# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_lyk_0m
_database_code_depnum_ccdc_archive 'CCDC 1506248'
_audit_update_record             
;
2016-09-26 deposited with the CCDC.
2018-08-20 downloaded from the CCDC.
;
_audit_creation_date             2016-09-19
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H24 F N O5'
_chemical_formula_sum            'C22 H24 F N O5'
_chemical_formula_weight         401.42
_chemical_absolute_configuration .
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.530(3)
_cell_length_b                   5.649(2)
_cell_length_c                   23.594(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.387(6)
_cell_angle_gamma                90
_cell_volume                     997.4(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7783
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.413
_cell_measurement_theta_min      2.606
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3586
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         0.868
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                3463
_reflns_number_total             3586
_reflns_special_details          
;
 _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 v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 
;
 Flack x determined using 1282 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3586
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0768
_refine_ls_restrained_S_all      1.196
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+3.4865P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2068
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.662(5) 0.338(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C9(H9), C11(H11), C13(H13), C14(H14)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B), C15(H15A,H15B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C18(H18), C19(H19), C20(H20), C21(H21),
 C22(H22)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
F1 F 1.3812(7) -0.1098(11) 1.0218(2) 0.0378(14) Uani 1 1 d . . . . .
O1 O 0.7990(9) -0.2837(11) 0.8152(3) 0.0363(17) Uani 1 1 d . . . . .
O2 O 0.3758(9) 0.2457(15) 0.8680(3) 0.0430(18) Uani 1 1 d . . . . .
O3 O 0.1673(8) 0.2070(15) 0.7985(3) 0.0427(19) Uani 1 1 d . . . . .
O4 O 0.4531(7) 0.2332(10) 0.6476(2) 0.0166(11) Uani 1 1 d . . . . .
O5 O 0.3178(8) 0.5521(10) 0.6894(2) 0.0186(12) Uani 1 1 d . . . . .
N1 N 0.3118(9) 0.1566(13) 0.8230(3) 0.0260(17) Uani 1 1 d . . . . .
C1 C 1.2507(11) -0.1028(17) 0.9771(4) 0.027(2) Uani 1 1 d . . . . .
C2 C 1.1363(11) 0.0864(16) 0.9735(3) 0.0232(18) Uani 1 1 d . . . . .
H2 H 1.1484 0.2091 1.0012 0.028 Uiso 1 1 calc R . . . .
C3 C 1.0016(12) 0.0936(16) 0.9280(3) 0.0229(18) Uani 1 1 d . . . . .
H3 H 0.9239 0.2264 0.9233 0.027 Uiso 1 1 calc R . . . .
C4 C 0.9806(11) -0.0929(15) 0.8893(3) 0.0172(16) Uani 1 1 d . . . . .
C5 C 1.1021(10) -0.2815(16) 0.8945(3) 0.0207(17) Uani 1 1 d . . . . .
H5 H 1.0899 -0.4066 0.8675 0.025 Uiso 1 1 calc R . . . .
C6 C 1.2408(12) -0.2877(16) 0.9390(4) 0.0261(19) Uani 1 1 d . . . . .
H6 H 1.3246 -0.4139 0.9427 0.031 Uiso 1 1 calc R . . . .
C7 C 0.8335(11) -0.0998(15) 0.8405(3) 0.0199(17) Uani 1 1 d . . . . .
C8 C 0.7405(10) 0.1276(14) 0.8233(3) 0.0170(16) Uani 1 1 d . . . . .
H8A H 0.8289 0.2411 0.8111 0.020 Uiso 1 1 calc R . . . .
H8B H 0.6908 0.1960 0.8568 0.020 Uiso 1 1 calc R . . . .
C9 C 0.5868(10) 0.0956(14) 0.7740(3) 0.0159(16) Uani 1 1 d . . . . .
H9 H 0.6318 -0.0158 0.7460 0.019 Uiso 1 1 calc R . . . .
C10 C 0.4238(11) -0.0207(14) 0.7950(3) 0.0207(17) Uani 1 1 d . . . . .
H10A H 0.3505 -0.0953 0.7624 0.025 Uiso 1 1 calc R . . . .
H10B H 0.4634 -0.1468 0.8228 0.025 Uiso 1 1 calc R . . . .
C11 C 0.5472(10) 0.3311(14) 0.7427(3) 0.0165(16) Uani 1 1 d . . . . .
H11 H 0.5287 0.4584 0.7709 0.020 Uiso 1 1 calc R . . . .
C12 C 0.6932(10) 0.4054(16) 0.7066(3) 0.0198(17) Uani 1 1 d . . . . .
H12A H 0.8118 0.3511 0.7241 0.024 Uiso 1 1 calc R . . . .
H12B H 0.6958 0.5796 0.7023 0.024 Uiso 1 1 calc R . . . .
C13 C 0.6426(11) 0.2847(14) 0.6490(3) 0.0203(18) Uani 1 1 d . . . . .
H13 H 0.7089 0.1315 0.6487 0.024 Uiso 1 1 calc R . . . .
C14 C 0.3855(10) 0.3203(14) 0.6971(3) 0.0156(16) Uani 1 1 d . . . . .
H14 H 0.2920 0.2115 0.7092 0.019 Uiso 1 1 calc R . . . .
C15 C 0.1578(11) 0.5577(16) 0.6499(4) 0.0238(19) Uani 1 1 d . . . . .
H15A H 0.0699 0.4427 0.6618 0.029 Uiso 1 1 calc R . . . .
H15B H 0.1859 0.5136 0.6113 0.029 Uiso 1 1 calc R . . . .
C16 C 0.0814(11) 0.8016(16) 0.6491(4) 0.028(2) Uani 1 1 d . . . . .
H16A H -0.0166 0.8140 0.6182 0.041 Uiso 1 1 calc GR . . . .
H16B H 0.1746 0.9168 0.6428 0.041 Uiso 1 1 calc GR . . . .
H16C H 0.0359 0.8343 0.6856 0.041 Uiso 1 1 calc GR . . . .
C17 C 0.6770(10) 0.4236(15) 0.5975(3) 0.0173(16) Uani 1 1 d . . . . .
C18 C 0.5919(11) 0.6402(14) 0.5853(3) 0.0202(17) Uani 1 1 d . . . . .
H18 H 0.5121 0.7007 0.6102 0.024 Uiso 1 1 calc R . . . .
C19 C 0.6227(11) 0.7680(16) 0.5372(4) 0.0256(19) Uani 1 1 d . . . . .
H19 H 0.5616 0.9132 0.5290 0.031 Uiso 1 1 calc R . . . .
C20 C 0.7410(12) 0.6864(17) 0.5013(4) 0.028(2) Uani 1 1 d . . . . .
H20 H 0.7631 0.7760 0.4687 0.033 Uiso 1 1 calc R . . . .
C21 C 0.8276(12) 0.4731(17) 0.5129(4) 0.026(2) Uani 1 1 d . . . . .
H21 H 0.9081 0.4153 0.4878 0.031 Uiso 1 1 calc R . . . .
C22 C 0.7979(10) 0.3431(15) 0.5605(3) 0.0208(18) Uani 1 1 d . . . . .
H22 H 0.8599 0.1983 0.5684 0.025 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C1 1.359(9) . ?
O1 C7 1.211(10) . ?
O2 N1 1.225(10) . ?
O3 N1 1.208(9) . ?
O4 C13 1.453(10) . ?
O4 C14 1.414(9) . ?
O5 C14 1.410(9) . ?
O5 C15 1.438(9) . ?
N1 C10 1.508(11) . ?
C1 C2 1.370(13) . ?
C1 C6 1.375(13) . ?
C2 H2 0.9500 . ?
C2 C3 1.394(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.390(12) . ?
C4 C5 1.400(12) . ?
C4 C7 1.508(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.396(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.497(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.558(10) . ?
C9 H9 1.0000 . ?
C9 C10 1.522(11) . ?
C9 C11 1.535(11) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11 1.0000 . ?
C11 C12 1.522(11) . ?
C11 C14 1.534(10) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.530(10) . ?
C13 H13 1.0000 . ?
C13 C17 1.495(11) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.493(13) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.396(11) . ?
C17 C22 1.404(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.386(12) . ?
C19 H19 0.9500 . ?
C19 C20 1.376(13) . ?
C20 H20 0.9500 . ?
C20 C21 1.383(13) . ?
C21 H21 0.9500 . ?
C21 C22 1.382(12) . ?
C22 H22 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
C14 O4 C13 110.7(6) . . ?
C14 O5 C15 111.6(6) . . ?
O2 N1 C10 117.8(7) . . ?
O3 N1 O2 124.4(8) . . ?
O3 N1 C10 117.8(8) . . ?
F1 C1 C2 117.8(8) . . ?
F1 C1 C6 117.9(8) . . ?
C2 C1 C6 124.3(8) . . ?
