# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_qzdw1018_0m
_database_code_depnum_ccdc_archive 'CCDC 1888466'
loop_
_audit_author_name
_audit_author_address
'Li xiao nian'
;UCAS, KIB
China
;
_audit_update_record             
;
2019-01-03 deposited with the CCDC.	2020-07-23 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         'C19 H19 F3 O7 S'
_chemical_formula_sum            'C19 H19 F3 O7 S'
_chemical_formula_weight         448.40

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'
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'
S S 0.1246 0.1234 '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/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.1889(12)
_cell_length_b                   15.6583(16)
_cell_length_c                   11.3387(12)
_cell_angle_alpha                90
_cell_angle_beta                 103.564(2)
_cell_angle_gamma                90
_cell_volume                     1931.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8004
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      30.68

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_F_000             928
_exptl_transmission_factor_min   0.4165
_exptl_transmission_factor_max   0.4939
_exptl_crystal_size_max          0.730
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.237
_shelx_estimated_absorpt_T_min   0.846
_shelx_estimated_absorpt_T_max   0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21253
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.260
_diffrn_reflns_theta_max         31.139
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5730
_reflns_number_gt                4723
_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 (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)+(0.0605P)²+0.5349P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5730
_refine_ls_number_parameters     273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.82167(3) 0.20475(2) 0.92476(3) 0.02000(9) Uani 1 1 d . . . . .
F1 F 0.96052(10) 0.32811(6) 0.87791(10) 0.0366(2) Uani 1 1 d . . . . .
F2 F 1.01699(9) 0.27798(6) 1.05940(9) 0.0325(2) Uani 1 1 d . . . . .
F3 F 0.85689(10) 0.35843(6) 1.01138(11) 0.0424(3) Uani 1 1 d . . . . .
O1 O 0.74368(9) -0.24943(6) 1.11181(8) 0.01820(19) Uani 1 1 d . . . . .
O2 O 0.90970(9) 0.14896(6) 0.87038(8) 0.01697(19) Uani 1 1 d . . . . .
O3 O 0.80862(11) 0.16502(8) 1.03332(10) 0.0310(3) Uani 1 1 d . . . . .
O4 O 0.71922(10) 0.23375(8) 0.83436(11) 0.0308(3) Uani 1 1 d . . . . .
O5 O 0.49680(8) -0.00677(6) 0.78987(9) 0.01785(19) Uani 1 1 d . . . . .
O6 O 0.83534(9) -0.00837(6) 0.50232(8) 0.01806(19) Uani 1 1 d . . . . .
O7 O 0.95723(9) -0.11831(6) 0.57314(9) 0.0216(2) Uani 1 1 d . . . . .
C1 C 0.70254(13) -0.26973(9) 1.21901(12) 0.0216(3) Uani 1 1 d . . . . .
H2 H 0.6803 -0.2170 1.2553 0.032 Uiso 1 1 calc R U . . .
H3 H 0.7686 -0.2988 1.2773 0.032 Uiso 1 1 calc R U . . .
H1 H 0.6306 -0.3073 1.1978 0.032 Uiso 1 1 calc R U . . .
C2 C 0.67393(12) -0.19090(8) 1.03379(11) 0.0146(2) Uani 1 1 d . . . . .
C3 C 0.73701(11) -0.14489(8) 0.96192(11) 0.0138(2) Uani 1 1 d . . . . .
H9 H 0.8218 -0.1563 0.9689 0.017 Uiso 1 1 calc R U . . .
C4 C 0.67881(11) -0.08234(8) 0.87975(11) 0.0128(2) Uani 1 1 d . . . . .
C5 C 0.75271(11) -0.03575(8) 0.80858(11) 0.0130(2) Uani 1 1 d . . . . .
C6 C 0.72425(11) 0.03631(8) 0.74294(11) 0.0152(2) Uani 1 1 d . . . . .
H18 H 0.6483 0.0657 0.7334 0.018 Uiso 1 1 calc R U . . .
C7 C 0.82662(11) 0.06476(8) 0.68644(11) 0.0131(2) Uani 1 1 d . . . . .
C8 C 0.89872(12) 0.14588(8) 0.73613(11) 0.0156(2) Uani 1 1 d . . . . .
H19 H 0.8623 0.1990 0.6935 0.019 Uiso 1 1 calc R U . . .
C9 C 0.92066(14) 0.29808(9) 0.97120(14) 0.0241(3) Uani 1 1 d . . . . .
C10 C 0.54967(12) -0.17674(9) 1.02301(12) 0.0170(2) Uani 1 1 d . . . . .
H8 H 0.5059 -0.2086 1.0705 0.020 Uiso 1 1 calc R U . . .
C11 C 0.48949(11) -0.11505(9) 0.94160(12) 0.0171(2) Uani 1 1 d . . . . .
H7 H 0.4043 -0.1050 0.9343 0.021 Uiso 1 1 calc R U . . .
C12 C 0.55198(11) -0.06784(8) 0.87079(11) 0.0141(2) Uani 1 1 d . . . . .
C13 C 0.36694(11) 0.00338(9) 0.77221(13) 0.0190(3) Uani 1 1 d . . . . .
H4 H 0.3259 -0.0509 0.7450 0.028 Uiso 1 1 calc R U . . .
H5 H 0.3380 0.0474 0.7107 0.028 Uiso 1 1 calc R U . . .
H6 H 0.3478 0.0206 0.8488 0.028 Uiso 1 1 calc R U . . .
C14 C 0.88081(11) -0.06737(8) 0.80696(11) 0.0151(2) Uani 1 1 d . . . . .
H16 H 0.8785 -0.1277 0.7806 0.018 Uiso 1 1 calc R U . . .
H17 H 0.9370 -0.0622 0.8883 0.018 Uiso 1 1 calc R U . . .
C15 C 0.92200(11) -0.00842(8) 0.71474(11) 0.0130(2) Uani 1 1 d . . . . .
C16 C 1.05033(11) 0.03390(9) 0.75723(12) 0.0177(2) Uani 1 1 d . . . . .
H13 H 1.0820 0.0274 0.8459 0.021 Uiso 1 1 calc R U . . .
H12 H 1.1099 0.0081 0.7154 0.021 Uiso 1 1 calc R U . . .
C17 C 1.02852(12) 0.12861(9) 0.72270(12) 0.0188(3) Uani 1 1 d . . . . .
H11 H 1.0887 0.1655 0.7779 0.023 Uiso 1 1 calc R U . . .
H10 H 1.0350 0.1387 0.6382 0.023 Uiso 1 1 calc R U . . .
C18 C 0.90961(11) -0.05255(8) 0.59331(11) 0.0150(2) Uani 1 1 d . . . . .
C19 C 0.78951(12) 0.06905(8) 0.54599(12) 0.0176(2) Uani 1 1 d . . . . .
H14 H 0.6990 0.0725 0.5171 0.021 Uiso 1 1 calc R U . . .
H15 H 0.8264 0.1199 0.5165 0.021 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
S1 O3 1.4170(11) . ?
S1 O4 1.4212(12) . ?
S1 O2 1.5488(9) . ?
S1 C9 1.8347(16) . ?
F1 C9 1.3267(18) . ?
F2 C9 1.3248(18) . ?
F3 C9 1.3275(16) . ?
O1 C2 1.3813(15) . ?
O1 C1 1.4327(16) . ?
O2 C8 1.4989(15) . ?
O5 C12 1.3681(15) . ?
O5 C13 1.4283(14) . ?
O6 C18 1.3534(16) . ?
O6 C19 1.4480(16) . ?
O7 C18 1.2056(16) . ?
C1 H2 0.9800 . ?
C1 H3 0.9800 . ?
C1 H1 0.9800 . ?
C2 C10 1.3846(18) . ?
C2 C3 1.3969(16) . ?
C3 C4 1.4024(17) . ?
C3 H9 0.9500 . ?
C4 C12 1.4170(16) . ?
C4 C5 1.4765(16) . ?
C5 C6 1.3480(17) . ?
C5 C14 1.5206(16) . ?
C6 C7 1.5050(16) . ?
C6 H18 0.9500 . ?
C7 C8 1.5389(17) . ?
C7 C15 1.5474(17) . ?
C7 C19 1.5502(18) . ?
C8 C17 1.5196(18) . ?
