# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_lvyun0902
#TrackingRef '15135_web_deposit_cif_file_1_LvYun_1352019239.LYT.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H58 Br2'
_chemical_formula_sum            'C56 H58 Br2'
_chemical_formula_weight         890.84

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6456(16)
_cell_length_b                   12.310(2)
_cell_length_c                   22.758(4)
_cell_angle_alpha                98.677(2)
_cell_angle_beta                 92.478(2)
_cell_angle_gamma                104.114(2)
_cell_volume                     2314.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4130
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      23.19

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5249
_exptl_absorpt_correction_T_max  0.9159
_exptl_absorpt_process_details   'APEX2 Software Suite (Bruker,2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22276
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         0.91
_diffrn_reflns_theta_max         24.76
_reflns_number_total             7919
_reflns_number_gt                5309
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0732P)²+9.9111P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7919
_refine_ls_number_parameters     527
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0781
_refine_ls_wR_factor_ref         0.2075
_refine_ls_wR_factor_gt          0.1845
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.70046(12) 1.02541(9) 0.46827(5) 0.1072(5) Uani 1 1 d . . .
C1 C 0.2615(10) 0.1229(7) 0.3615(4) 0.065(2) Uani 1 1 d . . .
H1 H 0.3295 0.1023 0.3881 0.078 Uiso 1 1 calc R . .
C2 C -0.1584(8) 0.3291(5) 0.1746(3) 0.0421(16) Uani 1 1 d . . .
Br2 Br -0.79321(8) -0.54095(5) 0.03212(3) 0.0472(2) Uani 1 1 d . . .
C3 C -0.4783(7) 0.0276(5) 0.1915(3) 0.0366(14) Uani 1 1 d . . .
H3 H -0.5833 0.0318 0.1956 0.044 Uiso 1 1 calc R . .
C4 C 0.4024(7) 0.7285(5) 0.3271(3) 0.0396(15) Uani 1 1 d . . .
C5 C 0.4990(8) 0.8029(6) 0.4289(3) 0.0555(19) Uani 1 1 d . . .
H5 H 0.5053 0.7953 0.4689 0.067 Uiso 1 1 calc R . .
C6 C -0.0538(7) 0.2125(5) 0.2375(3) 0.0378(14) Uani 1 1 d . . .
C7 C -0.0316(10) 0.6974(7) 0.4795(4) 0.072(2) Uani 1 1 d . . .
H7A H -0.0957 0.6226 0.4831 0.086 Uiso 1 1 calc R . .
H7B H 0.0335 0.7288 0.5168 0.086 Uiso 1 1 calc R . .
C8 C 0.5317(8) 0.4915(6) 0.3765(3) 0.0492(17) Uani 1 1 d . . .
H8A H 0.6052 0.5604 0.3691 0.059 Uiso 1 1 calc R . .
H8B H 0.4779 0.4499 0.3386 0.059 Uiso 1 1 calc R . .
C9 C 0.1858(8) 0.6104(5) 0.4396(3) 0.0428(16) Uani 1 1 d . . .
H9A H 0.1185 0.5353 0.4407 0.051 Uiso 1 1 calc R . .
H9B H 0.2422 0.6388 0.4788 0.051 Uiso 1 1 calc R . .
C10 C -0.3774(11) 0.3513(7) 0.0872(4) 0.068(2) Uani 1 1 d . . .
H10 H -0.4520 0.3576 0.0581 0.082 Uiso 1 1 calc R . .
C11 C 0.1476(8) 0.4947(6) 0.2107(3) 0.0440(16) Uani 1 1 d . . .
H11 H 0.1173 0.4755 0.1700 0.053 Uiso 1 1 calc R . .
C12 C 0.2197(8) 0.2009(6) 0.2734(3) 0.0537(18) Uani 1 1 d . . .
H12 H 0.2617 0.2327 0.2411 0.064 Uiso 1 1 calc R . .
C13 C -0.7174(7) -0.2123(5) 0.1216(3) 0.0356(14) Uani 1 1 d . . .
H13 H -0.7801 -0.1641 0.1357 0.043 Uiso 1 1 calc R . .
C14 C 0.5659(9) 0.9187(6) 0.3533(4) 0.067(2) Uani 1 1 d . . .
H14 H 0.6184 0.9876 0.3428 0.080 Uiso 1 1 calc R . .
C15 C 0.0823(7) 0.4193(5) 0.2482(3) 0.0376(14) Uani 1 1 d . . .
C16 C -0.4449(7) -0.0692(5) 0.1608(2) 0.0336(13) Uani 1 1 d . . .
C17 C -0.1921(7) 0.1133(5) 0.2117(3) 0.0371(14) Uani 1 1 d . . .
C18 C -0.1953(9) -0.1788(6) 0.0653(3) 0.056(2) Uani 1 1 d . . .
H18A H -0.0842 -0.1381 0.0760 0.067 Uiso 1 1 calc R . .
H18B H -0.1969 -0.2540 0.0446 0.067 Uiso 1 1 calc R . .
C19 C 0.1305(7) 0.4481(5) 0.3095(2) 0.0331(13) Uani 1 1 d . . .
H19 H 0.0897 0.3984 0.3353 0.040 Uiso 1 1 calc R . .
C20 C 0.4769(8) 0.8321(6) 0.3103(3) 0.0535(18) Uani 1 1 d . . .
H20 H 0.4667 0.8424 0.2708 0.064 Uiso 1 1 calc R . .
C21 C -0.3506(8) 0.1179(5) 0.2161(3) 0.0408(15) Uani 1 1 d . . .
H21 H -0.3716 0.1837 0.2361 0.049 Uiso 1 1 calc R . .
C22 C 0.2381(7) 0.5498(5) 0.3310(2) 0.0317(13) Uani 1 1 d . . .
C23 C 0.2984(7) 0.6248(5) 0.2921(3) 0.0357(14) Uani 1 1 d . . .
C24 C 0.2553(8) 0.5963(5) 0.2319(3) 0.0428(16) Uani 1 1 d . . .
H24 H 0.2984 0.6452 0.2060 0.051 Uiso 1 1 calc R . .
C25 C 0.0579(7) 0.1839(5) 0.2805(3) 0.0359(14) Uani 1 1 d . . .
C26 C -0.1619(7) 0.0134(5) 0.1824(3) 0.0416(15) Uani 1 1 d . . .
H26 H -0.0571 0.0070 0.1804 0.050 Uiso 1 1 calc R . .
C27 C -0.6935(7) -0.3913(5) 0.0712(2) 0.0316(13) Uani 1 1 d . . .
C28 C -0.1893(7) -0.2541(6) 0.1600(4) 0.056(2) Uani 1 1 d . . .
H28A H -0.1929 -0.3277 0.1369 0.067 Uiso 1 1 calc R . .
H28B H -0.0778 -0.2119 0.1667 0.067 Uiso 1 1 calc R . .
C29 C 0.4100(8) 0.5220(6) 0.4169(3) 0.0444(16) Uani 1 1 d . . .
H29A H 0.4655 0.5602 0.4552 0.053 Uiso 1 1 calc R . .
H29B H 0.3371 0.4522 0.4235 0.053 Uiso 1 1 calc R . .
