# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_jwrr220106
_database_code_depnum_ccdc_archive 'CCDC 2157002'
loop_
_audit_author_name
_audit_author_address
'Lydia Karmazin'
;CNRS and Universite de Strasbourg
France
;
_audit_update_record             
;
2022-03-07 deposited with the CCDC.	2022-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H17 Br O'
_chemical_formula_sum            'C27 H17 Br O'
_chemical_formula_weight         437.32

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.4721(3)
_cell_length_b                   16.1858(7)
_cell_length_c                   14.3123(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.9750(10)
_cell_angle_gamma                90
_cell_volume                     1886.82(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9816
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      29.10

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_F_000             888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.195
_shelx_estimated_absorpt_T_min   0.668
_shelx_estimated_absorpt_T_max   0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7044
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            68068
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.943
_diffrn_reflns_theta_max         29.192
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5098
_reflns_number_gt                4432
_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0269P)²+1.3350P] 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         5098
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0690
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.72756(17) 0.38929(9) 0.55092(10) 0.0154(3) Uani 1 1 d . . . . .
C2 C 0.71736(17) 0.32672(9) 0.61900(11) 0.0168(3) Uani 1 1 d . . . . .
C3 C 0.81995(19) 0.32724(10) 0.71254(11) 0.0208(3) Uani 1 1 d . . . . .
H3 H 0.813701 0.283791 0.756004 0.025 Uiso 1 1 calc R U . . .
C4 C 0.93284(19) 0.39122(11) 0.74367(11) 0.0223(3) Uani 1 1 d . . . . .
H4 H 1.005595 0.390510 0.807398 0.027 Uiso 1 1 calc R U . . .
C5 C 0.93786(18) 0.45471(10) 0.68193(11) 0.0197(3) Uani 1 1 d . . . . .
C6 C 0.83248(18) 0.45789(9) 0.58582(11) 0.0175(3) Uani 1 1 d . . . . .
C7 C 0.8175(2) 0.53054(10) 0.52711(12) 0.0222(3) Uani 1 1 d . . . . .
H7 H 0.893923 0.574408 0.546827 0.027 Uiso 1 1 calc R U . . .
C8 C 0.6952(2) 0.53716(10) 0.44368(12) 0.0220(3) Uani 1 1 d . . . . .
H8 H 0.676621 0.588673 0.410640 0.026 Uiso 1 1 calc R U . . .
C9 C 0.59335(19) 0.46822(10) 0.40433(11) 0.0190(3) Uani 1 1 d . . . . .
C10 C 0.4606(2) 0.47776(11) 0.31898(11) 0.0231(3) Uani 1 1 d . . . . .
H10 H 0.443047 0.529385 0.286164 0.028 Uiso 1 1 calc R U . . .
C11 C 0.3588(2) 0.41319(11) 0.28430(11) 0.0239(3) Uani 1 1 d . . . . .
H11 H 0.260149 0.422231 0.234288 0.029 Uiso 1 1 calc R U . . .
C12 C 0.39824(18) 0.33234(11) 0.32203(11) 0.0205(3) Uani 1 1 d . . . . .
C13 C 0.29525(19) 0.26378(12) 0.28305(12) 0.0259(3) Uani 1 1 d . . . . .
H13 H 0.194805 0.272869 0.234546 0.031 Uiso 1 1 calc R U . . .
C14 C 0.3388(2) 0.18597(12) 0.31428(12) 0.0268(4) Uani 1 1 d . . . . .
H14 H 0.263358 0.141905 0.293120 0.032 Uiso 1 1 calc R U . . .
C15 C 0.49697(19) 0.16944(10) 0.37870(12) 0.0217(3) Uani 1 1 d . . . . .
C16 C 0.5439(2) 0.08660(11) 0.40860(13) 0.0260(3) Uani 1 1 d . . . . .
H16 H 0.466424 0.043224 0.388568 0.031 Uiso 1 1 calc R U . . .
C17 C 0.6965(2) 0.06883(10) 0.46486(13) 0.0253(3) Uani 1 1 d . . . . .
H17 H 0.721048 0.014864 0.490921 0.030 Uiso 1 1 calc R U . . .
C18 C 0.82110(19) 0.13117(10) 0.48520(11) 0.0189(3) Uani 1 1 d . . . . .
C19 C 0.9874(2) 0.11038(10) 0.52882(11) 0.0222(3) Uani 1 1 d . . . . .
H19 H 1.014119 0.056669 0.555192 0.027 Uiso 1 1 calc R U . . .
C20 C 1.1102(2) 0.16645(10) 0.53358(12) 0.0234(3) Uani 1 1 d . . . . .
H20 H 1.221380 0.151410 0.562366 0.028 Uiso 1 1 calc R U . . .
C21 C 1.07155(18) 0.24622(10) 0.49582(12) 0.0211(3) Uani 1 1 d . . . . .
H21 H 1.157047 0.284095 0.495468 0.025 Uiso 1 1 calc R U . . .
C22 C 0.90988(18) 0.26982(9) 0.45924(11) 0.0168(3) Uani 1 1 d . . . . .
H22 H 0.885436 0.324732 0.436402 0.020 Uiso 1 1 calc R U . . .
C23 C 0.77946(18) 0.21389(9) 0.45499(10) 0.0156(3) Uani 1 1 d . . . . .
C24 C 0.60735(17) 0.23530(9) 0.41239(10) 0.0166(3) Uani 1 1 d . . . . .
C25 C 0.54631(17) 0.31887(10) 0.39715(10) 0.0165(3) Uani 1 1 d . . . . .
C26 C 0.62414(17) 0.39060(9) 0.45089(10) 0.0154(3) Uani 1 1 d . . . . .
C27 C 0.5995(2) 0.19888(11) 0.64793(13) 0.0270(4) Uani 1 1 d . . . . .
H27A H 0.707287 0.172373 0.660057 0.041 Uiso 1 1 calc R U . . .
H27B H 0.513942 0.160010 0.614394 0.041 Uiso 1 1 calc R U . . .
H27C H 0.580697 0.215177 0.709929 0.041 Uiso 1 1 calc R U . . .
O1 O 0.59468(13) 0.27027(7) 0.58888(8) 0.0192(2) Uani 1 1 d . . . . .
Br1 Br 1.08716(2) 0.54271(2) 0.73139(2) 0.02768(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.424(2) . ?
C1 C2 1.424(2) . ?
C1 C26 1.4586(19) . ?
C2 O1 1.3618(18) . ?
C2 C3 1.381(2) . ?
C3 C4 1.397(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.364(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.420(2) . ?
C5 Br1 1.9070(15) . ?
C6 C7 1.430(2) . ?
C7 C8 1.353(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.428(2) . ?
C8 H8 0.9500 . ?
C9 C26 1.412(2) . ?
C9 C10 1.423(2) . ?
C10 C11 1.359(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.420(2) . ?
C11 H11 0.9500 . ?
C12 C25 1.426(2) . ?
C12 C13 1.427(2) . ?
C13 C14 1.353(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.427(2) . ?
C14 H14 0.9500 . ?
C15 C24 1.413(2) . ?
C15 C16 1.430(2) . ?
C16 C17 1.353(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.431(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.416(2) . ?
C18 C23 1.421(2) . ?
C19 C20 1.368(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.403(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.417(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.459(2) . ?
C24 C25 1.443(2) . ?
C25 C26 1.447(2) . ?
C27 O1 1.4255(19) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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
C6 C1 C2 117.64(13) . . ?
C6 C1 C26 118.76(13) . . ?
C2 C1 C26 123.28(13) . . ?
O1 C2 C3 122.20(14) . . ?
O1 C2 C1 116.43(13) . . ?
C3 C2 C1 121.22(14) . . ?
C2 C3 C4 120.45(15) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 119.52(14) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 122.12(14) . . ?
C4 C5 Br1 117.27(12) . . ?
C6 C5 Br1 120.57(12) . . ?
C5 C6 C1 118.48(14) . . ?
C5 C6 C7 121.96(14) . . ?
C1 C6 C7 119.28(14) . . ?
C8 C7 C6 120.41(15) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 121.27(15) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C26 C9 C10 120.08(15) . . ?
C26 C9 C8 119.74(14) . . ?
C10 C9 C8 120.18(14) . . ?
C11 C10 C9 120.16(15) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.69(14) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C25 119.59(15) . . ?
C11 C12 C13 120.88(14) . . ?
C25 C12 C13 119.48(15) . . ?
C14 C13 C12 120.85(15) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 120.67(15) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C24 C15 C14 119.65(15) . . ?
C24 C15 C16 120.13(15) . . ?
C14 C15 C16 120.22(15) . . ?
C17 C16 C15 121.27(15) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 120.11(16) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C19 C18 C23 119.45(14) . . ?
C19 C18 C17 120.72(15) . . ?
C23 C18 C17 119.67(14) . . ?
C20 C19 C18 121.01(15) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 119.83(15) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 120.22(15) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 121.39(14) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C22 C23 C18 117.61(13) . . ?
C22 C23 C24 122.97(13) . . ?
C18 C23 C24 119.12(13) . . ?
C15 C24 C25 118.67(13) . . ?
C15 C24 C23 117.07(14) . . ?
C25 C24 C23 124.13(13) . . ?
C12 C25 C24 117.48(14) . . ?
C12 C25 C26 117.09(14) . . ?
C24 C25 C26 125.42(13) . . ?
C9 C26 C25 117.70(13) . . ?
C9 C26 C1 117.33(13) . . ?
C25 C26 C1 124.93(13) . . ?
O1 C27 H27A 109.5 . . ?
O1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C2 O1 C27 117.47(12) . . ?

