# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_mo_70612aa
_database_code_depnum_ccdc_archive 'CCDC 1887341'
loop_
_audit_author_name
_audit_author_address
'Zhan-Ting Li'
;Fudan University
China
;
_audit_update_record             
;
2018-12-26 deposited with the CCDC.	2019-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H46 N4 O6'
_chemical_formula_weight         606.75

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   23.393(10)
_cell_length_b                   9.538(4)
_cell_length_c                   15.832(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3532(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    2638
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      20.50

_exptl_crystal_description       block
_exptl_crystal_colour            block
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.078
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19796
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.741
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3205
_reflns_number_gt                1475
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1377P)²+1.3620P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3205
_refine_ls_number_parameters     208
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_gt           0.0866
_refine_ls_wR_factor_ref         0.2946
_refine_ls_wR_factor_gt          0.2404
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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
N1 N 0.63090(16) 1.0050(4) 0.1930(2) 0.0633(11) Uani 1 1 d . . . . .
H1A H 0.6359(19) 0.991(5) 0.140(3) 0.092(17) Uiso 1 1 d . . . . .
N2 N 0.5276(2) 0.8690(6) 0.3496(3) 0.0998(15) Uani 1 1 d . . . . .
O1 O 0.66838(16) 1.1157(4) 0.30645(19) 0.0975(13) Uani 1 1 d . . . . .
O2 O 0.67299(13) 1.0874(3) 0.04309(16) 0.0737(10) Uani 1 1 d . . . . .
O3 O 0.58152(15) 0.8087(3) 0.10313(19) 0.0860(11) Uani 1 1 d . . . . .
C1 C 0.7500 1.2500 0.2139(3) 0.0578(15) Uani 1 2 d S T P . .
H1 H 0.7500 1.2500 0.2733 0.069 Uiso 1 2 calc R U P . .
C2 C 0.70931(18) 1.1690(4) 0.1740(2) 0.0552(11) Uani 1 1 d . . . . .
C3 C 0.71087(19) 1.1689(5) 0.0844(3) 0.0603(12) Uani 1 1 d . . . . .
C4 C 0.7500 1.2500 0.0431(3) 0.0631(16) Uani 1 2 d S T P . .
H4 H 0.7500 1.2500 -0.0163 0.076 Uiso 1 2 calc R U P . .
C5 C 0.6681(2) 1.0942(5) 0.2294(3) 0.0654(12) Uani 1 1 d . . . . .
C6 C 0.5703(2) 0.9434(6) 0.3133(3) 0.0867(16) Uani 1 1 d . . . . .
H6 H 0.5886 1.0120 0.3463 0.104 Uiso 1 1 calc R U . . .
C7 C 0.5888(2) 0.9258(5) 0.2314(3) 0.0636(12) Uani 1 1 d . . . . .
C8 C 0.5622(2) 0.8199(5) 0.1848(3) 0.0675(13) Uani 1 1 d . . . . .
C9 C 0.5195(2) 0.7435(6) 0.2208(3) 0.0832(15) Uani 1 1 d . . . . .
H9 H 0.5012 0.6718 0.1904 0.100 Uiso 1 1 calc R U . . .
C10 C 0.5036(2) 0.7732(6) 0.3025(4) 0.0891(16) Uani 1 1 d . . . . .
H10 H 0.4734 0.7212 0.3260 0.107 Uiso 1 1 calc R U . . .
C11 C 0.5718(2) 0.6789(5) 0.0583(3) 0.0846(16) Uani 1 1 d . . . . .
H11A H 0.5783 0.6940 -0.0022 0.101 Uiso 1 1 calc R U . . .
H11B H 0.5319 0.6501 0.0658 0.101 Uiso 1 1 calc R U . . .
C12 C 0.6099(2) 0.5658(6) 0.0885(4) 0.0919(17) Uani 1 1 d . . . . .
H12 H 0.5992 0.5451 0.1477 0.110 Uiso 1 1 calc R U . . .
C13 C 0.6008(3) 0.4322(5) 0.0374(3) 0.0921(17) Uani 1 1 d . . . . .
H13A H 0.5601 0.4158 0.0304 0.138 Uiso 1 1 calc R U . . .
H13B H 0.6178 0.3535 0.0669 0.138 Uiso 1 1 calc R U . . .
H13C H 0.6185 0.4423 -0.0176 0.138 Uiso 1 1 calc R U . . .
C14 C 0.6728(3) 0.6062(7) 0.0883(5) 0.124(2) Uani 1 1 d . . . . .
H14A H 0.6853 0.6224 0.0307 0.186 Uiso 1 1 calc R U . . .
H14B H 0.6952 0.5310 0.1129 0.186 Uiso 1 1 calc R U . . .
H14C H 0.6781 0.6911 0.1211 0.186 Uiso 1 1 calc R U . . .
C15 C 0.6760(3) 1.0843(6) -0.0491(3) 0.0944(18) Uani 1 1 d . . . . .
H15A H 0.6722 1.1795 -0.0717 0.113 Uiso 1 1 calc R U . . .
H15B H 0.7129 1.0462 -0.0672 0.113 Uiso 1 1 calc R U . . .
C16 C 0.6301(3) 0.9974(7) -0.0799(3) 0.112(2) Uani 1 1 d . . . . .
H16 H 0.6341 0.9046 -0.0526 0.135 Uiso 1 1 calc R U . . .
C17 C 0.5715(3) 1.0515(8) -0.0590(4) 0.128(3) Uani 1 1 d . . . . .
H17A H 0.5703 1.0789 0.0000 0.192 Uiso 1 1 calc R U . . .
H17B H 0.5435 0.9784 -0.0692 0.192 Uiso 1 1 calc R U . . .
H17C H 0.5630 1.1320 -0.0942 0.192 Uiso 1 1 calc R U . . .
C18 C 0.6394(4) 0.9760(10) -0.1759(3) 0.167(4) Uani 1 1 d . U . . .
H18A H 0.6370 1.0657 -0.2045 0.251 Uiso 1 1 calc R U . . .
H18B H 0.6101 0.9137 -0.1978 0.251 Uiso 1 1 calc R U . . .
H18C H 0.6768 0.9350 -0.1855 0.251 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C5 1.346(6) . ?
N1 C7 1.382(6) . ?
N1 H1A 0.85(5) . ?
N2 C10 1.306(7) . ?
N2 C6 1.353(7) . ?
O1 C5 1.237(5) . ?
O2 C3 1.348(5) . ?
O2 C15 1.461(5) . ?
O3 C8 1.373(5) . ?
O3 C11 1.445(5) . ?
C1 C2 1.379(4) . ?
C1 C2 1.379(5) 2_675 ?
C1 H1 0.9400 . ?
C2 C3 1.420(5) . ?
C2 C5 1.486(6) . ?
C3 C4 1.365(5) . ?
C4 C3 1.365(5) 2_675 ?
C4 H4 0.9400 . ?
C6 C7 1.378(6) . ?
C6 H6 0.9400 . ?
C7 C8 1.396(6) . ?
C8 C9 1.362(7) . ?
C9 C10 1.375(7) . ?
C9 H9 0.9400 . ?
C10 H10 0.9400 . ?
C11 C12 1.479(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C14 1.520(8) . ?
C12 C13 1.525(7) . ?
C12 H12 0.9900 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 C16 1.441(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 C17 1.501(9) . ?
C16 C18 1.548(8) . ?
C16 H16 0.9900 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 N1 C7 128.2(4) . . ?
C5 N1 H1A 115(3) . . ?
C7 N1 H1A 116(3) . . ?
C10 N2 C6 116.2(5) . . ?
C3 O2 C15 117.7(4) . . ?
C8 O3 C11 118.5(4) . . ?
C2 C1 C2 125.5(5) . 2_675 ?
C2 C1 H1 117.2 . . ?
C2 C1 H1 117.2 2_675 . ?
C1 C2 C3 116.1(4) . . ?
C1 C2 C5 116.6(4) . . ?
C3 C2 C5 127.3(4) . . ?
O2 C3 C4 122.4(4) . . ?
O2 C3 C2 117.9(4) . . ?
C4 C3 C2 119.7(4) . . ?
C3 C4 C3 122.8(5) 2_675 . ?
C3 C4 H4 118.6 2_675 . ?
C3 C4 H4 118.6 . . ?
O1 C5 N1 122.0(5) . . ?
O1 C5 C2 119.9(4) . . ?
N1 C5 C2 118.1(4) . . ?
N2 C6 C7 124.6(5) . . ?
N2 C6 H6 117.7 . . ?
C7 C6 H6 117.7 . . ?
C6 C7 N1 124.8(5) . . ?
C6 C7 C8 116.5(5) . . ?
N1 C7 C8 118.7(4) . . ?
C9 C8 O3 126.4(4) . . ?
C9 C8 C7 119.5(5) . . ?
O3 C8 C7 114.1(4) . . ?
C8 C9 C10 118.8(5) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N2 C10 C9 124.4(5) . . ?
N2 C10 H10 117.8 . . ?
C9 C10 H10 117.8 . . ?
O3 C11 C12 111.8(4) . . ?
O3 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
O3 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 C14 113.4(5) . . ?
C11 C12 C13 110.7(4) . . ?
C14 C12 C13 110.3(5) . . ?
C11 C12 H12 107.4 . . ?
C14 C12 H12 107.4 . . ?
C13 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 O2 108.3(4) . . ?
C16 C15 H15A 110.0 . . ?
O2 C15 H15A 110.0 . . ?
C16 C15 H15B 110.0 . . ?
O2 C15 H15B 110.0 . . ?
H15A C15 H15B 108.4 . . ?
C15 C16 C17 114.0(6) . . ?
C15 C16 C18 107.7(5) . . ?
C17 C16 C18 113.0(6) . . ?
C15 C16 H16 107.3 . . ?
C17 C16 H16 107.3 . . ?
C18 C16 H16 107.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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
C2 C1 C2 C3 1.1(2) 2_675 . . . ?
C2 C1 C2 C5 -177.7(4) 2_675 . . . ?
C15 O2 C3 C4 1.8(6) . . . . ?
C15 O2 C3 C2 -178.1(4) . . . . ?
C1 C2 C3 O2 177.8(3) . . . . ?
C5 C2 C3 O2 -3.6(6) . . . . ?
C1 C2 C3 C4 -2.1(5) . . . . ?
C5 C2 C3 C4 176.4(3) . . . . ?
O2 C3 C4 C3 -178.8(4) . . . 2_675 ?
C2 C3 C4 C3 1.1(3) . . . 2_675 ?
C7 N1 C5 O1 0.1(7) . . . . ?
C7 N1 C5 C2 -179.3(4) . . . . ?
C1 C2 C5 O1 6.1(6) . . . . ?
C3 C2 C5 O1 -172.5(4) . . . . ?
C1 C2 C5 N1 -174.5(3) . . . . ?
C3 C2 C5 N1 7.0(6) . . . . ?
C10 N2 C6 C7 0.9(8) . . . . ?
N2 C6 C7 N1 177.5(5) . . . . ?
N2 C6 C7 C8 -2.2(8) . . . . ?
C5 N1 C7 C6 12.6(7) . . . . ?
C5 N1 C7 C8 -167.7(4) . . . . ?
C11 O3 C8 C9 -23.0(7) . . . . ?
C11 O3 C8 C7 160.1(4) . . . . ?
C6 C7 C8 C9 1.6(6) . . . . ?
N1 C7 C8 C9 -178.1(4) . . . . ?
C6 C7 C8 O3 178.8(4) . . . . ?
N1 C7 C8 O3 -0.9(6) . . . . ?
O3 C8 C9 C10 -176.7(4) . . . . ?
C7 C8 C9 C10 0.1(7) . . . . ?
C6 N2 C10 C9 1.0(8) . . . . ?
C8 C9 C10 N2 -1.5(8) . . . . ?
C8 O3 C11 C12 -73.8(6) . . . . ?
O3 C11 C12 C14 -52.8(7) . . . . ?
O3 C11 C12 C13 -177.3(5) . . . . ?
C3 O2 C15 C16 -176.9(5) . . . . ?
O2 C15 C16 C17 62.6(7) . . . . ?
O2 C15 C16 C18 -171.2(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O2 0.85(5) 1.99(5) 2.687(5) 138(5) .

_refine_diff_density_max         0.320
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.050

####################################################################### 
# 
# 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_mo_71203a
_database_code_depnum_ccdc_archive 'CCDC 1887363'
loop_
_audit_author_name
_audit_author_address
'Zhanting Li'
;Fudan University
China
;
_audit_update_record             
;
2018-12-26 deposited with the CCDC.	2019-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H24 F6 I2 N2 O4'
_chemical_formula_weight         820.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.727(2)
_cell_length_b                   11.231(3)
_cell_length_c                   17.977(5)
_cell_angle_alpha                73.848(4)
_cell_angle_beta                 79.220(4)
_cell_angle_gamma                86.104(4)
_cell_volume                     1471.8(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    5774
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.31

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_F_000             796
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.212
_shelx_estimated_absorpt_T_min   0.350
_shelx_estimated_absorpt_T_max   0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10247
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.888
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             6295
_reflns_number_gt                5304
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1136P)²+0.0355P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6295
_refine_ls_number_parameters     391
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1596
_refine_ls_wR_factor_gt          0.1425
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.40571(4) 1.59779(3) 0.30505(2) 0.03845(13) Uani 1 1 d . . . . .
I2 I 0.50679(5) 1.31057(3) 1.00693(2) 0.05374(15) Uani 1 1 d . . . . .
N1 N 0.7163(5) 1.0464(3) 0.49740(19) 0.0274(7) Uani 1 1 d D . . . .
H1 H 0.705(10) 0.999(7) 0.465(4) 0.10(3) Uiso 1 1 d D . . . .
N2 N 0.8318(5) 0.9514(3) 0.7698(2) 0.0297(7) Uani 1 1 d D . . . .
H2 H 0.884(7) 0.905(5) 0.802(3) 0.043(15) Uiso 1 1 d D . . . .
O1 O 0.6640(4) 1.2308(3) 0.52809(18) 0.0380(7) Uani 1 1 d . . . . .
