# Electronic Supplementary Material (ESI) for ChemComm.
# 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. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1817320'
_audit_update_record             
;
2018-01-16 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H20'
_chemical_formula_weight         356.44

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'

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

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

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

_cell_length_a                   9.9154(12)
_cell_length_b                   10.0178(12)
_cell_length_c                   10.4437(12)
_cell_angle_alpha                92.162(5)
_cell_angle_beta                 104.822(5)
_cell_angle_gamma                105.321(4)
_cell_volume                     961.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      2.5595
_cell_measurement_theta_max      24.781

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_F_000             376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.145
_exptl_absorpt_coefficient_mu    0.070
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.9105
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
The Ratio of minimum to maximum transmission is 0.9105.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24447
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.121
_diffrn_reflns_theta_max         24.801
_diffrn_reflns_theta_full        24.801
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3304
_reflns_number_gt                3034
_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 APEX3'
_computing_data_reduction        'SAINT V8.37A'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'USCF Chimera 1.10.1 and Ortep3'
_computing_publication_material  'WinGX CIF routines'
_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)+(0.0382P)²+0.4428P] 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         3304
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0958
_refine_ls_wR_factor_gt          0.0914
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_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
C1 C 0.32626(13) 0.34828(12) 0.46111(12) 0.0150(3) Uani 1 1 d . . . . .
C2 C 0.27494(13) 0.44871(13) 0.50219(12) 0.0164(3) Uani 1 1 d . . . . .
C3 C 0.22503(13) 0.54427(13) 0.53220(12) 0.0162(3) Uani 1 1 d . . . . .
C4 C 0.17287(13) 0.65042(12) 0.55728(12) 0.0147(3) Uani 1 1 d . . . . .
C5 C 0.32727(13) 0.33376(13) 0.31945(12) 0.0152(3) Uani 1 1 d . . . . .
C6 C 0.33644(15) 0.44932(13) 0.24743(13) 0.0210(3) Uani 1 1 d . . . . .
H6 H 0.346809 0.537909 0.290987 0.025 Uiso 1 1 calc R U . . .
C7 C 0.33059(16) 0.43619(15) 0.11379(14) 0.0256(3) Uani 1 1 d . . . . .
H7 H 0.337330 0.515821 0.066561 0.031 Uiso 1 1 calc R U . . .
C8 C 0.31499(15) 0.30795(15) 0.04802(13) 0.0228(3) Uani 1 1 d . . . . .
H8 H 0.311134 0.299418 -0.043837 0.027 Uiso 1 1 calc R U . . .
C9 C 0.30505(14) 0.19215(14) 0.11768(13) 0.0199(3) Uani 1 1 d . . . . .
H9 H 0.293516 0.103732 0.073097 0.024 Uiso 1 1 calc R U . . .
C10 C 0.31186(13) 0.20477(13) 0.25210(13) 0.0166(3) Uani 1 1 d . . . . .
H10 H 0.305997 0.124938 0.299002 0.020 Uiso 1 1 calc R U . . .
C11 C 0.37570(13) 0.25289(12) 0.55540(12) 0.0146(3) Uani 1 1 d . . . . .
C12 C 0.49295(14) 0.20256(13) 0.54969(12) 0.0170(3) Uani 1 1 d . . . . .
H12 H 0.540931 0.227593 0.482506 0.020 Uiso 1 1 calc R U . . .
C13 C 0.53996(14) 0.11627(13) 0.64136(13) 0.0196(3) Uani 1 1 d . . . . .
H13 H 0.621691 0.085061 0.638180 0.024 Uiso 1 1 calc R U . . .
C14 C 0.46834(15) 0.07536(13) 0.73751(13) 0.0206(3) Uani 1 1 d . . . . .
H14 H 0.499083 0.014295 0.798587 0.025 Uiso 1 1 calc R U . . .
C15 C 0.35145(15) 0.12428(13) 0.74382(13) 0.0204(3) Uani 1 1 d . . . . .
H15 H 0.301884 0.096322 0.809371 0.025 Uiso 1 1 calc R U . . .
C16 C 0.30643(14) 0.21388(13) 0.65492(12) 0.0174(3) Uani 1 1 d . . . . .
H16 H 0.228068 0.248928 0.661724 0.021 Uiso 1 1 calc R U . . .
C17 C 0.11297(13) 0.72245(13) 0.44439(12) 0.0147(3) Uani 1 1 d . . . . .
C18 C 0.05889(14) 0.65353(13) 0.31451(13) 0.0181(3) Uani 1 1 d . . . . .
H18 H 0.055283 0.558325 0.299831 0.022 Uiso 1 1 calc R U . . .
C19 C 0.01067(14) 0.72253(14) 0.20736(13) 0.0209(3) Uani 1 1 d . . . . .
H19 H -0.025666 0.674444 0.119921 0.025 Uiso 1 1 calc R U . . .
C20 C 0.01519(14) 0.86157(14) 0.22710(13) 0.0217(3) Uani 1 1 d . . . . .
H20 H -0.016964 0.909091 0.153431 0.026 Uiso 1 1 calc R U . . .
C21 C 0.06703(14) 0.93068(13) 0.35529(13) 0.0194(3) Uani 1 1 d . . . . .
H21 H 0.069143 1.025548 0.369331 0.023 Uiso 1 1 calc R U . . .
C22 C 0.11576(13) 0.86243(13) 0.46300(13) 0.0165(3) Uani 1 1 d . . . . .
H22 H 0.151376 0.911031 0.550212 0.020 Uiso 1 1 calc R U . . .
C23 C 0.18425(13) 0.69890(12) 0.69649(12) 0.0149(3) Uani 1 1 d . . . . .
C24 C 0.07240(14) 0.74048(13) 0.72988(13) 0.0174(3) Uani 1 1 d . . . . .
H24 H -0.012799 0.739123 0.662073 0.021 Uiso 1 1 calc R U . . .
C25 C 0.08486(15) 0.78362(13) 0.86109(13) 0.0206(3) Uani 1 1 d . . . . .
H25 H 0.007116 0.809236 0.882960 0.025 Uiso 1 1 calc R U . . .
C26 C 0.21021(15) 0.78964(13) 0.96068(13) 0.0214(3) Uani 1 1 d . . . . .
H26 H 0.219255 0.820856 1.050328 0.026 Uiso 1 1 calc R U . . .
C27 C 0.32230(14) 0.74970(13) 0.92836(13) 0.0203(3) Uani 1 1 d . . . . .
H27 H 0.408735 0.754491 0.996061 0.024 Uiso 1 1 calc R U . . .
C28 C 0.30886(14) 0.70287(13) 0.79788(13) 0.0173(3) Uani 1 1 d . . . . .
H28 H 0.385045 0.673225 0.777227 0.021 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3435(17) . ?
C1 C11 1.4815(17) . ?
C1 C5 1.4840(17) . ?
C2 C3 1.2516(18) . ?
C3 C4 1.3439(17) . ?
C4 C17 1.4818(17) . ?
C4 C23 1.4820(17) . ?
C5 C6 1.3997(18) . ?
C5 C10 1.4000(18) . ?
C6 C7 1.3818(19) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.3873(19) . ?
C8 H8 0.9500 . ?
C9 C10 1.3874(18) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.3973(18) . ?
C11 C16 1.3996(18) . ?
C12 C13 1.3886(18) . ?
C12 H12 0.9500 . ?
C13 C14 1.3865(19) . ?
C13 H13 0.9500 . ?
C14 C15 1.3873(19) . ?
C14 H14 0.9500 . ?
C15 C16 1.3891(18) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.4004(18) . ?
C17 C18 1.4020(18) . ?
C18 C19 1.3850(18) . ?
C18 H18 0.9500 . ?
C19 C20 1.3875(19) . ?
C19 H19 0.9500 . ?
C20 C21 1.3877(19) . ?
C20 H20 0.9500 . ?
C21 C22 1.3859(18) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.3967(18) . ?
C23 C24 1.3986(18) . ?
C24 C25 1.3857(18) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.3878(19) . ?
C26 H26 0.9500 . ?
C27 C28 1.3858(18) . ?
C27 H27 0.9500 . ?
C28 H28 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 C1 C11 119.99(11) . . ?
C2 C1 C5 118.25(11) . . ?
C11 C1 C5 121.74(10) . . ?
C3 C2 C1 175.98(13) . . ?
C2 C3 C4 176.31(13) . . ?
C3 C4 C17 118.66(11) . . ?
C3 C4 C23 119.98(11) . . ?
C17 C4 C23 121.25(10) . . ?
C6 C5 C10 118.07(11) . . ?
C6 C5 C1 120.13(11) . . ?
C10 C5 C1 121.73(11) . . ?
C7 C6 C5 120.85(12) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C8 120.61(13) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C9 119.33(12) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C8 C9 C10 120.35(12) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C5 120.79(12) . . ?
C9 C10 H10 119.6 . . ?
C5 C10 H10 119.6 . . ?
C12 C11 C16 118.59(11) . . ?
C12 C11 C1 121.55(11) . . ?
C16 C11 C1 119.85(11) . . ?
C13 C12 C11 120.57(12) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C12 120.41(12) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 119.49(12) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C16 120.43(12) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 120.46(12) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C22 C17 C18 118.27(11) . . ?
C22 C17 C4 121.23(11) . . ?
C18 C17 C4 120.42(11) . . ?
C19 C18 C17 120.81(12) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.31(12) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C21 119.49(12) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C22 C21 C20 120.54(12) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C17 120.58(12) . . ?
C21 C22 H22 119.7 . . ?
C17 C22 H22 119.7 . . ?
C28 C23 C24 118.62(11) . . ?
C28 C23 C4 119.74(11) . . ?
C24 C23 C4 121.63(11) . . ?
C25 C24 C23 120.53(12) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 120.39(12) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C27 119.49(12) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C28 C27 C26 120.38(12) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C23 120.56(12) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C5 C6 27.07(17) . . . . ?
C11 C1 C5 C6 -154.84(12) . . . . ?
C2 C1 C5 C10 -149.66(12) . . . . ?
C11 C1 C5 C10 28.44(17) . . . . ?
C10 C5 C6 C7 -0.08(19) . . . . ?
C1 C5 C6 C7 -176.92(12) . . . . ?
C5 C6 C7 C8 0.2(2) . . . . ?
C6 C7 C8 C9 0.1(2) . . . . ?
C7 C8 C9 C10 -0.5(2) . . . . ?
C8 C9 C10 C5 0.68(19) . . . . ?
C6 C5 C10 C9 -0.38(18) . . . . ?
C1 C5 C10 C9 176.42(11) . . . . ?
C2 C1 C11 C12 -145.03(12) . . . . ?
C5 C1 C11 C12 36.91(17) . . . . ?
C2 C1 C11 C16 33.51(17) . . . . ?
C5 C1 C11 C16 -144.55(12) . . . . ?
C16 C11 C12 C13 -0.32(18) . . . . ?
C1 C11 C12 C13 178.24(11) . . . . ?
C11 C12 C13 C14 1.96(19) . . . . ?
C12 C13 C14 C15 -1.70(19) . . . . ?
C13 C14 C15 C16 -0.18(19) . . . . ?
C14 C15 C16 C11 1.82(19) . . . . ?
C12 C11 C16 C15 -1.55(18) . . . . ?
C1 C11 C16 C15 179.86(11) . . . . ?
C3 C4 C17 C22 -151.92(12) . . . . ?
C23 C4 C17 C22 24.27(17) . . . . ?
C3 C4 C17 C18 24.66(17) . . . . ?
C23 C4 C17 C18 -159.15(11) . . . . ?
C22 C17 C18 C19 0.54(18) . . . . ?
C4 C17 C18 C19 -176.15(11) . . . . ?
C17 C18 C19 C20 -0.01(19) . . . . ?
C18 C19 C20 C21 -0.66(19) . . . . ?
C19 C20 C21 C22 0.79(19) . . . . ?
C20 C21 C22 C17 -0.26(19) . . . . ?
C18 C17 C22 C21 -0.40(18) . . . . ?
C4 C17 C22 C21 176.25(11) . . . . ?
C3 C4 C23 C28 38.03(17) . . . . ?
C17 C4 C23 C28 -138.11(12) . . . . ?
C3 C4 C23 C24 -141.59(13) . . . . ?
C17 C4 C23 C24 42.27(17) . . . . ?
C28 C23 C24 C25 -0.49(18) . . . . ?
C4 C23 C24 C25 179.13(11) . . . . ?
C23 C24 C25 C26 1.70(19) . . . . ?
C24 C25 C26 C27 -1.1(2) . . . . ?
C25 C26 C27 C28 -0.6(2) . . . . ?
C26 C27 C28 C23 1.82(19) . . . . ?
C24 C23 C28 C27 -1.26(18) . . . . ?
C4 C23 C28 C27 179.11(11) . . . . ?

_refine_diff_density_max         0.146
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.048

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1817322'
_audit_update_record             
;
2018-01-16 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H20'
_chemical_formula_weight         380.46

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'

_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                   14.7030(17)
_cell_length_b                   8.1421(10)
_cell_length_c                   17.264(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.638(2)
_cell_angle_gamma                90
_cell_volume                     2024.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3306
_cell_measurement_theta_min      2.7765
_cell_measurement_theta_max      26.881