C30 C 0.4122(7) 0.7148(5) 0.3863(3) 0.0417(15) Uani 1 1 d . . .
C31 C 0.0799(8) 0.6856(6) 0.4286(3) 0.0515(18) Uani 1 1 d . . .
H31A H 0.0153 0.6546 0.3911 0.062 Uiso 1 1 calc R . .
H31B H 0.1453 0.7601 0.4252 0.062 Uiso 1 1 calc R . .
C32 C -0.4583(7) -0.2489(5) 0.1087(3) 0.0358(14) Uani 1 1 d . . .
C33 C 0.0005(8) 0.1339(6) 0.3284(3) 0.0492(17) Uani 1 1 d . . .
H33 H -0.1085 0.1190 0.3334 0.059 Uiso 1 1 calc R . .
C34 C -0.7888(7) -0.3211(5) 0.0913(3) 0.0372(14) Uani 1 1 d . . .
H34 H -0.8997 -0.3462 0.0848 0.045 Uiso 1 1 calc R . .
C35 C 0.0055(13) -0.1874(8) 0.2871(5) 0.098(3) Uani 1 1 d . . .
H35A H 0.0606 -0.1636 0.2537 0.148 Uiso 1 1 calc R . .
H35B H 0.0795 -0.2030 0.3154 0.148 Uiso 1 1 calc R . .
H35C H -0.0394 -0.1281 0.3057 0.148 Uiso 1 1 calc R . .
C36 C -0.1373(12) 0.7695(11) 0.4696(5) 0.113(4) Uani 1 1 d . . .
H36A H -0.0747 0.8451 0.4686 0.170 Uiso 1 1 calc R . .
H36B H -0.2065 0.7713 0.5015 0.170 Uiso 1 1 calc R . .
H36C H -0.2007 0.7398 0.4324 0.170 Uiso 1 1 calc R . .
C37 C -0.1276(9) -0.2941(6) 0.2657(4) 0.073(3) Uani 1 1 d . . .
H37A H -0.1825 -0.3185 0.2996 0.087 Uiso 1 1 calc R . .
H37B H -0.0819 -0.3544 0.2477 0.087 Uiso 1 1 calc R . .
C38 C -0.5282(7) -0.3568(5) 0.0788(3) 0.0364(14) Uani 1 1 d . . .
H38 H -0.4661 -0.4052 0.0641 0.044 Uiso 1 1 calc R . .
C39 C -0.2875(7) -0.0758(5) 0.1564(3) 0.0367(14) Uani 1 1 d . . .
C40 C -0.2664(10) -0.1189(7) 0.0239(3) 0.071(3) Uani 1 1 d . . .
H40A H -0.2503 -0.0396 0.0412 0.085 Uiso 1 1 calc R . .
H40B H -0.3805 -0.1529 0.0161 0.085 Uiso 1 1 calc R . .
C41 C -0.2502(9) -0.2722(7) 0.2193(3) 0.058(2) Uani 1 1 d . . .
H41A H -0.3434 -0.3365 0.2129 0.070 Uiso 1 1 calc R . .
H41B H -0.2850 -0.2059 0.2363 0.070 Uiso 1 1 calc R . .
C42 C -0.2519(11) -0.0667(10) -0.0798(5) 0.114(4) Uani 1 1 d D . .
H42A H -0.3570 -0.1106 -0.0956 0.171 Uiso 1 1 calc R . .
H42B H -0.1836 -0.0571 -0.1118 0.171 Uiso 1 1 calc R . .
H42C H -0.2579 0.0064 -0.0597 0.171 Uiso 1 1 calc R . .
C43 C 0.7485(10) 0.3865(9) 0.3665(4) 0.079(3) Uani 1 1 d . . .
H43A H 0.6982 0.3459 0.3284 0.118 Uiso 1 1 calc R . .
H43B H 0.8000 0.3388 0.3857 0.118 Uiso 1 1 calc R . .
H43C H 0.8268 0.4536 0.3610 0.118 Uiso 1 1 calc R . .
C44 C -0.2789(7) -0.1907(5) 0.1219(3) 0.0436(16) Uani 1 1 d . . .
C45 C -0.5525(7) -0.1762(5) 0.1305(2) 0.0311(13) Uani 1 1 d . . .
C46 C 0.3100(7) 0.5983(5) 0.3947(3) 0.0368(14) Uani 1 1 d . . .
C47 C -0.1831(10) -0.1289(8) -0.0353(4) 0.080(3) Uani 1 1 d D . .
H47A H -0.0688 -0.0960 -0.0272 0.096 Uiso 1 1 calc R . .
H47B H -0.1999 -0.2084 -0.0525 0.096 Uiso 1 1 calc R . .
C48 C -0.2754(11) 0.2848(7) 0.0732(3) 0.070(2) Uani 1 1 d . . .
H48 H -0.2793 0.2470 0.0343 0.084 Uiso 1 1 calc R . .
C49 C 0.5762(9) 0.9024(7) 0.4107(4) 0.069(2) Uani 1 1 d . . .
C50 C 0.6250(9) 0.4194(7) 0.4044(3) 0.059(2) Uani 1 1 d . . .
H50A H 0.6771 0.4613 0.4426 0.071 Uiso 1 1 calc R . .
H50B H 0.5505 0.3510 0.4119 0.071 Uiso 1 1 calc R . .
C51 C -0.0417(7) 0.3140(5) 0.2217(3) 0.0388(15) Uani 1 1 d . . .
C52 C -0.1658(9) 0.2732(6) 0.1163(3) 0.0530(18) Uani 1 1 d . . .
H52 H -0.0964 0.2276 0.1063 0.064 Uiso 1 1 calc R . .
C53 C -0.2593(9) 0.3981(6) 0.1877(3) 0.0524(18) Uani 1 1 d . . .
H53 H -0.2533 0.4381 0.2262 0.063 Uiso 1 1 calc R . .
C54 C -0.3710(10) 0.4094(7) 0.1444(4) 0.068(2) Uani 1 1 d . . .
H54 H -0.4402 0.4554 0.1539 0.082 Uiso 1 1 calc R . .
C55 C 0.3200(9) 0.1711(8) 0.3139(4) 0.068(2) Uani 1 1 d . . .
H55 H 0.4286 0.1840 0.3087 0.081 Uiso 1 1 calc R . .
C56 C 0.1021(10) 0.1054(7) 0.3694(4) 0.063(2) Uani 1 1 d . . .
H56 H 0.0614 0.0745 0.4021 0.075 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C49 1.910(7) . ?
C1 C56 1.366(11) . ?
C1 C55 1.368(12) . ?
C1 H1 0.9300 . ?
C2 C53 1.371(10) . ?
C2 C52 1.391(9) . ?
C2 C51 1.504(9) . ?
Br2 C27 1.895(5) . ?
C3 C16 1.388(8) . ?
C3 C21 1.388(8) . ?
C3 H3 0.9300 . ?
C4 C30 1.385(9) . ?
C4 C20 1.398(9) . ?
C4 C23 1.464(8) . ?
C5 C49 1.377(11) . ?
C5 C30 1.379(9) . ?
