# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 1145/230

data_dart40

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C33 H29 Br6 N5 O3'
_chemical_formula_weight          1023.07

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'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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                    10.2450(16)
_cell_length_b                    12.6915(19)
_cell_length_c                    13.557(2)
_cell_angle_alpha                 80.371(3)
_cell_angle_beta                  87.000(3)
_cell_angle_gamma                 85.967(3)
_cell_volume                      1732.2(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     8484
_cell_measurement_theta_min       2.99
_cell_measurement_theta_max       25.42

_exptl_crystal_description        needle
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.01
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.962
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              992
_exptl_absorpt_coefficient_mu     6.996
_exptl_absorpt_correction_type    multiscans
_exptl_absorpt_correction_T_min   0.4873
_exptl_absorpt_correction_T_max   0.9333
_exptl_absorpt_process_details    ?

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.68840
_diffrn_radiation_type            synchrotron
_diffrn_radiation_source          'Station 9.8, Daresbury SRS'
_diffrn_radiation_monochromator   'Silicon 111'
_diffrn_measurement_device_type   'Siemens SMART CCD diffractometer'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         15
_diffrn_reflns_number             13879
_diffrn_reflns_av_R_equivalents   0.0580
_diffrn_reflns_av_sigmaI/netI     0.0947
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          1.93
_diffrn_reflns_theta_max          25.00
_reflns_number_total              6668
_reflns_number_gt                 4471
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Bruker SMART'
_computing_cell_refinement        'local programs'
_computing_data_reduction         'Bruker SHELXTL'
_computing_structure_solution     'Bruker SHELXTL'
_computing_structure_refinement   'Bruker SHELXTL'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'SHELXTL and local programs'