C8 H19 1.0000 . ?
C10 C11 1.3954(19) . ?
C10 H8 0.9500 . ?
C11 C12 1.3940(17) . ?
C11 H7 0.9500 . ?
C13 H4 0.9800 . ?
C13 H5 0.9800 . ?
C13 H6 0.9800 . ?
C14 C15 1.5440(17) . ?
C14 H16 0.9900 . ?
C14 H17 0.9900 . ?
C15 C18 1.5176(17) . ?
C15 C16 1.5519(17) . ?
C16 C17 1.5386(19) . ?
C16 H13 0.9900 . ?
C16 H12 0.9900 . ?
C17 H11 0.9900 . ?
C17 H10 0.9900 . ?
C19 H14 0.9900 . ?
C19 H15 0.9900 . ?

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
O3 S1 O4 122.47(7) . . ?
O3 S1 O2 107.63(6) . . ?
O4 S1 O2 111.95(6) . . ?
O3 S1 C9 106.18(7) . . ?
O4 S1 C9 106.44(7) . . ?
O2 S1 C9 99.56(6) . . ?
C2 O1 C1 116.41(10) . . ?
C8 O2 S1 120.94(8) . . ?
C12 O5 C13 117.14(10) . . ?
C18 O6 C19 111.76(10) . . ?
O1 C1 H2 109.5 . . ?
O1 C1 H3 109.5 . . ?
H2 C1 H3 109.5 . . ?
O1 C1 H1 109.5 . . ?
H2 C1 H1 109.5 . . ?
H3 C1 H1 109.5 . . ?
O1 C2 C10 124.58(11) . . ?
O1 C2 C3 115.40(11) . . ?
C10 C2 C3 120.01(12) . . ?
C2 C3 C4 121.90(11) . . ?
C2 C3 H9 119.1 . . ?
C4 C3 H9 119.1 . . ?
C3 C4 C12 117.43(11) . . ?
C3 C4 C5 118.41(10) . . ?
C12 C4 C5 124.16(11) . . ?
C6 C5 C4 128.70(11) . . ?
C6 C5 C14 111.54(10) . . ?
C4 C5 C14 119.73(11) . . ?
C5 C6 C7 112.21(10) . . ?
C5 C6 H18 123.9 . . ?
C7 C6 H18 123.9 . . ?
C6 C7 C8 118.32(10) . . ?
C6 C7 C15 104.43(10) . . ?
C8 C7 C15 104.98(10) . . ?
C6 C7 C19 113.76(10) . . ?
C8 C7 C19 109.36(10) . . ?
C15 C7 C19 104.52(10) . . ?
O2 C8 C17 104.76(10) . . ?
O2 C8 C7 108.03(9) . . ?
C17 C8 C7 104.34(10) . . ?
O2 C8 H19 113.0 . . ?
C17 C8 H19 113.0 . . ?
C7 C8 H19 113.0 . . ?
F2 C9 F1 108.66(13) . . ?
F2 C9 F3 108.52(12) . . ?
F1 C9 F3 109.24(13) . . ?
F2 C9 S1 110.91(10) . . ?
F1 C9 S1 110.28(10) . . ?
F3 C9 S1 109.18(11) . . ?
C2 C10 C11 119.21(11) . . ?
C2 C10 H8 120.4 . . ?
C11 C10 H8 120.4 . . ?
C12 C11 C10 121.24(11) . . ?
C12 C11 H7 119.4 . . ?
C10 C11 H7 119.4 . . ?
O5 C12 C11 123.26(11) . . ?
O5 C12 C4 116.54(10) . . ?
C11 C12 C4 120.20(11) . . ?
O5 C13 H4 109.5 . . ?
O5 C13 H5 109.5 . . ?
H4 C13 H5 109.5 . . ?
O5 C13 H6 109.5 . . ?
H4 C13 H6 109.5 . . ?
H5 C13 H6 109.5 . . ?
C5 C14 C15 104.21(10) . . ?
C5 C14 H16 110.9 . . ?
C15 C14 H16 110.9 . . ?
C5 C14 H17 110.9 . . ?
C15 C14 H17 110.9 . . ?
H16 C14 H17 108.9 . . ?
C18 C15 C14 111.34(10) . . ?
C18 C15 C7 103.73(10) . . ?
C14 C15 C7 106.40(9) . . ?
C18 C15 C16 110.92(9) . . ?
C14 C15 C16 116.52(10) . . ?
C7 C15 C16 106.92(10) . . ?
C17 C16 C15 104.63(10) . . ?
C17 C16 H13 110.8 . . ?
C15 C16 H13 110.8 . . ?
C17 C16 H12 110.8 . . ?
C15 C16 H12 110.8 . . ?
H13 C16 H12 108.9 . . ?
C8 C17 C16 104.14(10) . . ?
C8 C17 H11 110.9 . . ?
C16 C17 H11 110.9 . . ?
C8 C17 H10 110.9 . . ?
C16 C17 H10 110.9 . . ?
H11 C17 H10 108.9 . . ?
O7 C18 O6 120.77(12) . . ?
O7 C18 C15 127.64(12) . . ?
O6 C18 C15 111.59(10) . . ?
O6 C19 C7 106.50(10) . . ?
O6 C19 H14 110.4 . . ?
C7 C19 H14 110.4 . . ?
O6 C19 H15 110.4 . . ?
C7 C19 H15 110.4 . . ?
H14 C19 H15 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 S1 O2 C8 150.53(9) . . . . ?
O4 S1 O2 C8 13.19(11) . . . . ?
C9 S1 O2 C8 -98.98(10) . . . . ?
C1 O1 C2 C10 -26.87(18) . . . . ?
C1 O1 C2 C3 153.72(11) . . . . ?
O1 C2 C3 C4 -179.02(11) . . . . ?
C10 C2 C3 C4 1.54(19) . . . . ?
C2 C3 C4 C12 -0.76(18) . . . . ?
C2 C3 C4 C5 179.09(11) . . . . ?
C3 C4 C5 C6 -166.19(13) . . . . ?
C12 C4 C5 C6 13.6(2) . . . . ?
C3 C4 C5 C14 11.81(17) . . . . ?
C12 C4 C5 C14 -168.35(11) . . . . ?
C4 C5 C6 C7 178.37(12) . . . . ?
C14 C5 C6 C7 0.23(15) . . . . ?
C5 C6 C7 C8 -109.62(13) . . . . ?
C5 C6 C7 C15 6.61(14) . . . . ?
C5 C6 C7 C19 119.94(12) . . . . ?
S1 O2 C8 C17 150.42(9) . . . . ?
S1 O2 C8 C7 -98.78(10) . . . . ?
C6 C7 C8 O2 35.65(14) . . . . ?
C15 C7 C8 O2 -80.28(11) . . . . ?
C19 C7 C8 O2 168.06(9) . . . . ?
C6 C7 C8 C17 146.73(11) . . . . ?
C15 C7 C8 C17 30.81(12) . . . . ?
C19 C7 C8 C17 -80.85(12) . . . . ?
O3 S1 C9 F2 45.56(12) . . . . ?
O4 S1 C9 F2 177.51(10) . . . . ?
O2 S1 C9 F2 -66.08(11) . . . . ?
O3 S1 C9 F1 165.98(10) . . . . ?
O4 S1 C9 F1 -62.07(12) . . . . ?
O2 S1 C9 F1 54.35(11) . . . . ?
O3 S1 C9 F3 -73.98(12) . . . . ?
O4 S1 C9 F3 57.97(12) . . . . ?
O2 S1 C9 F3 174.38(10) . . . . ?
O1 C2 C10 C11 179.34(12) . . . . ?
C3 C2 C10 C11 -1.27(19) . . . . ?
C2 C10 C11 C12 0.3(2) . . . . ?
C13 O5 C12 C11 -4.80(18) . . . . ?
C13 O5 C12 C4 174.74(11) . . . . ?
C10 C11 C12 O5 180.00(12) . . . . ?
C10 C11 C12 C4 0.5(2) . . . . ?
C3 C4 C12 O5 -179.80(11) . . . . ?
C5 C4 C12 O5 0.37(18) . . . . ?
C3 C4 C12 C11 -0.24(18) . . . . ?
C5 C4 C12 C11 179.92(12) . . . . ?
C6 C5 C14 C15 -6.98(14) . . . . ?