C5 H5 0.9300 . ?
C6 C51 1.332(9) . ?
C6 C25 1.484(9) . ?
C6 C17 1.509(8) . ?
C7 C36 1.453(13) . ?
C7 C31 1.551(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C29 1.505(9) . ?
C8 C50 1.522(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C31 1.489(10) . ?
C9 C46 1.532(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C48 1.359(12) . ?
C10 C54 1.378(12) . ?
C10 H10 0.9300 . ?
C11 C24 1.370(9) . ?
C11 C15 1.391(9) . ?
C11 H11 0.9300 . ?
C12 C25 1.383(9) . ?
C12 C55 1.388(10) . ?
C12 H12 0.9300 . ?
C13 C45 1.382(8) . ?
C13 C34 1.389(8) . ?
C13 H13 0.9300 . ?
C14 C49 1.355(12) . ?
C14 C20 1.380(10) . ?
C14 H14 0.9300 . ?
C15 C19 1.405(8) . ?
C15 C51 1.492(8) . ?
C16 C39 1.390(8) . ?
C16 C45 1.466(8) . ?
C17 C21 1.392(9) . ?
C17 C26 1.396(8) . ?
C18 C40 1.480(11) . ?
C18 C44 1.514(9) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C22 1.372(8) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.399(8) . ?
C22 C46 1.524(8) . ?
C23 C24 1.375(8) . ?
C24 H24 0.9300 . ?
C25 C33 1.384(9) . ?
C26 C39 1.379(8) . ?
C26 H26 0.9300 . ?
C27 C34 1.378(9) . ?
C27 C38 1.383(8) . ?
C28 C41 1.497(11) . ?
C28 C44 1.550(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C46 1.545(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C46 1.533(8) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C38 1.377(8) . ?
C32 C45 1.402(8) . ?
C32 C44 1.537(8) . ?
C33 C56 1.393(10) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C37 1.519(11) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C41 1.563(10) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38 0.9300 . ?
C39 C44 1.531(8) . ?
C40 C47 1.557(11) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C47 1.5392(10) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C50 1.495(11) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C52 1.382(11) . ?
C48 H48 0.9300 . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C52 H52 0.9300 . ?
C53 C54 1.397(10) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 H55 0.9300 . ?
C56 H56 0.9300 . ?

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
C56 C1 C55 119.2(7) . . ?
C56 C1 H1 120.4 . . ?
C55 C1 H1 120.4 . . ?
C53 C2 C52 118.4(6) . . ?
C53 C2 C51 121.2(6) . . ?
C52 C2 C51 120.4(6) . . ?
C16 C3 C21 118.2(6) . . ?
C16 C3 H3 120.9 . . ?
C21 C3 H3 120.9 . . ?
C30 C4 C20 120.5(6) . . ?
C30 C4 C23 108.7(5) . . ?
C20 C4 C23 130.7(6) . . ?
C49 C5 C30 118.3(7) . . ?
C49 C5 H5 120.8 . . ?
C30 C5 H5 120.8 . . ?
C51 C6 C25 126.2(5) . . ?
C51 C6 C17 120.3(6) . . ?
C25 C6 C17 113.5(5) . . ?
C36 C7 C31 112.9(8) . . ?
C36 C7 H7A 109.0 . . ?
C31 C7 H7A 109.0 . . ?
C36 C7 H7B 109.0 . . ?
C31 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C29 C8 C50 110.8(6) . . ?
C29 C8 H8A 109.5 . . ?
C50 C8 H8A 109.5 . . ?
C29 C8 H8B 109.5 . . ?
C50 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C31 C9 C46 116.9(5) . . ?
C31 C9 H9A 108.1 . . ?
C46 C9 H9A 108.1 . . ?
C31 C9 H9B 108.1 . . ?
C46 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C48 C10 C54 120.5(7) . . ?
C48 C10 H10 119.7 . . ?
C54 C10 H10 119.7 . . ?
C24 C11 C15 122.0(6) . . ?
C24 C11 H11 119.0 . . ?
C15 C11 H11 119.0 . . ?
C25 C12 C55 120.7(7) . . ?
C25 C12 H12 119.7 . . ?
C55 C12 H12 119.7 . . ?
C45 C13 C34 119.6(6) . . ?
C45 C13 H13 120.2 . . ?
C34 C13 H13 120.2 . . ?
C49 C14 C20 119.5(7) . . ?
C49 C14 H14 120.3 . . ?
C20 C14 H14 120.3 . . ?
C11 C15 C19 118.7(5) . . ?
C11 C15 C51 118.2(5) . . ?
C19 C15 C51 123.0(5) . . ?
C3 C16 C39 120.4(5) . . ?
C3 C16 C45 130.6(6) . . ?
C39 C16 C45 109.0(5) . . ?
C21 C17 C26 118.4(5) . . ?
C21 C17 C6 122.0(5) . . ?
C26 C17 C6 119.6(5) . . ?
C40 C18 C44 114.5(6) . . ?
C40 C18 H18A 108.6 . . ?
C44 C18 H18A 108.6 . . ?
C40 C18 H18B 108.6 . . ?
C44 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C22 C19 C15 119.6(5) . . ?
C22 C19 H19 120.2 . . ?
C15 C19 H19 120.2 . . ?
C14 C20 C4 118.9(7) . . ?
C14 C20 H20 120.5 . . ?
C4 C20 H20 120.5 . . ?
C3 C21 C17 122.2(6) . . ?
C3 C21 H21 118.9 . . ?
C17 C21 H21 118.9 . . ?
C19 C22 C23 120.2(5) . . ?
C19 C22 C46 129.1(5) . . ?
C23 C22 C46 110.7(5) . . ?
C24 C23 C22 120.8(5) . . ?
C24 C23 C4 130.6(5) . . ?
C22 C23 C4 108.6(5) . . ?
C11 C24 C23 118.8(6) . . ?
C11 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C12 C25 C33 117.5(6) . . ?
C12 C25 C6 122.3(6) . . ?
C33 C25 C6 120.1(6) . . ?
C39 C26 C17 119.9(6) . . ?
C39 C26 H26 120.1 . . ?
C17 C26 H26 120.1 . . ?
C34 C27 C38 122.4(5) . . ?
C34 C27 Br2 118.6(4) . . ?
C38 C27 Br2 119.0(4) . . ?
C41 C28 C44 116.6(5) . . ?
C41 C28 H28A 108.1 . . ?
C44 C28 H28A 108.1 . . ?
C41 C28 H28B 108.1 . . ?
C44 C28 H28B 108.1 . . ?
H28A C28 H28B 107.3 . . ?
C8 C29 C46 116.2(5) . . ?
C8 C29 H29A 108.2 . . ?
C46 C29 H29A 108.2 . . ?
C8 C29 H29B 108.2 . . ?
C46 C29 H29B 108.2 . . ?
H29A C29 H29B 107.4 . . ?
C5 C30 C4 119.9(6) . . ?
C5 C30 C46 128.9(6) . . ?
C4 C30 C46 111.1(5) . . ?
C9 C31 C7 111.8(6) . . ?
C9 C31 H31A 109.3 . . ?
C7 C31 H31A 109.3 . . ?