C1 C2 H2 121.0 . . ?
C1 C2 C3 118.0(8) . . ?
C3 C2 H2 121.0 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(8) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 119.6(7) . . ?
C3 C4 C7 122.8(7) . . ?
C5 C4 C7 117.7(7) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 C4 120.8(8) . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 117.0(8) . . ?
C1 C6 H6 121.5 . . ?
C5 C6 H6 121.5 . . ?
O1 C7 C4 119.8(8) . . ?
O1 C7 C8 122.3(7) . . ?
C8 C7 C4 117.8(7) . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C7 C8 C9 112.9(7) . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C8 C9 H9 106.8 . . ?
C10 C9 C8 111.5(6) . . ?
C10 C9 H9 106.8 . . ?
C10 C9 C11 114.2(6) . . ?
C11 C9 C8 110.3(6) . . ?
C11 C9 H9 106.8 . . ?
N1 C10 C9 111.5(7) . . ?
N1 C10 H10A 109.3 . . ?
N1 C10 H10B 109.3 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C9 C11 H11 109.7 . . ?
C12 C11 C9 113.2(6) . . ?
C12 C11 H11 109.7 . . ?
C12 C11 C14 100.6(6) . . ?
C14 C11 C9 113.6(6) . . ?
C14 C11 H11 109.7 . . ?
C11 C12 H12A 110.9 . . ?
C11 C12 H12B 110.9 . . ?
C11 C12 C13 104.5(7) . . ?
H12A C12 H12B 108.9 . . ?
C13 C12 H12A 110.9 . . ?
C13 C12 H12B 110.9 . . ?
O4 C13 C12 104.9(6) . . ?
O4 C13 H13 108.5 . . ?
O4 C13 C17 110.2(6) . . ?
C12 C13 H13 108.5 . . ?
C17 C13 C12 116.1(7) . . ?
C17 C13 H13 108.5 . . ?
O4 C14 C11 105.3(6) . . ?
O4 C14 H14 110.6 . . ?
O5 C14 O4 112.0(6) . . ?
O5 C14 C11 107.5(6) . . ?
O5 C14 H14 110.6 . . ?
C11 C14 H14 110.6 . . ?
O5 C15 H15A 109.9 . . ?
O5 C15 H15B 109.9 . . ?
O5 C15 C16 108.9(7) . . ?
H15A C15 H15B 108.3 . . ?
C16 C15 H15A 109.9 . . ?
C16 C15 H15B 109.9 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C13 120.7(7) . . ?
C18 C17 C22 118.1(7) . . ?
C22 C17 C13 121.2(7) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.7(8) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.6(8) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 120.2 . . ?
C19 C20 C21 119.5(8) . . ?
C21 C20 H20 120.2 . . ?
C20 C21 H21 119.7 . . ?
C22 C21 C20 120.6(8) . . ?
C22 C21 H21 119.7 . . ?
C17 C22 H22 119.8 . . ?
C21 C22 C17 120.5(8) . . ?
C21 C22 H22 119.8 . . ?

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
F1 C1 C2 C3 -179.6(7) . . . . ?
F1 C1 C6 C5 177.8(8) . . . . ?
O1 C7 C8 C9 5.1(11) . . . . ?
O2 N1 C10 C9 -67.1(9) . . . . ?
O3 N1 C10 C9 110.4(8) . . . . ?
O4 C13 C17 C18 57.6(9) . . . . ?
O4 C13 C17 C22 -123.6(7) . . . . ?
C1 C2 C3 C4 3.1(12) . . . . ?
C2 C1 C6 C5 -1.3(13) . . . . ?
C2 C3 C4 C5 -3.7(12) . . . . ?
C2 C3 C4 C7 177.7(8) . . . . ?
C3 C4 C5 C6 1.9(12) . . . . ?
C3 C4 C7 O1 -165.3(8) . . . . ?
C3 C4 C7 C8 17.6(11) . . . . ?
C4 C5 C6 C1 0.6(12) . . . . ?
C4 C7 C8 C9 -177.8(7) . . . . ?
C5 C4 C7 O1 16.1(12) . . . . ?
C5 C4 C7 C8 -161.0(7) . . . . ?
C6 C1 C2 C3 -0.5(13) . . . . ?
C7 C4 C5 C6 -179.5(8) . . . . ?
C7 C8 C9 C10 74.3(8) . . . . ?
C7 C8 C9 C11 -157.6(7) . . . . ?
C8 C9 C10 N1 81.3(8) . . . . ?
C8 C9 C11 C12 71.4(8) . . . . ?
C8 C9 C11 C14 -174.6(6) . . . . ?
C9 C11 C12 C13 87.3(7) . . . . ?
C9 C11 C14 O4 -84.9(8) . . . . ?
C9 C11 C14 O5 155.5(6) . . . . ?
C10 C9 C11 C12 -162.1(7) . . . . ?
C10 C9 C11 C14 -48.1(9) . . . . ?
C11 C9 C10 N1 -44.6(9) . . . . ?
C11 C12 C13 O4 20.8(8) . . . . ?
C11 C12 C13 C17 142.7(7) . . . . ?
C12 C11 C14 O4 36.4(8) . . . . ?
C12 C11 C14 O5 -83.2(7) . . . . ?
C12 C13 C17 C18 -61.4(10) . . . . ?
C12 C13 C17 C22 117.3(9) . . . . ?
C13 O4 C14 O5 91.6(7) . . . . ?
C13 O4 C14 C11 -24.9(8) . . . . ?
C13 C17 C18 C19 -179.4(8) . . . . ?
C13 C17 C22 C21 179.7(7) . . . . ?
C14 O4 C13 C12 2.6(8) . . . . ?
C14 O4 C13 C17 -123.1(7) . . . . ?
C14 O5 C15 C16 173.3(7) . . . . ?
C14 C11 C12 C13 -34.2(8) . . . . ?
C15 O5 C14 O4 68.7(8) . . . . ?
C15 O5 C14 C11 -176.1(6) . . . . ?
C17 C18 C19 C20 -1.6(12) . . . . ?
C18 C17 C22 C21 -1.6(11) . . . . ?
C18 C19 C20 C21 1.1(13) . . . . ?
C19 C20 C21 C22 -0.8(13) . . . . ?
C20 C21 C22 C17 1.1(12) . . . . ?
C22 C17 C18 C19 1.8(11) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.662(5)
2 0.338(5)

####################################################################### 
# 
# 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_cu_20160411xl_lyk_0m
_database_code_depnum_ccdc_archive 'CCDC 1568738'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2018-08-20 downloaded from the CCDC.
;
_audit_creation_date             2017-04-17
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C31 H32 N2 O4), 4(C4 H8 O2)'
_chemical_formula_sum            'C140 H160 N8 O24'
_chemical_formula_weight         2338.75
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.9683(3)
_cell_length_b                   16.3532(6)
_cell_length_c                   23.8547(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3108.4(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6473
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.332
_cell_measurement_theta_min      4.588
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9202
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.416
_diffrn_reflns_theta_min         5.410
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.614
_reflns_Friedel_fraction_full    0.797
_reflns_Friedel_fraction_max     0.790
_reflns_number_gt                4893
_reflns_number_total             5132
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 
;
 Flack x determined using 1783 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5132
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0385
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0543P)²+0.6404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.0992
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17A-C16 = C16-C17
 1.5 with sigma of 0.02
3. Others
 Sof(H16C)=Sof(H16D)=Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15C)=Sof(H15D)=
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C17)=
 Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C4(H4), C2(H2), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C27(H27A,H27B), C1(H1A,H1B), C16(H16A,H16B), C16(H16C,H16D),
 C14(H14A,H14B), C14(H14C,H14D), C15(H15A,H15B), C34(H34A,H34B), C15A(H15C,H15D)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C20(H20), C7(H7), C21(H21), C28(H28), C11(H11), C31(H31), C13(H13),
 C30(H30), C24(H24), C22(H22), C23(H23), C12(H12), C29(H29)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C17A(H17D,H17E,
 H17F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
O3 O 0.7165(2) 0.49004(9) 0.42942(6) 0.0215(3) Uani 1 1 d . . . . .
O4 O 0.5686(2) 0.39083(9) 0.38517(7) 0.0287(4) Uani 1 1 d . . . . .
O1 O 0.4489(3) 0.50382(15) 0.63911(8) 0.0581(6) Uani 1 1 d . . . . .
O2 O 0.3240(4) 0.61905(14) 0.62839(9) 0.0599(7) Uani 1 1 d . . . . .
N1 N 0.3743(3) 0.55358(15) 0.61068(9) 0.0370(5) Uani 1 1 d . . . . .
N2 N 1.0145(3) 0.39611(14) 0.58270(8) 0.0347(5) Uani 1 1 d . . . . .
C6 C 0.8830(3) 0.46253(12) 0.51263(9) 0.0219(5) Uani 1 1 d . . . . .