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
C6 C1 C2 O1 168.03(12) . . . . ?
C26 C1 C2 O1 -5.4(2) . . . . ?
C6 C1 C2 C3 -7.7(2) . . . . ?
C26 C1 C2 C3 178.83(14) . . . . ?
O1 C2 C3 C4 -173.19(14) . . . . ?
C1 C2 C3 C4 2.3(2) . . . . ?
C2 C3 C4 C5 2.0(2) . . . . ?
C3 C4 C5 C6 -0.6(2) . . . . ?
C3 C4 C5 Br1 176.89(12) . . . . ?
C4 C5 C6 C1 -5.0(2) . . . . ?
Br1 C5 C6 C1 177.66(10) . . . . ?
C4 C5 C6 C7 168.93(15) . . . . ?
Br1 C5 C6 C7 -8.5(2) . . . . ?
C2 C1 C6 C5 8.8(2) . . . . ?
C26 C1 C6 C5 -177.39(13) . . . . ?
C2 C1 C6 C7 -165.22(13) . . . . ?
C26 C1 C6 C7 8.6(2) . . . . ?
C5 C6 C7 C8 -167.64(15) . . . . ?
C1 C6 C7 C8 6.2(2) . . . . ?
C6 C7 C8 C9 -9.5(2) . . . . ?
C7 C8 C9 C26 -2.5(2) . . . . ?
C7 C8 C9 C10 177.01(15) . . . . ?
C26 C9 C10 C11 2.8(2) . . . . ?
C8 C9 C10 C11 -176.72(14) . . . . ?
C9 C10 C11 C12 -10.7(2) . . . . ?
C10 C11 C12 C25 0.0(2) . . . . ?
C10 C11 C12 C13 -177.34(15) . . . . ?
C11 C12 C13 C14 175.29(15) . . . . ?
C25 C12 C13 C14 -2.1(2) . . . . ?
C12 C13 C14 C15 -7.2(2) . . . . ?
C13 C14 C15 C24 1.8(2) . . . . ?
C13 C14 C15 C16 -177.82(16) . . . . ?
C24 C15 C16 C17 -3.7(2) . . . . ?
C14 C15 C16 C17 175.98(16) . . . . ?
C15 C16 C17 C18 -8.2(3) . . . . ?
C16 C17 C18 C19 -168.63(15) . . . . ?
C16 C17 C18 C23 6.8(2) . . . . ?
C23 C18 C19 C20 -6.6(2) . . . . ?
C17 C18 C19 C20 168.86(15) . . . . ?
C18 C19 C20 C21 0.8(2) . . . . ?
C19 C20 C21 C22 3.9(2) . . . . ?
C20 C21 C22 C23 -2.6(2) . . . . ?
C21 C22 C23 C18 -3.1(2) . . . . ?
C21 C22 C23 C24 -176.85(14) . . . . ?
C19 C18 C23 C22 7.6(2) . . . . ?
C17 C18 C23 C22 -167.87(14) . . . . ?
C19 C18 C23 C24 -178.42(13) . . . . ?
C17 C18 C23 C24 6.1(2) . . . . ?
C14 C15 C24 C25 12.5(2) . . . . ?
C16 C15 C24 C25 -167.80(14) . . . . ?
C14 C15 C24 C23 -163.49(14) . . . . ?
C16 C15 C24 C23 16.2(2) . . . . ?
C22 C23 C24 C15 156.38(14) . . . . ?
C18 C23 C24 C15 -17.2(2) . . . . ?
C22 C23 C24 C25 -19.4(2) . . . . ?
C18 C23 C24 C25 166.98(13) . . . . ?
C11 C12 C25 C24 -161.24(13) . . . . ?
C13 C12 C25 C24 16.2(2) . . . . ?
C11 C12 C25 C26 17.9(2) . . . . ?
C13 C12 C25 C26 -164.70(13) . . . . ?
C15 C24 C25 C12 -21.2(2) . . . . ?
C23 C24 C25 C12 154.50(14) . . . . ?
C15 C24 C25 C26 159.72(14) . . . . ?
C23 C24 C25 C26 -24.6(2) . . . . ?
C10 C9 C26 C25 15.3(2) . . . . ?
C8 C9 C26 C25 -165.18(13) . . . . ?
C10 C9 C26 C1 -162.57(13) . . . . ?
C8 C9 C26 C1 16.9(2) . . . . ?
C12 C25 C26 C9 -25.21(19) . . . . ?
C24 C25 C26 C9 153.84(14) . . . . ?
C12 C25 C26 C1 152.50(14) . . . . ?
C24 C25 C26 C1 -28.5(2) . . . . ?
C6 C1 C26 C9 -19.82(19) . . . . ?
C2 C1 C26 C9 153.59(14) . . . . ?
C6 C1 C26 C25 162.47(13) . . . . ?
C2 C1 C26 C25 -24.1(2) . . . . ?
C3 C2 O1 C27 -15.5(2) . . . . ?
C1 C2 O1 C27 168.77(13) . . . . ?

_refine_diff_density_max         0.453
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_ejwvs211201
_database_code_depnum_ccdc_archive 'CCDC 2157005'
loop_
_audit_author_name
_audit_author_address
'Nathalie GRUBER'
;CNRS and Universite de Strasbourg
France
;
_audit_update_record             
;
2022-03-07 deposited with the CCDC.	2022-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H18 O2'
_chemical_formula_sum            'C28 H18 O2'
_chemical_formula_weight         386.42

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'

_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                   11.5972(4)
_cell_length_b                   12.8994(5)
_cell_length_c                   13.7902(5)
_cell_angle_alpha                90
_cell_angle_beta                 114.2170(10)
_cell_angle_gamma                90
_cell_volume                     1881.43(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      27.90

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.085
_shelx_estimated_absorpt_T_min   0.983
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7243
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            71287
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.262
_diffrn_reflns_theta_max         27.921
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4496
_reflns_number_gt                3925
_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0503P)²+0.7407P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4496
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.1034
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.60630(7) 0.30448(6) 0.38159(6) 0.02070(17) Uani 1 1 d . . . . .
O2 O 0.12585(9) 0.59728(8) 0.11795(9) 0.0409(2) Uani 1 1 d . . . . .
C22 C 0.67987(9) 0.49843(8) 0.21904(8) 0.0197(2) Uani 1 1 d . . . . .
H22 H 0.648011 0.552428 0.248014 0.024 Uiso 1 1 calc R U . . .
C2 C 0.50921(9) 0.35725(8) 0.30826(8) 0.0187(2) Uani 1 1 d . . . . .
C23 C 0.75829(9) 0.42159(8) 0.28766(8) 0.0190(2) Uani 1 1 d . . . . .
C24 C 0.79830(10) 0.42429(8) 0.40219(8) 0.0203(2) Uani 1 1 d . . . . .
C26 C 0.60815(10) 0.52036(8) 0.41032(8) 0.0209(2) Uani 1 1 d . . . . .
C1 C 0.50469(10) 0.46603(8) 0.32738(8) 0.0197(2) Uani 1 1 d . . . . .
C6 C 0.38884(10) 0.51856(8) 0.26935(9) 0.0219(2) Uani 1 1 d . . . . .
C3 C 0.41466(10) 0.30895(9) 0.22296(9) 0.0220(2) Uani 1 1 d . . . . .
H3 H 0.422157 0.237966 0.208104 0.026 Uiso 1 1 calc R U . . .
C25 C 0.73918(10) 0.48716(8) 0.45556(8) 0.0213(2) Uani 1 1 d . . . . .
C21 C 0.64849(10) 0.49704(9) 0.11136(9) 0.0243(2) Uani 1 1 d . . . . .
H21 H 0.596527 0.550218 0.067296 0.029 Uiso 1 1 calc R U . . .
C9 C 0.57768(11) 0.61141(9) 0.45193(9) 0.0255(2) Uani 1 1 d . . . . .
C5 C 0.29116(10) 0.46733(9) 0.18189(9) 0.0238(2) Uani 1 1 d . . . . .
C18 C 0.81112(10) 0.34629(8) 0.24226(9) 0.0238(2) Uani 1 1 d . . . . .
C27 C 0.62945(11) 0.20020(8) 0.35806(9) 0.0240(2) Uani 1 1 d . . . . .
H27A H 0.559652 0.155533 0.354934 0.036 Uiso 1 1 calc R U . . .
H27B H 0.708730 0.175205 0.413807 0.036 Uiso 1 1 calc R U . . .
H27C H 0.635780 0.198615 0.289358 0.036 Uiso 1 1 calc R U . . .
C12 C 0.81589(11) 0.52013(9) 0.56074(9) 0.0272(2) Uani 1 1 d . . . . .
C4 C 0.30858(10) 0.36565(9) 0.15932(9) 0.0242(2) Uani 1 1 d . . . . .
H4 H 0.246137 0.333500 0.098431 0.029 Uiso 1 1 calc R U . . .
C7 C 0.37058(11) 0.61961(9) 0.30445(10) 0.0286(3) Uani 1 1 d . . . . .
H7 H 0.296860 0.658376 0.263732 0.034 Uiso 1 1 calc R U . . .
C15 C 0.90847(10) 0.36862(9) 0.46454(9) 0.0260(2) Uani 1 1 d . . . . .
C20 C 0.69300(12) 0.41732(10) 0.06642(9) 0.0290(3) Uani 1 1 d . . . . .
H20 H 0.667450 0.414232 -0.008378 0.035 Uiso 1 1 calc R U . . .
C16 C 0.95879(11) 0.29338(9) 0.41630(11) 0.0310(3) Uani 1 1 d . . . . .
H16 H 1.029095 0.252577 0.460067 0.037 Uiso 1 1 calc R U . . .
C17 C 0.90881(11) 0.27900(9) 0.31016(11) 0.0299(3) Uani 1 1 d . . . . .
H17 H 0.938504 0.224141 0.280481 0.036 Uiso 1 1 calc R U . . .
C11 C 0.77652(13) 0.60500(10) 0.60547(9) 0.0325(3) Uani 1 1 d . . . . .
H11 H 0.828508 0.627472 0.675501 0.039 Uiso 1 1 calc R U . . .
C14 C 0.97348(11) 0.39171(10) 0.57467(10) 0.0322(3) Uani 1 1 d . . . . .
H14 H 1.045784 0.352334 0.617337 0.039 Uiso 1 1 calc R U . . .
C28 C 0.16785(11) 0.51196(10) 0.11305(10) 0.0307(3) Uani 1 1 d . . . . .
H28 H 0.113871 0.468397 0.057394 0.037 Uiso 1 1 calc R U . . .
C19 C 0.77323(11) 0.34422(9) 0.13077(10) 0.0293(3) Uani 1 1 d . . . . .
H19 H 0.804172 0.291007 0.100146 0.035 Uiso 1 1 calc R U . . .
C8 C 0.45845(12) 0.65964(9) 0.39558(10) 0.0302(3) Uani 1 1 d . . . . .
H8 H 0.439788 0.722064 0.422775 0.036 Uiso 1 1 calc R U . . .
C13 C 0.93323(12) 0.46926(11) 0.61914(9) 0.0331(3) Uani 1 1 d . . . . .
H13 H 0.983731 0.490058 0.690107 0.040 Uiso 1 1 calc R U . . .
C10 C 0.66608(13) 0.65416(10) 0.54971(10) 0.0316(3) Uani 1 1 d . . . . .
H10 H 0.647211 0.717283 0.575598 0.038 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 C2 1.3489(12) . ?
O1 C27 1.4347(13) . ?
O2 C28 1.2166(16) . ?
C22 C21 1.3764(15) . ?
C22 C23 1.4138(14) . ?
C22 H22 0.9500 . ?
C2 C3 1.3842(14) . ?
C2 C1 1.4328(15) . ?
C23 C18 1.4232(15) . ?
C23 C24 1.4525(14) . ?
C24 C15 1.4093(15) . ?
C24 C25 1.4435(15) . ?
C26 C9 1.4142(15) . ?
C26 C25 1.4506(15) . ?
C26 C1 1.4536(14) . ?
C1 C6 1.4222(15) . ?
C6 C5 1.4331(16) . ?
C6 C7 1.4360(15) . ?
C3 C4 1.3904(15) . ?
C3 H3 0.9500 . ?
C25 C12 1.4204(15) . ?
C21 C20 1.4038(17) . ?
C21 H21 0.9500 . ?
C9 C8 1.4218(17) . ?
C9 C10 1.4280(17) . ?
C5 C4 1.3819(16) . ?
C5 C28 1.4711(15) . ?
C18 C19 1.4154(17) . ?
C18 C17 1.4295(16) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C12 C11 1.4207(18) . ?
C12 C13 1.4255(18) . ?
C4 H4 0.9500 . ?
C7 C8 1.3541(18) . ?
C7 H7 0.9500 . ?
C15 C14 1.4228(17) . ?
C15 C16 1.4295(18) . ?
C20 C19 1.3656(18) . ?
C20 H20 0.9500 . ?
C16 C17 1.3478(19) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C11 C10 1.351(2) . ?
C11 H11 0.9500 . ?
C14 C13 1.353(2) . ?
C14 H14 0.9500 . ?
C28 H28 0.9500 . ?
C19 H19 0.9500 . ?
C8 H8 0.9500 . ?
C13 H13 0.9500 . ?
C10 H10 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
C2 O1 C27 118.66(8) . . ?
C21 C22 C23 121.72(10) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
O1 C2 C3 122.45(10) . . ?
O1 C2 C1 116.01(9) . . ?
C3 C2 C1 121.41(10) . . ?
C22 C23 C18 117.31(10) . . ?
C22 C23 C24 122.81(9) . . ?
C18 C23 C24 119.44(10) . . ?
C15 C24 C25 118.46(10) . . ?
C15 C24 C23 117.16(10) . . ?
C25 C24 C23 124.14(9) . . ?
C9 C26 C25 117.56(10) . . ?
C9 C26 C1 117.17(10) . . ?
C25 C26 C1 125.25(10) . . ?
C6 C1 C2 117.42(9) . . ?
C6 C1 C26 119.83(10) . . ?
C2 C1 C26 122.43(10) . . ?
C1 C6 C5 119.47(10) . . ?
C1 C6 C7 118.60(10) . . ?
C5 C6 C7 121.83(10) . . ?
C2 C3 C4 119.15(10) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C12 C25 C24 117.35(10) . . ?
C12 C25 C26 117.23(10) . . ?
C24 C25 C26 125.41(9) . . ?
C22 C21 C20 120.23(11) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C26 C9 C8 119.37(10) . . ?
C26 C9 C10 120.12(11) . . ?
C8 C9 C10 120.51(11) . . ?
C4 C5 C6 119.29(10) . . ?
C4 C5 C28 114.79(11) . . ?
C6 C5 C28 125.89(11) . . ?
C19 C18 C23 119.53(10) . . ?
C19 C18 C17 120.64(11) . . ?
C23 C18 C17 119.65(11) . . ?
O1 C27 H27A 109.5 . . ?
O1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C12 C11 119.73(11) . . ?
C25 C12 C13 119.47(12) . . ?
C11 C12 C13 120.78(11) . . ?
C5 C4 C3 122.03(10) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C8 C7 C6 120.01(11) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C24 C15 C14 119.70(11) . . ?
C24 C15 C16 120.20(11) . . ?
C14 C15 C16 120.01(11) . . ?
C19 C20 C21 119.66(11) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C17 C16 C15 121.54(11) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 120.00(11) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C10 C11 C12 120.86(11) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C14 C15 120.56(11) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
O2 C28 C5 128.58(13) . . ?
O2 C28 H28 115.7 . . ?
C5 C28 H28 115.7 . . ?
C20 C19 C18 121.20(11) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C7 C8 C9 122.23(11) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C14 C13 C12 120.76(11) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C11 C10 C9 120.12(11) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?

