# 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
#  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_(R)-2

_vrf_PLAT057_R-2                 
;
PROBLEM: Correction for Absorption Required   RT(exp) ...       1.43       
RESPONSE:correction in a multiscan-like manner,
         see: _exptl_special_details
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H12 Br2 O2'
_chemical_formula_weight         444.12

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   8.2300(2)
_cell_length_b                   11.8142(3)
_cell_length_c                   17.1253(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1665.11(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    14304
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      26.0

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    4.877
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
All data sets were measured with several scans to increase the number of
redundant reflections. In our experience this method of averaging redundant
reflections replaces in a good approximation semi-empirical absorptions
methods (absorption correction programs like SORTAV lead to no better data
sets).
 
;

_diffrn_ambient_temperature      233(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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10638
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         25.99
_reflns_number_total             3263
_reflns_number_gt                2985
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       ?
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Hydrogen at O1 and O2 could be localized and were refined isotropically
 with bond restraints (d=0.83 angs.).
;

_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)+(0.0269P)²+0.8033P] 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       0.0081(6)
_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   0.039(10)
_refine_ls_number_reflns         3263
_refine_ls_number_parameters     226
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0699
_refine_ls_wR_factor_gt          0.0676
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.71624(5) 0.66082(4) -0.12700(2) 0.05510(13) Uani 1 1 d . . .
Br2 Br 0.04465(5) 0.95747(4) 0.42308(2) 0.05977(15) Uani 1 1 d . . .
O1 O 0.8065(4) 1.0801(2) 0.25399(15) 0.0551(7) Uani 1 1 d D . .
H1O H 0.873(5) 1.130(3) 0.243(3) 0.091(19) Uiso 1 1 d D . .
O2 O 0.9332(3) 0.7495(2) 0.25349(15) 0.0453(6) Uani 1 1 d D . .
H2O H 0.950(6) 0.795(3) 0.2182(19) 0.062(14) Uiso 1 1 d D . .
C1 C 0.7949(4) 1.0271(3) 0.18321(18) 0.0362(7) Uani 1 1 d . . .
C2 C 0.8407(4) 1.0816(3) 0.1138(2) 0.0404(8) Uani 1 1 d . . .
H2 H 0.8807 1.1561 0.1156 0.049 Uiso 1 1 calc . . .
C3 C 0.8276(4) 1.0278(3) 0.04397(19) 0.0394(8) Uani 1 1 d . . .
H3 H 0.8574 1.0660 -0.0020 0.047 Uiso 1 1 calc . . .
C4 C 0.7695(4) 0.9142(3) 0.03933(17) 0.0341(7) Uani 1 1 d . . .
C5 C 0.7626(4) 0.8550(3) -0.03242(18) 0.0400(8) Uani 1 1 d . . .
H5 H 0.7939 0.8907 -0.0791 0.048 Uiso 1 1 calc . . .
C6 C 0.7104(4) 0.7463(3) -0.03291(18) 0.0407(8) Uani 1 1 d . . .
C7 C 0.6583(4) 0.6915(3) 0.0354(2) 0.0403(8) Uani 1 1 d . . .
H7 H 0.6219 0.6161 0.0332 0.048 Uiso 1 1 calc . . .
C8 C 0.6605(4) 0.7477(3) 0.10458(19) 0.0358(7) Uani 1 1 d . . .
H8 H 0.6218 0.7116 0.1498 0.043 Uiso 1 1 calc . . .
C9 C 0.7206(4) 0.8606(2) 0.10955(16) 0.0304(6) Uani 1 1 d . . .
C10 C 0.7331(4) 0.9180(2) 0.18305(17) 0.0316(6) Uani 1 1 d . . .
C11 C 0.6876(4) 0.8601(2) 0.25659(17) 0.0300(6) Uani 1 1 d . . .
C12 C 0.7855(4) 0.7765(3) 0.28686(18) 0.0349(7) Uani 1 1 d . . .
C13 C 0.7419(4) 0.7133(3) 0.35330(19) 0.0411(8) Uani 1 1 d . . .
H13 H 0.8115 0.6564 0.3721 0.049 Uiso 1 1 calc . . .
C14 C 0.5999(4) 0.7346(3) 0.39006(18) 0.0383(8) Uani 1 1 d . . .
H14 H 0.5709 0.6915 0.4341 0.046 Uiso 1 1 calc . . .
C15 C 0.4934(4) 0.8212(2) 0.36316(17) 0.0325(7) Uani 1 1 d . . .
C16 C 0.3453(4) 0.8446(3) 0.40121(18) 0.0376(7) Uani 1 1 d . . .
H16 H 0.3169 0.8048 0.4467 0.045 Uiso 1 1 calc . . .
C17 C 0.2435(4) 0.9247(3) 0.3722(2) 0.0399(7) Uani 1 1 d . . .
C18 C 0.2839(5) 0.9865(3) 0.30503(19) 0.0387(7) Uani 1 1 d . . .
H18 H 0.2113 1.0410 0.2854 0.046 Uiso 1 1 calc . . .
C19 C 0.4282(4) 0.9678(3) 0.26808(18) 0.0345(7) Uani 1 1 d . . .
H19 H 0.4559 1.0115 0.2242 0.041 Uiso 1 1 calc . . .
C20 C 0.5371(4) 0.8832(2) 0.29495(16) 0.0299(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C6 1.902(3) . ?
Br2 C17 1.894(3) . ?
O1 C1 1.367(4) . ?
O1 H1O 0.831(19) . ?
O2 C12 1.381(4) . ?
O2 H2O 0.823(19) . ?
C1 C10 1.386(4) . ?
C1 C2 1.404(5) . ?
C2 C3 1.358(5) . ?
C2 H2 0.9400 . ?
C3 C4 1.427(5) . ?
C3 H3 0.9400 . ?
C4 C5 1.415(4) . ?
C4 C9 1.418(4) . ?
C5 C6 1.355(5) . ?
C5 H5 0.9400 . ?
C6 C7 1.404(5) . ?
C7 C8 1.359(5) . ?
C7 H7 0.9400 . ?
C8 C9 1.425(4) . ?
C8 H8 0.9400 . ?
C9 C10 1.433(4) . ?
C10 C11 1.482(4) . ?
C11 C12 1.376(4) . ?
C11 C20 1.428(4) . ?
C12 C13 1.407(5) . ?
C13 C14 1.351(5) . ?
C13 H13 0.9400 . ?
C14 C15 1.424(5) . ?
C14 H14 0.9400 . ?
C15 C16 1.410(5) . ?
C15 C20 1.425(4) . ?
C16 C17 1.357(5) . ?
C16 H16 0.9400 . ?
C17 C18 1.403(5) . ?
C18 C19 1.364(5) . ?
C18 H18 0.9400 . ?
C19 C20 1.419(4) . ?
C19 H19 0.9400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1O 100(4) . . ?
C12 O2 H2O 108(3) . . ?
O1 C1 C10 116.9(3) . . ?
O1 C1 C2 121.5(3) . . ?
C10 C1 C2 121.6(3) . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 121.1(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C9 120.3(3) . . ?
C5 C4 C3 121.8(3) . . ?
C9 C4 C3 117.9(3) . . ?
C6 C5 C4 119.1(3) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C7 122.0(3) . . ?
C5 C6 Br1 120.0(3) . . ?
C7 C6 Br1 117.9(3) . . ?
C8 C7 C6 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 121.0(3) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C8 117.8(3) . . ?
C4 C9 C10 120.9(3) . . ?
C8 C9 C10 121.4(3) . . ?
C1 C10 C9 117.9(3) . . ?
C1 C10 C11 121.4(3) . . ?
C9 C10 C11 120.6(3) . . ?
C12 C11 C20 118.1(3) . . ?
C12 C11 C10 120.2(3) . . ?
C20 C11 C10 121.5(3) . . ?
C11 C12 O2 121.7(3) . . ?
C11 C12 C13 122.4(3) . . ?
O2 C12 C13 115.9(3) . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 121.0(3) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C16 C15 C14 121.6(3) . . ?
C16 C15 C20 119.7(3) . . ?
C14 C15 C20 118.6(3) . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 121.1(3) . . ?
C16 C17 Br2 120.5(2) . . ?
C18 C17 Br2 118.4(3) . . ?
C19 C18 C17 120.1(3) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 120.9(3) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C19 C20 C15 117.9(3) . . ?
C19 C20 C11 122.2(3) . . ?
C15 C20 C11 119.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.056

_database_code_depnum_ccdc_archive 'CCDC 1007143'
#######################################################################
#
#                 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_(R)-3

_vrf_PLAT057_R-3                 
;
PROBLEM: Correction for Absorption Required   RT(exp) ...       1.36       
RESPONSE:correction in a multiscan-like manner,
         see: _exptl_special_details
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H28 Br2 O6'
_chemical_formula_weight         620.32

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21

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

_cell_length_a                   9.0274(2)
_cell_length_b                   20.4427(4)
_cell_length_c                   14.5383(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.274(1)
_cell_angle_gamma                90.00
_cell_volume                     2647.89(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    26096
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      25.3

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_absorpt_coefficient_mu    3.102
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
All data sets were measured with several scans to increase the number of
redundant reflections. In our experience this method of averaging redundant
reflections replaces in a good approximation semi-empirical absorptions
methods (absorption correction programs like SORTAV lead to no better data
sets).
 