C9 C 0.9859(3) 0.39922(13) 0.48861(9) 0.0245(5) Uani 1 1 d . . . . .
C4 C 0.5953(3) 0.42735(13) 0.43810(9) 0.0235(5) Uani 1 1 d . . . . .
H4 H 0.6433 0.3855 0.4641 0.028 Uiso 1 1 calc R . . . .
C18 C 0.6321(3) 0.55792(13) 0.51597(9) 0.0222(5) Uani 1 1 d . . . . .
H18A H 0.6735 0.5728 0.5537 0.027 Uiso 1 1 calc R . . . .
H18B H 0.5880 0.6081 0.4981 0.027 Uiso 1 1 calc R . . . .
C19 C 0.8878(3) 0.59768(13) 0.46258(9) 0.0228(5) Uani 1 1 d . . . . .
C2 C 0.4895(3) 0.49598(13) 0.52196(8) 0.0239(5) Uani 1 1 d . . . . .
H2 H 0.5301 0.4493 0.5454 0.029 Uiso 1 1 calc R . . . .
C5 C 0.7797(3) 0.52501(12) 0.48083(8) 0.0208(5) Uani 1 1 d . . . . .
C10 C 1.0165(3) 0.37184(14) 0.43362(10) 0.0283(5) Uani 1 1 d . . . . .
H10 H 0.9659 0.3983 0.4024 0.034 Uiso 1 1 calc R . . . .
C27 C 0.3601(3) 0.52548(14) 0.42459(9) 0.0273(5) Uani 1 1 d . . . . .
H27A H 0.2452 0.5388 0.4374 0.033 Uiso 1 1 calc R . . . .
H27B H 0.4275 0.5763 0.4253 0.033 Uiso 1 1 calc R . . . .
C26 C 0.3536(3) 0.49253(14) 0.36565(9) 0.0266(5) Uani 1 1 d . . . . .
C20 C 0.9816(3) 0.63972(13) 0.50246(10) 0.0275(5) Uani 1 1 d . . . . .
H20 H 0.9799 0.6220 0.5404 0.033 Uiso 1 1 calc R . . . .
C25 C 0.4555(3) 0.42801(14) 0.34963(9) 0.0259(5) Uani 1 1 d . . . . .
C7 C 0.9044(3) 0.45803(15) 0.56928(10) 0.0297(5) Uani 1 1 d . . . . .
H7 H 0.8509 0.4927 0.5958 0.036 Uiso 1 1 calc R . . . .
C8 C 1.0651(3) 0.35894(14) 0.53377(10) 0.0298(5) Uani 1 1 d . . . . .
C3 C 0.4381(3) 0.46253(13) 0.46399(9) 0.0243(5) Uani 1 1 d . . . . .
H3 H 0.3557 0.4171 0.4696 0.029 Uiso 1 1 calc R . . . .
C21 C 1.0777(4) 0.70740(14) 0.48758(11) 0.0353(6) Uani 1 1 d . . . . .
H21 H 1.1418 0.7354 0.5151 0.042 Uiso 1 1 calc R . . . .
C28 C 0.2427(4) 0.52432(18) 0.32589(10) 0.0373(6) Uani 1 1 d . . . . .
H28 H 0.1712 0.5684 0.3360 0.045 Uiso 1 1 calc R . . . .
C11 C 1.1216(3) 0.30577(14) 0.42605(12) 0.0357(6) Uani 1 1 d . . . . .
H11 H 1.1420 0.2863 0.3892 0.043 Uiso 1 1 calc R . . . .
C31 C 0.4462(4) 0.39527(16) 0.29617(10) 0.0347(6) Uani 1 1 d . . . . .
H31 H 0.5157 0.3505 0.2861 0.042 Uiso 1 1 calc R . . . .
C13 C 1.1733(4) 0.29241(15) 0.52580(12) 0.0375(6) Uani 1 1 d . . . . .
H13 H 1.2268 0.2662 0.5565 0.045 Uiso 1 1 calc R . . . .
C30 C 0.3352(4) 0.42797(19) 0.25747(10) 0.0419(7) Uani 1 1 d . . . . .
H30 H 0.3286 0.4055 0.2208 0.050 Uiso 1 1 calc R . . . .
C24 C 0.8889(4) 0.62526(14) 0.40760(10) 0.0312(6) Uani 1 1 d . . . . .
H24 H 0.8247 0.5976 0.3799 0.037 Uiso 1 1 calc R . . . .
C1 C 0.3386(3) 0.53398(16) 0.55063(9) 0.0309(5) Uani 1 1 d . . . . .
H1A H 0.3066 0.5847 0.5307 0.037 Uiso 1 1 calc R . . . .
H1B H 0.2426 0.4956 0.5486 0.037 Uiso 1 1 calc R . . . .
C22 C 1.0792(4) 0.73360(14) 0.43235(12) 0.0415(7) Uani 1 1 d . . . . .
H22 H 1.1458 0.7792 0.4217 0.050 Uiso 1 1 calc R . . . .
C23 C 0.9839(4) 0.69340(15) 0.39295(11) 0.0412(7) Uani 1 1 d . . . . .
H23 H 0.9830 0.7123 0.3553 0.049 Uiso 1 1 calc R . . . .
C12 C 1.1988(4) 0.26676(15) 0.47147(14) 0.0414(7) Uani 1 1 d . . . . .
H12 H 1.2706 0.2215 0.4646 0.050 Uiso 1 1 calc R . . . .
C29 C 0.2347(4) 0.4930(2) 0.27206(10) 0.0442(7) Uani 1 1 d . . . . .
H29 H 0.1603 0.5162 0.2453 0.053 Uiso 1 1 calc R . . . .
C16 C 0.8022(5) 0.3483(2) 0.68876(13) 0.0544(8) Uani 1 1 d D . . . .
H16A H 0.7421 0.3640 0.6541 0.065 Uiso 0.658(8) 1 calc R . P A 1
H16B H 0.7430 0.3006 0.7049 0.065 Uiso 0.658(8) 1 calc R . P A 1
H16C H 0.8153 0.2896 0.6980 0.065 Uiso 0.342(8) 1 calc R . P A 2
H16D H 0.7384 0.3532 0.6533 0.065 Uiso 0.342(8) 1 calc R . P A 2
C14 C 1.0771(4) 0.3782(3) 0.63940(12) 0.0621(10) Uani 1 1 d . . . . .
H14A H 1.1937 0.3580 0.6359 0.075 Uiso 0.658(8) 1 calc R . P A 1
H14B H 1.0818 0.4304 0.6604 0.075 Uiso 0.658(8) 1 calc R . P A 1
H14C H 1.1129 0.3202 0.6400 0.075 Uiso 0.342(8) 1 calc R . P A 2
H14D H 1.1788 0.4118 0.6455 0.075 Uiso 0.342(8) 1 calc R . P A 2
C15 C 0.9858(7) 0.3209(2) 0.67233(17) 0.0428(14) Uani 0.658(8) 1 d . . P A 1
H15A H 1.0496 0.3102 0.7072 0.051 Uiso 0.658(8) 1 calc R . P A 1
H15B H 0.9788 0.2688 0.6514 0.051 Uiso 0.658(8) 1 calc R . P A 1
C17 C 0.7901(10) 0.4146(4) 0.7277(3) 0.0591(16) Uani 0.658(8) 1 d D . P A 1
H17A H 0.8619 0.4035 0.7601 0.089 Uiso 0.658(8) 1 calc GR . P A 1
H17B H 0.6735 0.4204 0.7401 0.089 Uiso 0.658(8) 1 calc GR . P A 1
H17C H 0.8266 0.4653 0.7094 0.089 Uiso 0.658(8) 1 calc GR . P A 1
O5 O 0.7786(3) 0.71582(11) 0.71277(7) 0.0412(5) Uani 1 1 d . . . . .
O6 O 0.8493(4) 0.62887(13) 0.64454(8) 0.0563(6) Uani 1 1 d . . . . .
C32 C 0.8705(4) 0.69281(17) 0.66853(11) 0.0421(7) Uani 1 1 d . . . . .
C34 C 0.6512(5) 0.6589(2) 0.73198(13) 0.0501(8) Uani 1 1 d . . . . .
H34A H 0.7015 0.6044 0.7388 0.060 Uiso 1 1 calc R . . . .
H34B H 0.5621 0.6530 0.7033 0.060 Uiso 1 1 calc R . . . .
C33 C 0.9974(6) 0.7556(2) 0.65351(13) 0.0580(9) Uani 1 1 d . . . . .
H33A H 0.9472 0.8102 0.6566 0.087 Uiso 1 1 calc GR . . . .
H33B H 1.0353 0.7467 0.6149 0.087 Uiso 1 1 calc GR . . . .
H33C H 1.0933 0.7515 0.6791 0.087 Uiso 1 1 calc GR . . . .