C4 C5 C14 C15 174.70(11) . . . . ?
C5 C14 C15 C18 -101.77(11) . . . . ?
C5 C14 C15 C7 10.60(13) . . . . ?
C5 C14 C15 C16 129.67(11) . . . . ?
C6 C7 C15 C18 107.03(10) . . . . ?
C8 C7 C15 C18 -127.80(10) . . . . ?
C19 C7 C15 C18 -12.73(12) . . . . ?
C6 C7 C15 C14 -10.51(12) . . . . ?
C8 C7 C15 C14 114.66(10) . . . . ?
C19 C7 C15 C14 -130.27(10) . . . . ?
C6 C7 C15 C16 -135.68(10) . . . . ?
C8 C7 C15 C16 -10.51(12) . . . . ?
C19 C7 C15 C16 104.56(11) . . . . ?
C18 C15 C16 C17 99.08(12) . . . . ?
C14 C15 C16 C17 -132.15(11) . . . . ?
C7 C15 C16 C17 -13.37(12) . . . . ?
O2 C8 C17 C16 73.91(12) . . . . ?
C7 C8 C17 C16 -39.53(12) . . . . ?
C15 C16 C17 C8 32.53(12) . . . . ?
C19 O6 C18 O7 -179.12(11) . . . . ?
C19 O6 C18 C15 0.60(13) . . . . ?
C14 C15 C18 O7 -58.18(16) . . . . ?
C7 C15 C18 O7 -172.22(12) . . . . ?
C16 C15 C18 O7 73.32(16) . . . . ?
C14 C15 C18 O6 122.12(11) . . . . ?
C7 C15 C18 O6 8.08(12) . . . . ?
C16 C15 C18 O6 -106.38(11) . . . . ?
C18 O6 C19 C7 -9.12(13) . . . . ?
C6 C7 C19 O6 -99.79(12) . . . . ?
C8 C7 C19 O6 125.45(10) . . . . ?
C15 C7 C19 O6 13.49(12) . . . . ?

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
C19 H15 O1 0.99 2.53 3.3325(17) 138.4 2_656
C17 H10 O7 0.99 2.44 3.3993(17) 163.1 3_756
C17 H11 O1 0.99 2.39 3.3695(17) 170.2 3_757
C1 H1 O7 0.98 2.42 3.3486(18) 159.1 4_556
C19 H15 O1 0.99 2.53 3.3325(17) 138.4 2_656
C17 H10 O7 0.99 2.44 3.3993(17) 163.1 3_756
C17 H11 O1 0.99 2.39 3.3695(17) 170.2 3_757
C1 H1 O7 0.98 2.42 3.3486(18) 159.1 4_556
C19 H15 O1 0.99 2.53 3.3325(17) 138.4 2_656
C17 H10 O7 0.99 2.44 3.3993(17) 163.1 3_756
C17 H11 O1 0.99 2.39 3.3695(17) 170.2 3_757
C1 H1 O7 0.98 2.42 3.3486(18) 159.1 4_556
C19 H15 O1 0.99 2.53 3.3325(17) 138.4 2_656
C17 H10 O7 0.99 2.44 3.3993(17) 163.1 3_756
C17 H11 O1 0.99 2.39 3.3695(17) 170.2 3_757
C1 H1 O7 0.98 2.42 3.3486(18) 159.1 4_556
C19 H15 O1 0.99 2.53 3.3325(17) 138.4 2_656
C17 H10 O7 0.99 2.44 3.3993(17) 163.1 3_756
C17 H11 O1 0.99 2.39 3.3695(17) 170.2 3_757
C1 H1 O7 0.98 2.42 3.3486(18) 159.1 4_556
C1 H1 O7 0.98 2.42 3.3486(18) 159.1 4_556
C17 H11 O1 0.99 2.39 3.3695(17) 170.2 3_757
C17 H10 O7 0.99 2.44 3.3993(17) 163.1 3_756
C19 H15 O1 0.99 2.53 3.3325(17) 138.4 2_656
C1 H1 O7 0.98 2.42 3.3486(18) 159.1 4_556
C17 H11 O1 0.99 2.39 3.3695(17) 170.2 3_757
C17 H10 O7 0.99 2.44 3.3993(17) 163.1 3_756
C19 H15 O1 0.99 2.53 3.3325(17) 138.4 2_656
C1 H1 O7 0.98 2.42 3.3486(18) 159.1 4_556
C17 H11 O1 0.99 2.39 3.3695(17) 170.2 3_757
C17 H10 O7 0.99 2.44 3.3993(17) 163.1 3_756
C19 H15 O1 0.99 2.53 3.3325(17) 138.4 2_656
C1 H1 O7 0.98 2.42 3.3486(18) 159.1 4_556
C17 H11 O1 0.99 2.39 3.3695(17) 170.2 3_757
C17 H10 O7 0.99 2.44 3.3993(17) 163.1 3_756
C19 H15 O1 0.99 2.53 3.3325(17) 138.4 2_656

_refine_diff_density_max         0.544
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.064



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# 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_v40261_0m
_database_code_depnum_ccdc_archive 'CCDC 1888467'
loop_
_audit_author_name
_audit_author_address
'Li xiao nian'
;UCAS, KIB
China
;
_audit_update_record             
;
2019-01-03 deposited with the CCDC.	2020-07-23 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         'C22 H25 N O8'
_chemical_formula_sum            'C22 H25 N O8'
_chemical_formula_weight         431.43

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   18.9306(14)
_cell_length_b                   11.0428(8)
_cell_length_c                   21.1989(16)
_cell_angle_alpha                90
_cell_angle_beta                 114.6950(10)
_cell_angle_gamma                90
_cell_volume                     4026.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6817
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      29.99

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_F_000             1824
_exptl_transmission_factor_min   0.6715
_exptl_transmission_factor_max   0.7462
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.109
_shelx_estimated_absorpt_T_min   0.969
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44978
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.214
_diffrn_reflns_theta_max         31.214
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             12107
_reflns_number_gt                8143
_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 (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)+(0.0576P)²+0.6560P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12107
_refine_ls_number_parameters     569
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1259
_refine_ls_wR_factor_gt          0.1096
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.02857(7) 0.91503(11) -0.04834(6) 0.0280(3) Uani 1 1 d . . . . .
O2 O 0.17181(6) 0.54976(9) 0.08492(5) 0.0196(2) Uani 1 1 d . . . . .
O3 O 0.28648(7) 0.25045(9) 0.06226(6) 0.0196(2) Uani 1 1 d . . . . .
H3 H 0.2412(11) 0.2614(17) 0.0298(10) 0.029 Uiso 1 1 d . U . . .
O4 O 0.44988(6) 0.33115(10) 0.21806(5) 0.0179(2) Uani 1 1 d . . . . .
O5 O 0.36685(6) 0.56058(10) 0.03606(6) 0.0235(2) Uani 1 1 d . . . . .
O6 O 0.19592(6) 0.35479(10) 0.19888(5) 0.0193(2) Uani 1 1 d . . . . .
O7 O 0.20023(6) 0.54085(10) 0.24122(6) 0.0242(2) Uani 1 1 d . . . . .
O8 O 0.33233(6) 0.82693(10) 0.13699(6) 0.0235(2) Uani 1 1 d . . . . .
O9 O 0.04478(6) 0.41911(9) 0.46549(5) 0.0200(2) Uani 1 1 d . . . . .
O10 O 0.43811(6) 1.03168(10) 0.71450(5) 0.0173(2) Uani 1 1 d . . . . .
O11 O 0.17110(6) 0.79103(9) 0.58391(5) 0.0188(2) Uani 1 1 d . . . . .
O12 O 0.36131(6) 0.79878(10) 0.52553(5) 0.0218(2) Uani 1 1 d . . . . .
O13 O 0.27973(6) 1.09339(9) 0.55570(5) 0.0163(2) Uani 1 1 d . . . . .
H32 H 0.2364(11) 1.0822(17) 0.5229(10) 0.024 Uiso 1 1 d . U . . .
O14 O 0.18290(6) 0.99943(9) 0.69024(6) 0.0189(2) Uani 1 1 d . . . . .
O15 O 0.18941(7) 0.81636(10) 0.73661(6) 0.0270(3) Uani 1 1 d . . . . .
