(5) . . ?
C5 C10 C41 114.1(5) . . ?
C11 C10 C5 107.8(5) . . ?
C11 C10 C41 113.5(5) . . ?
C12 C11 C10 119.2(5) . . ?
C12 C11 C16 117.8(6) . . ?
C16 C11 C10 122.8(5) . . ?
C11 C12 C13 121.3(6) . . ?
C11 C12 O2 120.9(6) . . ?
O2 C12 C13 117.8(5) . . ?
C12 C13 C17 120.0(6) . . ?
C14 C13 C12 119.2(5) . . ?
C14 C13 C17 120.7(6) . . ?
C13 C14 C15 121.4(6) . . ?
C13 C14 O3 117.5(5) . . ?
O3 C14 C15 121.1(5) . . ?
C14 C15 C20 119.0(5) . . ?
C16 C15 C14 117.8(5) . . ?
C16 C15 C20 123.2(5) . . ?
C15 C16 C11 122.6(5) . . ?
C18 C17 C13 178.1(7) . . ?
C17 C18 I2 177.6(6) . . ?
O4 C19 O3 112.7(5) . . ?
C15 C20 C47 115.3(5) . . ?
C21 C20 C15 108.0(5) . . ?
C21 C20 C47 113.2(5) . . ?
C22 C21 C20 119.9(6) . . ?
C26 C21 C20 122.5(5) . . ?
C26 C21 C22 117.6(6) . . ?
C23 C22 C21 121.7(6) . . ?
O4 C22 C21 120.5(5) . . ?
O4 C22 C23 117.6(5) . . ?
C22 C23 C24 118.4(6) . . ?
C22 C23 C27 121.7(6) . . ?
C24 C23 C27 119.9(6) . . ?
C25 C24 C23 121.9(6) . . ?
O5 C24 C23 117.2(5) . . ?
O5 C24 C25 120.9(6) . . ?
C24 C25 C26 117.9(6) . . ?
C24 C25 C30 119.8(5) . . ?
C26 C25 C30 122.1(5) . . ?
C21 C26 C25 122.5(5) . . ?
C28 C27 C23 177.9(7) . . ?
C27 C28 I3 177.4(6) . . ?
O5 C29 O6 112.3(5) . . ?
C25 C30 C53 114.7(5) . . ?
C31 C30 C25 106.9(5) . . ?
C31 C30 C53 114.0(5) . . ?
C32 C31 C30 119.9(5) . . ?
C32 C31 C36 117.8(5) . . ?
C36 C31 C30 122.2(5) . . ?
C31 C32 C33 121.4(5) . . ?
O6 C32 C31 120.8(5) . . ?
O6 C32 C33 117.7(5) . . ?
C32 C33 C37 120.8(6) . . ?
C34 C33 C32 118.7(5) . . ?
C34 C33 C37 120.5(6) . . ?
C35 C34 C33 121.5(5) . . ?
C35 C34 O7 121.2(5) . . ?
O7 C34 C33 117.1(5) . . ?
C34 C35 C36 118.2(5) . . ?
C34 C35 C40 119.6(5) . . ?
C36 C35 C40 122.0(5) . . ?
C35 C36 C31 122.3(5) . . ?
C38 C37 C33 178.7(8) . . ?
C37 C38 I4 178.5(7) . . ?
O7 C39 O8 111.8(5) . . ?
C1 C40 C35 107.6(5) . . ?
C1 C40 C59 115.6(5) . . ?
C35 C40 C59 113.7(5) . . ?
C42 C41 C10 114.4(5) . . ?
C43 C42 C41 114.4(6) . . ?
C42 C43 C44 113.6(6) . . ?
C45 C44 C43 112.4(7) . . ?
C44 C45 C46 113.5(7) . . ?
C48 C47 C20 112.9(5) . . ?
C47 C48 C49 114.1(6) . . ?
C48 C49 C50 114.5(6) . . ?
C49 C50 C51 113.1(6) . . ?
C50 C51 C52 113.0(7) . . ?
C54 C53 C30 112.3(5) . . ?
C53 C54 C55 113.3(6) . . ?
C56 C55 C54 114.8(6) . . ?
C55 C56 C57 111.3(7) . . ?
C58 C57 C56 111.4(8) . . ?
C60 C59 C40 114.0(5) . . ?
C59 C60 C61 114.9(6) . . ?
C62 C61 C60 115.3(7) . . ?
C61 C62 C63 112.3(8) . . ?
C64 C63 C62 112.6(11) . . ?
C4 O1 C9 116.8(4) . . ?
C12 O2 C9 116.0(4) . . ?
C14 O3 C19 115.6(5) . . ?
C22 O4 C19 116.7(5) . . ?
C24 O5 C29 117.1(4) . . ?
C32 O6 C29 116.3(4) . . ?
C34 O7 C39 115.6(5) . . ?
C2 O8 C39 116.6(5) . . ?
N1 C65 C66 176.9(11) . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2 -7 -10 0.0489 2.0000 -7.0000 -10.0000 -0.6927 0.6154 0.2432
-1 7 11 0.0498 -1.0000 7.0000 11.0000 0.7384 -0.7067 -0.1345
7 -7 4 0.0679 7.0000 -7.0000 4.0000 0.2117 -0.1832 0.9457
-7 7 -3 0.0962 -7.0000 7.0000 -3.0000 -0.1366 0.1452 -0.9281
0 15 -4 0.0882 -0.0000 15.0000 -4.0000 -0.5521 -0.5803 -0.5800
9 -3 -1 0.0756 9.0000 -3.0000 -1.0000 -0.2899 -0.2949 0.9037
-8 -8 4 0.0721 -8.0000 -8.0000 3.9999 0.6703 0.6647 -0.3861
2 -15 3 0.0676 2.0000 -15.0000 3.0000 0.4181 0.5118 0.7445

_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_3_acetone
_database_code_depnum_ccdc_archive 'CCDC 1556031'
_audit_update_record             
;
2017-07-12 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT082_3_acetone           
;
PROBLEM: High R1 Value ..................................       0.22 Report
RESPONSE: The structure is badly disordered, which include the main
resorcinarene frame and the many acetone molecules.
;
_vrf_PLAT084_3_acetone           
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.53 Report
RESPONSE: The structure is badly disordered, which include the main
resorcinarene frame and the many acetone molecules.
;
_vrf_PLAT413_3_acetone           
;
PROBLEM: Short Inter XH3 .. XHn     H74C   ..  H82B    ..       1.79 Ang.  
RESPONSE: The involved hydrogen atoms belong to the heavily disordered
groups.
;
_vrf_PLAT971_3_acetone           
;
PROBLEM: Check Calcd Residual Density  0.98A From      I3       5.26 eA-3  
RESPONSE:The larege residual density is very close to the heavy idoine
atom, which might be caused by the unsuitable absorption correction.
;
_vrf_PLAT097_3_acetone           
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       5.44 eA-3  
RESPONSE: The larege residual density is very close to the heavy idoine
atom, which might be caused by the unsuitable absorption correction.
;
_vrf_PLAT201_3_acetone           
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          5 Report
RESPONSE: The related atoms/grous are heavily disordered. They were 
refined with fixed isotropic thermal parameters.
;
_vrf_PLAT220_3_acetone           
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        7.7 Ratio 
RESPONSE: The realted carbon atoms are in disorder.
;
_vrf_PLAT234_3_acetone           
;
PROBLEM: Large Hirshfeld Difference C13    --  C14     ..       0.28 Ang.  
RESPONSE: The related carbon atoms belong to the hexyl groups, which
are in bad disorder. Only the main residual was assigned with full
occupancy.
;
_vrf_PLAT342_3_acetone           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04338 Ang.  
RESPONSE: The structure contains many heavily disordered groups.
;
_vrf_PLAT601_3_acetone           
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        138 Ang3  
RESPONSE: The structure contains many lattice solvent molecules. Most
of them are in serious disorder. Some of them were not assigned, which
resulted in the large un-assigned solvent accessible voids. Squeeze can
be used to help analyze the content of the voids, however, the squeeze
results could be not reliable due to the low quality of the crystal and 
diffraction data, and the information is not that important to our work.
;
# end Validation Reply Form
_audit_creation_date             2017-07-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H76 I4 O8, 3.5(C3 H6 O)'
_chemical_formula_sum            'C78.50 H97 I4 O11.50'
_chemical_formula_weight         1732.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C90 H100 N4 I4 O4'
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'
I I -0.3257 6.8362 '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                   16.4002(10)
_cell_length_b                   17.5718(8)
_cell_length_c                   19.1603(10)
_cell_angle_alpha                114.995(5)
_cell_angle_beta                 91.376(6)
_cell_angle_gamma                116.803(6)
_cell_volume                     4306.9(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7976
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.5820
_cell_measurement_theta_min      4.5450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.3525
_exptl_crystal_size_mid          0.2939
_exptl_crystal_size_min          0.2464
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30875
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.443
_diffrn_reflns_theta_min         3.015
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -41.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4013   37.0000   30.0000 74

#__ type_ start__ end____ width___ exp.time_
  2 omega  -14.00   30.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4013   37.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
  3 omega  -97.00  -69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4013  -77.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
  4 omega -120.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4013  -19.0000 -150.0000 118

#__ type_ start__ end____ width___ exp.time_
  5 omega  -39.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4013  -77.0000  -60.0000 30

#__ type_ start__ end____ width___ exp.time_
  6 omega  -95.00   -5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4013  125.0000   60.0000 90

#__ type_ start__ end____ width___ exp.time_
  7 omega   44.00   74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4013 -137.0000  -67.0000 30

#__ type_ start__ end____ width___ exp.time_
  8 omega   34.00   79.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000 -180.0000 45

#__ type_ start__ end____ width___ exp.time_
  9 omega   40.00   73.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -45.0000   90.0000 33

#__ type_ start__ end____ width___ exp.time_
 10 omega  130.00  159.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  137.0000   -4.0000 29

#__ type_ start__ end____ width___ exp.time_
 11 omega   50.00  105.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -94.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
 12 omega   37.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000  120.0000 54

#__ type_ start__ end____ width___ exp.time_
 13 omega   36.00  120.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818 -125.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
 14 omega   80.00  160.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   30.0000   30.0000 80

#__ type_ start__ end____ width___ exp.time_
 15 omega   46.00   89.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000   30.0000 43

#__ type_ start__ end____ width___ exp.time_
 16 omega   45.00  103.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -94.0000 -180.0000 58

#__ type_ start__ end____ width___ exp.time_
 17 omega   91.00  120.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818 -125.0000  120.0000 29

#__ type_ start__ end____ width___ exp.time_
 18 omega   96.00  178.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   30.0000   90.0000 82

#__ type_ start__ end____ width___ exp.time_
 19 omega   29.00   66.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000  -90.0000 37

#__ type_ start__ end____ width___ exp.time_
 20 omega   43.00   88.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000  -30.0000 45

#__ type_ start__ end____ width___ exp.time_
 21 omega  133.00  178.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   45.0000  -60.0000 45

#__ type_ start__ end____ width___ exp.time_
 22 omega   37.00  135.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -77.0000  -30.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0884608000
_diffrn_orient_matrix_UB_12      -0.0686522000
_diffrn_orient_matrix_UB_13      0.0148758000
_diffrn_orient_matrix_UB_21      0.0639128000
_diffrn_orient_matrix_UB_22      0.0053425000
_diffrn_orient_matrix_UB_23      0.0642216000
_diffrn_orient_matrix_UB_31      -0.0019518000
_diffrn_orient_matrix_UB_32      0.0887968000
_diffrn_orient_matrix_UB_33      0.0641836000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10948
_reflns_number_total             16680
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         5.437
_refine_diff_density_min         -2.267
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         16680
_refine_ls_number_restraints     565
_refine_ls_R_factor_all          0.2671
_refine_ls_R_factor_gt           0.2203
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1924P)²+181.5318P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4934
_refine_ls_wR_factor_ref         0.5261
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C81-O13
 1.2 with sigma of 0.02
 C82-C81 = C83-C81
 1.5 with sigma of 0.02
 C83-C82
 2.5 with sigma of 0.02
 C16-C17 = C16-C15 = C15-C14 = C68-C67 = C67-C66 = C66-C65 = C65-C64 = C64-C63
 = C14-C13 = C34-C33 = C33-C32 = C32-C31 = C31-C30 = C30-C29 = C51-C50 = C50-
 C49 = C49-C48 = C48-C47 = C47-C46 = C13-C12
 1.52 with sigma of 0.01
 H76C-H80C_$1 = H74B-H82B
 2.1 with sigma of 0.02
 C58B-C59B \\sim C59-C58
 with sigma of 0.01
 I4B-C59B \\sim I4-C59
 with sigma of 0.01
 C58-C59 \\sim C7-C8
 with sigma of 0.02
 C59-I4 \\sim C8-I1
 with sigma of 0.02
 C82-O13 \\sim O13-C83
 with sigma of 0.02
 C79-C78 \\sim C80-C78 \\sim C73-C72 \\sim C74-C72 \\sim C70-C69 \\sim C71-C69
\\sim C77-C75 \\sim C76-C75
 \\sim C82-C81 \\sim C83-C81
 with sigma of 0.02
 C58B-C53B \\sim C58-C53
 with sigma of 0.01
 C54-C53B \\sim C53B-C52 \\sim C54-C53 \\sim C53-C52
 with sigma of 0.01
 C53-C58 \\sim C2-C7
 with sigma of 0.02
3. Restrained planarity
 O13, C81, C82, C83
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(I1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C47) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C83)
\\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq,
Uanis(C74) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C69) \\sim Ueq,
Uanis(I4) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C79) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(I2) = Uanis(I2B)
Uanis(C59) = Uanis(C59B)
Uanis(C58) = Uanis(C58B)
Uanis(C53B) = Uanis(C53)
5. Others
 Fixed Sof: I2(0.9) I4(0.66667) C53(0.66667) C58(0.66667) C59(0.66667)
 C79(0.5) H79A(0.5) H79B(0.5) H79C(0.5) C78(0.5) O12(0.5) C80(0.5) H80A(0.5)
 H80B(0.5) H80C(0.5) O11(0.5) C75(0.5) C76(0.5) H76A(0.5) H76B(0.5) H76C(0.5)
 C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5) I4B(0.33333) I2B(0.1) C58B(0.33333)
 C59B(0.33333) C53B(0.33333) O13(0.5) C81(0.5) C82(0.5) H82A(0.5) H82B(0.5)
 H82C(0.5) C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5)
 Fixed Uiso: C16(0.19) C17(0.2) C32(0.16) C33(0.18) C34(0.2)
6.a Riding coordinates:
 C34(H34A,H34B,H34C), C82(H82A,H82B,H82C)
6.b Ternary CH refined with riding coordinates:
 C11(H11), C28(H28), C45(H45), C62(H62)
6.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,H29B),
  C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C43(H43A,
 H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C60(H60A,H60B), C61(H61A,H61B), C63(H63A,H63B),
  C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C22(H22), C39(H39), C56(H56)
6.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C51(H51A,H51B,H51C), C68(H68A,H68B,H68C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C76(H76A,
 H76B,H76C), C77(H77A,H77B,H77C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C),
 C83(H83A,H83B,H83C)
;
_atom_sites_solution_hydrogens   mixed
_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
I1 I 0.34946(12) 0.50244(12) 0.99263(16) 0.0994(8) Uani 1 1 d D U . . .
I2 I 0.78206(12) 0.37415(15) 1.25799(14) 0.0849(7) Uani 0.9 1 d . . P A 1
I3 I 1.14190(11) 0.14500(16) 0.88033(18) 0.1182(10) Uani 1 1 d . . . . .
I4 I 0.9088(4) 0.5214(3) 0.6956(4) 0.201(3) Uani 0.6667 1 d D U P B 1
O1 O 0.3432(10) 0.1922(12) 0.9487(11) 0.063(4) Uani 1 1 d . . . . .
O2 O 0.4724(8) 0.1646(9) 1.0252(8) 0.045(3) Uani 1 1 d . . . . .
O3 O 0.6996(8) 0.0619(9) 0.9942(8) 0.046(3) Uani 1 1 d . U . . .
O4 O 0.7962(8) -0.0140(9) 0.8840(7) 0.044(3) Uani 1 1 d . U . . .
O5 O 0.8479(10) 0.0549(11) 0.6670(8) 0.055(3) Uani 1 1 d . U . . .
O6 O 0.7856(10) 0.1703(12) 0.6368(11) 0.073(5) Uani 1 1 d . . . . .
O7 O 0.5587(10) 0.2760(11) 0.6709(9) 0.059(3) Uani 1 1 d . U . . .
O8 O 0.3987(10) 0.2620(11) 0.7322(9) 0.059(3) Uani 1 1 d . U . . .
C1 C 0.3920(13) 0.2056(13) 0.7685(12) 0.046(4) Uani 1 1 d . U . . .
C16 C -0.032(4) -0.162(4) 0.823(3) 0.190 Uiso 1 1 d D U . . .
H16A H 0.0049 -0.0938 0.8634 0.228 Uiso 1 1 calc R . . . .
H16B H -0.0378 -0.2027 0.8465 0.228 Uiso 1 1 calc R . . . .
C2 C 0.3808(13) 0.2346(12) 0.8467(11) 0.044(4) Uani 1 1 d D U . . .
C3 C 0.3652(12) 0.1741(12) 0.8813(10) 0.037(3) Uani 1 1 d . U . . .
C4 C 0.3703(11) 0.0880(12) 0.8376(10) 0.039(4) Uani 1 1 d . U . . .
C5 C 0.3862(12) 0.0664(12) 0.7635(11) 0.041(4) Uani 1 1 d . U . . .
H5 H 0.3889 0.0098 0.7366 0.049 Uiso 1 1 calc R . . . .
C6 C 0.3991(14) 0.1220(14) 0.7228(13) 0.052(5) Uani 1 1 d . U . . .
C7 C 0.3717(15) 0.3191(14) 0.8889(13) 0.058(5) Uani 1 1 d D U . . .
C8 C 0.3634(14) 0.3877(14) 0.9248(12) 0.054(5) Uani 1 1 d D U . . .
C9 C 0.4189(18) 0.2691(17) 1.0190(18) 0.071(7) Uani 1 1 d . . . . .
H9A H 0.3954 0.2721 1.0656 0.085 Uiso 1 1 calc R . . . .
H9B H 0.4386 0.3306 1.0200 0.085 Uiso 1 1 calc R . . . .
C10 C 0.5051(13) 0.2571(12) 1.0248(11) 0.043(4) Uani 1 1 d . U . . .
H10A H 0.5309 0.2556 0.9795 0.052 Uiso 1 1 calc R . . . .
H10B H 0.5541 0.3109 1.0734 0.052 Uiso 1 1 calc R . . . .
C11 C 0.3525(12) 0.0193(12) 0.8716(11) 0.040(4) Uani 1 1 d . U . . .
H11 H 0.3291 0.0413 0.9185 0.048 Uiso 1 1 calc R . . . .
C12 C 0.2763(11) -0.0856(14) 0.8134(13) 0.052(5) Uani 1 1 d D U . . .
H12A H 0.2953 -0.1083 0.7646 0.062 Uiso 1 1 calc R . . . .
H12B H 0.2704 -0.1268 0.8365 0.062 Uiso 1 1 calc R . . . .
C13 C 0.1809(12) -0.0948(17) 0.7936(16) 0.072(6) Uani 1 1 d D U . . .
H13A H 0.1717 -0.0551 0.8427 0.086 Uiso 1 1 calc R . . . .
H13B H 0.1835 -0.0675 0.7585 0.086 Uiso 1 1 calc R . . . .
C14 C 0.095(2) -0.197(2) 0.755(3) 0.152(16) Uani 1 1 d D U . . .
H14A H 0.0931 -0.2287 0.7858 0.182 Uiso 1 1 calc R . . . .
H14B H 0.0965 -0.2358 0.7012 0.182 Uiso 1 1 calc R . . . .
C15 C 0.009(3) -0.184(4) 0.751(3) 0.166(18) Uani 1 1 d D U . . .
H15A H 0.0253 -0.1324 0.7385 0.199 Uiso 1 1 calc R . . . .
H15B H -0.0415 -0.2436 0.7068 0.199 Uiso 1 1 calc R . . . .
C17 C -0.128(4) -0.188(4) 0.781(4) 0.200 Uiso 1 1 d D U . . .
H17A H -0.1770 -0.2273 0.7980 0.300 Uiso 1 1 calc GR . . . .
H17B H -0.1392 -0.2240 0.7243 0.300 Uiso 1 1 calc GR . . . .
H17C H -0.1294 -0.1294 0.7946 0.300 Uiso 1 1 calc GR . . . .
C18 C 0.5046(11) 0.1065(11) 0.9792(10) 0.036(3) Uani 1 1 d . U . . .
C19 C 0.5928(11) 0.1213(11) 1.0100(10) 0.034(3) Uani 1 1 d . U . . .
C20 C 0.6184(13) 0.0544(13) 0.9610(12) 0.046(4) Uani 1 1 d . U . . .
C21 C 0.5636(11) -0.0221(11) 0.8856(10) 0.035(3) Uani 1 1 d . U . . .
C22 C 0.4806(11) -0.0285(11) 0.8582(10) 0.036(3) Uani 1 1 d . U . . .
H22 H 0.4448 -0.0766 0.8062 0.043 Uiso 1 1 calc R . . . .
C23 C 0.4476(10) 0.0299(10) 0.9015(9) 0.030(3) Uani 1 1 d . U . . .
C24 C 0.6532(12) 0.2015(12) 1.0863(10) 0.038(4) Uani 1 1 d . U . . .
C25 C 0.7058(14) 0.2725(14) 1.1513(13) 0.052(5) Uani 1 1 d . U . . .
C26 C 0.7870(12) 0.1288(15) 0.9863(15) 0.060(6) Uani 1 1 d . . . . .
H26A H 0.8220 0.1888 1.0367 0.072 Uiso 1 1 calc R . . . .
H26B H 0.7735 0.1446 0.9462 0.072 Uiso 1 1 calc R . . . .
C27 C 0.8453(13) 0.0784(14) 0.9612(11) 0.049(4) Uani 1 1 d . U . . .
H27A H 0.9050 0.1226 0.9570 0.059 Uiso 1 1 calc R . . . .
H27B H 0.8593 0.0646 1.0025 0.059 Uiso 1 1 calc R . . . .
C28 C 0.5981(12) -0.0899(13) 0.8359(12) 0.045(4) Uani 1 1 d . . . . .
H28 H 0.6345 -0.0941 0.8741 0.054 Uiso 1 1 calc R . . . .
C29 C 0.5188(13) -0.1943(12) 0.7793(11) 0.045(4) Uani 1 1 d D U . . .
H29A H 0.4756 -0.2175 0.8089 0.054 Uiso 1 1 calc R . . . .
H29B H 0.4835 -0.1944 0.7379 0.054 Uiso 1 1 calc R . . . .
C30 C 0.5547(19) -0.2642(16) 0.7405(18) 0.088(8) Uani 1 1 d D U . . .
H30A H 0.5697 -0.2615 0.6926 0.105 Uiso 1 1 calc R . . . .
H30B H 0.6135 -0.2400 0.7767 0.105 Uiso 1 1 calc R . . . .
C31 C 0.490(3) -0.3706(19) 0.717(3) 0.146(15) Uani 1 1 d D U . . .
H31A H 0.4377 -0.4012 0.6719 0.175 Uiso 1 1 calc R . . . .
H31B H 0.4645 -0.3752 0.7615 0.175 Uiso 1 1 calc R . . . .
C32 C 0.547(3) -0.423(4) 0.697(3) 0.160 Uiso 1 1 d D . . . .
H32A H 0.4974 -0.4905 0.6747 0.192 Uiso 1 1 calc R . . . .
H32B H 0.5651 -0.4165 0.6507 0.192 Uiso 1 1 calc R . . . .
C33 C 0.630(3) -0.419(4) 0.737(3) 0.180 Uiso 1 1 d D . . . .
H33A H 0.6163 -0.4397 0.7767 0.216 Uiso 1 1 calc R . . . .
H33B H 0.6870 -0.3553 0.7599 0.216 Uiso 1 1 calc R . . . .
C34 C 0.638(4) -0.494(4) 0.663(3) 0.200 Uiso 1 1 d D . . . .
H34A H 0.6398 -0.4773 0.6210 0.300 Uiso 1 1 d R . . . .
H34B H 0.5839 -0.5578 0.6451 0.300 Uiso 1 1 d R . . . .
H34C H 0.6947 -0.4942 0.6757 0.300 Uiso 1 1 d R . . . .
C35 C 0.7625(12) -0.0095(11) 0.8209(10) 0.038(3) Uani 1 1 d . U . . .
C36 C 0.8259(14) 0.0295(14) 0.7816(12) 0.052(5) Uani 1 1 d . U . . .
C37 C 0.7903(13) 0.0275(12) 0.7117(10) 0.042(4) Uani 1 1 d . U . . .
C38 C 0.6938(14) -0.0110(14) 0.6857(12) 0.050(4) Uani 1 1 d . U . . .
C39 C 0.6347(13) -0.0460(12) 0.7285(11) 0.043(4) Uani 1 1 d . U . . .
H39 H 0.5703 -0.0702 0.7112 0.052 Uiso 1 1 calc R . . . .
C40 C 0.6658(11) -0.0470(12) 0.7948(10) 0.036(3) Uani 1 1 d . U . . .
C41 C 0.9250(15) 0.0664(15) 0.8067(15) 0.061(6) Uani 1 1 d . . . . .
C42 C 1.0054(17) 0.0960(19) 0.8343(18) 0.079(8) Uani 1 1 d . . . . .
C43 C 0.9067(16) 0.1588(18) 0.6977(16) 0.068(6) Uani 1 1 d . . . . .
H43A H 0.9429 0.1707 0.6604 0.082 Uiso 1 1 calc R . . . .
H43B H 0.9511 0.1871 0.7480 0.082 Uiso 1 1 calc R . . . .
C44 C 0.8473(17) 0.2086(17) 0.7108(16) 0.069(6) Uani 1 1 d . U . . .
H44A H 0.8108 0.1970 0.7480 0.082 Uiso 1 1 calc R . . . .
H44B H 0.8887 0.2784 0.7332 0.082 Uiso 1 1 calc R . . . .
C45 C 0.6531(15) -0.0189(14) 0.6060(11) 0.050(4) Uani 1 1 d . U . . .
H45 H 0.7035 -0.0056 0.5787 0.060 Uiso 1 1 calc R . . . .
C46 C 0.5705(19) -0.1219(16) 0.5509(16) 0.075(6) Uani 1 1 d D U . . .
H46A H 0.5156 -0.1292 0.5717 0.090 Uiso 1 1 calc R . . . .
H46B H 0.5560 -0.1276 0.4990 0.090 Uiso 1 1 calc R . . . .
C47 C 0.583(2) -0.207(2) 0.539(2) 0.117(11) Uani 1 1 d D U . . .
H47A H 0.5994 -0.2027 0.5897 0.141 Uiso 1 1 calc R . . . .
H47B H 0.5249 -0.2682 0.5057 0.141 Uiso 1 1 calc R . . . .
C48 C 0.662(2) -0.200(2) 0.498(2) 0.109(10) Uani 1 1 d D U . . .
H48A H 0.7221 -0.1460 0.5364 0.131 Uiso 1 1 calc R . . . .
H48B H 0.6530 -0.1864 0.4555 0.131 Uiso 1 1 calc R . . . .
C49 C 0.669(4) -0.292(3) 0.463(3) 0.18(2) Uani 1 1 d D U . . .
H49A H 0.6142 -0.3423 0.4174 0.211 Uiso 1 1 calc R . . . .
H49B H 0.7244 -0.2787 0.4424 0.211 Uiso 1 1 calc R . . . .
C50 C 0.674(5) -0.337(4) 0.515(3) 0.22(3) Uani 1 1 d D U . . .
H50A H 0.6130 -0.3643 0.5252 0.259 Uiso 1 1 calc R . . . .
H50B H 0.7196 -0.2841 0.5654 0.259 Uiso 1 1 calc R . . . .
C51 C 0.701(5) -0.415(5) 0.484(4) 0.23(3) Uani 1 1 d D U . . .
H51A H 0.6490 -0.4755 0.4767 0.351 Uiso 1 1 calc GR . . . .
H51B H 0.7554 -0.3957 0.5223 0.351 Uiso 1 1 calc GR . . . .
H51C H 0.7163 -0.4244 0.4341 0.351 Uiso 1 1 calc GR . . . .
C52 C 0.6966(14) 0.1530(14) 0.6418(13) 0.054(5) Uani 1 1 d D U . . .
C53 C 0.6695(13) 0.2190(15) 0.6450(18) 0.052(7) Uani 0.6667 1 d D U P B 1
C54 C 0.5829(13) 0.2068(14) 0.6608(12) 0.050(4) Uani 1 1 d D U . . .
C55 C 0.5084(13) 0.1104(13) 0.6408(11) 0.045(4) Uani 1 1 d . U . . .
C56 C 0.5367(15) 0.0406(15) 0.6255(16) 0.068(7) Uani 1 1 d . . . . .
H56 H 0.4903 -0.0216 0.6145 0.082 Uiso 1 1 calc R . . . .
C57 C 0.6264(14) 0.0577(14) 0.6258(12) 0.049(4) Uani 1 1 d . U . . .
C58 C 0.7406(14) 0.3143(13) 0.6595(15) 0.031(4) Uani 0.6667 1 d D U P B 1
C59 C 0.803(2) 0.395(2) 0.682(3) 0.081(10) Uani 0.6667 1 d D U P B 1
C60 C 0.5701(14) 0.3324(15) 0.7486(12) 0.053(5) Uani 1 1 d . U . . .
H60A H 0.6295 0.3938 0.7698 0.064 Uiso 1 1 calc R . . . .
H60B H 0.5717 0.3000 0.7785 0.064 Uiso 1 1 calc R . . . .
C61 C 0.4867(17) 0.3508(17) 0.7566(16) 0.070(6) Uani 1 1 d . U . . .
H61A H 0.4973 0.3968 0.8117 0.084 Uiso 1 1 calc R . . . .
H61B H 0.4834 0.3796 0.7239 0.084 Uiso 1 1 calc R . . . .
C62 C 0.4080(14) 0.0905(14) 0.6420(12) 0.051(4) Uani 1 1 d . U . . .
H62 H 0.3991 0.1319 0.6245 0.062 Uiso 1 1 calc R . . . .
C63 C 0.3336(14) -0.0147(17) 0.5823(14) 0.066(6) Uani 1 1 d D U . . .
H63A H 0.3465 -0.0252 0.5309 0.079 Uiso 1 1 calc R . . . .
H63B H 0.3481 -0.0550 0.5962 0.079 Uiso 1 1 calc R . . . .
C64 C 0.2269(16) -0.059(2) 0.567(2) 0.118(11) Uani 1 1 d D U . . .
H64A H 0.1960 -0.1209 0.5178 0.141 Uiso 1 1 calc R . . . .
H64B H 0.2073 -0.0722 0.6102 0.141 Uiso 1 1 calc R . . . .
C65 C 0.196(2) 0.007(3) 0.561(3) 0.126(13) Uani 1 1 d D U . . .
H65A H 0.2184 0.0239 0.5207 0.152 Uiso 1 1 calc R . . . .
H65B H 0.2226 0.0673 0.6120 0.152 Uiso 1 1 calc R . . . .
C66 C 0.088(2) -0.043(3) 0.541(2) 0.146(15) Uani 1 1 d D U . . .
H66A H 0.0684 -0.0047 0.5278 0.175 Uiso 1 1 calc R . . . .
H66B H 0.0611 -0.1065 0.4939 0.175 Uiso 1 1 calc R . . . .
C67 C 0.049(3) -0.054(3) 0.609(2) 0.144(15) Uani 1 1 d D U . . .
H67A H 0.0804 0.0078 0.6576 0.173 Uiso 1 1 calc R . . . .
H67B H 0.0608 -0.0997 0.6176 0.173 Uiso 1 1 calc R . . . .
C68 C -0.057(3) -0.093(4) 0.586(3) 0.163(18) Uani 1 1 d D U . . .
H68A H -0.0691 -0.0652 0.5570 0.244 Uiso 1 1 calc GR . . . .
H68B H -0.0780 -0.0765 0.6338 0.244 Uiso 1 1 calc GR . . . .
H68C H -0.0897 -0.1631 0.5536 0.244 Uiso 1 1 calc GR . . . .
C79 C 1.275(3) 0.410(3) 0.745(3) 0.065(11) Uani 0.5 1 d D U P . .
H79A H 1.2810 0.4469 0.8008 0.098 Uiso 0.5 1 calc GR . P . .
H79B H 1.2731 0.4437 0.7179 0.098 Uiso 0.5 1 calc GR . P . .
H79C H 1.3286 0.4004 0.7397 0.098 Uiso 0.5 1 calc GR . P . .
C78 C 1.188(3) 0.315(3) 0.711(3) 0.075(13) Uani 0.5 1 d D . P . .
O12 O 1.170(4) 0.227(5) 0.694(4) 0.15(2) Uani 0.5 1 d . . P . .
C80 C 1.118(4) 0.343(4) 0.731(4) 0.086(15) Uani 0.5 1 d D U P . .
H80A H 1.1394 0.4060 0.7367 0.129 Uiso 0.5 1 calc GR . P . .
H80B H 1.1073 0.3444 0.7810 0.129 Uiso 0.5 1 calc GR . P . .
H80C H 1.0593 0.2959 0.6901 0.129 Uiso 0.5 1 calc DGR . P . .
O10 O 0.652(2) 0.330(2) 0.9135(19) 0.142(9) Uani 1 1 d . U . . .
C72 C 0.702(2) 0.2939(15) 0.9054(15) 0.084(7) Uani 1 1 d D U . . .
C73 C 0.6637(16) 0.1924(13) 0.8480(12) 0.057(5) Uani 1 1 d D U . . .
H73A H 0.6036 0.1536 0.8544 0.085 Uiso 1 1 calc GR . . . .
H73B H 0.7068 0.1723 0.8564 0.085 Uiso 1 1 calc GR . . . .
H73C H 0.6554 0.1840 0.7949 0.085 Uiso 1 1 calc GR . . . .
C74 C 0.771(3) 0.339(3) 0.980(2) 0.165(18) Uani 1 1 d D U . . .
H74A H 0.7455 0.3630 1.0241 0.247 Uiso 1 1 calc GR . . . .
H74B H 0.8279 0.3929 0.9836 0.247 Uiso 1 1 calc DGR . . . .
H74C H 0.7837 0.2924 0.9824 0.247 Uiso 1 1 calc GR . . . .
O11 O -0.106(3) -0.490(3) 0.424(3) 0.105(13) Uani 0.5 1 d . . P . .
C75 C -0.053(3) -0.397(3) 0.450(3) 0.067(12) Uani 0.5 1 d D U P . .
C76 C -0.012(5) -0.361(5) 0.397(4) 0.11(2) Uani 0.5 1 d D U P . .
H76A H 0.0372 -0.3749 0.3834 0.168 Uiso 0.5 1 calc GR . P . .
H76B H 0.0136 -0.2914 0.4225 0.168 Uiso 0.5 1 calc GR . P . .
H76C H -0.0606 -0.3915 0.3488 0.168 Uiso 0.5 1 calc DGR . P . .
C77 C -0.033(5) -0.340(5) 0.536(3) 0.12(2) Uani 0.5 1 d D U P . .
H77A H -0.0606 -0.2996 0.5478 0.185 Uiso 0.5 1 calc GR . P . .
H77B H 0.0347 -0.2991 0.5588 0.185 Uiso 0.5 1 calc GR . P . .
H77C H -0.0586 -0.3824 0.5585 0.185 Uiso 0.5 1 calc GR . P . .
O9 O 0.6245(14) 0.1762(14) 0.3633(13) 0.097(6) Uani 1 1 d . U . . .
C69 C 0.6813(19) 0.2565(19) 0.4152(17) 0.081(7) Uani 1 1 d D U . . .
C70 C 0.663(3) 0.336(3) 0.445(3) 0.135(14) Uani 1 1 d D U . . .
H70A H 0.7142 0.3913 0.4437 0.202 Uiso 1 1 calc GR . . . .
H70B H 0.6588 0.3545 0.4989 0.202 Uiso 1 1 calc GR . . . .
H70C H 0.6049 0.3167 0.4121 0.202 Uiso 1 1 calc GR . . . .
C71 C 0.775(2) 0.275(4) 0.443(3) 0.159(17) Uani 1 1 d D U . . .
H71A H 0.7722 0.2144 0.4290 0.238 Uiso 1 1 calc GR . . . .
H71B H 0.7977 0.3160 0.4998 0.238 Uiso 1 1 calc GR . . . .
H71C H 0.8181 0.3071 0.4180 0.238 Uiso 1 1 calc GR . . . .
I4B I 0.8762(9) 0.5659(7) 0.7873(10) 0.199(6) Uani 0.3333 1 d D . P B 2
I2B I 0.8052(12) 0.4061(14) 1.2274(13) 0.0849(7) Uani 0.1 1 d . . P A 2
C58B C 0.753(3) 0.3332(16) 0.708(3) 0.031(4) Uani 0.3333 1 d D . P B 2
C59B C 0.803(5) 0.4193(18) 0.737(5) 0.081(10) Uani 0.3333 1 d D . P B 2
C53B C 0.6788(14) 0.2311(15) 0.672(4) 0.052(7) Uani 0.3333 1 d D . P B 2
O13 O 1.060(4) 0.374(5) 0.911(4) 0.22(3) Uani 0.5 1 d D U P . .
C81 C 1.015(3) 0.335(3) 0.946(3) 0.14(3) Uani 0.5 1 d D U P . .
C82 C 0.913(3) 0.267(4) 0.914(4) 0.11(2) Uani 0.5 1 d D U P . .
H82A H 0.8932 0.2540 0.8605 0.159 Uiso 0.5 1 d R . P . .
H82B H 0.8875 0.3034 0.9487 0.159 Uiso 0.5 1 d DR . P . .
H82C H 0.8895 0.2061 0.9142 0.159 Uiso 0.5 1 d R . P . .
C83 C 1.059(5) 0.355(6) 1.024(4) 0.16(4) Uani 0.5 1 d D U P . .
H83A H 1.1142 0.3482 1.0207 0.243 Uiso 0.5 1 calc GR . P . .
H83B H 1.0146 0.3086 1.0380 0.243 Uiso 0.5 1 calc GR . P . .
H83C H 1.0771 0.4195 1.0636 0.243 Uiso 0.5 1 calc GR . P . .