C35 C 0.5795(5) 0.6923(3) 0.78488(16) 0.0686(10) Uani 1 1 d . . . . .
H35A H 0.5346 0.7472 0.7779 0.103 Uiso 1 1 calc GR . . . .
H35B H 0.6677 0.6953 0.8135 0.103 Uiso 1 1 calc GR . . . .
H35C H 0.4892 0.6565 0.7980 0.103 Uiso 1 1 calc GR . . . .
C15A C 0.9742(13) 0.3902(5) 0.6837(3) 0.040(3) Uani 0.342(8) 1 d . . P A 2
H15C H 0.9538 0.4498 0.6861 0.048 Uiso 0.342(8) 1 calc R . P A 2
H15D H 1.0387 0.3749 0.7176 0.048 Uiso 0.342(8) 1 calc R . P A 2
C17A C 0.706(2) 0.3969(9) 0.7397(6) 0.069(4) Uani 0.342(8) 1 d D . P A 2
H17D H 0.7727 0.3925 0.7741 0.103 Uiso 0.342(8) 1 calc GR . P A 2
H17E H 0.5954 0.3726 0.7458 0.103 Uiso 0.342(8) 1 calc GR . P A 2
H17F H 0.6934 0.4546 0.7296 0.103 Uiso 0.342(8) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 C4 1.424(3) . ?
O3 C5 1.444(2) . ?
O4 C4 1.413(3) . ?
O4 C25 1.379(3) . ?
O1 N1 1.215(3) . ?
O2 N1 1.219(3) . ?
N1 C1 1.495(3) . ?
N2 C7 1.377(3) . ?
N2 C8 1.377(3) . ?
N2 C14 1.471(3) . ?
C6 C9 1.440(3) . ?
C6 C5 1.516(3) . ?
C6 C7 1.364(3) . ?
C9 C10 1.407(3) . ?
C9 C8 1.412(3) . ?
C4 H4 1.0000 . ?
C4 C3 1.511(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C2 1.529(3) . ?
C18 C5 1.541(3) . ?
C19 C5 1.531(3) . ?
C19 C20 1.391(3) . ?
C19 C24 1.387(3) . ?
C2 H2 1.0000 . ?
C2 C3 1.542(3) . ?
C2 C1 1.517(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.379(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C26 1.507(3) . ?
C27 C3 1.526(3) . ?
C26 C25 1.385(3) . ?
C26 C28 1.397(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.392(3) . ?
C25 C31 1.385(3) . ?
C7 H7 0.9500 . ?
C8 C13 1.401(3) . ?
C3 H3 1.0000 . ?
C21 H21 0.9500 . ?
C21 C22 1.386(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.384(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.400(4) . ?
C31 H31 0.9500 . ?
C31 C30 1.385(4) . ?
C13 H13 0.9500 . ?
C13 C12 1.377(4) . ?
C30 H30 0.9500 . ?
C30 C29 1.376(4) . ?
C24 H24 0.9500 . ?
C24 C23 1.392(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C22 H22 0.9500 . ?
C22 C23 1.375(4) . ?
C23 H23 0.9500 . ?
C12 H12 0.9500 . ?
C29 H29 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 H16C 0.9900 . ?
C16 H16D 0.9900 . ?
C16 C15 1.580(6) . ?
C16 C17 1.430(7) . ?
C16 C15A 1.537(10) . ?
C16 C17A 1.640(12) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 H14C 0.9900 . ?
C14 H14D 0.9900 . ?
C14 C15 1.423(6) . ?
C14 C15A 1.352(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O5 C32 1.339(3) . ?
O5 C34 1.452(4) . ?
O6 C32 1.204(3) . ?
C32 C33 1.485(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.489(5) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 O3 C5 113.46(15) . . ?
C25 O4 C4 117.50(17) . . ?
O1 N1 O2 123.8(2) . . ?
O1 N1 C1 119.0(2) . . ?
O2 N1 C1 117.2(2) . . ?
C7 N2 C14 125.2(2) . . ?
C8 N2 C7 108.32(19) . . ?
C8 N2 C14 126.3(2) . . ?
C9 C6 C5 126.51(19) . . ?
C7 C6 C9 106.5(2) . . ?
C7 C6 C5 126.9(2) . . ?
C10 C9 C6 134.3(2) . . ?
C10 C9 C8 119.1(2) . . ?
C8 C9 C6 106.6(2) . . ?
O3 C4 H4 108.9 . . ?
O3 C4 C3 110.36(17) . . ?
O4 C4 O3 106.06(17) . . ?
O4 C4 H4 108.9 . . ?
O4 C4 C3 113.65(19) . . ?
C3 C4 H4 108.9 . . ?
H18A C18 H18B 107.8 . . ?
C2 C18 H18A 109.0 . . ?
C2 C18 H18B 109.0 . . ?
C2 C18 C5 112.75(17) . . ?
C5 C18 H18A 109.0 . . ?
C5 C18 H18B 109.0 . . ?
C20 C19 C5 119.42(19) . . ?
C24 C19 C5 121.7(2) . . ?
C24 C19 C20 118.9(2) . . ?
C18 C2 H2 108.5 . . ?
C18 C2 C3 110.40(17) . . ?
C3 C2 H2 108.5 . . ?
C1 C2 C18 111.10(18) . . ?
C1 C2 H2 108.5 . . ?
C1 C2 C3 109.82(19) . . ?
O3 C5 C6 110.32(16) . . ?
O3 C5 C18 109.53(18) . . ?
O3 C5 C19 105.19(16) . . ?
C6 C5 C18 112.19(17) . . ?
C6 C5 C19 111.11(19) . . ?
C19 C5 C18 108.25(16) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 C9 118.4(2) . . ?
C11 C10 H10 120.8 . . ?
H27A C27 H27B 108.1 . . ?
C26 C27 H27A 109.6 . . ?
C26 C27 H27B 109.6 . . ?
C26 C27 C3 110.33(18) . . ?
C3 C27 H27A 109.6 . . ?
C3 C27 H27B 109.6 . . ?
C25 C26 C27 120.7(2) . . ?
C25 C26 C28 117.8(2) . . ?
C28 C26 C27 121.5(2) . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 120.9(2) . . ?
C21 C20 H20 119.5 . . ?
O4 C25 C26 123.33(19) . . ?
O4 C25 C31 115.5(2) . . ?
C26 C25 C31 121.1(2) . . ?
N2 C7 H7 124.8 . . ?
C6 C7 N2 110.5(2) . . ?
C6 C7 H7 124.8 . . ?
N2 C8 C9 108.1(2) . . ?
N2 C8 C13 129.7(2) . . ?
C13 C8 C9 122.3(2) . . ?
C4 C3 C2 106.34(19) . . ?
C4 C3 C27 110.04(18) . . ?
C4 C3 H3 108.5 . . ?
C2 C3 H3 108.5 . . ?
C27 C3 C2 114.90(18) . . ?
C27 C3 H3 108.5 . . ?
C20 C21 H21 120.2 . . ?
C22 C21 C20 119.5(2) . . ?
C22 C21 H21 120.2 . . ?
C26 C28 H28 119.3 . . ?
C29 C28 C26 121.4(3) . . ?
C29 C28 H28 119.3 . . ?
C10 C11 H11 119.2 . . ?
C10 C11 C12 121.5(3) . . ?
C12 C11 H11 119.2 . . ?
C25 C31 H31 120.1 . . ?
C25 C31 C30 119.9(2) . . ?
C30 C31 H31 120.1 . . ?
C8 C13 H13 121.5 . . ?
C12 C13 C8 117.1(2) . . ?
C12 C13 H13 121.5 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 C31 120.1(2) . . ?
C29 C30 H30 120.0 . . ?
C19 C24 H24 120.0 . . ?
C19 C24 C23 120.1(2) . . ?
C23 C24 H24 120.0 . . ?
N1 C1 C2 111.6(2) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C21 C22 H22 120.1 . . ?
C23 C22 C21 119.8(2) . . ?
C23 C22 H22 120.1 . . ?
C24 C23 H23 119.6 . . ?
C22 C23 C24 120.8(2) . . ?
C22 C23 H23 119.6 . . ?
C11 C12 H12 119.2 . . ?
C13 C12 C11 121.6(2) . . ?
C13 C12 H12 119.2 . . ?
C28 C29 H29 120.2 . . ?
C30 C29 C28 119.6(3) . . ?
C30 C29 H29 120.2 . . ?
H16A C16 H16B 107.4 . . ?
H16C C16 H16D 108.8 . . ?
C15 C16 H16A 108.3 . . ?
C15 C16 H16B 108.3 . . ?
C17 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
C17 C16 C15 116.0(4) . . ?
C15A C16 H16C 110.8 . . ?
C15A C16 H16D 110.8 . . ?
C15A C16 C17A 104.9(7) . . ?
C17A C16 H16C 110.8 . . ?