_exptl_crystal_description       'irregular block'
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_F_000             800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.071
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8341
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012/1) was used for absorption correction.
wR2(int) was 0.0355 after correction.
The Ratio of minimum to maximum transmission is 0.9257.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12686
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.662
_diffrn_reflns_theta_max         28.343
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4543
_reflns_number_gt                3435
_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 APEX3'
_computing_data_reduction        'Bruker SAINT V8.30C'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'USCF Chimera 1.10.1 and Ortep3'
_computing_publication_material  'WINGX CIF routines'
_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)+(0.0716P)²] 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         4543
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1270
_refine_ls_wR_factor_gt          0.1126
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_restrained_S_all      0.961
_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
C1 C 0.63482(9) 0.71854(16) 0.37897(8) 0.0199(3) Uani 1 1 d . . . . .
C2 C 0.57678(9) 0.69587(16) 0.29900(8) 0.0193(3) Uani 1 1 d . . . . .
C3 C 0.59377(9) 0.77710(16) 0.23131(8) 0.0192(3) Uani 1 1 d . . . . .
C4 C 0.66872(9) 0.89497(16) 0.23157(8) 0.0221(3) Uani 1 1 d . . . . .
H4 H 0.657207 0.975229 0.190827 0.026 Uiso 1 1 calc R U . . .
C5 C 0.75134(9) 0.90619(17) 0.28099(8) 0.0235(3) Uani 1 1 d . . . . .
H5 H 0.789869 0.993619 0.270428 0.028 Uiso 1 1 calc R U . . .
C6 C 0.79069(9) 0.80336(16) 0.34875(8) 0.0217(3) Uani 1 1 d . . . . .
C7 C 0.73775(9) 0.71392(16) 0.39382(8) 0.0197(3) Uani 1 1 d . . . . .
C8 C 0.49950(9) 0.59214(16) 0.29139(8) 0.0221(3) Uani 1 1 d . . . . .
H8 H 0.487418 0.537933 0.336991 0.027 Uiso 1 1 calc R U . . .
C9 C 0.44032(9) 0.56646(17) 0.21938(8) 0.0254(3) Uani 1 1 d . . . . .
H9 H 0.388573 0.494951 0.215758 0.030 Uiso 1 1 calc R U . . .
C10 C 0.45685(9) 0.64569(17) 0.15233(8) 0.0246(3) Uani 1 1 d . . . . .
H10 H 0.416754 0.628611 0.102494 0.030 Uiso 1 1 calc R U . . .
C11 C 0.53248(9) 0.74987(17) 0.15897(8) 0.0226(3) Uani 1 1 d . . . . .
H11 H 0.543189 0.804650 0.113050 0.027 Uiso 1 1 calc R U . . .
C12 C 0.88788(9) 0.79956(18) 0.37148(8) 0.0274(3) Uani 1 1 d . . . . .
H12 H 0.924086 0.861993 0.342366 0.033 Uiso 1 1 calc R U . . .
C13 C 0.93217(10) 0.70721(19) 0.43520(9) 0.0312(4) Uani 1 1 d . . . . .
H13 H 0.998050 0.706086 0.449390 0.037 Uiso 1 1 calc R U . . .
C14 C 0.87998(10) 0.61628(18) 0.47825(8) 0.0296(3) Uani 1 1 d . . . . .
H14 H 0.909933 0.551202 0.521630 0.036 Uiso 1 1 calc R U . . .
C15 C 0.78416(9) 0.62065(17) 0.45784(8) 0.0241(3) Uani 1 1 d . . . . .
H15 H 0.748908 0.558800 0.488007 0.029 Uiso 1 1 calc R U . . .
C16 C 0.59275(9) 0.72617(17) 0.44110(8) 0.0226(3) Uani 1 1 d . . . . .
C17 C 0.55323(9) 0.74456(17) 0.49820(8) 0.0239(3) Uani 1 1 d . . . . .
C18 C 0.51060(9) 0.77550(16) 0.55867(8) 0.0218(3) Uani 1 1 d . . . . .
C19 C 0.56804(9) 0.79902(16) 0.63892(8) 0.0216(3) Uani 1 1 d . . . . .
C20 C 0.65709(9) 0.73093(17) 0.65837(8) 0.0252(3) Uani 1 1 d . . . . .
H20 H 0.678654 0.663664 0.620861 0.030 Uiso 1 1 calc R U . . .
C21 C 0.71438(10) 0.75953(18) 0.73105(9) 0.0282(3) Uani 1 1 d . . . . .
H21 H 0.774795 0.712766 0.742900 0.034 Uiso 1 1 calc R U . . .
C22 C 0.68367(10) 0.85650(18) 0.78668(8) 0.0284(3) Uani 1 1 d . . . . .
H22 H 0.722733 0.875950 0.836778 0.034 Uiso 1 1 calc R U . . .
C23 C 0.59592(10) 0.92452(18) 0.76870(8) 0.0297(3) Uani 1 1 d . . . . .
H23 H 0.574618 0.990461 0.806818 0.036 Uiso 1 1 calc R U . . .
C24 C 0.53856(9) 0.89762(17) 0.69562(8) 0.0254(3) Uani 1 1 d . . . . .
H24 H 0.478691 0.946524 0.683887 0.031 Uiso 1 1 calc R U . . .
C25 C 0.40829(9) 0.80110(16) 0.54121(8) 0.0209(3) Uani 1 1 d . . . . .
C26 C 0.35293(9) 0.76561(17) 0.59591(8) 0.0241(3) Uani 1 1 d . . . . .
H26 H 0.380094 0.718030 0.645424 0.029 Uiso 1 1 calc R U . . .
C27 C 0.25854(9) 0.79935(18) 0.57847(8) 0.0266(3) Uani 1 1 d . . . . .
H27 H 0.221617 0.774645 0.616221 0.032 Uiso 1 1 calc R U . . .
C28 C 0.21747(10) 0.86868(18) 0.50661(9) 0.0284(3) Uani 1 1 d . . . . .
H28 H 0.153096 0.894147 0.495536 0.034 Uiso 1 1 calc R U . . .
C29 C 0.27143(10) 0.90049(18) 0.45101(8) 0.0286(3) Uani 1 1 d . . . . .
H29 H 0.243714 0.945834 0.401119 0.034 Uiso 1 1 calc R U . . .
C30 C 0.36541(9) 0.86633(17) 0.46808(8) 0.0248(3) Uani 1 1 d . . . . .
H30 H 0.401558 0.887592 0.429369 0.030 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 C16 1.3434(18) . ?
C1 C2 1.4809(18) . ?
C1 C7 1.4836(18) . ?
C2 C8 1.4006(18) . ?
C2 C3 1.4083(18) . ?
C3 C11 1.4025(18) . ?
C3 C4 1.4607(18) . ?
C4 C5 1.3392(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.4599(19) . ?
C5 H5 0.9500 . ?
C6 C12 1.4037(18) . ?
C6 C7 1.4092(18) . ?
C7 C15 1.3999(18) . ?
C8 C9 1.3821(18) . ?
C8 H8 0.9500 . ?
C9 C10 1.3888(19) . ?
C9 H9 0.9500 . ?
C10 C11 1.3848(19) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.382(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.3819(18) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.2502(18) . ?
C17 C18 1.3453(18) . ?
C18 C19 1.4824(18) . ?
C18 C25 1.4881(18) . ?
C19 C24 1.4006(19) . ?
C19 C20 1.3990(19) . ?
C20 C21 1.3828(19) . ?
C20 H20 0.9500 . ?
C21 C22 1.387(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.381(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3863(19) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.3957(18) . ?
C25 C30 1.3972(18) . ?
C26 C27 1.3870(19) . ?
C26 H26 0.9500 . ?
C27 C28 1.3858(19) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.3818(19) . ?
C29 H29 0.9500 . ?
C30 H30 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
C16 C1 C2 118.59(11) . . ?
C16 C1 C7 118.77(11) . . ?
C2 C1 C7 122.26(11) . . ?
C8 C2 C3 118.80(12) . . ?
C8 C2 C1 117.82(12) . . ?
C3 C2 C1 123.35(12) . . ?
C11 C3 C2 118.36(12) . . ?
C11 C3 C4 117.09(12) . . ?
C2 C3 C4 124.47(12) . . ?
C5 C4 C3 129.32(13) . . ?
C5 C4 H4 115.3 . . ?
C3 C4 H4 115.3 . . ?
C4 C5 C6 129.29(13) . . ?
C4 C5 H5 115.4 . . ?
C6 C5 H5 115.4 . . ?
C12 C6 C7 118.60(13) . . ?
C12 C6 C5 116.95(12) . . ?
C7 C6 C5 124.41(12) . . ?
C15 C7 C6 118.73(12) . . ?
C15 C7 C1 117.90(12) . . ?
C6 C7 C1 123.32(12) . . ?
C9 C8 C2 121.82(12) . . ?
C9 C8 H8 119.1 . . ?
C2 C8 H8 119.1 . . ?
C8 C9 C10 119.68(13) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 119.22(13) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C3 122.10(13) . . ?
C10 C11 H11 118.9 . . ?
C3 C11 H11 118.9 . . ?
C13 C12 C6 121.61(13) . . ?
C13 C12 H12 119.2 . . ?
C6 C12 H12 119.2 . . ?
C12 C13 C14 119.64(13) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 119.73(13) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C7 121.65(13) . . ?
C14 C15 H15 119.2 . . ?
C7 C15 H15 119.2 . . ?
C17 C16 C1 175.75(14) . . ?
C16 C17 C18 176.07(15) . . ?
C17 C18 C19 118.86(12) . . ?
C17 C18 C25 118.64(12) . . ?
C19 C18 C25 122.22(11) . . ?
C24 C19 C20 117.77(12) . . ?
C24 C19 C18 121.94(12) . . ?
C20 C19 C18 120.15(12) . . ?
C21 C20 C19 121.36(13) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C20 C21 C22 120.02(13) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 119.51(13) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 120.70(13) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C19 120.63(13) . . ?
C23 C24 H24 119.7 . . ?
C19 C24 H24 119.7 . . ?
C26 C25 C30 118.15(12) . . ?
C26 C25 C18 122.52(12) . . ?
C30 C25 C18 119.32(12) . . ?
C27 C26 C25 120.44(12) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C28 C27 C26 120.74(13) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C27 C28 C29 119.27(13) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 120.10(13) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 121.25(13) . . ?
C29 C30 H30 119.4 . . ?
C25 C30 H30 119.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 C1 C2 C8 -37.50(17) . . . . ?
C7 C1 C2 C8 135.33(13) . . . . ?
C16 C1 C2 C3 140.39(13) . . . . ?
C7 C1 C2 C3 -46.78(18) . . . . ?
C8 C2 C3 C11 -0.24(18) . . . . ?
C1 C2 C3 C11 -178.11(11) . . . . ?
C8 C2 C3 C4 176.63(12) . . . . ?
C1 C2 C3 C4 -1.2(2) . . . . ?
C11 C3 C4 C5 -155.50(14) . . . . ?
C2 C3 C4 C5 27.6(2) . . . . ?
C3 C4 C5 C6 0.3(2) . . . . ?
C4 C5 C6 C12 156.14(14) . . . . ?
C4 C5 C6 C7 -26.3(2) . . . . ?
C12 C6 C7 C15 -2.07(19) . . . . ?
C5 C6 C7 C15 -179.57(12) . . . . ?
C12 C6 C7 C1 175.39(12) . . . . ?
C5 C6 C7 C1 -2.1(2) . . . . ?
C16 C1 C7 C15 39.14(18) . . . . ?
C2 C1 C7 C15 -133.68(13) . . . . ?
C16 C1 C7 C6 -138.34(13) . . . . ?
C2 C1 C7 C6 48.84(18) . . . . ?
C3 C2 C8 C9 0.62(19) . . . . ?
C1 C2 C8 C9 178.60(12) . . . . ?
C2 C8 C9 C10 -0.4(2) . . . . ?
C8 C9 C10 C11 -0.2(2) . . . . ?
C9 C10 C11 C3 0.6(2) . . . . ?
C2 C3 C11 C10 -0.37(19) . . . . ?
C4 C3 C11 C10 -177.47(12) . . . . ?
C7 C6 C12 C13 1.8(2) . . . . ?
C5 C6 C12 C13 179.49(13) . . . . ?
C6 C12 C13 C14 -0.3(2) . . . . ?
C12 C13 C14 C15 -0.9(2) . . . . ?
C13 C14 C15 C7 0.6(2) . . . . ?
C6 C7 C15 C14 0.9(2) . . . . ?
C1 C7 C15 C14 -176.70(12) . . . . ?
C17 C18 C19 C24 151.40(14) . . . . ?
C25 C18 C19 C24 -22.44(19) . . . . ?
C17 C18 C19 C20 -24.27(19) . . . . ?
C25 C18 C19 C20 161.89(12) . . . . ?
C24 C19 C20 C21 0.0(2) . . . . ?
C18 C19 C20 C21 175.88(12) . . . . ?
C19 C20 C21 C22 0.5(2) . . . . ?
C20 C21 C22 C23 -0.3(2) . . . . ?
C21 C22 C23 C24 -0.3(2) . . . . ?
C22 C23 C24 C19 0.9(2) . . . . ?
C20 C19 C24 C23 -0.7(2) . . . . ?
C18 C19 C24 C23 -176.46(12) . . . . ?
C17 C18 C25 C26 152.29(14) . . . . ?
C19 C18 C25 C26 -33.85(19) . . . . ?
C17 C18 C25 C30 -29.10(19) . . . . ?
C19 C18 C25 C30 144.76(13) . . . . ?
C30 C25 C26 C27 -1.9(2) . . . . ?
C18 C25 C26 C27 176.69(13) . . . . ?
C25 C26 C27 C28 0.0(2) . . . . ?
C26 C27 C28 C29 1.6(2) . . . . ?
C27 C28 C29 C30 -1.3(2) . . . . ?
C28 C29 C30 C25 -0.6(2) . . . . ?
C26 C25 C30 C29 2.2(2) . . . . ?
C18 C25 C30 C29 -176.43(13) . . . . ?

_refine_diff_density_max         0.209
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.046

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1817323'
_audit_update_record             
;
2018-01-16 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C105 H92 O2'
_chemical_formula_weight         1385.78

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'
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/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                   11.1208(5)
_cell_length_b                   22.2219(11)
_cell_length_c                   16.4054(9)
_cell_angle_alpha                90
_cell_angle_beta                 108.564(2)
_cell_angle_gamma                90
_cell_volume                     3843.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9872
_cell_measurement_theta_min      2.8415
_cell_measurement_theta_max      44.5455