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
C27 O1 C2 C3 15.03(14) . . . . ?
C27 O1 C2 C1 -168.95(9) . . . . ?
C21 C22 C23 C18 4.27(15) . . . . ?
C21 C22 C23 C24 176.62(10) . . . . ?
C22 C23 C24 C15 -157.63(10) . . . . ?
C18 C23 C24 C15 14.57(14) . . . . ?
C22 C23 C24 C25 16.69(15) . . . . ?
C18 C23 C24 C25 -171.11(9) . . . . ?
O1 C2 C1 C6 -163.70(9) . . . . ?
C3 C2 C1 C6 12.37(15) . . . . ?
O1 C2 C1 C26 9.77(14) . . . . ?
C3 C2 C1 C26 -174.15(10) . . . . ?
C9 C26 C1 C6 18.91(14) . . . . ?
C25 C26 C1 C6 -162.82(10) . . . . ?
C9 C26 C1 C2 -154.42(10) . . . . ?
C25 C26 C1 C2 23.86(16) . . . . ?
C2 C1 C6 C5 -11.54(15) . . . . ?
C26 C1 C6 C5 174.81(9) . . . . ?
C2 C1 C6 C7 164.82(9) . . . . ?
C26 C1 C6 C7 -8.83(15) . . . . ?
O1 C2 C3 C4 170.91(9) . . . . ?
C1 C2 C3 C4 -4.91(15) . . . . ?
C15 C24 C25 C12 22.66(14) . . . . ?
C23 C24 C25 C12 -151.59(10) . . . . ?
C15 C24 C25 C26 -158.00(10) . . . . ?
C23 C24 C25 C26 27.75(16) . . . . ?
C9 C26 C25 C12 24.24(14) . . . . ?
C1 C26 C25 C12 -154.03(10) . . . . ?
C9 C26 C25 C24 -155.11(10) . . . . ?
C1 C26 C25 C24 26.63(16) . . . . ?
C23 C22 C21 C20 0.84(16) . . . . ?
C25 C26 C9 C8 166.04(10) . . . . ?
C1 C26 C9 C8 -15.55(15) . . . . ?
C25 C26 C9 C10 -14.02(15) . . . . ?
C1 C26 C9 C10 164.39(10) . . . . ?
C1 C6 C5 C4 3.65(15) . . . . ?
C7 C6 C5 C4 -172.59(10) . . . . ?
C1 C6 C5 C28 -178.58(10) . . . . ?
C7 C6 C5 C28 5.18(17) . . . . ?
C22 C23 C18 C19 -6.72(15) . . . . ?
C24 C23 C18 C19 -179.35(9) . . . . ?
C22 C23 C18 C17 168.43(9) . . . . ?
C24 C23 C18 C17 -4.19(15) . . . . ?
C24 C25 C12 C11 161.38(10) . . . . ?
C26 C25 C12 C11 -18.02(15) . . . . ?
C24 C25 C12 C13 -16.98(15) . . . . ?
C26 C25 C12 C13 163.62(10) . . . . ?
C6 C5 C4 C3 4.22(16) . . . . ?
C28 C5 C4 C3 -173.80(10) . . . . ?
C2 C3 C4 C5 -3.63(16) . . . . ?
C1 C6 C7 C8 -4.98(16) . . . . ?
C5 C6 C7 C8 171.29(11) . . . . ?
C25 C24 C15 C14 -13.23(15) . . . . ?
C23 C24 C15 C14 161.42(10) . . . . ?
C25 C24 C15 C16 170.31(10) . . . . ?
C23 C24 C15 C16 -15.04(15) . . . . ?
C22 C21 C20 C19 -3.55(17) . . . . ?
C24 C15 C16 C17 4.96(17) . . . . ?
C14 C15 C16 C17 -171.48(11) . . . . ?
C15 C16 C17 C18 6.05(17) . . . . ?
C19 C18 C17 C16 168.81(11) . . . . ?
C23 C18 C17 C16 -6.29(16) . . . . ?
C25 C12 C11 C10 0.80(16) . . . . ?
C13 C12 C11 C10 179.14(11) . . . . ?
C24 C15 C14 C13 -2.52(17) . . . . ?
C16 C15 C14 C13 173.94(11) . . . . ?
C4 C5 C28 O2 176.67(12) . . . . ?
C6 C5 C28 O2 -1.2(2) . . . . ?
C21 C20 C19 C18 0.96(17) . . . . ?
C23 C18 C19 C20 4.26(16) . . . . ?
C17 C18 C19 C20 -170.84(11) . . . . ?
C6 C7 C8 C9 8.54(18) . . . . ?
C26 C9 C8 C7 2.10(17) . . . . ?
C10 C9 C8 C7 -177.83(11) . . . . ?
C15 C14 C13 C12 8.54(17) . . . . ?
C25 C12 C13 C14 1.52(17) . . . . ?
C11 C12 C13 C14 -176.82(11) . . . . ?
C12 C11 C10 C9 10.15(17) . . . . ?
C26 C9 C10 C11 -3.28(16) . . . . ?
C8 C9 C10 C11 176.65(11) . . . . ?

_refine_diff_density_max         0.235
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.043

####################################################################### 
# 
# 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_JWVS210111_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2092869'
loop_
_audit_author_name
_audit_author_address
'Nathalie GRUBER'
;CNRS and Universite de Strasbourg
France
;
_audit_update_record             
;
2022-03-07 deposited with the CCDC.	2022-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H19 Br O2'
_chemical_formula_sum            'C28 H19 Br O2'
_chemical_formula_weight         467.34

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

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

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

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

_cell_length_a                   14.6897(5)
_cell_length_b                   14.0457(6)
_cell_length_c                   20.6528(7)
_cell_angle_alpha                90
_cell_angle_beta                 104.4410(10)
_cell_angle_gamma                90
_cell_volume                     4126.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9670
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      27.89