C9 C31 H31B 109.3 . . ?
C7 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
C38 C32 C45 120.7(5) . . ?
C38 C32 C44 127.9(5) . . ?
C45 C32 C44 111.4(5) . . ?
C25 C33 C56 121.5(7) . . ?
C25 C33 H33 119.2 . . ?
C56 C33 H33 119.2 . . ?
C27 C34 C13 119.2(5) . . ?
C27 C34 H34 120.4 . . ?
C13 C34 H34 120.4 . . ?
C37 C35 H35A 109.5 . . ?
C37 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C37 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C7 C36 H36A 109.5 . . ?
C7 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C7 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 C41 111.0(7) . . ?
C35 C37 H37A 109.4 . . ?
C41 C37 H37A 109.4 . . ?
C35 C37 H37B 109.4 . . ?
C41 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
C32 C38 C27 118.1(6) . . ?
C32 C38 H38 121.0 . . ?
C27 C38 H38 121.0 . . ?
C26 C39 C16 120.8(6) . . ?
C26 C39 C44 127.7(6) . . ?
C16 C39 C44 111.5(5) . . ?
C18 C40 C47 108.0(7) . . ?
C18 C40 H40A 110.1 . . ?
C47 C40 H40A 110.1 . . ?
C18 C40 H40B 110.1 . . ?
C47 C40 H40B 110.1 . . ?
H40A C40 H40B 108.4 . . ?
C28 C41 C37 115.4(7) . . ?
C28 C41 H41A 108.4 . . ?
C37 C41 H41A 108.4 . . ?
C28 C41 H41B 108.4 . . ?
C37 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
C47 C42 H42A 109.5 . . ?
C47 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C47 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C50 C43 H43A 109.5 . . ?
C50 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C50 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C18 C44 C39 112.2(5) . . ?
C18 C44 C32 111.9(5) . . ?
C39 C44 C32 100.0(5) . . ?
C18 C44 C28 107.8(6) . . ?
C39 C44 C28 111.7(5) . . ?
C32 C44 C28 113.1(5) . . ?
C13 C45 C32 120.0(5) . . ?
C13 C45 C16 132.0(6) . . ?
C32 C45 C16 107.9(5) . . ?
C22 C46 C9 114.0(5) . . ?
C22 C46 C30 100.8(5) . . ?
C9 C46 C30 111.2(5) . . ?
C22 C46 C29 110.4(5) . . ?
C9 C46 C29 107.5(5) . . ?
C30 C46 C29 113.0(5) . . ?
C42 C47 C40 110.0(8) . . ?
C42 C47 H47A 109.7 . . ?
C40 C47 H47A 109.7 . . ?
C42 C47 H47B 109.7 . . ?
C40 C47 H47B 109.7 . . ?
H47A C47 H47B 108.2 . . ?
C10 C48 C52 120.3(8) . . ?
C10 C48 H48 119.9 . . ?
C52 C48 H48 119.9 . . ?
C14 C49 C5 122.8(7) . . ?
C14 C49 Br1 117.6(6) . . ?
C5 C49 Br1 119.5(7) . . ?
C43 C50 C8 113.5(7) . . ?
C43 C50 H50A 108.9 . . ?
C8 C50 H50A 108.9 . . ?
C43 C50 H50B 108.9 . . ?
C8 C50 H50B 108.9 . . ?
H50A C50 H50B 107.7 . . ?
C6 C51 C15 124.5(6) . . ?
C6 C51 C2 120.5(5) . . ?
C15 C51 C2 115.0(5) . . ?
C48 C52 C2 120.6(8) . . ?
C48 C52 H52 119.7 . . ?
C2 C52 H52 119.7 . . ?
C2 C53 C54 121.2(7) . . ?
C2 C53 H53 119.4 . . ?
C54 C53 H53 119.4 . . ?
C10 C54 C53 119.0(8) . . ?
C10 C54 H54 120.5 . . ?
C53 C54 H54 120.5 . . ?
C1 C55 C12 121.1(7) . . ?
C1 C55 H55 119.5 . . ?
C12 C55 H55 119.5 . . ?
C1 C56 C33 120.0(8) . . ?
C1 C56 H56 120.0 . . ?
C33 C56 H56 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.76
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         3.415
_refine_diff_density_min         -2.185
_refine_diff_density_rms         0.098


_database_code_depnum_ccdc_archive 'CCDC 909142'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_lya_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H60'
_chemical_formula_sum            'C56 H60'
_chemical_formula_weight         733.04

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1014(9)
_cell_length_b                   11.6074(9)
_cell_length_c                   17.9752(14)
_cell_angle_alpha                101.9160(10)
_cell_angle_beta                 105.0510(10)
_cell_angle_gamma                92.1080(10)
_cell_volume                     2178.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'APEX2 Software Suite (Bruker,2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25685
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         27.53
_reflns_number_total             9872
_reflns_number_gt                8392
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0560P)²+0.6424P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9872
_refine_ls_number_parameters     509
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1136
_refine_ls_wR_factor_gt          0.1075
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.07792(16) 0.67328(18) 0.07523(10) 0.0527(4) Uani 1 1 d . . .
H1A H 0.1105 0.7523 0.1039 0.079 Uiso 1 1 calc R . .
H1B H 0.0361 0.6740 0.0214 0.079 Uiso 1 1 calc R . .
H1C H 0.1455 0.6238 0.0764 0.079 Uiso 1 1 calc R . .
C2 C -0.01460(13) 0.62520(14) 0.11320(8) 0.0360(3) Uani 1 1 d . . .
H2A H -0.0828 0.6753 0.1117 0.043 Uiso 1 1 calc R . .
H2B H -0.0497 0.5466 0.0828 0.043 Uiso 1 1 calc R . .
C3 C 0.04533(11) 0.61919(11) 0.19824(7) 0.0247(2) Uani 1 1 d . . .
H3A H 0.0818 0.6976 0.2284 0.030 Uiso 1 1 calc R . .
H3B H 0.1126 0.5680 0.1996 0.030 Uiso 1 1 calc R . .
C4 C -0.04702(10) 0.57315(10) 0.23729(6) 0.0207(2) Uani 1 1 d . . .
H4A H -0.0832 0.4949 0.2068 0.025 Uiso 1 1 calc R . .
H4B H -0.1145 0.6242 0.2351 0.025 Uiso 1 1 calc R . .
C5 C 0.00884(10) 0.56584(9) 0.32374(6) 0.0186(2) Uani 1 1 d . . .
C6 C 0.12045(10) 0.49133(9) 0.33430(6) 0.0182(2) Uani 1 1 d . . .
C7 C 0.13050(10) 0.37825(9) 0.29401(6) 0.0183(2) Uani 1 1 d . . .
H7 H 0.0624 0.3365 0.2544 0.022 Uiso 1 1 calc R . .
C8 C 0.24371(10) 0.32698(9) 0.31311(6) 0.0181(2) Uani 1 1 d . . .
C9 C 0.25747(10) 0.20479(9) 0.27083(6) 0.0178(2) Uani 1 1 d . . .
C10 C 0.29408(9) 0.12029(9) 0.31192(6) 0.0169(2) Uani 1 1 d . . .