C17A C16 H16D 110.8 . . ?
N2 C14 H14A 107.9 . . ?
N2 C14 H14B 107.9 . . ?
N2 C14 H14C 107.6 . . ?
N2 C14 H14D 107.6 . . ?
H14A C14 H14B 107.2 . . ?
H14C C14 H14D 107.0 . . ?
C15 C14 N2 117.7(3) . . ?
C15 C14 H14A 107.9 . . ?
C15 C14 H14B 107.9 . . ?
C15A C14 N2 119.0(4) . . ?
C15A C14 H14C 107.6 . . ?
C15A C14 H14D 107.6 . . ?
C16 C15 H15A 108.5 . . ?
C16 C15 H15B 108.5 . . ?
C14 C15 C16 115.1(3) . . ?
C14 C15 H15A 108.5 . . ?
C14 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C32 O5 C34 116.8(2) . . ?
O5 C32 C33 111.6(2) . . ?
O6 C32 O5 122.8(3) . . ?
O6 C32 C33 125.6(3) . . ?
O5 C34 H34A 110.2 . . ?
O5 C34 H34B 110.2 . . ?
O5 C34 C35 107.4(3) . . ?
H34A C34 H34B 108.5 . . ?
C35 C34 H34A 110.2 . . ?
C35 C34 H34B 110.2 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C16 C15A H15C 106.7 . . ?
C16 C15A H15D 106.7 . . ?
C14 C15A C16 122.5(6) . . ?
C14 C15A H15C 106.7 . . ?
C14 C15A H15D 106.7 . . ?
H15C C15A H15D 106.6 . . ?
C16 C17A H17D 109.5 . . ?
C16 C17A H17E 109.5 . . ?
C16 C17A H17F 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 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
O3 C4 C3 C2 -63.4(2) . . . . ?
O3 C4 C3 C27 61.6(2) . . . . ?
O4 C4 C3 C2 177.62(16) . . . . ?
O4 C4 C3 C27 -57.4(2) . . . . ?
O4 C25 C31 C30 179.5(2) . . . . ?
O1 N1 C1 C2 -43.5(3) . . . . ?
O2 N1 C1 C2 137.4(3) . . . . ?
N2 C8 C13 C12 178.6(3) . . . . ?
N2 C14 C15 C16 -64.9(5) . . . . ?
N2 C14 C15A C16 56.9(7) . . . . ?
C6 C9 C10 C11 -177.7(2) . . . . ?
C6 C9 C8 N2 -0.5(3) . . . . ?
C6 C9 C8 C13 178.8(2) . . . . ?
C9 C6 C5 O3 33.2(3) . . . . ?
C9 C6 C5 C18 155.6(2) . . . . ?
C9 C6 C5 C19 -83.1(3) . . . . ?
C9 C6 C7 N2 0.1(3) . . . . ?
C9 C10 C11 C12 -0.8(4) . . . . ?
C9 C8 C13 C12 -0.6(4) . . . . ?
C4 O3 C5 C6 67.6(2) . . . . ?
C4 O3 C5 C18 -56.4(2) . . . . ?
C4 O3 C5 C19 -172.53(16) . . . . ?
C4 O4 C25 C26 -8.0(3) . . . . ?
C4 O4 C25 C31 173.5(2) . . . . ?
C18 C2 C3 C4 56.2(2) . . . . ?
C18 C2 C3 C27 -65.8(3) . . . . ?
C18 C2 C1 N1 -67.9(2) . . . . ?
C19 C20 C21 C22 0.4(4) . . . . ?
C19 C24 C23 C22 0.8(4) . . . . ?
C2 C18 C5 O3 48.9(2) . . . . ?
C2 C18 C5 C6 -74.0(2) . . . . ?
C2 C18 C5 C19 163.09(17) . . . . ?
C5 O3 C4 O4 -170.33(16) . . . . ?
C5 O3 C4 C3 66.2(2) . . . . ?
C5 C6 C9 C10 -4.5(4) . . . . ?
C5 C6 C9 C8 176.9(2) . . . . ?
C5 C6 C7 N2 -176.5(2) . . . . ?
C5 C18 C2 C3 -51.1(2) . . . . ?
C5 C18 C2 C1 -173.13(18) . . . . ?
C5 C19 C20 C21 -178.3(2) . . . . ?
C5 C19 C24 C23 177.6(2) . . . . ?
C10 C9 C8 N2 -179.4(2) . . . . ?
C10 C9 C8 C13 0.0(3) . . . . ?
C10 C11 C12 C13 0.1(4) . . . . ?
C27 C26 C25 O4 -0.8(4) . . . . ?
C27 C26 C25 C31 177.6(2) . . . . ?
C27 C26 C28 C29 -178.8(3) . . . . ?
C26 C27 C3 C4 46.3(3) . . . . ?
C26 C27 C3 C2 166.3(2) . . . . ?
C26 C25 C31 C30 1.0(4) . . . . ?
C26 C28 C29 C30 1.4(5) . . . . ?
C20 C19 C5 O3 -173.4(2) . . . . ?
C20 C19 C5 C6 -54.0(3) . . . . ?
C20 C19 C5 C18 69.6(3) . . . . ?
C20 C19 C24 C23 0.6(4) . . . . ?
C20 C21 C22 C23 1.0(4) . . . . ?
C25 O4 C4 O3 -83.8(2) . . . . ?
C25 O4 C4 C3 37.6(3) . . . . ?
C25 C26 C28 C29 -0.3(4) . . . . ?
C25 C31 C30 C29 0.1(4) . . . . ?
C7 N2 C8 C9 0.6(3) . . . . ?
C7 N2 C8 C13 -178.7(3) . . . . ?
C7 N2 C14 C15 91.5(4) . . . . ?
C7 N2 C14 C15A 34.4(6) . . . . ?
C7 C6 C9 C10 178.9(3) . . . . ?
C7 C6 C9 C8 0.2(3) . . . . ?
C7 C6 C5 O3 -150.9(2) . . . . ?
C7 C6 C5 C18 -28.5(3) . . . . ?
C7 C6 C5 C19 92.8(3) . . . . ?
C8 N2 C7 C6 -0.4(3) . . . . ?
C8 N2 C14 C15 -94.2(4) . . . . ?
C8 N2 C14 C15A -151.2(5) . . . . ?
C8 C9 C10 C11 0.8(3) . . . . ?
C8 C13 C12 C11 0.6(4) . . . . ?
C3 C2 C1 N1 169.71(19) . . . . ?
C3 C27 C26 C25 -19.7(3) . . . . ?
C3 C27 C26 C28 158.8(2) . . . . ?
C21 C22 C23 C24 -1.6(5) . . . . ?
C28 C26 C25 O4 -179.3(2) . . . . ?
C28 C26 C25 C31 -0.9(4) . . . . ?
C31 C30 C29 C28 -1.3(5) . . . . ?
C24 C19 C5 O3 9.7(3) . . . . ?
C24 C19 C5 C6 129.0(2) . . . . ?
C24 C19 C5 C18 -107.4(2) . . . . ?
C24 C19 C20 C21 -1.2(4) . . . . ?
C1 C2 C3 C4 179.04(19) . . . . ?
C1 C2 C3 C27 57.0(3) . . . . ?
C14 N2 C7 C6 174.8(3) . . . . ?
C14 N2 C8 C9 -174.6(3) . . . . ?
C14 N2 C8 C13 6.2(4) . . . . ?
C17 C16 C15 C14 -69.0(5) . . . . ?
C32 O5 C34 C35 173.5(3) . . . . ?
C34 O5 C32 O6 1.1(4) . . . . ?
C34 O5 C32 C33 -179.3(3) . . . . ?
C17A C16 C15A C14 -166.7(7) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1568735'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2018-08-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H40 Br2 N2 O10'
_chemical_formula_sum            'C40 H40 Br2 N2 O10'
_chemical_formula_weight         868.56
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   6.6706(10)
_cell_length_b                   25.351(4)
_cell_length_c                   11.3316(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 89.90
_cell_angle_gamma                90.00
_cell_volume                     1916.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4507
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      23.46

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_absorpt_coefficient_mu    2.176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6122
_exptl_absorpt_correction_T_max  0.7222
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9707
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6468
_reflns_number_gt                5619
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1100P)²+0.0226P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.048(14)
_refine_ls_number_reflns         6468
_refine_ls_number_parameters     490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1664
_refine_ls_wR_factor_gt          0.1627
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 1.29800(11) 0.37836(3) 1.11549(7) 0.0449(2) Uani 1 1 d . . .
Br2 Br 0.18866(11) -0.07293(3) 0.72332(7) 0.0460(2) Uani 1 1 d . . .
C1 C 0.7020(13) 0.2441(3) 0.7566(7) 0.046(2) Uani 1 1 d . . .
C2 C 0.5933(14) 0.2032(4) 0.7039(8) 0.058(3) Uani 1 1 d . . .