O16 O 0.34402(6) 0.53277(9) 0.65335(6) 0.0203(2) Uani 1 1 d . . . . .
N1 N 0.38531(7) 0.39045(11) 0.10301(6) 0.0143(2) Uani 1 1 d . . . . .
N2 N 0.37782(7) 0.95329(11) 0.60288(6) 0.0132(2) Uani 1 1 d . . . . .
C1 C 0.49682(10) 0.47976(17) 0.10453(10) 0.0339(4) Uani 1 1 d . . . . .
H1 H 0.5198 0.5511 0.1344 0.041 Uiso 1 1 calc R U . . .
H9 H 0.5141 0.4789 0.0664 0.041 Uiso 1 1 calc R U . . .
C2 C 0.40937(9) 0.48317(14) 0.07591(8) 0.0186(3) Uani 1 1 d . . . . .
C3 C 0.30704(8) 0.36479(12) 0.09513(7) 0.0135(3) Uani 1 1 d . . . . .
H13 H 0.2704 0.4285 0.0660 0.016 Uiso 1 1 calc R U . . .
C4 C 0.30539(8) 0.35854(12) 0.16736(7) 0.0134(3) Uani 1 1 d . . . . .
C5 C 0.29970(8) 0.48046(13) 0.20304(7) 0.0140(3) Uani 1 1 d . . . . .
C6 C 0.29773(8) 0.60225(13) 0.16769(7) 0.0152(3) Uani 1 1 d . . . . .
H16 H 0.3092 0.6675 0.2026 0.018 Uiso 1 1 calc R U . . .
H17 H 0.3394 0.6029 0.1510 0.018 Uiso 1 1 calc R U . . .
C7 C 0.22108(8) 0.62983(13) 0.10712(7) 0.0148(3) Uani 1 1 d . . . . .
C8 C 0.20352(9) 0.75418(13) 0.07667(7) 0.0153(3) Uani 1 1 d . . . . .
C9 C 0.12644(9) 0.77479(14) 0.02849(7) 0.0168(3) Uani 1 1 d . . . . .
H23 H 0.0903 0.7097 0.0154 0.020 Uiso 1 1 calc R U . . .
C10 C 0.10240(9) 0.88795(14) -0.00011(8) 0.0203(3) Uani 1 1 d . . . . .
C11 C -0.02842(10) 0.82301(18) -0.06348(10) 0.0369(5) Uani 1 1 d . . . . .
H24 H -0.0138 0.7533 -0.0841 0.055 Uiso 1 1 calc R U . . .
H2 H -0.0789 0.8542 -0.0963 0.055 Uiso 1 1 calc R U . . .
H25 H -0.0320 0.7979 -0.0206 0.055 Uiso 1 1 calc R U . . .
C12 C 0.44699(9) 0.31501(14) 0.15088(7) 0.0171(3) Uani 1 1 d . . . . .
H12 H 0.4382 0.2280 0.1366 0.021 Uiso 1 1 calc R U . . .
C13 C 0.37863(8) 0.29373(13) 0.22173(7) 0.0166(3) Uani 1 1 d . . . . .
H8 H 0.3726 0.2037 0.2187 0.020 Uiso 1 1 calc R U . . .
C14 C 0.38520(9) 0.34119(15) 0.29106(7) 0.0219(3) Uani 1 1 d . . . . .
H7 H 0.4380 0.3280 0.3280 0.026 Uiso 1 1 calc R U . . .
H6 H 0.3466 0.3023 0.3048 0.026 Uiso 1 1 calc R U . . .
C15 C 0.36809(9) 0.47598(14) 0.27637(7) 0.0199(3) Uani 1 1 d . . . . .
H5 H 0.4141 0.5191 0.2767 0.024 Uiso 1 1 calc R U . . .
H4 H 0.3529 0.5133 0.3114 0.024 Uiso 1 1 calc R U . . .
C16 C 0.52074(9) 0.36296(15) 0.14680(9) 0.0233(3) Uani 1 1 d . . . . .
H10 H 0.5615 0.3794 0.1939 0.028 Uiso 1 1 calc R U . . .
H11 H 0.5411 0.3034 0.1236 0.028 Uiso 1 1 calc R U . . .
C17 C 0.23028(8) 0.29067(13) 0.15879(7) 0.0164(3) Uani 1 1 d . . . . .
H14 H 0.1933 0.2883 0.1092 0.020 Uiso 1 1 calc R U . . .
H15 H 0.2428 0.2064 0.1757 0.020 Uiso 1 1 calc R U . . .
C18 C 0.22655(9) 0.46623(14) 0.21546(7) 0.0173(3) Uani 1 1 d . . . . .
C19 C 0.25677(9) 0.85069(13) 0.09399(8) 0.0182(3) Uani 1 1 d . . . . .
C20 C 0.38553(10) 0.92632(15) 0.16111(9) 0.0274(4) Uani 1 1 d . . . . .
H19 H 0.3904 0.9652 0.1215 0.041 Uiso 1 1 calc R U . . .
H20 H 0.4365 0.8965 0.1937 0.041 Uiso 1 1 calc R U . . .
H18 H 0.3661 0.9853 0.1846 0.041 Uiso 1 1 calc R U . . .
C21 C 0.23120(10) 0.96490(14) 0.06506(8) 0.0243(3) Uani 1 1 d . . . . .
H22 H 0.2667 1.0308 0.0776 0.029 Uiso 1 1 calc R U . . .
C22 C 0.15528(11) 0.98311(14) 0.01865(9) 0.0253(4) Uani 1 1 d . . . . .
H21 H 0.1389 1.0612 -0.0007 0.030 Uiso 1 1 calc R U . . .
C23 C 0.02445(9) 0.29636(13) 0.44440(8) 0.0210(3) Uani 1 1 d . . . . .
H28 H 0.0572 0.2660 0.4222 0.031 Uiso 1 1 calc R U . . .
H26 H -0.0303 0.2923 0.4114 0.031 Uiso 1 1 calc R U . . .
H50 H 0.0326 0.2466 0.4851 0.031 Uiso 1 1 calc R U . . .
C24 C 0.11973(8) 0.43916(13) 0.51367(7) 0.0157(3) Uani 1 1 d . . . . .
C25 C 0.13817(9) 0.55713(13) 0.53724(7) 0.0156(3) Uani 1 1 d . . . . .
H49 H 0.0993 0.6180 0.5200 0.019 Uiso 1 1 calc R U . . .
C26 C 0.21264(8) 0.58844(12) 0.58579(7) 0.0136(3) Uani 1 1 d . . . . .
C27 C 0.22325(8) 0.71690(13) 0.61111(7) 0.0140(3) Uani 1 1 d . . . . .
C28 C 0.29670(8) 0.75474(12) 0.67297(7) 0.0141(3) Uani 1 1 d . . . . .
H43 H 0.3404 0.7551 0.6589 0.017 Uiso 1 1 calc R U . . .
H42 H 0.3085 0.6935 0.7101 0.017 Uiso 1 1 calc R U . . .
C29 C 0.29192(8) 0.87945(12) 0.70263(7) 0.0129(3) Uani 1 1 d . . . . .
C30 C 0.29496(8) 0.99706(12) 0.66256(7) 0.0115(3) Uani 1 1 d . . . . .
C31 C 0.36546(8) 1.07016(13) 0.71474(7) 0.0138(3) Uani 1 1 d . . . . .
H35 H 0.3575 1.1594 0.7073 0.017 Uiso 1 1 calc R U . . .
C32 C 0.43790(8) 1.03487(13) 0.64800(7) 0.0162(3) Uani 1 1 d . . . . .
H34 H 0.4295 1.1191 0.6289 0.019 Uiso 1 1 calc R U . . .
C33 C 0.51274(9) 0.98115(15) 0.64964(9) 0.0234(3) Uani 1 1 d . . . . .
H29 H 0.5393 0.9308 0.6916 0.028 Uiso 1 1 calc R U . . .
H27 H 0.5487 1.0457 0.6489 0.028 Uiso 1 1 calc R U . . .
C34 C 0.40166(9) 0.87651(13) 0.56618(7) 0.0158(3) Uani 1 1 d . . . . .
C35 C 0.48575(9) 0.90388(15) 0.58383(8) 0.0217(3) Uani 1 1 d . . . . .