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_F_000             1476
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.111
_exptl_absorpt_coefficient_mu    0.526
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.944
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.8839
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0503 after correction.
The ratio of minimum to maximum apparent transmission was 0.884.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20635
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.469
_diffrn_reflns_theta_max         44.573
_diffrn_reflns_theta_full        44.573
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3017
_reflns_number_gt                2634
_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 APEX3'
_computing_data_reduction        'SAINT V8.37A'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'USCF Chimera 1.10.1 and Ortep3'
_computing_publication_material  'WinGX CIF Routines'
_refine_special_details          
;
The OMe and OH groups are disordered as they partially occupy the
same positions in the unit cell, attached to each of the 7-membered
rings. These disorder was modelled using EADP, EXYZ, FREE, BIND and
PART instructions, with an occupancy factor of 0.5 for the atoms
involved.
One of the tert-butyl groups showed thermal disorder which was 
modelled with SIMU, DELU and ISOR restraints.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0591P)²+13.6929P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3017
_refine_ls_number_parameters     495
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0806
_refine_ls_wR_factor_ref         0.1914
_refine_ls_wR_factor_gt          0.1836
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.150
_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
C1 C 0.5943(9) 0.5326(3) 0.4177(6) 0.082(3) Uani 1 1 d . . . . .
C2 C 0.5133(6) 0.5444(3) 0.3238(5) 0.072(2) Uani 1 1 d . . . . .
C3 C 0.4498(6) 0.4963(3) 0.2736(5) 0.0464(18) Uani 1 1 d . . . . .
C4 C 0.4414(6) 0.4354(3) 0.3099(4) 0.0329(16) Uani 1 1 d . . . . .
C5 C 0.5512(5) 0.4050(3) 0.3571(4) 0.0308(15) Uani 1 1 d . . . . .
C6 C 0.6771(6) 0.4346(3) 0.3746(4) 0.0413(17) Uani 1 1 d . . . . .
C7 C 0.7015(7) 0.4930(3) 0.4096(4) 0.058(2) Uani 1 1 d . . . . .
C8 C 0.9120(9) 0.4882(6) 0.4042(7) 0.105(4) Uani 1 1 d . . . . .
H8 H 0.993752 0.505815 0.416468 0.127 Uiso 1 1 calc R U . . .
C9 C 0.8198(10) 0.5185(4) 0.4243(6) 0.088(3) Uani 1 1 d . . . . .
H9 H 0.836493 0.557623 0.448623 0.106 Uiso 1 1 calc R U . . .
C10 C 0.8891(8) 0.4319(5) 0.3661(6) 0.079(3) Uani 1 1 d . . . . .
H10 H 0.952918 0.411691 0.349495 0.094 Uiso 1 1 calc R U . . .
C11 C 0.7721(7) 0.4058(3) 0.3528(4) 0.0519(18) Uani 1 1 d . . . . .
H11 H 0.756522 0.366821 0.327897 0.062 Uiso 1 1 calc R U . . .
C12 C 0.3980(6) 0.5049(3) 0.1849(5) 0.0498(18) Uani 1 1 d . . . . .
H12 H 0.355324 0.472277 0.150175 0.060 Uiso 1 1 calc R U . . .
C13 C 0.4066(7) 0.5593(4) 0.1456(6) 0.077(3) Uani 1 1 d . . . . .
H13 H 0.372533 0.563750 0.084969 0.092 Uiso 1 1 calc R U . . .
C14 C 0.4649(8) 0.6060(4) 0.1961(8) 0.112(4) Uani 1 1 d . . . . .
H14 H 0.468619 0.644125 0.170748 0.135 Uiso 1 1 calc R U . . .
C15 C 0.5194(8) 0.5989(4) 0.2844(8) 0.124(4) Uani 1 1 d . . . . .
H15 H 0.561400 0.632009 0.318249 0.149 Uiso 1 1 calc R U . . .
C16 C 0.3212(6) 0.4079(3) 0.2910(3) 0.0327(16) Uani 1 1 d . . . . .
C17 C 0.3142(6) 0.3481(3) 0.3153(4) 0.0373(16) Uani 1 1 d . . . . .
C18 C 0.4256(6) 0.3165(3) 0.3601(4) 0.0387(16) Uani 1 1 d . . . . .
C19 C 0.5436(6) 0.3451(3) 0.3836(3) 0.0324(16) Uani 1 1 d . . . . .
C20 C 0.6593(5) 0.3128(3) 0.4371(4) 0.0315(15) Uani 1 1 d . . . . .
C21 C 0.6977(6) 0.2594(3) 0.4107(4) 0.0419(17) Uani 1 1 d . . . . .
H21 H 0.647149 0.242241 0.357918 0.050 Uiso 1 1 calc R U . . .
C22 C 0.8072(6) 0.2298(3) 0.4581(4) 0.0458(17) Uani 1 1 d . . . . .
H22 H 0.830179 0.193247 0.436937 0.055 Uiso 1 1 calc R U . . .
C23 C 0.8832(6) 0.2526(3) 0.5355(4) 0.0452(18) Uani 1 1 d . . . . .
C24 C 0.8436(6) 0.3058(3) 0.5647(4) 0.0453(18) Uani 1 1 d . . . . .
H24 H 0.892522 0.322139 0.618580 0.054 Uiso 1 1 calc R U . . .
C25 C 0.7336(6) 0.3353(3) 0.5161(4) 0.0421(17) Uani 1 1 d . . . . .
H25 H 0.708909 0.371433 0.537341 0.051 Uiso 1 1 calc R U . . .
C26 C 0.4123(5) 0.2530(3) 0.3854(5) 0.0482(18) Uani 1 1 d . . . . .
C27 C 0.3658(6) 0.2096(3) 0.3223(5) 0.057(2) Uani 1 1 d . . . . .
H27 H 0.346404 0.220487 0.263535 0.069 Uiso 1 1 calc R U . . .
C28 C 0.3473(7) 0.1509(4) 0.3433(6) 0.076(2) Uani 1 1 d . . . . .
H28 H 0.316111 0.121551 0.299431 0.092 Uiso 1 1 calc R U . . .
C29 C 0.3745(7) 0.1354(4) 0.4284(7) 0.089(3) Uani 1 1 d . . . . .
H29 H 0.360735 0.095221 0.443228 0.107 Uiso 1 1 calc R U . . .
C30 C 0.4203(7) 0.1763(4) 0.4907(6) 0.082(3) Uani 1 1 d . . . . .
H30 H 0.439132 0.164992 0.549288 0.099 Uiso 1 1 calc R U . . .
C31 C 0.4403(6) 0.2357(3) 0.4694(5) 0.067(2) Uani 1 1 d . . . . .
H31 H 0.473776 0.264348 0.513838 0.080 Uiso 1 1 calc R U . . .
C32 C 0.1870(6) 0.3196(3) 0.3015(5) 0.0430(17) Uani 1 1 d . . . . .
C33 C 0.1198(7) 0.2913(3) 0.2259(5) 0.0549(19) Uani 1 1 d . . . . .
H33 H 0.154303 0.288919 0.179982 0.066 Uiso 1 1 calc R U . . .
C34 C 0.0012(7) 0.2661(3) 0.2167(5) 0.061(2) Uani 1 1 d . . . . .
H34 H -0.045389 0.247168 0.164270 0.073 Uiso 1 1 calc R U . . .
C35 C -0.0479(7) 0.2687(3) 0.2829(7) 0.068(2) Uani 1 1 d . . . . .
H35 H -0.128680 0.251555 0.276315 0.081 Uiso 1 1 calc R U . . .
C36 C 0.0179(8) 0.2955(4) 0.3581(6) 0.071(2) Uani 1 1 d . . . . .
H36 H -0.015986 0.296656 0.404434 0.085 Uiso 1 1 calc R U . . .
C37 C 0.1354(7) 0.3214(3) 0.3671(5) 0.0556(19) Uani 1 1 d . . . . .
H37 H 0.180744 0.340561 0.419667 0.067 Uiso 1 1 calc R U . . .
C38 C 0.1206(6) 0.4303(3) 0.1691(4) 0.0434(17) Uani 1 1 d . . . . .
H38 H 0.141400 0.399214 0.136134 0.052 Uiso 1 1 calc R U . . .
C39 C 0.2026(6) 0.4429(3) 0.2497(4) 0.0339(16) Uani 1 1 d . . . . .
C40 C 0.1704(6) 0.4900(3) 0.2933(4) 0.0443(17) Uani 1 1 d . . . . .
H40 H 0.226495 0.500911 0.348262 0.053 Uiso 1 1 calc R U . . .
C41 C 0.0580(7) 0.5220(3) 0.2591(4) 0.0541(19) Uani 1 1 d . . . . .
H41 H 0.039061 0.554221 0.291092 0.065 Uiso 1 1 calc R U . . .
C42 C -0.0276(6) 0.5077(3) 0.1784(4) 0.0459(17) Uani 1 1 d . . . . .
C43 C 0.0091(6) 0.4616(3) 0.1351(4) 0.0455(17) Uani 1 1 d . . . . .
H43 H -0.044901 0.451114 0.079295 0.055 Uiso 1 1 calc R U . . .
C44 C 1.0050(7) 0.2199(4) 0.5896(5) 0.074(2) Uani 1 1 d . U . . .
C45 C 0.9699(10) 0.1753(6) 0.6453(7) 0.166(4) Uani 1 1 d . U . . .
H45A H 1.017932 0.138130 0.647007 0.249 Uiso 1 1 calc R U . . .
H45B H 0.878883 0.166774 0.622141 0.249 Uiso 1 1 calc R U . . .
H45C H 0.989680 0.191663 0.703585 0.249 Uiso 1 1 calc R U . . .
C46 C 1.0626(8) 0.1823(5) 0.5348(5) 0.122(3) Uani 1 1 d . U . . .
H46A H 1.080401 0.207910 0.491365 0.182 Uiso 1 1 calc R U . . .
H46B H 1.003088 0.150485 0.506256 0.182 Uiso 1 1 calc R U . . .
H46C H 1.141780 0.164133 0.571273 0.182 Uiso 1 1 calc R U . . .
C48 C 1.1014(9) 0.2631(5) 0.6367(9) 0.203(5) Uani 1 1 d . U . . .
H48A H 1.075519 0.281266 0.682944 0.305 Uiso 1 1 calc R U . . .
H48B H 1.110513 0.294634 0.597317 0.305 Uiso 1 1 calc R U . . .
H48C H 1.182629 0.242338 0.661361 0.305 Uiso 1 1 calc R U . . .
C49 C -0.1579(6) 0.5378(3) 0.1416(4) 0.059(2) Uani 1 1 d . . . . .
C50 C -0.1770(7) 0.5593(3) 0.0498(4) 0.071(2) Uani 1 1 d . . . . .
H50A H -0.113116 0.589822 0.050393 0.107 Uiso 1 1 calc R U . . .
H50B H -0.261947 0.576793 0.025857 0.107 Uiso 1 1 calc R U . . .
H50C H -0.168349 0.525143 0.014378 0.107 Uiso 1 1 calc R U . . .
C51 C -0.2603(7) 0.4905(4) 0.1380(5) 0.087(3) Uani 1 1 d . . . . .
H51A H -0.247509 0.455356 0.105620 0.130 Uiso 1 1 calc R U . . .
H51B H -0.344306 0.507747 0.109438 0.130 Uiso 1 1 calc R U . . .
H51C H -0.254299 0.478286 0.196524 0.130 Uiso 1 1 calc R U . . .
C52 C -0.1729(7) 0.5915(4) 0.1952(4) 0.075(2) Uani 1 1 d . . . . .
H52A H -0.161215 0.578303 0.254276 0.113 Uiso 1 1 calc R U . . .
H52B H -0.258032 0.608568 0.170418 0.113 Uiso 1 1 calc R U . . .
H52C H -0.109302 0.622029 0.195516 0.113 Uiso 1 1 calc R U . . .
C53 C 0.5890(12) 0.6285(9) 0.4616(9) 0.062(5) Uani 0.5 1 d . . P . .
H53A H 0.641(4) 0.664(3) 0.469(5) 0.093 Uiso 0.5 1 calc R U P A 2
H53B H 0.557(7) 0.6243(19) 0.509(5) 0.093 Uiso 0.5 1 calc R U P A 2
H53C H 0.519(7) 0.632(2) 0.409(5) 0.093 Uiso 0.5 1 calc R U P A 2
C54 C 0.5239(10) 0.5059(5) 0.4731(6) 0.085(5) Uani 1 1 d . . . . .
O1A O 0.6486(7) 0.5876(3) 0.4583(5) 0.149(4) Uani 0.5 1 d . . P B 1
H1A H 0.689180 0.604185 0.429175 0.224 Uiso 0.5 1 calc R U P B 1
O1B O 0.6486(7) 0.5876(3) 0.4583(5) 0.149(4) Uani 0.5 1 d . . P B 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
C1 O1B 1.430(9) . ?
C1 O1A 1.430(9) . ?
C1 C54 1.498(13) . ?
C1 C7 1.521(11) . ?
C1 C2 1.538(11) . ?
C2 C15 1.386(11) . ?
C2 C3 1.396(9) . ?
C3 C12 1.398(9) . ?
C3 C4 1.492(8) . ?
C4 C5 1.394(8) . ?
C4 C16 1.411(8) . ?
C5 C19 1.413(8) . ?
C5 C6 1.489(8) . ?
C6 C11 1.376(8) . ?
C6 C7 1.410(9) . ?
C7 C9 1.382(11) . ?
C8 C9 1.352(13) . ?
C8 C10 1.386(13) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.377(10) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.388(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.358(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(13) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.397(8) . ?
C16 C39 1.494(8) . ?
C17 C18 1.410(8) . ?
C17 C32 1.499(8) . ?
C18 C19 1.397(8) . ?
C18 C26 1.492(9) . ?
C19 C20 1.489(8) . ?
C20 C21 1.377(8) . ?
C20 C25 1.389(8) . ?
C21 C22 1.384(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.378(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.400(8) . ?
C23 C44 1.544(9) . ?
C24 C25 1.393(8) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C31 1.367(9) . ?
C26 C27 1.389(9) . ?
C27 C28 1.382(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.375(11) . ?
C28 H28 0.9500 . ?
C29 C30 1.342(11) . ?
C29 H29 0.9500 . ?
C30 C31 1.402(10) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C37 1.372(9) . ?
C32 C33 1.379(9) . ?
C33 C34 1.396(9) . ?
C33 H33 0.9500 . ?
C34 C35 1.362(10) . ?
C34 H34 0.9500 . ?
C35 C36 1.356(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.391(9) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.375(8) . ?
C38 C43 1.376(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.378(8) . ?
C40 C41 1.392(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.399(9) . ?
C41 H41 0.9500 . ?
C42 C43 1.380(8) . ?
C42 C49 1.535(9) . ?
C43 H43 0.9500 . ?
C44 C48 1.463(12) . ?
C44 C45 1.482(12) . ?
C44 C46 1.511(10) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C52 1.521(9) . ?
C49 C50 1.529(9) . ?
C49 C51 1.537(10) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 O1B 1.137(15) . ?
C53 H53A 0.96(8) . ?
C53 H53B 0.96(7) . ?
C53 H53C 0.96(7) . ?
C54 C54 1.20(2) 3_666 ?
O1Aa H1A 0.8400 . ?