_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0703P)^2^+4.6588P] where P=(Fo^2^+2Fc^2^)/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          6668
_refine_ls_number_parameters      424
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1077
_refine_ls_R_factor_gt            0.0654
_refine_ls_wR_factor_ref          0.1581
_refine_ls_wR_factor_gt           0.1457
_refine_ls_goodness_of_fit_ref    1.037
_refine_ls_restrained_S_all       1.037
_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
C1 C 0.2924(8) 0.0106(6) 1.0280(6) 0.0248(17) Uani 1 1 d . . .
C2 C 0.1945(8) -0.0397(6) 0.9868(6) 0.0234(17) Uani 1 1 d . . .
C3 C 0.1404(7) 0.0039(6) 0.8941(5) 0.0215(16) Uani 1 1 d . . .
C4 C 0.1886(8) 0.1014(6) 0.8419(5) 0.0228(17) Uani 1 1 d . . .
C5 C 0.2840(8) 0.1534(6) 0.8813(6) 0.0219(16) Uani 1 1 d . . .
C6 C 0.3362(8) 0.1073(6) 0.9732(6) 0.0226(17) Uani 1 1 d . . .
C1A C 0.2402(8) -0.1376(6) 1.1330(6) 0.0232(17) Uani 1 1 d . . .
C2A C 0.2402(8) -0.2179(6) 1.2196(6) 0.0270(18) Uani 1 1 d . . .
H2A H 0.1837 -0.2752 1.2272 0.032 Uiso 1 1 calc R . .
C3A C 0.3256(8) -0.2087(7) 1.2919(5) 0.0281(19) Uani 1 1 d . . .
C4A C 0.4099(9) -0.1272(7) 1.2813(6) 0.031(2) Uani 1 1 d . . .
C5A C 0.4108(8) -0.0483(7) 1.1964(6) 0.0254(18) Uani 1 1 d . . .
H5A H 0.4689 0.0079 1.1893 0.031 Uiso 1 1 calc R . .
C6A C 0.3235(8) -0.0546(6) 1.1223(5) 0.0236(17) Uani 1 1 d . . .
C1B C 0.0411(7) 0.0529(6) 0.7449(6) 0.0206(16) Uani 1 1 d . . .
C2B C -0.0351(8) 0.0434(7) 0.6667(6) 0.0269(18) Uani 1 1 d . . .
H2B H -0.0336 0.0946 0.6070 0.032 Uiso 1 1 calc R . .
C3B C -0.1144(8) -0.0424(6) 0.6769(6) 0.0240(17) Uani 1 1 d . . .
C4B C -0.1156(8) -0.1151(6) 0.7645(6) 0.0253(17) Uani 1 1 d . . .
C5B C -0.0387(8) -0.1099(6) 0.8416(6) 0.0239(17) Uani 1 1 d . . .
H5B H -0.0417 -0.1623 0.9004 0.029 Uiso 1 1 calc R . .
C6B C 0.0453(8) -0.0257(6) 0.8334(6) 0.0248(17) Uani 1 1 d . . .
C1C C 0.4393(7) 0.2582(6) 0.9216(5) 0.0196(16) Uani 1 1 d . . .
C2C C 0.5186(8) 0.3415(6) 0.9153(6) 0.0278(18) Uani 1 1 d . . .
H2C H 0.5787 0.3448 0.9656 0.033 Uiso 1 1 calc R . .
C3C C 0.5072(8) 0.4209(7) 0.8321(6) 0.0306(19) Uani 1 1 d . . .
C4C C 0.4199(8) 0.4156(6) 0.7580(6) 0.0262(18) Uani 1 1 d . . .
C5C C 0.3407(8) 0.3310(6) 0.7645(6) 0.0237(17) Uani 1 1 d . . .
H5C H 0.2805 0.3279 0.7143 0.028 Uiso 1 1 calc R . .
C6C C 0.3523(7) 0.2495(6) 0.8485(6) 0.0233(17) Uani 1 1 d . . .
N2 N 0.1636(6) -0.1291(5) 1.0530(5) 0.0224(14) Uani 1 1 d . . .
H2 H 0.1042 -0.1734 1.0450 0.027 Uiso 1 1 calc R . .
Br3A Br 0.32244(10) -0.31490(8) 1.40835(6) 0.0413(3) Uani 1 1 d . . .
Br4A Br 0.53580(10) -0.12049(8) 1.37672(7) 0.0427(3) Uani 1 1 d . . .
Br3B Br -0.21588(9) -0.05315(8) 0.56694(7) 0.0377(2) Uani 1 1 d . . .
Br4B Br -0.23218(10) -0.22796(7) 0.78150(7) 0.0394(3) Uani 1 1 d . . .
Br3C Br 0.61704(13) 0.53623(9) 0.82128(9) 0.0613(4) Uani 1 1 d . . .
Br4C Br 0.40272(10) 0.52565(7) 0.64501(7) 0.0414(3) Uani 1 1 d . . .
N4 N 0.1281(6) 0.1275(5) 0.7527(5) 0.0246(15) Uani 1 1 d . . .
H4 H 0.1431 0.1839 0.7072 0.030 Uiso 1 1 calc R . .
N6 N 0.4279(7) 0.1712(5) 0.9966(5) 0.0248(15) Uani 1 1 d . . .
H6 H 0.4730 0.1586 1.0513 0.030 Uiso 1 1 calc R . .
C50 C 0.8011(15) 0.2103(14) 1.3337(14) 0.100(5) Uani 1 1 d . . .
H50A H 0.7864 0.2056 1.4062 0.149 Uiso 1 1 calc R . .
H50B H 0.8313 0.2810 1.3052 0.149 Uiso 1 1 calc R . .
H50C H 0.8677 0.1548 1.3198 0.149 Uiso 1 1 calc R . .
C51 C 0.5696(16) 0.1769(12) 1.3534(12) 0.089(5) Uani 1 1 d . . .
H51A H 0.5901 0.1774 1.4231 0.133 Uiso 1 1 calc R . .
H51B H 0.5378 0.1073 1.3474 0.133 Uiso 1 1 calc R . .
H51C H 0.5017 0.2335 1.3327 0.133 Uiso 1 1 calc R . .
N52 N 0.6843(12) 0.1952(10) 1.2908(10) 0.081(4) Uani 1 1 d . . .
C53 C 0.6718(13) 0.1962(11) 1.2021(12) 0.072(4) Uani 1 1 d . . .
H53 H 0.7511 0.2083 1.1635 0.086 Uiso 1 1 calc R . .
O54 O 0.5873(9) 0.1859(8) 1.1551(7) 0.071(2) Uani 1 1 d . . .
O60 O 0.1098(8) 0.3074(7) 0.5925(6) 0.064(2) Uani 1 1 d . . .
C61 C 0.1355(10) 0.3465(9) 0.5049(7) 0.049(3) Uani 1 1 d . . .
C62 C 0.2735(12) 0.3555(10) 0.4656(9) 0.059(3) Uani 1 1 d . . .
H62A H 0.3332 0.3314 0.5202 0.089 Uiso 1 1 calc R . .
H62B H 0.2875 0.4302 0.4371 0.089 Uiso 1 1 calc R . .
H62C H 0.2908 0.3107 0.4134 0.089 Uiso 1 1 calc R . .
C63 C 0.0314(16) 0.3762(19) 0.4336(10) 0.123(8) Uani 1 1 d . . .
H63A H -0.0540 0.3663 0.4688 0.184 Uiso 1 1 calc R . .
H63B H 0.0419 0.3308 0.3816 0.184 Uiso 1 1 calc R . .
H63C H 0.0366 0.4514 0.4027 0.184 Uiso 1 1 calc R . .
O70 O 0.0007(8) -0.3066(6) 1.0579(6) 0.060(2) Uani 1 1 d . . .
C71 C -0.0799(15) -0.3671(12) 1.0524(14) 0.093(6) Uani 1 1 d . . .
H71 H -0.1413 -0.3364 1.0039 0.112 Uiso 1 1 calc R . .
N72 N -0.1077(13) -0.4556(9) 1.0895(11) 0.092(5) Uani 1 1 d . . .
C73 C -0.0240(16) -0.4908(16) 1.1827(10) 0.106(6) Uani 1 1 d . . .
H73A H -0.0449 -0.5630 1.2148 0.159 Uiso 1 1 calc R . .
H73B H -0.0432 -0.4408 1.2301 0.159 Uiso 1 1 calc R . .
H73C H 0.0692 -0.4907 1.1621 0.159 Uiso 1 1 calc R . .
C74 C -0.2080(16) -0.5211(14) 1.0719(14) 0.098(5) Uani 1 1 d . . .
H74A H -0.2011 -0.5891 1.1184 0.147 Uiso 1 1 calc R . .
H74B H -0.1985 -0.5351 1.0029 0.147 Uiso 1 1 calc R . .
H74C H -0.2938 -0.4844 1.0824 0.147 Uiso 1 1 calc R . .

loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
C1 0.025(4) 0.027(4) 0.019(4) -0.003(3) 0.010(3) 0.007(3)
C2 0.031(4) 0.022(4) 0.016(4) -0.002(3) -0.001(3) 0.004(3)
C3 0.021(4) 0.027(4) 0.016(4) -0.004(3) 0.003(3) 0.003(3)
C4 0.029(4) 0.023(4) 0.014(4) -0.004(3) 0.004(3) 0.005(3)
C5 0.024(4) 0.023(4) 0.019(4) -0.005(3) 0.005(3) -0.005(3)
C6 0.024(4) 0.025(4) 0.016(4) -0.003(3) 0.007(3) 0.006(3)
C1A 0.025(4) 0.025(4) 0.016(4) 0.001(3) 0.007(3) 0.006(3)
C2A 0.036(5) 0.022(4) 0.019(4) 0.002(3) 0.011(3) 0.002(4)
C3A 0.030(5) 0.041(5) 0.010(4) -0.003(3) 0.006(3) 0.012(4)
C4A 0.038(5) 0.040(5) 0.014(4) -0.007(4) 0.000(3) 0.011(4)
C5A 0.024(4) 0.029(4) 0.021(4) -0.005(3) 0.003(3) 0.009(4)
C6A 0.033(5) 0.020(4) 0.015(4) -0.001(3) 0.008(3) 0.013(3)
C1B 0.018(4) 0.022(4) 0.020(4) -0.002(3) 0.002(3) 0.005(3)
C2B 0.026(4) 0.030(4) 0.021(4) -0.001(3) 0.006(3) 0.008(4)
C3B 0.028(4) 0.029(4) 0.016(4) -0.006(3) 0.001(3) -0.001(3)
C4B 0.020(4) 0.028(4) 0.030(4) -0.013(3) 0.013(3) -0.004(3)
C5B 0.028(4) 0.013(4) 0.030(4) -0.004(3) 0.011(3) -0.004(3)
C6B 0.031(4) 0.023(4) 0.018(4) -0.005(3) 0.011(3) 0.006(3)
C1C 0.020(4) 0.025(4) 0.013(4) -0.006(3) 0.005(3) 0.001(3)
C2C 0.028(4) 0.027(4) 0.029(4) -0.009(4) 0.003(3) 0.000(4)
C3C 0.033(5) 0.030(4) 0.033(5) -0.011(4) -0.004(4) -0.010(4)
C4C 0.037(5) 0.020(4) 0.019(4) 0.004(3) 0.004(3) -0.004(3)
C5C 0.025(4) 0.024(4) 0.024(4) -0.008(3) -0.001(3) 0.000(3)
C6C 0.023(4) 0.021(4) 0.026(4) -0.006(3) 0.004(3) 0.002(3)
N2 0.029(4) 0.017(3) 0.020(3) 0.001(3) 0.000(3) 0.000(3)
Br3A 0.0556(6) 0.0402(5) 0.0216(5) 0.0086(4) 0.0010(4) 0.0070(4)
Br4A 0.0508(6) 0.0461(6) 0.0302(5) -0.0048(4) -0.0109(4) 0.0080(5)
Br3B 0.0427(5) 0.0451(5) 0.0270(5) -0.0089(4) -0.0061(4) -0.0052(4)
Br4B 0.0485(6) 0.0375(5) 0.0339(5) -0.0057(4) -0.0004(4) -0.0153(4)
Br3C 0.0805(8) 0.0471(6) 0.0576(7) 0.0069(5) -0.0197(6) -0.0371(6)
Br4C 0.0574(6) 0.0269(5) 0.0371(5) 0.0045(4) -0.0026(4) -0.0070(4)
N4 0.028(4) 0.028(4) 0.015(3) 0.003(3) -0.002(3) 0.003(3)
N6 0.031(4) 0.031(4) 0.011(3) -0.002(3) 0.003(3) 0.004(3)
C50 0.081(11) 0.110(13) 0.121(14) -0.062(11) -0.023(10) 0.020(9)
C51 0.112(13) 0.076(10) 0.081(10) -0.018(8) 0.020(9) -0.035(9)
N52 0.073(8) 0.087(8) 0.097(10) -0.060(7) -0.002(7) 0.004(6)
C53 0.056(8) 0.079(9) 0.089(11) -0.048(8) -0.023(8) 0.029(7)
O54 0.068(6) 0.090(7) 0.062(6) -0.038(5) -0.012(5) 0.000(5)
O60 0.075(5) 0.065(5) 0.045(5) 0.018(4) -0.009(4) -0.011(4)
C61 0.049(6) 0.074(7) 0.017(5) 0.016(5) -0.002(4) -0.014(5)
C62 0.076(8) 0.059(7) 0.047(6) -0.016(5) 0.008(6) -0.020(6)
C63 0.095(12) 0.23(2) 0.031(7) -0.008(10) -0.014(7) 0.038(13)
O70 0.064(5) 0.041(4) 0.073(6) -0.012(4) 0.016(4) -0.007(4)
C71 0.079(10) 0.056(9) 0.150(15) -0.050(9) 0.072(10) -0.015(8)
N72 0.094(9) 0.055(7) 0.133(12) -0.047(7) 0.065(8) -0.023(7)
C73 0.093(11) 0.159(16) 0.042(8) 0.047(9) -0.021(7) 0.018(11)
C74 0.090(11) 0.093(12) 0.113(14) -0.026(10) 0.010(10) -0.010(10)