H30 H 0.4910 0.9490 0.5457 0.026 Uiso 1 1 calc R U . . .
H31 H 0.5165 0.8283 0.5925 0.026 Uiso 1 1 calc R U . . .
C36 C 0.29904(8) 0.98165(12) 0.59195(7) 0.0120(3) Uani 1 1 d . . . . .
H33 H 0.2627 0.9165 0.5642 0.014 Uiso 1 1 calc R U . . .
C37 C 0.37041(9) 1.03214(13) 0.78541(7) 0.0186(3) Uani 1 1 d . . . . .
H36 H 0.3292 1.0711 0.7955 0.022 Uiso 1 1 calc R U . . .
H37 H 0.4218 1.0521 0.8228 0.022 Uiso 1 1 calc R U . . .
C38 C 0.35833(9) 0.89503(13) 0.77684(7) 0.0186(3) Uani 1 1 d . . . . .
H38 H 0.3428 0.8615 0.8125 0.022 Uiso 1 1 calc R U . . .
H39 H 0.4064 0.8540 0.7806 0.022 Uiso 1 1 calc R U . . .
C39 C 0.21818(8) 1.06245(13) 0.65072(8) 0.0159(3) Uani 1 1 d . . . . .
H40 H 0.2288 1.1477 0.6663 0.019 Uiso 1 1 calc R U . . .
H41 H 0.1826 1.0618 0.6007 0.019 Uiso 1 1 calc R U . . .
C40 C 0.21639(9) 0.89007(13) 0.71105(7) 0.0176(3) Uani 1 1 d . . . . .
C41 C 0.27065(8) 0.49806(13) 0.60928(7) 0.0148(3) Uani 1 1 d . . . . .
C42 C 0.40402(9) 0.44319(14) 0.67745(8) 0.0193(3) Uani 1 1 d . . . . .
H44 H 0.3906 0.3809 0.7036 0.029 Uiso 1 1 calc R U . . .
H46 H 0.4533 0.4814 0.7077 0.029 Uiso 1 1 calc R U . . .
H45 H 0.4092 0.4059 0.6376 0.029 Uiso 1 1 calc R U . . .
C43 C 0.25152(9) 0.37989(13) 0.58573(7) 0.0162(3) Uani 1 1 d . . . . .
H47 H 0.2902 0.3186 0.6021 0.019 Uiso 1 1 calc R U . . .
C44 C 0.17660(9) 0.35010(13) 0.53853(7) 0.0174(3) Uani 1 1 d . . . . .
H48 H 0.1643 0.2688 0.5233 0.021 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
O1 C10 1.3763(19) . ?
O1 C11 1.418(2) . ?
O2 C7 1.2274(17) . ?
O3 C3 1.4159(17) . ?
O3 H3 0.85(2) . ?
O4 C12 1.4134(17) . ?
O4 C13 1.4434(17) . ?
O5 C2 1.2346(17) . ?
O6 C18 1.3431(18) . ?
O6 C17 1.4522(17) . ?
O7 C18 1.2052(18) . ?
O8 C19 1.3625(19) . ?
O8 C20 1.4319(18) . ?
O9 C24 1.3764(17) . ?
O9 C23 1.4289(17) . ?
O10 C32 1.4084(17) . ?
O10 C31 1.4415(17) . ?
O11 C27 1.2253(17) . ?
O12 C34 1.2300(18) . ?
O13 C36 1.4185(16) . ?
O13 H32 0.834(18) . ?
O14 C40 1.3495(18) . ?
O14 C39 1.4489(17) . ?
O15 C40 1.2035(17) . ?
O16 C41 1.3655(17) . ?
O16 C42 1.4299(17) . ?
N1 C2 1.3434(18) . ?
N1 C3 1.4479(18) . ?
N1 C12 1.4482(18) . ?
N2 C34 1.3495(17) . ?
N2 C36 1.4448(17) . ?
N2 C32 1.4529(18) . ?
C1 C2 1.507(2) . ?
C1 C16 1.527(2) . ?
C1 H1 0.9900 . ?
C1 H9 0.9900 . ?
C3 C4 1.5461(19) . ?
C3 H13 1.0000 . ?
C4 C17 1.5494(19) . ?
C4 C13 1.5581(19) . ?
C4 C5 1.5699(19) . ?
C5 C18 1.522(2) . ?
C5 C6 1.532(2) . ?
C5 C15 1.5534(19) . ?
C6 C7 1.513(2) . ?
C6 H16 0.9900 . ?
C6 H17 0.9900 . ?
C7 C8 1.494(2) . ?
C8 C19 1.406(2) . ?
C8 C9 1.407(2) . ?
C9 C10 1.380(2) . ?
C9 H23 0.9500 . ?
C10 C22 1.390(2) . ?
C11 H24 0.9800 . ?
C11 H2 0.9800 . ?
C11 H25 0.9800 . ?
C12 C16 1.529(2) . ?
C12 H12 1.0000 . ?
C13 C14 1.516(2) . ?
C13 H8 1.0000 . ?
C14 C15 1.528(2) . ?
C14 H7 0.9900 . ?
C14 H6 0.9900 . ?
C15 H5 0.9900 . ?
C15 H4 0.9900 . ?
C16 H10 0.9900 . ?
C16 H11 0.9900 . ?
C17 H14 0.9900 . ?
C17 H15 0.9900 . ?
C19 C21 1.397(2) . ?
C20 H19 0.9800 . ?
C20 H20 0.9800 . ?
C20 H18 0.9800 . ?
C21 C22 1.376(2) . ?
C21 H22 0.9500 . ?
C22 H21 0.9500 . ?
C23 H28 0.9800 . ?
C23 H26 0.9800 . ?
C23 H50 0.9800 . ?
C24 C25 1.387(2) . ?
C24 C44 1.389(2) . ?
C25 C26 1.398(2) . ?
C25 H49 0.9500 . ?
C26 C41 1.412(2) . ?
C26 C27 1.5002(19) . ?
C27 C28 1.518(2) . ?
C28 C29 1.5321(19) . ?
C28 H43 0.9900 . ?
C28 H42 0.9900 . ?
C29 C40 1.518(2) . ?
C29 C38 1.5596(19) . ?
C29 C30 1.5661(19) . ?
C30 C36 1.5401(18) . ?
C30 C39 1.5468(19) . ?
C30 C31 1.5565(19) . ?
C31 C37 1.5206(19) . ?
C31 H35 1.0000 . ?
C32 C33 1.523(2) . ?
C32 H34 1.0000 . ?
C33 C35 1.530(2) . ?
C33 H29 0.9900 . ?
C33 H27 0.9900 . ?
C34 C35 1.506(2) . ?
C35 H30 0.9900 . ?
C35 H31 0.9900 . ?
C36 H33 1.0000 . ?
C37 C38 1.531(2) . ?
C37 H36 0.9900 . ?
C37 H37 0.9900 . ?
C38 H38 0.9900 . ?
C38 H39 0.9900 . ?
C39 H40 0.9900 . ?
C39 H41 0.9900 . ?
C41 C43 1.390(2) . ?
C42 H44 0.9800 . ?
C42 H46 0.9800 . ?
C42 H45 0.9800 . ?
C43 C44 1.391(2) . ?
C43 H47 0.9500 . ?
C44 H48 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 O1 C11 116.93(12) . . ?
C3 O3 H3 104.3(13) . . ?
C12 O4 C13 111.99(11) . . ?
C18 O6 C17 110.49(11) . . ?
C19 O8 C20 118.46(13) . . ?
C24 O9 C23 116.37(12) . . ?
C32 O10 C31 113.10(10) . . ?
C36 O13 H32 105.3(13) . . ?
C40 O14 C39 110.59(11) . . ?
C41 O16 C42 118.64(11) . . ?
C2 N1 C3 127.83(12) . . ?
C2 N1 C12 114.83(12) . . ?
C3 N1 C12 117.06(11) . . ?
C34 N2 C36 127.96(12) . . ?
C34 N2 C32 114.26(12) . . ?
C36 N2 C32 116.29(11) . . ?
C2 C1 C16 105.30(13) . . ?
C2 C1 H1 110.7 . . ?
C16 C1 H1 110.7 . . ?
C2 C1 H9 110.7 . . ?
C16 C1 H9 110.7 . . ?
H1 C1 H9 108.8 . . ?