O2 O 0.6717(5) 1.1304(3) 0.75164(19) 0.0445(8) Uani 1 1 d . . . . .
O3 O 0.9656(4) 0.7383(3) 0.75614(17) 0.0357(7) Uani 1 1 d . . . . .
O4 O 0.8359(4) 0.8299(3) 0.48966(16) 0.0318(6) Uani 1 1 d . . . . .
F1 F 0.4283(3) 1.4090(3) 0.19912(14) 0.0410(6) Uani 1 1 d . . . . .
F2 F 0.5442(4) 1.1745(3) 0.22050(14) 0.0429(6) Uani 1 1 d . . . . .
F3 F 0.6574(4) 1.0509(2) 0.35118(15) 0.0406(6) Uani 1 1 d . . . . .
F4 F 0.6858(5) 1.0697(3) 1.10659(17) 0.0606(9) Uani 1 1 d . . . . .
F5 F 0.8551(5) 0.8750(3) 1.06599(17) 0.0623(9) Uani 1 1 d . . . . .
F6 F 0.9039(4) 0.8577(3) 0.91958(15) 0.0468(7) Uani 1 1 d . . . . .
C1 C 0.7823(5) 0.9729(3) 0.5635(2) 0.0227(7) Uani 1 1 d . . . . .
C2 C 0.7781(5) 1.0079(4) 0.6324(2) 0.0275(8) Uani 1 1 d . . . . .
H2A H 0.7339 1.0866 0.6358 0.033 Uiso 1 1 calc R U . . .
C3 C 0.8388(5) 0.9272(4) 0.6954(2) 0.0265(8) Uani 1 1 d . . . . .
C4 C 0.9100(5) 0.8115(4) 0.6899(2) 0.0257(7) Uani 1 1 d . . . . .
C5 C 0.9165(5) 0.7763(4) 0.6208(2) 0.0270(8) Uani 1 1 d . . . . .
H5 H 0.9670 0.6995 0.6164 0.032 Uiso 1 1 calc R U . . .
C6 C 0.8482(5) 0.8554(4) 0.5590(2) 0.0250(7) Uani 1 1 d . . . . .
C7 C 0.6641(5) 1.1669(4) 0.4831(2) 0.0258(7) Uani 1 1 d . . . . .
C8 C 0.6011(5) 1.2242(4) 0.4056(2) 0.0251(7) Uani 1 1 d . . . . .
C9 C 0.5412(5) 1.3467(4) 0.3933(2) 0.0262(8) Uani 1 1 d . . . . .
H9 H 0.5394 1.3863 0.4332 0.031 Uiso 1 1 calc R U . . .
C10 C 0.4839(5) 1.4127(4) 0.3243(2) 0.0261(7) Uani 1 1 d . . . . .
C11 C 0.4852(5) 1.3509(4) 0.2664(2) 0.0321(9) Uani 1 1 d . . . . .
C12 C 0.5422(5) 1.2322(4) 0.2768(2) 0.0296(8) Uani 1 1 d . . . . .
C13 C 0.6007(5) 1.1675(4) 0.3457(2) 0.0273(8) Uani 1 1 d . . . . .
C14 C 0.7455(6) 1.0466(4) 0.7934(2) 0.0301(8) Uani 1 1 d . . . . .
C15 C 0.7417(5) 1.0467(4) 0.8778(2) 0.0300(8) Uani 1 1 d . . . . .
C16 C 0.6544(6) 1.1464(4) 0.9003(2) 0.0336(9) Uani 1 1 d . . . . .
H16 H 0.6069 1.2091 0.8625 0.040 Uiso 1 1 calc R U . . .
C17 C 0.6343(6) 1.1571(4) 0.9762(3) 0.0354(9) Uani 1 1 d . . . . .
C18 C 0.7027(6) 1.0662(5) 1.0314(2) 0.0396(10) Uani 1 1 d . . . . .
C19 C 0.7903(6) 0.9639(5) 1.0120(3) 0.0397(10) Uani 1 1 d . . . . .
C20 C 0.8107(6) 0.9571(4) 0.9350(2) 0.0349(9) Uani 1 1 d . . . . .
C21 C 1.0020(6) 0.6082(4) 0.7630(2) 0.0303(8) Uani 1 1 d . . . . .
H21A H 1.1198 0.5970 0.7340 0.036 Uiso 1 1 calc R U . . .
H21B H 0.9158 0.5747 0.7409 0.036 Uiso 1 1 calc R U . . .
C22 C 0.9914(7) 0.5405(4) 0.8496(3) 0.0376(9) Uani 1 1 d . . . . .
H22 H 0.8728 0.5566 0.8775 0.045 Uiso 1 1 calc R U . . .
C23 C 1.1257(7) 0.5850(6) 0.8866(3) 0.0525(13) Uani 1 1 d . . . . .
H23A H 1.1035 0.5474 0.9430 0.079 Uiso 1 1 calc R U . . .
H23B H 1.1168 0.6745 0.8762 0.079 Uiso 1 1 calc R U . . .
H23C H 1.2431 0.5615 0.8645 0.079 Uiso 1 1 calc R U . . .
C24 C 1.0097(10) 0.4023(5) 0.8575(4) 0.0660(16) Uani 1 1 d . . . . .
H24A H 1.1262 0.3838 0.8317 0.099 Uiso 1 1 calc R U . . .
H24B H 0.9215 0.3776 0.8330 0.099 Uiso 1 1 calc R U . . .
H24C H 0.9930 0.3572 0.9127 0.099 Uiso 1 1 calc R U . . .
C25 C 0.8840(5) 0.7077(4) 0.4820(2) 0.0280(8) Uani 1 1 d . . . . .
H25A H 0.8357 0.6455 0.5304 0.034 Uiso 1 1 calc R U . . .
H25B H 1.0126 0.6977 0.4727 0.034 Uiso 1 1 calc R U . . .
C26 C 0.8103(5) 0.6904(4) 0.4131(2) 0.0291(8) Uani 1 1 d . . . . .
H26 H 0.6810 0.7033 0.4230 0.035 Uiso 1 1 calc R U . . .
C27 C 0.8875(7) 0.7825(4) 0.3359(3) 0.0417(10) Uani 1 1 d . . . . .
H27A H 0.8716 0.8661 0.3418 0.063 Uiso 1 1 calc R U . . .
H27B H 0.8279 0.7755 0.2945 0.063 Uiso 1 1 calc R U . . .
H27C H 1.0123 0.7647 0.3225 0.063 Uiso 1 1 calc R U . . .
C28 C 0.8495(7) 0.5579(5) 0.4084(3) 0.0426(11) Uani 1 1 d . . . . .
H28A H 0.9759 0.5452 0.3961 0.064 Uiso 1 1 calc R U . . .
H28B H 0.7944 0.5432 0.3675 0.064 Uiso 1 1 calc R U . . .
H28C H 0.8031 0.5008 0.4585 0.064 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C10 2.077(4) . ?
I2 C17 2.083(4) . ?
N1 C7 1.354(5) . ?
N1 C1 1.407(5) . ?
N1 H1 0.91(4) . ?
N2 C14 1.347(5) . ?
N2 C3 1.429(5) . ?
N2 H2 0.80(4) . ?
O1 C7 1.220(5) . ?
O2 C14 1.212(5) . ?
O3 C4 1.370(5) . ?
O3 C21 1.444(5) . ?
O4 C6 1.374(4) . ?
O4 C25 1.434(5) . ?
F1 C11 1.343(5) . ?
F2 C12 1.342(4) . ?
F3 C13 1.335(4) . ?
F4 C18 1.345(5) . ?
F5 C19 1.328(5) . ?
F6 C20 1.353(5) . ?
C1 C2 1.393(5) . ?
C1 C6 1.401(5) . ?
C2 C3 1.376(6) . ?
C2 H2A 0.9400 . ?
C3 C4 1.398(5) . ?
C4 C5 1.396(5) . ?
C5 C6 1.382(6) . ?
C5 H5 0.9400 . ?
C7 C8 1.518(5) . ?
C8 C9 1.392(6) . ?
C8 C13 1.397(5) . ?
C9 C10 1.391(6) . ?
C9 H9 0.9400 . ?
C10 C11 1.401(6) . ?
C11 C12 1.348(6) . ?
C12 C13 1.390(6) . ?
C14 C15 1.513(5) . ?
C15 C20 1.382(6) . ?
C15 C16 1.385(6) . ?
C16 C17 1.383(6) . ?
C16 H16 0.9400 . ?
C17 C18 1.365(7) . ?
C18 C19 1.389(7) . ?
C19 C20 1.388(6) . ?
C21 C22 1.519(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C22 C23 1.511(7) . ?
C22 C24 1.518(7) . ?
C22 H22 0.9900 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 C26 1.521(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C26 C28 1.521(6) . ?
C26 C27 1.525(6) . ?
C26 H26 0.9900 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 H28C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N1 C1 127.8(3) . . ?
C7 N1 H1 122(5) . . ?
C1 N1 H1 110(5) . . ?
C14 N2 C3 126.2(4) . . ?
C14 N2 H2 115(4) . . ?
C3 N2 H2 119(4) . . ?
C4 O3 C21 119.4(3) . . ?
C6 O4 C25 118.2(3) . . ?
C2 C1 C6 119.7(3) . . ?
C2 C1 N1 124.3(3) . . ?
C6 C1 N1 116.0(3) . . ?
C3 C2 C1 120.0(3) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 N2 124.3(3) . . ?
C4 C3 N2 115.3(3) . . ?
O3 C4 C5 124.4(3) . . ?
O3 C4 C3 115.6(3) . . ?
C5 C4 C3 120.0(3) . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
O4 C6 C5 125.8(3) . . ?
O4 C6 C1 113.8(3) . . ?
C5 C6 C1 120.4(3) . . ?
O1 C7 N1 124.5(4) . . ?
O1 C7 C8 118.9(4) . . ?
N1 C7 C8 116.6(3) . . ?
C9 C8 C13 117.5(4) . . ?
C9 C8 C7 115.8(3) . . ?
C13 C8 C7 126.7(4) . . ?
C10 C9 C8 122.5(3) . . ?
C10 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
C9 C10 C11 117.6(4) . . ?
C9 C10 I1 121.9(3) . . ?
C11 C10 I1 120.5(3) . . ?
F1 C11 C12 118.4(4) . . ?
F1 C11 C10 120.3(4) . . ?
C12 C11 C10 121.2(4) . . ?
F2 C12 C11 120.6(4) . . ?
F2 C12 C13 118.7(4) . . ?
C11 C12 C13 120.7(4) . . ?
F3 C13 C12 117.2(3) . . ?
F3 C13 C8 122.2(4) . . ?
C12 C13 C8 120.5(4) . . ?
O2 C14 N2 124.4(4) . . ?
O2 C14 C15 118.8(4) . . ?
N2 C14 C15 116.9(4) . . ?
C20 C15 C16 116.9(4) . . ?
C20 C15 C14 127.3(4) . . ?
C16 C15 C14 115.8(4) . . ?
C17 C16 C15 122.5(4) . . ?
C17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C18 C17 C16 119.0(4) . . ?
C18 C17 I2 119.8(3) . . ?
C16 C17 I2 121.2(3) . . ?
F4 C18 C17 122.2(4) . . ?
F4 C18 C19 117.0(4) . . ?
C17 C18 C19 120.8(4) . . ?
F5 C19 C20 120.6(4) . . ?
F5 C19 C18 120.7(4) . . ?
C20 C19 C18 118.7(4) . . ?
F6 C20 C15 122.4(4) . . ?
F6 C20 C19 115.5(4) . . ?
C15 C20 C19 122.1(4) . . ?
O3 C21 C22 108.5(3) . . ?
O3 C21 H21A 110.0 . . ?
C22 C21 H21A 110.0 . . ?
O3 C21 H21B 110.0 . . ?
C22 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
C23 C22 C24 112.0(5) . . ?
C23 C22 C21 112.6(4) . . ?
C24 C22 C21 108.4(4) . . ?
C23 C22 H22 107.9 . . ?
C24 C22 H22 107.9 . . ?
C21 C22 H22 107.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O4 C25 C26 108.3(3) . . ?
O4 C25 H25A 110.0 . . ?
C26 C25 H25A 110.0 . . ?
O4 C25 H25B 110.0 . . ?
C26 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
C28 C26 C25 108.5(4) . . ?
C28 C26 C27 110.7(4) . . ?
C25 C26 C27 111.7(4) . . ?
C28 C26 H26 108.6 . . ?
C25 C26 H26 108.6 . . ?
C27 C26 H26 108.6 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 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
C7 N1 C1 C2 11.0(6) . . . . ?
C7 N1 C1 C6 -172.0(4) . . . . ?
C6 C1 C2 C3 0.1(6) . . . . ?
N1 C1 C2 C3 177.1(4) . . . . ?
C1 C2 C3 C4 2.0(6) . . . . ?
C1 C2 C3 N2 -176.6(4) . . . . ?
C14 N2 C3 C2 9.6(6) . . . . ?
C14 N2 C3 C4 -169.1(4) . . . . ?
C21 O3 C4 C5 -12.7(6) . . . . ?
C21 O3 C4 C3 165.6(3) . . . . ?
C2 C3 C4 O3 -179.7(3) . . . . ?
N2 C3 C4 O3 -1.0(5) . . . . ?
C2 C3 C4 C5 -1.3(6) . . . . ?
N2 C3 C4 C5 177.4(3) . . . . ?
O3 C4 C5 C6 176.6(4) . . . . ?
C3 C4 C5 C6 -1.6(6) . . . . ?
C25 O4 C6 C5 5.4(6) . . . . ?
C25 O4 C6 C1 -174.1(3) . . . . ?
C4 C5 C6 O4 -175.8(4) . . . . ?
C4 C5 C6 C1 3.8(6) . . . . ?
C2 C1 C6 O4 176.5(3) . . . . ?
N1 C1 C6 O4 -0.6(5) . . . . ?
C2 C1 C6 C5 -3.0(6) . . . . ?