_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
I1 C8 2.006(18) . ?
I2 C25 1.93(2) . ?
I3 C42 2.01(2) . ?
I4 C59 2.00(2) . ?
O1 C3 1.30(2) . ?
O1 C9 1.43(3) . ?
O2 C10 1.468(19) . ?
O2 C18 1.36(2) . ?
O3 C20 1.39(2) . ?
O3 C26 1.45(2) . ?
O4 C27 1.49(2) . ?
O4 C35 1.365(19) . ?
O5 C37 1.36(2) . ?
O5 C43 1.44(3) . ?
O6 C44 1.41(3) . ?
O6 C52 1.36(2) . ?
O7 C54 1.38(2) . ?
O7 C60 1.34(2) . ?
O8 C1 1.40(2) . ?
O8 C61 1.43(3) . ?
C1 C2 1.41(3) . ?
C1 C6 1.42(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C15 1.520(10) . ?
C16 C17 1.524(10) . ?
C2 C3 1.41(2) . ?
C2 C7 1.44(2) . ?
C3 C4 1.43(2) . ?
C4 C5 1.37(3) . ?
C4 C11 1.52(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.44(2) . ?
C6 C62 1.44(3) . ?
C7 C8 1.18(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.53(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11 0.9800 . ?
C11 C12 1.52(2) . ?
C11 C23 1.55(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.520(10) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.516(10) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.525(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.41(2) . ?
C18 C23 1.42(2) . ?
C19 C20 1.40(2) . ?
C19 C24 1.43(2) . ?
C20 C21 1.38(2) . ?
C21 C22 1.38(2) . ?
C21 C28 1.52(2) . ?
C22 H22 0.9300 . ?
C22 C23 1.36(2) . ?
C24 C25 1.23(3) . ?
C25 I2B 1.96(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.53(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28 0.9800 . ?
C28 C29 1.53(2) . ?
C28 C40 1.49(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.519(10) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.518(10) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.526(10) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.522(10) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.525(10) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9601 . ?
C34 H34C 0.9602 . ?
C35 C36 1.40(3) . ?
C35 C40 1.39(2) . ?
C36 C37 1.43(2) . ?
C36 C41 1.43(3) . ?
C37 C38 1.39(3) . ?
C38 C39 1.38(3) . ?
C38 C45 1.58(3) . ?
C39 H39 0.9300 . ?
C39 C40 1.37(2) . ?
C41 C42 1.18(3) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C44 1.54(3) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 H45 0.9800 . ?
C45 C46 1.53(3) . ?
C45 C57 1.50(3) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 C47 1.518(10) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 C48 1.518(10) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 C49 1.526(10) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 C50 1.519(10) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C50 C51 1.522(10) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 C53 1.398(17) . ?
C52 C57 1.43(3) . ?
C52 C53B 1.416(18) . ?
C53 C54 1.398(18) . ?
C53 C58 1.44(2) . ?
C54 C55 1.44(3) . ?
C54 C53B 1.414(18) . ?
C55 C56 1.42(3) . ?
C55 C62 1.52(3) . ?
C56 H56 0.9300 . ?
C56 C57 1.36(3) . ?
C58 C59 1.18(2) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C60 C61 1.54(3) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 H62 0.9800 . ?
C62 C63 1.53(3) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 C64 1.518(10) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C64 C65 1.514(10) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C65 C66 1.525(10) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C66 C67 1.515(10) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C67 C68 1.523(10) . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C79 H79A 0.9600 . ?
C79 H79B 0.9600 . ?
C79 H79C 0.9600 . ?
C79 C78 1.455(19) . ?
C78 O12 1.32(7) . ?
C78 C80 1.451(19) . ?
C80 H80A 0.9600 . ?
C80 H80B 0.9600 . ?
C80 H80C 0.9600 . ?
O10 C72 1.22(3) . ?
C72 C73 1.445(17) . ?
C72 C74 1.453(18) . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
O11 C75 1.29(6) . ?
C75 C76 1.454(19) . ?
C75 C77 1.452(19) . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?
O9 C69 1.20(3) . ?
C69 C70 1.446(18) . ?
C69 C71 1.458(18) . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C71 H71A 0.9600 . ?
C71 H71B 0.9600 . ?
C71 H71C 0.9600 . ?
I4B C59B 2.01(2) . ?
C58B C59B 1.19(3) . ?
C58B C53B 1.46(2) . ?
O13 C81 1.19(2) . ?
C81 C82 1.467(15) . ?
C81 C83 1.467(14) . ?
C82 H82A 0.9603 . ?
C82 H82B 0.9601 . ?
C82 H82C 0.9595 . ?
C83 H83A 0.9600 . ?
C83 H83B 0.9600 . ?
C83 H83C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 O1 C9 116.2(16) . . ?
C18 O2 C10 116.7(13) . . ?
C20 O3 C26 115.1(14) . . ?
C35 O4 C27 116.6(13) . . ?
C37 O5 C43 115.6(16) . . ?
C52 O6 C44 113.3(19) . . ?
C60 O7 C54 110.8(15) . . ?
C1 O8 C61 117.9(16) . . ?
O8 C1 C2 119.8(16) . . ?
O8 C1 C6 116.1(17) . . ?
C2 C1 C6 124.1(15) . . ?
H16A C16 H16B 109.6 . . ?
C15 C16 H16A 112.0 . . ?
C15 C16 H16B 112.0 . . ?
C15 C16 C17 99(4) . . ?
C17 C16 H16A 112.0 . . ?
C17 C16 H16B 112.0 . . ?
C1 C2 C3 120.5(15) . . ?
C1 C2 C7 121.1(16) . . ?
C3 C2 C7 117.9(17) . . ?
O1 C3 C2 122.3(16) . . ?
O1 C3 C4 119.9(14) . . ?
C2 C3 C4 117.7(15) . . ?
C3 C4 C11 119.8(15) . . ?
C5 C4 C3 118.7(14) . . ?
C5 C4 C11 121.4(15) . . ?
C4 C5 H5 116.5 . . ?
C4 C5 C6 127.0(17) . . ?
C6 C5 H5 116.5 . . ?
C1 C6 C5 111.6(18) . . ?
C1 C6 C62 124.3(16) . . ?
C5 C6 C62 123.8(17) . . ?
C8 C7 C2 178(2) . . ?
C7 C8 I1 176(2) . . ?
O1 C9 H9A 108.8 . . ?
O1 C9 H9B 108.8 . . ?
O1 C9 C10 113.8(18) . . ?
H9A C9 H9B 107.7 . . ?
C10 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
O2 C10 C9 106.8(14) . . ?
O2 C10 H10A 110.4 . . ?
O2 C10 H10B 110.4 . . ?
C9 C10 H10A 110.4 . . ?
C9 C10 H10B 110.4 . . ?
H10A C10 H10B 108.6 . . ?
C4 C11 H11 107.0 . . ?
C4 C11 C12 112.5(14) . . ?
C4 C11 C23 109.5(13) . . ?
C12 C11 H11 107.0 . . ?
C12 C11 C23 113.4(14) . . ?
C23 C11 H11 107.0 . . ?
C11 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?
C13 C12 C11 111.8(16) . . ?
C13 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C12 C13 H13A 108.2 . . ?
C12 C13 H13B 108.2 . . ?
H13A C13 H13B 107.3 . . ?
C14 C13 C12 117(2) . . ?
C14 C13 H13A 108.2 . . ?
C14 C13 H13B 108.2 . . ?
C13 C14 H14A 110.6 . . ?
C13 C14 H14B 110.6 . . ?
C13 C14 C15 106(3) . . ?
H14A C14 H14B 108.7 . . ?
C15 C14 H14A 110.6 . . ?
C15 C14 H14B 110.6 . . ?
C16 C15 C14 121(4) . . ?
C16 C15 H15A 107.1 . . ?
C16 C15 H15B 107.1 . . ?
C14 C15 H15A 107.1 . . ?
C14 C15 H15B 107.1 . . ?
H15A C15 H15B 106.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C18 C19 119.9(15) . . ?
O2 C18 C23 119.1(14) . . ?
C19 C18 C23 120.9(15) . . ?
C18 C19 C24 121.3(15) . . ?
C20 C19 C18 116.6(15) . . ?
C20 C19 C24 122.1(15) . . ?
O3 C20 C19 116.9(16) . . ?
C21 C20 O3 119.1(16) . . ?
C21 C20 C19 123.8(16) . . ?
C20 C21 C22 116.0(15) . . ?
C20 C21 C28 120.2(15) . . ?
C22 C21 C28 123.8(15) . . ?
C21 C22 H22 117.5 . . ?
C23 C22 C21 125.0(16) . . ?
C23 C22 H22 117.5 . . ?
C18 C23 C11 117.9(14) . . ?
C22 C23 C11 124.6(14) . . ?
C22 C23 C18 117.5(14) . . ?
C25 C24 C19 178.2(18) . . ?
C24 C25 I2 173.7(18) . . ?
C24 C25 I2B 158.1(19) . . ?
O3 C26 H26A 110.2 . . ?
O3 C26 H26B 110.2 . . ?
O3 C26 C27 107.5(15) . . ?
H26A C26 H26B 108.5 . . ?
C27 C26 H26A 110.2 . . ?
C27 C26 H26B 110.2 . . ?
O4 C27 C26 113.2(14) . . ?
O4 C27 H27A 108.9 . . ?
O4 C27 H27B 108.9 . . ?
C26 C27 H27A 108.9 . . ?
C26 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C21 C28 H28 106.0 . . ?
C21 C28 C29 114.1(14) . . ?
C29 C28 H28 106.0 . . ?
C40 C28 C21 111.4(13) . . ?
C40 C28 H28 106.0 . . ?
C40 C28 C29 112.6(16) . . ?
C28 C29 H29A 108.9 . . ?
C28 C29 H29B 108.9 . . ?
H29A C29 H29B 107.8 . . ?
C30 C29 C28 113.2(16) . . ?
C30 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C29 C30 H30A 107.8 . . ?
C29 C30 H30B 107.8 . . ?
H30A C30 H30B 107.2 . . ?
C31 C30 C29 118(2) . . ?
C31 C30 H30A 107.8 . . ?
C31 C30 H30B 107.8 . . ?
C30 C31 H31A 109.8 . . ?
C30 C31 H31B 109.8 . . ?
C30 C31 C32 109(3) . . ?
H31A C31 H31B 108.3 . . ?
C32 C31 H31A 109.8 . . ?
C32 C31 H31B 109.8 . . ?
C31 C32 H32A 102.3 . . ?
C31 C32 H32B 102.3 . . ?
H32A C32 H32B 104.9 . . ?
C33 C32 C31 139(4) . . ?
C33 C32 H32A 102.3 . . ?
C33 C32 H32B 102.3 . . ?
C32 C33 H33A 112.2 . . ?
C32 C33 H33B 112.2 . . ?
C32 C33 C34 98(4) . . ?
H33A C33 H33B 109.8 . . ?
C34 C33 H33A 112.2 . . ?
C34 C33 H33B 112.2 . . ?
C33 C34 H34A 109.4 . . ?
C33 C34 H34B 109.7 . . ?
C33 C34 H34C 109.3 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O4 C35 C36 118.8(15) . . ?
O4 C35 C40 119.9(15) . . ?
C40 C35 C36 121.2(15) . . ?
C35 C36 C37 119.1(17) . . ?
C35 C36 C41 121.8(18) . . ?
C41 C36 C37 119(2) . . ?
O5 C37 C36 121.0(17) . . ?
O5 C37 C38 119.5(16) . . ?
C38 C37 C36 119.2(17) . . ?
C37 C38 C45 119.5(18) . . ?
C39 C38 C37 119.0(16) . . ?
C39 C38 C45 121.4(17) . . ?
C38 C39 H39 118.2 . . ?
C40 C39 C38 123.6(17) . . ?
C40 C39 H39 118.2 . . ?
C35 C40 C28 121.2(14) . . ?
C39 C40 C28 121.0(15) . . ?
C39 C40 C35 117.8(16) . . ?
C42 C41 C36 173(3) . . ?
C41 C42 I3 179(3) . . ?
O5 C43 H43A 109.3 . . ?
O5 C43 H43B 109.3 . . ?
O5 C43 C44 111.8(18) . . ?
H43A C43 H43B 107.9 . . ?
C44 C43 H43A 109.3 . . ?
C44 C43 H43B 109.3 . . ?
O6 C44 C43 109(2) . . ?
O6 C44 H44A 109.9 . . ?
O6 C44 H44B 109.9 . . ?
C43 C44 H44A 109.9 . . ?
C43 C44 H44B 109.9 . . ?
H44A C44 H44B 108.3 . . ?
C38 C45 H45 108.0 . . ?
C46 C45 C38 110.4(17) . . ?
C46 C45 H45 108.0 . . ?
C57 C45 C38 109.4(15) . . ?
C57 C45 H45 108.0 . . ?
C57 C45 C46 112.8(17) . . ?
C45 C46 H46A 107.9 . . ?
C45 C46 H46B 107.9 . . ?
H46A C46 H46B 107.2 . . ?
C47 C46 C45 118(2) . . ?
C47 C46 H46A 107.9 . . ?
C47 C46 H46B 107.9 . . ?
C46 C47 H47A 110.3 . . ?
C46 C47 H47B 110.3 . . ?
H47A C47 H47B 108.6 . . ?
C48 C47 C46 107(2) . . ?
C48 C47 H47A 110.3 . . ?
C48 C47 H47B 110.3 . . ?
C47 C48 H48A 108.7 . . ?
C47 C48 H48B 108.7 . . ?
C47 C48 C49 114(3) . . ?
H48A C48 H48B 107.6 . . ?
C49 C48 H48A 108.7 . . ?
C49 C48 H48B 108.7 . . ?
C48 C49 H49A 107.3 . . ?
C48 C49 H49B 107.3 . . ?
H49A C49 H49B 106.9 . . ?
C50 C49 C48 120(4) . . ?
C50 C49 H49A 107.3 . . ?
C50 C49 H49B 107.3 . . ?
C49 C50 H50A 107.5 . . ?
C49 C50 H50B 107.5 . . ?
C49 C50 C51 119(5) . . ?
H50A C50 H50B 107.0 . . ?
C51 C50 H50A 107.5 . . ?
C51 C50 H50B 107.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O6 C52 C53 120.5(18) . . ?
O6 C52 C57 118.3(16) . . ?
O6 C52 C53B 120.0(19) . . ?
C53 C52 C57 119.7(17) . . ?
C53B C52 C57 121(2) . . ?
C52 C53 C54 119.6(18) . . ?
C52 C53 C58 119.4(17) . . ?
C54 C53 C58 117.7(16) . . ?
O7 C54 C53 120.2(17) . . ?
O7 C54 C55 118.3(16) . . ?
O7 C54 C53B 120.6(18) . . ?
C53 C54 C55 118.4(16) . . ?
C53B C54 C55 121.0(17) . . ?
C54 C55 C62 119.8(16) . . ?
C56 C55 C54 115.8(17) . . ?
C56 C55 C62 124.3(17) . . ?
C55 C56 H56 117.4 . . ?
C57 C56 C55 125.1(18) . . ?
C57 C56 H56 117.4 . . ?
C52 C57 C45 119.2(17) . . ?
C56 C57 C45 123.8(18) . . ?
C56 C57 C52 116.9(17) . . ?
C59 C58 C53 171(3) . . ?
C58 C59 I4 168(4) . . ?
O7 C60 H60A 110.0 . . ?
O7 C60 H60B 110.0 . . ?
O7 C60 C61 108.5(18) . . ?
H60A C60 H60B 108.4 . . ?
C61 C60 H60A 110.0 . . ?
C61 C60 H60B 110.0 . . ?
O8 C61 C60 111.3(17) . . ?
O8 C61 H61A 109.4 . . ?
O8 C61 H61B 109.4 . . ?
C60 C61 H61A 109.4 . . ?
C60 C61 H61B 109.4 . . ?
H61A C61 H61B 108.0 . . ?
C6 C62 C55 110.0(16) . . ?
C6 C62 H62 106.6 . . ?
C6 C62 C63 114.5(18) . . ?
C55 C62 H62 106.6 . . ?
C55 C62 C63 112.0(17) . . ?
C63 C62 H62 106.6 . . ?
C62 C63 H63A 105.8 . . ?
C62 C63 H63B 105.8 . . ?
H63A C63 H63B 106.2 . . ?
C64 C63 C62 126(2) . . ?
C64 C63 H63A 105.8 . . ?
C64 C63 H63B 105.8 . . ?
C63 C64 H64A 109.3 . . ?
C63 C64 H64B 109.3 . . ?
H64A C64 H64B 107.9 . . ?
C65 C64 C63 112(2) . . ?
C65 C64 H64A 109.3 . . ?
C65 C64 H64B 109.3 . . ?
C64 C65 H65A 109.6 . . ?
C64 C65 H65B 109.6 . . ?
C64 C65 C66 110(3) . . ?
H65A C65 H65B 108.2 . . ?
C66 C65 H65A 109.6 . . ?
C66 C65 H65B 109.6 . . ?
C65 C66 H66A 109.2 . . ?
C65 C66 H66B 109.2 . . ?
H66A C66 H66B 107.9 . . ?
C67 C66 C65 112(3) . . ?
C67 C66 H66A 109.2 . . ?
C67 C66 H66B 109.2 . . ?
C66 C67 H67A 110.2 . . ?
C66 C67 H67B 110.2 . . ?
C66 C67 C68 108(3) . . ?
H67A C67 H67B 108.5 . . ?
C68 C67 H67A 110.2 . . ?
C68 C67 H67B 110.2 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
O12 C78 C79 133(4) . . ?
O12 C78 C80 120(4) . . ?
C80 C78 C79 102(4) . . ?
C78 C80 H80A 109.5 . . ?
C78 C80 H80B 109.5 . . ?
C78 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
O10 C72 C73 120(3) . . ?
O10 C72 C74 111(3) . . ?
C73 C72 C74 121(3) . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C72 C74 H74A 109.5 . . ?
C72 C74 H74B 109.5 . . ?
C72 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
O11 C75 C76 120(5) . . ?
O11 C75 C77 113(5) . . ?
C77 C75 C76 126(6) . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76B 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C77 H77A 109.5 . . ?
C75 C77 H77B 109.5 . . ?
C75 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
O9 C69 C70 123(3) . . ?
O9 C69 C71 117(3) . . ?
C70 C69 C71 120(3) . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C69 C71 H71A 109.5 . . ?
C69 C71 H71B 109.5 . . ?
C69 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C59B C58B C53B 170(6) . . ?
C58B C59B I4B 174(7) . . ?
C52 C53B C58B 124(2) . . ?
C54 C53B C52 117.2(18) . . ?
C54 C53B C58B 119(2) . . ?
O13 C81 C82 121.4(15) . . ?
O13 C81 C83 121.7(16) . . ?
C83 C81 C82 117(2) . . ?
C81 C82 H82A 109.6 . . ?
C81 C82 H82B 102.3 . . ?
C81 C82 H82C 116.2 . . ?
H82A C82 H82B 109.4 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C3 C4 C5 174.8(16) . . . . ?
O1 C3 C4 C11 -2(2) . . . . ?
O1 C9 C10 O2 -60(2) . . . . ?
O2 C18 C19 C20 175.9(14) . . . . ?
O2 C18 C19 C24 -5(2) . . . . ?
O2 C18 C23 C11 3(2) . . . . ?
O2 C18 C23 C22 -178.0(14) . . . . ?
O3 C20 C21 C22 176.2(15) . . . . ?
O3 C20 C21 C28 -7(2) . . . . ?
O3 C26 C27 O4 60(2) . . . . ?
O4 C35 C36 C37 175.0(15) . . . . ?
O4 C35 C36 C41 -1(3) . . . . ?
O4 C35 C40 C28 2(2) . . . . ?
O4 C35 C40 C39 -176.3(15) . . . . ?
O5 C37 C38 C39 174.8(16) . . . . ?
O5 C37 C38 C45 -2(3) . . . . ?
O5 C43 C44 O6 -62(3) . . . . ?
O6 C52 C53 C54 -171(2) . . . . ?
O6 C52 C53 C58 -13(4) . . . . ?
O6 C52 C57 C45 1(3) . . . . ?
O6 C52 C57 C56 -175(2) . . . . ?
O6 C52 C53B C54 168(4) . . . . ?
O6 C52 C53B C58B -9(8) . . . . ?
O7 C54 C55 C56 175.6(19) . . . . ?
O7 C54 C55 C62 -8(3) . . . . ?
O7 C54 C53B C52 -165(4) . . . . ?
O7 C54 C53B C58B 12(8) . . . . ?
O7 C60 C61 O8 65(2) . . . . ?
O8 C1 C2 C3 174.1(16) . . . . ?
O8 C1 C2 C7 3(3) . . . . ?
O8 C1 C6 C5 -176.8(15) . . . . ?
O8 C1 C6 C62 -3(3) . . . . ?
C1 O8 C61 C60 54(3) . . . . ?
C1 C2 C3 O1 -171.4(17) . . . . ?
C1 C2 C3 C4 6(2) . . . . ?
C1 C6 C62 C55 107(2) . . . . ?
C1 C6 C62 C63 -125(2) . . . . ?
C2 C1 C6 C5 5(3) . . . . ?
C2 C1 C6 C62 178.2(18) . . . . ?
C2 C3 C4 C5 -3(2) . . . . ?
C2 C3 C4 C11 -179.1(15) . . . . ?
C3 O1 C9 C10 -53(2) . . . . ?
C3 C4 C5 C6 0(3) . . . . ?
C3 C4 C11 C12 126.3(17) . . . . ?
C3 C4 C11 C23 -106.7(17) . . . . ?
C4 C5 C6 C1 -1(3) . . . . ?
C4 C5 C6 C62 -174.8(17) . . . . ?
C4 C11 C12 C13 -62(2) . . . . ?
C4 C11 C23 C18 83.9(18) . . . . ?
C4 C11 C23 C22 -95.5(18) . . . . ?
C5 C4 C11 C12 -50(2) . . . . ?
C5 C4 C11 C23 76.9(19) . . . . ?
C5 C6 C62 C55 -80(2) . . . . ?
C5 C6 C62 C63 48(3) . . . . ?
C6 C1 C2 C3 -7(3) . . . . ?
C6 C1 C2 C7 -178.4(19) . . . . ?
C6 C62 C63 C64 54(3) . . . . ?
C7 C2 C3 O1 0(3) . . . . ?
C7 C2 C3 C4 177.4(16) . . . . ?
C9 O1 C3 C2 -76(2) . . . . ?
C9 O1 C3 C4 106.8(18) . . . . ?
C10 O2 C18 C19 85.5(18) . . . . ?
C10 O2 C18 C23 -96.2(17) . . . . ?
C11 C4 C5 C6 176.7(16) . . . . ?
C11 C12 C13 C14 -164(3) . . . . ?
C12 C11 C23 C18 -149.5(15) . . . . ?
C12 C11 C23 C22 31(2) . . . . ?
C12 C13 C14 C15 173(3) . . . . ?
C13 C14 C15 C16 -84(6) . . . . ?
C17 C16 C15 C14 -163(5) . . . . ?
C18 O2 C10 C9 136.8(17) . . . . ?
C18 C19 C20 O3 -173.0(14) . . . . ?
C18 C19 C20 C21 1(3) . . . . ?
C19 C18 C23 C11 -179.2(14) . . . . ?
C19 C18 C23 C22 0(2) . . . . ?
C19 C20 C21 C22 2(3) . . . . ?
C19 C20 C21 C28 178.7(16) . . . . ?
C20 O3 C26 C27 -135.9(16) . . . . ?
C20 C21 C22 C23 -4(2) . . . . ?
C20 C21 C28 C29 149.3(16) . . . . ?
C20 C21 C28 C40 -81.8(19) . . . . ?
C21 C22 C23 C11 -177.2(14) . . . . ?
C21 C22 C23 C18 3(2) . . . . ?
C21 C28 C29 C30 -170.7(18) . . . . ?
C21 C28 C40 C35 105.9(17) . . . . ?
C21 C28 C40 C39 -76(2) . . . . ?
C22 C21 C28 C29 -34(2) . . . . ?
C22 C21 C28 C40 94.6(18) . . . . ?
C23 C11 C12 C13 172.8(16) . . . . ?
C23 C18 C19 C20 -2(2) . . . . ?
C23 C18 C19 C24 176.3(15) . . . . ?
C24 C19 C20 O3 8(2) . . . . ?
C24 C19 C20 C21 -177.5(16) . . . . ?
C26 O3 C20 C19 -88(2) . . . . ?
C26 O3 C20 C21 98(2) . . . . ?
C27 O4 C35 C36 78(2) . . . . ?
C27 O4 C35 C40 -104.6(18) . . . . ?
C28 C21 C22 C23 179.0(15) . . . . ?
C28 C29 C30 C31 151(3) . . . . ?
C29 C28 C40 C35 -124.3(16) . . . . ?
C29 C28 C40 C39 54(2) . . . . ?
C29 C30 C31 C32 -168(3) . . . . ?
C30 C31 C32 C33 63(8) . . . . ?
C31 C32 C33 C34 -174(6) . . . . ?
C35 O4 C27 C26 52(2) . . . . ?
C35 C36 C37 O5 -172.9(16) . . . . ?
C35 C36 C37 C38 2(3) . . . . ?
C36 C35 C40 C28 179.1(16) . . . . ?
C36 C35 C40 C39 1(3) . . . . ?
C36 C37 C38 C39 0(3) . . . . ?
C36 C37 C38 C45 -176.7(16) . . . . ?
C37 O5 C43 C44 -56(2) . . . . ?
C37 C38 C39 C40 -2(3) . . . . ?
C37 C38 C45 C46 129(2) . . . . ?
C37 C38 C45 C57 -106(2) . . . . ?
C38 C39 C40 C28 -177.1(17) . . . . ?
C38 C39 C40 C35 1(3) . . . . ?
C38 C45 C46 C47 -46(3) . . . . ?
C38 C45 C57 C52 86(2) . . . . ?
C38 C45 C57 C56 -97(2) . . . . ?
C39 C38 C45 C46 -48(2) . . . . ?
C39 C38 C45 C57 77(2) . . . . ?
C40 C28 C29 C30 61(2) . . . . ?
C40 C35 C36 C37 -2(3) . . . . ?
C40 C35 C36 C41 -178.6(18) . . . . ?
C41 C36 C37 O5 4(3) . . . . ?
C41 C36 C37 C38 178.0(18) . . . . ?
C43 O5 C37 C36 -79(2) . . . . ?
C43 O5 C37 C38 106(2) . . . . ?
C44 O6 C52 C53 100(2) . . . . ?
C44 O6 C52 C57 -94(2) . . . . ?
C44 O6 C52 C53B 79(4) . . . . ?
C45 C38 C39 C40 175.3(17) . . . . ?
C45 C46 C47 C48 -64(4) . . . . ?
C46 C45 C57 C52 -150(2) . . . . ?
C46 C45 C57 C56 26(3) . . . . ?
C46 C47 C48 C49 -166(3) . . . . ?
C47 C48 C49 C50 -53(7) . . . . ?
C48 C49 C50 C51 -167(5) . . . . ?
C52 O6 C44 C43 138.0(19) . . . . ?
C52 C53 C54 O7 174(2) . . . . ?
C52 C53 C54 C55 -26(3) . . . . ?
C53 C52 C57 C45 168(2) . . . . ?
C53 C52 C57 C56 -9(3) . . . . ?
C53 C54 C55 C56 15(3) . . . . ?
C53 C54 C55 C62 -168(2) . . . . ?
C54 O7 C60 C61 -139.6(16) . . . . ?
C54 C55 C56 C57 -2(3) . . . . ?
C54 C55 C62 C6 -81(2) . . . . ?
C54 C55 C62 C63 150.6(18) . . . . ?
C55 C54 C53B C52 17(7) . . . . ?
C55 C54 C53B C58B -167(4) . . . . ?
C55 C56 C57 C45 -177(2) . . . . ?
C55 C56 C57 C52 -1(4) . . . . ?
C55 C62 C63 C64 -179(2) . . . . ?
C56 C55 C62 C6 95(2) . . . . ?
C56 C55 C62 C63 -33(3) . . . . ?
C57 C45 C46 C47 -169(2) . . . . ?
C57 C52 C53 C54 23(4) . . . . ?
C57 C52 C53 C58 -179(2) . . . . ?
C57 C52 C53B C54 -20(7) . . . . ?
C57 C52 C53B C58B 164(5) . . . . ?
C58 C53 C54 O7 15(4) . . . . ?
C58 C53 C54 C55 175(2) . . . . ?
C60 O7 C54 C53 -103(2) . . . . ?
C60 O7 C54 C55 97(2) . . . . ?
C60 O7 C54 C53B -82(4) . . . . ?
C61 O8 C1 C2 77(2) . . . . ?
C61 O8 C1 C6 -102(2) . . . . ?
C62 C55 C56 C57 -179(2) . . . . ?
C62 C63 C64 C65 44(4) . . . . ?
C63 C64 C65 C66 176(3) . . . . ?
C64 C65 C66 C67 69(5) . . . . ?
C65 C66 C67 C68 173(4) . . . . ?
C53B C52 C57 C45 -171(4) . . . . ?
C53B C52 C57 C56 12(5) . . . . ?
C53B C54 C55 C56 -6(4) . . . . ?
C53B C54 C55 C62 171(4) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
8 -11 4 0.1356 7.5020 -10.9861 4.0009 0.1501 0.6777 -0.7334
-7 10 -7 0.1202 -6.9878 9.9811 -7.0048 -0.1713 -0.8431 0.4503
-6 9 4 0.1253 -6.0324 9.0022 4.0082 -0.0248 -0.0800 1.0684
1 -1 -10 0.1528 0.5441 -1.0180 -10.0127 -0.1272 -0.6137 -0.7341
-3 5 -12 0.0010 -3.4576 4.9747 -12.0131 -0.2144 -0.9659 -0.3226
0 -1 11 0.0824 0.4545 -0.9788 11.0137 0.1908 0.7311 0.6191
1 -1 -11 0.2100 0.5483 -1.0199 -11.0140 -0.1423 -0.6777 -0.7986
-7 11 -5 0.1033 -7.4977 10.9842 -5.0022 -0.1653 -0.7418 0.6689
0 -1 11 0.1358 0.4545 -0.9788 11.0137 0.1908 0.7311 0.6191
6 -10 9 0.1636 6.4783 -9.9772 9.0080 0.2459 0.9393 -0.3204