O5 C2 N1 125.43(14) . . ?
O5 C2 C1 125.83(14) . . ?
N1 C2 C1 108.70(13) . . ?
O3 C3 N1 106.80(11) . . ?
O3 C3 C4 109.42(11) . . ?
N1 C3 C4 109.73(11) . . ?
O3 C3 H13 110.3 . . ?
N1 C3 H13 110.3 . . ?
C4 C3 H13 110.3 . . ?
C3 C4 C17 107.62(11) . . ?
C3 C4 C13 111.91(11) . . ?
C17 C4 C13 110.74(11) . . ?
C3 C4 C5 118.21(11) . . ?
C17 C4 C5 103.12(11) . . ?
C13 C4 C5 104.87(11) . . ?
C18 C5 C6 109.70(12) . . ?
C18 C5 C15 105.18(11) . . ?
C6 C5 C15 110.92(12) . . ?
C18 C5 C4 104.20(11) . . ?
C6 C5 C4 120.64(11) . . ?
C15 C5 C4 104.98(11) . . ?
C7 C6 C5 114.23(12) . . ?
C7 C6 H16 108.7 . . ?
C5 C6 H16 108.7 . . ?
C7 C6 H17 108.7 . . ?
C5 C6 H17 108.7 . . ?
H16 C6 H17 107.6 . . ?
O2 C7 C8 120.01(13) . . ?
O2 C7 C6 119.08(13) . . ?
C8 C7 C6 120.85(12) . . ?
C19 C8 C9 118.68(13) . . ?
C19 C8 C7 125.30(13) . . ?
C9 C8 C7 115.99(13) . . ?
C10 C9 C8 121.12(14) . . ?
C10 C9 H23 119.4 . . ?
C8 C9 H23 119.4 . . ?
O1 C10 C9 124.69(15) . . ?
O1 C10 C22 115.76(14) . . ?
C9 C10 C22 119.53(15) . . ?
O1 C11 H24 109.5 . . ?
O1 C11 H2 109.5 . . ?
H24 C11 H2 109.5 . . ?
O1 C11 H25 109.5 . . ?
H24 C11 H25 109.5 . . ?
H2 C11 H25 109.5 . . ?
O4 C12 N1 108.30(11) . . ?
O4 C12 C16 111.19(13) . . ?
N1 C12 C16 104.43(11) . . ?
O4 C12 H12 110.9 . . ?
N1 C12 H12 110.9 . . ?
C16 C12 H12 110.9 . . ?
O4 C13 C14 104.67(12) . . ?
O4 C13 C4 113.04(11) . . ?
C14 C13 C4 104.21(12) . . ?
O4 C13 H8 111.5 . . ?
C14 C13 H8 111.5 . . ?
C4 C13 H8 111.5 . . ?
C13 C14 C15 102.40(12) . . ?
C13 C14 H7 111.3 . . ?
C15 C14 H7 111.3 . . ?
C13 C14 H6 111.3 . . ?
C15 C14 H6 111.3 . . ?
H7 C14 H6 109.2 . . ?
C14 C15 C5 104.61(12) . . ?
C14 C15 H5 110.8 . . ?
C5 C15 H5 110.8 . . ?
C14 C15 H4 110.8 . . ?
C5 C15 H4 110.8 . . ?
H5 C15 H4 108.9 . . ?
C1 C16 C12 105.77(12) . . ?
C1 C16 H10 110.6 . . ?
C12 C16 H10 110.6 . . ?
C1 C16 H11 110.6 . . ?
C12 C16 H11 110.6 . . ?
H10 C16 H11 108.7 . . ?
O6 C17 C4 108.00(11) . . ?
O6 C17 H14 110.1 . . ?
C4 C17 H14 110.1 . . ?
O6 C17 H15 110.1 . . ?
C4 C17 H15 110.1 . . ?
H14 C17 H15 108.4 . . ?
O7 C18 O6 122.01(14) . . ?
O7 C18 C5 125.87(14) . . ?
O6 C18 C5 111.95(12) . . ?
O8 C19 C21 122.80(14) . . ?
O8 C19 C8 117.80(13) . . ?
C21 C19 C8 119.36(14) . . ?
O8 C20 H19 109.5 . . ?
O8 C20 H20 109.5 . . ?
H19 C20 H20 109.5 . . ?
O8 C20 H18 109.5 . . ?
H19 C20 H18 109.5 . . ?
H20 C20 H18 109.5 . . ?
C22 C21 C19 120.84(15) . . ?
C22 C21 H22 119.6 . . ?
C19 C21 H22 119.6 . . ?
C21 C22 C10 120.42(15) . . ?
C21 C22 H21 119.8 . . ?
C10 C22 H21 119.8 . . ?
O9 C23 H28 109.5 . . ?
O9 C23 H26 109.5 . . ?
H28 C23 H26 109.5 . . ?
O9 C23 H50 109.5 . . ?
H28 C23 H50 109.5 . . ?
H26 C23 H50 109.5 . . ?
O9 C24 C25 116.40(13) . . ?
O9 C24 C44 124.26(13) . . ?
C25 C24 C44 119.33(14) . . ?
C24 C25 C26 121.48(13) . . ?
C24 C25 H49 119.3 . . ?
C26 C25 H49 119.3 . . ?
C25 C26 C41 118.78(13) . . ?
C25 C26 C27 116.13(13) . . ?
C41 C26 C27 125.04(13) . . ?
O11 C27 C26 120.15(13) . . ?
O11 C27 C28 119.32(12) . . ?
C26 C27 C28 120.45(12) . . ?
C27 C28 C29 114.33(12) . . ?
C27 C28 H43 108.7 . . ?
C29 C28 H43 108.7 . . ?
C27 C28 H42 108.7 . . ?
C29 C28 H42 108.7 . . ?
H43 C28 H42 107.6 . . ?
C40 C29 C28 109.75(12) . . ?
C40 C29 C38 105.96(11) . . ?
C28 C29 C38 110.61(11) . . ?
C40 C29 C30 104.46(11) . . ?
C28 C29 C30 120.07(11) . . ?
C38 C29 C30 105.00(11) . . ?
C36 C30 C39 108.62(11) . . ?
C36 C30 C31 111.82(11) . . ?
C39 C30 C31 109.99(11) . . ?
C36 C30 C29 117.62(11) . . ?
C39 C30 C29 103.30(11) . . ?
C31 C30 C29 105.04(11) . . ?
O10 C31 C37 104.83(11) . . ?
O10 C31 C30 112.38(11) . . ?
C37 C31 C30 103.80(11) . . ?
O10 C31 H35 111.8 . . ?
C37 C31 H35 111.8 . . ?
C30 C31 H35 111.8 . . ?
O10 C32 N2 108.51(11) . . ?
O10 C32 C33 110.72(12) . . ?
N2 C32 C33 103.79(12) . . ?
O10 C32 H34 111.2 . . ?
N2 C32 H34 111.2 . . ?
C33 C32 H34 111.2 . . ?
C32 C33 C35 104.08(12) . . ?
C32 C33 H29 110.9 . . ?
C35 C33 H29 110.9 . . ?
C32 C33 H27 110.9 . . ?
C35 C33 H27 110.9 . . ?
H29 C33 H27 109.0 . . ?
O12 C34 N2 125.66(14) . . ?
O12 C34 C35 126.64(13) . . ?
N2 C34 C35 107.70(13) . . ?
C34 C35 C33 104.73(12) . . ?
C34 C35 H30 110.8 . . ?
C33 C35 H30 110.8 . . ?
C34 C35 H31 110.8 . . ?
C33 C35 H31 110.8 . . ?
H30 C35 H31 108.9 . . ?
O13 C36 N2 106.88(11) . . ?
O13 C36 C30 108.92(11) . . ?
N2 C36 C30 109.61(11) . . ?
O13 C36 H33 110.4 . . ?
N2 C36 H33 110.4 . . ?
C30 C36 H33 110.4 . . ?
C31 C37 C38 102.21(11) . . ?
C31 C37 H36 111.3 . . ?
C38 C37 H36 111.3 . . ?
C31 C37 H37 111.3 . . ?
C38 C37 H37 111.3 . . ?
H36 C37 H37 109.2 . . ?
C37 C38 C29 104.26(11) . . ?
C37 C38 H38 110.9 . . ?