N1 C1 C6 C5 179.8(3) . . . . ?
C1 N1 C7 O1 -1.4(7) . . . . ?
C1 N1 C7 C8 178.9(3) . . . . ?
O1 C7 C8 C9 -2.2(5) . . . . ?
N1 C7 C8 C9 177.5(3) . . . . ?
O1 C7 C8 C13 176.4(4) . . . . ?
N1 C7 C8 C13 -3.9(6) . . . . ?
C13 C8 C9 C10 -0.6(6) . . . . ?
C7 C8 C9 C10 178.2(3) . . . . ?
C8 C9 C10 C11 1.0(6) . . . . ?
C8 C9 C10 I1 -177.2(3) . . . . ?
C9 C10 C11 F1 178.7(3) . . . . ?
I1 C10 C11 F1 -3.0(5) . . . . ?
C9 C10 C11 C12 -0.9(6) . . . . ?
I1 C10 C11 C12 177.3(3) . . . . ?
F1 C11 C12 F2 1.0(6) . . . . ?
C10 C11 C12 F2 -179.4(3) . . . . ?
F1 C11 C12 C13 -179.3(4) . . . . ?
C10 C11 C12 C13 0.3(6) . . . . ?
F2 C12 C13 F3 0.6(6) . . . . ?
C11 C12 C13 F3 -179.1(4) . . . . ?
F2 C12 C13 C8 179.9(3) . . . . ?
C11 C12 C13 C8 0.2(6) . . . . ?
C9 C8 C13 F3 179.2(3) . . . . ?
C7 C8 C13 F3 0.6(6) . . . . ?
C9 C8 C13 C12 -0.1(6) . . . . ?
C7 C8 C13 C12 -178.6(4) . . . . ?
C3 N2 C14 O2 -5.6(7) . . . . ?
C3 N2 C14 C15 174.2(4) . . . . ?
O2 C14 C15 C20 176.8(4) . . . . ?
N2 C14 C15 C20 -3.0(6) . . . . ?
O2 C14 C15 C16 -1.1(6) . . . . ?
N2 C14 C15 C16 179.1(4) . . . . ?
C20 C15 C16 C17 -0.5(6) . . . . ?
C14 C15 C16 C17 177.6(4) . . . . ?
C15 C16 C17 C18 -0.1(7) . . . . ?
C15 C16 C17 I2 178.6(3) . . . . ?
C16 C17 C18 F4 -179.0(4) . . . . ?
I2 C17 C18 F4 2.3(7) . . . . ?
C16 C17 C18 C19 -0.4(7) . . . . ?
I2 C17 C18 C19 -179.1(4) . . . . ?
F4 C18 C19 F5 -0.6(7) . . . . ?
C17 C18 C19 F5 -179.3(5) . . . . ?
F4 C18 C19 C20 -179.9(4) . . . . ?
C17 C18 C19 C20 1.5(7) . . . . ?
C16 C15 C20 F6 -177.7(4) . . . . ?
C14 C15 C20 F6 4.5(7) . . . . ?
C16 C15 C20 C19 1.6(7) . . . . ?
C14 C15 C20 C19 -176.2(4) . . . . ?
F5 C19 C20 F6 -2.0(7) . . . . ?
C18 C19 C20 F6 177.2(4) . . . . ?
F5 C19 C20 C15 178.6(4) . . . . ?
C18 C19 C20 C15 -2.1(7) . . . . ?
C4 O3 C21 C22 -158.5(4) . . . . ?
O3 C21 C22 C23 -61.6(5) . . . . ?
O3 C21 C22 C24 173.8(4) . . . . ?
C6 O4 C25 C26 163.6(3) . . . . ?
O4 C25 C26 C28 -175.9(3) . . . . ?
O4 C25 C26 C27 61.8(4) . . . . ?

_refine_diff_density_max         1.268
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.178

####################################################################### 
# 
# 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_ga_80427a_a
_database_code_depnum_ccdc_archive 'CCDC 1887357'
loop_
_audit_author_name
_audit_author_address
'Zhanting Li'
;Fudan University
China
;
_audit_update_record             
;
2018-12-26 deposited with the CCDC.	2019-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H50 F8 I2 N4 O7'
_chemical_formula_weight         1092.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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'
F F 0.0583 0.0400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I 0.0030 5.4350 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6130(6)
_cell_length_b                   15.5774(10)
_cell_length_c                   16.8800(11)
_cell_angle_alpha                69.045(2)
_cell_angle_beta                 76.089(2)
_cell_angle_gamma                82.935(2)
_cell_volume                     2289.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9264
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      57.04

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    7.871
_shelx_estimated_absorpt_T_min   0.452
_shelx_estimated_absorpt_T_max   0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.34138
_diffrn_radiation_type           GaK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29970
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.495
_diffrn_reflns_theta_max         57.041
_diffrn_reflns_theta_full        53.594
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9294
_reflns_number_gt                7908
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0882P)²+3.9544P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9294
_refine_ls_number_parameters     637
_refine_ls_number_restraints     188
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0588
_refine_ls_wR_factor_ref         0.1694
_refine_ls_wR_factor_gt          0.1639
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.2722(5) 0.4033(3) 0.4971(3) 0.0493(10) Uani 1 1 d . . . . .
N2 N 0.3218(5) 0.5810(3) 0.5852(3) 0.0400(9) Uani 1 1 d . . . . .
H2 H 0.2898 0.6384 0.5765 0.048 Uiso 1 1 calc R U . . .
N3 N 0.6553(4) 0.5657(3) 0.9318(3) 0.0431(9) Uani 1 1 d . . . . .
H3 H 0.5917 0.6076 0.9435 0.052 Uiso 1 1 calc R U . . .
N4 N 0.8980(5) 0.3953(3) 1.0562(3) 0.0498(10) Uani 1 1 d . . . . .
O1 O 0.4627(4) 0.4682(2) 0.6582(2) 0.0481(8) Uani 1 1 d . . . . .
O2 O 0.7539(4) 0.5015(3) 0.8301(3) 0.0531(9) Uani 1 1 d . . . . .
O3 O 0.1705(4) 0.6757(2) 0.4658(3) 0.0507(9) Uani 1 1 d . . . . .
O4 O 0.2404(4) 0.7136(2) 0.6581(2) 0.0445(8) Uani 1 1 d . . . . .
O5 O 0.4961(4) 0.7193(3) 0.8688(3) 0.0597(11) Uani 1 1 d . . . . .
O6 O 0.6432(4) 0.6284(2) 1.0598(2) 0.0438(7) Uani 1 1 d . . . . .
C1 C 0.3155(6) 0.4445(3) 0.5451(3) 0.0454(11) Uani 1 1 d . . . . .
H1A H 0.3715 0.4093 0.5860 0.055 Uiso 1 1 calc R U . . .
C2 C 0.2812(5) 0.5355(3) 0.5366(3) 0.0366(9) Uani 1 1 d . . . . .
C3 C 0.2001(5) 0.5871(3) 0.4737(3) 0.0390(10) Uani 1 1 d . . . . .
C4 C 0.1599(6) 0.5439(4) 0.4244(3) 0.0443(11) Uani 1 1 d . . . . .
H4 H 0.1070 0.5768 0.3811 0.053 Uiso 1 1 calc R U . . .
C5 C 0.1979(6) 0.4521(4) 0.4393(3) 0.0467(11) Uani 1 1 d . . . . .
H5 H 0.1686 0.4227 0.4058 0.056 Uiso 1 1 calc R U . . .
C6 C 0.4057(5) 0.5451(3) 0.6445(3) 0.0370(9) Uani 1 1 d . . . . .
C7 C 0.4276(5) 0.6021(3) 0.6956(3) 0.0356(9) Uani 1 1 d . . . . .
C8 C 0.5308(5) 0.5678(3) 0.7446(3) 0.0347(9) Uani 1 1 d . . . . .
H8 H 0.5884 0.5158 0.7378 0.042 Uiso 1 1 calc R U . . .
C9 C 0.5557(5) 0.6051(3) 0.8033(3) 0.0377(9) Uani 1 1 d . . . . .
C10 C 0.4719(5) 0.6839(3) 0.8105(3) 0.0395(10) Uani 1 1 d . . . . .
C11 C 0.3707(5) 0.7222(3) 0.7598(3) 0.0402(10) Uani 1 1 d . . . . .
H11 H 0.3184 0.7772 0.7630 0.048 Uiso 1 1 calc R U . . .
C12 C 0.3453(5) 0.6809(3) 0.7047(3) 0.0375(9) Uani 1 1 d . . . . .
C13 C 0.6642(5) 0.5539(3) 0.8558(3) 0.0406(10) Uani 1 1 d . . . . .
C14 C 0.8195(6) 0.4380(4) 0.9964(3) 0.0471(11) Uani 1 1 d . . . . .
H14 H 0.8202 0.4124 0.9530 0.057 Uiso 1 1 calc R U . . .
C15 C 0.7372(5) 0.5181(3) 0.9952(3) 0.0400(10) Uani 1 1 d . . . . .
C16 C 0.7310(5) 0.5531(3) 1.0619(3) 0.0417(10) Uani 1 1 d . . . . .
C17 C 0.8148(6) 0.5090(4) 1.1229(3) 0.0464(11) Uani 1 1 d . . . . .
H17 H 0.8161 0.5318 1.1679 0.056 Uiso 1 1 calc R U . . .
C18 C 0.8959(6) 0.4313(4) 1.1166(3) 0.0508(12) Uani 1 1 d . . . . .
H18 H 0.9537 0.4019 1.1580 0.061 Uiso 1 1 calc R U . . .
C19 C 0.1131(7) 0.7327(4) 0.3899(4) 0.0591(15) Uani 1 1 d . . . . .
H19A H 0.0159 0.7131 0.3958 0.071 Uiso 1 1 calc R U . . .
H19B H 0.1750 0.7240 0.3371 0.071 Uiso 1 1 calc R U . . .
C20 C 0.1059(7) 0.8315(4) 0.3810(4) 0.0578(14) Uani 1 1 d . . . . .
H20 H 0.0334 0.8404 0.4311 0.069 Uiso 1 1 calc R U . . .
C21 C 0.2476(8) 0.8630(5) 0.3808(5) 0.0702(17) Uani 1 1 d . . . . .
H21A H 0.2815 0.8229 0.4327 0.105 Uiso 1 1 calc R U . . .
H21B H 0.2360 0.9264 0.3806 0.105 Uiso 1 1 calc R U . . .
H21C H 0.3177 0.8602 0.3288 0.105 Uiso 1 1 calc R U . . .
C22 C 0.0533(9) 0.8865(5) 0.2968(5) 0.077(2) Uani 1 1 d . . . . .
H22A H 0.0235 0.9491 0.2963 0.116 Uiso 1 1 calc R U . . .
H22B H -0.0282 0.8563 0.2941 0.116 Uiso 1 1 calc R U . . .
H22C H 0.1312 0.8889 0.2466 0.116 Uiso 1 1 calc R U . . .
C23 C 0.1454(6) 0.7877(3) 0.6722(3) 0.0436(11) Uani 1 1 d . . . . .
H23A H 0.1980 0.8452 0.6505 0.052 Uiso 1 1 calc R U . . .
H23B H 0.1042 0.7735 0.7349 0.052 Uiso 1 1 calc R U . . .
C24 C 0.0276(7) 0.7988(4) 0.6235(4) 0.0533(13) Uani 1 1 d . . . . .
H24 H 0.0731 0.7987 0.5636 0.064 Uiso 1 1 calc R U . . .
C25 C -0.0727(8) 0.7195(5) 0.6670(6) 0.074(2) Uani 1 1 d . . . . .
H25A H -0.0195 0.6620 0.6660 0.112 Uiso 1 1 calc R U . . .
H25B H -0.1506 0.7299 0.6359 0.112 Uiso 1 1 calc R U . . .
H25C H -0.1131 0.7155 0.7273 0.112 Uiso 1 1 calc R U . . .
C26 C -0.0505(8) 0.8915(4) 0.6158(5) 0.0681(17) Uani 1 1 d . . . . .
H26A H -0.0849 0.8962 0.6737 0.102 Uiso 1 1 calc R U . . .
H26B H -0.1323 0.8971 0.5887 0.102 Uiso 1 1 calc R U . . .
H26C H 0.0153 0.9408 0.5799 0.102 Uiso 1 1 calc R U . . .
C27 C 0.442(3) 0.816(2) 0.8611(17) 0.054(4) Uani 0.528(13) 1 d D U P A 1
H27A H 0.3511 0.8148 0.9041 0.064 Uiso 0.528(13) 1 calc R U P A 1
H27B H 0.4225 0.8488 0.8024 0.064 Uiso 0.528(13) 1 calc R U P A 1
C28 C 0.5513(12) 0.8662(7) 0.8766(7) 0.046(3) Uani 0.528(13) 1 d D U P A 1
H28 H 0.5844 0.8247 0.9299 0.055 Uiso 0.528(13) 1 calc R U P A 1
C29 C 0.681(2) 0.8858(19) 0.8024(12) 0.081(6) Uani 0.528(13) 1 d D U P A 1
H29A H 0.6518 0.9238 0.7484 0.121 Uiso 0.528(13) 1 calc R U P A 1
H29B H 0.7259 0.8276 0.7967 0.121 Uiso 0.528(13) 1 calc R U P A 1
H29C H 0.7505 0.9185 0.8142 0.121 Uiso 0.528(13) 1 calc R U P A 1
C30 C 0.4866(15) 0.9538(8) 0.8938(11) 0.073(4) Uani 0.528(13) 1 d D U P A 1
H30A H 0.5576 0.9810 0.9099 0.109 Uiso 0.528(13) 1 calc R U P A 1
H30B H 0.4019 0.9390 0.9414 0.109 Uiso 0.528(13) 1 calc R U P A 1
H30C H 0.4588 0.9978 0.8414 0.109 Uiso 0.528(13) 1 calc R U P A 1
C27' C 0.419(4) 0.797(2) 0.8856(17) 0.054(4) Uani 0.472(13) 1 d D . P A 2
H27C H 0.4171 0.7937 0.9454 0.064 Uiso 0.472(13) 1 calc R U P A 2
H27D H 0.3196 0.8001 0.8779 0.064 Uiso 0.472(13) 1 calc R U P A 2
C28' C 0.5015(14) 0.8781(8) 0.8194(8) 0.057(4) Uani 0.472(13) 1 d D U P A 2
H28' H 0.5101 0.8768 0.7596 0.068 Uiso 0.472(13) 1 calc R U P A 2
C29' C 0.651(2) 0.875(2) 0.8375(17) 0.097(8) Uani 0.472(13) 1 d D U P A 2
H29D H 0.6774 0.8112 0.8699 0.145 Uiso 0.472(13) 1 calc R U P A 2
H29E H 0.6502 0.9140 0.8718 0.145 Uiso 0.472(13) 1 calc R U P A 2
H29F H 0.7206 0.8967 0.7824 0.145 Uiso 0.472(13) 1 calc R U P A 2
C30' C 0.420(3) 0.9661(10) 0.8275(14) 0.112(9) Uani 0.472(13) 1 d D U P A 2
H30D H 0.3251 0.9691 0.8144 0.168 Uiso 0.472(13) 1 calc R U P A 2
H30E H 0.4735 1.0196 0.7864 0.168 Uiso 0.472(13) 1 calc R U P A 2
H30F H 0.4089 0.9659 0.8868 0.168 Uiso 0.472(13) 1 calc R U P A 2
C31 C 0.6320(6) 0.6645(4) 1.1289(3) 0.0494(12) Uani 1 1 d . . . . .