C11 C 0.33568(9) 0.00465(9) 0.27912(6) 0.0164(2) Uani 1 1 d . . .
C12 C 0.41356(9) -0.00384(9) 0.22825(6) 0.0164(2) Uani 1 1 d . . .
H12 H 0.4372 0.0628 0.2123 0.020 Uiso 1 1 calc R . .
C13 C 0.45488(9) -0.11155(9) 0.20205(6) 0.0162(2) Uani 1 1 d . . .
C14 C 0.53739(10) -0.14072(9) 0.14616(6) 0.0179(2) Uani 1 1 d . . .
C15 C 0.66489(10) -0.06505(10) 0.17726(6) 0.0205(2) Uani 1 1 d . . .
H15A H 0.7143 -0.0897 0.1405 0.025 Uiso 1 1 calc R . .
H15B H 0.6499 0.0167 0.1771 0.025 Uiso 1 1 calc R . .
C16 C 0.74228(11) -0.07047(11) 0.25967(7) 0.0243(2) Uani 1 1 d . . .
H16A H 0.7597 -0.1516 0.2603 0.029 Uiso 1 1 calc R . .
H16B H 0.6939 -0.0459 0.2970 0.029 Uiso 1 1 calc R . .
C17 C 0.86613(11) 0.00814(11) 0.28601(8) 0.0278(3) Uani 1 1 d . . .
H17A H 0.8484 0.0885 0.2829 0.033 Uiso 1 1 calc R . .
H17B H 0.9063 0.0087 0.3409 0.033 Uiso 1 1 calc R . .
C18 C 0.95665(12) -0.03063(13) 0.23742(9) 0.0373(3) Uani 1 1 d . . .
H18A H 0.9701 -0.1120 0.2369 0.056 Uiso 1 1 calc R . .
H18B H 1.0350 0.0176 0.2603 0.056 Uiso 1 1 calc R . .
H18C H 0.9221 -0.0220 0.1843 0.056 Uiso 1 1 calc R . .
C19 C 0.16342(13) -0.22851(12) -0.10372(8) 0.0358(3) Uani 1 1 d . . .
H19A H 0.1637 -0.3122 -0.1074 0.054 Uiso 1 1 calc R . .
H19B H 0.1380 -0.2136 -0.1559 0.054 Uiso 1 1 calc R . .
H19C H 0.1059 -0.1978 -0.0746 0.054 Uiso 1 1 calc R . .
C20 C 0.29423(12) -0.16828(12) -0.06144(7) 0.0284(3) Uani 1 1 d . . .
H20A H 0.2930 -0.0840 -0.0585 0.034 Uiso 1 1 calc R . .
H20B H 0.3508 -0.1973 -0.0925 0.034 Uiso 1 1 calc R . .
C21 C 0.34510(11) -0.18814(10) 0.02181(6) 0.0228(2) Uani 1 1 d . . .
H21A H 0.2873 -0.1622 0.0527 0.027 Uiso 1 1 calc R . .
H21B H 0.3510 -0.2720 0.0190 0.027 Uiso 1 1 calc R . .
C22 C 0.47361(10) -0.12131(10) 0.06291(6) 0.0209(2) Uani 1 1 d . . .
H22A H 0.4655 -0.0374 0.0672 0.025 Uiso 1 1 calc R . .
H22B H 0.5287 -0.1439 0.0295 0.025 Uiso 1 1 calc R . .
C23 C 0.55018(10) -0.27146(10) 0.14475(6) 0.0201(2) Uani 1 1 d . . .
C24 C 0.48329(10) -0.31148(10) 0.19227(6) 0.0197(2) Uani 1 1 d . . .
C25 C 0.48210(12) -0.42866(10) 0.19960(7) 0.0269(3) Uani 1 1 d . . .
H25 H 0.4388 -0.4549 0.2318 0.032 Uiso 1 1 calc R . .
C26 C 0.54706(13) -0.50566(11) 0.15771(8) 0.0325(3) Uani 1 1 d . . .
H26 H 0.5470 -0.5842 0.1618 0.039 Uiso 1 1 calc R . .
C27 C 0.61188(12) -0.46646(11) 0.10989(8) 0.0322(3) Uani 1 1 d . . .
H27 H 0.6542 -0.5192 0.0819 0.039 Uiso 1 1 calc R . .
C28 C 0.61433(11) -0.34894(11) 0.10328(7) 0.0267(3) Uani 1 1 d . . .
H28 H 0.6584 -0.3229 0.0714 0.032 Uiso 1 1 calc R . .
C29 C 0.42284(10) -0.21216(9) 0.22732(6) 0.0172(2) Uani 1 1 d . . .
C30 C 0.30088(10) 0.14290(9) 0.39796(6) 0.0189(2) Uani 1 1 d . . .
C31 C 0.20141(11) 0.18621(10) 0.42600(7) 0.0240(2) Uani 1 1 d . . .
H31 H 0.1269 0.1954 0.3904 0.029 Uiso 1 1 calc R . .
C32 C 0.21289(14) 0.21559(11) 0.50662(8) 0.0324(3) Uani 1 1 d . . .
H32 H 0.1462 0.2446 0.5247 0.039 Uiso 1 1 calc R . .
C33 C 0.32303(15) 0.20185(12) 0.56013(7) 0.0355(3) Uani 1 1 d . . .
H33 H 0.3314 0.2240 0.6141 0.043 Uiso 1 1 calc R . .
C34 C 0.42071(13) 0.15502(11) 0.53315(7) 0.0322(3) Uani 1 1 d . . .
H34 H 0.4941 0.1439 0.5689 0.039 Uiso 1 1 calc R . .
C35 C 0.40888(11) 0.12460(10) 0.45237(7) 0.0238(2) Uani 1 1 d . . .
H35 H 0.4741 0.0916 0.4345 0.029 Uiso 1 1 calc R . .
C36 C 0.34658(10) 0.39262(10) 0.37130(7) 0.0220(2) Uani 1 1 d . . .
H36 H 0.4217 0.3588 0.3839 0.026 Uiso 1 1 calc R . .
C37 C 0.33847(11) 0.50709(10) 0.41043(7) 0.0229(2) Uani 1 1 d . . .
H37 H 0.4076 0.5503 0.4484 0.027 Uiso 1 1 calc R . .
C38 C 0.22502(10) 0.55589(9) 0.39189(6) 0.0191(2) Uani 1 1 d . . .
C39 C 0.06988(10) 0.68479(9) 0.37750(6) 0.0192(2) Uani 1 1 d . . .
C40 C 0.01859(11) 0.79172(10) 0.38989(7) 0.0227(2) Uani 1 1 d . . .
H40 H -0.0625 0.7992 0.3614 0.027 Uiso 1 1 calc R . .
C41 C 0.09026(12) 0.88797(10) 0.44564(7) 0.0258(2) Uani 1 1 d . . .
H41 H 0.0570 0.9604 0.4536 0.031 Uiso 1 1 calc R . .
C42 C 0.21052(12) 0.87711(10) 0.48943(7) 0.0263(3) Uani 1 1 d . . .
H42 H 0.2562 0.9415 0.5275 0.032 Uiso 1 1 calc R . .