;

_diffrn_ambient_temperature      233(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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17115
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9297
_reflns_number_gt                7863
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       ?
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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)+(0.0466P)²+2.0519P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(7)
_refine_ls_number_reflns         9297
_refine_ls_number_parameters     649
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1021
_refine_ls_wR_factor_gt          0.0962
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.022
_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 0.74752(7) 0.63750(3) 0.60702(4) 0.06551(17) Uani 1 1 d . . .
Br2 Br 0.05109(8) 0.26345(3) 0.59463(5) 0.0796(2) Uani 1 1 d . . .
Br3 Br 1.19822(6) 0.58007(3) 0.64649(4) 0.06060(15) Uani 1 1 d . . .
Br4 Br 1.40584(8) 0.80987(4) 1.36491(4) 0.0816(2) Uani 1 1 d . . .
O1 O 0.3564(4) 0.48199(15) 1.0337(2) 0.0456(8) Uani 1 1 d . . .
O2 O 0.3337(4) 0.54977(15) 1.1615(2) 0.0481(8) Uani 1 1 d . . .
O3 O 0.3268(4) 0.5744(2) 1.3542(3) 0.0721(11) Uani 1 1 d . . .
O4 O 0.6617(4) 0.40874(14) 1.0296(2) 0.0467(8) Uani 1 1 d . . .
O5 O 0.7548(4) 0.33893(15) 1.1546(2) 0.0460(8) Uani 1 1 d . . .
O6 O 0.6401(4) 0.28197(18) 1.3077(2) 0.0574(9) Uani 1 1 d . . .
O7 O 0.8044(3) 0.63590(16) 1.1133(2) 0.0462(7) Uani 1 1 d . . .
O8 O 0.8324(5) 0.54457(18) 1.2108(3) 0.0695(11) Uani 1 1 d . . .
O9 O 0.8718(9) 0.4933(3) 1.3948(4) 0.131(3) Uani 1 1 d . . .
O10 O 0.7518(3) 0.75863(15) 0.9066(2) 0.0484(8) Uani 1 1 d . . .
O11 O 0.7425(5) 0.84755(18) 0.8043(3) 0.0677(11) Uani 1 1 d . . .
O12 O 0.6827(11) 0.8877(3) 0.6119(4) 0.148(3) Uani 1 1 d . . .
C1 C 0.4180(5) 0.5178(2) 0.9693(3) 0.0370(10) Uani 1 1 d . . .
C2 C 0.4247(5) 0.5868(2) 0.9720(3) 0.0428(10) Uani 1 1 d . . .
H2 H 0.3858 0.6096 1.0189 0.051 Uiso 1 1 calc . . .
C3 C 0.4870(5) 0.62062(19) 0.9070(3) 0.0409(11) Uani 1 1 d . . .
H3 H 0.4915 0.6665 0.9105 0.049 Uiso 1 1 calc . . .
C4 C 0.5444(5) 0.5885(2) 0.8353(3) 0.0387(10) Uani 1 1 d . . .
C5 C 0.6091(6) 0.6228(2) 0.7672(3) 0.0448(11) Uani 1 1 d . . .
H5 H 0.6162 0.6686 0.7703 0.054 Uiso 1 1 calc . . .
C6 C 0.6606(5) 0.5907(2) 0.6982(3) 0.0473(11) Uani 1 1 d . . .
C7 C 0.6536(6) 0.5213(2) 0.6919(3) 0.0476(12) Uani 1 1 d . . .
H7 H 0.6890 0.4993 0.6430 0.057 Uiso 1 1 calc . . .
C8 C 0.5945(5) 0.4874(2) 0.7580(3) 0.0406(10) Uani 1 1 d . . .
H8 H 0.5912 0.4415 0.7545 0.049 Uiso 1 1 calc . . .
C9 C 0.5380(5) 0.5187(2) 0.8318(3) 0.0363(10) Uani 1 1 d . . .
C10 C 0.4746(5) 0.4834(2) 0.9005(3) 0.0362(10) Uani 1 1 d . . .
C11 C 0.4708(5) 0.40975(19) 0.8997(3) 0.0352(9) Uani 1 1 d . . .
C12 C 0.5640(5) 0.3739(2) 0.9637(3) 0.0382(10) Uani 1 1 d . . .
C13 C 0.5591(5) 0.3051(2) 0.9645(3) 0.0435(11) Uani 1 1 d . . .
H13 H 0.6225 0.2815 1.0105 0.052 Uiso 1 1 calc . . .
C14 C 0.4622(6) 0.2729(2) 0.8985(3) 0.0477(12) Uani 1 1 d . . .
H14 H 0.4586 0.2269 0.8997 0.057 Uiso 1 1 calc . . .
C15 C 0.3678(5) 0.3071(2) 0.8288(3) 0.0419(10) Uani 1 1 d . . .
C16 C 0.2682(6) 0.2743(2) 0.7583(4) 0.0500(13) Uani 1 1 d . . .
H16 H 0.2644 0.2283 0.7584 0.060 Uiso 1 1 calc . . .
C17 C 0.1786(6) 0.3077(3) 0.6910(3) 0.0501(12) Uani 1 1 d . . .
C18 C 0.1792(5) 0.3763(3) 0.6908(3) 0.0493(12) Uani 1 1 d . . .
H18 H 0.1159 0.3994 0.6442 0.059 Uiso 1 1 calc . . .
C19 C 0.2723(5) 0.4096(2) 0.7588(3) 0.0444(11) Uani 1 1 d . . .
H19 H 0.2711 0.4555 0.7588 0.053 Uiso 1 1 calc . . .
C20 C 0.3700(5) 0.3762(2) 0.8289(3) 0.0376(10) Uani 1 1 d . . .
C21 C 0.2584(5) 0.5150(2) 1.0869(3) 0.0459(11) Uani 1 1 d . . .
H21A H 0.1942 0.5452 1.0458 0.055 Uiso 1 1 calc . . .
H21B H 0.1933 0.4827 1.1100 0.055 Uiso 1 1 calc . . .
C22 C 0.4047(7) 0.5099(3) 1.2364(4) 0.0621(15) Uani 1 1 d . . .
H22A H 0.4933 0.4887 1.2188 0.075 Uiso 1 1 calc . . .
H22B H 0.3352 0.4758 1.2500 0.075 Uiso 1 1 calc . . .
C23 C 0.4510(7) 0.5519(4) 1.3224(4) 0.0754(18) Uani 1 1 d . . .
H23A H 0.5123 0.5261 1.3710 0.091 Uiso 1 1 calc . . .
H23B H 0.5113 0.5890 1.3069 0.091 Uiso 1 1 calc . . .
C24 C 0.3670(12) 0.6141(4) 1.4362(5) 0.108(3) Uani 1 1 d . . .
H24A H 0.2767 0.6294 1.4576 0.161 Uiso 1 1 calc . . .
H24B H 0.4254 0.6514 1.4214 0.161 Uiso 1 1 calc . . .
H24C H 0.4262 0.5884 1.4849 0.161 Uiso 1 1 calc . . .
C25 C 0.7882(5) 0.3762(2) 1.0803(3) 0.0459(11) Uani 1 1 d . . .
H25A H 0.8317 0.3475 1.0377 0.055 Uiso 1 1 calc . . .
H25B H 0.8641 0.4089 1.1043 0.055 Uiso 1 1 calc . . .
C26 C 0.7070(6) 0.3765(2) 1.2273(4) 0.0549(13) Uani 1 1 d . . .
H26A H 0.6007 0.3878 1.2098 0.066 Uiso 1 1 calc . . .
H26B H 0.7648 0.4172 1.2361 0.066 Uiso 1 1 calc . . .
C27 C 0.7290(8) 0.3386(3) 1.3153(4) 0.0701(17) Uani 1 1 d . . .
H27A H 0.8349 0.3262 1.3313 0.084 Uiso 1 1 calc . . .
H27B H 0.7034 0.3661 1.3656 0.084 Uiso 1 1 calc . . .
C28 C 0.6459(9) 0.2495(3) 1.3934(4) 0.086(2) Uani 1 1 d . . .
H28A H 0.5797 0.2118 1.3853 0.129 Uiso 1 1 calc . . .
H28B H 0.6140 0.2791 1.4386 0.129 Uiso 1 1 calc . . .
H28C H 0.7478 0.2352 1.4155 0.129 Uiso 1 1 calc . . .
C29 C 0.8603(5) 0.6153(2) 1.0352(3) 0.0356(10) Uani 1 1 d . . .
C30 C 0.8439(5) 0.5506(2) 1.0024(4) 0.0429(11) Uani 1 1 d . . .
H30 H 0.7943 0.5195 1.0342 0.051 Uiso 1 1 calc . . .
C31 C 0.8999(5) 0.53298(19) 0.9248(3) 0.0414(11) Uani 1 1 d . . .
H31 H 0.8847 0.4901 0.9018 0.050 Uiso 1 1 calc . . .
C32 C 0.9810(4) 0.5780(2) 0.8774(3) 0.0357(9) Uani 1 1 d . . .
C33 C 1.0417(5) 0.5606(2) 0.7970(3) 0.0431(11) Uani 1 1 d . . .
H33 H 1.0284 0.5179 0.7728 0.052 Uiso 1 1 calc . . .
C34 C 1.1178(5) 0.6045(2) 0.7553(3) 0.0447(11) Uani 1 1 d . . .
C35 C 1.1388(5) 0.6698(2) 0.7879(4) 0.0440(11) Uani 1 1 d . . .
H35 H 1.1928 0.6999 0.7575 0.053 Uiso 1 1 calc . . .
C36 C 1.0795(5) 0.6877(2) 0.8635(3) 0.0395(10) Uani 1 1 d . . .
H36 H 1.0927 0.7309 0.8851 0.047 Uiso 1 1 calc . . .
C37 C 0.9981(4) 0.6435(2) 0.9117(3) 0.0346(9) Uani 1 1 d . . .
C38 C 0.9346(5) 0.66172(19) 0.9919(3) 0.0342(9) Uani 1 1 d . . .
C39 C 0.9482(5) 0.7305(2) 1.0268(3) 0.0376(10) Uani 1 1 d . . .
C40 C 0.8540(5) 0.7785(2) 0.9820(3) 0.0395(10) Uani 1 1 d . . .
C41 C 0.8606(5) 0.8434(2) 1.0144(4) 0.0436(11) Uani 1 1 d . . .
H41 H 0.7956 0.8751 0.9833 0.052 Uiso 1 1 calc . . .
C42 C 0.9612(6) 0.8601(2) 1.0907(4) 0.0506(13) Uani 1 1 d . . .
H42 H 0.9637 0.9034 1.1126 0.061 Uiso 1 1 calc . . .
C43 C 1.0620(5) 0.8137(2) 1.1376(3) 0.0434(11) Uani 1 1 d . . .
C44 C 1.1684(6) 0.8309(3) 1.2171(4) 0.0528(14) Uani 1 1 d . . .
H44 H 1.1726 0.8741 1.2396 0.063 Uiso 1 1 calc . . .
C45 C 1.2619(6) 0.7861(3) 1.2593(4) 0.0559(14) Uani 1 1 d . . .
C46 C 1.2593(6) 0.7196(3) 1.2292(4) 0.0547(13) Uani 1 1 d . . .
H46 H 1.3267 0.6887 1.2602 0.066 Uiso 1 1 calc . . .
C47 C 1.1553(6) 0.7022(2) 1.1534(3) 0.0451(11) Uani 1 1 d . . .
H47 H 1.1518 0.6585 1.1327 0.054 Uiso 1 1 calc . . .
C48 C 1.0527(5) 0.7482(2) 1.1053(3) 0.0370(10) Uani 1 1 d . . .
C49 C 0.7335(5) 0.5881(2) 1.1629(4) 0.0491(12) Uani 1 1 d . . .
H49A H 0.6791 0.6104 1.2070 0.059 Uiso 1 1 calc . . .
H49B H 0.6599 0.5640 1.1187 0.059 Uiso 1 1 calc . . .
C50 C 0.9329(12) 0.5716(4) 1.2877(6) 0.133(4) Uani 1 1 d . . .
H50A H 1.0344 0.5712 1.2719 0.159 Uiso 1 1 calc . . .
H50B H 0.9052 0.6175 1.2948 0.159 Uiso 1 1 calc . . .
C51 C 0.9370(12) 0.5422(6) 1.3688(6) 0.138(4) Uani 1 1 d . . .
H51A H 1.0437 0.5326 1.3885 0.165 Uiso 1 1 calc . . .
H51B H 0.9136 0.5772 1.4102 0.165 Uiso 1 1 calc . . .
C52 C 0.8786(11) 0.4680(4) 1.4792(5) 0.105(3) Uani 1 1 d . . .
H52A H 0.8066 0.4326 1.4772 0.157 Uiso 1 1 calc . . .
H52B H 0.8552 0.5016 1.5218 0.157 Uiso 1 1 calc . . .
H52C H 0.9789 0.4514 1.5004 0.157 Uiso 1 1 calc . . .
C53 C 0.6618(6) 0.8078(3) 0.8544(4) 0.0574(13) Uani 1 1 d . . .
H53A H 0.5815 0.7865 0.8114 0.069 Uiso 1 1 calc . . .
H53B H 0.6148 0.8348 0.8974 0.069 Uiso 1 1 calc . . .
C54 C 0.7969(11) 0.8145(4) 0.7298(5) 0.102(3) Uani 1 1 d . . .
H54A H 0.9024 0.8028 0.7500 0.122 Uiso 1 1 calc . . .
H54B H 0.7402 0.7738 0.7160 0.122 Uiso 1 1 calc . . .
C55 C 0.7853(12) 0.8514(6) 0.6493(6) 0.133(4) Uani 1 1 d . . .
H55A H 0.8749 0.8793 0.6584 0.159 Uiso 1 1 calc . . .
H55B H 0.8002 0.8201 0.6006 0.159 Uiso 1 1 calc . . .
C56 C 0.6671(11) 0.9153(4) 0.5313(5) 0.104(3) Uani 1 1 d . . .
H56A H 0.5746 0.9403 0.5213 0.156 Uiso 1 1 calc . . .
H56B H 0.6634 0.8820 0.4834 0.156 Uiso 1 1 calc . . .
H56C H 0.7514 0.9442 0.5285 0.156 Uiso 1 1 calc . . .