H31A H 0.7257 0.6875 1.1253 0.059 Uiso 1 1 calc R U . . .
H31B H 0.6058 0.6151 1.1857 0.059 Uiso 1 1 calc R U . . .
C32 C 0.5195(7) 0.7417(4) 1.1215(4) 0.0588(14) Uani 1 1 d . . . . .
H32 H 0.5482 0.7914 1.0642 0.071 Uiso 1 1 calc R U . . .
C33 C 0.3742(7) 0.7108(5) 1.1277(5) 0.0752(19) Uani 1 1 d . . . . .
H33A H 0.3807 0.6810 1.0847 0.113 Uiso 1 1 calc R U . . .
H33B H 0.3068 0.7642 1.1165 0.113 Uiso 1 1 calc R U . . .
H33C H 0.3402 0.6670 1.1860 0.113 Uiso 1 1 calc R U . . .
C34 C 0.5179(11) 0.7798(6) 1.1937(6) 0.094(3) Uani 1 1 d . . . . .
H34A H 0.4676 0.8403 1.1813 0.141 Uiso 1 1 calc R U . . .
H34B H 0.6167 0.7859 1.1966 0.141 Uiso 1 1 calc R U . . .
H34C H 0.4684 0.7377 1.2493 0.141 Uiso 1 1 calc R U . . .
C35 C 0.3732(7) 0.0779(4) 0.5619(5) 0.0600(15) Uani 1 1 d . . . . .
C36 C 0.4814(6) 0.0520(4) 0.4917(4) 0.0492(12) Uani 1 1 d . . . . .
F1 F 0.2495(4) 0.0386(3) 0.5743(4) 0.109(2) Uani 1 1 d . U . . .
F2 F 0.4152(7) 0.0417(3) 0.6375(3) 0.1077(19) Uani 1 1 d . U . . .
F3 F 0.6042(4) 0.0926(2) 0.4796(3) 0.0721(11) Uani 1 1 d . . . . .
F4 F 0.4342(5) 0.0879(3) 0.4176(3) 0.0818(12) Uani 1 1 d . . . . .
I1 I 0.33475(4) 0.22542(2) 0.52956(2) 0.05122(13) Uani 1 1 d . . . . .
C37 C 0.0870(16) 0.1065(11) 0.0022(11) 0.082(4) Uani 0.586(13) 1 d D U P B 1
C38 C -0.0241(16) 0.0404(13) 0.0132(10) 0.063(4) Uani 0.586(13) 1 d D U P B 1
F5 F 0.1787(18) 0.0566(11) 0.0559(16) 0.164(9) Uani 0.586(13) 1 d D U P B 1
F6 F 0.1498(19) 0.1348(10) -0.0836(11) 0.164(7) Uani 0.586(13) 1 d D U P B 1
F7 F -0.1191(13) 0.0898(8) -0.0318(8) 0.088(4) Uani 0.586(13) 1 d D U P B 1
F8 F -0.0859(14) 0.0155(5) 0.0991(6) 0.116(4) Uani 0.586(13) 1 d D U P B 1
C37' C 0.0748(19) 0.0948(15) 0.0409(10) 0.069(4) Uani 0.414(13) 1 d D U P B 2
C38' C -0.011(2) 0.055(2) -0.0004(13) 0.065(5) Uani 0.414(13) 1 d D U P B 2
F5' F 0.2092(13) 0.0934(11) -0.0117(14) 0.095(6) Uani 0.414(13) 1 d D U P B 2
F6' F 0.073(3) 0.0337(11) 0.1189(10) 0.162(10) Uani 0.414(13) 1 d D U P B 2
F7' F -0.1523(17) 0.0712(17) 0.0159(17) 0.130(10) Uani 0.414(13) 1 d D U P B 2
F8' F 0.036(2) 0.1049(12) -0.0851(9) 0.136(7) Uani 0.414(13) 1 d D U P B 2
I2 I 0.00590(4) 0.22668(3) 0.04185(3) 0.06271(15) Uani 1 1 d . . . . .
C39 C 0.0340(8) 0.3618(6) 0.7649(5) 0.075(2) Uani 1 1 d . . . . .
O7 O 0.0144(6) 0.4591(4) 0.7308(3) 0.0826(15) 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
N1 C5 1.307(7) . ?
N1 C1 1.356(6) . ?
N2 C6 1.356(6) . ?
N2 C2 1.402(6) . ?
N2 H2 0.8800 . ?
N3 C13 1.340(6) . ?
N3 C15 1.418(6) . ?
N3 H3 0.8800 . ?
N4 C18 1.322(8) . ?
N4 C14 1.339(7) . ?
O1 C6 1.221(6) . ?
O2 C13 1.223(6) . ?
O3 C3 1.340(6) . ?
O3 C19 1.463(6) . ?
O4 C12 1.365(6) . ?
O4 C23 1.433(6) . ?
O5 C10 1.362(6) . ?
O5 C27' 1.41(4) . ?
O5 C27 1.50(3) . ?
O6 C16 1.353(6) . ?
O6 C31 1.443(6) . ?
C1 C2 1.379(7) . ?
C1 H1A 0.9500 . ?
C2 C3 1.420(7) . ?
C3 C4 1.383(7) . ?
C4 C5 1.378(8) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.502(6) . ?
C7 C8 1.379(7) . ?
C7 C12 1.412(6) . ?
C8 C9 1.392(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.409(7) . ?
C9 C13 1.498(7) . ?
C10 C11 1.388(7) . ?
C11 C12 1.384(6) . ?
C11 H11 0.9500 . ?
C14 C15 1.389(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.403(7) . ?
C16 C17 1.392(7) . ?
C17 C18 1.380(8) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.486(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.502(9) . ?
C20 C22 1.541(9) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.512(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.515(10) . ?
C24 C26 1.521(8) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.505(18) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.513(15) . ?
C28 C30 1.524(12) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C27' C28' 1.515(17) . ?
C27' H27C 0.9900 . ?
C27' H27D 0.9900 . ?
C28' C30' 1.526(15) . ?
C28' C29' 1.529(18) . ?
C28' H28' 1.0000 . ?
C29' H29D 0.9800 . ?
C29' H29E 0.9800 . ?
C29' H29F 0.9800 . ?
C30' H30D 0.9800 . ?
C30' H30E 0.9800 . ?
C30' H30F 0.9800 . ?
C31 C32 1.506(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.502(10) . ?
C32 C34 1.530(9) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 F2 1.338(9) . ?
C35 F1 1.342(7) . ?
C35 C36 1.515(9) . ?
C35 I1 2.170(6) . ?
C36 F4 1.338(7) . ?
C36 F3 1.346(6) . ?
C36 C36 1.552(10) 2_656 ?
C37 F6 1.358(15) . ?
C37 F5 1.383(15) . ?
C37 C38 1.508(15) . ?
C37 I2 2.201(16) . ?
C38 F7 1.321(14) . ?
C38 F8 1.358(15) . ?
C38 C38 1.47(4) 2 ?
C37' F6' 1.316(16) . ?
C37' F5' 1.384(16) . ?
C37' C38' 1.508(18) . ?
C37' I2 2.08(2) . ?
C38' F7' 1.332(18) . ?
C38' F8' 1.354(18) . ?
C38' C38' 1.68(6) 2 ?
C39 O7 1.422(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
C5 N1 C1 118.9(4) . . ?
C6 N2 C2 126.3(4) . . ?
C6 N2 H2 116.9 . . ?
C2 N2 H2 116.9 . . ?
C13 N3 C15 127.1(4) . . ?
C13 N3 H3 116.5 . . ?
C15 N3 H3 116.5 . . ?
C18 N4 C14 118.1(5) . . ?
C3 O3 C19 115.9(4) . . ?
C12 O4 C23 119.3(4) . . ?
C10 O5 C27' 123.9(12) . . ?
C10 O5 C27 118.1(10) . . ?
C16 O6 C31 116.8(4) . . ?
N1 C1 C2 122.4(5) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C1 C2 N2 124.7(4) . . ?
C1 C2 C3 117.7(4) . . ?
N2 C2 C3 117.6(4) . . ?
O3 C3 C4 124.9(4) . . ?
O3 C3 C2 116.4(4) . . ?
C4 C3 C2 118.6(4) . . ?
C5 C4 C3 118.8(5) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 123.5(4) . . ?
N1 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
O1 C6 N2 122.5(4) . . ?
O1 C6 C7 119.0(4) . . ?
N2 C6 C7 118.5(4) . . ?
C8 C7 C12 117.4(4) . . ?
C8 C7 C6 115.4(4) . . ?
C12 C7 C6 126.9(4) . . ?
C7 C8 C9 123.8(4) . . ?
C7 C8 H8 118.1 . . ?
C9 C8 H8 118.1 . . ?
C8 C9 C10 117.1(4) . . ?
C8 C9 C13 116.1(4) . . ?
C10 C9 C13 126.7(4) . . ?
O5 C10 C11 122.8(4) . . ?
O5 C10 C9 116.7(4) . . ?
C11 C10 C9 120.5(4) . . ?
C12 C11 C10 120.5(4) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
O4 C12 C11 121.8(4) . . ?
O4 C12 C7 117.7(4) . . ?
C11 C12 C7 120.5(4) . . ?
O2 C13 N3 122.5(5) . . ?
O2 C13 C9 120.0(4) . . ?
N3 C13 C9 117.5(4) . . ?
N4 C14 C15 122.8(5) . . ?
N4 C14 H14 118.6 . . ?
C15 C14 H14 118.6 . . ?
C14 C15 C16 118.4(4) . . ?
C14 C15 N3 124.0(4) . . ?
C16 C15 N3 117.6(4) . . ?
O6 C16 C17 126.2(5) . . ?
O6 C16 C15 115.7(4) . . ?
C17 C16 C15 118.2(5) . . ?
C18 C17 C16 118.5(5) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
N4 C18 C17 123.9(5) . . ?
N4 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
O3 C19 C20 110.9(4) . . ?
O3 C19 H19A 109.5 . . ?
C20 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C19 C20 C21 112.1(5) . . ?
C19 C20 C22 107.3(5) . . ?
C21 C20 C22 112.0(6) . . ?
C19 C20 H20 108.5 . . ?
C21 C20 H20 108.5 . . ?
C22 C20 H20 108.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O4 C23 C24 107.4(4) . . ?
O4 C23 H23A 110.2 . . ?
C24 C23 H23A 110.2 . . ?
O4 C23 H23B 110.2 . . ?
C24 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
C23 C24 C25 111.1(5) . . ?
C23 C24 C26 108.8(5) . . ?
C25 C24 C26 112.3(6) . . ?
C23 C24 H24 108.2 . . ?
C25 C24 H24 108.2 . . ?
C26 C24 H24 108.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O5 C27 C28 110(2) . . ?
O5 C27 H27A 109.6 . . ?
C28 C27 H27A 109.6 . . ?
O5 C27 H27B 109.6 . . ?
C28 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
C27 C28 C29 111.3(18) . . ?
C27 C28 C30 111.7(16) . . ?
C29 C28 C30 111.5(14) . . ?
C27 C28 H28 107.4 . . ?
C29 C28 H28 107.4 . . ?
C30 C28 H28 107.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O5 C27' C28' 104(2) . . ?
O5 C27' H27C 110.9 . . ?
C28' C27' H27C 110.9 . . ?
O5 C27' H27D 110.9 . . ?
C28' C27' H27D 110.9 . . ?
H27C C27' H27D 108.9 . . ?
C27' C28' C30' 108.4(19) . . ?
C27' C28' C29' 109.6(19) . . ?
C30' C28' C29' 109.4(18) . . ?
C27' C28' H28' 109.8 . . ?
C30' C28' H28' 109.8 . . ?
C29' C28' H28' 109.8 . . ?
C28' C29' H29D 109.5 . . ?
C28' C29' H29E 109.5 . . ?
H29D C29' H29E 109.5 . . ?
C28' C29' H29F 109.5 . . ?
H29D C29' H29F 109.5 . . ?
H29E C29' H29F 109.5 . . ?
C28' C30' H30D 109.5 . . ?
C28' C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C28' C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
O6 C31 C32 109.7(4) . . ?
O6 C31 H31A 109.7 . . ?
C32 C31 H31A 109.7 . . ?
O6 C31 H31B 109.7 . . ?
C32 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C33 C32 C31 112.3(5) . . ?
C33 C32 C34 111.3(7) . . ?
C31 C32 C34 107.2(6) . . ?
C33 C32 H32 108.7 . . ?
C31 C32 H32 108.7 . . ?
C34 C32 H32 108.7 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
F2 C35 F1 105.6(6) . . ?