C29 C38 H38 110.9 . . ?
C37 C38 H39 110.9 . . ?
C29 C38 H39 110.9 . . ?
H38 C38 H39 108.9 . . ?
O14 C39 C30 108.11(11) . . ?
O14 C39 H40 110.1 . . ?
C30 C39 H40 110.1 . . ?
O14 C39 H41 110.1 . . ?
C30 C39 H41 110.1 . . ?
H40 C39 H41 108.4 . . ?
O15 C40 O14 121.50(14) . . ?
O15 C40 C29 126.77(14) . . ?
O14 C40 C29 111.58(12) . . ?
O16 C41 C43 123.17(13) . . ?
O16 C41 C26 117.51(12) . . ?
C43 C41 C26 119.30(13) . . ?
O16 C42 H44 109.5 . . ?
O16 C42 H46 109.5 . . ?
H44 C42 H46 109.5 . . ?
O16 C42 H45 109.5 . . ?
H44 C42 H45 109.5 . . ?
H46 C42 H45 109.5 . . ?
C41 C43 C44 120.98(13) . . ?
C41 C43 H47 119.5 . . ?
C44 C43 H47 119.5 . . ?
C24 C44 C43 120.08(13) . . ?
C24 C44 H48 120.0 . . ?
C43 C44 H48 120.0 . . ?

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
C3 N1 C2 O5 -3.7(2) . . . . ?
C12 N1 C2 O5 -177.38(14) . . . . ?
C3 N1 C2 C1 173.95(14) . . . . ?
C12 N1 C2 C1 0.31(18) . . . . ?
C16 C1 C2 O5 -176.41(16) . . . . ?
C16 C1 C2 N1 5.91(19) . . . . ?
C2 N1 C3 O3 118.83(15) . . . . ?
C12 N1 C3 O3 -67.65(15) . . . . ?
C2 N1 C3 C4 -122.67(15) . . . . ?
C12 N1 C3 C4 50.85(16) . . . . ?
O3 C3 C4 C17 -44.61(15) . . . . ?
N1 C3 C4 C17 -161.48(11) . . . . ?
O3 C3 C4 C13 77.26(14) . . . . ?
N1 C3 C4 C13 -39.60(15) . . . . ?
O3 C3 C4 C5 -160.76(12) . . . . ?
N1 C3 C4 C5 82.37(15) . . . . ?
C3 C4 C5 C18 122.28(13) . . . . ?
C17 C4 C5 C18 3.74(13) . . . . ?
C13 C4 C5 C18 -112.23(12) . . . . ?
C3 C4 C5 C6 -1.37(19) . . . . ?
C17 C4 C5 C6 -119.91(13) . . . . ?
C13 C4 C5 C6 124.11(13) . . . . ?
C3 C4 C5 C15 -127.40(13) . . . . ?
C17 C4 C5 C15 114.07(12) . . . . ?
C13 C4 C5 C15 -1.91(14) . . . . ?
C18 C5 C6 C7 -46.59(15) . . . . ?
C15 C5 C6 C7 -162.35(12) . . . . ?
C4 C5 C6 C7 74.41(16) . . . . ?
C5 C6 C7 O2 -10.01(19) . . . . ?
C5 C6 C7 C8 166.97(12) . . . . ?
O2 C7 C8 C19 -175.04(14) . . . . ?
C6 C7 C8 C19 8.0(2) . . . . ?
O2 C7 C8 C9 6.99(19) . . . . ?
C6 C7 C8 C9 -169.97(13) . . . . ?
C19 C8 C9 C10 -1.7(2) . . . . ?
C7 C8 C9 C10 176.39(13) . . . . ?
C11 O1 C10 C9 7.3(2) . . . . ?
C11 O1 C10 C22 -174.13(15) . . . . ?
C8 C9 C10 O1 178.84(13) . . . . ?
C8 C9 C10 C22 0.3(2) . . . . ?
C13 O4 C12 N1 62.02(14) . . . . ?
C13 O4 C12 C16 176.19(11) . . . . ?
C2 N1 C12 O4 112.21(14) . . . . ?
C3 N1 C12 O4 -62.16(16) . . . . ?
C2 N1 C12 C16 -6.36(17) . . . . ?
C3 N1 C12 C16 179.28(12) . . . . ?
C12 O4 C13 C14 -168.40(11) . . . . ?
C12 O4 C13 C4 -55.63(15) . . . . ?
C3 C4 C13 O4 43.61(16) . . . . ?
C17 C4 C13 O4 163.68(11) . . . . ?
C5 C4 C13 O4 -85.73(14) . . . . ?
C3 C4 C13 C14 156.67(12) . . . . ?
C17 C4 C13 C14 -83.26(14) . . . . ?
C5 C4 C13 C14 27.33(14) . . . . ?
O4 C13 C14 C15 76.47(13) . . . . ?
C4 C13 C14 C15 -42.46(14) . . . . ?
C13 C14 C15 C5 41.32(15) . . . . ?
C18 C5 C15 C14 85.64(14) . . . . ?
C6 C5 C15 C14 -155.83(12) . . . . ?
C4 C5 C15 C14 -23.99(15) . . . . ?
C2 C1 C16 C12 -9.42(19) . . . . ?
O4 C12 C16 C1 -107.09(15) . . . . ?
N1 C12 C16 C1 9.49(17) . . . . ?
C18 O6 C17 C4 15.92(15) . . . . ?
C3 C4 C17 O6 -137.07(11) . . . . ?
C13 C4 C17 O6 100.33(13) . . . . ?
C5 C4 C17 O6 -11.38(14) . . . . ?
C17 O6 C18 O7 170.76(13) . . . . ?
C17 O6 C18 C5 -13.68(16) . . . . ?
C6 C5 C18 O7 -48.43(19) . . . . ?
C15 C5 C18 O7 70.93(18) . . . . ?
C4 C5 C18 O7 -178.89(14) . . . . ?
C6 C5 C18 O6 136.22(12) . . . . ?
C15 C5 C18 O6 -104.43(13) . . . . ?
C4 C5 C18 O6 5.75(15) . . . . ?
C20 O8 C19 C21 8.8(2) . . . . ?
C20 O8 C19 C8 -173.36(13) . . . . ?
C9 C8 C19 O8 -175.54(13) . . . . ?
C7 C8 C19 O8 6.5(2) . . . . ?
C9 C8 C19 C21 2.3(2) . . . . ?
C7 C8 C19 C21 -175.57(14) . . . . ?
O8 C19 C21 C22 176.11(14) . . . . ?
C8 C19 C21 C22 -1.7(2) . . . . ?
C19 C21 C22 C10 0.3(2) . . . . ?
O1 C10 C22 C21 -178.23(14) . . . . ?
C9 C10 C22 C21 0.4(2) . . . . ?
C23 O9 C24 C25 -176.31(13) . . . . ?
C23 O9 C24 C44 4.6(2) . . . . ?
O9 C24 C25 C26 -179.53(12) . . . . ?
C44 C24 C25 C26 -0.4(2) . . . . ?
C24 C25 C26 C41 2.1(2) . . . . ?
C24 C25 C26 C27 -175.39(13) . . . . ?
C25 C26 C27 O11 -7.98(19) . . . . ?
C41 C26 C27 O11 174.65(13) . . . . ?
C25 C26 C27 C28 168.74(12) . . . . ?
C41 C26 C27 C28 -8.6(2) . . . . ?
O11 C27 C28 C29 9.59(18) . . . . ?
C26 C27 C28 C29 -167.15(12) . . . . ?
C27 C28 C29 C40 47.06(15) . . . . ?
C27 C28 C29 C38 163.61(12) . . . . ?
C27 C28 C29 C30 -73.89(16) . . . . ?
C40 C29 C30 C36 -120.80(13) . . . . ?
C28 C29 C30 C36 2.73(18) . . . . ?
C38 C29 C30 C36 127.91(12) . . . . ?
C40 C29 C30 C39 -1.20(13) . . . . ?
C28 C29 C30 C39 122.33(13) . . . . ?
C38 C29 C30 C39 -112.48(12) . . . . ?
C40 C29 C30 C31 114.10(12) . . . . ?
C28 C29 C30 C31 -122.37(13) . . . . ?
C38 C29 C30 C31 2.81(14) . . . . ?