_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 C6 1.904(5) . ?
Br2 C17 1.894(5) . ?
Br3 C34 1.910(5) . ?
Br4 C45 1.907(5) . ?
O1 C1 1.375(5) . ?
O1 C21 1.434(5) . ?
O2 C21 1.381(6) . ?
O2 C22 1.426(6) . ?
O3 C23 1.360(7) . ?
O3 C24 1.440(8) . ?
O4 C12 1.390(6) . ?
O4 C25 1.420(6) . ?
O5 C25 1.394(6) . ?
O5 C26 1.427(6) . ?
O6 C27 1.402(7) . ?
O6 C28 1.405(7) . ?
O7 C29 1.381(5) . ?
O7 C49 1.426(5) . ?
O8 C49 1.369(6) . ?
O8 C50 1.432(8) . ?
O9 C51 1.249(10) . ?
O9 C52 1.323(9) . ?
O10 C40 1.376(6) . ?
O10 C53 1.430(6) . ?
O11 C53 1.376(7) . ?
O11 C54 1.429(7) . ?
O12 C55 1.241(10) . ?
O12 C56 1.288(9) . ?
C1 C10 1.386(6) . ?
C1 C2 1.411(6) . ?
C2 C3 1.363(7) . ?
C2 H2 0.9400 . ?
C3 C4 1.400(6) . ?
C3 H3 0.9400 . ?
C4 C5 1.413(6) . ?
C4 C9 1.431(6) . ?
C5 C6 1.343(7) . ?
C5 H5 0.9400 . ?
C6 C7 1.422(7) . ?
C7 C8 1.362(7) . ?
C7 H7 0.9400 . ?
C8 C9 1.412(6) . ?
C8 H8 0.9400 . ?
C9 C10 1.426(6) . ?
C10 C11 1.505(6) . ?
C11 C12 1.363(6) . ?
C11 C20 1.435(6) . ?
C12 C13 1.406(7) . ?
C13 C14 1.359(7) . ?
C13 H13 0.9400 . ?
C14 C15 1.401(7) . ?
C14 H14 0.9400 . ?
C15 C20 1.413(6) . ?
C15 C16 1.419(7) . ?
C16 C17 1.351(7) . ?
C16 H16 0.9400 . ?
C17 C18 1.402(8) . ?
C18 C19 1.370(7) . ?
C18 H18 0.9400 . ?
C19 C20 1.411(7) . ?
C19 H19 0.9400 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C22 C23 1.518(9) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C26 C27 1.481(8) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 H28C 0.9700 . ?
C29 C38 1.373(6) . ?
C29 C30 1.406(6) . ?
C30 C31 1.358(7) . ?
C30 H30 0.9400 . ?
C31 C32 1.421(6) . ?
C31 H31 0.9400 . ?
C32 C33 1.415(6) . ?
C32 C37 1.429(6) . ?
C33 C34 1.334(7) . ?
C33 H33 0.9400 . ?
C34 C35 1.419(7) . ?
C35 C36 1.348(7) . ?
C35 H35 0.9400 . ?
C36 C37 1.418(6) . ?
C36 H36 0.9400 . ?
C37 C38 1.428(6) . ?
C38 C39 1.492(6) . ?
C39 C40 1.391(6) . ?
C39 C48 1.406(6) . ?
C40 C41 1.405(6) . ?
C41 C42 1.359(7) . ?
C41 H41 0.9400 . ?
C42 C43 1.413(7) . ?
C42 H42 0.9400 . ?
C43 C48 1.418(6) . ?
C43 C44 1.422(7) . ?
C44 C45 1.327(8) . ?
C44 H44 0.9400 . ?
C45 C46 1.428(8) . ?
C46 C47 1.375(7) . ?
C46 H46 0.9400 . ?
C47 C48 1.422(7) . ?
C47 H47 0.9400 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C50 C51 1.318(11) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 H52C 0.9700 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C54 C55 1.383(12) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 H56C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C21 117.9(3) . . ?
C21 O2 C22 114.2(4) . . ?
C23 O3 C24 111.1(6) . . ?
C12 O4 C25 119.0(3) . . ?
C25 O5 C26 114.1(4) . . ?
C27 O6 C28 112.4(5) . . ?
C29 O7 C49 117.4(3) . . ?
C49 O8 C50 115.1(5) . . ?
C51 O9 C52 129.8(7) . . ?
C40 O10 C53 117.7(4) . . ?
C53 O11 C54 113.4(5) . . ?
C55 O12 C56 128.7(9) . . ?
O1 C1 C10 117.1(4) . . ?
O1 C1 C2 122.3(4) . . ?
C10 C1 C2 120.6(4) . . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 121.5(4) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 122.3(4) . . ?
C3 C4 C9 118.5(4) . . ?
C5 C4 C9 119.3(4) . . ?
C6 C5 C4 120.9(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 121.2(4) . . ?
C5 C6 Br1 120.4(4) . . ?
C7 C6 Br1 118.4(4) . . ?
C8 C7 C6 118.7(4) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
C7 C8 C9 122.5(4) . . ?
C7 C8 H8 118.8 . . ?
C9 C8 H8 118.8 . . ?
C8 C9 C10 122.6(4) . . ?
C8 C9 C4 117.5(4) . . ?
C10 C9 C4 119.9(4) . . ?
C1 C10 C9 119.0(4) . . ?
C1 C10 C11 120.3(4) . . ?
C9 C10 C11 120.8(4) . . ?
C12 C11 C20 118.9(4) . . ?
C12 C11 C10 121.5(4) . . ?
C20 C11 C10 119.6(4) . . ?
C11 C12 O4 116.6(4) . . ?
C11 C12 C13 121.8(4) . . ?
O4 C12 C13 121.6(4) . . ?
C14 C13 C12 119.7(4) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 121.0(4) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C14 C15 C20 119.4(4) . . ?
C14 C15 C16 121.9(4) . . ?
C20 C15 C16 118.7(4) . . ?
C17 C16 C15 121.3(4) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 120.4(4) . . ?
C16 C17 Br2 121.0(4) . . ?
C18 C17 Br2 118.6(4) . . ?
C19 C18 C17 119.8(5) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 121.4(4) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C19 C20 C15 118.4(4) . . ?
C19 C20 C11 122.5(4) . . ?
C15 C20 C11 119.1(4) . . ?
O2 C21 O1 113.5(4) . . ?
O2 C21 H21A 108.9 . . ?
O1 C21 H21A 108.9 . . ?
O2 C21 H21B 108.9 . . ?
O1 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
O2 C22 C23 109.6(4) . . ?
O2 C22 H22A 109.7 . . ?
C23 C22 H22A 109.7 . . ?
O2 C22 H22B 109.7 . . ?
C23 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
O3 C23 C22 109.8(5) . . ?
O3 C23 H23A 109.7 . . ?
C22 C23 H23A 109.7 . . ?
O3 C23 H23B 109.7 . . ?
C22 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O5 C25 O4 113.7(4) . . ?
O5 C25 H25A 108.8 . . ?
O4 C25 H25A 108.8 . . ?
O5 C25 H25B 108.8 . . ?
O4 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
O5 C26 C27 110.1(4) . . ?
O5 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
O5 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.2 . . ?
O6 C27 C26 111.6(5) . . ?
O6 C27 H27A 109.3 . . ?
C26 C27 H27A 109.3 . . ?
O6 C27 H27B 109.3 . . ?
C26 C27 H27B 109.3 . . ?
H27A C27 H27B 108.0 . . ?
O6 C28 H28A 109.5 . . ?
O6 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O6 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C38 C29 O7 115.9(4) . . ?
C38 C29 C30 121.8(4) . . ?
O7 C29 C30 122.3(4) . . ?
C31 C30 C29 119.9(4) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 121.4(4) . . ?
C30 C31 H31 119.3 . . ?
C32 C31 H31 119.3 . . ?
C33 C32 C31 122.4(4) . . ?
C33 C32 C37 119.3(4) . . ?
C31 C32 C37 118.2(4) . . ?
C34 C33 C32 120.2(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 122.1(4) . . ?
C33 C34 Br3 119.5(4) . . ?
C35 C34 Br3 118.3(4) . . ?
C36 C35 C34 118.6(4) . . ?
C36 C35 H35 120.7 . . ?
C34 C35 H35 120.7 . . ?
C35 C36 C37 122.4(4) . . ?
C35 C36 H36 118.8 . . ?
C37 C36 H36 118.8 . . ?
C36 C37 C38 123.1(4) . . ?
C36 C37 C32 117.3(4) . . ?
C38 C37 C32 119.6(4) . . ?
C29 C38 C37 119.0(4) . . ?
C29 C38 C39 121.0(4) . . ?
C37 C38 C39 120.0(4) . . ?
C40 C39 C48 118.5(4) . . ?
C40 C39 C38 119.7(4) . . ?
C48 C39 C38 121.8(4) . . ?
O10 C40 C39 116.4(4) . . ?
O10 C40 C41 122.2(4) . . ?
C39 C40 C41 121.4(4) . . ?
C42 C41 C40 119.8(4) . . ?
C42 C41 H41 120.1 . . ?
C40 C41 H41 120.1 . . ?
C41 C42 C43 121.3(4) . . ?
C41 C42 H42 119.4 . . ?
C43 C42 H42 119.4 . . ?
C42 C43 C48 118.4(4) . . ?
C42 C43 C44 121.6(4) . . ?
C48 C43 C44 120.0(5) . . ?
C45 C44 C43 120.1(5) . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
C44 C45 C46 122.5(5) . . ?
C44 C45 Br4 119.8(4) . . ?
C46 C45 Br4 117.7(4) . . ?
C47 C46 C45 117.9(5) . . ?
C47 C46 H46 121.0 . . ?
C45 C46 H46 121.0 . . ?
C46 C47 C48 121.9(5) . . ?
C46 C47 H47 119.0 . . ?
C48 C47 H47 119.0 . . ?
C39 C48 C43 120.6(4) . . ?
C39 C48 C47 121.8(4) . . ?
C43 C48 C47 117.5(4) . . ?
O8 C49 O7 113.2(4) . . ?
O8 C49 H49A 108.9 . . ?
O7 C49 H49A 108.9 . . ?
O8 C49 H49B 108.9 . . ?
O7 C49 H49B 108.9 . . ?
H49A C49 H49B 107.8 . . ?
C51 C50 O8 116.4(6) . . ?
C51 C50 H50A 108.2 . . ?
O8 C50 H50A 108.2 . . ?
C51 C50 H50B 108.2 . . ?
O8 C50 H50B 108.2 . . ?
H50A C50 H50B 107.3 . . ?
O9 C51 C50 133.6(8) . . ?
O9 C51 H51A 103.8 . . ?
C50 C51 H51A 103.8 . . ?
O9 C51 H51B 103.8 . . ?
C50 C51 H51B 103.8 . . ?
H51A C51 H51B 105.4 . . ?
O9 C52 H52A 109.5 . . ?
O9 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
O9 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O11 C53 O10 113.1(4) . . ?
O11 C53 H53A 109.0 . . ?
O10 C53 H53A 109.0 . . ?
O11 C53 H53B 109.0 . . ?
O10 C53 H53B 109.0 . . ?
H53A C53 H53B 107.8 . . ?
C55 C54 O11 113.2(6) . . ?
C55 C54 H54A 108.9 . . ?
O11 C54 H54A 108.9 . . ?
C55 C54 H54B 108.9 . . ?
O11 C54 H54B 108.9 . . ?
H54A C54 H54B 107.7 . . ?
O12 C55 C54 130.3(8) . . ?
O12 C55 H55A 104.7 . . ?
C54 C55 H55A 104.7 . . ?
O12 C55 H55B 104.7 . . ?
C54 C55 H55B 104.7 . . ?
H55A C55 H55B 105.7 . . ?
O12 C56 H56A 109.5 . . ?
O12 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
O12 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.058