H2 H 0.4939 0.1857 0.7463 0.069 Uiso 1 1 calc R . .
C3 C 0.6340(18) 0.1888(4) 0.5886(9) 0.071(3) Uani 1 1 d . . .
H3 H 0.5586 0.1624 0.5527 0.086 Uiso 1 1 calc R . .
C4 C 0.7859(18) 0.2133(4) 0.5263(9) 0.065(3) Uani 1 1 d . . .
H4 H 0.8164 0.2031 0.4495 0.078 Uiso 1 1 calc R . .
C5 C 0.8933(16) 0.2539(4) 0.5818(8) 0.056(2) Uani 1 1 d . . .
H5 H 0.9923 0.2715 0.5392 0.067 Uiso 1 1 calc R . .
C6 C 0.8588(12) 0.2684(3) 0.6933(7) 0.0401(18) Uani 1 1 d . . .
C7 C 0.9791(13) 0.3122(4) 0.7540(7) 0.048(2) Uani 1 1 d . . .
H7A H 1.1047 0.2979 0.7829 0.057 Uiso 1 1 calc R . .
H7B H 1.0100 0.3397 0.6972 0.057 Uiso 1 1 calc R . .
C8 C 0.8617(11) 0.3357(3) 0.8562(7) 0.0353(16) Uani 1 1 d . . .
H8 H 0.7543 0.3576 0.8235 0.042 Uiso 1 1 calc R . .
C9 C 0.7662(10) 0.2932(3) 0.9329(6) 0.0337(16) Uani 1 1 d . . .
H9 H 0.6819 0.3104 0.9924 0.040 Uiso 1 1 calc R . .
C10 C 1.0210(10) 0.2924(3) 1.0779(6) 0.0293(15) Uani 1 1 d . . .
C11 C 1.1330(10) 0.3352(3) 1.0090(6) 0.0315(15) Uani 1 1 d . . .
H11 H 1.2222 0.3179 0.9522 0.038 Uiso 1 1 calc R . .
C12 C 0.9891(10) 0.3705(3) 0.9409(6) 0.0326(15) Uani 1 1 d . . .
H12 H 0.8978 0.3870 0.9978 0.039 Uiso 1 1 calc R . .
C13 C 1.0976(11) 0.4145(3) 0.8744(7) 0.0401(18) Uani 1 1 d . . .
H13A H 1.1719 0.4363 0.9294 0.048 Uiso 1 1 calc R . .
H13B H 1.1917 0.3994 0.8184 0.048 Uiso 1 1 calc R . .
C14 C 1.1661(11) 0.2535(3) 1.1350(7) 0.0328(16) Uani 1 1 d . . .
C15 C 1.2604(12) 0.2147(3) 1.0697(8) 0.0418(18) Uani 1 1 d . . .
H15 H 1.2397 0.2126 0.9887 0.050 Uiso 1 1 calc R . .
C16 C 1.3858(14) 0.1792(4) 1.1252(10) 0.057(2) Uani 1 1 d . . .
H16 H 1.4493 0.1532 1.0809 0.069 Uiso 1 1 calc R . .
C17 C 1.4182(14) 0.1817(4) 1.2450(9) 0.054(2) Uani 1 1 d . . .
H17 H 1.5013 0.1573 1.2818 0.065 Uiso 1 1 calc R . .
C18 C 1.3248(12) 0.2213(4) 1.3104(8) 0.045(2) Uani 1 1 d . . .
H18 H 1.3457 0.2237 1.3914 0.054 Uiso 1 1 calc R . .
C19 C 1.2042(14) 0.2559(3) 1.2552(7) 0.047(2) Uani 1 1 d . . .
H19 H 1.1440 0.2825 1.2994 0.057 Uiso 1 1 calc R . .
C20 C 0.7480(13) 0.2837(4) 1.2151(8) 0.047(2) Uani 1 1 d . . .
H20A H 0.7735 0.2475 1.1953 0.070 Uiso 1 1 calc R . .
H20B H 0.6158 0.2933 1.1895 0.070 Uiso 1 1 calc R . .
H20C H 0.7579 0.2883 1.2990 0.070 Uiso 1 1 calc R . .
C21 C 0.8194(12) 0.0546(3) 0.3727(6) 0.0410(18) Uani 1 1 d . . .
C22 C 0.9448(15) 0.0928(4) 0.3234(8) 0.058(2) Uani 1 1 d . . .
H22 H 1.0471 0.1079 0.3676 0.069 Uiso 1 1 calc R . .
C23 C 0.9132(16) 0.1079(4) 0.2058(9) 0.056(2) Uani 1 1 d . . .
H23 H 0.9932 0.1337 0.1715 0.067 Uiso 1 1 calc R . .
C24 C 0.7654(16) 0.0845(4) 0.1426(9) 0.055(2) Uani 1 1 d . . .
H24 H 0.7472 0.0941 0.0641 0.066 Uiso 1 1 calc R . .
C25 C 0.6432(14) 0.0475(4) 0.1912(7) 0.049(2) Uani 1 1 d . . .
H25 H 0.5420 0.0323 0.1462 0.059 Uiso 1 1 calc R . .
C26 C 0.6694(12) 0.0319(3) 0.3100(6) 0.0372(17) Uani 1 1 d . . .
C27 C 0.5330(12) -0.0082(4) 0.3688(7) 0.045(2) Uani 1 1 d . . .
H27A H 0.4134 0.0093 0.3978 0.054 Uiso 1 1 calc R . .
H27B H 0.4923 -0.0345 0.3114 0.054 Uiso 1 1 calc R . .
C28 C 0.6384(11) -0.0346(3) 0.4693(7) 0.0376(17) Uani 1 1 d . . .
H28 H 0.7416 -0.0579 0.4362 0.045 Uiso 1 1 calc R . .
C29 C 0.7417(11) 0.0057(4) 0.5476(7) 0.0417(19) Uani 1 1 d . . .
H29 H 0.8168 -0.0124 0.6097 0.050 Uiso 1 1 calc R . .
C30 C 0.4684(10) 0.0121(3) 0.6840(6) 0.0313(15) Uani 1 1 d . . .
C31 C 0.3571(10) -0.0309(3) 0.6181(6) 0.0319(15) Uani 1 1 d . . .
H31 H 0.2703 -0.0141 0.5594 0.038 Uiso 1 1 calc R . .
C32 C 0.5049(9) -0.0678(3) 0.5521(5) 0.0314(14) Uani 1 1 d . . .
H32 H 0.5911 -0.0850 0.6106 0.038 Uiso 1 1 calc R . .
C33 C 0.3942(12) -0.1103(3) 0.4837(7) 0.0402(18) Uani 1 1 d . . .
H33A H 0.3111 -0.1307 0.5371 0.048 Uiso 1 1 calc R . .
H33B H 0.3078 -0.0941 0.4253 0.048 Uiso 1 1 calc R . .
C34 C 0.3287(11) 0.0521(3) 0.7381(7) 0.0367(17) Uani 1 1 d . . .
C35 C 0.2395(13) 0.0908(3) 0.6675(9) 0.052(2) Uani 1 1 d . . .
H35 H 0.2656 0.0927 0.5869 0.062 Uiso 1 1 calc R . .
C36 C 0.1059(15) 0.1276(4) 0.7240(14) 0.071(3) Uani 1 1 d . . .
H36 H 0.0436 0.1532 0.6783 0.086 Uiso 1 1 calc R . .
C37 C 0.0687(16) 0.1263(5) 0.8374(16) 0.085(4) Uani 1 1 d . . .
H37 H -0.0144 0.1516 0.8712 0.102 Uiso 1 1 calc R . .
C38 C 0.1498(15) 0.0888(6) 0.9046(11) 0.076(4) Uani 1 1 d . . .
H38 H 0.1181 0.0879 0.9846 0.091 Uiso 1 1 calc R . .
C39 C 0.2799(13) 0.0510(4) 0.8596(8) 0.052(2) Uani 1 1 d . . .
H39 H 0.3343 0.0253 0.9087 0.062 Uiso 1 1 calc R . .
C40 C 0.7260(11) 0.0203(4) 0.8281(7) 0.0429(19) Uani 1 1 d . . .
H40A H 0.7943 0.0422 0.7718 0.064 Uiso 1 1 calc R . .
H40B H 0.8221 -0.0008 0.8699 0.064 Uiso 1 1 calc R . .
H40C H 0.6544 0.0421 0.8831 0.064 Uiso 1 1 calc R . .
N1 N 0.9450(11) 0.4475(3) 0.8103(7) 0.0489(18) Uani 1 1 d . . .
N2 N 0.5422(12) -0.1459(3) 0.4237(7) 0.0541(19) Uani 1 1 d . . .
O1 O 0.6456(9) 0.2577(3) 0.8675(5) 0.0526(15) Uani 1 1 d . . .