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
O1Bb C1 C54 106.2(9) . . ?
O1Aa C1 C54 106.2(9) . . ?
O1Bb C1 C7 108.0(7) . . ?
O1Aa C1 C7 108.0(7) . . ?
C54 C1 C7 113.5(7) . . ?
O1Bb C1 C2 110.3(7) . . ?
O1Aa C1 C2 110.3(7) . . ?
C54 C1 C2 115.0(7) . . ?
C7 C1 C2 103.7(8) . . ?
C15 C2 C3 119.0(7) . . ?
C15 C2 C1 121.0(7) . . ?
C3 C2 C1 119.0(7) . . ?
C2 C3 C12 118.2(6) . . ?
C2 C3 C4 122.9(6) . . ?
C12 C3 C4 118.8(6) . . ?
C5 C4 C16 120.9(5) . . ?
C5 C4 C3 120.3(5) . . ?
C16 C4 C3 118.6(5) . . ?
C4 C5 C19 120.0(5) . . ?
C4 C5 C6 119.8(6) . . ?
C19 C5 C6 120.1(5) . . ?
C11 C6 C7 118.0(6) . . ?
C11 C6 C5 119.8(6) . . ?
C7 C6 C5 122.1(6) . . ?
C9 C7 C6 119.8(7) . . ?
C9 C7 C1 118.5(8) . . ?
C6 C7 C1 120.9(6) . . ?
C9 C8 C10 121.0(8) . . ?
C9 C8 H8 119.5 . . ?
C10 C8 H8 119.5 . . ?
C8 C9 C7 120.5(9) . . ?
C8 C9 H9 119.7 . . ?
C7 C9 H9 119.7 . . ?
C11 C10 C8 118.7(8) . . ?
C11 C10 H10 120.6 . . ?
C8 C10 H10 120.6 . . ?
C10 C11 C6 121.9(7) . . ?
C10 C11 H11 119.1 . . ?
C6 C11 H11 119.1 . . ?
C13 C12 C3 122.5(7) . . ?
C13 C12 H12 118.8 . . ?
C3 C12 H12 118.8 . . ?
C14 C13 C12 118.2(8) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C13 C14 C15 121.0(7) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C2 C15 C14 121.1(8) . . ?
C2 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C17 C16 C4 118.9(5) . . ?
C17 C16 C39 120.2(5) . . ?
C4 C16 C39 120.8(5) . . ?
C16 C17 C18 120.2(5) . . ?
C16 C17 C32 119.7(6) . . ?
C18 C17 C32 119.9(6) . . ?
C19 C18 C17 120.7(5) . . ?
C19 C18 C26 121.3(6) . . ?
C17 C18 C26 117.9(6) . . ?
C18 C19 C5 119.1(5) . . ?
C18 C19 C20 120.3(5) . . ?
C5 C19 C20 120.7(5) . . ?
C21 C20 C25 116.8(5) . . ?
C21 C20 C19 121.7(5) . . ?
C25 C20 C19 121.5(6) . . ?
C20 C21 C22 122.6(6) . . ?
C20 C21 H21 118.7 . . ?
C22 C21 H21 118.7 . . ?
C23 C22 C21 121.0(6) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 117.3(6) . . ?
C22 C23 C44 121.7(7) . . ?
C24 C23 C44 121.0(7) . . ?
C25 C24 C23 121.1(6) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C20 C25 C24 121.2(6) . . ?
C20 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C31 C26 C27 117.9(6) . . ?
C31 C26 C18 122.3(7) . . ?
C27 C26 C18 119.8(6) . . ?
C28 C27 C26 121.4(7) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C29 C28 C27 119.1(8) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C30 C29 C28 120.8(8) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 120.0(8) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C26 C31 C30 120.8(8) . . ?
C26 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C37 C32 C33 118.4(6) . . ?
C37 C32 C17 118.7(6) . . ?
C33 C32 C17 122.9(6) . . ?
C32 C33 C34 120.2(7) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C35 C34 C33 120.1(7) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C36 C35 C34 120.4(7) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 C37 119.6(7) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C32 C37 C36 121.2(7) . . ?
C32 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?
C39 C38 C43 121.6(6) . . ?
C39 C38 H38 119.2 . . ?
C43 C38 H38 119.2 . . ?
C38 C39 C40 116.9(5) . . ?
C38 C39 C16 123.3(6) . . ?
C40 C39 C16 119.8(6) . . ?
C39 C40 C41 121.8(6) . . ?
C39 C40 H40 119.1 . . ?
C41 C40 H40 119.1 . . ?
C40 C41 C42 121.2(6) . . ?
C40 C41 H41 119.4 . . ?
C42 C41 H41 119.4 . . ?
C43 C42 C41 115.6(6) . . ?
C43 C42 C49 121.2(6) . . ?
C41 C42 C49 123.0(6) . . ?
C38 C43 C42 122.9(6) . . ?
C38 C43 H43 118.6 . . ?
C42 C43 H43 118.6 . . ?
C48 C44 C45 113.9(9) . . ?
C48 C44 C46 107.4(8) . . ?
C45 C44 C46 104.0(8) . . ?
C48 C44 C23 110.9(7) . . ?
C45 C44 C23 108.3(6) . . ?
C46 C44 C23 112.3(6) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C52 C49 C50 108.6(6) . . ?
C52 C49 C42 112.3(6) . . ?
C50 C49 C42 110.0(6) . . ?
C52 C49 C51 110.0(6) . . ?
C50 C49 C51 107.8(6) . . ?
C42 C49 C51 108.1(6) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C49 C52 H52A 109.5 . . ?
C49 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C49 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O1Bb C53 H53A 109.5 . . ?
O1Bb C53 H53B 109.5 . . ?
H53Ab C53 H53B 109.5 . . ?
O1Bb C53 H53C 109.5 . . ?
H53Ab C53 H53C 109.5 . . ?
H53Bb C53 H53C 109.5 . . ?
C54 C54 C1 167.5(15) 3_666 . ?
C1 O1Aa H1A 109.5 . . ?
C53 O1Bb C1 122.7(10) . . ?

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
O1Bb C1 C2 C15 12.4(14) . . . . ?
O1Aa C1 C2 C15 12.4(14) . . . . ?
C54 C1 C2 C15 132.5(9) . . . . ?
C7 C1 C2 C15 -103.0(9) . . . . ?
O1Bb C1 C2 C3 -178.6(8) . . . . ?
O1Aa C1 C2 C3 -178.6(8) . . . . ?
C54 C1 C2 C3 -58.5(10) . . . . ?
C7 C1 C2 C3 66.0(9) . . . . ?
C15 C2 C3 C12 1.8(11) . . . . ?
C1 C2 C3 C12 -167.4(7) . . . . ?
C15 C2 C3 C4 178.3(7) . . . . ?
C1 C2 C3 C4 9.0(11) . . . . ?
C2 C3 C4 C5 -54.6(8) . . . . ?
C12 C3 C4 C5 121.8(6) . . . . ?
C2 C3 C4 C16 129.3(6) . . . . ?
C12 C3 C4 C16 -54.3(8) . . . . ?
C16 C4 C5 C19 2.6(8) . . . . ?
C3 C4 C5 C19 -173.4(5) . . . . ?
C16 C4 C5 C6 178.7(5) . . . . ?
C3 C4 C5 C6 2.7(8) . . . . ?
C4 C5 C6 C11 -126.1(6) . . . . ?
C19 C5 C6 C11 50.0(8) . . . . ?
C4 C5 C6 C7 51.0(8) . . . . ?
C19 C5 C6 C7 -132.9(6) . . . . ?
C11 C6 C7 C9 -2.6(9) . . . . ?
C5 C6 C7 C9 -179.7(6) . . . . ?
C11 C6 C7 C1 167.0(7) . . . . ?
C5 C6 C7 C1 -10.1(10) . . . . ?
O1Bb C1 C7 C9 -12.6(11) . . . . ?
O1Aa C1 C7 C9 -12.6(11) . . . . ?
C54 C1 C7 C9 -130.1(8) . . . . ?
C2 C1 C7 C9 104.5(7) . . . . ?
O1Bb C1 C7 C6 177.7(7) . . . . ?
O1Aa C1 C7 C6 177.7(7) . . . . ?
C54 C1 C7 C6 60.2(9) . . . . ?
C2 C1 C7 C6 -65.3(9) . . . . ?
C10 C8 C9 C7 2.1(13) . . . . ?
C6 C7 C9 C8 0.9(11) . . . . ?
C1 C7 C9 C8 -169.0(8) . . . . ?
C9 C8 C10 C11 -3.2(12) . . . . ?
C8 C10 C11 C6 1.4(10) . . . . ?
C7 C6 C11 C10 1.4(9) . . . . ?
C5 C6 C11 C10 178.6(6) . . . . ?
C2 C3 C12 C13 -0.6(10) . . . . ?
C4 C3 C12 C13 -177.2(6) . . . . ?
C3 C12 C13 C14 -1.7(11) . . . . ?
C12 C13 C14 C15 2.7(13) . . . . ?
C3 C2 C15 C14 -0.9(14) . . . . ?
C1 C2 C15 C14 168.2(9) . . . . ?
C13 C14 C15 C2 -1.5(15) . . . . ?
C5 C4 C16 C17 -4.2(8) . . . . ?
C3 C4 C16 C17 171.9(5) . . . . ?
C5 C4 C16 C39 172.6(5) . . . . ?
C3 C4 C16 C39 -11.3(8) . . . . ?
C4 C16 C17 C18 1.7(8) . . . . ?
C39 C16 C17 C18 -175.2(5) . . . . ?
C4 C16 C17 C32 175.5(5) . . . . ?
C39 C16 C17 C32 -1.3(8) . . . . ?
C16 C17 C18 C19 2.4(9) . . . . ?
C32 C17 C18 C19 -171.4(6) . . . . ?
C16 C17 C18 C26 179.3(6) . . . . ?
C32 C17 C18 C26 5.5(9) . . . . ?
C17 C18 C19 C5 -4.0(8) . . . . ?
C26 C18 C19 C5 179.2(6) . . . . ?
C17 C18 C19 C20 175.0(5) . . . . ?
C26 C18 C19 C20 -1.8(9) . . . . ?
C4 C5 C19 C18 1.5(8) . . . . ?
C6 C5 C19 C18 -174.6(5) . . . . ?
C4 C5 C19 C20 -177.5(5) . . . . ?
C6 C5 C19 C20 6.4(8) . . . . ?
C18 C19 C20 C21 58.5(8) . . . . ?
C5 C19 C20 C21 -122.5(6) . . . . ?
C18 C19 C20 C25 -121.5(6) . . . . ?
C5 C19 C20 C25 57.5(7) . . . . ?
C25 C20 C21 C22 -2.2(8) . . . . ?
C19 C20 C21 C22 177.8(5) . . . . ?
C20 C21 C22 C23 0.6(9) . . . . ?
C21 C22 C23 C24 1.4(9) . . . . ?
C21 C22 C23 C44 179.5(6) . . . . ?
C22 C23 C24 C25 -1.8(9) . . . . ?
C44 C23 C24 C25 -179.9(6) . . . . ?
C21 C20 C25 C24 1.8(8) . . . . ?
C19 C20 C25 C24 -178.2(5) . . . . ?
C23 C24 C25 C20 0.1(9) . . . . ?
C19 C18 C26 C31 63.5(9) . . . . ?
C17 C18 C26 C31 -113.3(7) . . . . ?
C19 C18 C26 C27 -118.7(6) . . . . ?
C17 C18 C26 C27 64.4(8) . . . . ?
C31 C26 C27 C28 0.5(9) . . . . ?
C18 C26 C27 C28 -177.3(6) . . . . ?
C26 C27 C28 C29 0.5(10) . . . . ?
C27 C28 C29 C30 -1.0(12) . . . . ?
C28 C29 C30 C31 0.3(12) . . . . ?
C27 C26 C31 C30 -1.2(10) . . . . ?
C18 C26 C31 C30 176.6(6) . . . . ?
C29 C30 C31 C26 0.8(11) . . . . ?
C16 C17 C32 C37 -92.6(7) . . . . ?
C18 C17 C32 C37 81.2(8) . . . . ?
C16 C17 C32 C33 87.8(8) . . . . ?
C18 C17 C32 C33 -98.4(7) . . . . ?
C37 C32 C33 C34 1.1(9) . . . . ?
C17 C32 C33 C34 -179.3(6) . . . . ?
C32 C33 C34 C35 -0.9(10) . . . . ?
C33 C34 C35 C36 -0.1(11) . . . . ?
C34 C35 C36 C37 1.0(11) . . . . ?
C33 C32 C37 C36 -0.2(9) . . . . ?
C17 C32 C37 C36 -179.8(6) . . . . ?
C35 C36 C37 C32 -0.8(10) . . . . ?
C43 C38 C39 C40 -2.6(9) . . . . ?
C43 C38 C39 C16 176.7(6) . . . . ?
C17 C16 C39 C38 -67.6(8) . . . . ?
C4 C16 C39 C38 115.6(6) . . . . ?
C17 C16 C39 C40 111.7(6) . . . . ?
C4 C16 C39 C40 -65.1(7) . . . . ?
C38 C39 C40 C41 2.3(9) . . . . ?
C16 C39 C40 C41 -177.0(6) . . . . ?
C39 C40 C41 C42 0.0(10) . . . . ?
C40 C41 C42 C43 -2.0(9) . . . . ?
C40 C41 C42 C49 174.3(6) . . . . ?
C39 C38 C43 C42 0.5(9) . . . . ?
C41 C42 C43 C38 1.8(9) . . . . ?
C49 C42 C43 C38 -174.6(6) . . . . ?
C22 C23 C44 C48 147.7(9) . . . . ?
C24 C23 C44 C48 -34.3(11) . . . . ?
C22 C23 C44 C45 -86.7(9) . . . . ?
C24 C23 C44 C45 91.3(9) . . . . ?
C22 C23 C44 C46 27.6(10) . . . . ?
C24 C23 C44 C46 -154.4(7) . . . . ?
C43 C42 C49 C52 -174.1(6) . . . . ?
C41 C42 C49 C52 9.7(9) . . . . ?
C43 C42 C49 C50 -53.1(8) . . . . ?
C41 C42 C49 C50 130.7(7) . . . . ?
C43 C42 C49 C51 64.4(8) . . . . ?
C41 C42 C49 C51 -111.8(7) . . . . ?
O1Bb C1 C54 C54 -1(6) . . . 3_666 ?
O1Aa C1 C54 C54 -1(6) . . . 3_666 ?
C7 C1 C54 C54 118(6) . . . 3_666 ?
C2 C1 C54 C54 -123(6) . . . 3_666 ?
C54 C1 O1Bb C53 -69.2(15) . . . . ?
C7 C1 O1Bb C53 168.8(13) . . . . ?
C2 C1 O1Bb C53 56.1(18) . . . . ?

_refine_diff_density_max         0.420
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.053


# start Validation Reply Form
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A full set of data was collected, however at very high 
angle only noise was mainly observed and these data were omitted.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1817321'
_audit_update_record             
;
2018-01-16 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C109 H93 Cl15'
_chemical_formula_weight         1934.58

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

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

_cell_length_a                   11.3561(10)
_cell_length_b                   27.561(3)
_cell_length_c                   31.571(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9881.1(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9064
_cell_measurement_theta_min      3.2265
_cell_measurement_theta_max      59.071

_exptl_crystal_description       'irregular block'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_F_000             4008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    4.188
_shelx_estimated_absorpt_T_min   0.473
_shelx_estimated_absorpt_T_max   0.656
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8435
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0761 after correction.
The ratio of minimum to maximum apparent transmission was 0.8435.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            73156
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.128
_diffrn_reflns_theta_max         59.072
_diffrn_reflns_theta_full        59.072
_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             14174
_reflns_number_gt                13473
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.996

_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 APEX3'
_computing_data_reduction        'Bruker SAINT V8.37A'
_computing_structure_solution    'SIR2014 (Burla et al. 2014)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep 3 and Chimera 1.10.1'
_computing_publication_material  'WinGX CIF routines'
_refine_special_details          
;
 Refined as a 2-component inversion twin.

Due to the limited quality of the crystals obtained, the thermal
ellipsoids of some atoms had to be modelled by using ISOR restraints.