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_F_000             1904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.016
_shelx_estimated_absorpt_T_min   0.689
_shelx_estimated_absorpt_T_max   0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6577
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            91304
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.036
_diffrn_reflns_theta_max         27.924
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9892
_reflns_number_gt                8445
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0339P)²+3.7757P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9892
_refine_ls_number_parameters     563
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0709
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.004
_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
C1 C 0.78280(11) 0.34557(12) 0.55939(8) 0.0134(3) Uani 1 1 d . . . . .
C2 C 0.87211(11) 0.30183(12) 0.58490(8) 0.0135(3) Uani 1 1 d . . . . .
C3 C 0.88982(11) 0.25500(13) 0.64529(8) 0.0169(3) Uani 1 1 d . . . . .
C4 C 0.82500(12) 0.25044(13) 0.68487(8) 0.0179(3) Uani 1 1 d . . . . .
H4 H 0.838500 0.215112 0.725370 0.021 Uiso 1 1 calc R U . . .
C5 C 0.74152(12) 0.29845(13) 0.66344(8) 0.0165(3) Uani 1 1 d . . . . .
C6 C 0.72067(11) 0.35019(12) 0.60216(8) 0.0142(3) Uani 1 1 d . . . . .
C7 C 0.64181(12) 0.41335(13) 0.58730(9) 0.0177(3) Uani 1 1 d . . . . .
H7 H 0.598097 0.413267 0.614319 0.021 Uiso 1 1 calc R U . . .
C8 C 0.62989(11) 0.47299(13) 0.53471(9) 0.0171(3) Uani 1 1 d . . . . .
H8 H 0.583388 0.521398 0.528960 0.021 Uiso 1 1 calc R U . . .
C9 C 0.68584(12) 0.46483(12) 0.48744(8) 0.0155(3) Uani 1 1 d . . . . .
C10 C 0.67048(12) 0.53010(13) 0.43322(9) 0.0192(3) Uani 1 1 d . . . . .
H10 H 0.622213 0.576566 0.428110 0.023 Uiso 1 1 calc R U . . .
C11 C 0.72442(13) 0.52632(13) 0.38878(9) 0.0196(3) Uani 1 1 d . . . . .
H11 H 0.719792 0.575383 0.356454 0.024 Uiso 1 1 calc R U . . .
C12 C 0.78778(12) 0.44965(13) 0.39015(8) 0.0169(3) Uani 1 1 d . . . . .
C13 C 0.84471(12) 0.44855(13) 0.34338(8) 0.0192(3) Uani 1 1 d . . . . .
H13 H 0.838807 0.498199 0.311359 0.023 Uiso 1 1 calc R U . . .
C14 C 0.90701(12) 0.37738(14) 0.34427(8) 0.0195(4) Uani 1 1 d . . . . .
H14 H 0.951810 0.382502 0.318282 0.023 Uiso 1 1 calc R U . . .
C15 C 0.90570(12) 0.29470(13) 0.38405(8) 0.0166(3) Uani 1 1 d . . . . .
C16 C 0.96567(12) 0.21611(14) 0.37916(9) 0.0210(4) Uani 1 1 d . . . . .
H16 H 1.010575 0.222551 0.353360 0.025 Uiso 1 1 calc R U . . .
C17 C 0.95945(12) 0.13282(14) 0.41068(9) 0.0212(4) Uani 1 1 d . . . . .
H17 H 1.003546 0.083484 0.410286 0.025 Uiso 1 1 calc R U . . .
C18 C 0.88658(12) 0.11883(13) 0.44462(8) 0.0177(3) Uani 1 1 d . . . . .
C19 C 0.87271(13) 0.02828(13) 0.47052(9) 0.0211(4) Uani 1 1 d . . . . .
H19 H 0.916109 -0.021528 0.469547 0.025 Uiso 1 1 calc R U . . .
C20 C 0.79734(13) 0.01141(13) 0.49705(9) 0.0218(4) Uani 1 1 d . . . . .
H20 H 0.790441 -0.048646 0.516445 0.026 Uiso 1 1 calc R U . . .
C21 C 0.73055(13) 0.08343(13) 0.49535(9) 0.0205(4) Uani 1 1 d . . . . .
H21 H 0.675778 0.070360 0.510406 0.025 Uiso 1 1 calc R U . . .
C22 C 0.74382(12) 0.17288(13) 0.47202(8) 0.0169(3) Uani 1 1 d . . . . .
H22 H 0.697862 0.220742 0.471221 0.020 Uiso 1 1 calc R U . . .
C23 C 0.82451(11) 0.19498(12) 0.44920(8) 0.0147(3) Uani 1 1 d . . . . .
C24 C 0.84232(11) 0.28885(12) 0.42552(8) 0.0147(3) Uani 1 1 d . . . . .
C25 C 0.79489(11) 0.37486(12) 0.43772(8) 0.0145(3) Uani 1 1 d . . . . .
C26 C 0.75464(11) 0.39257(12) 0.49417(8) 0.0136(3) Uani 1 1 d . . . . .
O1 O 0.94253(8) 0.30734(8) 0.55186(6) 0.0144(2) Uani 1 1 d . . . . .
C27 C 0.98439(12) 0.39991(13) 0.55512(10) 0.0224(4) Uani 1 1 d . . . . .
H27A H 0.935615 0.447252 0.537184 0.034 Uiso 1 1 calc R U . . .
H27B H 1.031262 0.400416 0.528666 0.034 Uiso 1 1 calc R U . . .
H27C H 1.014917 0.415374 0.601754 0.034 Uiso 1 1 calc R U . . .
Br1 Br 1.00749(2) 0.19373(2) 0.67886(2) 0.02717(6) Uani 1 1 d . . . . .
O2 O 0.67376(9) 0.30244(10) 0.69832(6) 0.0214(3) Uani 1 1 d . . . . .
C28 C 0.69728(13) 0.26522(15) 0.76501(9) 0.0236(4) Uani 1 1 d . . . . .
H28A H 0.708659 0.196582 0.763653 0.035 Uiso 1 1 calc R U . . .
H28B H 0.645193 0.276805 0.785812 0.035 Uiso 1 1 calc R U . . .
H28C H 0.754082 0.296802 0.791198 0.035 Uiso 1 1 calc R U . . .
C29 C 0.29080(11) 0.18347(12) 0.87065(8) 0.0146(3) Uani 1 1 d . . . . .
C30 C 0.37437(11) 0.23422(12) 0.90091(8) 0.0153(3) Uani 1 1 d . . . . .
C31 C 0.38083(12) 0.27802(13) 0.96141(9) 0.0188(3) Uani 1 1 d . . . . .
C32 C 0.31020(12) 0.27210(13) 0.99599(9) 0.0193(3) Uani 1 1 d . . . . .
H32 H 0.315502 0.306278 1.036459 0.023 Uiso 1 1 calc R U . . .
C33 C 0.23335(12) 0.21607(12) 0.97030(8) 0.0161(3) Uani 1 1 d . . . . .
C34 C 0.22401(12) 0.16711(12) 0.90865(8) 0.0156(3) Uani 1 1 d . . . . .
C35 C 0.15133(12) 0.09838(13) 0.88620(9) 0.0185(3) Uani 1 1 d . . . . .
H35 H 0.104401 0.090020 0.910105 0.022 Uiso 1 1 calc R U . . .
C36 C 0.14872(12) 0.04511(13) 0.83123(9) 0.0209(4) Uani 1 1 d . . . . .
H36 H 0.105693 -0.006440 0.820629 0.025 Uiso 1 1 calc R U . . .
C37 C 0.20989(12) 0.06531(13) 0.78878(9) 0.0192(3) Uani 1 1 d . . . . .
C38 C 0.20904(14) 0.00809(14) 0.73152(9) 0.0241(4) Uani 1 1 d . . . . .
H38 H 0.165638 -0.043046 0.720248 0.029 Uiso 1 1 calc R U . . .
C39 C 0.26978(14) 0.02611(14) 0.69296(9) 0.0250(4) Uani 1 1 d . . . . .
H39 H 0.276220 -0.018515 0.659820 0.030 Uiso 1 1 calc R U . . .
C40 C 0.32387(13) 0.11156(13) 0.70195(8) 0.0200(4) Uani 1 1 d . . . . .
C41 C 0.38801(13) 0.13269(14) 0.66218(9) 0.0237(4) Uani 1 1 d . . . . .
H41 H 0.395391 0.088779 0.628876 0.028 Uiso 1 1 calc R U . . .
C42 C 0.43859(13) 0.21454(15) 0.67124(9) 0.0235(4) Uani 1 1 d . . . . .
H42 H 0.487136 0.223456 0.648852 0.028 Uiso 1 1 calc R U . . .
C43 C 0.41941(12) 0.28735(13) 0.71415(8) 0.0190(3) Uani 1 1 d . . . . .
C44 C 0.46989(12) 0.37522(15) 0.72249(9) 0.0233(4) Uani 1 1 d . . . . .
H44 H 0.519287 0.383979 0.700875 0.028 Uiso 1 1 calc R U . . .
C45 C 0.44882(13) 0.44624(15) 0.76053(9) 0.0248(4) Uani 1 1 d . . . . .
H45 H 0.487789 0.501099 0.769354 0.030 Uiso 1 1 calc R U . . .
C46 C 0.36848(13) 0.43954(13) 0.78759(9) 0.0206(4) Uani 1 1 d . . . . .
C47 C 0.33839(16) 0.51809(14) 0.81985(10) 0.0278(4) Uani 1 1 d . . . . .
H47 H 0.376204 0.573769 0.828432 0.033 Uiso 1 1 calc R U . . .
C48 C 0.25549(16) 0.51495(14) 0.83888(10) 0.0288(4) Uani 1 1 d . . . . .
H48 H 0.237067 0.567357 0.861778 0.035 Uiso 1 1 calc R U . . .
C49 C 0.19800(14) 0.43419(14) 0.82445(9) 0.0245(4) Uani 1 1 d . . . . .
H49 H 0.138814 0.433597 0.835256 0.029 Uiso 1 1 calc R U . . .
C50 C 0.22650(12) 0.35572(13) 0.79478(9) 0.0183(3) Uani 1 1 d . . . . .
H50 H 0.186461 0.301732 0.785031 0.022 Uiso 1 1 calc R U . . .
C51 C 0.31478(12) 0.35426(12) 0.77854(8) 0.0160(3) Uani 1 1 d . . . . .
C52 C 0.34912(11) 0.27250(13) 0.74894(8) 0.0155(3) Uani 1 1 d . . . . .
C53 C 0.31447(12) 0.17706(13) 0.75210(8) 0.0163(3) Uani 1 1 d . . . . .
C54 C 0.27185(11) 0.14332(12) 0.80357(8) 0.0155(3) Uani 1 1 d . . . . .
O3 O 0.44865(8) 0.24154(9) 0.87172(6) 0.0181(2) Uani 1 1 d . . . . .
C55 C 0.50425(14) 0.15697(16) 0.87692(12) 0.0317(5) Uani 1 1 d . . . . .
H55A H 0.531367 0.142187 0.924174 0.048 Uiso 1 1 calc R U . . .
H55B H 0.554916 0.166885 0.854466 0.048 Uiso 1 1 calc R U . . .
H55C H 0.464573 0.103897 0.855674 0.048 Uiso 1 1 calc R U . . .
Br2 Br 0.49010(2) 0.34882(2) 1.00137(2) 0.03618(7) Uani 1 1 d . . . . .
O4 O 0.16214(9) 0.20227(10) 1.00090(6) 0.0214(3) Uani 1 1 d . . . . .