O2 O 0.9110(7) 0.26260(19) 0.9910(4) 0.0339(11) Uani 1 1 d . . .
O3 O 0.8973(7) 0.3178(2) 1.1556(4) 0.0366(11) Uani 1 1 d . . .
O4 O 0.9413(11) 0.4470(3) 0.7045(7) 0.074(2) Uani 1 1 d . . .
O5 O 0.8276(14) 0.4736(4) 0.8690(8) 0.095(3) Uani 1 1 d . . .
O6 O 0.8689(8) 0.0402(3) 0.4870(5) 0.0491(15) Uani 1 1 d . . .
O7 O 0.5897(7) 0.0396(2) 0.6007(4) 0.0341(11) Uani 1 1 d . . .
O8 O 0.5908(7) -0.0127(2) 0.7693(4) 0.0355(11) Uani 1 1 d . . .
O9 O 0.5520(11) -0.1442(3) 0.3167(6) 0.075(2) Uani 1 1 d . . .
O10 O 0.6573(16) -0.1718(4) 0.4835(7) 0.096(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C11 1.966(6) . ?
Br2 C31 1.953(6) . ?
C1 O1 1.355(11) . ?
C1 C2 1.400(11) . ?
C1 C6 1.410(12) . ?
C2 C3 1.383(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.381(16) . ?
C3 H3 0.9300 . ?
C4 C5 1.404(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.335(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.534(11) . ?
C7 C8 1.518(12) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.524(11) . ?
C8 C12 1.558(9) . ?
C8 H8 0.9800 . ?
C9 O2 1.404(9) . ?
C9 O1 1.417(9) . ?
C9 H9 0.9800 . ?
C10 O3 1.367(9) . ?
C10 O2 1.443(8) . ?
C10 C14 1.528(10) . ?
C10 C11 1.530(10) . ?
C11 C12 1.524(9) . ?
C11 H11 0.9800 . ?
C12 C13 1.527(10) . ?
C12 H12 0.9800 . ?
C13 N1 1.505(10) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.380(11) . ?
C14 C19 1.388(11) . ?
C15 C16 1.381(12) . ?
C15 H15 0.9300 . ?
C16 C17 1.376(14) . ?
C16 H16 0.9300 . ?
C17 C18 1.394(14) . ?
C17 H17 0.9300 . ?
C18 C19 1.346(12) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 O3 1.479(10) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C26 1.356(11) . ?
C21 O6 1.386(10) . ?
C21 C22 1.395(12) . ?
C22 C23 1.403(14) . ?
C22 H22 0.9300 . ?
C23 C24 1.356(15) . ?
C23 H23 0.9300 . ?
C24 C25 1.360(13) . ?
C24 H24 0.9300 . ?
C25 C26 1.414(11) . ?
C25 H25 0.9300 . ?
C26 C27 1.517(10) . ?
C27 C28 1.498(12) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.520(11) . ?
C28 C32 1.542(10) . ?
C28 H28 0.9800 . ?
C29 O6 1.397(9) . ?
C29 O7 1.457(10) . ?
C29 H29 0.9800 . ?
C30 O8 1.414(8) . ?
C30 O7 1.424(9) . ?
C30 C34 1.506(10) . ?
C30 C31 1.518(10) . ?
C31 C32 1.549(10) . ?
C31 H31 0.9800 . ?
C32 C33 1.520(10) . ?
C32 H32 0.9800 . ?
C33 N2 1.499(11) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.400(12) . ?
C34 C39 1.414(12) . ?
C35 C36 1.439(15) . ?
C35 H35 0.9300 . ?
C36 C37 1.308(19) . ?
C36 H36 0.9300 . ?
C37 C38 1.33(2) . ?
C37 H37 0.9300 . ?
C38 C39 1.389(15) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 O8 1.400(9) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
N1 O4 1.199(10) . ?
N1 O5 1.222(11) . ?
N2 O9 1.214(10) . ?
N2 O10 1.217(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 116.2(8) . . ?
O1 C1 C6 124.4(7) . . ?
C2 C1 C6 119.4(8) . . ?
C3 C2 C1 119.9(9) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 120.4(8) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 118.4(9) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
C6 C5 C4 122.5(10) . . ?
C6 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C5 C6 C1 119.2(7) . . ?
C5 C6 C7 122.3(8) . . ?
C1 C6 C7 118.5(7) . . ?
C8 C7 C6 110.9(7) . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 C9 111.9(7) . . ?
C7 C8 C12 114.3(6) . . ?
C9 C8 C12 106.1(6) . . ?
C7 C8 H8 108.1 . . ?
C9 C8 H8 108.1 . . ?
C12 C8 H8 108.1 . . ?
O2 C9 O1 106.7(6) . . ?
O2 C9 C8 111.8(6) . . ?
O1 C9 C8 112.8(6) . . ?
O2 C9 H9 108.5 . . ?
O1 C9 H9 108.5 . . ?
C8 C9 H9 108.5 . . ?
O3 C10 O2 112.3(5) . . ?
O3 C10 C14 114.4(6) . . ?
O2 C10 C14 105.8(5) . . ?
O3 C10 C11 106.8(6) . . ?
O2 C10 C11 105.8(5) . . ?
C14 C10 C11 111.5(6) . . ?
C12 C11 C10 111.6(6) . . ?
C12 C11 Br1 109.8(4) . . ?
C10 C11 Br1 110.8(5) . . ?
C12 C11 H11 108.2 . . ?
C10 C11 H11 108.2 . . ?
Br1 C11 H11 108.2 . . ?
C11 C12 C13 112.4(6) . . ?
C11 C12 C8 108.9(5) . . ?
C13 C12 C8 111.6(6) . . ?
C11 C12 H12 107.9 . . ?
C13 C12 H12 107.9 . . ?
C8 C12 H12 107.9 . . ?
N1 C13 C12 108.9(6) . . ?
N1 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
N1 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C15 C14 C19 118.3(7) . . ?
C15 C14 C10 121.4(7) . . ?
C19 C14 C10 120.3(7) . . ?
C14 C15 C16 119.7(8) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 121.1(9) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 119.1(8) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
C19 C18 C17 119.3(8) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C14 122.6(8) . . ?
C18 C19 H19 118.7 . . ?
C14 C19 H19 118.7 . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 O6 123.7(6) . . ?
C26 C21 C22 121.8(8) . . ?
O6 C21 C22 114.4(7) . . ?
C21 C22 C23 118.6(9) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
C24 C23 C22 119.6(9) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 121.6(9) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C24 C25 C26 120.3(9) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 118.2(7) . . ?
C21 C26 C27 119.8(7) . . ?
C25 C26 C27 122.0(7) . . ?
C28 C27 C26 110.6(6) . . ?
C28 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C27 C28 C29 110.9(7) . . ?
C27 C28 C32 115.8(6) . . ?
C29 C28 C32 105.9(6) . . ?
C27 C28 H28 108.0 . . ?
C29 C28 H28 108.0 . . ?
C32 C28 H28 108.0 . . ?
O6 C29 O7 104.9(7) . . ?
O6 C29 C28 114.2(6) . . ?
O7 C29 C28 108.7(6) . . ?
O6 C29 H29 109.6 . . ?
O7 C29 H29 109.6 . . ?
C28 C29 H29 109.6 . . ?
O8 C30 O7 110.0(5) . . ?
O8 C30 C34 112.3(6) . . ?
O7 C30 C34 107.0(6) . . ?
O8 C30 C31 107.4(6) . . ?
O7 C30 C31 107.6(5) . . ?
C34 C30 C31 112.4(6) . . ?
C30 C31 C32 111.1(5) . . ?
C30 C31 Br2 111.9(5) . . ?
C32 C31 Br2 109.3(5) . . ?
C30 C31 H31 108.1 . . ?
C32 C31 H31 108.1 . . ?
Br2 C31 H31 108.1 . . ?
C33 C32 C28 110.9(6) . . ?
C33 C32 C31 111.4(5) . . ?
C28 C32 C31 109.4(6) . . ?
C33 C32 H32 108.4 . . ?
C28 C32 H32 108.4 . . ?
C31 C32 H32 108.4 . . ?
N2 C33 C32 109.7(6) . . ?
N2 C33 H33A 109.7 . . ?
C32 C33 H33A 109.7 . . ?
N2 C33 H33B 109.7 . . ?
C32 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
C35 C34 C39 118.2(8) . . ?
C35 C34 C30 120.1(7) . . ?
C39 C34 C30 121.6(8) . . ?
C34 C35 C36 117.6(10) . . ?
C34 C35 H35 121.2 . . ?
C36 C35 H35 121.2 . . ?
C37 C36 C35 122.5(11) . . ?
C37 C36 H36 118.8 . . ?
C35 C36 H36 118.8 . . ?
C36 C37 C38 120.2(10) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C37 C38 C39 122.4(12) . . ?