C43 C 0.26304(11) 0.77044(10) 0.47673(7) 0.0240(2) Uani 1 1 d . . .
H43 H 0.3438 0.7629 0.5058 0.029 Uiso 1 1 calc R . .
C44 C 0.19265(10) 0.67517(9) 0.41979(6) 0.0197(2) Uani 1 1 d . . .
C45 C -0.09486(11) 0.52408(10) 0.35893(7) 0.0225(2) Uani 1 1 d . . .
H45A H -0.0560 0.5233 0.4138 0.027 Uiso 1 1 calc R . .
H45B H -0.1545 0.5831 0.3586 0.027 Uiso 1 1 calc R . .
C46 C -0.16796(11) 0.40399(10) 0.31914(8) 0.0266(3) Uani 1 1 d . . .
H46A H -0.1121 0.3424 0.3261 0.032 Uiso 1 1 calc R . .
H46B H -0.1997 0.3994 0.2629 0.032 Uiso 1 1 calc R . .
C47 C -0.27711(13) 0.38253(12) 0.35284(8) 0.0323(3) Uani 1 1 d . . .
H47A H -0.2447 0.3856 0.4089 0.039 Uiso 1 1 calc R . .
H47B H -0.3314 0.4456 0.3472 0.039 Uiso 1 1 calc R . .
C48 C -0.35391(13) 0.26488(12) 0.31308(9) 0.0373(3) Uani 1 1 d . . .
H48A H -0.3835 0.2598 0.2572 0.056 Uiso 1 1 calc R . .
H48B H -0.4241 0.2587 0.3344 0.056 Uiso 1 1 calc R . .
H48C H -0.3027 0.2017 0.3224 0.056 Uiso 1 1 calc R . .
C49 C 0.23317(10) 0.18829(10) 0.18363(6) 0.0196(2) Uani 1 1 d . . .
C50 C 0.17416(10) 0.08384(10) 0.13041(7) 0.0228(2) Uani 1 1 d . . .
H50 H 0.1480 0.0212 0.1493 0.027 Uiso 1 1 calc R . .
C51 C 0.15414(11) 0.07257(12) 0.04967(7) 0.0294(3) Uani 1 1 d . . .
H51 H 0.1158 0.0021 0.0150 0.035 Uiso 1 1 calc R . .
C52 C 0.19081(15) 0.16532(13) 0.02043(8) 0.0385(3) Uani 1 1 d . . .
H52 H 0.1774 0.1572 -0.0337 0.046 Uiso 1 1 calc R . .
C53 C 0.24737(17) 0.27004(13) 0.07202(8) 0.0432(4) Uani 1 1 d . . .
H53 H 0.2715 0.3329 0.0526 0.052 Uiso 1 1 calc R . .
C54 C 0.26812(13) 0.28118(11) 0.15279(7) 0.0315(3) Uani 1 1 d . . .
H54 H 0.3061 0.3520 0.1871 0.038 Uiso 1 1 calc R . .
C55 C 0.30285(10) -0.09717(9) 0.30297(6) 0.0180(2) Uani 1 1 d . . .
H55 H 0.2510 -0.0921 0.3364 0.022 Uiso 1 1 calc R . .
C56 C 0.34600(10) -0.20532(9) 0.27778(6) 0.0184(2) Uani 1 1 d . . .
H56 H 0.3239 -0.2719 0.2944 0.022 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.520(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.5177(17) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.5224(16) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.5377(15) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C39 1.5295(15) . ?
C5 C6 1.5309(15) . ?
C5 C45 1.5571(15) . ?
C6 C7 1.3857(15) . ?
C6 C38 1.4043(15) . ?
C7 C8 1.4025(15) . ?
C7 H7 0.9300 . ?
C8 C36 1.4018(15) . ?
C8 C9 1.4978(14) . ?
C9 C10 1.3585(15) . ?
C9 C49 1.4897(15) . ?
C10 C11 1.4910(14) . ?
C10 C30 1.4956(14) . ?
C11 C55 1.4043(15) . ?
C11 C12 1.4046(14) . ?
C12 C13 1.3808(14) . ?
C12 H12 0.9300 . ?
C13 C29 1.4032(15) . ?
C13 C14 1.5243(14) . ?
C14 C23 1.5251(15) . ?
C14 C15 1.5435(15) . ?
C14 C22 1.5466(15) . ?
C15 C16 1.5225(16) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.5292(16) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.5173(18) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.5191(18) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.5246(16) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.5223(16) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C28 1.3848(15) . ?
C23 C24 1.4016(16) . ?
C24 C25 1.3932(16) . ?
C24 C29 1.4674(15) . ?
C25 C26 1.3919(17) . ?
C25 H25 0.9300 . ?
C26 C27 1.386(2) . ?
C26 H26 0.9300 . ?
C27 C28 1.3934(18) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C56 1.3905(15) . ?
C30 C35 1.3909(16) . ?
C30 C31 1.3969(15) . ?
C31 C32 1.3891(17) . ?
C31 H31 0.9300 . ?
C32 C33 1.383(2) . ?
C32 H32 0.9300 . ?
C33 C34 1.384(2) . ?
C33 H33 0.9300 . ?
C34 C35 1.3914(17) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.3870(15) . ?
C36 H36 0.9300 . ?
C37 C38 1.3894(16) . ?
C37 H37 0.9300 . ?
C38 C44 1.4633(15) . ?
C39 C40 1.3849(15) . ?
C39 C44 1.3986(16) . ?
C40 C41 1.3941(17) . ?
C40 H40 0.9300 . ?
C41 C42 1.3876(18) . ?
C41 H41 0.9300 . ?
C42 C43 1.3895(16) . ?
C42 H42 0.9300 . ?
C43 C44 1.3909(15) . ?
C43 H43 0.9300 . ?
C45 C46 1.5221(16) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.5228(16) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.5158(18) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 C50 1.3968(15) . ?
C49 C54 1.3957(17) . ?
C50 C51 1.3873(17) . ?
C50 H50 0.9300 . ?
C51 C52 1.383(2) . ?
C51 H51 0.9300 . ?
C52 C53 1.381(2) . ?
C52 H52 0.9300 . ?
C53 C54 1.3873(18) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 C56 1.3902(15) . ?
C55 H55 0.9300 . ?
C56 H56 0.9300 . ?

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 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 112.57(12) . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C2 C3 C4 113.01(10) . . ?
C2 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C5 115.12(9) . . ?
C3 C4 H4A 108.5 . . ?
C5 C4 H4A 108.5 . . ?
C3 C4 H4B 108.5 . . ?
C5 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C39 C5 C6 100.79(8) . . ?
C39 C5 C4 113.04(9) . . ?
C6 C5 C4 112.76(9) . . ?
C39 C5 C45 106.43(9) . . ?
C6 C5 C45 112.61(9) . . ?
C4 C5 C45 110.72(9) . . ?
C7 C6 C38 119.89(10) . . ?
C7 C6 C5 129.48(10) . . ?
C38 C6 C5 110.56(9) . . ?
C6 C7 C8 119.81(10) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C36 119.30(10) . . ?
C7 C8 C9 121.11(9) . . ?