C56 C 0.16833(14) 0.25432(14) 1.06161(10) 0.0255(4) Uani 1 1 d . . . . .
H56A H 0.222357 0.231467 1.096193 0.038 Uiso 1 1 calc R U . . .
H56B H 0.110634 0.244805 1.076488 0.038 Uiso 1 1 calc R U . . .
H56C H 0.176211 0.322246 1.053620 0.038 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
C1 C6 1.421(2) . ?
C1 C2 1.425(2) . ?
C1 C26 1.464(2) . ?
C2 C3 1.376(2) . ?
C2 O1 1.3762(19) . ?
C3 C4 1.403(2) . ?
C3 Br1 1.9003(16) . ?
C4 C5 1.373(2) . ?
C4 H4 0.9500 . ?
C5 O2 1.368(2) . ?
C5 C6 1.425(2) . ?
C6 C7 1.430(2) . ?
C7 C8 1.348(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.429(2) . ?
C8 H8 0.9500 . ?
C9 C26 1.415(2) . ?
C9 C10 1.421(2) . ?
C10 C11 1.355(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.419(3) . ?
C11 H11 0.9500 . ?
C12 C25 1.424(2) . ?
C12 C13 1.427(2) . ?
C13 C14 1.352(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.425(2) . ?
C14 H14 0.9500 . ?
C15 C24 1.416(2) . ?
C15 C16 1.431(3) . ?
C16 C17 1.353(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.432(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.414(3) . ?
C18 C23 1.424(2) . ?
C19 C20 1.373(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.404(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.377(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.415(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.453(2) . ?
C24 C25 1.448(2) . ?
C25 C26 1.454(2) . ?
O1 C27 1.433(2) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O2 C28 1.433(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C34 1.420(2) . ?
C29 C30 1.422(2) . ?
C29 C54 1.457(2) . ?
C30 C31 1.375(2) . ?
C30 O3 1.3757(19) . ?
C31 C32 1.401(2) . ?
C31 Br2 1.8936(17) . ?
C32 C33 1.370(2) . ?
C32 H32 0.9500 . ?
C33 O4 1.3642(19) . ?
C33 C34 1.423(2) . ?
C34 C35 1.428(2) . ?
C35 C36 1.352(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.432(2) . ?
C36 H36 0.9500 . ?
C37 C54 1.408(2) . ?
C37 C38 1.427(3) . ?
C38 C39 1.360(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.426(3) . ?
C39 H39 0.9500 . ?
C40 C53 1.418(2) . ?
C40 C41 1.427(3) . ?
C41 C42 1.356(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.427(3) . ?
C42 H42 0.9500 . ?
C43 C52 1.413(2) . ?
C43 C44 1.428(3) . ?
C44 C45 1.353(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.429(3) . ?
C45 H45 0.9500 . ?
C46 C47 1.415(3) . ?
C46 C51 1.421(3) . ?
C47 C48 1.370(3) . ?
C47 H47 0.9500 . ?
C48 C49 1.401(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.376(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.418(2) . ?
C50 H50 0.9500 . ?
C51 C52 1.449(2) . ?
C52 C53 1.441(2) . ?
C53 C54 1.442(2) . ?
O3 C55 1.430(2) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
O4 C56 1.435(2) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 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
C6 C1 C2 117.68(14) . . ?
C6 C1 C26 118.25(14) . . ?
C2 C1 C26 123.87(14) . . ?
C3 C2 O1 118.73(14) . . ?
C3 C2 C1 119.31(15) . . ?
O1 C2 C1 121.93(14) . . ?
C2 C3 C4 123.20(15) . . ?
C2 C3 Br1 119.76(12) . . ?
C4 C3 Br1 117.04(12) . . ?
C5 C4 C3 118.13(15) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
O2 C5 C4 124.02(15) . . ?
O2 C5 C6 115.05(15) . . ?
C4 C5 C6 120.92(15) . . ?
C1 C6 C5 119.98(15) . . ?
C1 C6 C7 120.42(15) . . ?
C5 C6 C7 119.35(15) . . ?
C8 C7 C6 119.59(15) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 121.29(16) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C26 C9 C10 120.63(15) . . ?
C26 C9 C8 120.60(15) . . ?
C10 C9 C8 118.77(16) . . ?
C11 C10 C9 120.25(16) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.51(16) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C25 120.56(15) . . ?
C11 C12 C13 119.14(16) . . ?
C25 C12 C13 120.30(16) . . ?
C14 C13 C12 120.51(16) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 120.25(16) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C24 C15 C14 120.08(16) . . ?
C24 C15 C16 120.47(16) . . ?
C14 C15 C16 119.38(16) . . ?
C17 C16 C15 121.08(16) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 120.18(17) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C19 C18 C23 119.70(16) . . ?
C19 C18 C17 120.30(16) . . ?
C23 C18 C17 119.91(16) . . ?
C20 C19 C18 120.85(17) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 119.60(17) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C22 C21 C20 120.48(16) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 121.35(16) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C22 C23 C18 117.44(16) . . ?
C22 C23 C24 123.20(15) . . ?
C18 C23 C24 119.17(15) . . ?
C15 C24 C25 118.33(15) . . ?
C15 C24 C23 117.20(15) . . ?
C25 C24 C23 124.33(15) . . ?
C12 C25 C24 116.81(15) . . ?
C12 C25 C26 116.90(15) . . ?
C24 C25 C26 126.29(15) . . ?
C9 C26 C25 117.86(15) . . ?
C9 C26 C1 116.42(14) . . ?
C25 C26 C1 125.62(15) . . ?
C2 O1 C27 113.23(13) . . ?
O1 C27 H27A 109.5 . . ?
O1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C5 O2 C28 117.31(13) . . ?
O2 C28 H28A 109.5 . . ?
O2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C34 C29 C30 118.56(15) . . ?
C34 C29 C54 117.94(15) . . ?
C30 C29 C54 123.44(15) . . ?
C31 C30 O3 118.84(15) . . ?
C31 C30 C29 118.68(15) . . ?
O3 C30 C29 122.48(15) . . ?
C30 C31 C32 123.01(16) . . ?
C30 C31 Br2 119.35(13) . . ?
C32 C31 Br2 117.64(13) . . ?
C33 C32 C31 118.69(16) . . ?
C33 C32 H32 120.7 . . ?
C31 C32 H32 120.7 . . ?
O4 C33 C32 123.73(16) . . ?
O4 C33 C34 115.58(15) . . ?
C32 C33 C34 120.69(15) . . ?
C29 C34 C33 119.38(15) . . ?
C29 C34 C35 119.58(16) . . ?
C33 C34 C35 120.96(15) . . ?
C36 C35 C34 120.60(16) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C37 120.91(17) . . ?
C35 C36 H36 119.5 . . ?
C37 C36 H36 119.5 . . ?
C54 C37 C38 119.31(16) . . ?
C54 C37 C36 119.45(16) . . ?
C38 C37 C36 121.24(17) . . ?
C39 C38 C37 120.60(18) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C38 C39 C40 120.41(17) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C53 C40 C39 119.26(17) . . ?
C53 C40 C41 118.96(17) . . ?
C39 C40 C41 121.78(17) . . ?
C42 C41 C40 120.97(17) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C43 120.47(17) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
C52 C43 C42 119.52(17) . . ?
C52 C43 C44 119.32(17) . . ?
C42 C43 C44 121.16(16) . . ?
C45 C44 C43 121.35(17) . . ?
C45 C44 H44 119.3 . . ?
C43 C44 H44 119.3 . . ?
C44 C45 C46 120.62(18) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 H45 119.7 . . ?
C47 C46 C51 119.39(17) . . ?
C47 C46 C45 121.19(18) . . ?
C51 C46 C45 119.32(17) . . ?
C48 C47 C46 120.93(19) . . ?
C48 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
C47 C48 C49 119.77(18) . . ?
C47 C48 H48 120.1 . . ?
C49 C48 H48 120.1 . . ?
C50 C49 C48 120.59(18) . . ?
C50 C49 H49 119.7 . . ?
C48 C49 H49 119.7 . . ?
C49 C50 C51 120.97(18) . . ?
C49 C50 H50 119.5 . . ?
C51 C50 H50 119.5 . . ?
C50 C51 C46 117.85(16) . . ?
C50 C51 C52 123.10(16) . . ?
C46 C51 C52 118.90(15) . . ?
C43 C52 C53 118.14(16) . . ?
C43 C52 C51 118.22(16) . . ?
C53 C52 C51 123.64(15) . . ?
C40 C53 C52 118.08(15) . . ?
C40 C53 C54 117.70(16) . . ?
C52 C53 C54 124.22(15) . . ?
C37 C54 C53 118.15(16) . . ?
C37 C54 C29 117.86(15) . . ?
C53 C54 C29 123.97(15) . . ?
C30 O3 C55 113.93(14) . . ?
O3 C55 H55A 109.5 . . ?
O3 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
O3 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C33 O4 C56 116.35(14) . . ?
O4 C56 H56A 109.5 . . ?
O4 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
O4 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