F2 C35 C36 110.2(5) . . ?
F1 C35 C36 108.3(5) . . ?
F2 C35 I1 110.3(4) . . ?
F1 C35 I1 109.3(4) . . ?
C36 C35 I1 112.9(4) . . ?
F4 C36 F3 107.3(5) . . ?
F4 C36 C35 108.3(5) . . ?
F3 C36 C35 107.4(5) . . ?
F4 C36 C36 108.6(6) . 2_656 ?
F3 C36 C36 107.3(5) . 2_656 ?
C35 C36 C36 117.4(6) . 2_656 ?
F6 C37 F5 113.9(16) . . ?
F6 C37 C38 105.3(13) . . ?
F5 C37 C38 105.6(13) . . ?
F6 C37 I2 109.8(10) . . ?
F5 C37 I2 106.6(10) . . ?
C38 C37 I2 115.8(12) . . ?
F7 C38 F8 108.7(14) . . ?
F7 C38 C38 109.1(17) . 2 ?
F8 C38 C38 111.5(16) . 2 ?
F7 C38 C37 105.8(15) . . ?
F8 C38 C37 103.3(14) . . ?
C38 C38 C37 118.1(17) 2 . ?
F6' C37' F5' 109.9(18) . . ?
F6' C37' C38' 105.3(18) . . ?
F5' C37' C38' 100.1(16) . . ?
F6' C37' I2 113.5(14) . . ?
F5' C37' I2 112.2(14) . . ?
C38' C37' I2 114.8(15) . . ?
F7' C38' F8' 105.2(18) . . ?
F7' C38' C37' 116(2) . . ?
F8' C38' C37' 100.0(17) . . ?
F7' C38' C38' 105(2) . 2 ?
F8' C38' C38' 104(2) . 2 ?
C37' C38' C38' 124(2) . 2 ?

_refine_diff_density_max         2.071
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.117

####################################################################### 
# 
# 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_z
_database_code_depnum_ccdc_archive 'CCDC 1887343'
loop_
_audit_author_name
_audit_author_address
'Zhan-Ting Li'
;Fudan University
China
;
_audit_update_record             
;
2018-12-26 deposited with the CCDC.	2019-03-06 downloaded from the CCDC.
;
_audit_creation_date             2018-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '1.5(C6 F4 I2), C34 H46 N4 O6'
_chemical_formula_sum            'C43 H46 F6 I3 N4 O6'
_chemical_formula_weight         1209.54
_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 0.0033 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   9.3189(3)
_cell_length_b                   16.8147(5)
_cell_length_c                   18.3190(6)
_cell_angle_alpha                116.2490(10)
_cell_angle_beta                 96.2380(10)
_cell_angle_gamma                100.8410(10)
_cell_volume                     2467.84(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9078
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   0.770
_shelx_estimated_absorpt_T_min   0.546
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0602 before and 0.0425 after correction. The Ratio of minimum to maximum transmission is 0.9221. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1186
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28784
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.374
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6635
_reflns_number_total             8618
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         8618
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.033
_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)+(0.0412P)²+2.2823P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0919
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C26 \\sim C27: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
3.a Ternary CH refined with riding coordinates:
 C18(H18), C22(H22), C26(H26), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C21(H21A,H21B), C25(H25A,H25B), C29(H29A,H29B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12),
 C15(H15)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 -0.00462(3) 0.83985(2) 0.04699(2) 0.05638(10) Uani 1 1 d . . . . .
I2 I -0.15178(4) 0.63079(2) 0.29898(2) 0.06096(11) Uani 1 1 d . . . . .
F1 F -0.0554(4) 0.62876(18) 0.01357(17) 0.0760(8) Uani 1 1 d . . . . .
F2 F -0.0988(4) 0.55310(18) 0.11149(19) 0.0849(9) Uani 1 1 d . . . . .
F3 F -0.1365(5) 0.8328(2) 0.32283(19) 0.1030(12) Uani 1 1 d . . . . .
F4 F -0.0734(5) 0.9127(2) 0.2292(2) 0.1011(11) Uani 1 1 d . . . . .
C35 C -0.0611(5) 0.7743(3) 0.1188(3) 0.0513(11) Uani 1 1 d . . . . .
C36 C -0.0822(6) 0.8226(3) 0.1981(3) 0.0637(13) Uani 1 1 d . . . . .
C37 C -0.1111(6) 0.7816(3) 0.2470(3) 0.0641(13) Uani 1 1 d . . . . .
C38 C -0.1165(5) 0.6902(3) 0.2207(3) 0.0530(11) Uani 1 1 d . . . . .
C39 C -0.0943(5) 0.6424(3) 0.1418(3) 0.0530(11) Uani 1 1 d . . . . .
C40 C -0.0704(5) 0.6823(3) 0.0917(3) 0.0527(11) Uani 1 1 d . . . . .
I3 I 0.05017(4) 0.84361(2) 0.57005(2) 0.06782(12) Uani 1 1 d . . . . .
F5 F 0.2156(4) 0.9124(3) 0.4566(2) 0.1048(12) Uani 1 1 d . . . . .
F6 F -0.1771(4) 0.9684(2) 0.5963(2) 0.0960(10) Uani 1 1 d . . . . .
C41 C 0.1094(6) 0.9557(3) 0.4792(3) 0.0657(13) Uani 1 1 d . . . . .
C42 C 0.0203(6) 0.9368(3) 0.5279(3) 0.0567(12) Uani 1 1 d . . . . .
C43 C -0.0888(6) 0.9820(4) 0.5480(3) 0.0674(14) Uani 1 1 d . . . . .
O1 O -0.3013(4) 0.4390(2) 0.55459(18) 0.0608(8) Uani 1 1 d . . . . .
O2 O 0.1004(4) 0.7098(2) 0.63227(19) 0.0644(9) Uani 1 1 d . . . . .
O3 O -0.0687(3) 0.5637(2) 0.74962(19) 0.0624(9) Uani 1 1 d . . . . .
O4 O 0.3662(3) 0.7291(2) 0.97271(18) 0.0579(8) Uani 1 1 d . . . . .
O5 O 0.5402(4) 0.8618(2) 0.84583(18) 0.0655(9) Uani 1 1 d . . . . .
O6 O 0.6031(3) 0.9479(2) 1.13877(17) 0.0581(8) Uani 1 1 d . . . . .
N1 N -0.1985(5) 0.5539(3) 0.4034(2) 0.0623(10) Uani 1 1 d . . . . .
N2 N -0.0648(4) 0.5810(2) 0.6123(2) 0.0509(9) Uani 1 1 d . . . . .
H2 H -0.091106 0.548115 0.636026 0.061 Uiso 1 1 calc R . . . .
N3 N 0.5427(4) 0.8778(2) 0.97489(19) 0.0474(8) Uani 1 1 d . . . . .
H3 H 0.497638 0.855037 1.002663 0.057 Uiso 1 1 calc R . . . .
N4 N 0.8804(4) 1.0671(3) 1.0338(2) 0.0574(10) Uani 1 1 d . . . . .
C1 C -0.1161(5) 0.5857(3) 0.4794(3) 0.0555(11) Uani 1 1 d . . . . .
H1 H -0.031703 0.634773 0.497936 0.067 Uiso 1 1 calc R . . . .
C2 C -0.1489(5) 0.5498(3) 0.5322(2) 0.0450(10) Uani 1 1 d . . . . .
C3 C -0.2736(5) 0.4742(3) 0.5025(3) 0.0510(11) Uani 1 1 d . . . . .
C4 C -0.3571(6) 0.4401(3) 0.4227(3) 0.0621(12) Uani 1 1 d . . . . .
H4 H -0.439731 0.389367 0.400703 0.075 Uiso 1 1 calc R . . . .
C5 C -0.3149(6) 0.4830(4) 0.3769(3) 0.0648(13) Uani 1 1 d . . . . .
H5 H -0.372468 0.460409 0.323653 0.078 Uiso 1 1 calc R . . . .
C6 C 0.9092(5) 1.0978(3) 1.1153(3) 0.0582(12) Uani 1 1 d . . . . .
H6 H 0.993333 1.146538 1.147618 0.070 Uiso 1 1 calc R . . . .
C7 C 0.8226(5) 1.0622(3) 1.1547(3) 0.0536(11) Uani 1 1 d . . . . .
H7 H 0.847169 1.086845 1.212399 0.064 Uiso 1 1 calc R . . . .
C8 C 0.6988(5) 0.9895(3) 1.1083(3) 0.0468(10) Uani 1 1 d . . . . .
C9 C 0.6674(4) 0.9531(3) 1.0211(2) 0.0422(9) Uani 1 1 d . . . . .
C10 C 0.7624(5) 0.9961(3) 0.9881(3) 0.0520(11) Uani 1 1 d . . . . .
H10 H 0.742120 0.973652 0.930672 0.062 Uiso 1 1 calc R . . . .
C11 C 0.1265(4) 0.6700(3) 0.7406(2) 0.0399(9) Uani 1 1 d . . . . .
C12 C 0.2629(4) 0.7353(3) 0.7796(2) 0.0427(9) Uani 1 1 d . . . . .
H12 H 0.303046 0.765415 0.751381 0.051 Uiso 1 1 calc R . . . .
C13 C 0.3441(4) 0.7590(3) 0.8578(2) 0.0404(9) Uani 1 1 d . . . . .
C14 C 0.2835(4) 0.7104(3) 0.8980(2) 0.0422(9) Uani 1 1 d . . . . .
C15 C 0.1485(5) 0.6455(3) 0.8615(3) 0.0469(10) Uani 1 1 d . . . . .
H15 H 0.110038 0.613510 0.888606 0.056 Uiso 1 1 calc R . . . .
C16 C 0.0683(4) 0.6267(3) 0.7849(3) 0.0442(9) Uani 1 1 d . . . . .
C17 C -0.4231(6) 0.3554(3) 0.5224(3) 0.0665(13) Uani 1 1 d . . . . .
H17A H -0.405584 0.307441 0.472571 0.080 Uiso 1 1 calc R . . . .
H17B H -0.517035 0.367268 0.507658 0.080 Uiso 1 1 calc R . . . .
C18 C -0.4319(6) 0.3248(3) 0.5867(3) 0.0686(14) Uani 1 1 d . . . . .
H18 H -0.452152 0.373877 0.635592 0.082 Uiso 1 1 calc R . . . .
C19 C -0.2875(8) 0.3077(5) 0.6140(5) 0.113(2) Uani 1 1 d . . . . .
H19A H -0.270978 0.255105 0.568834 0.169 Uiso 1 1 calc GR . . . .
H19B H -0.293394 0.296400 0.660747 0.169 Uiso 1 1 calc GR . . . .
H19C H -0.206052 0.360599 0.629864 0.169 Uiso 1 1 calc GR . . . .
C20 C -0.5638(8) 0.2402(4) 0.5531(4) 0.107(2) Uani 1 1 d . . . . .
H20A H -0.652667 0.253378 0.534925 0.160 Uiso 1 1 calc GR . . . .
H20B H -0.577767 0.223760 0.596360 0.160 Uiso 1 1 calc GR . . . .
H20C H -0.544131 0.189959 0.506980 0.160 Uiso 1 1 calc GR . . . .
C21 C -0.1678(5) 0.5522(4) 0.8021(3) 0.0726(15) Uani 1 1 d . . . . .
H21A H -0.118555 0.592396 0.860220 0.087 Uiso 1 1 calc R . . . .
H21B H -0.188852 0.489327 0.792712 0.087 Uiso 1 1 calc R . . . .
C22 C -0.3107(7) 0.5741(4) 0.7843(4) 0.0810(16) Uani 1 1 d . . . . .
H22 H -0.356203 0.531156 0.725417 0.097 Uiso 1 1 calc R . . . .
C23 C -0.2940(9) 0.6667(5) 0.7929(6) 0.131(3) Uani 1 1 d . . . . .
H23A H -0.236397 0.711606 0.847476 0.196 Uiso 1 1 calc GR . . . .
H23B H -0.391041 0.677047 0.785187 0.196 Uiso 1 1 calc GR . . . .
H23C H -0.243552 0.671894 0.751561 0.196 Uiso 1 1 calc GR . . . .
C24 C -0.4164(8) 0.5516(7) 0.8328(5) 0.134(3) Uani 1 1 d . . . . .
H24A H -0.438093 0.487045 0.815920 0.202 Uiso 1 1 calc GR . . . .
H24B H -0.507566 0.567260 0.822296 0.202 Uiso 1 1 calc GR . . . .
H24C H -0.371184 0.586116 0.891276 0.202 Uiso 1 1 calc GR . . . .
C25 C 0.3053(6) 0.6851(4) 1.0183(3) 0.0795(17) Uani 1 1 d . . . . .
H25A H 0.260758 0.620282 0.980264 0.095 Uiso 1 1 calc R . . . .
H25B H 0.226726 0.711659 1.041663 0.095 Uiso 1 1 calc R . . . .
C26 C 0.4161(8) 0.6945(6) 1.0842(5) 0.123(2) Uani 1 1 d . U . . .
H26 H 0.462620 0.760572 1.118695 0.148 Uiso 1 1 calc R . . . .
C27 C 0.3420(8) 0.6625(6) 1.1397(5) 0.131(2) Uani 1 1 d . U . . .
H27A H 0.274995 0.698977 1.163351 0.197 Uiso 1 1 calc GR . . . .
H27B H 0.417244 0.669107 1.183729 0.197 Uiso 1 1 calc GR . . . .
H27C H 0.286785 0.599038 1.107336 0.197 Uiso 1 1 calc GR . . . .
C28 C 0.5369(9) 0.6524(7) 1.0598(5) 0.152(4) Uani 1 1 d . . . . .
H28A H 0.497485 0.586937 1.027924 0.229 Uiso 1 1 calc GR . . . .
H28B H 0.608481 0.667172 1.108748 0.229 Uiso 1 1 calc GR . . . .
H28C H 0.584951 0.675367 1.026550 0.229 Uiso 1 1 calc GR . . . .