_database_code_depnum_ccdc_archive 'CCDC 1007144'
#######################################################################
#
#                 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:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_(RS)-2

_vrf_PLAT057_RS-2                
;
PROBLEM: Correction for Absorption Required   RT(exp) ...       1.36       
RESPONSE:correction in a multiscan-like manner,
         see: _exptl_special_details
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H12 Br2 O2'
_chemical_formula_weight         444.12

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   9.9622(3)
_cell_length_b                   8.3317(2)
_cell_length_c                   19.9628(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.208(1)
_cell_angle_gamma                90.00
_cell_volume                     1639.98(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    10750
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      26.0

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    4.952
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
All data sets were measured with several scans to increase the number of
redundant reflections. In our experience this method of averaging redundant
reflections replaces in a good approximation semi-empirical absorptions
methods (absorption correction programs like SORTAV lead to no better data
sets).
 
;

_diffrn_ambient_temperature      233(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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10154
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3215
_reflns_number_gt                2781
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       ?
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Hydrogen at O1 and O2 could be localized and were refined isotropically
 with bond restraints (d=0.83 angs.).
;

_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)+(0.0354P)²+1.1082P] 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         3215
_refine_ls_number_parameters     225
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0724
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.10924(3) 0.24936(3) 0.065072(18) 0.04927(12) Uani 1 1 d . . .
Br2 Br -0.48007(3) 1.34473(4) -0.078092(15) 0.04155(11) Uani 1 1 d . . .
O1 O -0.0121(2) 1.1369(2) 0.22752(12) 0.0470(5) Uani 1 1 d D . .
H1O H -0.093(2) 1.156(5) 0.216(2) 0.077(14) Uiso 1 1 d D . .
O2 O -0.2524(2) 0.8291(2) 0.27256(10) 0.0362(4) Uani 1 1 d D . .
H2O H -0.176(2) 0.793(4) 0.2714(18) 0.056(11) Uiso 1 1 d D . .
C1 C 0.0162(3) 0.9909(3) 0.20221(13) 0.0314(6) Uani 1 1 d . . .
C2 C 0.1550(3) 0.9506(3) 0.20984(14) 0.0360(6) Uani 1 1 d . . .
H2 H 0.2198 1.0232 0.2311 0.043 Uiso 1 1 calc . . .
C3 C 0.1959(2) 0.8088(3) 0.18683(13) 0.0308(6) Uani 1 1 d . . .
H3 H 0.2887 0.7834 0.1925 0.037 Uiso 1 1 calc . . .
C4 C 0.1001(3) 0.6983(3) 0.15433(12) 0.0270(5) Uani 1 1 d . . .
C5 C 0.1413(2) 0.5499(3) 0.12962(13) 0.0307(6) Uani 1 1 d . . .
H5 H 0.2339 0.5230 0.1348 0.037 Uiso 1 1 calc . . .
C6 C 0.0475(3) 0.4460(3) 0.09837(14) 0.0341(6) Uani 1 1 d . . .
C7 C -0.0914(3) 0.4818(3) 0.09016(15) 0.0394(7) Uani 1 1 d . . .
H7 H -0.1550 0.4080 0.0688 0.047 Uiso 1 1 calc . . .
C8 C -0.1337(3) 0.6251(3) 0.11352(14) 0.0329(6) Uani 1 1 d . . .
H8 H -0.2268 0.6491 0.1078 0.039 Uiso 1 1 calc . . .
C9 C -0.0403(2) 0.7374(3) 0.14591(12) 0.0250(5) Uani 1 1 d . . .
C10 C -0.0820(2) 0.8885(3) 0.17093(12) 0.0255(5) Uani 1 1 d . . .
C11 C -0.2271(2) 0.9406(3) 0.16357(12) 0.0242(5) Uani 1 1 d . . .
C12 C -0.3019(2) 0.9163(3) 0.21578(12) 0.0275(5) Uani 1 1 d . . .
C13 C -0.4334(3) 0.9814(3) 0.21478(13) 0.0302(6) Uani 1 1 d . . .
H13 H -0.4817 0.9626 0.2511 0.036 Uiso 1 1 calc . . .
C14 C -0.4895(2) 1.0709(3) 0.16132(14) 0.0312(6) Uani 1 1 d . . .
H14 H -0.5760 1.1158 0.1614 0.037 Uiso 1 1 calc . . .
C15 C -0.4192(2) 1.0979(3) 0.10516(13) 0.0265(5) Uani 1 1 d . . .
C16 C -0.4763(2) 1.1921(3) 0.04915(13) 0.0297(5) Uani 1 1 d . . .
H16 H -0.5622 1.2391 0.0486 0.036 Uiso 1 1 calc . . .
C17 C -0.4059(3) 1.2141(3) -0.00389(13) 0.0300(6) Uani 1 1 d . . .
C18 C -0.2780(3) 1.1429(3) -0.00522(13) 0.0311(6) Uani 1 1 d . . .
H18 H -0.2326 1.1565 -0.0430 0.037 Uiso 1 1 calc . . .
C19 C -0.2208(2) 1.0539(3) 0.04886(13) 0.0290(5) Uani 1 1 d . . .
H19 H -0.1350 1.0077 0.0482 0.035 Uiso 1 1 calc . . .
C20 C -0.2882(2) 1.0298(3) 0.10588(12) 0.0245(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C6 1.903(3) . ?
Br2 C17 1.901(3) . ?
O1 C1 1.362(3) . ?
O1 H1O 0.820(19) . ?
O2 C12 1.377(3) . ?
O2 H2O 0.817(18) . ?
C1 C10 1.379(4) . ?
C1 C2 1.410(4) . ?
C2 C3 1.352(4) . ?
C2 H2 0.9400 . ?
C3 C4 1.415(4) . ?
C3 H3 0.9400 . ?
C4 C5 1.414(4) . ?
C4 C9 1.423(3) . ?
C5 C6 1.359(4) . ?
C5 H5 0.9400 . ?
C6 C7 1.402(4) . ?
C7 C8 1.370(4) . ?
C7 H7 0.9400 . ?
C8 C9 1.410(4) . ?
C8 H8 0.9400 . ?
C9 C10 1.437(3) . ?
C10 C11 1.496(3) . ?
C11 C12 1.379(3) . ?
C11 C20 1.431(3) . ?
C12 C13 1.415(4) . ?
C13 C14 1.355(4) . ?
C13 H13 0.9400 . ?
C14 C15 1.422(4) . ?
C14 H14 0.9400 . ?
C15 C16 1.417(4) . ?
C15 C20 1.421(3) . ?
C16 C17 1.363(4) . ?
C16 H16 0.9400 . ?
C17 C18 1.409(4) . ?
C18 C19 1.365(4) . ?
C18 H18 0.9400 . ?
C19 C20 1.416(3) . ?
C19 H19 0.9400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1O 109(3) . . ?
C12 O2 H2O 113(3) . . ?
O1 C1 C10 123.3(2) . . ?
O1 C1 C2 115.1(2) . . ?
C10 C1 C2 121.6(2) . . ?
C3 C2 C1 120.6(2) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.6(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 121.2(2) . . ?
C5 C4 C9 119.3(2) . . ?
C3 C4 C9 119.5(2) . . ?
C6 C5 C4 120.1(2) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 121.4(2) . . ?
C5 C6 Br1 118.2(2) . . ?
C7 C6 Br1 120.3(2) . . ?
C8 C7 C6 119.4(2) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 121.3(2) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C8 C9 C4 118.4(2) . . ?
C8 C9 C10 122.4(2) . . ?
C4 C9 C10 119.2(2) . . ?
C1 C10 C9 118.5(2) . . ?
C1 C10 C11 118.5(2) . . ?
C9 C10 C11 122.9(2) . . ?
C12 C11 C20 118.1(2) . . ?
C12 C11 C10 120.1(2) . . ?
C20 C11 C10 121.6(2) . . ?
O2 C12 C11 122.1(2) . . ?
O2 C12 C13 115.8(2) . . ?
C11 C12 C13 122.1(2) . . ?
C14 C13 C12 119.9(2) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.9(2) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C16 C15 C20 119.6(2) . . ?
C16 C15 C14 121.5(2) . . ?
C20 C15 C14 118.9(2) . . ?
C17 C16 C15 119.6(2) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 121.6(2) . . ?
C16 C17 Br2 119.76(19) . . ?
C18 C17 Br2 118.59(19) . . ?
C19 C18 C17 119.4(2) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 121.4(2) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C19 C20 C15 118.4(2) . . ?
C19 C20 C11 121.6(2) . . ?
C15 C20 C11 120.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.073

_database_code_depnum_ccdc_archive 'CCDC 1007145'
#######################################################################
#
#                 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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#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_(RS)-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H28 Br2 O6'
_chemical_formula_weight         620.32

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.8523(3)
_cell_length_b                   10.1793(3)
_cell_length_c                   13.9220(3)
_cell_angle_alpha                70.723(2)
_cell_angle_beta                 89.926(2)
_cell_angle_gamma                82.549(2)
_cell_volume                     1305.53(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    13819
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      26.0

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             628
_exptl_absorpt_coefficient_mu    3.146
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      233(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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7962
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4588
_reflns_number_gt                3713
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       ?
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 The crystal structure shows splitting of bromine positions by positional and
 occupational disorders. The major bromine position Br1 at C6 with occupancy
 of 0.96 and Br2 at C17 with 0.93 comes generally from the main compound.
 Br1A at C5 with occupancy of 0.04 and Br2A at C16 with 0.03 from impurities
 of an isomeric compound.
 Within the cell, the Br1A position has a distance of 2.71 angs. to O3 of a
 neighboring molecule. This distance is too close and the alkoxy chain
 C23-O3-C24 of the neighboring molecule will be moved to the new position of
 C23A-O3A-C24A with an occupancy of 0.04 for each atom and Br1A-O3A distance
 of 3.15 angs.. This sterical repulsion leads also to a small twist of the
 Br1A-isomer, which can not be exactly observed or solved as disorder at the
 carbon atoms, but can be seen as a further position Br2B (with a distance of
 0.6 angs. to Br2 and an occupation factor of 0.04).
 Because of the possible disorder of the carbon framework could not by solved,
 we have an averged framework, which will be dominated by the major carbon
 positions. Therefore the Br1A-C and the Br2A-C distance of around 1.62 angs.
 is too short.
 For hydrogen calculations at disordered position C5=C5A,C6=C6A,C16=C16A,
 C17=C17A and C22=C22A were used with equal coordinates and displacement
 parameters.
 The positons C23A, C24A, O3A and Br2B were refined with isotropic
 displacement parameters.
;