_refine_diff_density_max         0.749
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_ea
_database_code_depnum_ccdc_archive 'CCDC 2157003'
loop_
_audit_author_name
_audit_author_address
'Nathalie GRUBER'
;CNRS and Universite de Strasbourg
France
;
_audit_update_record             
;
2022-03-07 deposited with the CCDC.	2022-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H80 N4 O2, solvent'
_chemical_formula_sum            'C84 H80 N4 O2, solvent'
_chemical_formula_weight         1177.52

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'

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

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

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

_cell_length_a                   13.2857(5)
_cell_length_b                   15.5135(6)
_cell_length_c                   35.8022(15)
_cell_angle_alpha                90
_cell_angle_beta                 95.347(2)
_cell_angle_gamma                90
_cell_volume                     7347.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9191
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      66.33

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_F_000             2512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.485
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6091
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   none
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            86405
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.479
_diffrn_reflns_theta_max         66.731
_diffrn_reflns_theta_full        66.731
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             12979
_reflns_number_gt                10278
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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-2018/3 (Sheldrick, 2018)'
_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=exp[0.0801(sinθ/λ)²)]/[σ²(Fo²)+(0.1522P)²+0.0379P-0.0014+0.0292sinθ/λ] where P=(0.0193Fo²+0.9807Fc²)'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12979
_refine_ls_number_parameters     859
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.2271
_refine_ls_wR_factor_gt          0.2214
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_restrained_S_all      1.217
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.62711(13) 0.59045(11) 0.62708(5) 0.0395(4) Uani 1 1 d . . . . .
H1 H 0.576059 0.610872 0.638359 0.047 Uiso 1 1 calc R U . . .
N2 N 0.44193(13) 0.52525(11) 0.65116(5) 0.0390(4) Uani 1 1 d . . . . .
N3 N 0.38237(13) 0.69514(11) 0.67677(5) 0.0419(4) Uani 1 1 d . . . . .
H3A H 0.435916 0.673284 0.667520 0.050 Uiso 1 1 calc R U . . .
N4 N 0.56656(13) 0.76215(11) 0.65214(5) 0.0408(4) Uani 1 1 d . . . . .
C1 C 0.70620(15) 0.63869(14) 0.61668(6) 0.0418(5) Uani 1 1 d . . . . .
C2 C 0.77215(16) 0.58014(15) 0.59993(6) 0.0469(5) Uani 1 1 d . . . . .
H2 H 0.833537 0.595087 0.589898 0.056 Uiso 1 1 calc R U . . .
C3 C 0.73237(16) 0.49998(15) 0.60079(6) 0.0455(5) Uani 1 1 d . . . . .
H3 H 0.761523 0.448887 0.591909 0.055 Uiso 1 1 calc R U . . .
C4 C 0.63889(16) 0.50555(13) 0.61738(6) 0.0401(4) Uani 1 1 d . . . . .
C5 C 0.56961(15) 0.43935(13) 0.62196(6) 0.0397(4) Uani 1 1 d . . . . .
C6 C 0.47657(15) 0.45026(13) 0.63642(6) 0.0391(4) Uani 1 1 d . . . . .
C7 C 0.39927(17) 0.38384(14) 0.63538(6) 0.0454(5) Uani 1 1 d . . . . .
H7 H 0.404704 0.326698 0.626245 0.055 Uiso 1 1 calc R U . . .
C8 C 0.31899(17) 0.41836(14) 0.64973(6) 0.0460(5) Uani 1 1 d . . . . .
H8 H 0.256514 0.390522 0.652649 0.055 Uiso 1 1 calc R U . . .
C9 C 0.34565(16) 0.50633(14) 0.65995(6) 0.0406(4) Uani 1 1 d . . . . .
C10 C 0.27954(15) 0.56219(14) 0.67626(6) 0.0418(5) Uani 1 1 d . . . . .
C11 C 0.29804(16) 0.64951(14) 0.68396(6) 0.0433(5) Uani 1 1 d . . . . .
C12 C 0.23089(17) 0.70886(15) 0.69898(7) 0.0496(5) Uani 1 1 d . . . . .
H12 H 0.166359 0.695306 0.706813 0.059 Uiso 1 1 calc R U . . .
C13 C 0.27401(17) 0.78742(16) 0.70026(7) 0.0497(5) Uani 1 1 d . . . . .
H13 H 0.245105 0.838755 0.709017 0.060 Uiso 1 1 calc R U . . .
C14 C 0.37071(16) 0.78027(14) 0.68618(6) 0.0423(5) Uani 1 1 d . . . . .
C15 C 0.43868(16) 0.84720(13) 0.68158(6) 0.0414(5) Uani 1 1 d . . . . .
C16 C 0.52995(16) 0.83790(13) 0.66541(6) 0.0400(4) Uani 1 1 d . . . . .
C17 C 0.59836(17) 0.90864(14) 0.65967(6) 0.0462(5) Uani 1 1 d . . . . .
H17 H 0.590260 0.967087 0.666720 0.055 Uiso 1 1 calc R U . . .
C18 C 0.67510(17) 0.87570(14) 0.64251(7) 0.0477(5) Uani 1 1 d . . . . .
H18 H 0.731551 0.906339 0.634832 0.057 Uiso 1 1 calc R U . . .
C19 C 0.65525(16) 0.78389(14) 0.63793(6) 0.0414(5) Uani 1 1 d . . . . .
C20 C 0.71995(16) 0.72719(14) 0.62087(6) 0.0417(5) Uani 1 1 d . . . . .
C21 C 0.59773(15) 0.34943(13) 0.61115(6) 0.0403(4) Uani 1 1 d . . . . .
C22 C 0.60910(17) 0.28742(14) 0.64001(6) 0.0451(5) Uani 1 1 d . . . . .
H22 H 0.606600 0.304418 0.665395 0.054 Uiso 1 1 calc R U . . .
C23 C 0.62376(18) 0.20258(15) 0.63137(7) 0.0500(5) Uani 1 1 d . . . . .
C24 C 0.63078(18) 0.17663(15) 0.59368(7) 0.0516(5) Uani 1 1 d . . . . .
C25 C 0.6343(2) 0.08681(17) 0.58494(9) 0.0652(7) Uani 1 1 d . . . . .
H25 H 0.645494 0.045410 0.604439 0.078 Uiso 1 1 calc R U . . .
C26 C 0.6216(2) 0.06126(18) 0.54869(9) 0.0713(8) Uani 1 1 d . . . . .
H26 H 0.617737 0.001374 0.543189 0.086 Uiso 1 1 calc R U . . .
C27 C 0.6139(2) 0.12112(19) 0.51865(8) 0.0633(7) Uani 1 1 d . . . . .
C28 C 0.5841(2) 0.0932(2) 0.48163(10) 0.0779(9) Uani 1 1 d . . . . .
H28 H 0.576429 0.033516 0.476215 0.093 Uiso 1 1 calc R U . . .
C29 C 0.5661(2) 0.1536(3) 0.45344(9) 0.0815(10) Uani 1 1 d . . . . .
H29 H 0.532113 0.136736 0.430061 0.098 Uiso 1 1 calc R U . . .
C30 C 0.59707(19) 0.2382(2) 0.45877(7) 0.0678(8) Uani 1 1 d . . . . .
C31 C 0.5850(2) 0.2980(3) 0.42882(8) 0.0806(10) Uani 1 1 d . . . . .
H31 H 0.548145 0.281603 0.405900 0.097 Uiso 1 1 calc R U . . .
C32 C 0.6248(3) 0.3777(3) 0.43229(8) 0.0853(11) Uani 1 1 d . . . . .
H32 H 0.608690 0.418916 0.413051 0.102 Uiso 1 1 calc R U . . .
C33 C 0.6906(2) 0.4011(2) 0.46431(7) 0.0655(7) Uani 1 1 d . . . . .
C34 C 0.7431(3) 0.4813(2) 0.46487(9) 0.0770(9) Uani 1 1 d . . . . .
H34 H 0.726426 0.521949 0.445409 0.092 Uiso 1 1 calc R U . . .
C35 C 0.8159(2) 0.5010(2) 0.49245(9) 0.0708(8) Uani 1 1 d . . . . .
H35 H 0.846240 0.556472 0.493243 0.085 Uiso 1 1 calc R U . . .
C36 C 0.8473(2) 0.43862(18) 0.52032(8) 0.0607(6) Uani 1 1 d . . . . .
C37 C 0.9341(2) 0.4540(2) 0.54478(9) 0.0664(7) Uani 1 1 d . . . . .
H37 H 0.967439 0.508013 0.544055 0.080 Uiso 1 1 calc R U . . .
C38 C 0.9717(2) 0.3923(2) 0.56974(8) 0.0675(7) Uani 1 1 d . . . . .
H38 H 1.029967 0.403669 0.586459 0.081 Uiso 1 1 calc R U . . .
C39 C 0.92335(19) 0.3126(2) 0.57025(7) 0.0604(6) Uani 1 1 d . . . . .
H39 H 0.950253 0.268926 0.586924 0.072 Uiso 1 1 calc R U . . .
C40 C 0.83700(18) 0.29625(17) 0.54690(6) 0.0516(5) Uani 1 1 d . . . . .
H40 H 0.805443 0.241439 0.547832 0.062 Uiso 1 1 calc R U . . .
C41 C 0.79450(18) 0.35883(17) 0.52171(6) 0.0524(6) Uani 1 1 d . . . . .
C42 C 0.70800(18) 0.34227(17) 0.49481(6) 0.0534(6) Uani 1 1 d . . . . .
C43 C 0.64604(18) 0.26530(18) 0.49434(7) 0.0559(6) Uani 1 1 d . . . . .
C44 C 0.63147(18) 0.21045(16) 0.52608(7) 0.0521(6) Uani 1 1 d . . . . .
C45 C 0.62688(16) 0.23923(15) 0.56453(6) 0.0462(5) Uani 1 1 d . . . . .
C46 C 0.60535(16) 0.32639(14) 0.57467(6) 0.0433(5) Uani 1 1 d . . . . .
O1 O 0.62864(16) 0.13742(11) 0.65728(5) 0.0655(5) Uani 1 1 d . . . . .
C47 C 0.6001(3) 0.15839(19) 0.69369(8) 0.0725(8) Uani 1 1 d . . . . .
H47A H 0.652020 0.195180 0.706762 0.109 Uiso 1 1 calc R U . . .
H47B H 0.593345 0.105298 0.708082 0.109 Uiso 1 1 calc R U . . .
H47C H 0.535342 0.189076 0.691211 0.109 Uiso 1 1 calc R U . . .
O2 O 0.58615(12) 0.38848(10) 0.54712(4) 0.0479(4) Uani 1 1 d . . . . .
C48 C 0.4853(2) 0.38790(19) 0.53019(8) 0.0622(6) Uani 1 1 d . . . . .
H48A H 0.469756 0.331131 0.519092 0.093 Uiso 1 1 calc R U . . .
H48B H 0.477562 0.432044 0.510548 0.093 Uiso 1 1 calc R U . . .
H48C H 0.438756 0.400114 0.549219 0.093 Uiso 1 1 calc R U . . .
C49 C 0.18023(16) 0.52514(14) 0.68527(6) 0.0429(5) Uani 1 1 d . . . . .
C50 C 0.17352(17) 0.48109(15) 0.71913(6) 0.0466(5) Uani 1 1 d . . . . .
C51 C 0.08498(17) 0.43756(16) 0.72460(6) 0.0495(5) Uani 1 1 d . . . . .
H51 H 0.080914 0.407473 0.747519 0.059 Uiso 1 1 calc R U . . .
C52 C 0.00198(16) 0.43606(16) 0.69801(6) 0.0477(5) Uani 1 1 d . . . . .
C53 C 0.00862(17) 0.48548(16) 0.66578(6) 0.0485(5) Uani 1 1 d . . . . .
H53 H -0.048906 0.489264 0.647995 0.058 Uiso 1 1 calc R U . . .
C54 C 0.09569(17) 0.52927(14) 0.65865(6) 0.0454(5) Uani 1 1 d . . . . .
C55 C 0.2600(2) 0.47959(19) 0.74942(7) 0.0621(7) Uani 1 1 d . . . . .
H55A H 0.323655 0.471745 0.738055 0.093 Uiso 1 1 calc R U . . .
H55B H 0.250611 0.431866 0.766691 0.093 Uiso 1 1 calc R U . . .
H55C H 0.261950 0.534185 0.763238 0.093 Uiso 1 1 calc R U . . .
C56 C -0.09259(18) 0.38205(18) 0.70246(7) 0.0570(6) Uani 1 1 d . . . . .
C57 C -0.0804(2) 0.3251(2) 0.73705(9) 0.0797(9) Uani 1 1 d . . . . .