Moreover, there was some disorder in a chloroform solvent molecule
which was modelled by using SIMU and DELU restraints.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         14174
_refine_ls_number_parameters     1130
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.1095
_refine_ls_wR_factor_ref         0.3233
_refine_ls_wR_factor_gt          0.3178
_refine_ls_goodness_of_fit_ref   1.588
_refine_ls_restrained_S_all      1.586
_refine_ls_shift/su_max          0.174
_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
CL6 Cl 0.4111(3) 0.99930(11) 0.39113(10) 0.0577(8) Uani 1 1 d . . . . .
C1A C 0.2332(6) 0.0692(2) 0.5001(2) 0.0106(14) Uani 1 1 d . . . . .
C2 C 0.2492(6) 0.0976(3) 0.4602(2) 0.0151(15) Uani 1 1 d . . . . .
CL2 Cl 0.5015(3) 0.00195(14) 0.57352(10) 0.0756(10) Uani 1 1 d . . . . .
CL3 Cl 0.5682(4) 0.00635(13) 0.48541(9) 0.0750(10) Uani 1 1 d . . . . .
C3A C 0.3213(6) 0.1391(2) 0.4595(2) 0.0132(14) Uani 1 1 d . . . . .
C4 C 0.4080(7) 0.1478(2) 0.4932(2) 0.0146(15) Uani 1 1 d . . . . .
CL1 Cl 0.7437(4) -0.00932(18) 0.54937(14) 0.0909(12) Uani 1 1 d . . . . .
C5 C 0.3752(6) 0.1482(2) 0.5366(2) 0.0119(15) Uani 1 1 d . . . . .
CL5 Cl 0.2210(4) 1.00111(13) 0.33140(13) 0.0925(14) Uani 1 1 d . . . . .
C6 C 0.2492(6) 0.1407(3) 0.5483(2) 0.0131(15) Uani 1 1 d . . . . .
C7 C 0.1895(6) 0.0990(2) 0.5353(2) 0.0128(14) Uani 1 1 d . U . . .
C8A C 0.1791(6) 0.0860(3) 0.4251(2) 0.0173(15) Uani 1 1 d . . . . .
H8A H 0.134602 0.056818 0.425220 0.021 Uiso 1 1 calc R U . . .
CL4 Cl 0.4657(6) 1.01101(18) 0.30374(13) 0.1132(19) Uani 1 1 d . . . . .
C9A C 0.1738(7) 0.1163(3) 0.3902(2) 0.0255(18) Uani 1 1 d . . . . .
H9A H 0.126194 0.108078 0.366487 0.031 Uiso 1 1 calc R U . . .
C10 C 0.2391(8) 0.1589(3) 0.3904(2) 0.0284(19) Uani 1 1 d . . . . .
H10 H 0.232944 0.180667 0.367097 0.034 Uiso 1 1 calc R U . . .
C11 C 0.3117(6) 0.1702(3) 0.4233(2) 0.0137(14) Uani 1 1 d . . . . .
H11 H 0.356940 0.199156 0.422188 0.016 Uiso 1 1 calc R U . . .
C12 C 0.0756(7) 0.0892(3) 0.5522(2) 0.0222(17) Uani 1 1 d . . . . .
H12 H 0.035172 0.060368 0.544341 0.027 Uiso 1 1 calc R U . . .
C13 C 0.0240(8) 0.1216(3) 0.5798(3) 0.0309(19) Uani 1 1 d . . . . .
H13 H -0.051341 0.114572 0.591384 0.037 Uiso 1 1 calc R U . . .
C14 C 0.0804(7) 0.1638(3) 0.5908(2) 0.0216(17) Uani 1 1 d . . . . .
H14 H 0.042239 0.186895 0.608365 0.026 Uiso 1 1 calc R U . . .
C15 C 0.1938(7) 0.1726(3) 0.5759(2) 0.0173(15) Uani 1 1 d . . . . .
H15 H 0.234225 0.200933 0.584907 0.021 Uiso 1 1 calc R U . . .
C16 C 0.5270(6) 0.1569(2) 0.4823(2) 0.0088(13) Uani 1 1 d . U . . .
C17 C 0.6126(6) 0.1637(2) 0.5142(2) 0.0120(14) Uani 1 1 d . . . . .
C18 C 0.5795(7) 0.1618(2) 0.5574(2) 0.0142(15) Uani 1 1 d . . . . .
C19 C 0.4594(6) 0.1545(2) 0.5676(2) 0.0109(14) Uani 1 1 d . U . . .
C20 C 0.5661(6) 0.1581(3) 0.4369(2) 0.0129(14) Uani 1 1 d . . . . .
C21 C 0.5629(7) 0.1181(3) 0.4113(2) 0.0173(16) Uani 1 1 d . . . . .
H21 H 0.536021 0.088176 0.422637 0.021 Uiso 1 1 calc R U . . .
C22 C 0.5976(7) 0.1199(3) 0.3694(2) 0.0215(17) Uani 1 1 d . . . . .
H22 H 0.591126 0.091552 0.352423 0.026 Uiso 1 1 calc R U . . .
C23 C 0.6422(7) 0.1627(3) 0.3513(2) 0.0204(16) Uani 1 1 d . . . . .
C24 C 0.6433(8) 0.2042(3) 0.3784(2) 0.0244(18) Uani 1 1 d . . . . .
H24 H 0.667956 0.234568 0.367260 0.029 Uiso 1 1 calc R U . . .
C25 C 0.6100(7) 0.2012(3) 0.4196(2) 0.0183(16) Uani 1 1 d . . . . .
H25 H 0.616669 0.229081 0.437169 0.022 Uiso 1 1 calc R U . . .
C26 C 0.7390(7) 0.1692(3) 0.5018(2) 0.0157(15) Uani 1 1 d . . . . .
C27 C 0.8010(7) 0.1292(3) 0.4871(2) 0.0212(17) Uani 1 1 d . . . . .
H27 H 0.764627 0.098143 0.487862 0.025 Uiso 1 1 calc R U . . .
C28 C 0.9146(8) 0.1333(3) 0.4713(3) 0.0290(19) Uani 1 1 d . . . . .
H28 H 0.954049 0.105725 0.460123 0.035 Uiso 1 1 calc R U . . .
C29 C 0.9706(8) 0.1787(3) 0.4720(2) 0.0282(19) Uani 1 1 d . . . . .
H29 H 1.049719 0.181849 0.462567 0.034 Uiso 1 1 calc R U . . .
C30 C 0.9093(7) 0.2191(3) 0.4865(2) 0.0208(16) Uani 1 1 d . . . . .
H30 H 0.946073 0.250069 0.486493 0.025 Uiso 1 1 calc R U . . .
C31 C 0.7948(7) 0.2143(3) 0.5011(2) 0.0189(16) Uani 1 1 d . . . . .
H31 H 0.753565 0.242196 0.510664 0.023 Uiso 1 1 calc R U . . .
C32 C 0.6695(6) 0.1642(3) 0.5918(2) 0.0162(15) Uani 1 1 d . . . . .
C33 C 0.7255(7) 0.2068(3) 0.6023(2) 0.0187(16) Uani 1 1 d . . . . .
H33 H 0.710898 0.235338 0.586239 0.022 Uiso 1 1 calc R U . . .
C34 C 0.8023(7) 0.2086(3) 0.6359(2) 0.0266(19) Uani 1 1 d . . . . .
H34 H 0.840773 0.238115 0.642834 0.032 Uiso 1 1 calc R U . . .
C35 C 0.8238(8) 0.1667(4) 0.6599(2) 0.034(2) Uani 1 1 d . . . . .
H35 H 0.877225 0.167979 0.683017 0.041 Uiso 1 1 calc R U . . .
C36 C 0.7688(8) 0.1244(4) 0.6503(2) 0.031(2) Uani 1 1 d . . . . .
H36 H 0.783149 0.096072 0.666714 0.037 Uiso 1 1 calc R U . . .
C37 C 0.6913(7) 0.1230(3) 0.6163(2) 0.0262(18) Uani 1 1 d . . . . .
H37 H 0.652431 0.093438 0.609596 0.031 Uiso 1 1 calc R U . . .
C38 C 0.4268(6) 0.1526(3) 0.6129(2) 0.0132(15) Uani 1 1 d . . . . .
C39 C 0.4428(7) 0.1926(3) 0.6401(2) 0.0173(16) Uani 1 1 d . . . . .
H39 H 0.473850 0.221956 0.629056 0.021 Uiso 1 1 calc R U . . .
C40 C 0.4141(7) 0.1897(3) 0.6828(2) 0.0219(17) Uani 1 1 d . . . . .
H40 H 0.427187 0.217133 0.700467 0.026 Uiso 1 1 calc R U . . .
C41 C 0.3672(7) 0.1482(3) 0.7001(3) 0.0254(18) Uani 1 1 d . . . . .
C42 C 0.3473(7) 0.1084(3) 0.6736(2) 0.0238(17) Uani 1 1 d . . . . .
H42 H 0.313748 0.079501 0.684789 0.029 Uiso 1 1 calc R U . . .
C43 C 0.3762(6) 0.1109(3) 0.6311(2) 0.0168(16) Uani 1 1 d . . . . .
H43 H 0.361479 0.083531 0.613620 0.020 Uiso 1 1 calc R U . . .
C44 C 0.2398(6) 0.0216(3) 0.5006(2) 0.0184(17) Uani 1 1 d . . . . .
C45 C 0.2469(6) -0.0242(3) 0.5016(2) 0.0192(17) Uani 1 1 d . . . . .
C46 C 0.2554(6) -0.0729(3) 0.5015(2) 0.0148(15) Uani 1 1 d . . . . .
C47 C 0.2776(6) -0.1001(2) 0.4611(2) 0.0129(14) Uani 1 1 d . . . . .
C48 C 0.3539(6) -0.1401(3) 0.4610(2) 0.0141(15) Uani 1 1 d . . . . .
C49 C 0.4419(6) -0.1476(2) 0.4953(2) 0.0111(14) Uani 1 1 d . . . . .
C50 C 0.4080(6) -0.1491(2) 0.5381(2) 0.0117(14) Uani 1 1 d . U . . .
C51 C 0.2809(6) -0.1445(3) 0.5500(2) 0.0130(15) Uani 1 1 d . . . . .
C52 C 0.2143(7) -0.1036(2) 0.5367(2) 0.0154(15) Uani 1 1 d . . . . .
C53 C 0.1037(7) -0.0955(3) 0.5541(3) 0.0231(17) Uani 1 1 d . . . . .
H53 H 0.061389 -0.067012 0.546762 0.028 Uiso 1 1 calc R U . . .
C54 C 0.0548(7) -0.1282(3) 0.5818(2) 0.0270(19) Uani 1 1 d . . . . .
H54 H -0.020349 -0.122013 0.593908 0.032 Uiso 1 1 calc R U . . .
C55 C 0.1156(7) -0.1707(3) 0.5923(3) 0.0253(18) Uani 1 1 d . . . . .
H55 H 0.079777 -0.194647 0.609702 0.030 Uiso 1 1 calc R U . . .
C56 C 0.2274(6) -0.1774(3) 0.5772(2) 0.0151(15) Uani 1 1 d . . . . .
H56 H 0.269852 -0.205518 0.585575 0.018 Uiso 1 1 calc R U . . .
C57 C 0.2105(7) -0.0890(3) 0.4258(2) 0.0200(16) Uani 1 1 d . . . . .
H57 H 0.162885 -0.060613 0.425663 0.024 Uiso 1 1 calc R U . . .
C58 C 0.2126(7) -0.1193(3) 0.3906(2) 0.0249(18) Uani 1 1 d . . . . .
H58 H 0.167789 -0.111280 0.366158 0.030 Uiso 1 1 calc R U . . .
C59 C 0.2802(7) -0.1612(3) 0.3911(2) 0.0232(17) Uani 1 1 d . . . . .
H59 H 0.278119 -0.183161 0.367881 0.028 Uiso 1 1 calc R U . . .
C60 C 0.3501(7) -0.1705(3) 0.4256(2) 0.0167(15) Uani 1 1 d . . . . .
H60 H 0.398019 -0.198737 0.425379 0.020 Uiso 1 1 calc R U . . .
C61 C 0.5612(6) -0.1540(2) 0.4850(2) 0.0123(14) Uani 1 1 d . . . . .
C62 C 0.6455(6) -0.1626(2) 0.5165(2) 0.0121(14) Uani 1 1 d . . . . .
C63 C 0.6105(7) -0.1618(2) 0.5594(2) 0.0141(15) Uani 1 1 d . . . . .
C64 C 0.5997(6) -0.1528(3) 0.4395(2) 0.0135(15) Uani 1 1 d . . . . .
C64A C 0.4924(7) -0.1553(2) 0.5704(2) 0.0128(14) Uani 1 1 d . . . . .
C65 C 0.5855(6) -0.1114(3) 0.4157(2) 0.0160(15) Uani 1 1 d . . . . .
H65 H 0.559583 -0.082355 0.428945 0.019 Uiso 1 1 calc R U . . .
C66 C 0.6087(7) -0.1116(3) 0.3721(2) 0.0213(17) Uani 1 1 d . . . . .
H66 H 0.597786 -0.082908 0.355853 0.026 Uiso 1 1 calc R U . . .
C67 C 0.6489(8) -0.1550(3) 0.3520(3) 0.0266(19) Uani 1 1 d . . . . .
C68 C 0.6678(7) -0.1947(3) 0.3762(2) 0.0211(17) Uani 1 1 d . U . . .
H68 H 0.697418 -0.223407 0.363404 0.025 Uiso 1 1 calc R U . . .
C69 C 0.6442(7) -0.1942(3) 0.4199(2) 0.0202(16) Uani 1 1 d . . . . .
H69 H 0.658890 -0.222429 0.436248 0.024 Uiso 1 1 calc R U . . .
C70 C 0.7715(7) -0.1689(3) 0.5042(2) 0.0147(15) Uani 1 1 d . . . . .
C71A C 0.8352(7) -0.1288(3) 0.4893(3) 0.0231(17) Uani 1 1 d . . . . .
H71A H 0.800441 -0.097498 0.489862 0.028 Uiso 1 1 calc R U . . .
C72 C 0.9507(8) -0.1346(3) 0.4736(3) 0.0287(19) Uani 1 1 d . . . . .
H72 H 0.993265 -0.107113 0.463808 0.034 Uiso 1 1 calc R U . . .
C73 C 1.0022(7) -0.1799(3) 0.4722(2) 0.0235(17) Uani 1 1 d . . . . .
H73 H 1.079556 -0.183932 0.461298 0.028 Uiso 1 1 calc R U . . .
C74 C 0.9382(7) -0.2201(3) 0.4874(2) 0.0215(17) Uani 1 1 d . . . . .
H74 H 0.973003 -0.251420 0.487073 0.026 Uiso 1 1 calc R U . . .
C75 C 0.8259(7) -0.2143(3) 0.5027(2) 0.0197(16) Uani 1 1 d . . . . .
H75 H 0.784047 -0.241913 0.512508 0.024 Uiso 1 1 calc R U . . .
C76 C 0.6999(7) -0.1640(3) 0.5948(2) 0.0193(16) Uani 1 1 d . . . . .
C77 C 0.7214(7) -0.1241(3) 0.6196(2) 0.0224(17) Uani 1 1 d . . . . .
H77 H 0.683084 -0.094328 0.613403 0.027 Uiso 1 1 calc R U . . .
C78 C 0.7978(8) -0.1266(4) 0.6535(2) 0.031(2) Uani 1 1 d . . . . .
H78 H 0.810425 -0.098670 0.670509 0.038 Uiso 1 1 calc R U . . .
C79 C 0.8560(8) -0.1689(4) 0.6630(2) 0.032(2) Uani 1 1 d . . . . .
H79 H 0.908579 -0.170187 0.686360 0.038 Uiso 1 1 calc R U . . .
C80 C 0.8374(7) -0.2099(3) 0.6382(2) 0.0278(19) Uani 1 1 d . . . . .
H80 H 0.878365 -0.239078 0.644329 0.033 Uiso 1 1 calc R U . . .
C81 C 0.7591(7) -0.2081(3) 0.6046(2) 0.0195(16) Uani 1 1 d . . . . .
H81 H 0.744956 -0.236363 0.588117 0.023 Uiso 1 1 calc R U . . .
C82 C 0.4547(6) -0.1546(3) 0.6157(2) 0.0153(15) Uani 1 1 d . . . . .
C83 C 0.4003(7) -0.1136(3) 0.6328(2) 0.0239(17) Uani 1 1 d . . . . .