_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)+(0.0287P)²+0.6581P] 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     SHELXL
_refine_ls_extinction_coef       0.0087(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4588
_refine_ls_number_parameters     360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
O1 O 0.34548(19) 1.1272(2) -0.47244(13) 0.0560(5) Uani 1 1 d . . .
O2 O 0.2986(2) 1.2856(2) -0.63909(14) 0.0586(5) Uani 1 1 d . . .
O4 O 0.14199(19) 0.88699(19) -0.41232(14) 0.0539(5) Uani 1 1 d . . .
O5 O 0.1908(2) 0.72383(19) -0.49887(14) 0.0546(5) Uani 1 1 d . . .
O6 O 0.4437(2) 0.6648(3) -0.59520(18) 0.0765(6) Uani 1 1 d . . .
C1 C 0.2518(3) 1.1808(3) -0.41719(19) 0.0457(6) Uani 1 1 d . . .
C2 C 0.1968(3) 1.3238(3) -0.4447(2) 0.0534(7) Uani 1 1 d . . .
H2 H 0.2237 1.3887 -0.5047 0.064 Uiso 1 1 calc . . .
C3 C 0.1055(3) 1.3683(3) -0.3853(2) 0.0522(7) Uani 1 1 d . . .
H3 H 0.0729 1.4647 -0.4033 0.063 Uiso 1 1 calc . . .
C4 C 0.0581(3) 1.2736(3) -0.2969(2) 0.0460(6) Uani 1 1 d . . .
C7 C -0.0433(3) 1.0766(3) -0.1300(2) 0.0543(7) Uani 1 1 d . . .
H7 H -0.0800 1.0111 -0.0752 0.065 Uiso 1 1 calc . A 1
C8 C 0.0559(3) 1.0321(3) -0.18498(19) 0.0488(6) Uani 1 1 d . C .
H8 H 0.0889 0.9357 -0.1662 0.059 Uiso 1 1 calc . . .
C9 C 0.1106(3) 1.1282(3) -0.27019(18) 0.0424(6) Uani 1 1 d . C .
C10 C 0.2117(3) 1.0836(3) -0.32994(18) 0.0411(6) Uani 1 1 d . . .
C11 C 0.2772(2) 0.9342(3) -0.29391(18) 0.0405(6) Uani 1 1 d . . .
C12 C 0.2371(3) 0.8366(3) -0.33212(19) 0.0449(6) Uani 1 1 d . . .
C13 C 0.2911(3) 0.6930(3) -0.2893(2) 0.0529(7) Uani 1 1 d . . .
H13 H 0.2627 0.6272 -0.3163 0.063 Uiso 1 1 calc . . .
C14 C 0.3844(3) 0.6496(3) -0.2091(2) 0.0506(7) Uani 1 1 d . . .
H14 H 0.4170 0.5534 -0.1799 0.061 Uiso 1 1 calc . . .
C15 C 0.4329(3) 0.7459(3) -0.16885(18) 0.0437(6) Uani 1 1 d . D .
C18 C 0.5368(3) 0.9463(3) -0.1017(2) 0.0517(7) Uani 1 1 d . . .
H18 H 0.5747 1.0130 -0.0806 0.062 Uiso 1 1 calc . B 1
C19 C 0.4365(3) 0.9881(3) -0.17789(19) 0.0476(6) Uani 1 1 d . . .
H19 H 0.4036 1.0843 -0.2070 0.057 Uiso 1 1 calc . . .
C20 C 0.3810(2) 0.8912(3) -0.21401(18) 0.0412(6) Uani 1 1 d . . .
C21 C 0.3981(3) 1.2225(3) -0.5600(2) 0.0616(8) Uani 1 1 d . . .
H21A H 0.4343 1.2958 -0.5404 0.074 Uiso 1 1 calc . . .
H21B H 0.4741 1.1716 -0.5844 0.074 Uiso 1 1 calc . . .
C25 C 0.0906(3) 0.7908(3) -0.4531(2) 0.0540(7) Uani 1 1 d . . .
H25A H 0.0520 0.7194 -0.3982 0.065 Uiso 1 1 calc . . .
H25B H 0.0164 0.8415 -0.5037 0.065 Uiso 1 1 calc . . .
C26 C 0.2452(3) 0.8177(3) -0.5857(2) 0.0617(8) Uani 1 1 d . . .
H26A H 0.3066 0.8717 -0.5637 0.074 Uiso 1 1 calc . . .
H26B H 0.1703 0.8840 -0.6285 0.074 Uiso 1 1 calc . . .
C27 C 0.3222(3) 0.7374(4) -0.6460(2) 0.0705(9) Uani 1 1 d . . .
H27A H 0.2658 0.6711 -0.6576 0.085 Uiso 1 1 calc . . .
H27B H 0.3416 0.8026 -0.7125 0.085 Uiso 1 1 calc . . .
C28 C 0.5154(4) 0.5852(4) -0.6506(3) 0.0833(11) Uani 1 1 d . . .
H28A H 0.6005 0.5358 -0.6137 0.125 Uiso 1 1 calc . . .
H28B H 0.5354 0.6477 -0.7170 0.125 Uiso 1 1 calc . . .
H28C H 0.4594 0.5179 -0.6591 0.125 Uiso 1 1 calc . . .
Br1 Br -0.22928(4) 1.27564(4) -0.07594(3) 0.07919(16) Uani 0.96 1 d P C 1
Br2 Br 0.71926(4) 0.74549(6) 0.05142(3) 0.06663(15) Uani 0.93 1 d P D 1
C5 C -0.0418(3) 1.3175(3) -0.2358(2) 0.0555(7) Uani 0.96 1 d P C 1
H5 H -0.0742 1.4134 -0.2509 0.067 Uiso 0.96 1 calc P E 1
C6 C -0.0900(3) 1.2196(3) -0.1553(2) 0.0569(7) Uani 0.96 1 d P C 1
C16 C 0.5330(3) 0.7044(3) -0.08730(19) 0.0504(7) Uani 0.97 1 d P D 1
H16 H 0.5655 0.6087 -0.0552 0.061 Uiso 0.97 1 calc P F 1
C17 C 0.5818(3) 0.8024(3) -0.05576(19) 0.0527(7) Uani 0.97 1 d P D 1
O3 O 0.0479(2) 1.3379(2) -0.76677(15) 0.0632(6) Uani 0.96 1 d P G 1
C22 C 0.2506(3) 1.1903(3) -0.6808(2) 0.0596(8) Uani 0.96 1 d P G 1
H22A H 0.1891 1.1346 -0.6339 0.071 Uiso 0.96 1 calc P H 1
H22B H 0.3281 1.1260 -0.6907 0.071 Uiso 0.96 1 calc P I 1
C23 C 0.1758(3) 1.2699(4) -0.7808(2) 0.0627(8) Uani 0.96 1 d P G 1
H23A H 0.2309 1.3397 -0.8223 0.075 Uiso 0.96 1 calc P J 1
H23B H 0.1627 1.2050 -0.8175 0.075 Uiso 0.96 1 calc P K 1
C24 C -0.0227(4) 1.4101(4) -0.8624(3) 0.0837(11) Uani 0.96 1 d P G 1
H24A H -0.1118 1.4549 -0.8516 0.125 Uiso 0.96 1 calc P L 1
H24B H -0.0346 1.3437 -0.8972 0.125 Uiso 0.96 1 calc P M 1
H24C H 0.0300 1.4809 -0.9035 0.125 Uiso 0.96 1 calc P N 1
Br1A Br -0.1089(9) 1.4799(7) -0.2610(6) 0.0615(19) Uani 0.04 1 d P C 2
Br2A Br 0.6108(10) 0.5484(9) -0.0277(8) 0.059(3) Uani 0.03 1 d P . 2
C5A C -0.0418(3) 1.3175(3) -0.2358(2) 0.0555(7) Uani 0.04 1 d P C 2
C6A C -0.0900(3) 1.2196(3) -0.1553(2) 0.0569(7) Uani 0.04 1 d P C 2
H6A H -0.1567 1.2494 -0.1158 0.068 Uiso 0.04 1 calc P O 2
C16A C 0.5330(3) 0.7044(3) -0.08730(19) 0.0504(7) Uani 0.03 1 d P D 2
C17A C 0.5818(3) 0.8024(3) -0.05576(19) 0.0527(7) Uani 0.03 1 d P D 2
H17A H 0.6477 0.7732 -0.0015 0.063 Uiso 0.03 1 calc P P 2
O3A O 0.052(4) 1.240(4) -0.772(3) 0.026(8) Uiso 0.04 1 d P G 2