_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_2_dmf
_database_code_depnum_ccdc_archive 'CCDC 1556030'
_audit_update_record             
;
2017-06-14 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_2_dmf               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The structure contains large amount of disorder, which
causes the low resolution of the diffraction experiment.
;
_vrf_PLAT601_2_dmf               
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        211 Ang3  
RESPONSE: The large voids involve disordered solvent molecules,
however, no model was assigned due to the bad disorder.
;
_vrf_PLAT234_2_dmf               
;
PROBLEM: Large Hirshfeld Difference C35    --  C36     ..       0.26 Ang.  
RESPONSE: The relevant atoms belong to the disordered hexyl group.
;
_vrf_PLAT241_2_dmf               
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C32 Check 
RESPONSE: The atoms with high Ueq are resulted from the disorder and 
no split was treated for them.
;
_vrf_PLAT242_2_dmf               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C31 Check 
RESPONSE: The neigboring atoms are disordered with relatively high
Ueq.
;
_vrf_PLAT342_2_dmf               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02239 Ang.  
RESPONSE: Large amount disorder exists in the strucutre.
;
# end Validation Reply Form

_audit_creation_date             2017-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C64 H68 I4 O8, 2.5(C3 H7 N O), C1.5 H5.5 N0.5 O0.5'
_chemical_formula_sum            'C73 H91 I4 N3 O11'
_chemical_formula_weight         1694.08
_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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.1144(11)
_cell_length_b                   22.3258(17)
_cell_length_c                   17.2116(6)
_cell_angle_alpha                90
_cell_angle_beta                 101.036(4)
_cell_angle_gamma                90
_cell_volume                     8340.6(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4953
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      61.1780
_cell_measurement_theta_min      3.5790
_shelx_estimated_absorpt_T_max   0.529
_shelx_estimated_absorpt_T_min   0.281
_exptl_absorpt_coefficient_mu    12.147
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11003
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        59.997
_diffrn_reflns_theta_max         59.997
_diffrn_reflns_theta_min         3.588
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4268
_reflns_number_total             6292
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.740
_refine_diff_density_min         -1.840
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         6292
_refine_ls_number_restraints     179
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.1010
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1931P)²+60.7294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2903
_refine_ls_wR_factor_ref         0.3324
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2A-N1 = C3A-N1 = C10-C21 = N2-C39 = N3-C43B = N3-C43 = N3B-C43B = N3B-C44B =
 N3-C44
 1.45 with sigma of 0.01
 C1A-N1
 1.32 with sigma of 0.01
 C1A-O5 = C37-O6
 1.23 with sigma of 0.01
 C19-C20
 1.2 with sigma of 0.01
 C29-C30 = C35-C36 = C29B-C30B
 1.54 with sigma of 0.01
 C33-C34 = C27-C28B = C31-C32 = C32-C33 = C34-C35 = C5-C25 = C26-C27 = C27-C28
 = C28-C29 = C28B-C29B
 1.52 with sigma of 0.01
 N1-O5
 2.3 with sigma of 0.01
 H34A_$1-H28D
 2.2 with sigma of 0.04
 C28-C30 = C26-C28 = C26-C28B = C31-C33 = C27-C29
 2.62 with sigma of 0.01
 H32A-H29C_$1
 2.2 with sigma of 0.04
 H34B-H36C
 2.2 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(N3B) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(O7)
\\sim Ueq, Uanis(C43B) \\sim Ueq, Uanis(C44B) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C28B) \\sim Ueq, Uanis(C29B) \\sim Ueq,
Uanis(C30B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C27) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3A) = Uanis(C2A)
Uanis(C44) = Uanis(N3)
Uanis(C43) = Uanis(C43B)
Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35)
4. Others
 Fixed Sof: H27A(0.6) H27B(0.6) H27C(0.4) H27D(0.4) C28(0.6) H28A(0.6)
 H28B(0.6) C28B(0.4) H28C(0.4) H28D(0.4) C29(0.6) H29A(0.6) H29B(0.6) C29B(0.4)
 H29C(0.4) H29D(0.4) C30(0.6) H30A(0.6) H30B(0.6) H30C(0.6) C30B(0.4) H30D(0.4)
 H30E(0.4) H30F(0.4) H42A(0.5) H42(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
 C43B(0.5) H43D(0.5) H43E(0.5) H43F(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5)
 C44B(0.5) H44D(0.5) H44E(0.5) H44F(0.5) N3(0.5) N3B(0.5) C1A(0.25) H1A(0.25)
 C2A(0.25) H2AA(0.25) H2AB(0.5) H2AC(0.5) C3A(0.25) H3AA(0.25) H3AB(0.5)
 H3AC(0.5) N1(0.25) O5(0.25) C37(0.25) H37(0.25) C38(0.25) H38A(0.25)
 H38B(0.25) H38C(0.25) C39(0.25) H39A(0.25) H39B(0.25) H39C(0.25) N2(0.25)
 O6(0.25)
5.a Riding coordinates:
 C30B(H30D,H30E,H30F), C39(H39A,H39B,H39C)
5.b Ternary CH refined with riding coordinates:
 C5(H5), C12(H12)
5.c Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C27(H27C,H27D), C28(H28A,H28B), C28B(H28C,H28D), C29(H29A,H29B),
 C29B(H29C,H29D), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B)
5.d Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC)
5.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C14(H14), C42(H42A), C42(H42), C1A(H1A), C37(H37)
5.f Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C43B(H43D,H43E,H43F), C44(H44A,H44B,
 H44C), C44B(H44D,H44E,H44F), C38(H38A,H38B,H38C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.4105(7) 0.5000 0.0753(7) 0.074(4) Uani 1 2 d S T P . .
H1 H 0.3667 0.5000 0.0670 0.089 Uiso 1 2 calc RS T P . .
C2 C 0.4407(5) 0.5542(6) 0.0811(6) 0.079(3) Uani 1 1 d . . . . .
C3 C 0.5055(5) 0.5539(6) 0.0960(5) 0.073(3) Uani 1 1 d . . . . .
C4 C 0.5367(7) 0.5000 0.1058(7) 0.071(4) Uani 1 2 d S T P . .
C5 C 0.4066(5) 0.6140(7) 0.0752(6) 0.088(4) Uani 1 1 d D . . . .
H5 H 0.4331 0.6435 0.0535 0.106 Uiso 1 1 calc R . . . .
C6 C 0.4042(6) 0.6347(6) 0.1592(7) 0.090(4) Uani 1 1 d . . . . .
C7 C 0.3555(6) 0.6181(6) 0.1965(7) 0.089(3) Uani 1 1 d . . . . .
H7 H 0.3224 0.5952 0.1677 0.107 Uiso 1 1 calc R . . . .
C8 C 0.3540(6) 0.6340(6) 0.2740(7) 0.087(3) Uani 1 1 d . . . . .
C9 C 0.4042(6) 0.6649(6) 0.3151(7) 0.090(4) Uani 1 1 d . . . . .
C10 C 0.4547(6) 0.6805(6) 0.2818(7) 0.089(3) Uani 1 1 d D . . . .
C11 C 0.4537(6) 0.6663(6) 0.2039(6) 0.082(3) Uani 1 1 d . . . . .
C12 C 0.3027(7) 0.6151(8) 0.3167(9) 0.112(5) Uani 1 1 d . . . . .
H12 H 0.3001 0.6457 0.3583 0.134 Uiso 1 1 calc R . . . .
C13 C 0.3220(7) 0.5562(8) 0.3581(9) 0.101(4) Uani 1 1 d . . . . .
C14 C 0.3044(9) 0.5000 0.3226(12) 0.108(7) Uani 1 2 d S T P . .
H14 H 0.2790 0.5000 0.2714 0.130 Uiso 1 2 calc RS T P . .
C15 C 0.3815(10) 0.5000 0.4700(10) 0.101(6) Uani 1 2 d S T P . .
C16 C 0.3598(7) 0.5551(9) 0.4318(7) 0.109(5) Uani 1 1 d . . . . .
C17 C 0.5479(6) 0.6393(7) 0.1684(6) 0.089(4) Uani 1 1 d . . . . .
H17A H 0.5484 0.6117 0.2135 0.107 Uiso 1 1 calc R . . . .
H17B H 0.5886 0.6590 0.1754 0.107 Uiso 1 1 calc R . . . .
C18 C 0.4247(7) 0.6411(6) 0.4528(7) 0.096(4) Uani 1 1 d . . . . .
H18A H 0.4464 0.6618 0.5011 0.115 Uiso 1 1 calc R . . . .
H18B H 0.4545 0.6138 0.4349 0.115 Uiso 1 1 calc R . . . .
C19 C 0.6029(7) 0.5000 0.1284(9) 0.084(5) Uani 1 2 d DS T P . .
C20 C 0.6577(7) 0.5000 0.1511(9) 0.092(5) Uani 1 2 d DS T P . .
C21 C 0.5067(6) 0.7134(6) 0.3267(7) 0.096(4) Uani 1 1 d D U . . .
C22 C 0.5494(7) 0.7407(7) 0.3633(8) 0.102(4) Uani 1 1 d . . . . .
C23 C 0.4245(11) 0.5000 0.5438(11) 0.097(6) Uani 1 2 d S T P . .
C24 C 0.4609(10) 0.5000 0.6045(11) 0.095(5) Uani 1 2 d S T P . .
C25 C 0.3445(6) 0.6130(8) 0.0174(8) 0.113(5) Uani 1 1 d D . . . .
H25A H 0.3505 0.5971 -0.0343 0.135 Uiso 1 1 calc R . . . .
H25B H 0.3159 0.5859 0.0380 0.135 Uiso 1 1 calc R . . . .
C26 C 0.3164(8) 0.6747(8) 0.0057(10) 0.142(7) Uani 1 1 d D . . . .
H26A H 0.3477 0.7024 -0.0080 0.171 Uiso 1 1 calc R . . . .
H26B H 0.3069 0.6882 0.0568 0.171 Uiso 1 1 calc R . . . .
C27 C 0.2587(8) 0.6805(11) -0.0567(11) 0.187(10) Uani 1 1 d D U . . .
H27A H 0.2699 0.6713 -0.1085 0.225 Uiso 0.6 1 calc R . . A 1
H27B H 0.2460 0.7230 -0.0584 0.225 Uiso 0.6 1 calc R . . A 1
H27C H 0.2450 0.7227 -0.0565 0.225 Uiso 0.4 1 calc R . . B 2
H27D H 0.2265 0.6558 -0.0394 0.225 Uiso 0.4 1 calc R . . B 2
C28 C 0.2025(9) 0.6429(16) -0.0505(16) 0.169(14) Uani 0.6 1 d D U . C 1
H28A H 0.1847 0.6586 -0.0060 0.203 Uiso 0.6 1 calc R . . C 1
H28B H 0.2164 0.6015 -0.0368 0.203 Uiso 0.6 1 calc R . . C 1
C28B C 0.2592(18) 0.664(2) -0.1418(11) 0.21(3) Uani 0.4 1 d D U . C 2
H28C H 0.2577 0.6197 -0.1470 0.256 Uiso 0.4 1 calc R . . C 2
H28D H 0.2984 0.6777 -0.1555 0.256 Uiso 0.4 1 calc DR . . C 2
C29 C 0.1508(12) 0.6403(13) -0.124(2) 0.180(15) Uani 0.6 1 d D U . C 1
H29A H 0.1127 0.6260 -0.1078 0.217 Uiso 0.6 1 calc R . . C 1
H29B H 0.1622 0.6102 -0.1612 0.217 Uiso 0.6 1 calc R . . C 1
C29B C 0.2059(18) 0.691(2) -0.201(3) 0.163(19) Uani 0.4 1 d D U . C 2
H29C H 0.1993 0.7330 -0.1871 0.195 Uiso 0.4 1 calc DR . . C 2
H29D H 0.1675 0.6680 -0.1999 0.195 Uiso 0.4 1 calc R . . C 2
C30 C 0.136(2) 0.7001(16) -0.170(2) 0.194(17) Uani 0.6 1 d D U . C 1
H30A H 0.1028 0.6938 -0.2152 0.290 Uiso 0.6 1 calc R . . C 1
H30B H 0.1235 0.7300 -0.1343 0.290 Uiso 0.6 1 calc R . . C 1
H30C H 0.1730 0.7142 -0.1878 0.290 Uiso 0.6 1 calc R . . C 1
C30B C 0.224(4) 0.686(4) -0.282(4) 0.24(4) Uani 0.4 1 d D U . C 2
H30D H 0.2200 0.6436 -0.2954 0.354 Uiso 0.4 1 d R . . C 2
H30E H 0.2673 0.6983 -0.2766 0.354 Uiso 0.4 1 d R . . C 2
H30F H 0.1990 0.7096 -0.3251 0.354 Uiso 0.4 1 d R . . C 2
C31 C 0.2414(7) 0.6104(8) 0.2653(10) 0.120(5) Uani 1 1 d D U . . .
H31A H 0.2128 0.5923 0.2963 0.144 Uiso 1 1 calc R . . . .
H31B H 0.2444 0.5826 0.2213 0.144 Uiso 1 1 calc R . . . .
C32 C 0.2139(13) 0.6689(9) 0.2302(18) 0.241(7) Uani 1 1 d D . . . .
H32A H 0.2455 0.6900 0.2069 0.290 Uiso 1 1 calc DR . . . .
H32B H 0.2050 0.6941 0.2740 0.290 Uiso 1 1 calc R . . . .
C33 C 0.1551(13) 0.6650(13) 0.1670(17) 0.241(7) Uani 1 1 d D . . . .
H33A H 0.1674 0.6585 0.1153 0.290 Uiso 1 1 calc R . . . .
H33B H 0.1323 0.6288 0.1782 0.290 Uiso 1 1 calc R . . . .
C34 C 0.1107(13) 0.7170(13) 0.1579(18) 0.241(7) Uani 1 1 d D U . . .
H34A H 0.1324 0.7554 0.1543 0.290 Uiso 1 1 calc DR . . . .
H34B H 0.0887 0.7190 0.2027 0.290 Uiso 1 1 calc DR . . . .
C35 C 0.0665(14) 0.7031(16) 0.0807(17) 0.241(7) Uani 1 1 d D . . . .
H35A H 0.0860 0.6779 0.0450 0.290 Uiso 1 1 calc R . . . .
H35B H 0.0497 0.7399 0.0526 0.290 Uiso 1 1 calc R . . . .
C36 C 0.0173(13) 0.6686(16) 0.1146(18) 0.222(14) Uani 1 1 d D . . . .
H36A H 0.0373 0.6381 0.1518 0.333 Uiso 1 1 calc GR . . . .
H36B H -0.0112 0.6492 0.0714 0.333 Uiso 1 1 calc GR . . . .
H36C H -0.0055 0.6965 0.1422 0.333 Uiso 1 1 calc DGR . . . .
I1 I 0.74988(6) 0.5000 0.18427(10) 0.1378(7) Uani 1 2 d S T P . .
I2 I 0.61996(5) 0.78769(6) 0.42070(6) 0.1241(5) Uani 1 1 d . . . . .
I3 I 0.52257(7) 0.5000 0.70202(6) 0.0957(5) Uani 1 2 d S T P . .
O1 O 0.5381(4) 0.6054(4) 0.0967(4) 0.081(2) Uani 1 1 d . . . . .
O2 O 0.5025(5) 0.6831(4) 0.1694(4) 0.090(2) Uani 1 1 d . . . . .
O3 O 0.4052(5) 0.6838(4) 0.3936(5) 0.103(3) Uani 1 1 d . . . . .
O4 O 0.3761(5) 0.6072(5) 0.4718(5) 0.106(3) Uani 1 1 d . . . . .
C42 C 0.2439(11) 0.8621(13) 0.4530(15) 0.158(7) Uani 1 1 d . U . . .
H42A H 0.2065 0.8665 0.4719 0.190 Uiso 0.5 1 calc R . . D -1
H42 H 0.2290 0.8228 0.4400 0.190 Uiso 0.5 1 calc R . . E -2
C43 C 0.1860(19) 0.854(2) 0.3049(18) 0.152(12) Uani 0.5 1 d D . . F -1
H43A H 0.1589 0.8885 0.3060 0.228 Uiso 0.5 1 calc GR . . F -1
H43B H 0.1617 0.8170 0.3010 0.228 Uiso 0.5 1 calc GR . . F -1
H43C H 0.2062 0.8571 0.2591 0.228 Uiso 0.5 1 calc GR . . F -1
C43B C 0.1718(13) 0.8789(19) 0.3481(19) 0.152(12) Uani 0.5 1 d D U . G -2
H43D H 0.1615 0.8384 0.3634 0.228 Uiso 0.5 1 calc GR . . G -2
H43E H 0.1895 0.8767 0.3001 0.228 Uiso 0.5 1 calc GR . . G -2
H43F H 0.1345 0.9035 0.3378 0.228 Uiso 0.5 1 calc GR . . G -2
C44 C 0.272(2) 0.804(2) 0.362(3) 0.180(12) Uani 0.5 1 d D U . F -1
H44A H 0.2549 0.7849 0.3116 0.270 Uiso 0.5 1 calc GR . . F -1
H44B H 0.2746 0.7741 0.4049 0.270 Uiso 0.5 1 calc GR . . F -1
H44C H 0.3132 0.8193 0.3612 0.270 Uiso 0.5 1 calc GR . . F -1
C44B C 0.2361(18) 0.9674(13) 0.417(2) 0.151(14) Uani 0.5 1 d D U . G -2
H44D H 0.2713 0.9719 0.4607 0.226 Uiso 0.5 1 calc GR . . G -2
H44E H 0.2022 0.9930 0.4262 0.226 Uiso 0.5 1 calc GR . . G -2
H44F H 0.2484 0.9793 0.3673 0.226 Uiso 0.5 1 calc GR . . G -2
N3 N 0.2323(15) 0.853(2) 0.377(2) 0.180(12) Uani 0.5 1 d D U . F -1
N3B N 0.2161(14) 0.9053(14) 0.4114(17) 0.136(10) Uani 0.5 1 d D U . G -2
O7 O 0.2877(8) 0.8670(12) 0.5074(12) 0.227(9) Uani 1 1 d . U . . .
C1A C 0.2021(8) 0.5000 0.0503(12) 0.099(11) Uani 0.5 2 d DS TU P . .
H1A H 0.2160 0.5000 0.0014 0.119 Uiso 0.5 2 calc RS T P . .
C2A C 0.116(3) 0.5000 0.115(2) 0.151(14) Uani 0.5 2 d DS TU P . .
H2AA H 0.0706 0.5000 0.0999 0.226 Uiso 0.5 2 calc RS T P . .
H2AB H 0.1292 0.4642 0.1462 0.226 Uiso 0.5 1 calc R . . . .
H2AC H 0.1292 0.5358 0.1462 0.226 Uiso 0.5 1 calc R . . . .
C3A C 0.096(2) 0.5000 -0.028(2) 0.151(14) Uani 0.5 2 d DS T P . .
H3AA H 0.0551 0.5000 -0.0151 0.226 Uiso 0.5 2 calc RS T P . .
H3AB H 0.1015 0.5358 -0.0591 0.226 Uiso 0.5 1 calc R . . . .
H3AC H 0.1015 0.4642 -0.0591 0.226 Uiso 0.5 1 calc R . . . .
N1 N 0.1421(8) 0.5000 0.0440(17) 0.101(9) Uani 0.5 2 d DS T P . .
O5 O 0.2431(7) 0.5000 0.1090(9) 0.074(5) Uani 0.5 2 d DS T P . .
C37 C 0.385(3) 0.939(3) 0.297(3) 0.106(16) Uani 0.25 1 d D U . H -1
H37 H 0.3520 0.9362 0.3237 0.127 Uiso 0.25 1 calc R . . H -1
C38 C 0.434(3) 0.857(3) 0.382(4) 0.117(19) Uani 0.25 1 d . U . H -1
H38A H 0.3910 0.8436 0.3781 0.176 Uiso 0.25 1 calc GR . . H -1
H38B H 0.4501 0.8701 0.4362 0.176 Uiso 0.25 1 calc GR . . H -1
H38C H 0.4586 0.8235 0.3685 0.176 Uiso 0.25 1 calc GR . . H -1
C39 C 0.493(3) 0.892(5) 0.304(6) 0.18(3) Uani 0.25 1 d D U . H -1
H39A H 0.4800 0.8735 0.2513 0.263 Uiso 0.25 1 d R . . H -1
H39B H 0.5130 0.9302 0.2982 0.263 Uiso 0.25 1 d R . . H -1
H39C H 0.5227 0.8649 0.3368 0.263 Uiso 0.25 1 d R . . H -1
N2 N 0.436(3) 0.905(3) 0.328(4) 0.15(2) Uani 0.25 1 d D U . H -1
O6 O 0.3762(16) 0.973(2) 0.239(3) 0.138(16) Uani 0.25 1 d D U . H -1


_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 H1 0.9500 . ?
C1 C2 1.377(14) . ?
C1 C2 1.377(14) 6_565 ?
C2 C3 1.406(16) . ?
C2 C5 1.527(18) . ?
C3 C4 1.381(14) . ?
C3 O1 1.357(14) . ?
C4 C3 1.381(14) 6_565 ?
C4 C19 1.44(2) . ?
C5 H5 1.0000 . ?
C5 C6 1.530(17) . ?
C5 C25 1.534(9) . ?
C6 C7 1.405(19) . ?
C6 C11 1.402(19) . ?
C7 H7 0.9500 . ?
C7 C8 1.387(17) . ?
C8 C9 1.382(19) . ?
C8 C12 1.52(2) . ?
C9 C10 1.394(18) . ?
C9 O3 1.412(14) . ?
C10 C11 1.374(17) . ?
C10 C21 1.455(9) . ?
C11 O2 1.380(15) . ?
C12 H12 1.0000 . ?
C12 C13 1.52(2) . ?
C12 C31 1.47(2) . ?
C13 C14 1.416(18) . ?
C13 C16 1.38(2) . ?
C14 C13 1.416(18) 6_565 ?
C14 H14 0.9500 . ?
C15 C16 1.43(2) . ?
C15 C16 1.43(2) 6_565 ?
C15 C23 1.43(3) . ?
C16 O4 1.365(19) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 O1 1.427(14) . ?
C17 O2 1.403(16) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 O3 1.402(15) . ?
C18 O4 1.405(17) . ?
C19 C20 1.201(10) . ?
C20 I1 2.009(15) . ?
C21 C22 1.196(18) . ?
C22 I2 1.981(16) . ?
C23 C24 1.19(3) . ?
C24 I3 1.95(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.51(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.508(9) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 H27C 0.9900 . ?
C27 H27D 0.9900 . ?
C27 C28 1.520(10) . ?
C27 C28B 1.513(10) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.537(10) . ?
C28B H28C 0.9900 . ?
C28B H28D 0.9900 . ?
C28B C29B 1.521(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.548(10) . ?
C29B H29C 0.9900 . ?
C29B H29D 0.9900 . ?
C29B C30B 1.542(10) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9802 . ?
C30B H30F 0.9796 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.518(10) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.530(10) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.509(10) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.523(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.536(10) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C42 H42A 0.9500 . ?
C42 H42 0.9500 . ?
C42 N3 1.30(4) . ?
C42 N3B 1.29(4) . ?
C42 O7 1.22(3) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 N3 1.446(10) . ?
C43B H43D 0.9800 . ?
C43B H43E 0.9800 . ?
C43B H43F 0.9800 . ?
C43B N3B 1.445(10) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C44 N3 1.450(10) . ?
C44B H44D 0.9800 . ?
C44B H44E 0.9800 . ?
C44B H44F 0.9800 . ?
C44B N3B 1.453(10) . ?
C1A H1A 0.9500 . ?
C1A N1 1.312(10) . ?
C1A O5 1.221(10) . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2A N1 1.450(10) . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3A N1 1.443(10) . ?
C37 H37 0.9500 . ?
C37 N2 1.37(8) . ?
C37 O6 1.232(10) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C38 N2 1.43(9) . ?
C39 H39A 0.9807 . ?
C39 H39B 0.9802 . ?
C39 H39C 0.9805 . ?
C39 N2 1.448(10) . ?

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 H1 118.5 . . ?
C2 C1 H1 118.5 6_565 . ?
C2 C1 C2 122.9(15) . 6_565 ?
C1 C2 C3 118.2(12) . . ?
C1 C2 C5 122.4(11) . . ?
C3 C2 C5 119.4(12) . . ?
C4 C3 C2 119.7(12) . . ?
O1 C3 C2 121.1(11) . . ?
O1 C3 C4 119.1(10) . . ?
C3 C4 C3 121.1(15) . 6_565 ?
C3 C4 C19 119.4(7) . . ?
C3 C4 C19 119.4(7) 6_565 . ?
C2 C5 H5 106.4 . . ?
C2 C5 C6 107.9(8) . . ?
C2 C5 C25 113.6(11) . . ?
C6 C5 H5 106.4 . . ?
C6 C5 C25 115.3(11) . . ?
C25 C5 H5 106.4 . . ?
C7 C6 C5 121.4(13) . . ?
C11 C6 C5 120.4(12) . . ?
C11 C6 C7 118.0(11) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 C6 122.2(13) . . ?
C8 C7 H7 118.9 . . ?
C7 C8 C12 123.3(13) . . ?
C9 C8 C7 117.0(12) . . ?
C9 C8 C12 119.5(11) . . ?
C8 C9 C10 122.9(11) . . ?
C8 C9 O3 120.1(12) . . ?
C10 C9 O3 116.9(12) . . ?
C9 C10 C21 121.4(12) . . ?
C11 C10 C9 118.6(11) . . ?
C11 C10 C21 119.9(12) . . ?
C10 C11 C6 121.1(12) . . ?
C10 C11 O2 119.3(11) . . ?
O2 C11 C6 119.6(10) . . ?
C8 C12 H12 107.8 . . ?
C13 C12 C8 107.3(11) . . ?
C13 C12 H12 107.8 . . ?
C31 C12 C8 114.5(13) . . ?
C31 C12 H12 107.8 . . ?
C31 C12 C13 111.4(15) . . ?
C14 C13 C12 122.3(14) . . ?
C16 C13 C12 120.9(16) . . ?
C16 C13 C14 116.7(17) . . ?
C13 C14 C13 125(2) 6_565 . ?
C13 C14 H14 117.7 6_565 . ?
C13 C14 H14 117.7 . . ?
C16 C15 C16 118.2(19) . 6_565 ?
C16 C15 C23 120.9(9) . . ?
C16 C15 C23 120.9(9) 6_565 . ?
C13 C16 C15 121.8(17) . . ?
O4 C16 C13 120.3(16) . . ?
O4 C16 C15 117.8(11) . . ?
H17A C17 H17B 107.8 . . ?
O1 C17 H17A 109.0 . . ?
O1 C17 H17B 109.0 . . ?
O2 C17 H17A 109.0 . . ?
O2 C17 H17B 109.0 . . ?
O2 C17 O1 112.9(9) . . ?
H18A C18 H18B 107.8 . . ?
O3 C18 H18A 109.0 . . ?
O3 C18 H18B 109.0 . . ?
O3 C18 O4 113.1(12) . . ?
O4 C18 H18A 109.0 . . ?
O4 C18 H18B 109.0 . . ?
C20 C19 C4 176.7(16) . . ?
C19 C20 I1 177.5(14) . . ?
C22 C21 C10 179.7(17) . . ?
C21 C22 I2 177.9(14) . . ?
C24 C23 C15 179(2) . . ?
C23 C24 I3 178.2(18) . . ?
C5 C25 H25A 109.3 . . ?
C5 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 C5 111.6(13) . . ?
C26 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
C25 C26 H26A 108.2 . . ?
C25 C26 H26B 108.2 . . ?
C25 C26 C27 116.4(14) . . ?
H26A C26 H26B 107.3 . . ?
C27 C26 H26A 108.2 . . ?
C27 C26 H26B 108.2 . . ?
C26 C27 H27A 107.4 . . ?
C26 C27 H27B 107.4 . . ?
C26 C27 H27C 107.2 . . ?
C26 C27 H27D 107.2 . . ?
C26 C27 C28 119.6(11) . . ?
C26 C27 C28B 120.4(11) . . ?
H27A C27 H27B 106.9 . . ?
H27C C27 H27D 106.8 . . ?
C28 C27 H27A 107.4 . . ?
C28 C27 H27B 107.4 . . ?
C28B C27 H27C 107.2 . . ?
C28B C27 H27D 107.2 . . ?
C27 C28 H28A 108.1 . . ?
C27 C28 H28B 108.1 . . ?
C27 C28 C29 116.9(10) . . ?
H28A C28 H28B 107.3 . . ?
C29 C28 H28A 108.1 . . ?
C29 C28 H28B 108.1 . . ?
C27 C28B H28C 108.9 . . ?
C27 C28B H28D 108.9 . . ?
C27 C28B C29B 113(3) . . ?
H28C C28B H28D 107.7 . . ?
C29B C28B H28C 108.9 . . ?
C29B C28B H28D 108.9 . . ?
C28 C29 H29A 108.4 . . ?
C28 C29 H29B 108.4 . . ?
C28 C29 C30 115.7(10) . . ?
H29A C29 H29B 107.4 . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
C28B C29B H29C 110.5 . . ?
C28B C29B H29D 110.5 . . ?
C28B C29B C30B 106(4) . . ?
H29C C29B H29D 108.7 . . ?
C30B C29B H29C 110.5 . . ?
C30B C29B H29D 110.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29B C30B H30D 104.0 . . ?
C29B C30B H30E 107.9 . . ?
C29B C30B H30F 116.3 . . ?
H30D C30B H30E 109.4 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C12 C31 H31A 108.4 . . ?
C12 C31 H31B 108.4 . . ?
C12 C31 C32 115.5(16) . . ?
H31A C31 H31B 107.5 . . ?
C32 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
C31 C32 H32A 108.0 . . ?
C31 C32 H32B 108.0 . . ?
C31 C32 C33 117.1(11) . . ?
H32A C32 H32B 107.3 . . ?
C33 C32 H32A 108.0 . . ?
C33 C32 H32B 108.0 . . ?
C32 C33 H33A 107.7 . . ?
C32 C33 H33B 107.7 . . ?
H33A C33 H33B 107.1 . . ?
C34 C33 C32 118(2) . . ?
C34 C33 H33A 107.7 . . ?
C34 C33 H33B 107.7 . . ?
C33 C34 H34A 111.1 . . ?
C33 C34 H34B 111.1 . . ?
C33 C34 C35 103(2) . . ?
H34A C34 H34B 109.1 . . ?
C35 C34 H34A 111.1 . . ?
C35 C34 H34B 111.1 . . ?
C34 C35 H35A 112.0 . . ?
C34 C35 H35B 112.0 . . ?
C34 C35 C36 99(2) . . ?
H35A C35 H35B 109.7 . . ?
C36 C35 H35A 112.0 . . ?
C36 C35 H35B 112.0 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C3 O1 C17 116.8(8) . . ?
C11 O2 C17 115.8(10) . . ?
C18 O3 C9 116.0(10) . . ?
C16 O4 C18 118.8(10) . . ?
N3 C42 H42A 110.1 . . ?
N3B C42 H42 117.0 . . ?
O7 C42 H42A 110.1 . . ?
O7 C42 H42 117.0 . . ?
O7 C42 N3 140(3) . . ?
O7 C42 N3B 126(3) . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N3 C43 H43A 109.5 . . ?
N3 C43 H43B 109.5 . . ?
N3 C43 H43C 109.5 . . ?
H43D C43B H43E 109.5 . . ?
H43D C43B H43F 109.5 . . ?
H43E C43B H43F 109.5 . . ?
N3B C43B H43D 109.5 . . ?
N3B C43B H43E 109.5 . . ?
N3B C43B H43F 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N3 C44 H44A 109.5 . . ?
N3 C44 H44B 109.5 . . ?
N3 C44 H44C 109.5 . . ?
H44D C44B H44E 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H44E C44B H44F 109.5 . . ?
N3B C44B H44D 109.5 . . ?
N3B C44B H44E 109.5 . . ?
N3B C44B H44F 109.5 . . ?
C42 N3 C43 146(4) . . ?
C42 N3 C44 106(3) . . ?
C43 N3 C44 103(4) . . ?
C42 N3B C43B 107(3) . . ?
C42 N3B C44B 125(3) . . ?
C43B N3B C44B 126(3) . . ?
N1 C1A H1A 114.8 . . ?
O5 C1A H1A 114.8 . . ?
O5 C1A N1 130.4(16) . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N1 C2A H2AA 109.5 . . ?
N1 C2A H2AB 109.5 . . ?
N1 C2A H2AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N1 C3A H3AA 109.5 . . ?
N1 C3A H3AB 109.5 . . ?
N1 C3A H3AC 109.5 . . ?
C1A N1 C2A 120(3) . . ?
C1A N1 C3A 127(3) . . ?
C3A N1 C2A 113(4) . . ?
N2 C37 H37 114.3 . . ?
O6 C37 H37 114.3 . . ?
O6 C37 N2 131(6) . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N2 C38 H38A 109.5 . . ?
N2 C38 H38B 109.5 . . ?
N2 C38 H38C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.4 . . ?
H39B C39 H39C 109.4 . . ?
N2 C39 H39A 103.5 . . ?
N2 C39 H39B 105.8 . . ?
N2 C39 H39C 118.8 . . ?
C37 N2 C38 124(6) . . ?
C37 N2 C39 134(7) . . ?
C38 N2 C39 100(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.2(15) . . . . ?
C1 C2 C3 O1 175.3(9) . . . . ?
C1 C2 C5 C6 94.6(13) . . . . ?
C1 C2 C5 C25 -34.6(15) . . . . ?
C2 C1 C2 C3 -2.1(19) 6_565 . . . ?
C2 C1 C2 C5 -179.6(8) 6_565 . . . ?
C2 C3 C4 C3 4.5(19) . . . 6_565 ?
C2 C3 C4 C19 -174.2(11) . . . . ?
C2 C3 O1 C17 82.7(12) . . . . ?
C2 C5 C6 C7 -89.4(13) . . . . ?
C2 C5 C6 C11 84.6(14) . . . . ?
C2 C5 C25 C26 -172.8(13) . . . . ?
C3 C2 C5 C6 -82.9(13) . . . . ?
C3 C2 C5 C25 147.9(11) . . . . ?
C4 C3 O1 C17 -100.8(12) . . . . ?
C5 C2 C3 C4 176.4(10) . . . . ?
C5 C2 C3 O1 -7.1(13) . . . . ?
C5 C6 C7 C8 176.8(12) . . . . ?
C5 C6 C11 C10 -174.1(12) . . . . ?
C5 C6 C11 O2 5.5(17) . . . . ?
C5 C25 C26 C27 173.4(13) . . . . ?
C6 C5 C25 C26 61.9(17) . . . . ?
C6 C7 C8 C9 -2.8(19) . . . . ?
C6 C7 C8 C12 -178.1(13) . . . . ?
C6 C11 O2 C17 -83.6(13) . . . . ?
C7 C6 C11 C10 0.1(18) . . . . ?
C7 C6 C11 O2 179.7(11) . . . . ?
C7 C8 C9 C10 0(2) . . . . ?
C7 C8 C9 O3 178.5(11) . . . . ?
C7 C8 C12 C13 90.7(16) . . . . ?
C7 C8 C12 C31 -33(2) . . . . ?
C8 C9 C10 C11 2(2) . . . . ?
C8 C9 C10 C21 179.7(13) . . . . ?
C8 C9 O3 C18 83.9(15) . . . . ?
C8 C12 C13 C14 -93.3(16) . . . . ?
C8 C12 C13 C16 84.3(15) . . . . ?
C8 C12 C31 C32 -66(2) . . . . ?
C9 C8 C12 C13 -84.5(16) . . . . ?
C9 C8 C12 C31 151.4(14) . . . . ?
C9 C10 C11 C6 -2.4(19) . . . . ?
C9 C10 C11 O2 178.0(11) . . . . ?
C10 C9 O3 C18 -97.9(15) . . . . ?
C10 C11 O2 C17 96.0(13) . . . . ?
C11 C6 C7 C8 2.6(19) . . . . ?
C12 C8 C9 C10 175.9(13) . . . . ?
C12 C8 C9 O3 -6.0(19) . . . . ?
C12 C13 C14 C13 178.9(11) . . . 6_565 ?
C12 C13 C16 C15 -176.4(14) . . . . ?
C12 C13 C16 O4 6(2) . . . . ?
C12 C31 C32 C33 171(3) . . . . ?
C13 C12 C31 C32 171.7(19) . . . . ?
C13 C16 O4 C18 -81.7(17) . . . . ?
C14 C13 C16 C15 1(2) . . . . ?
C14 C13 C16 O4 -176.4(13) . . . . ?
C15 C16 O4 C18 100.5(16) . . . . ?
C16 C13 C14 C13 1(3) . . . 6_565 ?
C16 C15 C16 C13 -4(3) 6_565 . . . ?
C16 C15 C16 O4 174.1(10) 6_565 . . . ?
C21 C10 C11 C6 -179.9(12) . . . . ?
C21 C10 C11 O2 0.5(19) . . . . ?
C23 C15 C16 C13 175.1(15) . . . . ?
C23 C15 C16 O4 -7(2) . . . . ?
C25 C5 C6 C7 38.9(18) . . . . ?
C25 C5 C6 C11 -147.1(13) . . . . ?
C25 C26 C27 C28 58(3) . . . . ?
C25 C26 C27 C28B -59(3) . . . . ?
C26 C27 C28 C29 -167(3) . . . . ?
C26 C27 C28B C29B -161(3) . . . . ?
C27 C28 C29 C30 -40(5) . . . . ?
C27 C28B C29B C30B 163(5) . . . . ?
C31 C12 C13 C14 32.7(19) . . . . ?
C31 C12 C13 C16 -149.7(14) . . . . ?
C31 C32 C33 C34 152(3) . . . . ?
C32 C33 C34 C35 169(3) . . . . ?
C33 C34 C35 C36 92(3) . . . . ?
O1 C3 C4 C3 -172.1(8) . . . 6_565 ?
O1 C3 C4 C19 9.3(17) . . . . ?
O1 C17 O2 C11 93.9(11) . . . . ?
O2 C17 O1 C3 -92.6(12) . . . . ?
O3 C9 C10 C11 -175.9(11) . . . . ?
O3 C9 C10 C21 1.5(19) . . . . ?
O3 C18 O4 C16 90.7(14) . . . . ?
O4 C18 O3 C9 -91.2(14) . . . . ?
O7 C42 N3 C43 -167(6) . . . . ?
O7 C42 N3 C44 45(7) . . . . ?
O7 C42 N3B C43B 174(3) . . . . ?
O7 C42 N3B C44B 7(5) . . . . ?
O5 C1A N1 C2A 0.000(1) . . . . ?
O5 C1A N1 C3A 180.000(0) . . . . ?
O6 C37 N2 C38 -163(7) . . . . ?
O6 C37 N2 C39 -7(15) . . . . ?