H57A H -0.070300 0.361190 0.759540 0.120 Uiso 1 1 calc R U . . .
H57B H -0.021642 0.287330 0.735716 0.120 Uiso 1 1 calc R U . . .
H57C H -0.141245 0.289872 0.738219 0.120 Uiso 1 1 calc R U . . .
C58 C -0.1128(2) 0.32263(19) 0.66832(8) 0.0653(7) Uani 1 1 d . . . . .
H58A H -0.171566 0.286178 0.671598 0.098 Uiso 1 1 calc R U . . .
H58B H -0.053487 0.286164 0.665948 0.098 Uiso 1 1 calc R U . . .
H58C H -0.126221 0.357590 0.645601 0.098 Uiso 1 1 calc R U . . .
C59 C -0.1845(2) 0.4409(2) 0.70456(9) 0.0737(8) Uani 1 1 d . . . . .
H59A H -0.194087 0.476054 0.681763 0.110 Uiso 1 1 calc R U . . .
H59B H -0.173213 0.478688 0.726499 0.110 Uiso 1 1 calc R U . . .
H59C H -0.244830 0.405685 0.706782 0.110 Uiso 1 1 calc R U . . .
C60 C 0.1005(2) 0.57902(18) 0.62257(7) 0.0585(6) Uani 1 1 d . . . . .
H60A H 0.117712 0.639278 0.628383 0.088 Uiso 1 1 calc R U . . .
H60B H 0.034719 0.576354 0.607783 0.088 Uiso 1 1 calc R U . . .
H60C H 0.152319 0.553687 0.608153 0.088 Uiso 1 1 calc R U . . .
C61 C 0.40622(16) 0.93481(14) 0.69361(6) 0.0427(5) Uani 1 1 d . . . . .
C62 C 0.41654(16) 0.95768(14) 0.73153(6) 0.0438(5) Uani 1 1 d . . . . .
C63 C 0.37822(19) 1.03642(15) 0.74239(7) 0.0504(5) Uani 1 1 d . . . . .
H63 H 0.387418 1.052582 0.768079 0.061 Uiso 1 1 calc R U . . .
C64 C 0.32726(19) 1.09176(15) 0.71698(7) 0.0529(6) Uani 1 1 d . . . . .
C65 C 0.3207(2) 1.06939(17) 0.67904(8) 0.0606(6) Uani 1 1 d . . . . .
H65 H 0.288376 1.107747 0.661028 0.073 Uiso 1 1 calc R U . . .
C66 C 0.3603(2) 0.99217(16) 0.66699(7) 0.0554(6) Uani 1 1 d . . . . .
C67 C 0.4653(2) 0.89746(17) 0.76066(7) 0.0580(6) Uani 1 1 d . . . . .
H67A H 0.421590 0.847236 0.762993 0.087 Uiso 1 1 calc R U . . .
H67B H 0.475289 0.927349 0.784833 0.087 Uiso 1 1 calc R U . . .
H67C H 0.530835 0.878500 0.753156 0.087 Uiso 1 1 calc R U . . .
C68 C 0.2801(2) 1.17648(17) 0.72953(8) 0.0652(7) Uani 1 1 d . . . . .
C69 C 0.1692(5) 1.1640(4) 0.7288(3) 0.090(2) Uani 0.640(9) 1 d . . P A 1
H69A H 0.155112 1.117713 0.746192 0.135 Uiso 0.640(9) 1 calc R U P A 1
H69B H 0.141576 1.148620 0.703373 0.135 Uiso 0.640(9) 1 calc R U P A 1
H69C H 0.137817 1.217605 0.736448 0.135 Uiso 0.640(9) 1 calc R U P A 1
C70 C 0.3228(5) 1.2012(3) 0.76973(13) 0.0749(18) Uani 0.640(9) 1 d . . P A 1
H70A H 0.396767 1.202457 0.771183 0.112 Uiso 0.640(9) 1 calc R U P A 1
H70B H 0.301041 1.158607 0.787522 0.112 Uiso 0.640(9) 1 calc R U P A 1
H70C H 0.297502 1.258291 0.775973 0.112 Uiso 0.640(9) 1 calc R U P A 1
C71 C 0.3049(6) 1.2490(3) 0.70357(15) 0.0770(19) Uani 0.640(9) 1 d . . P A 1
H71A H 0.272704 1.302330 0.711072 0.116 Uiso 0.640(9) 1 calc R U P A 1
H71B H 0.279738 1.234498 0.677739 0.116 Uiso 0.640(9) 1 calc R U P A 1
H71C H 0.378328 1.257177 0.705119 0.116 Uiso 0.640(9) 1 calc R U P A 1
C69A C 0.2088(9) 1.2228(6) 0.6938(4) 0.107(5) Uani 0.360(9) 1 d . . P A 2
H69D H 0.186701 1.279774 0.701545 0.160 Uiso 0.360(9) 1 calc R U P A 2
H69E H 0.149504 1.186649 0.686810 0.160 Uiso 0.360(9) 1 calc R U P A 2
H69F H 0.248590 1.228843 0.672251 0.160 Uiso 0.360(9) 1 calc R U P A 2
C70A C 0.1939(16) 1.1542(9) 0.7564(6) 0.136(8) Uani 0.360(9) 1 d . . P A 2
H70D H 0.224578 1.126502 0.779351 0.203 Uiso 0.360(9) 1 calc R U P A 2
H70E H 0.144499 1.114959 0.743451 0.203 Uiso 0.360(9) 1 calc R U P A 2
H70F H 0.159924 1.207382 0.763003 0.203 Uiso 0.360(9) 1 calc R U P A 2
C71A C 0.3524(11) 1.2411(8) 0.7383(7) 0.146(10) Uani 0.360(9) 1 d . . P A 2
H71D H 0.407283 1.218019 0.755652 0.219 Uiso 0.360(9) 1 calc R U P A 2
H71E H 0.320647 1.289786 0.750135 0.219 Uiso 0.360(9) 1 calc R U P A 2
H71F H 0.379875 1.260726 0.715296 0.219 Uiso 0.360(9) 1 calc R U P A 2
C72 C 0.3536(3) 0.9725(2) 0.62544(8) 0.0822(10) Uani 1 1 d . . . . .
H72A H 0.308593 1.014252 0.611821 0.123 Uiso 1 1 calc R U . . .
H72B H 0.326871 0.914195 0.620980 0.123 Uiso 1 1 calc R U . . .
H72C H 0.421124 0.976430 0.616617 0.123 Uiso 1 1 calc R U . . .
C73 C 0.80951(17) 0.76447(14) 0.60430(7) 0.0472(5) Uani 1 1 d . . . . .
C74 C 0.90143(19) 0.77399(17) 0.62567(8) 0.0588(6) Uani 1 1 d . . . . .
C75 C 0.9831(2) 0.80812(19) 0.60794(10) 0.0704(8) Uani 1 1 d . . . . .
H75 H 1.045939 0.816383 0.622455 0.085 Uiso 1 1 calc R U . . .
C76 C 0.9758(2) 0.83008(18) 0.57031(10) 0.0742(9) Uani 1 1 d . . . . .
C77 C 0.8834(2) 0.8195(2) 0.55016(9) 0.0763(8) Uani 1 1 d . . . . .
H77 H 0.876499 0.834163 0.524285 0.092 Uiso 1 1 calc R U . . .
C78 C 0.8000(2) 0.7879(2) 0.56636(8) 0.0650(7) Uani 1 1 d . . . . .
C79 C 0.9134(2) 0.7496(3) 0.66608(9) 0.0841(9) Uani 1 1 d . . . . .
H79A H 0.866339 0.783396 0.679724 0.126 Uiso 1 1 calc R U . . .
H79B H 0.982868 0.761318 0.676483 0.126 Uiso 1 1 calc R U . . .
H79C H 0.898718 0.688090 0.668620 0.126 Uiso 1 1 calc R U . . .
C80 C 1.0682(3) 0.8649(2) 0.55273(14) 0.1085(15) Uani 1 1 d . . . . .
C81 C 1.0921(3) 0.9557(3) 0.56769(14) 0.1132(15) Uani 1 1 d . . . . .
H81A H 1.033779 0.993311 0.561341 0.170 Uiso 1 1 calc R U . . .
H81B H 1.150936 0.978382 0.556310 0.170 Uiso 1 1 calc R U . . .
H81C H 1.106939 0.953460 0.595002 0.170 Uiso 1 1 calc R U . . .
C82 C 1.1600(4) 0.8073(3) 0.5645(3) 0.198(4) Uani 1 1 d . . . . .
H82A H 1.220924 0.832902 0.555680 0.297 Uiso 1 1 calc R U . . .
H82B H 1.149106 0.749888 0.553408 0.297 Uiso 1 1 calc R U . . .
H82C H 1.168449 0.802331 0.591900 0.297 Uiso 1 1 calc R U . . .
C83 C 1.0494(5) 0.8704(4) 0.50982(16) 0.162(3) Uani 1 1 d . . . . .
H83A H 0.994722 0.911494 0.502993 0.243 Uiso 1 1 calc R U . . .
H83B H 1.030167 0.813421 0.499683 0.243 Uiso 1 1 calc R U . . .
H83C H 1.111170 0.889715 0.499412 0.243 Uiso 1 1 calc R U . . .
C84 C 0.6991(3) 0.7767(3) 0.54259(9) 0.1056(14) Uani 1 1 d . . . . .
H84A H 0.684517 0.715134 0.539189 0.158 Uiso 1 1 calc R U . . .
H84B H 0.703068 0.803805 0.518041 0.158 Uiso 1 1 calc R U . . .
H84C H 0.645182 0.803975 0.555290 0.158 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.370(3) . ?
N1 C4 1.375(3) . ?
N1 H1 0.8800 . ?
N2 C6 1.374(3) . ?
N2 C9 1.377(3) . ?
N3 C11 1.370(3) . ?
N3 C14 1.375(3) . ?
N3 H3A 0.8800 . ?
N4 C19 1.368(3) . ?
N4 C16 1.373(3) . ?
C1 C20 1.391(3) . ?
C1 C2 1.432(3) . ?
C2 C3 1.353(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.428(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(3) . ?
C5 C6 1.394(3) . ?
C5 C21 1.504(3) . ?
C6 C7 1.453(3) . ?
C7 C8 1.338(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.448(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.400(3) . ?
C10 C11 1.400(3) . ?
C10 C49 1.502(3) . ?
C11 C12 1.422(3) . ?
C12 C13 1.346(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.427(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.396(3) . ?
C15 C16 1.399(3) . ?
C15 C61 1.501(3) . ?
C16 C17 1.452(3) . ?
C17 C18 1.340(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.455(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.408(3) . ?
C20 C73 1.494(3) . ?
C21 C46 1.367(3) . ?
C21 C22 1.409(3) . ?
C22 C23 1.370(3) . ?
C22 H22 0.9500 . ?
C23 O1 1.369(3) . ?
C23 C24 1.420(3) . ?
C24 C45 1.423(3) . ?
C24 C25 1.430(3) . ?
C25 C26 1.353(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.417(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.415(4) . ?
C27 C44 1.426(4) . ?
C28 C29 1.381(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.383(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.416(5) . ?
C30 C43 1.438(4) . ?
C31 C32 1.346(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.423(5) . ?
C32 H32 0.9500 . ?
C33 C42 1.425(4) . ?
C33 C34 1.426(5) . ?
C34 C35 1.351(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.424(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.402(4) . ?
C36 C41 1.426(4) . ?
C37 C38 1.372(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.394(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.379(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.407(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.452(3) . ?
C42 C43 1.450(4) . ?
C43 C44 1.447(4) . ?
C44 C45 1.454(3) . ?
C45 C46 1.436(3) . ?
C46 O2 1.385(3) . ?
O1 C47 1.429(3) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
O2 C48 1.419(3) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.402(3) . ?
C49 C54 1.405(3) . ?
C50 C51 1.386(3) . ?
C50 C55 1.504(3) . ?
C51 C52 1.388(3) . ?
C51 H51 0.9500 . ?
C52 C53 1.395(3) . ?
C52 C56 1.531(3) . ?
C53 C54 1.386(3) . ?
C53 H53 0.9500 . ?
C54 C60 1.511(3) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C57 1.518(4) . ?
C56 C59 1.532(4) . ?
C56 C58 1.534(4) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.397(3) . ?
C61 C66 1.402(3) . ?
C62 C63 1.393(3) . ?
C62 C67 1.501(3) . ?
C63 C64 1.381(4) . ?
C63 H63 0.9500 . ?
C64 C65 1.397(4) . ?
C64 C68 1.541(3) . ?
C65 C66 1.393(4) . ?
C65 H65 0.9500 . ?
C66 C72 1.513(4) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 C71A 1.404(13) . ?
C68 C69 1.483(7) . ?
C68 C71 1.515(6) . ?
C68 C70 1.545(5) . ?
C68 C70A 1.602(14) . ?
C68 C69A 1.680(15) . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C69A H69D 0.9800 . ?
C69A H69E 0.9800 . ?