C29 C 0.6204(6) 0.9939(4) 1.2292(3) 0.0689(14) Uani 1 1 d . . . . .
H29A H 0.612579 1.056373 1.248376 0.083 Uiso 1 1 calc R . . . .
H29B H 0.718249 0.996332 1.255669 0.083 Uiso 1 1 calc R . . . .
C30 C 0.5013(6) 0.9422(4) 1.2521(3) 0.0789(16) Uani 1 1 d . . . . .
H30 H 0.507988 0.878569 1.229599 0.095 Uiso 1 1 calc R . . . .
C31 C 0.5296(10) 0.9854(7) 1.3477(4) 0.158(4) Uani 1 1 d . . . . .
H31A H 0.623743 0.979510 1.368669 0.238 Uiso 1 1 calc GR . . . .
H31B H 0.450736 0.954404 1.363051 0.238 Uiso 1 1 calc GR . . . .
H31C H 0.531790 1.049359 1.371007 0.238 Uiso 1 1 calc GR . . . .
C32 C 0.3508(8) 0.9415(7) 1.2172(5) 0.132(3) Uani 1 1 d . . . . .
H32A H 0.342146 1.003501 1.239007 0.197 Uiso 1 1 calc GR . . . .
H32B H 0.276912 0.906858 1.232162 0.197 Uiso 1 1 calc GR . . . .
H32C H 0.335158 0.913821 1.157510 0.197 Uiso 1 1 calc GR . . . .
C33 C 0.0530(5) 0.6562(3) 0.6574(2) 0.0437(9) Uani 1 1 d . . . . .
C34 C 0.4841(5) 0.8363(3) 0.8921(2) 0.0436(9) 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
I1 C35 2.106(4) . ?
I2 C38 2.100(4) . ?
F1 C40 1.353(5) . ?
F2 C39 1.341(5) . ?
F3 C37 1.348(5) . ?
F4 C36 1.344(5) . ?
C35 C36 1.374(6) . ?
C35 C40 1.381(6) . ?
C36 C37 1.371(7) . ?
C37 C38 1.381(6) . ?
C38 C39 1.371(6) . ?
C39 C40 1.369(6) . ?
I3 C42 2.078(4) . ?
F5 C41 1.332(6) . ?
F6 C43 1.335(5) . ?
C41 C42 1.377(7) . ?
C41 C43 1.378(7) 2_576 ?
C42 C43 1.369(7) . ?
O1 C3 1.350(5) . ?
O1 C17 1.460(5) . ?
O2 C33 1.218(5) . ?
O3 C16 1.370(5) . ?
O3 C21 1.451(5) . ?
O4 C14 1.365(5) . ?
O4 C25 1.435(5) . ?
O5 C34 1.230(5) . ?
O6 C8 1.347(5) . ?
O6 C29 1.459(5) . ?
N1 C1 1.330(5) . ?
N1 C5 1.312(6) . ?
N2 H2 0.8600 . ?
N2 C2 1.398(5) . ?
N2 C33 1.358(5) . ?
N3 H3 0.8600 . ?
N3 C9 1.398(5) . ?
N3 C34 1.350(5) . ?
N4 C6 1.322(6) . ?
N4 C10 1.326(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.381(6) . ?
C2 C3 1.399(6) . ?
C3 C4 1.383(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.371(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.363(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.373(6) . ?
C8 C9 1.407(5) . ?
C9 C10 1.390(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.383(5) . ?
C11 C16 1.397(5) . ?
C11 C33 1.498(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.390(5) . ?
C13 C14 1.407(5) . ?
C13 C34 1.499(5) . ?
C14 C15 1.370(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.386(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.484(7) . ?
C18 H18 0.9800 . ?
C18 C19 1.507(8) . ?
C18 C20 1.523(7) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.487(7) . ?
C22 H22 0.9800 . ?
C22 C23 1.470(8) . ?
C22 C24 1.500(8) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.431(8) . ?
C26 H26 0.9800 . ?
C26 C27 1.517(8) . ?
C26 C28 1.448(10) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.491(7) . ?
C30 H30 0.9800 . ?
C30 C31 1.538(8) . ?
C30 C32 1.473(9) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 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
C36 C35 I1 121.3(3) . . ?
C36 C35 C40 115.9(4) . . ?
C40 C35 I1 122.6(3) . . ?
F4 C36 C35 119.5(4) . . ?
F4 C36 C37 118.8(4) . . ?
C37 C36 C35 121.8(4) . . ?
F3 C37 C36 118.2(4) . . ?
F3 C37 C38 119.5(4) . . ?
C36 C37 C38 122.2(4) . . ?
C37 C38 I2 121.4(3) . . ?
C39 C38 I2 122.9(3) . . ?
C39 C38 C37 115.7(4) . . ?
F2 C39 C38 119.3(4) . . ?
F2 C39 C40 118.5(4) . . ?
C38 C39 C40 122.2(4) . . ?
F1 C40 C35 120.0(4) . . ?
F1 C40 C39 117.9(4) . . ?
C39 C40 C35 122.0(4) . . ?
F5 C41 C42 120.1(4) . . ?
F5 C41 C43 119.0(5) . 2_576 ?
C43 C41 C42 120.9(5) 2_576 . ?
C41 C42 I3 121.5(4) . . ?
C43 C42 I3 120.9(3) . . ?
C43 C42 C41 117.6(4) . . ?
F6 C43 C41 117.7(5) . 2_576 ?
F6 C43 C42 120.8(4) . . ?
C42 C43 C41 121.5(5) . 2_576 ?
C3 O1 C17 117.4(3) . . ?
C16 O3 C21 120.0(3) . . ?
C14 O4 C25 119.3(3) . . ?
C8 O6 C29 116.0(3) . . ?
C5 N1 C1 117.7(4) . . ?
C2 N2 H2 115.7 . . ?
C33 N2 H2 115.7 . . ?
C33 N2 C2 128.6(3) . . ?
C9 N3 H3 115.9 . . ?
C34 N3 H3 115.9 . . ?
C34 N3 C9 128.2(3) . . ?
C6 N4 C10 117.6(4) . . ?
N1 C1 H1 118.2 . . ?
N1 C1 C2 123.6(4) . . ?
C2 C1 H1 118.2 . . ?
N2 C2 C3 117.1(3) . . ?
C1 C2 N2 125.3(4) . . ?
C1 C2 C3 117.5(4) . . ?
O1 C3 C2 116.4(4) . . ?
O1 C3 C4 125.0(4) . . ?
C4 C3 C2 118.6(4) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 C3 118.3(4) . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 124.1(4) . . ?
N1 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
N4 C6 H6 118.1 . . ?
N4 C6 C7 123.8(4) . . ?
C7 C6 H6 118.1 . . ?
C6 C7 H7 120.4 . . ?
C6 C7 C8 119.3(4) . . ?
C8 C7 H7 120.4 . . ?
O6 C8 C7 125.7(4) . . ?
O6 C8 C9 115.8(4) . . ?
C7 C8 C9 118.5(4) . . ?
N3 C9 C8 117.6(3) . . ?
C10 C9 N3 125.4(4) . . ?
C10 C9 C8 116.9(4) . . ?
N4 C10 C9 123.9(4) . . ?
N4 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
C12 C11 C16 116.4(3) . . ?
C12 C11 C33 117.0(3) . . ?
C16 C11 C33 126.6(4) . . ?
C11 C12 H12 117.7 . . ?
C11 C12 C13 124.6(3) . . ?
C13 C12 H12 117.7 . . ?
C12 C13 C14 116.6(4) . . ?
C12 C13 C34 116.7(3) . . ?
C14 C13 C34 126.6(3) . . ?
O4 C14 C13 117.3(3) . . ?
O4 C14 C15 122.3(3) . . ?
C15 C14 C13 120.4(4) . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 121.0(4) . . ?
C16 C15 H15 119.5 . . ?
O3 C16 C11 118.2(3) . . ?
O3 C16 C15 120.9(3) . . ?
C15 C16 C11 120.9(4) . . ?
O1 C17 H17A 109.7 . . ?
O1 C17 H17B 109.7 . . ?
O1 C17 C18 109.6(4) . . ?
H17A C17 H17B 108.2 . . ?
C18 C17 H17A 109.7 . . ?
C18 C17 H17B 109.7 . . ?
C17 C18 H18 107.9 . . ?
C17 C18 C19 112.3(5) . . ?
C17 C18 C20 108.6(5) . . ?
C19 C18 H18 107.9 . . ?
C19 C18 C20 112.2(5) . . ?
C20 C18 H18 107.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 H21A 109.4 . . ?
O3 C21 H21B 109.4 . . ?
O3 C21 C22 111.3(4) . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
C21 C22 H22 105.9 . . ?
C21 C22 C24 109.7(5) . . ?
C23 C22 C21 114.9(6) . . ?
C23 C22 H22 105.9 . . ?
C23 C22 C24 113.7(7) . . ?
C24 C22 H22 105.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O4 C25 H25A 109.1 . . ?
O4 C25 H25B 109.1 . . ?
O4 C25 C26 112.4(4) . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
C25 C26 H26 106.2 . . ?
C25 C26 C27 110.2(6) . . ?
C25 C26 C28 116.6(7) . . ?
C27 C26 H26 106.2 . . ?
C28 C26 H26 106.2 . . ?
C28 C26 C27 110.7(7) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O6 C29 H29A 109.8 . . ?
O6 C29 H29B 109.8 . . ?
O6 C29 C30 109.3(4) . . ?
H29A C29 H29B 108.3 . . ?
C30 C29 H29A 109.8 . . ?
C30 C29 H29B 109.8 . . ?
C29 C30 H30 108.4 . . ?
C29 C30 C31 108.9(5) . . ?
C31 C30 H30 108.4 . . ?
C32 C30 C29 111.6(5) . . ?
C32 C30 H30 108.4 . . ?
C32 C30 C31 110.8(6) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O2 C33 N2 122.8(4) . . ?
O2 C33 C11 120.4(4) . . ?
N2 C33 C11 116.7(3) . . ?
O5 C34 N3 121.8(4) . . ?
O5 C34 C13 120.1(4) . . ?
N3 C34 C13 118.0(3) . . ?

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
I1 C35 C36 F4 3.1(7) . . . . ?
I1 C35 C36 C37 -176.5(4) . . . . ?
I1 C35 C40 F1 -5.7(6) . . . . ?
I1 C35 C40 C39 174.2(3) . . . . ?
I2 C38 C39 F2 1.8(6) . . . . ?
I2 C38 C39 C40 -179.5(4) . . . . ?
F2 C39 C40 F1 1.2(6) . . . . ?
F2 C39 C40 C35 -178.7(4) . . . . ?
F3 C37 C38 I2 -3.4(7) . . . . ?
F3 C37 C38 C39 177.9(4) . . . . ?
F4 C36 C37 F3 3.1(8) . . . . ?
F4 C36 C37 C38 -177.6(5) . . . . ?
C35 C36 C37 F3 -177.3(5) . . . . ?
C35 C36 C37 C38 2.0(8) . . . . ?
C36 C35 C40 F1 178.1(4) . . . . ?
C36 C35 C40 C39 -2.0(7) . . . . ?
C36 C37 C38 I2 177.3(4) . . . . ?
C36 C37 C38 C39 -1.4(8) . . . . ?
C37 C38 C39 F2 -179.6(4) . . . . ?
C37 C38 C39 C40 -0.9(7) . . . . ?
C38 C39 C40 F1 -177.5(4) . . . . ?
C38 C39 C40 C35 2.6(7) . . . . ?
C40 C35 C36 F4 179.3(5) . . . . ?
C40 C35 C36 C37 -0.2(8) . . . . ?
I3 C42 C43 F6 1.0(7) . . . . ?
I3 C42 C43 C41 179.7(4) . . . 2_576 ?
F5 C41 C42 I3 1.5(7) . . . . ?
F5 C41 C42 C43 -178.9(5) . . . . ?
C41 C42 C43 F6 -178.6(5) . . . . ?
C41 C42 C43 C41 0.0(9) . . . 2_576 ?
C43 C41 C42 I3 -179.7(4) 2_576 . . . ?
C43 C41 C42 C43 0.0(9) 2_576 . . . ?
O1 C3 C4 C5 -179.7(5) . . . . ?
O1 C17 C18 C19 -57.9(6) . . . . ?
O1 C17 C18 C20 177.5(5) . . . . ?
O3 C21 C22 C23 -56.6(8) . . . . ?
O3 C21 C22 C24 173.8(6) . . . . ?
O4 C14 C15 C16 -178.8(4) . . . . ?
O4 C25 C26 C27 169.7(6) . . . . ?
O4 C25 C26 C28 -63.1(10) . . . . ?
O6 C8 C9 N3 -0.5(6) . . . . ?
O6 C8 C9 C10 178.6(4) . . . . ?
O6 C29 C30 C31 174.4(6) . . . . ?
O6 C29 C30 C32 -62.9(7) . . . . ?
N1 C1 C2 N2 179.7(4) . . . . ?
N1 C1 C2 C3 1.8(7) . . . . ?
N2 C2 C3 O1 0.5(6) . . . . ?
N2 C2 C3 C4 -178.3(4) . . . . ?
N3 C9 C10 N4 -179.6(4) . . . . ?
N4 C6 C7 C8 0.8(7) . . . . ?
C1 N1 C5 C4 0.3(8) . . . . ?
C1 C2 C3 O1 178.5(4) . . . . ?
C1 C2 C3 C4 -0.3(7) . . . . ?
C2 N2 C33 O2 1.5(7) . . . . ?
C2 N2 C33 C11 -177.1(4) . . . . ?
C2 C3 C4 C5 -1.0(7) . . . . ?
C3 O1 C17 C18 177.3(4) . . . . ?
C3 C4 C5 N1 1.1(8) . . . . ?
C5 N1 C1 C2 -1.9(7) . . . . ?
C6 N4 C10 C9 0.7(7) . . . . ?
C6 C7 C8 O6 -179.7(4) . . . . ?
C6 C7 C8 C9 1.3(7) . . . . ?
C7 C8 C9 N3 178.6(4) . . . . ?