C32 O10 C31 C37 166.84(11) . . . . ?
C32 O10 C31 C30 54.76(15) . . . . ?
C36 C30 C31 O10 -44.45(15) . . . . ?
C39 C30 C31 O10 -165.22(11) . . . . ?
C29 C30 C31 O10 84.22(13) . . . . ?
C36 C30 C31 C37 -157.16(11) . . . . ?
C39 C30 C31 C37 82.07(13) . . . . ?
C29 C30 C31 C37 -28.50(14) . . . . ?
C31 O10 C32 N2 -60.83(15) . . . . ?
C31 O10 C32 C33 -174.12(12) . . . . ?
C34 N2 C32 O10 -131.16(12) . . . . ?
C36 N2 C32 O10 61.66(15) . . . . ?
C34 N2 C32 C33 -13.37(16) . . . . ?
C36 N2 C32 C33 179.45(12) . . . . ?
O10 C32 C33 C35 137.88(13) . . . . ?
N2 C32 C33 C35 21.63(15) . . . . ?
C36 N2 C34 O12 -15.6(2) . . . . ?
C32 N2 C34 O12 179.04(13) . . . . ?
C36 N2 C34 C35 164.16(13) . . . . ?
C32 N2 C34 C35 -1.22(16) . . . . ?
O12 C34 C35 C33 -164.99(14) . . . . ?
N2 C34 C35 C33 15.27(16) . . . . ?
C32 C33 C35 C34 -22.58(16) . . . . ?
C34 N2 C36 O13 -99.78(15) . . . . ?
C32 N2 C36 O13 65.36(14) . . . . ?
C34 N2 C36 C30 142.33(13) . . . . ?
C32 N2 C36 C30 -52.54(15) . . . . ?
C39 C30 C36 O13 47.17(14) . . . . ?
C31 C30 C36 O13 -74.39(14) . . . . ?
C29 C30 C36 O13 163.94(11) . . . . ?
C39 C30 C36 N2 163.79(11) . . . . ?
C31 C30 C36 N2 42.23(15) . . . . ?
C29 C30 C36 N2 -79.44(15) . . . . ?
O10 C31 C37 C38 -74.61(13) . . . . ?
C30 C31 C37 C38 43.46(14) . . . . ?
C31 C37 C38 C29 -41.70(14) . . . . ?
C40 C29 C38 C37 -86.50(13) . . . . ?
C28 C29 C38 C37 154.62(12) . . . . ?
C30 C29 C38 C37 23.70(14) . . . . ?
C40 O14 C39 C30 -14.49(15) . . . . ?
C36 C30 C39 O14 134.55(11) . . . . ?
C31 C30 C39 O14 -102.77(13) . . . . ?
C29 C30 C39 O14 8.93(14) . . . . ?
C39 O14 C40 O15 -170.09(14) . . . . ?
C39 O14 C40 C29 14.00(16) . . . . ?
C28 C29 C40 O15 46.8(2) . . . . ?
C38 C29 C40 O15 -72.68(18) . . . . ?
C30 C29 C40 O15 176.73(15) . . . . ?
C28 C29 C40 O14 -137.59(12) . . . . ?
C38 C29 C40 O14 102.96(13) . . . . ?
C30 C29 C40 O14 -7.63(15) . . . . ?
C42 O16 C41 C43 -1.0(2) . . . . ?
C42 O16 C41 C26 -179.48(12) . . . . ?
C25 C26 C41 O16 175.99(12) . . . . ?
C27 C26 C41 O16 -6.7(2) . . . . ?
C25 C26 C41 C43 -2.5(2) . . . . ?
C27 C26 C41 C43 174.78(13) . . . . ?
O16 C41 C43 C44 -177.24(13) . . . . ?
C26 C41 C43 C44 1.2(2) . . . . ?
O9 C24 C44 C43 178.05(13) . . . . ?
C25 C24 C44 C43 -1.0(2) . . . . ?
C41 C43 C44 C24 0.6(2) . . . . ?

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
C44 H48 O5 0.95 2.57 3.5089(18) 170.6 2_545
C43 H47 O13 0.95 2.65 3.3142(18) 127.3 1_545
C42 H45 O1 0.98 2.62 3.4835(19) 147.5 2_545
C42 H44 O15 0.98 2.45 3.3317(19) 149.0 2_546
C39 H41 O5 0.99 2.65 3.5979(18) 160.5 2
C36 H33 O11 1.00 2.39 3.1591(17) 133.4 .
C31 H35 O15 1.00 2.47 3.2295(18) 132.6 2_556
C23 H28 O5 0.98 2.63 3.2361(19) 120.0 2_545
C21 H22 O3 0.95 2.50 3.3308(19) 146.6 1_565
C20 H18 O7 0.98 2.46 3.366(2) 152.8 2
C20 H20 O10 0.98 2.49 3.310(2) 141.4 3_676
C20 H19 O9 0.98 2.66 3.451(2) 138.2 2
C17 H15 O7 0.99 2.45 3.3919(19) 158.1 2_545
C17 H14 O12 0.99 2.60 3.5526(18) 160.8 2_545
C13 H8 O7 1.00 2.61 3.4095(18) 136.5 2_545
C3 H13 O2 1.00 2.46 3.2109(18) 131.3 .
O13 H32 O5 0.834(18) 1.844(18) 2.6655(15) 168.4(18) 2
O3 H3 O12 0.85(2) 1.85(2) 2.6879(16) 167.9(18) 2_545
C44 H48 O5 0.95 2.57 3.5089(18) 170.6 2_545
C43 H47 O13 0.95 2.65 3.3142(18) 127.3 1_545
C42 H45 O1 0.98 2.62 3.4835(19) 147.5 2_545
C42 H44 O15 0.98 2.45 3.3317(19) 149.0 2_546
C39 H41 O5 0.99 2.65 3.5979(18) 160.5 2
C36 H33 O11 1.00 2.39 3.1591(17) 133.4 .
C31 H35 O15 1.00 2.47 3.2295(18) 132.6 2_556
C23 H28 O5 0.98 2.63 3.2361(19) 120.0 2_545
C21 H22 O3 0.95 2.50 3.3308(19) 146.6 1_565
C20 H18 O7 0.98 2.46 3.366(2) 152.8 2
C20 H20 O10 0.98 2.49 3.310(2) 141.4 3_676
C17 H15 O7 0.99 2.45 3.3919(19) 158.1 2_545
C17 H14 O12 0.99 2.60 3.5526(18) 160.8 2_545
C13 H8 O7 1.00 2.61 3.4095(18) 136.5 2_545
C3 H13 O2 1.00 2.46 3.2109(18) 131.3 .
O13 H32 O5 0.834(18) 1.844(18) 2.6655(15) 168.4(18) 2
O3 H3 O12 0.85(2) 1.85(2) 2.6879(16) 167.9(18) 2_545
O3 H3 O12 0.85(2) 1.85(2) 2.6879(16) 167.9(18) 2_545
O13 H32 O5 0.834(18) 1.844(18) 2.6655(15) 168.4(18) 2
C3 H13 O2 1.00 2.46 3.2109(18) 131.3 .
C13 H8 O7 1.00 2.61 3.4095(18) 136.5 2_545
C17 H14 O12 0.99 2.60 3.5526(18) 160.8 2_545
C17 H15 O7 0.99 2.45 3.3919(19) 158.1 2_545
C20 H20 O10 0.98 2.49 3.310(2) 141.4 3_676
C20 H18 O7 0.98 2.46 3.366(2) 152.8 2
C21 H22 O3 0.95 2.50 3.3308(19) 146.6 1_565
C23 H28 O5 0.98 2.63 3.2361(19) 120.0 2_545
C31 H35 O15 1.00 2.47 3.2295(18) 132.6 2_556
C36 H33 O11 1.00 2.39 3.1591(17) 133.4 .
C39 H41 O5 0.99 2.65 3.5979(18) 160.5 2
C42 H44 O15 0.98 2.45 3.3317(19) 149.0 2_546
C42 H45 O1 0.98 2.62 3.4835(19) 147.5 2_545
C43 H47 O13 0.95 2.65 3.3142(18) 127.3 1_545
C44 H48 O5 0.95 2.57 3.5089(18) 170.6 2_545

_refine_diff_density_max         0.416
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.058



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