_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 1.412(12) . ?
C1 C6 1.413(11) . ?
C1 C6A 1.439(11) . ?
C2 N2 1.368(10) . ?
C2 C3 1.411(11) . ?
C3 C6B 1.416(11) . ?
C3 C4 1.425(11) . ?
C4 N4 1.368(10) . ?
C4 C5 1.393(11) . ?
C5 C6 1.401(11) . ?
C5 C6C 1.443(11) . ?
C6 N6 1.365(11) . ?
C1A N2 1.357(10) . ?
C1A C6A 1.387(12) . ?
C1A C2A 1.421(11) . ?
C2A C3A 1.372(12) . ?
C3A C4A 1.379(13) . ?
C3A Br3A 1.897(8) . ?
C4A C5A 1.393(11) . ?
C4A Br4A 1.890(8) . ?
C5A C6A 1.395(11) . ?
C1B N4 1.366(10) . ?
C1B C2B 1.374(11) . ?
C1B C6B 1.427(11) . ?
C2B C3B 1.389(12) . ?
C3B C4B 1.376(11) . ?
C3B Br3B 1.890(8) . ?
C4B C5B 1.355(12) . ?
C4B Br4B 1.906(8) . ?
C5B C6B 1.405(11) . ?
C1C C2C 1.367(11) . ?
C1C N6 1.377(10) . ?
C1C C6C 1.390(11) . ?
C2C C3C 1.385(12) . ?
C3C C4C 1.393(11) . ?
C3C Br3C 1.890(8) . ?
C4C C5C 1.379(11) . ?
C4C Br4C 1.899(8) . ?
C5C C6C 1.408(11) . ?
C50 N52 1.396(18) . ?
C51 N52 1.423(18) . ?
N52 C53 1.213(17) . ?
C53 O54 1.129(14) . ?
O60 C61 1.231(11) . ?
C61 C63 1.465(17) . ?
C61 C62 1.490(15) . ?
O70 C71 1.179(16) . ?
C71 N72 1.199(18) . ?
N72 C74 1.42(2) . ?
N72 C73 1.55(2) . ?