C7 C8 C9 C10 -2.3(6) . . . . ?
C8 O6 C29 C30 176.7(4) . . . . ?
C8 C9 C10 N4 1.3(7) . . . . ?
C9 N3 C34 O5 1.1(7) . . . . ?
C9 N3 C34 C13 -177.0(4) . . . . ?
C10 N4 C6 C7 -1.8(7) . . . . ?
C11 C12 C13 C14 2.0(6) . . . . ?
C11 C12 C13 C34 -175.6(4) . . . . ?
C12 C11 C16 O3 178.1(4) . . . . ?
C12 C11 C16 C15 -3.4(6) . . . . ?
C12 C11 C33 O2 -11.0(6) . . . . ?
C12 C11 C33 N2 167.7(4) . . . . ?
C12 C13 C14 O4 176.3(4) . . . . ?
C12 C13 C14 C15 -2.1(6) . . . . ?
C12 C13 C34 O5 -16.1(6) . . . . ?
C12 C13 C34 N3 162.0(4) . . . . ?
C13 C14 C15 C16 -0.5(6) . . . . ?
C14 O4 C25 C26 166.3(6) . . . . ?
C14 C13 C34 O5 166.6(4) . . . . ?
C14 C13 C34 N3 -15.3(6) . . . . ?
C14 C15 C16 O3 -178.2(4) . . . . ?
C14 C15 C16 C11 3.4(7) . . . . ?
C16 O3 C21 C22 118.6(5) . . . . ?
C16 C11 C12 C13 0.7(6) . . . . ?
C16 C11 C33 O2 165.9(4) . . . . ?
C16 C11 C33 N2 -15.5(6) . . . . ?
C17 O1 C3 C2 -174.9(4) . . . . ?
C17 O1 C3 C4 3.9(7) . . . . ?
C21 O3 C16 C11 -148.1(4) . . . . ?
C21 O3 C16 C15 33.5(6) . . . . ?
C25 O4 C14 C13 176.5(4) . . . . ?
C25 O4 C14 C15 -5.1(6) . . . . ?
C29 O6 C8 C7 10.4(6) . . . . ?
C29 O6 C8 C9 -170.5(4) . . . . ?
C33 N2 C2 C1 7.6(7) . . . . ?
C33 N2 C2 C3 -174.5(4) . . . . ?
C33 C11 C12 C13 177.9(4) . . . . ?
C33 C11 C16 O3 1.2(6) . . . . ?
C33 C11 C16 C15 179.7(4) . . . . ?
C34 N3 C9 C8 174.2(4) . . . . ?
C34 N3 C9 C10 -4.9(7) . . . . ?
C34 C13 C14 O4 -6.4(6) . . . . ?
C34 C13 C14 C15 175.2(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.284 0.181 0.313 79.5 14.8 ?
2 -0.284 -0.181 0.687 79.5 16.1 ?
3 0.227 0.808 0.294 8.8 0.0 ?
4 0.773 0.192 0.706 8.8 0.0 ?

_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_ga_80530a_a
_database_code_depnum_ccdc_archive 'CCDC 1887359'
loop_
_audit_author_name
_audit_author_address
'Zhanting Li'
;Fudan University
China
;
_audit_update_record             
;
2018-12-26 deposited with the CCDC.	2019-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H50 N4 O10'
_chemical_formula_weight         722.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   8.6303(2)
_cell_length_b                   14.1861(4)
_cell_length_c                   31.0691(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.6650(10)
_cell_angle_gamma                90
_cell_volume                     3796.02(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9943
_cell_measurement_theta_min      3.67
_cell_measurement_theta_max      54.91

_exptl_crystal_description       sheet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_F_000             1544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.482
_shelx_estimated_absorpt_T_min   0.849
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.34138
_diffrn_radiation_type           GaK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29491
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.674
_diffrn_reflns_theta_max         54.922
_diffrn_reflns_theta_full        53.594
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7213
_reflns_number_gt                5984
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0963P)²+3.6137P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7213
_refine_ls_number_parameters     493
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.1860
_refine_ls_wR_factor_gt          0.1737
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 1.0192(2) 0.37497(13) 0.35865(6) 0.0304(4) Uani 1 1 d . . . . .
H1 H 0.998(5) 0.297(3) 0.3470(13) 0.095(13) Uiso 1 1 d . . . . .
N2 N 0.9006(2) 0.52920(13) 0.44635(6) 0.0252(4) Uani 1 1 d . . . . .
H2 H 0.921(3) 0.588(2) 0.4527(9) 0.033(7) Uiso 1 1 d . . . . .
N3 N 0.4188(2) 0.49533(13) 0.63077(6) 0.0272(4) Uani 1 1 d . . . . .
H3 H 0.435(3) 0.555(2) 0.6363(9) 0.034(7) Uiso 1 1 d . . . . .
N4 N 0.1902(2) 0.31146(13) 0.68257(6) 0.0326(4) Uani 1 1 d . . . . .
O1 O 0.7721(2) 0.39934(11) 0.46676(5) 0.0366(4) Uani 1 1 d . . . . .
O2 O 0.4667(2) 0.37770(11) 0.58444(6) 0.0354(4) Uani 1 1 d . . . . .
O3 O 0.5457(2) 0.65916(11) 0.61454(5) 0.0352(4) Uani 1 1 d . . . . .
O4 O 0.84857(18) 0.68531(10) 0.49054(5) 0.0309(4) Uani 1 1 d . . . . .
O5 O 1.07822(17) 0.64279(10) 0.40570(5) 0.0281(3) Uani 1 1 d . . . . .
O6 O 0.3337(2) 0.58563(12) 0.69870(6) 0.0398(4) Uani 1 1 d . . . . .
C1 C 0.9525(3) 0.40239(15) 0.39468(7) 0.0275(5) Uani 1 1 d . . . . .
H1A H 0.8926 0.3583 0.4096 0.033 Uiso 1 1 calc R U . . .
C2 C 0.9695(2) 0.49317(14) 0.41043(6) 0.0233(4) Uani 1 1 d . . . . .
C3 C 1.0632(2) 0.55612(15) 0.38834(7) 0.0246(4) Uani 1 1 d . . . . .
C4 C 1.1305(3) 0.52619(16) 0.35138(7) 0.0291(5) Uani 1 1 d . . . . .
H4 H 1.1930 0.5678 0.3359 0.035 Uiso 1 1 calc R U . . .
C5 C 1.1050(3) 0.43501(16) 0.33745(7) 0.0316(5) Uani 1 1 d . . . . .
H5 H 1.1500 0.4144 0.3120 0.038 Uiso 1 1 calc R U . . .
C6 C 0.8036(2) 0.48241(14) 0.47213(7) 0.0239(4) Uani 1 1 d . . . . .
C7 C 0.7389(2) 0.53772(14) 0.50799(7) 0.0228(4) Uani 1 1 d . . . . .
C8 C 0.6464(2) 0.48740(14) 0.53471(7) 0.0229(4) Uani 1 1 d . . . . .
H8 H 0.6278 0.4227 0.5284 0.027 Uiso 1 1 calc R U . . .
C9 C 0.5788(2) 0.52609(14) 0.57032(7) 0.0230(4) Uani 1 1 d . . . . .
C10 C 0.6092(2) 0.62171(15) 0.57929(7) 0.0263(5) Uani 1 1 d . . . . .
C11 C 0.6995(3) 0.67420(15) 0.55283(7) 0.0298(5) Uani 1 1 d . . . . .
H11 H 0.7186 0.7388 0.5592 0.036 Uiso 1 1 calc R U . . .
C12 C 0.7624(2) 0.63406(15) 0.51714(7) 0.0248(4) Uani 1 1 d . . . . .
C13 C 0.4836(2) 0.45999(14) 0.59531(7) 0.0242(4) Uani 1 1 d . . . . .
C14 C 0.2769(3) 0.35452(15) 0.65406(7) 0.0279(5) Uani 1 1 d . . . . .
H14 H 0.3044 0.3204 0.6294 0.033 Uiso 1 1 calc R U . . .
C15 C 0.3279(2) 0.44639(15) 0.65916(7) 0.0256(4) Uani 1 1 d . . . . .
C16 C 0.2835(3) 0.49599(16) 0.69566(7) 0.0307(5) Uani 1 1 d . . . . .
C17 C 0.1946(3) 0.45079(19) 0.72493(8) 0.0407(6) Uani 1 1 d . . . . .
H17 H 0.1636 0.4829 0.7498 0.049 Uiso 1 1 calc R U . . .
C18 C 0.1519(3) 0.35825(18) 0.71728(8) 0.0400(6) Uani 1 1 d . . . . .
H18 H 0.0928 0.3268 0.7377 0.048 Uiso 1 1 calc R U . . .
C19 C 0.5817(3) 0.75292(16) 0.62988(8) 0.0371(6) Uani 1 1 d . . . . .
H19A H 0.6714 0.7777 0.6151 0.045 Uiso 1 1 calc R U . . .
H19B H 0.6107 0.7508 0.6612 0.045 Uiso 1 1 calc R U . . .
C20 C 0.4429(5) 0.8184(2) 0.62147(13) 0.0700(10) Uani 1 1 d . . . . .
H20 H 0.3530 0.7902 0.6357 0.084 Uiso 1 1 calc R U . . .
C21 C 0.4851(6) 0.9116(2) 0.64467(18) 0.1013(17) Uani 1 1 d . . . . .
H21A H 0.5760 0.9395 0.6322 0.152 Uiso 1 1 calc R U . . .
H21B H 0.5090 0.8994 0.6754 0.152 Uiso 1 1 calc R U . . .
H21C H 0.3973 0.9553 0.6412 0.152 Uiso 1 1 calc R U . . .
C22 C 0.3957(6) 0.8317(4) 0.57589(16) 0.1012(16) Uani 1 1 d . . . . .
H22A H 0.4786 0.8640 0.5616 0.152 Uiso 1 1 calc R U . . .
H22B H 0.3008 0.8698 0.5732 0.152 Uiso 1 1 calc R U . . .
H22C H 0.3760 0.7702 0.5623 0.152 Uiso 1 1 calc R U . . .
C23 C 0.8784(3) 0.78418(15) 0.49982(8) 0.0299(5) Uani 1 1 d . . . . .
H23A H 0.9708 0.8045 0.4849 0.036 Uiso 1 1 calc R U . . .
H23B H 0.9023 0.7919 0.5312 0.036 Uiso 1 1 calc R U . . .
C24 C 0.7422(3) 0.84736(16) 0.48581(8) 0.0325(5) Uani 1 1 d . . . . .
H24 H 0.6485 0.8240 0.4999 0.039 Uiso 1 1 calc R U . . .
C25 C 0.7069(3) 0.8460(2) 0.43743(9) 0.0450(6) Uani 1 1 d . . . . .
H25A H 0.7984 0.8672 0.4230 0.068 Uiso 1 1 calc R U . . .
H25B H 0.6195 0.8882 0.4299 0.068 Uiso 1 1 calc R U . . .
H25C H 0.6800 0.7817 0.4281 0.068 Uiso 1 1 calc R U . . .
C26 C 0.7769(5) 0.9470(2) 0.50180(12) 0.0690(10) Uani 1 1 d . . . . .
H26A H 0.8012 0.9458 0.5330 0.103 Uiso 1 1 calc R U . . .
H26B H 0.6860 0.9871 0.4952 0.103 Uiso 1 1 calc R U . . .
H26C H 0.8659 0.9721 0.4874 0.103 Uiso 1 1 calc R U . . .
C27 C 1.1735(3) 0.71035(15) 0.38453(7) 0.0296(5) Uani 1 1 d . . . . .
H27A H 1.1266 0.7245 0.3553 0.035 Uiso 1 1 calc R U . . .
H27B H 1.2784 0.6839 0.3816 0.035 Uiso 1 1 calc R U . . .
C28 C 1.1850(3) 0.79951(15) 0.41116(8) 0.0316(5) Uani 1 1 d . . . . .
H28 H 1.0777 0.8229 0.4153 0.038 Uiso 1 1 calc R U . . .
C29 C 1.2678(3) 0.78220(17) 0.45538(8) 0.0364(5) Uani 1 1 d . . . . .
H29A H 1.2124 0.7334 0.4706 0.055 Uiso 1 1 calc R U . . .
H29B H 1.2697 0.8407 0.4722 0.055 Uiso 1 1 calc R U . . .
H29C H 1.3744 0.7613 0.4517 0.055 Uiso 1 1 calc R U . . .
C30 C 1.2701(3) 0.87310(18) 0.38577(10) 0.0448(6) Uani 1 1 d . . . . .
H30A H 1.3737 0.8495 0.3801 0.067 Uiso 1 1 calc R U . . .
H30B H 1.2801 0.9316 0.4025 0.067 Uiso 1 1 calc R U . . .
H30C H 1.2114 0.8855 0.3583 0.067 Uiso 1 1 calc R U . . .
C31 C 0.2833(4) 0.6431(2) 0.73382(11) 0.0561(8) Uani 1 1 d . . . . .
H31A H 0.1740 0.6625 0.7276 0.067 Uiso 1 1 calc R U . . .
H31B H 0.2893 0.6059 0.7608 0.067 Uiso 1 1 calc R U . . .
C32 C 0.3794(4) 0.7249(3) 0.73911(12) 0.0679(10) Uani 1 1 d . . . . .
H32 H 0.3652 0.7593 0.7110 0.081 Uiso 1 1 calc R U . . .
C33 C 0.3222(5) 0.7923(2) 0.77219(12) 0.0732(11) Uani 1 1 d . . . . .
H33A H 0.2104 0.8024 0.7666 0.110 Uiso 1 1 calc R U . . .
H33B H 0.3768 0.8526 0.7703 0.110 Uiso 1 1 calc R U . . .
H33C H 0.3423 0.7657 0.8011 0.110 Uiso 1 1 calc R U . . .
C34 C 0.5460(5) 0.7104(4) 0.74579(15) 0.0926(14) Uani 1 1 d . . . . .
H34A H 0.5698 0.6833 0.7745 0.139 Uiso 1 1 calc R U . . .