_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_3_dmf
_database_code_depnum_ccdc_archive 'CCDC 1556032'
_audit_update_record             
;
2017-07-12 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_3_dmf               
;
PROBLEM: Check Calcd Residual Density  0.03A From      I8       3.85 eA-3  
RESPONSE: The relatively large residual density is ver close to the 
heavy atom iodine, which might be the caused by the unsuitable 
absorption correction for iodine.
;
_vrf_PLAT201_3_dmf               
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          7 Report
RESPONSE: The atoms in main residue without anisotropic refinement are
involved in bad disorder, for which a model with fixed isotropic
parameters based on the difference Fourier map was made.
;
_vrf_PLAT972_3_dmf               
;
PROBLEM: Check Calcd Residual Density  0.66A From      I6      -2.87 eA-3  
RESPONSE: The density hole is close to the heavy atom, which might be
caused by the unsuitable absorption correction, same reason inducing
high residual density.
;
# end Validation Reply Form

_audit_creation_date             2017-07-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H76 I4 O8, 3.5(C3 H7 N O)'
_chemical_formula_sum            'C78.50 H100.50 I4 N3.50 O11.50'
_chemical_formula_weight         1784.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C64 H96 N16 O8 I4'
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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   16.7987(4)
_cell_length_b                   20.0128(4)
_cell_length_c                   24.3284(7)
_cell_angle_alpha                90.053(2)
_cell_angle_beta                 92.142(2)
_cell_angle_gamma                97.4128(19)
_cell_volume                     8104.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15558
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.2300
_cell_measurement_theta_min      3.6100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.537
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.1043
_exptl_crystal_size_mid          0.0723
_exptl_crystal_size_min          0.0393
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.1085
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         3.160
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -96.00   -5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  125.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
  2 omega -122.00   -1.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -19.0000  -60.0000 121

#__ type_ start__ end____ width___ exp.time_
  3 omega  -49.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000  120.0000 82

#__ type_ start__ end____ width___ exp.time_
  4 omega  102.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  125.0000   60.0000 76

#__ type_ start__ end____ width___ exp.time_
  5 omega   46.00  121.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818 -125.0000  -90.0000 75

#__ type_ start__ end____ width___ exp.time_
  6 omega   29.00   82.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000    0.0000 53

#__ type_ start__ end____ width___ exp.time_
  7 omega   31.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000   90.0000 60

#__ type_ start__ end____ width___ exp.time_
  8 omega   33.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -94.0000    0.0000 76

#__ type_ start__ end____ width___ exp.time_
  9 omega   84.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   45.0000  120.0000 94

#__ type_ start__ end____ width___ exp.time_
 10 omega   79.00  173.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   45.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
 11 omega   94.00  162.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  125.0000   30.0000 68

#__ type_ start__ end____ width___ exp.time_
 12 omega   29.00   54.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
 13 omega -115.00  -14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -57.0000 -120.0000 101

#__ type_ start__ end____ width___ exp.time_
 14 omega -118.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -77.0000   90.0000 109

#__ type_ start__ end____ width___ exp.time_
 15 omega -115.00  -14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -57.0000  150.0000 101

#__ type_ start__ end____ width___ exp.time_
 16 omega   22.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -94.0000  120.0000 87