C37 C38 H38 118.8 . . ?
C39 C38 H38 118.8 . . ?
C38 C39 C34 119.1(11) . . ?
C38 C39 H39 120.4 . . ?
C34 C39 H39 120.4 . . ?
O8 C40 H40A 109.5 . . ?
O8 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O8 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O4 N1 O5 122.4(8) . . ?
O4 N1 C13 119.5(8) . . ?
O5 N1 C13 118.1(8) . . ?
O9 N2 O10 122.8(9) . . ?
O9 N2 C33 117.7(8) . . ?
O10 N2 C33 119.2(8) . . ?
C1 O1 C9 119.3(6) . . ?
C9 O2 C10 112.5(5) . . ?
C10 O3 C20 115.1(6) . . ?
C21 O6 C29 118.6(5) . . ?
C30 O7 C29 112.4(5) . . ?
C40 O8 C30 115.6(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
O1 C1 C2 C3 176.5(9) . . . . ?
C6 C1 C2 C3 -3.1(14) . . . . ?
C1 C2 C3 C4 2.2(16) . . . . ?
C2 C3 C4 C5 -1.8(16) . . . . ?
C3 C4 C5 C6 2.4(16) . . . . ?
C4 C5 C6 C1 -3.4(14) . . . . ?
C4 C5 C6 C7 178.9(9) . . . . ?
O1 C1 C6 C5 -175.9(9) . . . . ?
C2 C1 C6 C5 3.6(13) . . . . ?
O1 C1 C6 C7 1.9(13) . . . . ?
C2 C1 C6 C7 -178.6(8) . . . . ?
C5 C6 C7 C8 157.0(8) . . . . ?
C1 C6 C7 C8 -20.7(11) . . . . ?
C6 C7 C8 C9 45.5(9) . . . . ?
C6 C7 C8 C12 166.1(6) . . . . ?
C7 C8 C9 O2 66.0(8) . . . . ?
C12 C8 C9 O2 -59.3(8) . . . . ?
C7 C8 C9 O1 -54.2(8) . . . . ?
C12 C8 C9 O1 -179.5(6) . . . . ?
O3 C10 C11 C12 -60.7(7) . . . . ?
O2 C10 C11 C12 59.1(7) . . . . ?
C14 C10 C11 C12 173.7(6) . . . . ?
O3 C10 C11 Br1 61.9(6) . . . . ?
O2 C10 C11 Br1 -178.3(4) . . . . ?
C14 C10 C11 Br1 -63.7(7) . . . . ?
C10 C11 C12 C13 178.4(6) . . . . ?
Br1 C11 C12 C13 55.1(7) . . . . ?
C10 C11 C12 C8 -57.4(8) . . . . ?
Br1 C11 C12 C8 179.4(5) . . . . ?
C7 C8 C12 C11 -69.6(8) . . . . ?
C9 C8 C12 C11 54.2(8) . . . . ?
C7 C8 C12 C13 55.1(8) . . . . ?
C9 C8 C12 C13 178.8(6) . . . . ?
C11 C12 C13 N1 -179.7(6) . . . . ?
C8 C12 C13 N1 57.6(8) . . . . ?
O3 C10 C14 C15 161.9(7) . . . . ?
O2 C10 C14 C15 37.8(9) . . . . ?
C11 C10 C14 C15 -76.8(8) . . . . ?
O3 C10 C14 C19 -17.3(10) . . . . ?
O2 C10 C14 C19 -141.4(7) . . . . ?
C11 C10 C14 C19 104.0(8) . . . . ?
C19 C14 C15 C16 1.2(12) . . . . ?
C10 C14 C15 C16 -178.0(8) . . . . ?
C14 C15 C16 C17 0.1(13) . . . . ?
C15 C16 C17 C18 -1.0(14) . . . . ?
C16 C17 C18 C19 0.5(13) . . . . ?
C17 C18 C19 C14 0.9(13) . . . . ?
C15 C14 C19 C18 -1.7(13) . . . . ?
C10 C14 C19 C18 177.5(8) . . . . ?
C26 C21 C22 C23 0.1(14) . . . . ?
O6 C21 C22 C23 176.6(8) . . . . ?
C21 C22 C23 C24 -1.2(14) . . . . ?
C22 C23 C24 C25 1.5(15) . . . . ?
C23 C24 C25 C26 -0.7(14) . . . . ?
O6 C21 C26 C25 -175.5(8) . . . . ?
C22 C21 C26 C25 0.7(13) . . . . ?
O6 C21 C26 C27 5.8(13) . . . . ?
C22 C21 C26 C27 -178.1(8) . . . . ?
C24 C25 C26 C21 -0.4(13) . . . . ?
C24 C25 C26 C27 178.3(8) . . . . ?
C21 C26 C27 C28 -25.9(11) . . . . ?
C25 C26 C27 C28 155.4(8) . . . . ?
C26 C27 C28 C29 47.4(9) . . . . ?
C26 C27 C28 C32 168.1(7) . . . . ?
C27 C28 C29 O6 -52.9(9) . . . . ?
C32 C28 C29 O6 -179.3(6) . . . . ?
C27 C28 C29 O7 63.8(8) . . . . ?
C32 C28 C29 O7 -62.6(8) . . . . ?
O8 C30 C31 C32 -62.2(7) . . . . ?
O7 C30 C31 C32 56.2(7) . . . . ?
C34 C30 C31 C32 173.7(6) . . . . ?
O8 C30 C31 Br2 60.2(6) . . . . ?
O7 C30 C31 Br2 178.7(4) . . . . ?
C34 C30 C31 Br2 -63.8(7) . . . . ?
C27 C28 C32 C33 57.2(9) . . . . ?
C29 C28 C32 C33 -179.4(6) . . . . ?
C27 C28 C32 C31 -65.9(8) . . . . ?
C29 C28 C32 C31 57.4(7) . . . . ?
C30 C31 C32 C33 -178.8(6) . . . . ?
Br2 C31 C32 C33 57.3(6) . . . . ?
C30 C31 C32 C28 -55.9(7) . . . . ?
Br2 C31 C32 C28 -179.8(4) . . . . ?
C28 C32 C33 N2 59.4(8) . . . . ?
C31 C32 C33 N2 -178.6(6) . . . . ?
O8 C30 C34 C35 161.6(7) . . . . ?
O7 C30 C34 C35 40.7(9) . . . . ?
C31 C30 C34 C35 -77.2(9) . . . . ?
O8 C30 C34 C39 -20.0(10) . . . . ?
O7 C30 C34 C39 -140.8(7) . . . . ?
C31 C30 C34 C39 101.3(8) . . . . ?
C39 C34 C35 C36 0.9(12) . . . . ?
C30 C34 C35 C36 179.4(8) . . . . ?
C34 C35 C36 C37 1.0(15) . . . . ?
C35 C36 C37 C38 -2.5(18) . . . . ?
C36 C37 C38 C39 2.1(18) . . . . ?
C37 C38 C39 C34 -0.1(16) . . . . ?
C35 C34 C39 C38 -1.4(12) . . . . ?
C30 C34 C39 C38 -179.8(8) . . . . ?
C12 C13 N1 O4 -112.5(8) . . . . ?
C12 C13 N1 O5 66.8(9) . . . . ?
C32 C33 N2 O9 -111.2(8) . . . . ?
C32 C33 N2 O10 63.0(10) . . . . ?
C2 C1 O1 C9 170.8(7) . . . . ?
C6 C1 O1 C9 -9.6(12) . . . . ?
O2 C9 O1 C1 -87.5(8) . . . . ?
C8 C9 O1 C1 35.6(10) . . . . ?
O1 C9 O2 C10 -169.3(5) . . . . ?
C8 C9 O2 C10 66.9(7) . . . . ?
O3 C10 O2 C9 52.8(7) . . . . ?
C14 C10 O2 C9 178.3(5) . . . . ?
C11 C10 O2 C9 -63.3(7) . . . . ?
O2 C10 O3 C20 53.5(8) . . . . ?
C14 C10 O3 C20 -67.2(8) . . . . ?
C11 C10 O3 C20 169.0(6) . . . . ?
C26 C21 O6 C29 -9.2(12) . . . . ?
C22 C21 O6 C29 174.3(8) . . . . ?
O7 C29 O6 C21 -86.0(8) . . . . ?
C28 C29 O6 C21 32.9(10) . . . . ?
O8 C30 O7 C29 53.8(7) . . . . ?
C34 C30 O7 C29 176.1(5) . . . . ?
C31 C30 O7 C29 -62.9(7) . . . . ?
O6 C29 O7 C30 -169.0(5) . . . . ?
C28 C29 O7 C30 68.5(7) . . . . ?
O7 C30 O8 C40 54.7(7) . . . . ?
C34 C30 O8 C40 -64.3(8) . . . . ?
C31 C30 O8 C40 171.6(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.106