C36 C8 C9 119.57(10) . . ?
C10 C9 C49 124.89(10) . . ?
C10 C9 C8 120.47(9) . . ?
C49 C9 C8 114.60(9) . . ?
C9 C10 C11 125.10(9) . . ?
C9 C10 C30 119.81(9) . . ?
C11 C10 C30 115.03(9) . . ?
C55 C11 C12 118.85(9) . . ?
C55 C11 C10 119.62(9) . . ?
C12 C11 C10 121.42(9) . . ?
C13 C12 C11 119.69(9) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C29 120.81(9) . . ?
C12 C13 C14 128.28(9) . . ?
C29 C13 C14 110.91(9) . . ?
C13 C14 C23 101.13(8) . . ?
C13 C14 C15 112.04(9) . . ?
C23 C14 C15 112.57(9) . . ?
C13 C14 C22 111.80(9) . . ?
C23 C14 C22 111.45(9) . . ?
C15 C14 C22 107.85(8) . . ?
C16 C15 C14 116.10(9) . . ?
C16 C15 H15A 108.3 . . ?
C14 C15 H15A 108.3 . . ?
C16 C15 H15B 108.3 . . ?
C14 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
C15 C16 C17 112.53(10) . . ?
C15 C16 H16A 109.1 . . ?
C17 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
C17 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C18 C17 C16 113.99(10) . . ?
C18 C17 H17A 108.8 . . ?
C16 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
C16 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C19 C20 C21 113.91(11) . . ?
C19 C20 H20A 108.8 . . ?
C21 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C22 C21 C20 111.78(10) . . ?
C22 C21 H21A 109.3 . . ?
C20 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C20 C21 H21B 109.3 . . ?
H21A C21 H21B 107.9 . . ?
C21 C22 C14 116.13(9) . . ?
C21 C22 H22A 108.3 . . ?
C14 C22 H22A 108.3 . . ?
C21 C22 H22B 108.3 . . ?
C14 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C28 C23 C24 120.14(11) . . ?
C28 C23 C14 128.79(10) . . ?
C24 C23 C14 111.05(9) . . ?
C25 C24 C23 120.72(10) . . ?
C25 C24 C29 130.90(11) . . ?
C23 C24 C29 108.38(9) . . ?
C26 C25 C24 118.60(12) . . ?
C26 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C27 C26 C25 120.68(11) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 120.74(11) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C23 C28 C27 119.10(12) . . ?
C23 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C56 C29 C13 120.24(10) . . ?
C56 C29 C24 131.24(10) . . ?
C13 C29 C24 108.52(9) . . ?
C35 C30 C31 118.42(10) . . ?
C35 C30 C10 120.33(10) . . ?
C31 C30 C10 121.22(10) . . ?
C32 C31 C30 120.52(12) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C33 C32 C31 120.28(12) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C32 C33 C34 119.84(11) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C33 C34 C35 119.89(12) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C30 C35 C34 120.93(11) . . ?
C30 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C37 C36 C8 121.31(10) . . ?
C37 C36 H36 119.3 . . ?
C8 C36 H36 119.3 . . ?
C36 C37 C38 118.73(10) . . ?
C36 C37 H37 120.6 . . ?
C38 C37 H37 120.6 . . ?
C37 C38 C6 120.92(10) . . ?
C37 C38 C44 130.15(10) . . ?
C6 C38 C44 108.79(9) . . ?
C40 C39 C44 119.92(10) . . ?
C40 C39 C5 129.02(10) . . ?
C44 C39 C5 111.02(9) . . ?
C39 C40 C41 119.06(11) . . ?
C39 C40 H40 120.5 . . ?
C41 C40 H40 120.5 . . ?
C42 C41 C40 120.90(11) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C43 120.32(11) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
C42 C43 C44 118.77(11) . . ?
C42 C43 H43 120.6 . . ?
C44 C43 H43 120.6 . . ?
C43 C44 C39 120.97(10) . . ?
C43 C44 C38 130.62(11) . . ?
C39 C44 C38 108.41(9) . . ?
C46 C45 C5 118.03(9) . . ?
C46 C45 H45A 107.8 . . ?
C5 C45 H45A 107.8 . . ?
C46 C45 H45B 107.8 . . ?
C5 C45 H45B 107.8 . . ?
H45A C45 H45B 107.1 . . ?
C45 C46 C47 111.98(10) . . ?
C45 C46 H46A 109.2 . . ?
C47 C46 H46A 109.2 . . ?
C45 C46 H46B 109.2 . . ?
C47 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
C48 C47 C46 113.35(11) . . ?
C48 C47 H47A 108.9 . . ?
C46 C47 H47A 108.9 . . ?
C48 C47 H47B 108.9 . . ?
C46 C47 H47B 108.9 . . ?
H47A C47 H47B 107.7 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 C54 117.88(10) . . ?
C50 C49 C9 122.82(10) . . ?
C54 C49 C9 119.29(10) . . ?
C51 C50 C49 120.66(11) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C52 C51 C50 120.49(12) . . ?
C52 C51 H51 119.8 . . ?
C50 C51 H51 119.8 . . ?
C51 C52 C53 119.72(12) . . ?
C51 C52 H52 120.1 . . ?
C53 C52 H52 120.1 . . ?
C52 C53 C54 119.84(13) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C53 C54 C49 121.39(12) . . ?
C53 C54 H54 119.3 . . ?
C49 C54 H54 119.3 . . ?
C56 C55 C11 121.61(10) . . ?
C56 C55 H55 119.2 . . ?
C11 C55 H55 119.2 . . ?
C55 C56 C29 118.77(10) . . ?
C55 C56 H56 120.6 . . ?
C29 C56 H56 120.6 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.041
_database_code_depnum_ccdc_archive 'CCDC 974227'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H26 Br2'
_chemical_formula_weight         666.41

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2

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

_cell_length_a                   25.721(5)
_cell_length_b                   5.527(5)
_cell_length_c                   11.027(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 110.517(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     1468.2(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    2.789
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3395[1874]
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         27.55
_reflns_number_total             8269
_reflns_number_gt                6925
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1253P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0030(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.040(14)
_refine_ls_number_reflns         8269
_refine_ls_number_parameters     192
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1589
_refine_ls_wR_factor_gt          0.1469
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_restrained_S_all      0.829
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.686933(16) 0.04276(9) 1.39841(4) 0.02408(14) Uani 1 1 d . . .
C2 C 0.91221(18) 0.0889(9) 0.5985(4) 0.0257(13) Uani 1 1 d . . .
H2 H 0.8909 -0.0302 0.5440 0.031 Uiso 1 1 calc R . .
C3 C 0.81174(14) 0.0489(13) 1.2460(3) 0.0167(7) Uani 1 1 d . . .
C4 C 0.91963(14) 0.0540(13) 1.0931(3) 0.0178(8) Uani 1 1 d . . .
H4 H 0.9445 -0.0739 1.1206 0.021 Uiso 1 1 calc R . .
C5 C 0.79970(18) 0.2590(8) 1.1681(4) 0.0181(9) Uani 1 1 d . . .
C6 C 0.92523(17) 0.2222(8) 1.0028(4) 0.0156(9) Uani 1 1 d . . .