#__ type_ start__ end____ width___ exp.time_
 17 omega   72.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   77.0000  150.0000 37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0823405000
_diffrn_orient_matrix_UB_12      -0.0013175000
_diffrn_orient_matrix_UB_13      -0.0255305000
_diffrn_orient_matrix_UB_21      -0.0335709000
_diffrn_orient_matrix_UB_22      0.0252167000
_diffrn_orient_matrix_UB_23      -0.0548741000
_diffrn_orient_matrix_UB_31      0.0256490000
_diffrn_orient_matrix_UB_32      0.0734071000
_diffrn_orient_matrix_UB_33      0.0187806000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                18131
_reflns_number_total             28379
_reflns_odcompleteness_completeness 98.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         3.570
_refine_diff_density_min         -2.831
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1740
_refine_ls_number_reflns         28379
_refine_ls_number_restraints     105
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0935
_refine_ls_restrained_S_all      1.039
_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)+(0.1773P)²+5.9991P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2546
_refine_ls_wR_factor_ref         0.3063
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H15N_$1-H83A
 2.2 with sigma of 0.02
 C130-C132 = C131-C133 = C132-C134
 2.5 with sigma of 0.02
 C130-C131 = C131-C132 = C132-C133 = C82-C83
 1.54 with sigma of 0.02
 C133-C134
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C12 \\sim C13: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C147) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C142) \\sim Ueq, Uanis(C144)
\\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C154) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C157) \\sim Ueq, Uanis(C139) \\sim Ueq,
Uanis(C13) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(I4) = Uanis(I4B)
4. Others
 Sof(I4B)=1-FVAR(1)
 Sof(I4)=FVAR(1)
 Fixed Uiso: C83(0.18) C132(0.13) C133(0.15) C134(0.18) C14(0.16) C15(0.19)
5.a Riding coordinates:
 C66(H66A,H66B,H66C)
5.b Ternary CH refined with riding coordinates:
 C77(H77), C94(H94), C111(H111), C128(H128), C9(H9), C26(H26), C43(H43),
 C60(H60)
5.c Secondary CH2 refined with riding coordinates:
 C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,
 H82B), C84(H84A,H84B), C85(H85A,H85B), C95(H95A,H95B), C96(H96A,H96B),
 C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C101(H10F,H10G), C102(H10H,
 H10I), C112(H11C,H11D), C113(H11E,H11F), C114(H11G,H11H), C115(H11I,H11J),
 C116(H11K,H11L), C118(H11P,H11Q), C119(H11R,H11S), C129(H12C,H12D), C130(H13C,
 H13D), C131(H13E,H13F), C132(H13G,H13H), C133(H13I,H13J), C135(H13N,H13O),
 C136(H13P,H13Q), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,
 H13B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B),
  C34(H34A,H34B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C61(H61A,H61B),
 C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C67(H67A,H67B),
  C68(H68A,H68B)
5.d Aromatic/amide H refined with riding coordinates:
 C71(H71), C88(H88), C105(H105), C122(H122), C146(H146), C3(H3), C20(H20),
 C37(H37), C54(H54), C155(H155), C140(H140), C149(H149), C152(H152), C143(H143),
  C137(H137)
5.e Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C100(H10C,H10D,H10E), C117(H11M,H11N,H11O), C134(H13K,
 H13L,H13M), C147(H14C,H14D,H14E), C148(H14F,H14G,H14H), C15(H15A,H15B,H15C),
 C32(H32A,H32B,H32C), C49(H49A,H49B,H49C), C156(H15D,H15E,H15F), C157(H15G,H15H,
 H15I), C141(H14I,H14J,H14K), C142(H14L,H14M,H14N), C150(H15J,H15K,H15L),
 C151(H15M,H15N,H15O), C153(H15P,H15Q,H15R), C154(H15S,H15T,H15U), C144(H14O,
 H14P,H14Q), C145(H14R,H14S,H14T), C138(H13R,H13S,H13T), C139(H13U,H13V,H13W)
;
_atom_sites_solution_hydrogens   mixed
_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
I5 I -0.02344(6) -0.06403(6) 0.78865(5) 0.0936(4) Uani 1 1 d . . . . .
I6 I 0.16092(6) 0.20648(6) 0.40156(4) 0.0796(3) Uani 1 1 d . . . . .
I7 I 0.60672(5) 0.53504(3) 0.47000(2) 0.0535(2) Uani 1 1 d . . . . .
I8 I 0.30054(4) 0.45038(3) 0.81763(3) 0.04750(18) Uani 1 1 d . . . . .
O9 O 0.2005(6) -0.0428(4) 0.6590(4) 0.071(2) Uani 1 1 d . . . . .
O10 O 0.2411(6) 0.0260(5) 0.5565(4) 0.074(3) Uani 1 1 d . . . . .
O11 O 0.4316(6) 0.1783(4) 0.4607(3) 0.065(2) Uani 1 1 d . . . . .
O12 O 0.5732(6) 0.2728(4) 0.4728(3) 0.059(2) Uani 1 1 d . . . . .
O13 O 0.6448(5) 0.3863(3) 0.6454(3) 0.0460(16) Uani 1 1 d . . . . .
O14 O 0.5494(5) 0.3606(3) 0.7408(3) 0.0441(15) Uani 1 1 d . . . . .
O15 O 0.3644(5) 0.2020(4) 0.8333(3) 0.0531(17) Uani 1 1 d . . . . .
O16 O 0.2766(5) 0.0679(4) 0.8302(4) 0.060(2) Uani 1 1 d . . . . .
O21 O 0.3971(7) 0.3447(4) 0.5837(4) 0.070(2) Uani 1 1 d . . . . .
N5 N 0.3157(9) 0.2656(8) 0.6292(8) 0.103(5) Uani 1 1 d . . . . .
C69 C 0.2964(7) 0.0475(5) 0.7780(5) 0.053(3) Uani 1 1 d . . . . .
C70 C 0.3772(6) 0.0569(5) 0.7640(4) 0.044(2) Uani 1 1 d . . . . .
C71 C 0.3946(7) 0.0340(5) 0.7137(4) 0.048(2) Uani 1 1 d . . . . .
H71 H 0.4489 0.0411 0.7032 0.057 Uiso 1 1 calc R . . . .
C72 C 0.3378(7) 0.0009(5) 0.6770(5) 0.051(3) Uani 1 1 d . . . . .
C73 C 0.2588(8) -0.0081(6) 0.6927(5) 0.059(3) Uani 1 1 d . . . . .
C74 C 0.2354(7) 0.0146(5) 0.7435(5) 0.053(3) Uani 1 1 d . . . . .
C75 C 0.1549(7) -0.0014(6) 0.7599(6) 0.061(3) Uani 1 1 d . . . . .
C76 C 0.0891(9) -0.0200(7) 0.7714(7) 0.075(4) Uani 1 1 d . . . . .
C77 C 0.3618(8) -0.0271(5) 0.6219(5) 0.057(3) Uani 1 1 d . . . . .
H77 H 0.3138 -0.0566 0.6061 0.068 Uiso 1 1 calc R . . . .
C78 C 0.4283(9) -0.0700(6) 0.6298(5) 0.060(3) Uani 1 1 d . . . . .
H78A H 0.4733 -0.0448 0.6516 0.072 Uiso 1 1 calc R . . . .
H78B H 0.4483 -0.0809 0.5935 0.072 Uiso 1 1 calc R . . . .
C79 C 0.3978(10) -0.1361(6) 0.6599(6) 0.071(4) Uani 1 1 d . . . . .
H79A H 0.3593 -0.1646 0.6352 0.085 Uiso 1 1 calc R . . . .
H79B H 0.3690 -0.1251 0.6928 0.085 Uiso 1 1 calc R . . . .
C80 C 0.4675(11) -0.1765(6) 0.6780(6) 0.078(4) Uani 1 1 d . . . . .
H80A H 0.4447 -0.2232 0.6868 0.094 Uiso 1 1 calc R . . . .
H80B H 0.5034 -0.1786 0.6469 0.094 Uiso 1 1 calc R . . . .
C81 C 0.5169(13) -0.1459(8) 0.7278(7) 0.089(5) Uani 1 1 d . . . . .
H81A H 0.5419 -0.0999 0.7186 0.107 Uiso 1 1 calc R . . . .
H81B H 0.4809 -0.1421 0.7586 0.107 Uiso 1 1 calc R . . . .
C82 C 0.5805(17) -0.1871(13) 0.7452(11) 0.130(8) Uani 1 1 d D U . . .
H82A H 0.6185 -0.1903 0.7155 0.157 Uiso 1 1 calc R . . A .
H82B H 0.5570 -0.2330 0.7555 0.157 Uiso 1 1 calc R . . A .
C83 C 0.621(2) -0.1496(17) 0.7940(13) 0.180 Uiso 1 1 d D . . B 1
H83A H 0.6776 -0.1582 0.7971 0.270 Uiso 1 1 calc DGR . . B 1
H83B H 0.5941 -0.1651 0.8275 0.270 Uiso 1 1 calc GR . . B 1
H83C H 0.6195 -0.1012 0.7894 0.270 Uiso 1 1 calc GR . . B 1
C84 C 0.1486(10) 0.0008(9) 0.6300(8) 0.092(5) Uani 1 1 d . . . . .
H84A H 0.1182 0.0230 0.6572 0.110 Uiso 1 1 calc R . . . .
H84B H 0.1094 -0.0272 0.6054 0.110 Uiso 1 1 calc R . . . .
C85 C 0.1987(9) 0.0555(7) 0.5953(6) 0.075(4) Uani 1 1 d . . . . .
H85A H 0.1623 0.0842 0.5767 0.089 Uiso 1 1 calc R . . . .
H85B H 0.2366 0.0847 0.6200 0.089 Uiso 1 1 calc R . . . .
C86 C 0.3200(9) 0.0546(7) 0.5503(5) 0.066(3) Uani 1 1 d . . . . .
C87 C 0.3823(8) 0.0305(6) 0.5813(4) 0.054(3) Uani 1 1 d . . . . .
C88 C 0.4605(8) 0.0592(5) 0.5728(4) 0.052(3) Uani 1 1 d . . . . .
H88 H 0.5030 0.0445 0.5945 0.063 Uiso 1 1 calc R . . . .
C89 C 0.4787(8) 0.1093(5) 0.5333(4) 0.050(3) Uani 1 1 d . . . . .
C90 C 0.4141(9) 0.1310(6) 0.5023(4) 0.059(3) Uani 1 1 d . . . . .
C91 C 0.3383(10) 0.1046(6) 0.5113(5) 0.070(4) Uani 1 1 d . . . . .
C92 C 0.2727(11) 0.1299(8) 0.4810(6) 0.080(4) Uani 1 1 d . . . . .
C93 C 0.2292(10) 0.1547(8) 0.4540(7) 0.080(4) Uani 1 1 d . . . . .
C94 C 0.5653(8) 0.1415(6) 0.5239(4) 0.057(3) Uani 1 1 d . . . . .
H94 H 0.5686 0.1528 0.4839 0.068 Uiso 1 1 calc R . . . .
C95 C 0.6267(9) 0.0962(6) 0.5367(5) 0.060(3) Uani 1 1 d . . . . .
H95A H 0.6108 0.0526 0.5175 0.072 Uiso 1 1 calc R . . . .
H95B H 0.6280 0.0873 0.5767 0.072 Uiso 1 1 calc R . . . .
C96 C 0.7112(9) 0.1252(7) 0.5197(5) 0.066(3) Uani 1 1 d . . . . .
H96A H 0.7125 0.1249 0.4791 0.079 Uiso 1 1 calc R . . . .
H96B H 0.7221 0.1728 0.5321 0.079 Uiso 1 1 calc R . . . .
C97 C 0.7781(9) 0.0871(7) 0.5430(6) 0.072(3) Uani 1 1 d . . . . .
H97A H 0.7806 0.0908 0.5836 0.086 Uiso 1 1 calc R . . . .
H97B H 0.7656 0.0388 0.5331 0.086 Uiso 1 1 calc R . . . .
C98 C 0.8561(12) 0.1135(10) 0.5219(9) 0.100(6) Uani 1 1 d . . . . .
H98A H 0.8700 0.1608 0.5343 0.120 Uiso 1 1 calc R . . . .
H98B H 0.8518 0.1134 0.4812 0.120 Uiso 1 1 calc R . . . .
C99 C 0.9248(15) 0.0733(13) 0.5403(12) 0.128(8) Uani 1 1 d . . . . .
H99A H 0.9314 0.0757 0.5809 0.153 Uiso 1 1 calc R . . . .
H99B H 0.9096 0.0254 0.5298 0.153 Uiso 1 1 calc R . . . .
C100 C 1.0051(13) 0.0990(19) 0.5153(13) 0.173(14) Uani 1 1 d . . . . .
H10C H 0.9957 0.1131 0.4773 0.259 Uiso 1 1 calc GR . . . .
H10D H 1.0393 0.0628 0.5157 0.259 Uiso 1 1 calc GR . . . .
H10E H 1.0317 0.1374 0.5369 0.259 Uiso 1 1 calc GR . . . .
C101 C 0.4282(9) 0.2471(6) 0.4753(5) 0.059(3) Uani 1 1 d . . . . .
H10F H 0.4287 0.2517 0.5159 0.071 Uiso 1 1 calc R . . . .
H10G H 0.3777 0.2615 0.4601 0.071 Uiso 1 1 calc R . . . .
C102 C 0.4971(9) 0.2901(6) 0.4537(5) 0.064(3) Uani 1 1 d . . . . .
H10H H 0.4938 0.2872 0.4130 0.076 Uiso 1 1 calc R . . . .
H10I H 0.4936 0.3374 0.4642 0.076 Uiso 1 1 calc R . . . .
C103 C 0.5848(7) 0.2701(5) 0.5302(4) 0.046(2) Uani 1 1 d . . . . .
C104 C 0.5813(6) 0.2081(5) 0.5561(4) 0.041(2) Uani 1 1 d . . . . .
C105 C 0.5981(7) 0.2072(5) 0.6122(4) 0.044(2) Uani 1 1 d . . . . .
H105 H 0.5956 0.1649 0.6303 0.053 Uiso 1 1 calc R . . . .
C106 C 0.6185(6) 0.2658(5) 0.6431(4) 0.039(2) Uani 1 1 d . . . . .
C107 C 0.6200(7) 0.3265(5) 0.6161(4) 0.044(2) Uani 1 1 d . . . . .
C108 C 0.6027(7) 0.3300(5) 0.5603(4) 0.044(2) Uani 1 1 d . . . . .
C109 C 0.6084(7) 0.3931(5) 0.5319(4) 0.046(2) Uani 1 1 d . . . . .
C110 C 0.6105(7) 0.4467(6) 0.5088(4) 0.053(3) Uani 1 1 d . . . . .
C111 C 0.6411(6) 0.2628(5) 0.7047(4) 0.040(2) Uani 1 1 d . . . . .
H111 H 0.6650 0.3091 0.7168 0.048 Uiso 1 1 calc R . . . .
C112 C 0.7047(6) 0.2144(6) 0.7172(4) 0.048(2) Uani 1 1 d . . . . .
H11C H 0.7147 0.2126 0.7575 0.058 Uiso 1 1 calc R . . . .
H11D H 0.6826 0.1685 0.7045 0.058 Uiso 1 1 calc R . . . .
C113 C 0.7836(7) 0.2346(6) 0.6904(6) 0.058(3) Uani 1 1 d . . . . .
H11E H 0.8053 0.2809 0.7023 0.070 Uiso 1 1 calc R . . . .
H11F H 0.7741 0.2351 0.6500 0.070 Uiso 1 1 calc R . . . .
C114 C 0.8455(9) 0.1877(9) 0.7043(9) 0.091(5) Uani 1 1 d . . . . .
H11G H 0.8495 0.1841 0.7449 0.109 Uiso 1 1 calc R . . . .
H11H H 0.8240 0.1424 0.6899 0.109 Uiso 1 1 calc R . . . .
C115 C 0.9265(11) 0.2037(10) 0.6850(10) 0.106(6) Uani 1 1 d . U . . .
H11I H 0.9476 0.2502 0.6967 0.127 Uiso 1 1 calc R . . . .
H11J H 0.9243 0.2026 0.6443 0.127 Uiso 1 1 calc R . . . .
C116 C 0.9851(13) 0.1557(12) 0.7062(12) 0.119(7) Uani 1 1 d . U . . .
H11K H 0.9884 0.1581 0.7469 0.143 Uiso 1 1 calc R . . . .
H11L H 0.9626 0.1091 0.6957 0.143 Uiso 1 1 calc R . . . .
C117 C 1.0641(15) 0.1687(13) 0.6867(14) 0.142(9) Uani 1 1 d . U . . .
H11M H 1.0615 0.1735 0.6466 0.214 Uiso 1 1 calc GR . . . .
H11N H 1.0938 0.1311 0.6965 0.214 Uiso 1 1 calc GR . . . .
H11O H 1.0915 0.2103 0.7035 0.214 Uiso 1 1 calc GR . . . .
C118 C 0.5819(7) 0.4246(5) 0.6588(4) 0.048(2) Uani 1 1 d . . . . .
H11P H 0.5583 0.4414 0.6245 0.057 Uiso 1 1 calc R . . . .
H11Q H 0.6049 0.4642 0.6813 0.057 Uiso 1 1 calc R . . . .
C119 C 0.5160(7) 0.3844(5) 0.6901(4) 0.044(2) Uani 1 1 d . . . . .
H11R H 0.4739 0.4130 0.6981 0.053 Uiso 1 1 calc R . . . .
H11S H 0.4911 0.3455 0.6674 0.053 Uiso 1 1 calc R . . . .
C120 C 0.5232(6) 0.2950(5) 0.7531(4) 0.043(2) Uani 1 1 d . . . . .
C121 C 0.5667(6) 0.2429(5) 0.7378(3) 0.0367(19) Uani 1 1 d . . . . .
C122 C 0.5389(6) 0.1778(5) 0.7525(3) 0.0369(19) Uani 1 1 d . . . . .
H122 H 0.5663 0.1422 0.7403 0.044 Uiso 1 1 calc R . . . .
C123 C 0.4709(6) 0.1621(5) 0.7853(4) 0.040(2) Uani 1 1 d . . . . .
C124 C 0.4299(6) 0.2145(5) 0.8004(4) 0.041(2) Uani 1 1 d . . . . .
C125 C 0.4522(6) 0.2808(5) 0.7839(4) 0.043(2) Uani 1 1 d . . . . .
C126 C 0.4072(6) 0.3331(5) 0.7963(4) 0.043(2) Uani 1 1 d . . . . .
C127 C 0.3662(7) 0.3763(5) 0.8038(4) 0.049(3) Uani 1 1 d . . . . .
C128 C 0.4434(7) 0.0902(5) 0.8035(4) 0.048(2) Uani 1 1 d . . . . .
H128 H 0.4189 0.0934 0.8401 0.057 Uiso 1 1 calc R . . . .
C129 C 0.5094(7) 0.0454(6) 0.8111(4) 0.052(2) Uani 1 1 d . . . . .
H12C H 0.4845 -0.0002 0.8215 0.062 Uiso 1 1 calc R . . . .
H12D H 0.5345 0.0412 0.7753 0.062 Uiso 1 1 calc R . . . .
C130 C 0.5731(8) 0.0689(8) 0.8526(6) 0.071(3) Uani 1 1 d D . . . .
H13C H 0.5475 0.0757 0.8879 0.085 Uiso 1 1 calc R . . . .
H13D H 0.6000 0.1133 0.8410 0.085 Uiso 1 1 calc R . . . .
C131 C 0.6370(11) 0.0226(11) 0.8629(10) 0.124(8) Uani 1 1 d D . . . .
H13E H 0.6579 0.0092 0.8276 0.149 Uiso 1 1 calc R . . . .
H13F H 0.6140 -0.0187 0.8821 0.149 Uiso 1 1 calc R . . . .
C132 C 0.7067(11) 0.0628(11) 0.8997(10) 0.130 Uiso 1 1 d D . . . .
H13G H 0.7131 0.1110 0.8896 0.156 Uiso 1 1 calc R . . . .
H13H H 0.6933 0.0592 0.9390 0.156 Uiso 1 1 calc R . . . .
C133 C 0.7847(11) 0.0333(13) 0.8907(11) 0.150 Uiso 1 1 d D . . . .
H13I H 0.8308 0.0693 0.8947 0.180 Uiso 1 1 calc R . . . .
H13J H 0.7838 0.0146 0.8530 0.180 Uiso 1 1 calc R . . . .
C134 C 0.794(2) -0.0227(15) 0.9330(13) 0.180 Uiso 1 1 d D . . . .
H13K H 0.7833 -0.0069 0.9698 0.270 Uiso 1 1 calc GR . . . .
H13L H 0.8493 -0.0341 0.9329 0.270 Uiso 1 1 calc GR . . . .
H13M H 0.7563 -0.0628 0.9233 0.270 Uiso 1 1 calc GR . . . .
C135 C 0.2878(8) 0.1873(6) 0.8046(6) 0.061(3) Uani 1 1 d . . . . .