H83 H 0.392176 -0.084976 0.616374 0.029 Uiso 1 1 calc R U . . .
C84 C 0.3586(8) -0.1151(3) 0.6736(3) 0.0284(19) Uani 1 1 d . . . . .
H84 H 0.320515 -0.087157 0.684597 0.034 Uiso 1 1 calc R U . . .
C85 C 0.3693(7) -0.1554(3) 0.6993(2) 0.0245(18) Uani 1 1 d . . . . .
C86 C 0.4288(7) -0.1953(3) 0.6825(2) 0.0234(17) Uani 1 1 d . . . . .
H86 H 0.441320 -0.223209 0.699681 0.028 Uiso 1 1 calc R U . . .
C87 C 0.4703(6) -0.1948(3) 0.6407(2) 0.0190(16) Uani 1 1 d . . . . .
H87 H 0.509427 -0.222517 0.629541 0.023 Uiso 1 1 calc R U . . .
C88 C 0.3373(9) 0.1434(4) 0.7468(3) 0.042(2) Uani 1 1 d . . . . .
C89 C 0.2063(12) 0.1357(7) 0.7531(3) 0.075(4) Uani 1 1 d . . . . .
H89A H 0.162547 0.157518 0.734228 0.112 Uiso 1 1 calc R U . . .
H89B H 0.185480 0.142761 0.782555 0.112 Uiso 1 1 calc R U . . .
H89C H 0.186133 0.102009 0.746446 0.112 Uiso 1 1 calc R U . . .
C90 C 0.3747(11) 0.1885(4) 0.7728(3) 0.049(3) Uani 1 1 d . . . . .
H90A H 0.458871 0.194681 0.768443 0.074 Uiso 1 1 calc R U . . .
H90B H 0.359683 0.182660 0.802888 0.074 Uiso 1 1 calc R U . . .
H90C H 0.329319 0.216773 0.763349 0.074 Uiso 1 1 calc R U . . .
C91 C 0.4040(13) 0.0992(4) 0.7660(3) 0.053(3) Uani 1 1 d . . . . .
H91A H 0.377626 0.069371 0.752115 0.079 Uiso 1 1 calc R U . . .
H91B H 0.387427 0.097238 0.796446 0.079 Uiso 1 1 calc R U . . .
H91C H 0.488809 0.103338 0.761643 0.079 Uiso 1 1 calc R U . . .
C92 C 0.6857(10) 0.1664(3) 0.3068(3) 0.040(2) Uani 1 1 d . . . . .
C93 C 0.6331(14) 0.2101(4) 0.2835(3) 0.057(3) Uani 1 1 d . . . . .
H93A H 0.547572 0.210584 0.287563 0.085 Uiso 1 1 calc R U . . .
H93B H 0.651018 0.207692 0.253233 0.085 Uiso 1 1 calc R U . . .
H93C H 0.667184 0.240121 0.294877 0.085 Uiso 1 1 calc R U . . .
C94 C 0.6597(11) 0.1210(4) 0.2806(3) 0.044(3) Uani 1 1 d . . . . .
H94A H 0.685679 0.092223 0.296194 0.065 Uiso 1 1 calc R U . . .
H94B H 0.701783 0.122950 0.253575 0.065 Uiso 1 1 calc R U . . .
H94C H 0.574809 0.118876 0.275274 0.065 Uiso 1 1 calc R U . . .
C95 C 0.8180(12) 0.1723(5) 0.3072(4) 0.063(4) Uani 1 1 d . . . . .
H95A H 0.838985 0.201301 0.323454 0.095 Uiso 1 1 calc R U . . .
H95B H 0.846615 0.175663 0.278056 0.095 Uiso 1 1 calc R U . . .
H95C H 0.854059 0.143683 0.320281 0.095 Uiso 1 1 calc R U . . .
C96 C 0.6716(11) -0.1561(4) 0.3043(3) 0.044(3) Uani 1 1 d . U . . .
C97 C 0.6316(14) -0.1091(4) 0.2814(3) 0.059(3) Uani 1 1 d . . . . .
H97A H 0.685791 -0.082629 0.288304 0.088 Uiso 1 1 calc R U . . .
H97B H 0.551898 -0.100547 0.290601 0.088 Uiso 1 1 calc R U . . .
H97C H 0.631801 -0.114552 0.250677 0.088 Uiso 1 1 calc R U . . .
C98 C 0.8025(14) -0.1690(5) 0.2968(4) 0.068(4) Uani 1 1 d . . . . .
H98A H 0.852610 -0.144284 0.309993 0.102 Uiso 1 1 calc R U . . .
H98B H 0.818343 -0.170153 0.266317 0.102 Uiso 1 1 calc R U . . .
H98C H 0.819515 -0.200722 0.309412 0.102 Uiso 1 1 calc R U . . .
C99A C 0.5958(11) -0.1993(4) 0.2857(3) 0.047(3) Uani 1 1 d . . . . .
H99A H 0.616428 -0.204322 0.255835 0.070 Uiso 1 1 calc R U . . .
H99B H 0.511919 -0.191298 0.287883 0.070 Uiso 1 1 calc R U . . .
H99C H 0.612069 -0.228952 0.301712 0.070 Uiso 1 1 calc R U . . .
C100 C 0.3152(10) -0.1557(4) 0.7442(3) 0.045(3) Uani 1 1 d . . . . .
C101 C 0.1792(12) -0.1530(5) 0.7376(4) 0.067(4) Uani 1 1 d . . . . .
H10A H 0.139255 -0.158284 0.764694 0.101 Uiso 1 1 calc R U . . .
H10B H 0.154815 -0.178050 0.717360 0.101 Uiso 1 1 calc R U . . .
H10C H 0.157988 -0.120943 0.726464 0.101 Uiso 1 1 calc R U . . .
C102 C 0.3607(16) -0.1118(5) 0.7684(3) 0.069(4) Uani 1 1 d . . . . .
H10D H 0.325543 -0.111254 0.796716 0.104 Uiso 1 1 calc R U . . .
H10E H 0.339255 -0.082133 0.753140 0.104 Uiso 1 1 calc R U . . .
H10F H 0.446555 -0.113849 0.770838 0.104 Uiso 1 1 calc R U . . .
C103 C 0.3415(15) -0.2029(5) 0.7676(3) 0.068(4) Uani 1 1 d . . . . .
H10G H 0.419221 -0.200824 0.780921 0.102 Uiso 1 1 calc R U . . .
H10H H 0.340724 -0.229974 0.747384 0.102 Uiso 1 1 calc R U . . .
H10I H 0.281471 -0.208386 0.789337 0.102 Uiso 1 1 calc R U . . .
C119 C 0.5930(14) -0.0198(5) 0.5340(4) 0.068(4) Uani 1 1 d . . . . .
H119 H 0.580423 -0.055617 0.531392 0.082 Uiso 1 1 calc R U . . .
C120 C 0.3610(16) 1.0235(5) 0.3446(5) 0.080(5) Uani 1 1 d . . . . .
H120 H 0.355130 1.059504 0.348109 0.096 Uiso 1 1 calc R U . . .
CL8 Cl 0.5466(4) 1.00182(18) 0.12461(14) 0.0932(12) Uani 1 1 d . . . . .
CL9 Cl 0.2923(4) 1.00443(16) 0.12378(18) 0.1005(14) Uani 1 1 d . . . . .
CL7 Cl 0.4169(10) 0.9884(6) 0.2009(2) 0.275(9) Uani 1 1 d . . . . .
C150 C 0.418(3) 0.9782(7) 0.1455(6) 0.128(9) Uani 1 1 d . . . . .
H150 H 0.416430 0.942499 0.140071 0.154 Uiso 1 1 calc R U . . .
CL21 Cl 0.9306(4) 0.99402(14) 0.45209(16) 0.0938(13) Uani 1 1 d . . . . .
CL20 Cl 0.7602(6) 1.0213(3) 0.3896(2) 0.138(2) Uani 1 1 d . . . . .
C151 C 0.8502(13) 0.9779(10) 0.4090(6) 0.111(7) Uani 1 1 d . . . . .
H151 H 0.795520 0.952235 0.419756 0.133 Uiso 1 1 calc R U . . .
CL26 Cl 0.9075(9) 1.0111(3) 0.2772(3) 0.172(3) Uani 1 1 d . . . . .
CL22 Cl 0.9338(6) 0.9483(3) 0.3688(2) 0.153(3) Uani 1 1 d . . . . .
CL27 Cl 0.7277(13) 1.0090(4) 0.2144(5) 0.225(5) Uani 1 1 d . . . . .
CL28 Cl 0.973(6) 0.9946(9) 0.1906(13) 1.01(7) Uani 1 1 d . . . . .
C200 C 0.866(4) 1.0155(16) 0.224(2) 0.36(5) Uani 1 1 d . . . . .
H200 H 0.874735 1.051228 0.219855 0.433 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
CL6 C120 1.710(17) . ?
C1A C44 1.315(11) . ?
C1A C7 1.468(10) . ?
C1A C2 1.494(10) . ?
C2 C8A 1.401(10) . ?
C2 C3A 1.407(11) . ?
CL2 C119 1.731(15) . ?
CL3 C119 1.719(14) . ?
C3A C11 1.434(10) . ?
C3A C4 1.469(11) . ?
C4 C16 1.417(11) . ?
C4 C5 1.419(10) . ?
CL1 C119 1.803(17) . ?
C5 C19 1.379(10) . ?
C5 C6 1.492(10) . ?
CL5 C120 1.756(19) . ?
C6 C15 1.389(11) . ?
C6 C7 1.395(10) . ?
C7 C12 1.426(11) . ?
C8A C9A 1.383(11) . ?
C8A H8A 0.9500 . ?
CL4 C120 1.789(15) . ?
C9A C10 1.390(13) . ?
C9A H9A 0.9500 . ?
C10 C11 1.363(11) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.379(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.373(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.392(11) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.412(10) . ?
C16 C20 1.502(9) . ?
C17 C18 1.416(10) . ?
C17 C26 1.496(10) . ?
C18 C19 1.415(11) . ?
C18 C32 1.493(11) . ?
C19 C38 1.478(10) . ?
C20 C21 1.369(10) . ?
C20 C25 1.398(10) . ?
C21 C22 1.380(11) . ?
C21 H21 0.9500 . ?
C22 C23 1.404(12) . ?
C22 H22 0.9500 . ?
C23 C24 1.427(12) . ?
C23 C92 1.494(12) . ?
C24 C25 1.359(11) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.387(11) . ?
C26 C31 1.397(11) . ?
C27 C28 1.389(12) . ?
C27 H27 0.9500 . ?
C28 C29 1.404(13) . ?
C28 H28 0.9500 . ?
C29 C30 1.391(12) . ?
C29 H29 0.9500 . ?
C30 C31 1.385(11) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.376(11) . ?
C32 C37 1.398(12) . ?
C33 C34 1.372(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.402(14) . ?
C34 H34 0.9500 . ?
C35 C36 1.357(14) . ?
C35 H35 0.9500 . ?
C36 C37 1.389(12) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.408(10) . ?
C38 C43 1.408(10) . ?
C39 C40 1.389(11) . ?
C39 H39 0.9500 . ?
C40 C41 1.376(12) . ?
C40 H40 0.9500 . ?
C41 C42 1.400(12) . ?
C41 C88 1.518(12) . ?
C42 C43 1.382(11) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.266(11) . ?
C45 C46 1.345(11) . ?
C46 C52 1.473(10) . ?
C46 C47 1.499(10) . ?
C47 C57 1.385(11) . ?
C47 C48 1.403(10) . ?
C48 C60 1.397(11) . ?
C48 C49 1.489(10) . ?
C49 C61 1.405(11) . ?
C49 C50 1.405(10) . ?
C50 C64A 1.409(10) . ?
C50 C51 1.497(10) . ?
C51 C56 1.389(10) . ?
C51 C52 1.421(11) . ?
C52 C53 1.388(11) . ?
C53 C54 1.374(11) . ?
C53 H53 0.9500 . ?
C54 C55 1.399(12) . ?
C54 H54 0.9500 . ?
C55 C56 1.369(12) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C58 1.392(12) . ?
C57 H57 0.9500 . ?
C58 C59 1.387(13) . ?
C58 H58 0.9500 . ?
C59 C60 1.372(11) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 C62 1.403(10) . ?
C61 C64 1.502(10) . ?
C62 C63 1.412(10) . ?
C62 C70 1.492(11) . ?
C63 C64A 1.397(11) . ?
C63 C76 1.509(10) . ?
C64 C65 1.374(11) . ?
C64 C69 1.393(11) . ?
C64A C82 1.495(10) . ?
C65 C66 1.402(11) . ?
C65 H65 0.9500 . ?
C66 C67 1.427(12) . ?
C66 H66 0.9500 . ?
C67 C68 1.350(12) . ?
C67 C96 1.530(11) . ?
C68 C69 1.405(10) . ?
C68 H68 0.9500 . ?
C69 H69 0.9500 . ?
C70 C75 1.396(11) . ?
C70 C71A 1.401(11) . ?
C71A C72 1.412(12) . ?
C71A H71A 0.9500 . ?
C72 C73 1.379(13) . ?
C72 H72 0.9500 . ?
C73 C74 1.409(12) . ?
C73 H73 0.9500 . ?
C74 C75 1.373(11) . ?
C74 H74 0.9500 . ?
C75 H75 0.9500 . ?
C76 C77 1.373(12) . ?
C76 C81 1.424(12) . ?
C77 C78 1.379(12) . ?
C77 H77 0.9500 . ?
C78 C79 1.373(14) . ?
C78 H78 0.9500 . ?
C79 C80 1.389(13) . ?
C79 H79 0.9500 . ?
C80 C81 1.385(11) . ?
C80 H80 0.9500 . ?
C81 H81 0.9500 . ?
C82 C87 1.371(11) . ?
C82 C83 1.396(12) . ?
C83 C84 1.371(12) . ?
C83 H83 0.9500 . ?
C84 C85 1.381(13) . ?
C84 H84 0.9500 . ?
C85 C86 1.397(13) . ?
C85 C100 1.544(11) . ?
C86 C87 1.404(11) . ?
C86 H86 0.9500 . ?
C87 H87 0.9500 . ?
C88 C89 1.515(17) . ?
C88 C90 1.549(16) . ?
C88 C91 1.556(16) . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 C95 1.511(18) . ?
C92 C94 1.529(14) . ?
C92 C93 1.533(16) . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?
C96 C98 1.546(19) . ?
C96 C97 1.550(15) . ?
C96 C99A 1.583(16) . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
C99A H99A 0.9800 . ?
C99A H99B 0.9800 . ?
C99A H99C 0.9800 . ?
C100 C102 1.519(17) . ?
C100 C103 1.527(17) . ?
C100 C101 1.561(19) . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
C102 H10F 0.9800 . ?
C103 H10G 0.9800 . ?
C103 H10H 0.9800 . ?
C103 H10I 0.9800 . ?
C119 H119 1.0000 . ?
C120 H120 1.0000 . ?
CL8 C150 1.73(3) . ?
CL9 C150 1.74(3) . ?
CL7 C150 1.77(2) . ?
C150 H150 1.0000 . ?
CL21 C151 1.70(2) . ?
CL20 C151 1.69(2) . ?
C151 CL22 1.78(2) . ?
C151 H151 1.0000 . ?
CL26 C200 1.74(6) . ?
CL27 C200 1.61(4) . ?
CL28 C200 1.71(6) . ?
C200 H200 1.0000 . ?