C22A C 0.2506(3) 1.1903(3) -0.6808(2) 0.0596(8) Uani 0.04 1 d P G 2
H22C H 0.1802 1.1543 -0.6332 0.071 Uiso 0.04 1 calc P Q 2
H22D H 0.3276 1.1141 -0.6626 0.071 Uiso 0.04 1 calc P R 2
C23A C 0.196(6) 1.178(7) -0.774(4) 0.033(13) Uiso 0.04 1 d P G 2
H23C H 0.2028 1.0793 -0.7708 0.040 Uiso 0.04 1 calc P S 2
H23D H 0.2417 1.2311 -0.8341 0.040 Uiso 0.04 1 calc P T 2
C24A C 0.004(9) 1.299(9) -0.894(7) 0.07(2) Uiso 0.04 1 d P G 2
H24D H -0.0907 1.3438 -0.9022 0.110 Uiso 0.04 1 calc P U 2
H24E H 0.0110 1.2209 -0.9200 0.110 Uiso 0.04 1 calc P V 2
H24F H 0.0619 1.3666 -0.9317 0.110 Uiso 0.04 1 calc P W 2
Br2B Br 0.7366(9) 0.8027(9) 0.0318(7) 0.041(2) Uiso 0.04 1 d P X 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.373(3) . ?
O1 C21 1.429(3) . ?
O2 C21 1.400(3) . ?
O2 C22 1.412(4) . ?
O4 C12 1.374(3) . ?
O4 C25 1.427(3) . ?
O5 C25 1.398(3) . ?
O5 C26 1.425(4) . ?
O6 C27 1.381(4) . ?
O6 C28 1.419(4) . ?
C1 C10 1.384(4) . ?
C1 C2 1.409(4) . ?
C2 C3 1.357(4) . ?
C2 H2 0.9400 . ?
C3 C4 1.411(4) . ?
C3 H3 0.9400 . ?
C4 C5 1.423(4) . ?
C4 C9 1.427(4) . ?
C7 C8 1.363(4) . ?
C7 C6 1.394(4) . ?
C7 H7 0.9400 . ?
C8 C9 1.423(4) . ?
C8 H8 0.9400 . ?
C9 C10 1.421(3) . ?
C10 C11 1.491(3) . ?
C11 C12 1.370(4) . ?
C11 C20 1.428(3) . ?
C12 C13 1.414(4) . ?
C13 C14 1.364(4) . ?
C13 H13 0.9400 . ?
C14 C15 1.410(4) . ?
C14 H14 0.9400 . ?
C15 C16 1.421(4) . ?
C15 C20 1.426(3) . ?
C18 C19 1.371(4) . ?
C18 C17 1.402(4) . ?
C18 H18 0.9400 . ?
C19 C20 1.412(4) . ?
C19 H19 0.9400 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C26 C27 1.496(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 H28C 0.9700 . ?
Br1 C6 1.907(3) . ?
Br2 C17 1.904(3) . ?
C5 C6 1.364(4) . ?
C5 H5 0.9400 . ?
C16 C17 1.354(4) . ?
C16 H16 0.9400 . ?
O3 C23 1.403(4) . ?
O3 C24 1.421(4) . ?
C22 C23 1.497(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
Br2A Br2A 2.53(2) 2_665 ?
O3A C23A 1.48(7) . ?
O3A C24A 1.65(9) . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C24A H24D 0.9700 . ?
C24A H24E 0.9700 . ?
C24A H24F 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C21 118.5(2) . . ?
C21 O2 C22 113.7(2) . . ?
C12 O4 C25 119.3(2) . . ?
C25 O5 C26 113.4(2) . . ?
C27 O6 C28 111.1(3) . . ?
O1 C1 C10 115.4(2) . . ?
O1 C1 C2 124.2(2) . . ?
C10 C1 C2 120.4(2) . . ?
C3 C2 C1 120.4(2) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 121.7(2) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 122.5(2) . . ?
C3 C4 C9 118.1(2) . . ?
C5 C4 C9 119.3(3) . . ?
C8 C7 C6 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 121.4(2) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C10 C9 C8 122.3(2) . . ?
C10 C9 C4 119.8(2) . . ?
C8 C9 C4 117.9(2) . . ?
C1 C10 C9 119.5(2) . . ?
C1 C10 C11 121.6(2) . . ?
C9 C10 C11 118.9(2) . . ?
C12 C11 C20 119.3(2) . . ?
C12 C11 C10 122.1(2) . . ?
C20 C11 C10 118.5(2) . . ?
C11 C12 O4 116.1(2) . . ?
C11 C12 C13 120.8(2) . . ?
O4 C12 C13 123.1(2) . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 121.4(2) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C14 C15 C16 122.7(2) . . ?
C14 C15 C20 118.2(2) . . ?
C16 C15 C20 119.1(2) . . ?
C19 C18 C17 118.8(3) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C20 122.0(2) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 H19 119.0 . . ?
C19 C20 C15 117.9(2) . . ?
C19 C20 C11 122.3(2) . . ?
C15 C20 C11 119.8(2) . . ?
O2 C21 O1 112.5(2) . . ?
O2 C21 H21A 109.1 . . ?
O1 C21 H21A 109.1 . . ?
O2 C21 H21B 109.1 . . ?
O1 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
O5 C25 O4 113.1(2) . . ?
O5 C25 H25A 109.0 . . ?
O4 C25 H25A 109.0 . . ?
O5 C25 H25B 109.0 . . ?
O4 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
O5 C26 C27 110.2(3) . . ?
O5 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
O5 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
O6 C27 C26 110.8(2) . . ?
O6 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
O6 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
O6 C28 H28A 109.5 . . ?
O6 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O6 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 121.8(3) . . ?
C5 C6 Br1 120.2(2) . . ?
C7 C6 Br1 117.9(2) . . ?
C17 C16 C15 120.2(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 121.9(2) . . ?
C16 C17 Br2 119.7(2) . . ?
C18 C17 Br2 118.5(2) . . ?
C23 O3 C24 110.2(3) . . ?
O2 C22 C23 109.5(3) . . ?
O2 C22 H22A 109.8 . . ?
C23 C22 H22A 109.8 . . ?
O2 C22 H22B 109.8 . . ?
C23 C22 H22B 109.8 . . ?
H22A C22 H22B 108.2 . . ?
O3 C23 C22 111.1(2) . . ?
O3 C23 H23A 109.4 . . ?
C22 C23 H23A 109.4 . . ?
O3 C23 H23B 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23A O3A C24A 102(4) . . ?
O3A C23A H23C 111.9 . . ?
O3A C23A H23D 111.9 . . ?
H23C C23A H23D 109.6 . . ?
O3A C24A H24D 109.5 . . ?
O3A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
O3A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.047