H13N H 0.2959 0.1765 0.7656 0.073 Uiso 1 1 calc R . . . .
H13O H 0.2590 0.2274 0.8054 0.073 Uiso 1 1 calc R . . . .
C136 C 0.2380(8) 0.1286(6) 0.8307(6) 0.064(3) Uani 1 1 d . . . . .
H13P H 0.2284 0.1404 0.8692 0.076 Uiso 1 1 calc R . . . .
H13Q H 0.1852 0.1199 0.8108 0.076 Uiso 1 1 calc R . . . .
C146 C 0.3335(11) 0.3244(7) 0.6024(7) 0.085(5) Uani 1 1 d . . . . .
H146 H 0.2919 0.3522 0.5980 0.102 Uiso 1 1 calc R . . . .
C147 C 0.2393(17) 0.2460(15) 0.6512(14) 0.156(10) Uani 1 1 d . U . . .
H14C H 0.2051 0.2182 0.6242 0.235 Uiso 1 1 calc GR . . . .
H14D H 0.2144 0.2862 0.6598 0.235 Uiso 1 1 calc GR . . . .
H14E H 0.2456 0.2200 0.6849 0.235 Uiso 1 1 calc GR . . . .
C148 C 0.3749(10) 0.2214(6) 0.6386(6) 0.070(4) Uani 1 1 d . . . . .
H14F H 0.3937 0.2244 0.6772 0.105 Uiso 1 1 calc GR . . . .
H14G H 0.4203 0.2343 0.6150 0.105 Uiso 1 1 calc GR . . . .
H14H H 0.3514 0.1750 0.6300 0.105 Uiso 1 1 calc GR . . . .
I1 I 0.04409(7) 0.35237(5) 0.56648(4) 0.0851(3) Uani 1 1 d . . . . .
I2 I 0.01792(16) 0.11156(12) 0.92384(13) 0.1971(12) Uani 1 1 d . . . . .
I3 I 0.62041(6) 0.26101(5) 0.89665(3) 0.0736(3) Uani 1 1 d . . . . .
I4 I 0.68143(8) 0.60614(12) 0.62060(6) 0.0523(4) Uani 0.937(8) 1 d . . P C 1
O1 O 0.0368(5) 0.4143(5) 0.7680(3) 0.061(2) Uani 1 1 d . . . . .
O2 O 0.0067(5) 0.3540(6) 0.8711(4) 0.071(3) Uani 1 1 d . . . . .
O3 O 0.2153(5) 0.3177(5) 1.0049(3) 0.061(2) Uani 1 1 d . . . . .
O4 O 0.3821(5) 0.3580(4) 0.9838(3) 0.0505(17) Uani 1 1 d . . . . .
O5 O 0.5671(4) 0.5101(4) 0.8850(3) 0.0410(14) Uani 1 1 d . . . . .
O6 O 0.5855(4) 0.6183(3) 0.8088(3) 0.0420(14) Uani 1 1 d . . . . .
O7 O 0.3762(4) 0.6510(3) 0.6747(2) 0.0409(14) Uani 1 1 d . . . . .
O8 O 0.2251(5) 0.5630(4) 0.6665(3) 0.0523(17) Uani 1 1 d . . . . .
C1 C 0.1883(6) 0.5458(6) 0.7158(4) 0.046(2) Uani 1 1 d . . . . .
C2 C 0.2032(6) 0.5897(6) 0.7611(4) 0.046(2) Uani 1 1 d . . . . .
C3 C 0.1630(6) 0.5714(6) 0.8089(4) 0.049(2) Uani 1 1 d . . . . .
H3 H 0.1740 0.5995 0.8405 0.059 Uiso 1 1 calc R . . . .
C4 C 0.1066(6) 0.5128(6) 0.8127(4) 0.051(3) Uani 1 1 d . . . . .
C5 C 0.0940(6) 0.4724(7) 0.7664(5) 0.057(3) Uani 1 1 d . . . . .
C6 C 0.1338(7) 0.4870(6) 0.7177(4) 0.052(3) Uani 1 1 d . . . . .
C7 C 0.1164(7) 0.4429(7) 0.6702(5) 0.058(3) Uani 1 1 d . . . . .
C8 C 0.0983(9) 0.4067(7) 0.6325(5) 0.064(3) Uani 1 1 d . . . . .
C9 C 0.0611(6) 0.4959(7) 0.8644(5) 0.058(3) Uani 1 1 d . . . . .
H9 H 0.0089 0.4697 0.8517 0.070 Uiso 1 1 calc R . . . .
C10 C 0.0384(8) 0.5566(9) 0.8950(5) 0.075(4) Uani 1 1 d . . . . .
H10A H 0.0092 0.5404 0.9280 0.090 Uiso 1 1 calc R . . . .
H10B H 0.0885 0.5849 0.9079 0.090 Uiso 1 1 calc R . . . .
C11 C -0.0127(8) 0.6005(9) 0.8622(7) 0.081(4) Uani 1 1 d . . . . .
H11A H -0.0613 0.5710 0.8485 0.097 Uiso 1 1 calc R . . . .
H11B H 0.0176 0.6164 0.8296 0.097 Uiso 1 1 calc R . . . .
C12 C -0.0411(13) 0.6627(13) 0.8890(11) 0.120(6) Uani 1 1 d . U . . .
H12A H -0.0882 0.6761 0.8681 0.144 Uiso 1 1 calc R . . . .
H12B H -0.0563 0.6529 0.9274 0.144 Uiso 1 1 calc R . . . .
C13 C 0.0269(15) 0.7162(14) 0.8876(11) 0.128(7) Uani 1 1 d . U . . .
H13A H 0.0430 0.7260 0.8494 0.154 Uiso 1 1 calc R . . . .
H13B H 0.0737 0.7040 0.9096 0.154 Uiso 1 1 calc R . . . .
C14 C -0.008(2) 0.7783(16) 0.9142(14) 0.160 Uiso 1 1 d . . . . .
H14A H -0.0531 0.7919 0.8916 0.192 Uiso 1 1 calc R . . . .
H14B H -0.0253 0.7683 0.9520 0.192 Uiso 1 1 calc R . . . .
C15 C 0.065(2) 0.8317(19) 0.9140(16) 0.190 Uiso 1 1 d . . . . .
H15A H 0.0791 0.8422 0.8760 0.285 Uiso 1 1 calc GR . . . .
H15B H 0.1103 0.8149 0.9336 0.285 Uiso 1 1 calc GR . . . .
H15C H 0.0526 0.8725 0.9323 0.285 Uiso 1 1 calc GR . . . .
C16 C 0.0700(7) 0.3544(7) 0.7823(5) 0.062(3) Uani 1 1 d . . . . .
H16A H 0.1248 0.3660 0.7988 0.075 Uiso 1 1 calc R . . . .
H16B H 0.0737 0.3267 0.7490 0.075 Uiso 1 1 calc R . . . .
C17 C 0.0177(9) 0.3157(9) 0.8223(5) 0.079(4) Uani 1 1 d . . . . .
H17A H -0.0354 0.3010 0.8042 0.095 Uiso 1 1 calc R . . . .
H17B H 0.0417 0.2748 0.8332 0.095 Uiso 1 1 calc R . . . .
C18 C 0.0768(7) 0.3777(8) 0.9014(5) 0.068(4) Uani 1 1 d . . . . .
C19 C 0.1013(6) 0.4490(7) 0.9009(4) 0.058(3) Uani 1 1 d . . . . .
C20 C 0.1694(6) 0.4718(7) 0.9355(5) 0.056(3) Uani 1 1 d . . . . .
H20 H 0.1897 0.5183 0.9349 0.068 Uiso 1 1 calc R . . . .
C21 C 0.2082(6) 0.4298(7) 0.9702(4) 0.052(3) Uani 1 1 d . . . . .
C22 C 0.1818(7) 0.3612(7) 0.9691(4) 0.058(3) Uani 1 1 d . . . . .
C23 C 0.1154(8) 0.3349(8) 0.9355(5) 0.065(3) Uani 1 1 d . . . . .
C24 C 0.0868(9) 0.2627(9) 0.9351(6) 0.081(5) Uani 1 1 d . . . . .
C25 C 0.0604(11) 0.2069(10) 0.9313(8) 0.095(5) Uani 1 1 d . . . . .
C26 C 0.2818(6) 0.4582(6) 1.0071(4) 0.052(3) Uani 1 1 d . . . . .
H26 H 0.2923 0.4217 1.0334 0.062 Uiso 1 1 calc R . . . .
C27 C 0.2694(6) 0.5190(7) 1.0416(4) 0.052(3) Uani 1 1 d . . . . .
H27A H 0.3226 0.5409 1.0554 0.062 Uiso 1 1 calc R . . . .
H27B H 0.2457 0.5516 1.0175 0.062 Uiso 1 1 calc R . . . .
C28 C 0.2165(7) 0.5041(8) 1.0901(5) 0.068(4) Uani 1 1 d . . . . .
H28A H 0.1596 0.4993 1.0768 0.082 Uiso 1 1 calc R . . . .
H28B H 0.2268 0.4605 1.1062 0.082 Uiso 1 1 calc R . . . .
C29 C 0.2291(8) 0.5574(9) 1.1348(5) 0.073(4) Uani 1 1 d . . . . .
H29A H 0.2106 0.5993 1.1204 0.088 Uiso 1 1 calc R . . . .
H29B H 0.2873 0.5674 1.1440 0.088 Uiso 1 1 calc R . . . .
C30 C 0.1851(9) 0.5373(10) 1.1874(7) 0.089(5) Uani 1 1 d . . . . .
H30A H 0.1266 0.5358 1.1800 0.107 Uiso 1 1 calc R . . . .
H30B H 0.1957 0.4915 1.1982 0.107 Uiso 1 1 calc R . . . .
C31 C 0.2098(11) 0.5834(10) 1.2320(7) 0.092(5) Uani 1 1 d . . . . .
H31A H 0.2001 0.6293 1.2209 0.110 Uiso 1 1 calc R . . . .
H31B H 0.2682 0.5842 1.2397 0.110 Uiso 1 1 calc R . . . .
C32 C 0.1636(10) 0.5636(11) 1.2862(6) 0.094(5) Uani 1 1 d . . . . .
H32A H 0.1088 0.5753 1.2823 0.141 Uiso 1 1 calc GR . . . .
H32B H 0.1918 0.5881 1.3175 0.141 Uiso 1 1 calc GR . . . .
H32C H 0.1616 0.5150 1.2923 0.141 Uiso 1 1 calc GR . . . .
C33 C 0.2658(8) 0.2737(7) 0.9809(6) 0.066(3) Uani 1 1 d . . . . .
H33A H 0.2324 0.2404 0.9569 0.079 Uiso 1 1 calc R . . . .
H33B H 0.2910 0.2487 1.0105 0.079 Uiso 1 1 calc R . . . .
C34 C 0.3316(7) 0.3121(6) 0.9473(4) 0.052(2) Uani 1 1 d . . . . .
H34A H 0.3639 0.2802 0.9303 0.062 Uiso 1 1 calc R . . . .
H34B H 0.3073 0.3375 0.9176 0.062 Uiso 1 1 calc R . . . .
C35 C 0.4029(6) 0.4224(5) 0.9623(4) 0.042(2) Uani 1 1 d . . . . .
C36 C 0.3571(6) 0.4729(6) 0.9724(4) 0.045(2) Uani 1 1 d . . . . .
C37 C 0.3806(5) 0.5375(6) 0.9511(4) 0.045(2) Uani 1 1 d . . . . .
H37 H 0.3488 0.5726 0.9572 0.054 Uiso 1 1 calc R . . . .
C38 C 0.4513(6) 0.5510(5) 0.9204(4) 0.041(2) Uani 1 1 d . . . . .
C39 C 0.4950(5) 0.4986(5) 0.9117(3) 0.039(2) Uani 1 1 d . . . . .
C40 C 0.4721(6) 0.4336(5) 0.9317(4) 0.0380(19) Uani 1 1 d . . . . .
C41 C 0.5173(6) 0.3814(5) 0.9206(4) 0.043(2) Uani 1 1 d . . . . .
C42 C 0.5567(8) 0.3359(7) 0.9110(4) 0.060(3) Uani 1 1 d . . . . .
C43 C 0.4798(6) 0.6207(5) 0.8990(4) 0.041(2) Uani 1 1 d . . . . .
H43 H 0.5398 0.6249 0.8996 0.049 Uiso 1 1 calc R . . . .
C44 C 0.4584(6) 0.6794(5) 0.9339(4) 0.044(2) Uani 1 1 d . . . . .
H44A H 0.3996 0.6801 0.9311 0.053 Uiso 1 1 calc R . . . .
H44B H 0.4734 0.6719 0.9729 0.053 Uiso 1 1 calc R . . . .
C45 C 0.4986(9) 0.7443(8) 0.9168(7) 0.081(5) Uani 1 1 d . . . . .
H45A H 0.4737 0.7569 0.8814 0.097 Uiso 1 1 calc R . . . .
H45B H 0.5557 0.7400 0.9105 0.097 Uiso 1 1 calc R . . . .
C46 C 0.4948(12) 0.8006(8) 0.9588(9) 0.101(6) Uani 1 1 d . . . . .
H46A H 0.4376 0.8069 0.9620 0.121 Uiso 1 1 calc R . . . .
H46B H 0.5136 0.7847 0.9950 0.121 Uiso 1 1 calc R . . . .
C47 C 0.5378(15) 0.8637(10) 0.9493(9) 0.108(6) Uani 1 1 d . U . . .
H47A H 0.5110 0.8841 0.9177 0.129 Uiso 1 1 calc R . . . .
H47B H 0.5919 0.8564 0.9377 0.129 Uiso 1 1 calc R . . . .
C48 C 0.5490(18) 0.9158(14) 0.9961(9) 0.132(9) Uani 1 1 d . . . . .
H48A H 0.5665 0.9605 0.9801 0.159 Uiso 1 1 calc R . . . .
H48B H 0.4961 0.9178 1.0121 0.159 Uiso 1 1 calc R . . . .
C49 C 0.6068(19) 0.9037(15) 1.0411(12) 0.147(10) Uiso 1 1 d . . . . .
H49A H 0.6588 0.8987 1.0258 0.221 Uiso 1 1 calc GR . . . .
H49B H 0.5868 0.8626 1.0607 0.221 Uiso 1 1 calc GR . . . .
H49C H 0.6132 0.9420 1.0667 0.221 Uiso 1 1 calc GR . . . .
C50 C 0.5573(6) 0.4978(5) 0.8267(4) 0.041(2) Uani 1 1 d . . . . .
H50A H 0.5005 0.4983 0.8144 0.049 Uiso 1 1 calc R . . . .
H50B H 0.5732 0.4533 0.8174 0.049 Uiso 1 1 calc R . . . .
C51 C 0.6102(5) 0.5529(5) 0.7992(4) 0.041(2) Uani 1 1 d . . . . .
H51A H 0.6663 0.5530 0.8132 0.049 Uiso 1 1 calc R . . . .
H51B H 0.6086 0.5439 0.7591 0.049 Uiso 1 1 calc R . . . .
C52 C 0.5067(5) 0.6233(4) 0.7963(3) 0.0318(17) Uani 1 1 d . . . . .
C53 C 0.4520(6) 0.6262(4) 0.8383(3) 0.0349(18) Uani 1 1 d . . . . .
C54 C 0.3737(5) 0.6349(5) 0.8238(4) 0.039(2) Uani 1 1 d . . . . .
H54 H 0.3365 0.6350 0.8523 0.047 Uiso 1 1 calc R . . . .
C55 C 0.3459(6) 0.6436(5) 0.7697(4) 0.041(2) Uani 1 1 d . . . . .
C56 C 0.4006(6) 0.6396(5) 0.7287(4) 0.0376(19) Uani 1 1 d . . . . .
C57 C 0.4801(6) 0.6299(5) 0.7409(4) 0.040(2) Uani 1 1 d . . . . .
C58 C 0.5386(6) 0.6281(5) 0.6992(4) 0.0385(19) Uani 1 1 d . . . . .
C59 C 0.5895(7) 0.6249(6) 0.6687(4) 0.053(3) Uani 1 1 d . . . . .
C60 C 0.2590(6) 0.6544(5) 0.7564(4) 0.042(2) Uani 1 1 d . . . . .
H60 H 0.2565 0.6677 0.7168 0.050 Uiso 1 1 calc R . . . .
C61 C 0.2365(7) 0.7140(6) 0.7894(5) 0.054(3) Uani 1 1 d . . . . .
H61A H 0.1785 0.7173 0.7832 0.064 Uiso 1 1 calc R . . . .
H61B H 0.2465 0.7064 0.8291 0.064 Uiso 1 1 calc R . . . .
C62 C 0.2847(9) 0.7791(7) 0.7727(5) 0.065(3) Uani 1 1 d . . . . .
H62A H 0.2774 0.7840 0.7324 0.078 Uiso 1 1 calc R . . . .
H62B H 0.3422 0.7756 0.7807 0.078 Uiso 1 1 calc R . . . .
C63 C 0.2647(12) 0.8423(8) 0.7998(7) 0.085(5) Uani 1 1 d . . . . .
H63A H 0.2065 0.8448 0.7944 0.102 Uiso 1 1 calc R . . . .
H63B H 0.2939 0.8820 0.7818 0.102 Uiso 1 1 calc R . . . .
C64 C 0.2874(16) 0.8454(10) 0.8633(8) 0.107(6) Uani 1 1 d . U . . .
H64A H 0.2510 0.8108 0.8824 0.129 Uiso 1 1 calc R . . . .
H64B H 0.3429 0.8346 0.8692 0.129 Uiso 1 1 calc R . . . .
C65 C 0.2814(19) 0.9134(11) 0.8882(8) 0.124(8) Uani 1 1 d . . . . .
H65A H 0.3240 0.9471 0.8740 0.148 Uiso 1 1 calc R . . . .
H65B H 0.2287 0.9278 0.8778 0.148 Uiso 1 1 calc R . . . .
C66 C 0.290(2) 0.9098(14) 0.9488(10) 0.167(12) Uani 1 1 d . U . . .
H66A H 0.3451 0.9009 0.9589 0.250 Uiso 1 1 d R . . . .
H66B H 0.2517 0.8733 0.9622 0.250 Uiso 1 1 d R . . . .
H66C H 0.2808 0.9526 0.9653 0.250 Uiso 1 1 d R . . . .
C67 C 0.3621(6) 0.5929(5) 0.6394(4) 0.047(2) Uani 1 1 d . . . . .
H67A H 0.4134 0.5747 0.6347 0.057 Uiso 1 1 calc R . . . .
H67B H 0.3427 0.6067 0.6027 0.057 Uiso 1 1 calc R . . . .
C68 C 0.3003(6) 0.5371(5) 0.6618(4) 0.044(2) Uani 1 1 d . . . . .
H68A H 0.2935 0.4978 0.6365 0.052 Uiso 1 1 calc R . . . .
H68B H 0.3193 0.5223 0.6982 0.052 Uiso 1 1 calc R . . . .
O23 O 0.6093(6) 0.0436(4) 0.6830(4) 0.064(2) Uani 1 1 d . . . . .
N7 N 0.7106(12) -0.0189(9) 0.6800(8) 0.113(5) Uani 1 1 d . U . . .
C155 C 0.6679(14) 0.0249(9) 0.6929(11) 0.110(7) Uani 1 1 d . . . . .
H155 H 0.6952 0.0521 0.7215 0.132 Uiso 1 1 calc R . . . .
C156 C 0.654(2) -0.0591(12) 0.6275(12) 0.159(12) Uani 1 1 d . . . . .
H15D H 0.6396 -0.1067 0.6368 0.238 Uiso 1 1 calc GR . . . .
H15E H 0.6843 -0.0556 0.5938 0.238 Uiso 1 1 calc GR . . . .
H15F H 0.6046 -0.0380 0.6216 0.238 Uiso 1 1 calc GR . . . .
C157 C 0.7878(18) -0.0379(15) 0.6866(16) 0.177(13) Uani 1 1 d . U . . .
H15G H 0.8252 -0.0082 0.6647 0.266 Uiso 1 1 calc GR . . . .
H15H H 0.7870 -0.0845 0.6742 0.266 Uiso 1 1 calc GR . . . .
H15I H 0.8052 -0.0341 0.7255 0.266 Uiso 1 1 calc GR . . . .
O18 O 0.7994(8) 0.5487(8) 0.5615(5) 0.101(4) Uani 1 1 d . . . . .
N2 N 0.8162(9) 0.4443(9) 0.5349(7) 0.099(4) Uani 1 1 d . . . . .
C140 C 0.7931(10) 0.4879(8) 0.5698(7) 0.082(4) Uani 1 1 d . . . . .
H140 H 0.7704 0.4713 0.6031 0.098 Uiso 1 1 calc R . . . .
C141 C 0.8008(14) 0.3714(9) 0.5460(11) 0.114(7) Uani 1 1 d . . . . .
H14I H 0.8058 0.3638 0.5857 0.171 Uiso 1 1 calc GR . . . .
H14J H 0.8399 0.3481 0.5272 0.171 Uiso 1 1 calc GR . . . .
H14K H 0.7464 0.3538 0.5326 0.171 Uiso 1 1 calc GR . . . .
C142 C 0.8489(16) 0.4659(11) 0.4803(9) 0.119(7) Uani 1 1 d . U . . .
H14L H 0.8462 0.5141 0.4753 0.178 Uiso 1 1 calc GR . . . .
H14M H 0.8170 0.4404 0.4509 0.178 Uiso 1 1 calc GR . . . .
H14N H 0.9049 0.4572 0.4791 0.178 Uiso 1 1 calc GR . . . .
O19 O -0.1651(10) -0.1474(8) 0.8117(8) 0.137(6) Uani 1 1 d . . . . .
N3 N -0.2145(9) -0.2585(8) 0.8031(5) 0.095(5) Uani 1 1 d . . . . .
C149 C -0.1718(10) -0.1994(12) 0.7878(9) 0.109(7) Uani 1 1 d . . . . .
H149 H -0.1444 -0.2001 0.7544 0.130 Uiso 1 1 calc R . . . .
C150 C -0.2254(12) -0.3166(11) 0.7692(8) 0.108(7) Uani 1 1 d . . . . .
H15J H -0.2821 -0.3265 0.7574 0.162 Uiso 1 1 calc GR . . . .
H15K H -0.2091 -0.3550 0.7898 0.162 Uiso 1 1 calc GR . . . .
H15L H -0.1925 -0.3087 0.7368 0.162 Uiso 1 1 calc GR . . . .
C151 C -0.2553(12) -0.2647(13) 0.8566(8) 0.114(7) Uani 1 1 d . . . . .
H15M H -0.2752 -0.3122 0.8632 0.172 Uiso 1 1 calc GR . . . .
H15N H -0.3004 -0.2382 0.8554 0.172 Uiso 1 1 calc DGR . . . .
H15O H -0.2170 -0.2479 0.8864 0.172 Uiso 1 1 calc GR . . . .
O22 O 0.2240(5) 0.6488(6) 0.9430(4) 0.073(3) Uani 1 1 d . . . . .
N6 N 0.1663(8) 0.6961(9) 1.0133(5) 0.088(4) Uani 1 1 d . . . . .
C152 C 0.2189(7) 0.6952(8) 0.9748(5) 0.061(3) Uani 1 1 d . . . . .
H152 H 0.2567 0.7345 0.9713 0.074 Uiso 1 1 calc R . . . .
C153 C 0.1065(10) 0.6352(12) 1.0238(7) 0.100(6) Uani 1 1 d . . . . .
H15P H 0.1232 0.5957 1.0058 0.150 Uiso 1 1 calc GR . . . .
H15Q H 0.0534 0.6428 1.0090 0.150 Uiso 1 1 calc GR . . . .
H15R H 0.1039 0.6274 1.0635 0.150 Uiso 1 1 calc GR . . . .