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
C44 C1A C7 124.6(6) . . ?
C44 C1A C2 121.8(6) . . ?
C7 C1A C2 112.8(6) . . ?
C8A C2 C3A 120.4(7) . . ?
C8A C2 C1A 118.6(6) . . ?
C3A C2 C1A 120.5(6) . . ?
C2 C3A C11 116.9(6) . . ?
C2 C3A C4 120.9(6) . . ?
C11 C3A C4 122.1(6) . . ?
C16 C4 C5 118.9(7) . . ?
C16 C4 C3A 119.5(6) . . ?
C5 C4 C3A 121.6(7) . . ?
C19 C5 C4 120.3(7) . . ?
C19 C5 C6 120.4(6) . . ?
C4 C5 C6 119.3(6) . . ?
C15 C6 C7 119.0(7) . . ?
C15 C6 C5 120.1(7) . . ?
C7 C6 C5 120.5(6) . . ?
C6 C7 C12 119.2(7) . . ?
C6 C7 C1A 121.2(6) . . ?
C12 C7 C1A 118.9(6) . . ?
C9A C8A C2 121.1(7) . . ?
C9A C8A H8A 119.4 . . ?
C2 C8A H8A 119.4 . . ?
C8A C9A C10 118.9(7) . . ?
C8A C9A H9A 120.5 . . ?
C10 C9A H9A 120.5 . . ?
C11 C10 C9A 121.2(7) . . ?
C11 C10 H10 119.4 . . ?
C9A C10 H10 119.4 . . ?
C10 C11 C3A 121.3(7) . . ?
C10 C11 H11 119.4 . . ?
C3A C11 H11 119.4 . . ?
C13 C12 C7 120.0(7) . . ?
C13 C12 H12 120.0 . . ?
C7 C12 H12 120.0 . . ?
C14 C13 C12 120.6(8) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 119.6(7) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C6 C15 C14 121.4(7) . . ?
C6 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C17 C16 C4 120.4(6) . . ?
C17 C16 C20 118.3(6) . . ?
C4 C16 C20 121.2(6) . . ?
C16 C17 C18 119.9(7) . . ?
C16 C17 C26 119.3(6) . . ?
C18 C17 C26 120.7(6) . . ?
C19 C18 C17 118.7(7) . . ?
C19 C18 C32 120.0(6) . . ?
C17 C18 C32 121.1(7) . . ?
C5 C19 C18 121.6(6) . . ?
C5 C19 C38 120.5(6) . . ?
C18 C19 C38 117.8(6) . . ?
C21 C20 C25 117.6(6) . . ?
C21 C20 C16 122.6(6) . . ?
C25 C20 C16 119.8(6) . . ?
C20 C21 C22 122.0(7) . . ?
C20 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
C21 C22 C23 121.5(7) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C22 C23 C24 115.7(7) . . ?
C22 C23 C92 124.1(7) . . ?
C24 C23 C92 120.2(7) . . ?
C25 C24 C23 121.5(7) . . ?
C25 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C24 C25 C20 121.6(7) . . ?
C24 C25 H25 119.2 . . ?
C20 C25 H25 119.2 . . ?
C27 C26 C31 118.2(7) . . ?
C27 C26 C17 119.6(7) . . ?
C31 C26 C17 122.0(7) . . ?
C26 C27 C28 121.8(7) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 H27 119.1 . . ?
C27 C28 C29 119.2(8) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 119.5(8) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C31 C30 C29 120.2(7) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C26 121.1(7) . . ?
C30 C31 H31 119.4 . . ?
C26 C31 H31 119.4 . . ?
C33 C32 C37 118.6(7) . . ?
C33 C32 C18 122.1(7) . . ?
C37 C32 C18 119.2(7) . . ?
C34 C33 C32 120.6(7) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C33 C34 C35 120.0(8) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.5(7) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 C37 119.2(8) . . ?
C35 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C36 C37 C32 121.2(8) . . ?
C36 C37 H37 119.4 . . ?
C32 C37 H37 119.4 . . ?
C39 C38 C43 116.2(6) . . ?
C39 C38 C19 122.0(6) . . ?
C43 C38 C19 121.8(6) . . ?
C40 C39 C38 121.2(7) . . ?
C40 C39 H39 119.4 . . ?
C38 C39 H39 119.4 . . ?
C41 C40 C39 121.5(7) . . ?
C41 C40 H40 119.2 . . ?
C39 C40 H40 119.2 . . ?
C40 C41 C42 118.5(7) . . ?
C40 C41 C88 123.0(8) . . ?
C42 C41 C88 118.4(8) . . ?
C43 C42 C41 120.1(7) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C42 C43 C38 122.3(7) . . ?
C42 C43 H43 118.8 . . ?
C38 C43 H43 118.8 . . ?
C45 C44 C1A 179.2(9) . . ?
C44 C45 C46 178.3(8) . . ?
C45 C46 C52 123.2(7) . . ?
C45 C46 C47 120.9(6) . . ?
C52 C46 C47 114.1(6) . . ?
C57 C47 C48 120.8(6) . . ?
C57 C47 C46 118.7(6) . . ?
C48 C47 C46 120.0(6) . . ?
C60 C48 C47 117.0(7) . . ?
C60 C48 C49 121.4(6) . . ?
C47 C48 C49 121.4(6) . . ?
C61 C49 C50 119.0(6) . . ?
C61 C49 C48 119.6(6) . . ?
C50 C49 C48 121.3(6) . . ?
C49 C50 C64A 120.8(7) . . ?
C49 C50 C51 120.2(6) . . ?
C64A C50 C51 119.0(6) . . ?
C56 C51 C52 117.9(6) . . ?
C56 C51 C50 121.4(6) . . ?
C52 C51 C50 120.4(6) . . ?
C53 C52 C51 119.4(7) . . ?
C53 C52 C46 119.6(7) . . ?
C51 C52 C46 120.6(6) . . ?
C54 C53 C52 120.9(7) . . ?
C54 C53 H53 119.6 . . ?
C52 C53 H53 119.6 . . ?
C53 C54 C55 120.0(7) . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C56 C55 C54 119.2(7) . . ?
C56 C55 H55 120.4 . . ?
C54 C55 H55 120.4 . . ?
C55 C56 C51 122.2(7) . . ?
C55 C56 H56 118.9 . . ?
C51 C56 H56 118.9 . . ?
C47 C57 C58 120.0(7) . . ?
C47 C57 H57 120.0 . . ?
C58 C57 H57 120.0 . . ?
C59 C58 C57 120.1(7) . . ?
C59 C58 H58 120.0 . . ?
C57 C58 H58 120.0 . . ?
C60 C59 C58 119.0(7) . . ?
C60 C59 H59 120.5 . . ?
C58 C59 H59 120.5 . . ?
C59 C60 C48 122.8(7) . . ?
C59 C60 H60 118.6 . . ?
C48 C60 H60 118.6 . . ?
C62 C61 C49 120.9(6) . . ?
C62 C61 C64 119.0(6) . . ?
C49 C61 C64 120.1(6) . . ?
C61 C62 C63 119.2(7) . . ?
C61 C62 C70 119.2(6) . . ?
C63 C62 C70 121.5(6) . . ?
C64A C63 C62 120.6(7) . . ?
C64A C63 C76 117.9(6) . . ?
C62 C63 C76 121.3(7) . . ?
C65 C64 C69 118.7(6) . . ?
C65 C64 C61 120.4(6) . . ?
C69 C64 C61 120.8(6) . . ?
C63 C64A C50 119.4(7) . . ?
C63 C64A C82 120.9(6) . . ?
C50 C64A C82 119.8(6) . . ?
C64 C65 C66 120.7(7) . . ?
C64 C65 H65 119.6 . . ?
C66 C65 H65 119.6 . . ?
C65 C66 C67 119.9(7) . . ?
C65 C66 H66 120.1 . . ?
C67 C66 H66 120.1 . . ?
C68 C67 C66 118.7(7) . . ?
C68 C67 C96 120.9(8) . . ?
C66 C67 C96 120.4(8) . . ?
C67 C68 C69 121.0(7) . . ?
C67 C68 H68 119.5 . . ?
C69 C68 H68 119.5 . . ?
C64 C69 C68 120.9(7) . . ?
C64 C69 H69 119.6 . . ?
C68 C69 H69 119.6 . . ?
C75 C70 C71A 117.7(7) . . ?
C75 C70 C62 122.5(7) . . ?
C71A C70 C62 119.4(7) . . ?
C70 C71A C72 120.6(7) . . ?
C70 C71A H71A 119.7 . . ?
C72 C71A H71A 119.7 . . ?
C73 C72 C71A 120.4(8) . . ?
C73 C72 H72 119.8 . . ?
C71A C72 H72 119.8 . . ?
C72 C73 C74 118.8(7) . . ?
C72 C73 H73 120.6 . . ?
C74 C73 H73 120.6 . . ?
C75 C74 C73 120.5(7) . . ?
C75 C74 H74 119.8 . . ?
C73 C74 H74 119.8 . . ?
C74 C75 C70 121.9(7) . . ?
C74 C75 H75 119.1 . . ?
C70 C75 H75 119.1 . . ?
C77 C76 C81 118.4(7) . . ?
C77 C76 C63 120.7(7) . . ?
C81 C76 C63 120.9(7) . . ?
C76 C77 C78 121.0(8) . . ?
C76 C77 H77 119.5 . . ?
C78 C77 H77 119.5 . . ?
C79 C78 C77 121.0(8) . . ?
C79 C78 H78 119.5 . . ?
C77 C78 H78 119.5 . . ?
C78 C79 C80 119.6(7) . . ?
C78 C79 H79 120.2 . . ?
C80 C79 H79 120.2 . . ?
C81 C80 C79 120.1(8) . . ?
C81 C80 H80 120.0 . . ?
C79 C80 H80 120.0 . . ?
C80 C81 C76 120.0(7) . . ?
C80 C81 H81 120.0 . . ?
C76 C81 H81 120.0 . . ?
C87 C82 C83 119.3(7) . . ?
C87 C82 C64A 120.2(6) . . ?
C83 C82 C64A 120.4(7) . . ?
C84 C83 C82 119.4(8) . . ?
C84 C83 H83 120.3 . . ?
C82 C83 H83 120.3 . . ?
C83 C84 C85 123.1(8) . . ?
C83 C84 H84 118.4 . . ?
C85 C84 H84 118.4 . . ?
C84 C85 C86 116.9(7) . . ?
C84 C85 C100 120.6(8) . . ?
C86 C85 C100 122.5(8) . . ?
C85 C86 C87 120.8(7) . . ?
C85 C86 H86 119.6 . . ?
C87 C86 H86 119.6 . . ?
C82 C87 C86 120.4(7) . . ?
C82 C87 H87 119.8 . . ?
C86 C87 H87 119.8 . . ?
C89 C88 C41 111.0(9) . . ?
C89 C88 C90 108.2(10) . . ?
C41 C88 C90 112.4(8) . . ?
C89 C88 C91 108.5(11) . . ?
C41 C88 C91 109.8(8) . . ?
C90 C88 C91 106.7(8) . . ?
C88 C89 H89A 109.5 . . ?
C88 C89 H89B 109.5 . . ?
H89A C89 H89B 109.5 . . ?
C88 C89 H89C 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C88 C90 H90A 109.5 . . ?
C88 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
C88 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C88 C91 H91A 109.5 . . ?
C88 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C88 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C23 C92 C95 109.2(9) . . ?
C23 C92 C94 112.9(8) . . ?
C95 C92 C94 106.5(10) . . ?
C23 C92 C93 112.2(8) . . ?
C95 C92 C93 107.9(10) . . ?
C94 C92 C93 107.9(8) . . ?
C92 C93 H93A 109.5 . . ?
C92 C93 H93B 109.5 . . ?
H93A C93 H93B 109.5 . . ?
C92 C93 H93C 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C92 C94 H94A 109.5 . . ?
C92 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C92 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
C92 C95 H95A 109.5 . . ?
C92 C95 H95B 109.5 . . ?
H95A C95 H95B 109.5 . . ?
C92 C95 H95C 109.5 . . ?
H95A C95 H95C 109.5 . . ?
H95B C95 H95C 109.5 . . ?
C67 C96 C98 108.4(9) . . ?
C67 C96 C97 113.2(8) . . ?
C98 C96 C97 113.8(10) . . ?
C67 C96 C99A 106.8(8) . . ?
C98 C96 C99A 107.0(9) . . ?
C97 C96 C99A 107.2(9) . . ?
C96 C97 H97A 109.5 . . ?
C96 C97 H97B 109.5 . . ?
H97A C97 H97B 109.5 . . ?
C96 C97 H97C 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
C96 C98 H98A 109.5 . . ?
C96 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C96 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
C96 C99A H99A 109.5 . . ?
C96 C99A H99B 109.5 . . ?
H99A C99A H99B 109.5 . . ?
C96 C99A H99C 109.5 . . ?
H99A C99A H99C 109.5 . . ?
H99B C99A H99C 109.5 . . ?
C102 C100 C103 111.7(10) . . ?
C102 C100 C85 108.8(9) . . ?
C103 C100 C85 111.7(9) . . ?
C102 C100 C101 111.5(11) . . ?
C103 C100 C101 107.4(11) . . ?
C85 C100 C101 105.7(9) . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C100 C102 H10D 109.5 . . ?
C100 C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
C100 C102 H10F 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
C100 C103 H10G 109.5 . . ?
C100 C103 H10H 109.5 . . ?
H10G C103 H10H 109.5 . . ?
C100 C103 H10I 109.5 . . ?
H10G C103 H10I 109.5 . . ?
H10H C103 H10I 109.5 . . ?
CL3 C119 CL2 113.5(8) . . ?
CL3 C119 CL1 109.1(8) . . ?
CL2 C119 CL1 108.7(8) . . ?
CL3 C119 H119 108.4 . . ?
CL2 C119 H119 108.4 . . ?
CL1 C119 H119 108.4 . . ?
CL6 C120 CL5 111.6(7) . . ?
CL6 C120 CL4 108.8(10) . . ?
CL5 C120 CL4 111.3(9) . . ?
CL6 C120 H120 108.3 . . ?
CL5 C120 H120 108.3 . . ?
CL4 C120 H120 108.3 . . ?
CL8 C150 CL9 112.8(9) . . ?
CL8 C150 CL7 108.9(14) . . ?
CL9 C150 CL7 108.3(17) . . ?
CL8 C150 H150 108.9 . . ?
CL9 C150 H150 108.9 . . ?
CL7 C150 H150 108.9 . . ?
CL20 C151 CL21 115.5(16) . . ?
CL20 C151 CL22 112.9(11) . . ?
CL21 C151 CL22 113.8(9) . . ?
CL20 C151 H151 104.4 . . ?
CL21 C151 H151 104.4 . . ?
CL22 C151 H151 104.4 . . ?
CL27 C200 CL28 122(3) . . ?
CL27 C200 CL26 116(5) . . ?
CL28 C200 CL26 112(3) . . ?
CL27 C200 H200 100.1 . . ?
CL28 C200 H200 100.1 . . ?
CL26 C200 H200 100.1 . . ?