_database_code_depnum_ccdc_archive 'CCDC 1007146'
#######################################################################
#
#                 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_(RS)-4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H24 Br2 O6'
_chemical_formula_weight         616.29

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.8364(2)
_cell_length_b                   10.5814(3)
_cell_length_c                   14.7993(3)
_cell_angle_alpha                108.781(1)
_cell_angle_beta                 94.787(1)
_cell_angle_gamma                97.419(1)
_cell_volume                     1287.54(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    12921
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      27.0

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             620
_exptl_absorpt_coefficient_mu    3.189
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      233(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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8475
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5044
_reflns_number_gt                4026
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       ?
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 The crystal shows splitting of bromine positions by a positional and
 occupational disorders. The major bromine position Br1 at C6 with occupancy
 of 0.90 and Br2 at C17 with 0.88 comes general from the main compound.
 Br1A at C5 with occupancy of 0.04 and Br2A at C16 with 0.06 from impuritiy
 of an isomeric compound.
 Within the cell, the Br2A position has a distance of 2.62 (and 2.67) angs. to
 Br1 (and Br1A) of a neighboring molecule. This distance is to close and the
 neighboring molecule will be twisted. Therefore positional disorder around
 Br1 and Br2 (twisting) occurs by additional position Br1B and Br2B, each
 occupied with 0.06. The Br1A position shows also a short distance to the
 position Br2B wit 2.74 angs., but because of 4% and 6% distribution of these
 positions this plays no further role.
 Because only 6% of neighboring molecules are twisted, this disorder can not
 observed at the carbon atoms (low movement and anistropic displacement
 parameters look normal).
 For hydrogen calculations at disordered position C5=C5A,C6=C6A,C16=C16A and
 C17=C17A were used with equal coordinates and displacement parameters.
;