C7 C 0.83951(18) 0.2723(8) 1.1003(4) 0.0143(8) Uani 1 1 d . . .
C8 C 0.86195(19) -0.0749(8) 1.2362(4) 0.0173(9) Uani 1 1 d . . .
H8A H 0.8533 -0.2391 1.2044 0.021 Uiso 1 1 calc R . .
H8B H 0.8919 -0.0786 1.3194 0.021 Uiso 1 1 calc R . .
C9 C 0.84314(18) 0.4355(9) 1.0073(4) 0.0187(9) Uani 1 1 d . . .
H9 H 0.8177 0.5613 0.9792 0.022 Uiso 1 1 calc R . .
C10 C 0.95960(17) 0.2409(8) 0.8149(4) 0.0168(9) Uani 1 1 d . . .
C11 C 0.75617(17) 0.4103(8) 1.1651(4) 0.0192(9) Uani 1 1 d . . .
H11 H 0.7490 0.5499 1.1148 0.023 Uiso 1 1 calc R . .
C12 C 0.88558(17) 0.4070(8) 0.9572(4) 0.0184(9) Uani 1 1 d . . .
H12 H 0.8877 0.5113 0.8929 0.022 Uiso 1 1 calc R . .
C13 C 0.87698(17) 0.0802(9) 1.1404(4) 0.0164(10) Uani 1 1 d . . .
C14 C 0.92507(16) 0.0693(12) 0.7312(4) 0.0199(10) Uani 1 1 d . . .
H14 H 0.9107 -0.0581 0.7649 0.024 Uiso 1 1 calc R . .
C15 C 0.9311(2) 0.2864(10) 0.5458(5) 0.0285(11) Uani 1 1 d . . .
H15 H 0.9214 0.3026 0.4567 0.034 Uiso 1 1 calc R . .
C16 C 0.97347(18) 0.2226(7) 0.9582(4) 0.0161(9) Uani 1 1 d . . .
C17 C 0.9645(2) 0.4577(8) 0.6295(4) 0.0244(10) Uani 1 1 d . . .
H17 H 0.9778 0.5883 0.5957 0.029 Uiso 1 1 calc R . .
C18 C 0.77841(18) -0.0117(7) 1.3153(4) 0.0171(10) Uani 1 1 d . . .
H18 H 0.7850 -0.1525 1.3646 0.021 Uiso 1 1 calc R . .
C19 C 0.72341(18) 0.3523(8) 1.2375(4) 0.0206(10) Uani 1 1 d . . .
H19 H 0.6944 0.4529 1.2375 0.025 Uiso 1 1 calc R . .
C20 C 0.73487(18) 0.1395(8) 1.3107(4) 0.0187(9) Uani 1 1 d . . .
C25 C 0.97844(19) 0.4371(9) 0.7618(4) 0.0222(10) Uani 1 1 d . . .
H25 H 1.0005 0.5547 0.8161 0.027 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C20 1.891(4) . ?
C2 C14 1.387(6) . ?
C2 C15 1.401(7) . ?
C2 H2 0.9300 . ?
C3 C18 1.375(6) . ?
C3 C5 1.413(7) . ?
C3 C8 1.499(6) . ?
C4 C13 1.378(5) . ?
C4 C6 1.405(7) . ?
C4 H4 0.9300 . ?
C5 C11 1.389(6) . ?
C5 C7 1.466(6) . ?
C6 C12 1.406(6) . ?
C6 C16 1.486(6) . ?
C7 C9 1.393(6) . ?
C7 C13 1.398(6) . ?
C8 C13 1.511(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C12 1.395(6) . ?
C9 H9 0.9300 . ?
C10 C25 1.397(6) . ?
C10 C14 1.402(7) . ?
C10 C16 1.497(6) . ?
C11 C19 1.386(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C14 H14 0.9300 . ?
C15 C17 1.389(7) . ?
C15 H15 0.9300 . ?
C16 C16 1.352(9) 2_757 ?
C17 C25 1.380(6) . ?
C17 H17 0.9300 . ?
C18 C20 1.384(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.398(7) . ?
C19 H19 0.9300 . ?
C25 H25 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 C2 C15 120.6(5) . . ?
C14 C2 H2 119.7 . . ?
C15 C2 H2 119.7 . . ?
C18 C3 C5 119.5(4) . . ?
C18 C3 C8 130.5(5) . . ?
C5 C3 C8 110.0(3) . . ?
C13 C4 C6 119.5(5) . . ?
C13 C4 H4 120.3 . . ?
C6 C4 H4 120.3 . . ?
C11 C5 C3 120.8(4) . . ?
C11 C5 C7 131.2(4) . . ?
C3 C5 C7 108.0(4) . . ?
C4 C6 C12 119.5(4) . . ?
C4 C6 C16 122.7(4) . . ?
C12 C6 C16 117.7(4) . . ?
C9 C7 C13 120.6(4) . . ?
C9 C7 C5 130.3(4) . . ?
C13 C7 C5 109.1(4) . . ?
C3 C8 C13 103.3(4) . . ?
C3 C8 H8A 111.1 . . ?
C13 C8 H8A 111.1 . . ?
C3 C8 H8B 111.1 . . ?
C13 C8 H8B 111.1 . . ?
H8A C8 H8B 109.1 . . ?
C7 C9 C12 118.8(4) . . ?
C7 C9 H9 120.6 . . ?
C12 C9 H9 120.6 . . ?
C25 C10 C14 118.9(4) . . ?
C25 C10 C16 120.4(4) . . ?
C14 C10 C16 120.7(4) . . ?
C19 C11 C5 119.7(4) . . ?
C19 C11 H11 120.2 . . ?
C5 C11 H11 120.2 . . ?
C9 C12 C6 120.7(4) . . ?
C9 C12 H12 119.7 . . ?
C6 C12 H12 119.7 . . ?
C4 C13 C7 120.8(4) . . ?
C4 C13 C8 129.6(5) . . ?
C7 C13 C8 109.6(4) . . ?
C2 C14 C10 120.2(5) . . ?
C2 C14 H14 119.9 . . ?
C10 C14 H14 119.9 . . ?
C17 C15 C2 118.7(4) . . ?
C17 C15 H15 120.7 . . ?
C2 C15 H15 120.7 . . ?
C16 C16 C6 122.3(5) 2_757 . ?
C16 C16 C10 122.0(5) 2_757 . ?
C6 C16 C10 115.6(4) . . ?
C25 C17 C15 121.1(5) . . ?
C25 C17 H17 119.5 . . ?
C15 C17 H17 119.5 . . ?
C3 C18 C20 119.1(4) . . ?
C3 C18 H18 120.4 . . ?
C20 C18 H18 120.4 . . ?
C11 C19 C20 118.6(4) . . ?
C11 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
C18 C20 C19 122.2(4) . . ?
C18 C20 Br1 118.3(3) . . ?
C19 C20 Br1 119.3(3) . . ?
C17 C25 C10 120.5(4) . . ?
C17 C25 H25 119.8 . . ?
C10 C25 H25 119.8 . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.118
_database_code_depnum_ccdc_archive 'CCDC 974229'