C69A H69F 0.9800 . ?
C70A H70D 0.9800 . ?
C70A H70E 0.9800 . ?
C70A H70F 0.9800 . ?
C71A H71D 0.9800 . ?
C71A H71E 0.9800 . ?
C71A H71F 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 C74 1.387(4) . ?
C73 C78 1.401(4) . ?
C74 C75 1.410(4) . ?
C74 C79 1.490(4) . ?
C75 C76 1.384(5) . ?
C75 H75 0.9500 . ?
C76 C77 1.374(5) . ?
C76 C80 1.530(4) . ?
C77 C78 1.388(4) . ?
C77 H77 0.9500 . ?
C78 C84 1.529(4) . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 C81 1.529(5) . ?
C80 C83 1.535(8) . ?
C80 C82 1.540(8) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 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
C1 N1 C4 110.28(17) . . ?
C1 N1 H1 124.9 . . ?
C4 N1 H1 124.9 . . ?
C6 N2 C9 105.00(17) . . ?
C11 N3 C14 109.71(17) . . ?
C11 N3 H3A 125.1 . . ?
C14 N3 H3A 125.1 . . ?
C19 N4 C16 105.23(17) . . ?
N1 C1 C20 127.32(19) . . ?
N1 C1 C2 106.39(18) . . ?
C20 C1 C2 126.3(2) . . ?
C3 C2 C1 108.54(19) . . ?
C3 C2 H2 125.7 . . ?
C1 C2 H2 125.7 . . ?
C2 C3 C4 108.10(19) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 H3 126.0 . . ?
N1 C4 C5 125.60(18) . . ?
N1 C4 C3 106.67(18) . . ?
C5 C4 C3 127.69(19) . . ?
C6 C5 C4 124.76(19) . . ?
C6 C5 C21 117.27(18) . . ?
C4 C5 C21 117.96(18) . . ?
N2 C6 C5 125.84(19) . . ?
N2 C6 C7 110.42(17) . . ?
C5 C6 C7 123.61(19) . . ?
C8 C7 C6 107.05(19) . . ?
C8 C7 H7 126.5 . . ?
C6 C7 H7 126.5 . . ?
C7 C8 C9 106.81(19) . . ?
C7 C8 H8 126.6 . . ?
C9 C8 H8 126.6 . . ?
N2 C9 C10 126.56(19) . . ?
N2 C9 C8 110.70(18) . . ?
C10 C9 C8 122.73(19) . . ?
C11 C10 C9 125.2(2) . . ?
C11 C10 C49 118.03(19) . . ?
C9 C10 C49 116.79(18) . . ?
N3 C11 C10 126.50(19) . . ?
N3 C11 C12 106.83(19) . . ?
C10 C11 C12 126.6(2) . . ?
C13 C12 C11 108.60(19) . . ?
C13 C12 H12 125.7 . . ?
C11 C12 H12 125.7 . . ?
C12 C13 C14 108.2(2) . . ?
C12 C13 H13 125.9 . . ?
C14 C13 H13 125.9 . . ?
N3 C14 C15 126.62(19) . . ?
N3 C14 C13 106.67(19) . . ?
C15 C14 C13 126.7(2) . . ?
C14 C15 C16 124.56(19) . . ?
C14 C15 C61 115.68(18) . . ?
C16 C15 C61 119.69(19) . . ?
N4 C16 C15 125.45(19) . . ?
N4 C16 C17 110.56(18) . . ?
C15 C16 C17 123.97(19) . . ?
C18 C17 C16 106.84(19) . . ?
C18 C17 H17 126.6 . . ?
C16 C17 H17 126.6 . . ?
C17 C18 C19 106.71(19) . . ?
C17 C18 H18 126.6 . . ?
C19 C18 H18 126.6 . . ?
N4 C19 C20 126.07(19) . . ?
N4 C19 C18 110.65(18) . . ?
C20 C19 C18 123.28(19) . . ?
C1 C20 C19 125.72(19) . . ?
C1 C20 C73 116.13(19) . . ?
C19 C20 C73 118.11(19) . . ?
C46 C21 C22 120.63(19) . . ?
C46 C21 C5 122.06(19) . . ?
C22 C21 C5 117.16(18) . . ?
C23 C22 C21 119.9(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
O1 C23 C22 123.7(2) . . ?
O1 C23 C24 115.6(2) . . ?
C22 C23 C24 120.7(2) . . ?
C23 C24 C45 120.2(2) . . ?
C23 C24 C25 119.4(2) . . ?
C45 C24 C25 120.3(2) . . ?
C26 C25 C24 119.5(3) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 122.0(3) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 H26 119.0 . . ?
C28 C27 C26 120.3(3) . . ?
C28 C27 C44 119.9(3) . . ?
C26 C27 C44 119.7(2) . . ?
C29 C28 C27 119.4(3) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 120.9(3) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C29 C30 C31 120.4(3) . . ?
C29 C30 C43 120.3(3) . . ?
C31 C30 C43 119.3(3) . . ?
C32 C31 C30 121.1(3) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C31 C32 C33 121.1(3) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C32 C33 C42 119.8(3) . . ?
C32 C33 C34 119.8(3) . . ?
C42 C33 C34 120.3(3) . . ?
C35 C34 C33 121.5(3) . . ?
C35 C34 H34 119.2 . . ?
C33 C34 H34 119.2 . . ?
C34 C35 C36 120.1(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C37 C36 C35 119.5(3) . . ?
C37 C36 C41 120.3(3) . . ?
C35 C36 C41 120.1(3) . . ?
C38 C37 C36 121.1(3) . . ?
C38 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?
C37 C38 C39 119.1(3) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C40 C39 C38 120.9(3) . . ?
C40 C39 H39 119.6 . . ?
C38 C39 H39 119.6 . . ?
C39 C40 C41 121.6(3) . . ?
C39 C40 H40 119.2 . . ?
C41 C40 H40 119.2 . . ?
C40 C41 C36 116.9(2) . . ?
C40 C41 C42 123.3(2) . . ?
C36 C41 C42 119.5(2) . . ?
C33 C42 C43 117.9(2) . . ?
C33 C42 C41 117.2(2) . . ?
C43 C42 C41 124.5(2) . . ?
C30 C43 C44 116.2(3) . . ?
C30 C43 C42 117.4(2) . . ?
C44 C43 C42 126.3(2) . . ?
C27 C44 C43 117.2(2) . . ?
C27 C44 C45 117.0(2) . . ?
C43 C44 C45 125.7(2) . . ?
C24 C45 C46 116.9(2) . . ?
C24 C45 C44 118.9(2) . . ?
C46 C45 C44 123.7(2) . . ?
C21 C46 O2 118.25(19) . . ?
C21 C46 C45 121.5(2) . . ?
O2 C46 C45 120.18(19) . . ?
C23 O1 C47 116.75(19) . . ?
O1 C47 H47A 109.5 . . ?
O1 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
O1 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 O2 C48 113.82(18) . . ?
O2 C48 H48A 109.5 . . ?
O2 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
O2 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 C54 119.8(2) . . ?
C50 C49 C10 120.02(19) . . ?
C54 C49 C10 119.98(19) . . ?
C51 C50 C49 118.9(2) . . ?
C51 C50 C55 119.4(2) . . ?
C49 C50 C55 121.7(2) . . ?
C50 C51 C52 122.8(2) . . ?
C50 C51 H51 118.6 . . ?
C52 C51 H51 118.6 . . ?
C51 C52 C53 116.8(2) . . ?
C51 C52 C56 123.0(2) . . ?
C53 C52 C56 120.2(2) . . ?
C54 C53 C52 122.7(2) . . ?
C54 C53 H53 118.7 . . ?
C52 C53 H53 118.7 . . ?
C53 C54 C49 118.8(2) . . ?
C53 C54 C60 120.7(2) . . ?
C49 C54 C60 120.5(2) . . ?
C50 C55 H55A 109.5 . . ?
C50 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C50 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C57 C56 C52 112.2(2) . . ?
C57 C56 C59 109.4(2) . . ?
C52 C56 C59 110.1(2) . . ?
C57 C56 C58 107.3(3) . . ?
C52 C56 C58 109.29(19) . . ?
C59 C56 C58 108.4(2) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C56 C59 H59A 109.5 . . ?
C56 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C56 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C54 C60 H60A 109.5 . . ?
C54 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C54 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 C66 119.8(2) . . ?
C62 C61 C15 120.3(2) . . ?
C66 C61 C15 119.88(19) . . ?
C63 C62 C61 119.3(2) . . ?
C63 C62 C67 119.8(2) . . ?
C61 C62 C67 120.9(2) . . ?
C64 C63 C62 122.0(2) . . ?
C64 C63 H63 119.0 . . ?
C62 C63 H63 119.0 . . ?
C63 C64 C65 117.9(2) . . ?
C63 C64 C68 121.7(2) . . ?
C65 C64 C68 120.3(2) . . ?
C66 C65 C64 121.6(2) . . ?
C66 C65 H65 119.2 . . ?
C64 C65 H65 119.2 . . ?
C65 C66 C61 119.2(2) . . ?
C65 C66 C72 119.3(2) . . ?
C61 C66 C72 121.5(2) . . ?
C62 C67 H67A 109.5 . . ?
C62 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C62 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C69 C68 C71 111.0(5) . . ?
C71A C68 C64 112.7(5) . . ?
C69 C68 C64 108.3(3) . . ?
C71 C68 C64 109.7(3) . . ?
C69 C68 C70 109.0(4) . . ?
C71 C68 C70 107.8(4) . . ?
C64 C68 C70 111.1(3) . . ?
C71A C68 C70A 122.1(11) . . ?
C64 C68 C70A 108.9(5) . . ?
C71A C68 C69A 101.0(10) . . ?
C64 C68 C69A 111.0(4) . . ?
C70A C68 C69A 99.6(9) . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C68 C71 H71A 109.5 . . ?
C68 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C68 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C68 C69A H69D 109.5 . . ?
C68 C69A H69E 109.5 . . ?
H69D C69A H69E 109.5 . . ?
C68 C69A H69F 109.5 . . ?
H69D C69A H69F 109.5 . . ?
H69E C69A H69F 109.5 . . ?
C68 C70A H70D 109.5 . . ?
C68 C70A H70E 109.5 . . ?
H70D C70A H70E 109.5 . . ?
C68 C70A H70F 109.5 . . ?
H70D C70A H70F 109.5 . . ?
H70E C70A H70F 109.5 . . ?
C68 C71A H71D 109.5 . . ?
C68 C71A H71E 109.5 . . ?
H71D C71A H71E 109.5 . . ?
C68 C71A H71F 109.5 . . ?
H71D C71A H71F 109.5 . . ?
H71E C71A H71F 109.5 . . ?
C66 C72 H72A 109.5 . . ?
C66 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C66 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C74 C73 C78 120.2(2) . . ?
C74 C73 C20 121.0(2) . . ?
C78 C73 C20 118.8(2) . . ?
C73 C74 C75 117.8(3) . . ?
C73 C74 C79 121.1(2) . . ?
C75 C74 C79 121.0(3) . . ?
C76 C75 C74 122.9(3) . . ?
C76 C75 H75 118.6 . . ?
C74 C75 H75 118.6 . . ?
C77 C76 C75 117.4(2) . . ?
C77 C76 C80 122.5(3) . . ?
C75 C76 C80 120.1(3) . . ?
C76 C77 C78 122.1(3) . . ?
C76 C77 H77 118.9 . . ?
C78 C77 H77 118.9 . . ?
C77 C78 C73 119.6(3) . . ?
C77 C78 C84 120.0(3) . . ?
C73 C78 C84 120.4(2) . . ?
C74 C79 H79A 109.5 . . ?
C74 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C74 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C81 C80 C76 109.3(3) . . ?
C81 C80 C83 108.0(4) . . ?
C76 C80 C83 111.7(4) . . ?
C81 C80 C82 107.8(4) . . ?
C76 C80 C82 109.2(4) . . ?
C83 C80 C82 110.9(4) . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C80 C82 H82A 109.5 . . ?
C80 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C80 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C80 C83 H83A 109.5 . . ?
C80 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C80 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C78 C84 H84A 109.5 . . ?
C78 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C78 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?

_refine_diff_density_max         0.268
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.050