_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)+(0.0251P)²+0.8015P] 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     SHELXL
_refine_ls_extinction_coef       0.0070(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5044
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0815
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
O1 O 1.1483(2) 0.69342(18) 0.30488(14) 0.0526(5) Uani 1 1 d . . .
O2 O 1.2833(2) 0.5030(2) 0.44469(14) 0.0633(6) Uani 1 1 d . . .
O3 O 1.1247(2) 0.6548(2) 0.47981(15) 0.0628(5) Uani 1 1 d . . .
O4 O 0.8416(2) 0.90677(18) 0.39678(13) 0.0523(5) Uani 1 1 d . C .
O5 O 0.5894(2) 0.9855(2) 0.33913(14) 0.0677(6) Uani 1 1 d . . .
O6 O 0.5730(2) 1.1291(2) 0.48507(14) 0.0622(5) Uani 1 1 d . . .
C1 C 1.0009(3) 0.6261(2) 0.26809(17) 0.0424(6) Uani 1 1 d . C .
C2 C 0.9546(3) 0.4878(3) 0.25406(19) 0.0495(6) Uani 1 1 d . . .
H2 H 1.0252 0.4380 0.2721 0.059 Uiso 1 1 calc . . .
C3 C 0.8085(3) 0.4262(3) 0.21464(19) 0.0512(7) Uani 1 1 d . C .
H3 H 0.7794 0.3338 0.2055 0.061 Uiso 1 1 calc . . .
C4 C 0.6996(3) 0.4972(3) 0.18712(17) 0.0448(6) Uani 1 1 d . . .
C7 C 0.4886(3) 0.6458(3) 0.13478(19) 0.0541(7) Uani 1 1 d . . .
H7 H 0.4167 0.6949 0.1174 0.065 Uiso 1 1 calc . A 1
C8 C 0.6358(3) 0.7088(3) 0.17409(18) 0.0481(6) Uani 1 1 d . C .
H8 H 0.6641 0.8012 0.1829 0.058 Uiso 1 1 calc . . .
C9 C 0.7462(3) 0.6380(2) 0.20172(16) 0.0406(5) Uani 1 1 d . C .
C10 C 0.9001(3) 0.7011(2) 0.24249(16) 0.0399(5) Uani 1 1 d . . .
C11 C 0.9518(3) 0.8464(2) 0.25456(17) 0.0383(5) Uani 1 1 d . C .
C12 C 0.9171(3) 0.9477(2) 0.33103(17) 0.0424(6) Uani 1 1 d . . .
C13 C 0.9590(3) 1.0856(3) 0.3407(2) 0.0511(7) Uani 1 1 d . C .
H13 H 0.9348 1.1539 0.3935 0.061 Uiso 1 1 calc . . .
C14 C 1.0346(3) 1.1184(3) 0.2729(2) 0.0548(7) Uani 1 1 d . . .
H14 H 1.0620 1.2102 0.2797 0.066 Uiso 1 1 calc . . .
C15 C 1.0730(3) 1.0190(3) 0.19302(19) 0.0458(6) Uani 1 1 d . . .
C18 C 1.1515(3) 0.8161(3) 0.03738(19) 0.0564(7) Uani 1 1 d . . .
H18 H 1.1798 0.7487 -0.0144 0.068 Uiso 1 1 calc . B 1
C19 C 1.0765(3) 0.7818(3) 0.10478(18) 0.0479(6) Uani 1 1 d . C .
H19 H 1.0525 0.6900 0.0985 0.058 Uiso 1 1 calc . . .
C20 C 1.0332(3) 0.8810(2) 0.18465(17) 0.0406(5) Uani 1 1 d . . .
C21 C 1.2534(3) 0.6228(3) 0.33883(18) 0.0480(6) Uani 1 1 d . . .
H21A H 1.3573 0.6755 0.3521 0.058 Uiso 1 1 calc . . .
H21B H 1.2542 0.5358 0.2887 0.058 Uiso 1 1 calc . . .
C22 C 1.2111(3) 0.5981(3) 0.42917(19) 0.0477(6) Uani 1 1 d . . .
C23 C 1.2589(5) 0.4733(4) 0.5331(2) 0.0827(11) Uani 1 1 d . . .
H23A H 1.3154 0.5473 0.5891 0.099 Uiso 1 1 calc . . .
H23B H 1.1492 0.4652 0.5403 0.099 Uiso 1 1 calc . . .
C24 C 1.3118(5) 0.3499(4) 0.5285(3) 0.0919(12) Uani 1 1 d . . .
H24A H 1.2959 0.3303 0.5870 0.138 Uiso 1 1 calc . . .
H24B H 1.4206 0.3587 0.5220 0.138 Uiso 1 1 calc . . .
H24C H 1.2548 0.2768 0.4735 0.138 Uiso 1 1 calc . . .
C25 C 0.7779(3) 1.0023(3) 0.4686(2) 0.0530(7) Uani 1 1 d . . .
H25A H 0.8569 1.0824 0.4996 0.064 Uiso 1 1 calc . . .
H25B H 0.7519 0.9627 0.5179 0.064 Uiso 1 1 calc . . .
C26 C 0.6367(3) 1.0468(3) 0.4329(2) 0.0508(7) Uani 1 1 d . C .
C27 C 0.4568(4) 1.0290(4) 0.2983(2) 0.0739(10) Uani 1 1 d . . .
H27A H 0.3796 1.0414 0.3428 0.089 Uiso 1 1 calc . . .
H27B H 0.4099 0.9587 0.2375 0.089 Uiso 1 1 calc . . .
C28 C 0.5047(5) 1.1583(5) 0.2805(3) 0.0966(13) Uani 1 1 d . . .
H28A H 0.4156 1.1849 0.2531 0.145 Uiso 1 1 calc . . .
H28B H 0.5806 1.1459 0.2361 0.145 Uiso 1 1 calc . . .
H28C H 0.5490 1.2284 0.3409 0.145 Uiso 1 1 calc . . .
C5 C 0.5461(3) 0.4350(3) 0.14538(19) 0.0524(7) Uani 0.96 1 d P C 1
H5 H 0.5145 0.3425 0.1350 0.063 Uiso 0.96 1 calc P D 1
C6 C 0.4454(3) 0.5077(3) 0.12049(18) 0.0526(7) Uani 0.96 1 d P C 1
C16 C 1.1487(3) 1.0522(3) 0.1206(2) 0.0555(7) Uani 0.94 1 d P . 1
H16 H 1.1728 1.1431 0.1245 0.067 Uiso 0.94 1 calc P E 1
C17 C 1.1863(3) 0.9527(3) 0.0457(2) 0.0556(7) Uani 0.94 1 d P . 1
Br1 Br 0.24030(5) 0.42169(5) 0.06682(3) 0.06125(14) Uani 0.90 1 d P C 1
Br2 Br 1.28733(9) 0.99546(7) -0.05170(5) 0.0722(2) Uani 0.88 1 d P . 1
C5A C 0.5461(3) 0.4350(3) 0.14538(19) 0.0524(7) Uani 0.04 1 d P . 2
C6A C 0.4454(3) 0.5077(3) 0.12049(18) 0.0526(7) Uani 0.04 1 d P . 2
H6A H 0.3443 0.4650 0.0930 0.063 Uiso 0.04 1 calc P F 2
C16A C 1.1487(3) 1.0522(3) 0.1206(2) 0.0555(7) Uani 0.06 1 d P . 2
C17A C 1.1863(3) 0.9527(3) 0.0457(2) 0.0556(7) Uani 0.06 1 d P . 2
H17A H 1.2367 0.9760 -0.0015 0.067 Uiso 0.06 1 calc P G 2
Br1A Br 0.4789(14) 0.2725(10) 0.1051(11) 0.113(4) Uani 0.04 1 d P . 2
Br2A Br 1.1812(7) 1.2079(6) 0.1189(5) 0.0740(15) Uani 0.06 1 d P . 2
Br1B Br 0.2439(6) 0.4809(5) 0.0497(4) 0.0358(11) Uani 0.06 1 d P H 3
Br2B Br 1.2951(11) 1.0507(6) -0.0260(5) 0.0383(15) Uani 0.06 1 d P I 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.375(3) . ?
O1 C21 1.420(3) . ?
O2 C22 1.327(3) . ?
O2 C23 1.467(4) . ?
O3 C22 1.196(3) . ?
O4 C12 1.373(3) . ?
O4 C25 1.423(3) . ?
O5 C26 1.332(3) . ?
O5 C27 1.466(4) . ?
O6 C26 1.199(3) . ?
C1 C10 1.373(4) . ?
C1 C2 1.411(4) . ?
C2 C3 1.358(4) . ?
C2 H2 0.9400 . ?
C3 C4 1.405(4) . ?
C3 H3 0.9400 . ?
C4 C5 1.422(4) . ?
C4 C9 1.433(4) . ?
C7 C8 1.369(4) . ?
C7 C6 1.403(4) . ?
C7 H7 0.9400 . ?
C8 C9 1.414(4) . ?
C8 H8 0.9400 . ?
C9 C10 1.425(3) . ?
C10 C11 1.495(3) . ?
C11 C12 1.373(3) . ?
C11 C20 1.422(3) . ?
C12 C13 1.415(4) . ?
C13 C14 1.360(4) . ?
C13 H13 0.9400 . ?
C14 C15 1.407(4) . ?
C14 H14 0.9400 . ?
C15 C20 1.420(4) . ?
C15 C16 1.421(4) . ?
C18 C19 1.359(4) . ?
C18 C17 1.401(4) . ?
C18 H18 0.9400 . ?
C19 C20 1.423(3) . ?
C19 H19 0.9400 . ?
C21 C22 1.509(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C23 C24 1.426(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 C26 1.503(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C27 C28 1.490(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 H28C 0.9700 . ?
C5 C6 1.351(4) . ?
C5 H5 0.9400 . ?
C6 Br1 1.901(3) . ?
C16 C17 1.359(4) . ?
C16 H16 0.9400 . ?
C17 Br2 1.900(3) . ?
Br1A Br2A 2.673(14) 1_445 ?
Br2A Br1A 2.673(14) 1_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C21 117.78(19) . . ?
C22 O2 C23 116.2(2) . . ?
C12 O4 C25 119.6(2) . . ?
C26 O5 C27 116.7(2) . . ?
C10 C1 O1 115.9(2) . . ?
C10 C1 C2 121.0(2) . . ?
O1 C1 C2 123.1(2) . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 121.6(2) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 122.6(2) . . ?
C3 C4 C9 118.3(2) . . ?
C5 C4 C9 119.0(2) . . ?
C8 C7 C6 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 121.4(2) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C8 C9 C10 122.5(2) . . ?
C8 C9 C4 118.0(2) . . ?
C10 C9 C4 119.5(2) . . ?
C1 C10 C9 119.3(2) . . ?
C1 C10 C11 120.6(2) . . ?
C9 C10 C11 120.1(2) . . ?
C12 C11 C20 119.3(2) . . ?
C12 C11 C10 120.7(2) . . ?
C20 C11 C10 120.0(2) . . ?
O4 C12 C11 116.0(2) . . ?
O4 C12 C13 122.8(2) . . ?
C11 C12 C13 121.2(2) . . ?
C14 C13 C12 119.5(2) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 121.8(2) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C14 C15 C20 118.4(2) . . ?
C14 C15 C16 122.3(2) . . ?
C20 C15 C16 119.3(2) . . ?
C19 C18 C17 119.4(3) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 121.9(3) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 H19 119.0 . . ?
C15 C20 C11 119.8(2) . . ?
C15 C20 C19 117.7(2) . . ?
C11 C20 C19 122.5(2) . . ?
O1 C21 C22 111.7(2) . . ?
O1 C21 H21A 109.3 . . ?
C22 C21 H21A 109.3 . . ?
O1 C21 H21B 109.3 . . ?
C22 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
O3 C22 O2 124.3(3) . . ?
O3 C22 C21 125.5(3) . . ?
O2 C22 C21 110.2(2) . . ?
C24 C23 O2 109.4(3) . . ?
C24 C23 H23A 109.8 . . ?
O2 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
O2 C23 H23B 109.8 . . ?
H23A C23 H23B 108.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O4 C25 C26 115.2(2) . . ?
O4 C25 H25A 108.5 . . ?
C26 C25 H25A 108.5 . . ?
O4 C25 H25B 108.5 . . ?
C26 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
O6 C26 O5 123.9(3) . . ?
O6 C26 C25 122.4(3) . . ?
O5 C26 C25 113.8(2) . . ?
O5 C27 C28 110.8(3) . . ?
O5 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
O5 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C6 C5 C4 120.5(3) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 121.3(3) . . ?
C5 C6 Br1 119.2(2) . . ?
C7 C6 Br1 119.4(2) . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 121.5(3) . . ?
C16 C17 Br2 120.6(2) . . ?
C18 C17 Br2 117.9(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.049


_database_code_depnum_ccdc_archive 'CCDC 1007147'