C154 C 0.1587(13) 0.7522(11) 1.0490(8) 0.107(6) Uani 1 1 d . U . . .
H15S H 0.2009 0.7893 1.0415 0.160 Uiso 1 1 calc GR . . . .
H15T H 0.1642 0.7383 1.0874 0.160 Uiso 1 1 calc GR . . . .
H15U H 0.1059 0.7672 1.0424 0.160 Uiso 1 1 calc GR . . . .
O20 O 0.0824(8) 0.2887(7) 0.3366(6) 0.099(4) Uani 1 1 d . . . . .
N4 N 0.0283(9) 0.3868(8) 0.3437(5) 0.086(4) Uani 1 1 d . . . . .
C143 C 0.0702(10) 0.3396(10) 0.3636(8) 0.086(5) Uani 1 1 d . . . . .
H143 H 0.0920 0.3447 0.4002 0.103 Uiso 1 1 calc R . . . .
C144 C -0.0020(19) 0.3848(16) 0.2904(12) 0.155(10) Uani 1 1 d . U . . .
H14O H 0.0313 0.3604 0.2673 0.232 Uiso 1 1 calc GR . . . .
H14P H -0.0018 0.4309 0.2767 0.232 Uiso 1 1 calc GR . . . .
H14Q H -0.0572 0.3617 0.2891 0.232 Uiso 1 1 calc GR . . . .
C145 C 0.0111(13) 0.4436(10) 0.3774(7) 0.098(5) Uani 1 1 d . . . . .
H14R H -0.0405 0.4319 0.3947 0.147 Uiso 1 1 calc GR . . . .
H14S H 0.0087 0.4832 0.3540 0.147 Uiso 1 1 calc GR . . . .
H14T H 0.0537 0.4536 0.4059 0.147 Uiso 1 1 calc GR . . . .
O17 O -0.0538(8) 0.2980(7) 0.4735(6) 0.105(4) Uani 1 1 d . . . . .
N1 N -0.1146(10) 0.2454(7) 0.3981(6) 0.092(4) Uani 1 1 d . . . . .
C137 C -0.0603(11) 0.2586(9) 0.4373(7) 0.087(5) Uani 1 1 d . . . . .
H137 H -0.0180 0.2314 0.4366 0.104 Uiso 1 1 calc R . . . .
C138 C -0.1121(18) 0.1975(11) 0.3553(11) 0.137(10) Uani 1 1 d . . . . .
H13R H -0.0673 0.1716 0.3628 0.206 Uiso 1 1 calc GR . . . .
H13S H -0.1047 0.2210 0.3202 0.206 Uiso 1 1 calc GR . . . .
H13T H -0.1627 0.1669 0.3534 0.206 Uiso 1 1 calc GR . . . .
C139 C -0.198(2) 0.2776(19) 0.4045(16) 0.194(15) Uani 1 1 d . U . . .
H13U H -0.1973 0.2992 0.4407 0.291 Uiso 1 1 calc GR . . . .
H13V H -0.2433 0.2419 0.4009 0.291 Uiso 1 1 calc GR . . . .
H13W H -0.2025 0.3112 0.3757 0.291 Uiso 1 1 calc GR . . . .
I4B I 0.6960(12) 0.6305(16) 0.6302(8) 0.0523(4) Uani 0.063(8) 1 d . . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I5 C76 2.039(15) . ?
I6 C93 2.053(15) . ?
I7 C110 2.012(12) . ?
I8 C127 1.995(13) . ?
O9 C73 1.370(14) . ?
O9 C84 1.472(19) . ?
O10 C85 1.38(2) . ?
O10 C86 1.388(17) . ?
O11 C90 1.399(14) . ?
O11 C101 1.431(15) . ?
O12 C102 1.428(16) . ?
O12 C103 1.406(11) . ?
O13 C107 1.400(12) . ?
O13 C118 1.431(14) . ?
O14 C119 1.443(12) . ?
O14 C120 1.366(12) . ?
O15 C124 1.382(13) . ?
O15 C135 1.438(15) . ?
O16 C69 1.398(15) . ?
O16 C136 1.450(16) . ?
O21 C146 1.20(2) . ?
N5 C146 1.352(19) . ?
N5 C147 1.42(3) . ?
N5 C148 1.43(2) . ?
C69 C70 1.401(17) . ?
C69 C74 1.396(16) . ?
C70 C71 1.361(16) . ?
C70 C128 1.528(14) . ?
C71 C72 1.384(14) . ?
C72 C73 1.385(19) . ?
C72 C77 1.538(18) . ?
C73 C74 1.405(19) . ?
C74 C75 1.421(17) . ?
C75 C76 1.16(2) . ?
C77 C78 1.501(19) . ?
C77 C87 1.533(16) . ?
C78 C79 1.551(16) . ?
C79 C80 1.56(2) . ?
C80 C81 1.52(2) . ?
C81 C82 1.48(3) . ?
C82 C83 1.500(18) . ?
C84 C85 1.56(2) . ?
C86 C87 1.403(18) . ?
C86 C91 1.393(19) . ?
C87 C88 1.386(18) . ?
C88 C89 1.403(15) . ?
C89 C90 1.413(17) . ?
C89 C94 1.539(18) . ?
C90 C91 1.34(2) . ?
C91 C92 1.45(2) . ?
C92 C93 1.13(2) . ?
C94 C95 1.483(19) . ?
C94 C104 1.534(13) . ?
C95 C96 1.54(2) . ?
C96 C97 1.53(2) . ?
C97 C98 1.46(2) . ?
C98 C99 1.54(3) . ?
C99 C100 1.53(3) . ?
C101 C102 1.46(2) . ?
C103 C104 1.386(14) . ?
C103 C108 1.397(14) . ?
C104 C105 1.385(13) . ?
C105 C106 1.391(14) . ?
C106 C107 1.380(14) . ?
C106 C111 1.537(12) . ?
C107 C108 1.381(14) . ?
C108 C109 1.435(13) . ?
C109 C110 1.208(15) . ?
C111 C112 1.555(15) . ?
C111 C121 1.521(14) . ?
C112 C113 1.506(16) . ?
C113 C114 1.517(19) . ?
C114 C115 1.45(3) . ?
C115 C116 1.54(3) . ?
C116 C117 1.42(3) . ?
C118 C119 1.511(15) . ?
C120 C121 1.405(15) . ?
C120 C125 1.431(15) . ?
C121 C122 1.378(13) . ?
C122 C123 1.419(15) . ?
C123 C124 1.384(15) . ?
C123 C128 1.525(13) . ?
C124 C125 1.395(14) . ?
C125 C126 1.406(15) . ?
C126 C127 1.189(16) . ?
C128 C129 1.519(17) . ?
C129 C130 1.476(16) . ?
C130 C131 1.520(16) . ?
C131 C132 1.580(17) . ?
C132 C133 1.527(17) . ?
C133 C134 1.544(10) . ?
C135 C136 1.508(17) . ?
I1 C8 2.056(11) . ?
I2 C25 1.954(19) . ?
I3 C42 1.989(16) . ?
I4 C59 2.045(14) . ?
O1 C5 1.412(15) . ?
O1 C16 1.424(17) . ?
O2 C17 1.442(18) . ?
O2 C18 1.397(14) . ?
O3 C22 1.388(16) . ?
O3 C33 1.437(18) . ?
O4 C34 1.447(13) . ?
O4 C35 1.398(13) . ?
O5 C39 1.390(11) . ?
O5 C50 1.439(11) . ?
O6 C51 1.445(12) . ?
O6 C52 1.364(11) . ?
O7 C56 1.391(11) . ?
O7 C67 1.435(12) . ?
O8 C1 1.394(13) . ?
O8 C68 1.434(13) . ?
C1 C2 1.405(15) . ?
C1 C6 1.396(17) . ?
C2 C3 1.392(15) . ?
C2 C60 1.504(15) . ?
C3 C4 1.415(17) . ?
C4 C5 1.379(17) . ?
C4 C9 1.513(15) . ?
C5 C6 1.395(16) . ?
C6 C7 1.451(17) . ?
C7 C8 1.173(17) . ?
C9 C10 1.52(2) . ?
C9 C19 1.500(18) . ?
C10 C11 1.51(2) . ?
C11 C12 1.54(3) . ?
C12 C13 1.46(3) . ?
C13 C14 1.59(4) . ?
C14 C15 1.52(4) . ?
C16 C17 1.487(17) . ?
C18 C19 1.43(2) . ?
C18 C23 1.39(2) . ?
C19 C20 1.420(15) . ?
C20 C21 1.394(17) . ?
C21 C22 1.388(19) . ?
C21 C26 1.546(15) . ?
C22 C23 1.403(17) . ?
C23 C24 1.46(2) . ?
C24 C25 1.15(2) . ?
C26 C27 1.518(17) . ?
C26 C36 1.544(14) . ?
C27 C28 1.511(15) . ?
C28 C29 1.51(2) . ?
C29 C30 1.53(2) . ?
C30 C31 1.44(2) . ?
C31 C32 1.58(2) . ?
C33 C34 1.526(16) . ?
C35 C36 1.374(15) . ?
C35 C40 1.398(14) . ?
C36 C37 1.408(16) . ?
C37 C38 1.423(13) . ?
C38 C39 1.375(15) . ?
C38 C43 1.514(15) . ?
C39 C40 1.400(14) . ?
C40 C41 1.400(15) . ?
C41 C42 1.220(18) . ?
C43 C44 1.535(13) . ?
C43 C53 1.542(12) . ?
C44 C45 1.453(19) . ?
C45 C46 1.531(18) . ?
C46 C47 1.40(3) . ?
C47 C48 1.53(3) . ?
C48 C49 1.48(4) . ?
C50 C51 1.498(14) . ?
C52 C53 1.405(12) . ?
C52 C57 1.416(13) . ?
C53 C54 1.382(13) . ?
C54 C55 1.398(13) . ?
C55 C56 1.390(13) . ?
C55 C60 1.526(13) . ?
C56 C57 1.395(14) . ?
C57 C58 1.443(12) . ?
C58 C59 1.159(16) . ?
C59 I4B 2.04(2) . ?
C60 C61 1.533(14) . ?
C61 C62 1.506(19) . ?
C62 C63 1.508(18) . ?
C63 C64 1.58(3) . ?
C64 C65 1.51(3) . ?
C65 C66 1.48(3) . ?
C67 C68 1.538(14) . ?
O23 C155 1.12(2) . ?
N7 C155 1.25(3) . ?
N7 C156 1.70(4) . ?
N7 C157 1.40(3) . ?
O18 C140 1.22(2) . ?
N2 C140 1.32(2) . ?
N2 C141 1.48(2) . ?
N2 C142 1.50(2) . ?
O19 C149 1.18(3) . ?
N3 C149 1.36(2) . ?
N3 C150 1.41(2) . ?
N3 C151 1.49(2) . ?
O22 C152 1.222(17) . ?
N6 C152 1.313(19) . ?
N6 C153 1.51(3) . ?
N6 C154 1.44(2) . ?
O20 C143 1.25(2) . ?
N4 C143 1.33(2) . ?
N4 C144 1.37(3) . ?
N4 C145 1.46(2) . ?
O17 C137 1.17(2) . ?
N1 C137 1.30(2) . ?
N1 C138 1.42(3) . ?
N1 C139 1.62(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C73 O9 C84 113.6(10) . . ?
C85 O10 C86 116.3(10) . . ?
C90 O11 C101 116.0(9) . . ?
C103 O12 C102 115.5(9) . . ?
C107 O13 C118 115.2(8) . . ?
C120 O14 C119 114.9(7) . . ?
C124 O15 C135 115.5(9) . . ?
C69 O16 C136 114.5(9) . . ?
C146 N5 C147 122.2(18) . . ?
C146 N5 C148 120.9(16) . . ?
C147 N5 C148 116.8(16) . . ?
O16 C69 C70 118.7(10) . . ?
C74 C69 O16 118.4(11) . . ?
C74 C69 C70 122.8(11) . . ?
C69 C70 C128 121.8(10) . . ?
C71 C70 C69 117.1(10) . . ?
C71 C70 C128 121.1(10) . . ?
C70 C71 C72 123.9(11) . . ?
C71 C72 C73 117.3(12) . . ?
C71 C72 C77 121.5(11) . . ?
C73 C72 C77 121.2(9) . . ?
O9 C73 C72 119.9(12) . . ?
O9 C73 C74 117.4(12) . . ?
C72 C73 C74 122.6(10) . . ?
C69 C74 C73 116.4(11) . . ?
C69 C74 C75 123.0(12) . . ?
C73 C74 C75 120.4(11) . . ?
C76 C75 C74 174.1(15) . . ?
C75 C76 I5 172.9(13) . . ?
C78 C77 C72 111.7(9) . . ?
C78 C77 C87 112.6(11) . . ?
C87 C77 C72 110.2(9) . . ?
C77 C78 C79 110.4(12) . . ?
C78 C79 C80 112.3(12) . . ?
C81 C80 C79 113.2(12) . . ?
C82 C81 C80 111.8(16) . . ?
C81 C82 C83 104(2) . . ?
O9 C84 C85 111.5(13) . . ?
O10 C85 C84 110.7(13) . . ?
O10 C86 C87 119.8(11) . . ?
O10 C86 C91 120.5(12) . . ?
C91 C86 C87 119.6(13) . . ?
C86 C87 C77 119.1(11) . . ?
C88 C87 C77 122.8(11) . . ?
C88 C87 C86 118.1(11) . . ?
C87 C88 C89 122.1(11) . . ?
C88 C89 C90 117.7(12) . . ?
C88 C89 C94 122.3(11) . . ?
C90 C89 C94 119.9(10) . . ?
O11 C90 C89 118.4(12) . . ?
C91 C90 O11 121.2(11) . . ?
C91 C90 C89 120.4(11) . . ?
C86 C91 C92 118.4(15) . . ?
C90 C91 C86 122.1(13) . . ?
C90 C91 C92 119.6(12) . . ?
C93 C92 C91 171.0(19) . . ?
C92 C93 I6 173.7(17) . . ?
C95 C94 C89 113.8(10) . . ?
C95 C94 C104 112.4(10) . . ?
C104 C94 C89 108.7(10) . . ?
C94 C95 C96 113.1(10) . . ?
C97 C96 C95 114.1(11) . . ?
C98 C97 C96 111.7(14) . . ?
C97 C98 C99 113.9(18) . . ?
C100 C99 C98 113(2) . . ?
O11 C101 C102 109.9(12) . . ?
O12 C102 C101 114.1(9) . . ?
C104 C103 O12 119.7(9) . . ?
C104 C103 C108 120.8(8) . . ?
C108 C103 O12 119.4(9) . . ?
C103 C104 C94 122.0(9) . . ?
C105 C104 C94 119.6(9) . . ?
C105 C104 C103 118.3(8) . . ?
C104 C105 C106 122.3(9) . . ?
C105 C106 C111 120.9(8) . . ?
C107 C106 C105 117.7(8) . . ?
C107 C106 C111 121.3(8) . . ?
C106 C107 O13 119.0(8) . . ?
C106 C107 C108 121.9(9) . . ?
C108 C107 O13 119.0(9) . . ?
C103 C108 C109 119.3(9) . . ?
C107 C108 C103 118.8(9) . . ?
C107 C108 C109 121.7(9) . . ?
C110 C109 C108 177.6(13) . . ?
C109 C110 I7 176.5(11) . . ?
C106 C111 C112 112.4(8) . . ?
C121 C111 C106 110.6(8) . . ?
C121 C111 C112 110.5(8) . . ?
C113 C112 C111 113.9(9) . . ?
C112 C113 C114 112.9(12) . . ?
C115 C114 C113 119.2(16) . . ?
C114 C115 C116 114(2) . . ?
C117 C116 C115 115(2) . . ?
O13 C118 C119 113.0(8) . . ?
O14 C119 C118 109.5(9) . . ?
O14 C120 C121 120.9(9) . . ?
O14 C120 C125 118.4(10) . . ?
C121 C120 C125 120.7(9) . . ?
C120 C121 C111 116.9(8) . . ?
C122 C121 C111 124.5(9) . . ?
C122 C121 C120 118.6(9) . . ?
C121 C122 C123 122.4(9) . . ?
C122 C123 C128 121.8(9) . . ?
C124 C123 C122 117.6(9) . . ?
C124 C123 C128 120.6(9) . . ?
O15 C124 C123 119.8(9) . . ?
O15 C124 C125 117.6(10) . . ?
C123 C124 C125 122.6(10) . . ?
C124 C125 C120 117.9(10) . . ?
C124 C125 C126 122.3(10) . . ?
C126 C125 C120 119.8(9) . . ?
C127 C126 C125 175.8(10) . . ?
C126 C127 I8 178.1(9) . . ?
C123 C128 C70 110.1(8) . . ?
C129 C128 C70 110.1(9) . . ?
C129 C128 C123 115.5(9) . . ?
C130 C129 C128 115.3(10) . . ?
C129 C130 C131 115.9(13) . . ?
C130 C131 C132 107.4(14) . . ?
C133 C132 C131 108.9(15) . . ?
C132 C133 C134 109.8(15) . . ?
O15 C135 C136 110.5(11) . . ?
O16 C136 C135 112.3(10) . . ?
O21 C146 N5 125.8(16) . . ?
C5 O1 C16 114.1(9) . . ?
C18 O2 C17 115.6(10) . . ?
C22 O3 C33 116.2(9) . . ?
C35 O4 C34 114.5(8) . . ?
C39 O5 C50 112.7(7) . . ?
C52 O6 C51 115.4(7) . . ?
C56 O7 C67 116.2(7) . . ?
C1 O8 C68 113.1(8) . . ?
O8 C1 C2 119.3(9) . . ?
O8 C1 C6 118.7(9) . . ?
C6 C1 C2 121.8(10) . . ?
C1 C2 C60 120.1(9) . . ?
C3 C2 C1 117.2(10) . . ?
C3 C2 C60 122.6(10) . . ?
C2 C3 C4 123.0(10) . . ?
C3 C4 C9 121.7(10) . . ?
C5 C4 C3 116.6(10) . . ?
C5 C4 C9 121.6(11) . . ?
C4 C5 O1 118.4(10) . . ?
C4 C5 C6 123.2(11) . . ?
C6 C5 O1 118.4(10) . . ?
C1 C6 C7 121.7(10) . . ?
C5 C6 C1 118.0(10) . . ?
C5 C6 C7 120.2(11) . . ?
C8 C7 C6 176.6(13) . . ?
C7 C8 I1 167.7(13) . . ?
C4 C9 C10 114.7(12) . . ?
C19 C9 C4 112.0(9) . . ?
C19 C9 C10 113.1(10) . . ?
C11 C10 C9 115.4(12) . . ?
C10 C11 C12 120.4(17) . . ?
C13 C12 C11 105.9(17) . . ?
C12 C13 C14 103(2) . . ?
C15 C14 C13 101(3) . . ?
O1 C16 C17 109.0(12) . . ?
O2 C17 C16 113.0(12) . . ?
O2 C18 C19 116.7(13) . . ?
C23 C18 O2 121.0(13) . . ?
C23 C18 C19 121.8(11) . . ?
C18 C19 C9 122.7(10) . . ?
C20 C19 C9 122.1(12) . . ?
C20 C19 C18 115.1(12) . . ?
C21 C20 C19 123.8(12) . . ?
C20 C21 C26 121.0(11) . . ?
C22 C21 C20 118.5(11) . . ?
C22 C21 C26 120.4(11) . . ?
O3 C22 C21 120.8(10) . . ?
O3 C22 C23 118.1(12) . . ?
C21 C22 C23 120.8(12) . . ?
C18 C23 C22 119.9(13) . . ?
C18 C23 C24 119.5(12) . . ?
C22 C23 C24 120.6(14) . . ?
C25 C24 C23 174.5(19) . . ?
C24 C25 I2 178.5(18) . . ?
C27 C26 C21 114.6(10) . . ?
C27 C26 C36 111.3(9) . . ?
C36 C26 C21 110.4(8) . . ?
C28 C27 C26 115.3(11) . . ?
C29 C28 C27 114.1(12) . . ?
C28 C29 C30 113.9(14) . . ?
C31 C30 C29 112.2(15) . . ?
C30 C31 C32 112.5(17) . . ?
O3 C33 C34 112.2(10) . . ?
O4 C34 C33 108.2(9) . . ?
C36 C35 O4 120.3(9) . . ?
C36 C35 C40 121.8(9) . . ?
C40 C35 O4 117.9(9) . . ?
C35 C36 C26 119.8(10) . . ?
C35 C36 C37 118.9(9) . . ?
C37 C36 C26 121.3(10) . . ?
C36 C37 C38 120.8(10) . . ?
C37 C38 C43 121.9(9) . . ?
C39 C38 C37 117.8(10) . . ?
C39 C38 C43 120.3(8) . . ?
O5 C39 C40 117.5(9) . . ?
C38 C39 O5 120.0(9) . . ?
C38 C39 C40 122.4(9) . . ?
C35 C40 C39 118.3(9) . . ?
C35 C40 C41 121.3(9) . . ?
C39 C40 C41 120.4(9) . . ?
C42 C41 C40 179.8(12) . . ?
C41 C42 I3 179.0(10) . . ?
C38 C43 C44 115.3(8) . . ?
C38 C43 C53 110.0(7) . . ?
C44 C43 C53 111.9(8) . . ?
C45 C44 C43 112.7(9) . . ?
C44 C45 C46 113.4(12) . . ?
C47 C46 C45 118.4(16) . . ?
C46 C47 C48 119(2) . . ?
C49 C48 C47 116(2) . . ?
O5 C50 C51 106.9(7) . . ?
O6 C51 C50 112.0(8) . . ?
O6 C52 C53 120.6(8) . . ?
O6 C52 C57 120.2(8) . . ?
C53 C52 C57 119.1(8) . . ?
C52 C53 C43 120.2(8) . . ?
C54 C53 C43 121.3(8) . . ?
C54 C53 C52 118.5(8) . . ?
C53 C54 C55 123.9(8) . . ?
C54 C55 C60 121.4(8) . . ?
C56 C55 C54 116.7(9) . . ?
C56 C55 C60 121.9(9) . . ?
O7 C56 C57 119.7(8) . . ?
C55 C56 O7 118.2(9) . . ?
C55 C56 C57 121.9(9) . . ?
C52 C57 C58 117.3(9) . . ?
C56 C57 C52 119.8(8) . . ?
C56 C57 C58 122.8(9) . . ?
C59 C58 C57 174.8(11) . . ?
C58 C59 I4 171.6(10) . . ?
C58 C59 I4B 166.1(13) . . ?
C2 C60 C55 111.2(9) . . ?
C2 C60 C61 115.3(9) . . ?
C55 C60 C61 110.7(8) . . ?
C62 C61 C60 111.0(9) . . ?
C61 C62 C63 116.3(12) . . ?
C62 C63 C64 112.7(14) . . ?
C65 C64 C63 112.6(17) . . ?
C66 C65 C64 110(2) . . ?
O7 C67 C68 112.9(8) . . ?
O8 C68 C67 108.9(9) . . ?
C155 N7 C156 101(2) . . ?
C155 N7 C157 143(3) . . ?
C157 N7 C156 114(2) . . ?
O23 C155 N7 143(3) . . ?
C140 N2 C141 120.0(17) . . ?
C140 N2 C142 121.7(17) . . ?
C141 N2 C142 117.9(17) . . ?
O18 C140 N2 123.4(16) . . ?
C149 N3 C150 122.8(16) . . ?
C149 N3 C151 121.3(17) . . ?
C150 N3 C151 115.9(15) . . ?
O19 C149 N3 127.0(19) . . ?
C152 N6 C153 120.9(14) . . ?