H34B H 0.5996 0.7710 0.7436 0.139 Uiso 1 1 calc R U . . .
H34C H 0.5808 0.6672 0.7238 0.139 Uiso 1 1 calc R U . . .
C35 C 1.0009(3) 0.14686(17) 0.36117(8) 0.0359(5) Uani 1 1 d . . . . .
C36 C 0.9619(3) 0.04694(16) 0.35042(8) 0.0340(5) Uani 1 1 d . . . . .
H36 H 0.9644 0.0028 0.3735 0.041 Uiso 1 1 calc R U . . .
C37 C 0.9243(3) 0.01545(16) 0.31138(7) 0.0324(5) Uani 1 1 d . . . . .
H37 H 0.9140 0.0597 0.2884 0.039 Uiso 1 1 calc R U . . .
C38 C 0.8969(3) -0.08587(16) 0.30124(8) 0.0346(5) Uani 1 1 d . . . . .
O7 O 0.9755(2) 0.20771(12) 0.33107(6) 0.0431(4) Uani 1 1 d . . . . .
O8 O 1.0561(3) 0.16499(15) 0.39734(6) 0.0636(6) Uani 1 1 d . . . . .
O9 O 0.8762(2) -0.13864(12) 0.33429(6) 0.0421(4) Uani 1 1 d . . . . .
H9 H 0.855(5) -0.203(3) 0.3271(13) 0.085(12) Uiso 1 1 d . . . . .
O10 O 0.8996(3) -0.11510(14) 0.26487(6) 0.0674(7) 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
N1 C5 1.330(3) . ?
N1 C1 1.348(3) . ?
N1 H1 1.17(4) . ?
N2 C6 1.367(3) . ?
N2 C2 1.394(3) . ?
N2 H2 0.87(3) . ?
N3 C13 1.362(3) . ?
N3 C15 1.402(3) . ?
N3 H3 0.87(3) . ?
N4 C18 1.326(3) . ?
N4 C14 1.343(3) . ?
O1 C6 1.218(3) . ?
O2 C13 1.221(3) . ?
O3 C10 1.363(3) . ?
O3 C19 1.440(3) . ?
O4 C12 1.358(3) . ?
O4 C23 1.452(2) . ?
O5 C3 1.345(3) . ?
O5 C27 1.448(3) . ?
O6 C16 1.345(3) . ?
O6 C31 1.451(3) . ?
C1 C2 1.382(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.412(3) . ?
C3 C4 1.386(3) . ?
C4 C5 1.377(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.499(3) . ?
C7 C8 1.386(3) . ?
C7 C12 1.408(3) . ?
C8 C9 1.396(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.406(3) . ?
C9 C13 1.496(3) . ?
C10 C11 1.385(3) . ?
C11 C12 1.388(3) . ?
C11 H11 0.9500 . ?
C14 C15 1.381(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.408(3) . ?
C16 C17 1.384(3) . ?
C17 C18 1.380(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.525(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C22 1.460(6) . ?
C20 C21 1.539(5) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.519(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.515(4) . ?
C24 C26 1.521(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.511(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C30 1.525(3) . ?
C28 C29 1.527(3) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.430(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C34 1.454(6) . ?
C32 C33 1.510(4) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 O8 1.220(3) . ?
C35 O7 1.281(3) . ?
C35 C36 1.490(3) . ?
C36 C37 1.314(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.487(3) . ?
C37 H37 0.9500 . ?
C38 O10 1.205(3) . ?
C38 O9 1.292(3) . ?
O7 H1 1.37(4) . ?
O9 H9 0.96(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
C5 N1 C1 120.46(19) . . ?
C5 N1 H1 122(2) . . ?
C1 N1 H1 117(2) . . ?
C6 N2 C2 126.82(18) . . ?
C6 N2 H2 117.0(18) . . ?
C2 N2 H2 116.2(18) . . ?
C13 N3 C15 126.99(19) . . ?
C13 N3 H3 116.6(18) . . ?
C15 N3 H3 116.4(18) . . ?
C18 N4 C14 119.2(2) . . ?
C10 O3 C19 122.46(17) . . ?
C12 O4 C23 119.58(16) . . ?
C3 O5 C27 117.75(16) . . ?
C16 O6 C31 118.3(2) . . ?
N1 C1 C2 121.4(2) . . ?
N1 C1 H1A 119.3 . . ?
C2 C1 H1A 119.3 . . ?
C1 C2 N2 125.73(19) . . ?
C1 C2 C3 117.92(19) . . ?
N2 C2 C3 116.34(18) . . ?
O5 C3 C4 125.3(2) . . ?
O5 C3 C2 115.24(18) . . ?
C4 C3 C2 119.49(19) . . ?
C5 C4 C3 118.7(2) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 121.9(2) . . ?
N1 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
O1 C6 N2 121.91(19) . . ?
O1 C6 C7 121.18(19) . . ?
N2 C6 C7 116.90(18) . . ?
C8 C7 C12 117.38(18) . . ?
C8 C7 C6 115.57(18) . . ?
C12 C7 C6 127.05(19) . . ?
C7 C8 C9 123.94(19) . . ?
C7 C8 H8 118.0 . . ?
C9 C8 H8 118.0 . . ?
C8 C9 C10 117.00(19) . . ?
C8 C9 C13 115.86(18) . . ?
C10 C9 C13 127.13(19) . . ?
O3 C10 C11 122.50(19) . . ?
O3 C10 C9 117.09(19) . . ?
C11 C10 C9 120.40(19) . . ?
C10 C11 C12 121.1(2) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
O4 C12 C11 121.61(19) . . ?
O4 C12 C7 118.31(18) . . ?
C11 C12 C7 120.08(19) . . ?
O2 C13 N3 121.8(2) . . ?
O2 C13 C9 121.00(19) . . ?
N3 C13 C9 117.14(18) . . ?
N4 C14 C15 122.7(2) . . ?
N4 C14 H14 118.6 . . ?
C15 C14 H14 118.6 . . ?
C14 C15 N3 125.6(2) . . ?
C14 C15 C16 117.6(2) . . ?
N3 C15 C16 116.82(19) . . ?
O6 C16 C17 125.5(2) . . ?
O6 C16 C15 115.2(2) . . ?
C17 C16 C15 119.2(2) . . ?
C18 C17 C16 118.7(2) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
N4 C18 C17 122.6(2) . . ?
N4 C18 H18 118.7 . . ?
C17 C18 H18 118.7 . . ?
O3 C19 C20 110.8(2) . . ?
O3 C19 H19A 109.5 . . ?
C20 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C22 C20 C19 114.3(3) . . ?
C22 C20 C21 112.7(4) . . ?
C19 C20 C21 106.4(3) . . ?
C22 C20 H20 107.7 . . ?
C19 C20 H20 107.7 . . ?
C21 C20 H20 107.7 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O4 C23 C24 112.88(18) . . ?
O4 C23 H23A 109.0 . . ?
C24 C23 H23A 109.0 . . ?
O4 C23 H23B 109.0 . . ?
C24 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C25 C24 C23 112.3(2) . . ?
C25 C24 C26 111.0(2) . . ?
C23 C24 C26 108.8(2) . . ?
C25 C24 H24 108.2 . . ?
C23 C24 H24 108.2 . . ?
C26 C24 H24 108.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O5 C27 C28 108.95(18) . . ?
O5 C27 H27A 109.9 . . ?
C28 C27 H27A 109.9 . . ?
O5 C27 H27B 109.9 . . ?
C28 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C27 C28 C30 107.9(2) . . ?
C27 C28 C29 111.62(19) . . ?
C30 C28 C29 111.2(2) . . ?
C27 C28 H28 108.7 . . ?
C30 C28 H28 108.7 . . ?
C29 C28 H28 108.7 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 O6 110.1(3) . . ?
C32 C31 H31A 109.6 . . ?
O6 C31 H31A 109.6 . . ?
C32 C31 H31B 109.6 . . ?
O6 C31 H31B 109.6 . . ?
H31A C31 H31B 108.2 . . ?
C31 C32 C34 117.5(4) . . ?
C31 C32 C33 112.3(3) . . ?
C34 C32 C33 110.8(3) . . ?
C31 C32 H32 104.9 . . ?
C34 C32 H32 104.9 . . ?
C33 C32 H32 104.9 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O8 C35 O7 124.7(2) . . ?
O8 C35 C36 118.5(2) . . ?
O7 C35 C36 116.8(2) . . ?
C37 C36 C35 124.7(2) . . ?
C37 C36 H36 117.6 . . ?
C35 C36 H36 117.6 . . ?
C36 C37 C38 123.4(2) . . ?
C36 C37 H37 118.3 . . ?
C38 C37 H37 118.3 . . ?
O10 C38 O9 123.9(2) . . ?
O10 C38 C37 121.2(2) . . ?
O9 C38 C37 114.8(2) . . ?
C35 O7 H1 110.2(18) . . ?
C38 O9 H9 114(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
C5 N1 C1 C2 0.7(3) . . . . ?
N1 C1 C2 N2 177.4(2) . . . . ?
N1 C1 C2 C3 -1.9(3) . . . . ?
C6 N2 C2 C1 -0.7(3) . . . . ?
C6 N2 C2 C3 178.70(19) . . . . ?
C27 O5 C3 C4 -0.7(3) . . . . ?
C27 O5 C3 C2 179.80(18) . . . . ?
C1 C2 C3 O5 -178.58(18) . . . . ?
N2 C2 C3 O5 2.0(3) . . . . ?
C1 C2 C3 C4 1.9(3) . . . . ?
N2 C2 C3 C4 -177.53(19) . . . . ?
O5 C3 C4 C5 179.9(2) . . . . ?
C2 C3 C4 C5 -0.7(3) . . . . ?
C1 N1 C5 C4 0.7(3) . . . . ?
C3 C4 C5 N1 -0.6(3) . . . . ?
C2 N2 C6 O1 3.3(3) . . . . ?
C2 N2 C6 C7 -177.60(18) . . . . ?
O1 C6 C7 C8 1.8(3) . . . . ?
N2 C6 C7 C8 -177.29(17) . . . . ?
O1 C6 C7 C12 -178.3(2) . . . . ?
N2 C6 C7 C12 2.7(3) . . . . ?
C12 C7 C8 C9 -1.4(3) . . . . ?
C6 C7 C8 C9 178.51(18) . . . . ?
C7 C8 C9 C10 -0.7(3) . . . . ?
C7 C8 C9 C13 -179.63(18) . . . . ?
C19 O3 C10 C11 -7.2(3) . . . . ?
C19 O3 C10 C9 173.1(2) . . . . ?
C8 C9 C10 O3 -178.79(18) . . . . ?
C13 C9 C10 O3 0.0(3) . . . . ?
C8 C9 C10 C11 1.5(3) . . . . ?
C13 C9 C10 C11 -179.6(2) . . . . ?
O3 C10 C11 C12 -179.9(2) . . . . ?
C9 C10 C11 C12 -0.3(3) . . . . ?
C23 O4 C12 C11 1.0(3) . . . . ?
C23 O4 C12 C7 -178.29(19) . . . . ?
C10 C11 C12 O4 178.7(2) . . . . ?
C10 C11 C12 C7 -1.9(3) . . . . ?
C8 C7 C12 O4 -177.94(18) . . . . ?
C6 C7 C12 O4 2.1(3) . . . . ?
C8 C7 C12 C11 2.7(3) . . . . ?
C6 C7 C12 C11 -177.2(2) . . . . ?
C15 N3 C13 O2 0.2(3) . . . . ?
C15 N3 C13 C9 -178.96(19) . . . . ?
C8 C9 C13 O2 -0.5(3) . . . . ?
C10 C9 C13 O2 -179.3(2) . . . . ?
C8 C9 C13 N3 178.68(18) . . . . ?
C10 C9 C13 N3 -0.2(3) . . . . ?
C18 N4 C14 C15 -0.4(3) . . . . ?
N4 C14 C15 N3 179.8(2) . . . . ?
N4 C14 C15 C16 -1.0(3) . . . . ?
C13 N3 C15 C14 -5.7(4) . . . . ?
C13 N3 C15 C16 175.1(2) . . . . ?
C31 O6 C16 C17 -4.4(4) . . . . ?
C31 O6 C16 C15 175.7(2) . . . . ?
C14 C15 C16 O6 -178.8(2) . . . . ?
N3 C15 C16 O6 0.4(3) . . . . ?
C14 C15 C16 C17 1.2(3) . . . . ?
N3 C15 C16 C17 -179.5(2) . . . . ?
O6 C16 C17 C18 179.9(2) . . . . ?
C15 C16 C17 C18 -0.1(4) . . . . ?
C14 N4 C18 C17 1.6(4) . . . . ?
C16 C17 C18 N4 -1.3(4) . . . . ?
C10 O3 C19 C20 109.3(3) . . . . ?
O3 C19 C20 C22 -62.8(4) . . . . ?
O3 C19 C20 C21 172.0(3) . . . . ?
C12 O4 C23 C24 -79.5(2) . . . . ?
O4 C23 C24 C25 -63.6(3) . . . . ?
O4 C23 C24 C26 173.1(2) . . . . ?
C3 O5 C27 C28 -175.42(18) . . . . ?
O5 C27 C28 C30 -173.71(19) . . . . ?
O5 C27 C28 C29 63.8(2) . . . . ?
C16 O6 C31 C32 163.9(3) . . . . ?
O6 C31 C32 C34 -55.5(5) . . . . ?
O6 C31 C32 C33 174.1(3) . . . . ?
O8 C35 C36 C37 -169.3(3) . . . . ?
O7 C35 C36 C37 9.8(4) . . . . ?
C35 C36 C37 C38 175.5(2) . . . . ?
C36 C37 C38 O10 -161.9(3) . . . . ?
C36 C37 C38 O9 15.7(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O4 0.87(3) 1.95(3) 2.659(2) 138(2) .
N3 H3 O3 0.87(3) 1.91(3) 2.632(2) 139(2) .
O9 H9 N4 0.96(4) 1.61(4) 2.564(3) 176(4) 3_656

_refine_diff_density_max         1.359
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.066