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
C44 C1A C2 C8A 54.1(10) . . . . ?
C7 C1A C2 C8A -115.6(7) . . . . ?
C44 C1A C2 C3A -134.3(7) . . . . ?
C7 C1A C2 C3A 56.1(9) . . . . ?
C8A C2 C3A C11 5.0(10) . . . . ?
C1A C2 C3A C11 -166.5(6) . . . . ?
C8A C2 C3A C4 -170.8(6) . . . . ?
C1A C2 C3A C4 17.7(10) . . . . ?
C2 C3A C4 C16 127.0(7) . . . . ?
C11 C3A C4 C16 -48.5(9) . . . . ?
C2 C3A C4 C5 -54.1(9) . . . . ?
C11 C3A C4 C5 130.4(7) . . . . ?
C16 C4 C5 C19 -3.8(10) . . . . ?
C3A C4 C5 C19 177.4(6) . . . . ?
C16 C4 C5 C6 177.6(6) . . . . ?
C3A C4 C5 C6 -1.3(10) . . . . ?
C19 C5 C6 C15 51.4(9) . . . . ?
C4 C5 C6 C15 -130.0(7) . . . . ?
C19 C5 C6 C7 -121.9(7) . . . . ?
C4 C5 C6 C7 56.7(9) . . . . ?
C15 C6 C7 C12 -2.8(10) . . . . ?
C5 C6 C7 C12 170.5(6) . . . . ?
C15 C6 C7 C1A 167.8(6) . . . . ?
C5 C6 C7 C1A -18.9(10) . . . . ?
C44 C1A C7 C6 134.8(8) . . . . ?
C2 C1A C7 C6 -55.9(9) . . . . ?
C44 C1A C7 C12 -54.6(10) . . . . ?
C2 C1A C7 C12 114.7(7) . . . . ?
C3A C2 C8A C9A -3.9(11) . . . . ?
C1A C2 C8A C9A 167.8(7) . . . . ?
C2 C8A C9A C10 -0.2(12) . . . . ?
C8A C9A C10 C11 3.0(12) . . . . ?
C9A C10 C11 C3A -1.7(12) . . . . ?
C2 C3A C11 C10 -2.3(10) . . . . ?
C4 C3A C11 C10 173.4(7) . . . . ?
C6 C7 C12 C13 2.3(11) . . . . ?
C1A C7 C12 C13 -168.5(7) . . . . ?
C7 C12 C13 C14 1.2(12) . . . . ?
C12 C13 C14 C15 -4.1(12) . . . . ?
C7 C6 C15 C14 -0.1(10) . . . . ?
C5 C6 C15 C14 -173.5(7) . . . . ?
C13 C14 C15 C6 3.6(11) . . . . ?
C5 C4 C16 C17 3.3(10) . . . . ?
C3A C4 C16 C17 -177.8(6) . . . . ?
C5 C4 C16 C20 -178.5(6) . . . . ?
C3A C4 C16 C20 0.4(10) . . . . ?
C4 C16 C17 C18 -0.5(10) . . . . ?
C20 C16 C17 C18 -178.7(6) . . . . ?
C4 C16 C17 C26 175.0(6) . . . . ?
C20 C16 C17 C26 -3.3(9) . . . . ?
C16 C17 C18 C19 -2.0(10) . . . . ?
C26 C17 C18 C19 -177.4(6) . . . . ?
C16 C17 C18 C32 174.3(6) . . . . ?
C26 C17 C18 C32 -1.1(10) . . . . ?
C4 C5 C19 C18 1.4(10) . . . . ?
C6 C5 C19 C18 180.0(6) . . . . ?
C4 C5 C19 C38 -177.0(6) . . . . ?
C6 C5 C19 C38 1.6(10) . . . . ?
C17 C18 C19 C5 1.5(10) . . . . ?
C32 C18 C19 C5 -174.7(6) . . . . ?
C17 C18 C19 C38 180.0(6) . . . . ?
C32 C18 C19 C38 3.7(9) . . . . ?
C17 C16 C20 C21 113.1(8) . . . . ?
C4 C16 C20 C21 -65.1(9) . . . . ?
C17 C16 C20 C25 -65.6(9) . . . . ?
C4 C16 C20 C25 116.2(8) . . . . ?
C25 C20 C21 C22 -2.2(11) . . . . ?
C16 C20 C21 C22 179.1(7) . . . . ?
C20 C21 C22 C23 2.4(12) . . . . ?
C21 C22 C23 C24 -3.1(12) . . . . ?
C21 C22 C23 C92 177.4(8) . . . . ?
C22 C23 C24 C25 3.9(12) . . . . ?
C92 C23 C24 C25 -176.5(9) . . . . ?
C23 C24 C25 C20 -4.0(12) . . . . ?
C21 C20 C25 C24 3.0(11) . . . . ?
C16 C20 C25 C24 -178.2(7) . . . . ?
C16 C17 C26 C27 -71.8(9) . . . . ?
C18 C17 C26 C27 103.6(8) . . . . ?
C16 C17 C26 C31 102.4(8) . . . . ?
C18 C17 C26 C31 -82.2(9) . . . . ?
C31 C26 C27 C28 -1.0(11) . . . . ?
C17 C26 C27 C28 173.4(7) . . . . ?
C26 C27 C28 C29 3.0(12) . . . . ?
C27 C28 C29 C30 -3.1(12) . . . . ?
C28 C29 C30 C31 1.4(12) . . . . ?
C29 C30 C31 C26 0.6(11) . . . . ?
C27 C26 C31 C30 -0.8(10) . . . . ?
C17 C26 C31 C30 -175.1(7) . . . . ?
C19 C18 C32 C33 -109.5(8) . . . . ?
C17 C18 C32 C33 74.3(9) . . . . ?
C19 C18 C32 C37 65.4(9) . . . . ?
C17 C18 C32 C37 -110.8(8) . . . . ?
C37 C32 C33 C34 0.8(11) . . . . ?
C18 C32 C33 C34 175.8(7) . . . . ?
C32 C33 C34 C35 -0.3(11) . . . . ?
C33 C34 C35 C36 -0.3(12) . . . . ?
C34 C35 C36 C37 0.3(12) . . . . ?
C35 C36 C37 C32 0.2(12) . . . . ?
C33 C32 C37 C36 -0.8(11) . . . . ?
C18 C32 C37 C36 -175.9(7) . . . . ?
C5 C19 C38 C39 -118.8(8) . . . . ?
C18 C19 C38 C39 62.7(9) . . . . ?
C5 C19 C38 C43 60.3(9) . . . . ?
C18 C19 C38 C43 -118.2(7) . . . . ?
C43 C38 C39 C40 2.4(11) . . . . ?
C19 C38 C39 C40 -178.5(7) . . . . ?
C38 C39 C40 C41 -1.0(12) . . . . ?
C39 C40 C41 C42 -0.7(12) . . . . ?
C39 C40 C41 C88 178.6(9) . . . . ?
C40 C41 C42 C43 1.0(12) . . . . ?
C88 C41 C42 C43 -178.4(8) . . . . ?
C41 C42 C43 C38 0.4(12) . . . . ?
C39 C38 C43 C42 -2.1(11) . . . . ?
C19 C38 C43 C42 178.8(7) . . . . ?
C45 C46 C47 C57 -47.9(10) . . . . ?
C52 C46 C47 C57 117.0(7) . . . . ?
C45 C46 C47 C48 140.4(7) . . . . ?
C52 C46 C47 C48 -54.7(9) . . . . ?
C57 C47 C48 C60 -6.1(10) . . . . ?
C46 C47 C48 C60 165.5(6) . . . . ?
C57 C47 C48 C49 168.9(7) . . . . ?
C46 C47 C48 C49 -19.5(10) . . . . ?
C60 C48 C49 C61 48.6(10) . . . . ?
C47 C48 C49 C61 -126.2(7) . . . . ?
C60 C48 C49 C50 -130.3(7) . . . . ?
C47 C48 C49 C50 54.9(10) . . . . ?
C61 C49 C50 C64A 2.2(10) . . . . ?
C48 C49 C50 C64A -178.9(6) . . . . ?
C61 C49 C50 C51 -177.4(6) . . . . ?
C48 C49 C50 C51 1.6(10) . . . . ?
C49 C50 C51 C56 129.7(7) . . . . ?
C64A C50 C51 C56 -49.9(9) . . . . ?
C49 C50 C51 C52 -56.0(9) . . . . ?
C64A C50 C51 C52 124.5(7) . . . . ?
C56 C51 C52 C53 6.0(10) . . . . ?
C50 C51 C52 C53 -168.5(7) . . . . ?
C56 C51 C52 C46 -167.3(6) . . . . ?
C50 C51 C52 C46 18.2(10) . . . . ?
C45 C46 C52 C53 47.0(10) . . . . ?
C47 C46 C52 C53 -117.5(7) . . . . ?
C45 C46 C52 C51 -139.8(7) . . . . ?
C47 C46 C52 C51 55.7(9) . . . . ?
C51 C52 C53 C54 -4.4(11) . . . . ?
C46 C52 C53 C54 168.9(7) . . . . ?
C52 C53 C54 C55 -1.1(12) . . . . ?
C53 C54 C55 C56 4.9(12) . . . . ?
C54 C55 C56 C51 -3.2(12) . . . . ?
C52 C51 C56 C55 -2.2(10) . . . . ?
C50 C51 C56 C55 172.3(7) . . . . ?
C48 C47 C57 C58 4.0(11) . . . . ?
C46 C47 C57 C58 -167.7(7) . . . . ?
C47 C57 C58 C59 1.3(12) . . . . ?
C57 C58 C59 C60 -4.1(12) . . . . ?
C58 C59 C60 C48 1.9(12) . . . . ?
C47 C48 C60 C59 3.2(11) . . . . ?
C49 C48 C60 C59 -171.8(7) . . . . ?
C50 C49 C61 C62 1.0(10) . . . . ?
C48 C49 C61 C62 -177.9(6) . . . . ?
C50 C49 C61 C64 179.7(6) . . . . ?
C48 C49 C61 C64 0.7(10) . . . . ?
C49 C61 C62 C63 -3.9(10) . . . . ?
C64 C61 C62 C63 177.4(6) . . . . ?
C49 C61 C62 C70 -179.6(6) . . . . ?
C64 C61 C62 C70 1.7(10) . . . . ?
C61 C62 C63 C64A 3.6(10) . . . . ?
C70 C62 C63 C64A 179.2(6) . . . . ?
C61 C62 C63 C76 -171.6(7) . . . . ?
C70 C62 C63 C76 4.0(10) . . . . ?
C62 C61 C64 C65 -118.8(8) . . . . ?
C49 C61 C64 C65 62.5(9) . . . . ?
C62 C61 C64 C69 64.9(9) . . . . ?
C49 C61 C64 C69 -113.8(8) . . . . ?
C62 C63 C64A C50 -0.5(10) . . . . ?
C76 C63 C64A C50 174.8(6) . . . . ?
C62 C63 C64A C82 179.7(6) . . . . ?
C76 C63 C64A C82 -4.9(10) . . . . ?
C49 C50 C64A C63 -2.4(10) . . . . ?
C51 C50 C64A C63 177.1(6) . . . . ?
C49 C50 C64A C82 177.4(6) . . . . ?
C51 C50 C64A C82 -3.1(9) . . . . ?
C69 C64 C65 C66 3.7(11) . . . . ?
C61 C64 C65 C66 -172.7(7) . . . . ?
C64 C65 C66 C67 -0.7(12) . . . . ?
C65 C66 C67 C68 -2.4(12) . . . . ?
C65 C66 C67 C96 178.4(9) . . . . ?
C66 C67 C68 C69 2.4(13) . . . . ?
C96 C67 C68 C69 -178.4(9) . . . . ?
C65 C64 C69 C68 -3.7(12) . . . . ?
C61 C64 C69 C68 172.7(7) . . . . ?
C67 C68 C69 C64 0.6(13) . . . . ?
C61 C62 C70 C75 -103.2(8) . . . . ?
C63 C62 C70 C75 81.3(9) . . . . ?
C61 C62 C70 C71A 70.1(9) . . . . ?
C63 C62 C70 C71A -105.4(8) . . . . ?
C75 C70 C71A C72 -0.2(11) . . . . ?
C62 C70 C71A C72 -173.8(7) . . . . ?
C70 C71A C72 C73 0.5(12) . . . . ?
C71A C72 C73 C74 -0.9(12) . . . . ?
C72 C73 C74 C75 0.9(11) . . . . ?
C73 C74 C75 C70 -0.6(11) . . . . ?
C71A C70 C75 C74 0.2(10) . . . . ?
C62 C70 C75 C74 173.6(7) . . . . ?
C64A C63 C76 C77 -65.8(9) . . . . ?
C62 C63 C76 C77 109.6(8) . . . . ?
C64A C63 C76 C81 110.8(8) . . . . ?
C62 C63 C76 C81 -73.9(9) . . . . ?
C81 C76 C77 C78 -0.4(11) . . . . ?
C63 C76 C77 C78 176.2(7) . . . . ?
C76 C77 C78 C79 1.0(12) . . . . ?
C77 C78 C79 C80 -0.2(12) . . . . ?
C78 C79 C80 C81 -1.1(12) . . . . ?
C79 C80 C81 C76 1.6(11) . . . . ?
C77 C76 C81 C80 -0.8(11) . . . . ?
C63 C76 C81 C80 -177.5(7) . . . . ?
C63 C64A C82 C87 -62.3(9) . . . . ?
C50 C64A C82 C87 117.9(7) . . . . ?
C63 C64A C82 C83 119.6(8) . . . . ?
C50 C64A C82 C83 -60.2(9) . . . . ?
C87 C82 C83 C84 -3.0(11) . . . . ?
C64A C82 C83 C84 175.2(7) . . . . ?
C82 C83 C84 C85 1.1(13) . . . . ?
C83 C84 C85 C86 1.9(12) . . . . ?
C83 C84 C85 C100 -177.0(9) . . . . ?
C84 C85 C86 C87 -2.9(12) . . . . ?
C100 C85 C86 C87 176.0(8) . . . . ?
C83 C82 C87 C86 1.9(11) . . . . ?
C64A C82 C87 C86 -176.2(7) . . . . ?
C85 C86 C87 C82 1.1(11) . . . . ?
C40 C41 C88 C89 116.7(12) . . . . ?
C42 C41 C88 C89 -63.9(13) . . . . ?
C40 C41 C88 C90 -4.7(13) . . . . ?
C42 C41 C88 C90 174.7(9) . . . . ?
C40 C41 C88 C91 -123.3(10) . . . . ?
C42 C41 C88 C91 56.1(11) . . . . ?
C22 C23 C92 C95 -109.5(11) . . . . ?
C24 C23 C92 C95 71.0(12) . . . . ?
C22 C23 C92 C94 8.8(13) . . . . ?
C24 C23 C92 C94 -170.7(9) . . . . ?
C22 C23 C92 C93 131.0(9) . . . . ?
C24 C23 C92 C93 -48.5(12) . . . . ?
C68 C67 C96 C98 -59.3(13) . . . . ?
C66 C67 C96 C98 119.9(10) . . . . ?
C68 C67 C96 C97 173.5(10) . . . . ?
C66 C67 C96 C97 -7.4(15) . . . . ?
C68 C67 C96 C99A 55.8(12) . . . . ?
C66 C67 C96 C99A -125.1(9) . . . . ?
C84 C85 C100 C102 -54.2(13) . . . . ?
C86 C85 C100 C102 127.0(11) . . . . ?
C84 C85 C100 C103 -177.9(10) . . . . ?
C86 C85 C100 C103 3.2(14) . . . . ?
C84 C85 C100 C101 65.6(12) . . . . ?
C86 C85 C100 C101 -113.2(10) . . . . ?

_refine_diff_density_max         1.421
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.174


# start Validation Reply Form
_vrf_PLAT934_shelx               
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....         11 Check 
RESPONSE: This is due to the limited quality of the crystals obtained. 
Different attempts to get higher quality crystals were unsuccessful.
;
# end Validation Reply Form