C152 N6 C154 125.8(18) . . ?
C154 N6 C153 113.3(15) . . ?
O22 C152 N6 126.3(15) . . ?
C143 N4 C144 121.8(19) . . ?
C143 N4 C145 122.1(15) . . ?
C144 N4 C145 116.0(17) . . ?
O20 C143 N4 123.5(17) . . ?
C137 N1 C138 125(2) . . ?
C137 N1 C139 116(2) . . ?
C138 N1 C139 118(2) . . ?
O17 C137 N1 132(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O9 C73 C74 C69 177.7(10) . . . . ?
O9 C73 C74 C75 3.3(16) . . . . ?
O9 C84 C85 O10 59.7(16) . . . . ?
O10 C86 C87 C77 -0.4(17) . . . . ?
O10 C86 C87 C88 178.4(11) . . . . ?
O10 C86 C91 C90 -176.7(12) . . . . ?
O10 C86 C91 C92 5(2) . . . . ?
O11 C90 C91 C86 176.2(11) . . . . ?
O11 C90 C91 C92 -5.7(19) . . . . ?
O11 C101 C102 O12 -58.6(12) . . . . ?
O12 C103 C104 C94 0.3(17) . . . . ?
O12 C103 C104 C105 175.9(10) . . . . ?
O12 C103 C108 C107 -175.1(10) . . . . ?
O12 C103 C108 C109 0.5(17) . . . . ?
O13 C107 C108 C103 174.5(10) . . . . ?
O13 C107 C108 C109 -1.0(17) . . . . ?
O13 C118 C119 O14 59.8(10) . . . . ?
O14 C120 C121 C111 -2.9(12) . . . . ?
O14 C120 C121 C122 178.2(8) . . . . ?
O14 C120 C125 C124 -174.6(8) . . . . ?
O14 C120 C125 C126 5.9(13) . . . . ?
O15 C124 C125 C120 175.7(8) . . . . ?
O15 C124 C125 C126 -4.8(13) . . . . ?
O15 C135 C136 O16 -59.8(14) . . . . ?
O16 C69 C70 C71 177.3(9) . . . . ?
O16 C69 C70 C128 -1.6(15) . . . . ?
O16 C69 C74 C73 -176.6(10) . . . . ?
O16 C69 C74 C75 -2.4(17) . . . . ?
C69 O16 C136 C135 -56.4(14) . . . . ?
C69 C70 C71 C72 -1.7(16) . . . . ?
C69 C70 C128 C123 -104.5(11) . . . . ?
C69 C70 C128 C129 127.0(11) . . . . ?
C70 C69 C74 C73 -1.2(16) . . . . ?
C70 C69 C74 C75 173.1(11) . . . . ?
C70 C71 C72 C73 0.9(16) . . . . ?
C70 C71 C72 C77 -176.8(10) . . . . ?
C70 C128 C129 C130 -174.3(10) . . . . ?
C71 C70 C128 C123 76.6(13) . . . . ?
C71 C70 C128 C129 -51.9(12) . . . . ?
C71 C72 C73 O9 -177.5(10) . . . . ?
C71 C72 C73 C74 -0.1(16) . . . . ?
C71 C72 C77 C78 51.0(13) . . . . ?
C71 C72 C77 C87 -74.9(13) . . . . ?
C72 C73 C74 C69 0.3(16) . . . . ?
C72 C73 C74 C75 -174.2(11) . . . . ?
C72 C77 C78 C79 68.6(12) . . . . ?
C72 C77 C87 C86 -84.0(12) . . . . ?
C72 C77 C87 C88 97.4(13) . . . . ?
C73 O9 C84 C85 56.8(19) . . . . ?
C73 C72 C77 C78 -126.5(11) . . . . ?
C73 C72 C77 C87 107.6(12) . . . . ?
C74 C69 C70 C71 1.9(16) . . . . ?
C74 C69 C70 C128 -177.0(10) . . . . ?
C77 C72 C73 O9 0.2(16) . . . . ?
C77 C72 C73 C74 177.5(10) . . . . ?
C77 C78 C79 C80 -170.2(10) . . . . ?
C77 C87 C88 C89 176.4(10) . . . . ?
C78 C77 C87 C86 150.7(11) . . . . ?
C78 C77 C87 C88 -28.0(14) . . . . ?
C78 C79 C80 C81 75.1(16) . . . . ?
C79 C80 C81 C82 177.7(17) . . . . ?
C80 C81 C82 C83 -180(2) . . . . ?
C84 O9 C73 C72 -105.3(15) . . . . ?
C84 O9 C73 C74 77.2(15) . . . . ?
C85 O10 C86 C87 91.3(15) . . . . ?
C85 O10 C86 C91 -92.2(15) . . . . ?
C86 O10 C85 C84 -137.0(11) . . . . ?
C86 C87 C88 C89 -2.3(16) . . . . ?
C87 C77 C78 C79 -166.8(9) . . . . ?
C87 C86 C91 C90 0(2) . . . . ?
C87 C86 C91 C92 -178.3(12) . . . . ?
C87 C88 C89 C90 1.1(15) . . . . ?
C87 C88 C89 C94 179.8(9) . . . . ?
C88 C89 C90 O11 -176.7(9) . . . . ?
C88 C89 C90 C91 0.7(16) . . . . ?
C88 C89 C94 C95 29.1(13) . . . . ?
C88 C89 C94 C104 -97.0(12) . . . . ?
C89 C90 C91 C86 -1.1(19) . . . . ?
C89 C90 C91 C92 177.0(12) . . . . ?
C89 C94 C95 C96 172.1(9) . . . . ?
C89 C94 C104 C103 -105.7(12) . . . . ?
C89 C94 C104 C105 78.7(13) . . . . ?
C90 O11 C101 C102 136.5(11) . . . . ?
C90 C89 C94 C95 -152.2(10) . . . . ?
C90 C89 C94 C104 81.7(11) . . . . ?
C91 C86 C87 C77 -176.9(11) . . . . ?
C91 C86 C87 C88 1.9(18) . . . . ?
C94 C89 C90 O11 4.5(14) . . . . ?
C94 C89 C90 C91 -178.1(10) . . . . ?
C94 C95 C96 C97 167.8(10) . . . . ?
C94 C104 C105 C106 175.5(11) . . . . ?
C95 C94 C104 C103 127.4(12) . . . . ?
C95 C94 C104 C105 -48.1(15) . . . . ?
C95 C96 C97 C98 175.3(13) . . . . ?
C96 C97 C98 C99 -175.4(17) . . . . ?
C97 C98 C99 C100 177(2) . . . . ?
C101 O11 C90 C89 -96.5(13) . . . . ?
C101 O11 C90 C91 86.1(14) . . . . ?
C102 O12 C103 C104 104.8(12) . . . . ?
C102 O12 C103 C108 -77.6(14) . . . . ?
C103 O12 C102 C101 -54.3(13) . . . . ?
C103 C104 C105 C106 -0.3(17) . . . . ?
C104 C94 C95 C96 -63.8(13) . . . . ?
C104 C103 C108 C107 2.4(17) . . . . ?
C104 C103 C108 C109 178.0(11) . . . . ?
C104 C105 C106 C107 1.4(16) . . . . ?
C104 C105 C106 C111 -176.8(10) . . . . ?
C105 C106 C107 O13 -176.3(10) . . . . ?
C105 C106 C107 C108 -0.5(16) . . . . ?
C105 C106 C111 C112 49.2(13) . . . . ?
C105 C106 C111 C121 -74.8(12) . . . . ?
C106 C107 C108 C103 -1.3(17) . . . . ?
C106 C107 C108 C109 -176.8(11) . . . . ?
C106 C111 C112 C113 61.6(12) . . . . ?
C106 C111 C121 C120 -85.3(10) . . . . ?
C106 C111 C121 C122 93.5(10) . . . . ?
C107 O13 C118 C119 55.4(10) . . . . ?
C107 C106 C111 C112 -128.8(10) . . . . ?
C107 C106 C111 C121 107.1(11) . . . . ?
C108 C103 C104 C94 -177.3(11) . . . . ?
C108 C103 C104 C105 -1.7(17) . . . . ?
C111 C106 C107 O13 1.8(15) . . . . ?
C111 C106 C107 C108 177.6(10) . . . . ?
C111 C112 C113 C114 178.5(11) . . . . ?
C111 C121 C122 C123 177.4(8) . . . . ?
C112 C111 C121 C120 149.5(8) . . . . ?
C112 C111 C121 C122 -31.6(12) . . . . ?
C112 C113 C114 C115 -175.1(16) . . . . ?
C113 C114 C115 C116 174.8(17) . . . . ?
C114 C115 C116 C117 178(2) . . . . ?
C118 O13 C107 C106 -105.6(11) . . . . ?
C118 O13 C107 C108 78.5(12) . . . . ?
C119 O14 C120 C121 93.6(11) . . . . ?
C119 O14 C120 C125 -88.8(10) . . . . ?
C120 O14 C119 C118 -136.1(9) . . . . ?
C120 C121 C122 C123 -3.7(13) . . . . ?
C121 C111 C112 C113 -174.3(9) . . . . ?
C121 C120 C125 C124 3.0(13) . . . . ?
C121 C120 C125 C126 -176.5(8) . . . . ?
C121 C122 C123 C124 2.9(13) . . . . ?
C121 C122 C123 C128 -177.0(8) . . . . ?
C122 C123 C124 O15 -178.5(8) . . . . ?
C122 C123 C124 C125 1.1(13) . . . . ?
C122 C123 C128 C70 -95.7(11) . . . . ?
C122 C123 C128 C129 29.8(13) . . . . ?
C123 C124 C125 C120 -3.9(14) . . . . ?
C123 C124 C125 C126 175.6(9) . . . . ?
C123 C128 C129 C130 60.3(13) . . . . ?
C124 O15 C135 C136 136.1(10) . . . . ?
C124 C123 C128 C70 84.4(11) . . . . ?
C124 C123 C128 C129 -150.1(9) . . . . ?
C125 C120 C121 C111 179.6(8) . . . . ?
C125 C120 C121 C122 0.7(13) . . . . ?
C128 C70 C71 C72 177.2(10) . . . . ?
C128 C123 C124 O15 1.4(13) . . . . ?
C128 C123 C124 C125 -179.0(9) . . . . ?
C128 C129 C130 C131 176.7(14) . . . . ?
C129 C130 C131 C132 169.7(16) . . . . ?
C130 C131 C132 C133 -155.5(17) . . . . ?
C131 C132 C133 C134 -91(3) . . . . ?
C135 O15 C124 C123 -91.7(11) . . . . ?
C135 O15 C124 C125 88.8(11) . . . . ?
C136 O16 C69 C70 106.4(12) . . . . ?
C136 O16 C69 C74 -77.9(12) . . . . ?
C147 N5 C146 O21 179(2) . . . . ?
C148 N5 C146 O21 1(3) . . . . ?
O1 C5 C6 C1 177.9(10) . . . . ?
O1 C5 C6 C7 0.0(17) . . . . ?
O1 C16 C17 O2 -56.9(15) . . . . ?
O2 C18 C19 C9 -7.7(16) . . . . ?
O2 C18 C19 C20 175.5(10) . . . . ?
O2 C18 C23 C22 -174.6(11) . . . . ?
O2 C18 C23 C24 6.4(19) . . . . ?
O3 C22 C23 C18 176.0(11) . . . . ?
O3 C22 C23 C24 -5.0(18) . . . . ?
O3 C33 C34 O4 61.8(13) . . . . ?
O4 C35 C36 C26 -0.6(13) . . . . ?
O4 C35 C36 C37 178.8(8) . . . . ?
O4 C35 C40 C39 -177.7(8) . . . . ?
O4 C35 C40 C41 2.9(13) . . . . ?
O5 C39 C40 C35 175.2(7) . . . . ?
O5 C39 C40 C41 -5.4(12) . . . . ?
O5 C50 C51 O6 -63.8(10) . . . . ?
O6 C52 C53 C43 -2.7(13) . . . . ?
O6 C52 C53 C54 176.6(8) . . . . ?
O6 C52 C57 C56 -175.6(8) . . . . ?
O6 C52 C57 C58 2.7(13) . . . . ?
O7 C56 C57 C52 175.3(8) . . . . ?
O7 C56 C57 C58 -2.9(14) . . . . ?
O7 C67 C68 O8 60.9(10) . . . . ?
O8 C1 C2 C3 177.9(9) . . . . ?
O8 C1 C2 C60 -0.6(15) . . . . ?
O8 C1 C6 C5 -176.3(10) . . . . ?
O8 C1 C6 C7 1.6(16) . . . . ?
C1 O8 C68 C67 -135.7(8) . . . . ?
C1 C2 C3 C4 -2.6(16) . . . . ?
C1 C2 C60 C55 -87.4(11) . . . . ?
C1 C2 C60 C61 145.6(10) . . . . ?
C2 C1 C6 C5 -0.2(17) . . . . ?
C2 C1 C6 C7 177.8(11) . . . . ?
C2 C3 C4 C5 1.7(17) . . . . ?
C2 C3 C4 C9 -177.1(10) . . . . ?
C2 C60 C61 C62 -167.8(10) . . . . ?
C3 C2 C60 C55 94.2(11) . . . . ?
C3 C2 C60 C61 -32.8(14) . . . . ?
C3 C4 C5 O1 -178.6(10) . . . . ?
C3 C4 C5 C6 0.1(18) . . . . ?
C3 C4 C9 C10 35.8(15) . . . . ?
C3 C4 C9 C19 -94.8(14) . . . . ?
C4 C5 C6 C1 -0.8(18) . . . . ?
C4 C5 C6 C7 -178.8(12) . . . . ?
C4 C9 C10 C11 58.3(15) . . . . ?
C4 C9 C19 C18 -98.0(12) . . . . ?
C4 C9 C19 C20 78.6(14) . . . . ?
C5 O1 C16 C17 136.6(10) . . . . ?
C5 C4 C9 C10 -142.9(12) . . . . ?
C5 C4 C9 C19 86.4(13) . . . . ?
C6 C1 C2 C3 1.8(16) . . . . ?
C6 C1 C2 C60 -176.7(10) . . . . ?
C9 C4 C5 O1 0.2(17) . . . . ?
C9 C4 C5 C6 178.9(11) . . . . ?
C9 C10 C11 C12 178.7(14) . . . . ?
C9 C19 C20 C21 179.6(10) . . . . ?
C10 C9 C19 C18 130.6(12) . . . . ?
C10 C9 C19 C20 -52.8(14) . . . . ?
C10 C11 C12 C13 81(2) . . . . ?
C11 C12 C13 C14 179(2) . . . . ?
C12 C13 C14 C15 178(3) . . . . ?
C16 O1 C5 C4 -94.7(13) . . . . ?
C16 O1 C5 C6 86.5(13) . . . . ?
C17 O2 C18 C19 110.2(14) . . . . ?
C17 O2 C18 C23 -77.0(15) . . . . ?
C18 O2 C17 C16 -59.2(18) . . . . ?
C18 C19 C20 C21 -3.5(16) . . . . ?
C19 C9 C10 C11 -171.6(11) . . . . ?
C19 C18 C23 C22 -2.2(18) . . . . ?
C19 C18 C23 C24 178.8(11) . . . . ?
C19 C20 C21 C22 3.5(17) . . . . ?
C19 C20 C21 C26 -179.6(10) . . . . ?
C20 C21 C22 O3 -176.4(10) . . . . ?
C20 C21 C22 C23 -2.7(17) . . . . ?
C20 C21 C26 C27 50.9(13) . . . . ?
C20 C21 C26 C36 -75.6(14) . . . . ?
C21 C22 C23 C18 2.1(18) . . . . ?
C21 C22 C23 C24 -178.9(12) . . . . ?
C21 C26 C27 C28 73.8(12) . . . . ?
C21 C26 C36 C35 -86.1(12) . . . . ?
C21 C26 C36 C37 94.5(12) . . . . ?
C22 O3 C33 C34 52.7(13) . . . . ?
C22 C21 C26 C27 -132.3(11) . . . . ?
C22 C21 C26 C36 101.2(12) . . . . ?
C23 C18 C19 C9 179.6(11) . . . . ?
C23 C18 C19 C20 2.8(16) . . . . ?
C26 C21 C22 O3 6.7(16) . . . . ?
C26 C21 C22 C23 -179.6(10) . . . . ?
C26 C27 C28 C29 158.4(11) . . . . ?
C26 C36 C37 C38 178.2(8) . . . . ?
C27 C26 C36 C35 145.6(9) . . . . ?
C27 C26 C36 C37 -33.8(13) . . . . ?
C27 C28 C29 C30 -171.1(12) . . . . ?
C28 C29 C30 C31 169.5(15) . . . . ?
C29 C30 C31 C32 179.0(14) . . . . ?
C33 O3 C22 C21 -108.5(13) . . . . ?
C33 O3 C22 C23 77.6(13) . . . . ?
C34 O4 C35 C36 92.7(11) . . . . ?
C34 O4 C35 C40 -88.7(11) . . . . ?
C35 O4 C34 C33 -136.7(10) . . . . ?
C35 C36 C37 C38 -1.2(13) . . . . ?
C36 C26 C27 C28 -160.2(9) . . . . ?
C36 C35 C40 C39 0.9(13) . . . . ?
C36 C35 C40 C41 -178.4(9) . . . . ?
C36 C37 C38 C39 1.0(13) . . . . ?
C36 C37 C38 C43 -177.4(8) . . . . ?
C37 C38 C39 O5 -176.1(8) . . . . ?
C37 C38 C39 C40 0.2(13) . . . . ?
C37 C38 C43 C44 30.0(12) . . . . ?
C37 C38 C43 C53 -97.6(10) . . . . ?
C38 C39 C40 C35 -1.1(13) . . . . ?
C38 C39 C40 C41 178.3(8) . . . . ?
C38 C43 C44 C45 170.1(11) . . . . ?
C38 C43 C53 C52 -103.4(9) . . . . ?
C38 C43 C53 C54 77.4(11) . . . . ?
C39 O5 C50 C51 138.9(8) . . . . ?
C39 C38 C43 C44 -148.4(8) . . . . ?
C39 C38 C43 C53 84.0(10) . . . . ?
C40 C35 C36 C26 -179.2(9) . . . . ?
C40 C35 C36 C37 0.2(13) . . . . ?
C43 C38 C39 O5 2.4(12) . . . . ?
C43 C38 C39 C40 178.6(8) . . . . ?
C43 C44 C45 C46 -166.0(14) . . . . ?
C43 C53 C54 C55 176.7(9) . . . . ?
C44 C43 C53 C52 127.1(9) . . . . ?
C44 C43 C53 C54 -52.1(12) . . . . ?
C44 C45 C46 C47 174.0(19) . . . . ?
C45 C46 C47 C48 -167(2) . . . . ?
C46 C47 C48 C49 74(4) . . . . ?
C50 O5 C39 C38 -93.3(10) . . . . ?
C50 O5 C39 C40 90.3(10) . . . . ?
C51 O6 C52 C53 105.9(9) . . . . ?
C51 O6 C52 C57 -78.1(10) . . . . ?
C52 O6 C51 C50 -52.7(10) . . . . ?
C52 C53 C54 C55 -2.5(15) . . . . ?
C53 C43 C44 C45 -63.2(13) . . . . ?
C53 C52 C57 C56 0.4(13) . . . . ?
C53 C52 C57 C58 178.7(8) . . . . ?
C53 C54 C55 C56 3.3(15) . . . . ?
C53 C54 C55 C60 -178.7(9) . . . . ?
C54 C55 C56 O7 -177.2(8) . . . . ?
C54 C55 C56 C57 -2.3(14) . . . . ?
C54 C55 C60 C2 -74.9(11) . . . . ?
C54 C55 C60 C61 54.6(13) . . . . ?
C55 C56 C57 C52 0.5(14) . . . . ?
C55 C56 C57 C58 -177.7(9) . . . . ?
C55 C60 C61 C62 65.0(12) . . . . ?
C56 O7 C67 C68 56.2(11) . . . . ?
C56 C55 C60 C2 103.0(11) . . . . ?
C56 C55 C60 C61 -127.6(10) . . . . ?
C57 C52 C53 C43 -178.7(8) . . . . ?
C57 C52 C53 C54 0.5(13) . . . . ?
C60 C2 C3 C4 175.9(10) . . . . ?
C60 C55 C56 O7 4.9(14) . . . . ?
C60 C55 C56 C57 179.8(9) . . . . ?
C60 C61 C62 C63 176.5(12) . . . . ?
C61 C62 C63 C64 67(2) . . . . ?
C62 C63 C64 C65 170(2) . . . . ?
C63 C64 C65 C66 171(2) . . . . ?
C67 O7 C56 C55 -107.3(10) . . . . ?
C67 O7 C56 C57 77.6(11) . . . . ?
C68 O8 C1 C2 92.0(12) . . . . ?
C68 O8 C1 C6 -91.8(11) . . . . ?
C156 N7 C155 O23 2(4) . . . . ?
C157 N7 C155 O23 168(4) . . . . ?
C141 N2 C140 O18 -175.3(19) . . . . ?
C142 N2 C140 O18 -3(3) . . . . ?
C150 N3 C149 O19 174(2) . . . . ?
C151 N3 C149 O19 -4(4) . . . . ?
C153 N6 C152 O22 3(2) . . . . ?
C154 N6 C152 O22 -177.2(14) . . . . ?
C144 N4 C143 O20 -3(3) . . . . ?
C145 N4 C143 O20 176.4(17) . . . . ?
C138 N1 C137 O17 177(2) . . . . ?
C139 N1 C137 O17 -13(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-10 4 -4 0.0213 -10.0000 4.0000 -4.0002 -0.7265 0.6561 -0.0380
10 -4 4 0.0180 10.0000 -4.0000 4.0002 0.7265 -0.6561 0.0380
10 0 6 0.0155 10.0000 0.0000 6.0002 0.6702 -0.6650 0.3692
8 6 6 0.0313 8.0000 6.0001 6.0002 0.4976 -0.4465 0.7583
-1 -12 -4 0.0559 -1.0000 -12.0000 -4.0000 0.0356 -0.0495 -0.9817
6 -4 -13 0.0250 6.0000 -4.0000 -12.9998 0.8312 0.4111 -0.3839
-7 -1 12 0.0394 -7.0000 -1.0000 11.9998 -0.8814 -0.4487 -0.0276
3 12 2 0.0418 3.0000 12.0000 2.0001 0.1801 0.0921 0.9954
6 8 -7 0.0351 6.0000 8.0000 -6.9998 0.6622 0.3844 0.6097
-4 7 12 0.0476 -4.0000 7.0000 11.9998 -0.6449 -0.3477 0.6366
-1 -4 -15 0.0246 -1.0000 -4.0000 -14.9999 0.3059 0.7558 -0.6010
0 7 -14 0.0219 -0.0000 7.0000 -13.9999 0.3482 0.9447 0.2509
8 -4 10 0.0246 8.0000 -4.0000 10.0001 0.4087 -0.9182 0.0994

_olex2_submission_special_instructions 'No special instructions were received'