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 C6 118.0(7) . . ?
C2 C1 C6A 107.1(7) . . ?
C6 C1 C6A 134.9(8) . . ?
N2 C2 C3 129.6(7) . . ?
N2 C2 C1 108.3(7) . . ?
C3 C2 C1 122.0(7) . . ?
C2 C3 C6B 135.8(8) . . ?
C2 C3 C4 117.7(7) . . ?
C6B C3 C4 106.5(7) . . ?
N4 C4 C5 129.9(7) . . ?
N4 C4 C3 108.5(7) . . ?
C5 C4 C3 121.6(7) . . ?
C4 C5 C6 119.2(7) . . ?
C4 C5 C6C 135.1(7) . . ?
C6 C5 C6C 105.7(7) . . ?
N6 C6 C5 109.0(7) . . ?
N6 C6 C1 129.4(7) . . ?
C5 C6 C1 121.6(7) . . ?
N2 C1A C6A 111.4(7) . . ?
N2 C1A C2A 127.4(7) . . ?
C6A C1A C2A 121.2(7) . . ?
C3A C2A C1A 116.8(8) . . ?
C2A C3A C4A 122.3(7) . . ?
C2A C3A Br3A 116.4(7) . . ?
C4A C3A Br3A 121.3(6) . . ?
C3A C4A C5A 121.2(8) . . ?
C3A C4A Br4A 122.1(6) . . ?
C5A C4A Br4A 116.6(7) . . ?
C4A C5A C6A 117.8(8) . . ?
C1A C6A C5A 120.7(7) . . ?
C1A C6A C1 104.8(7) . . ?
C5A C6A C1 134.5(8) . . ?
N4 C1B C2B 130.0(7) . . ?
N4 C1B C6B 108.2(7) . . ?
C2B C1B C6B 121.7(7) . . ?
C1B C2B C3B 118.7(7) . . ?
C4B C3B C2B 119.6(7) . . ?
C4B C3B Br3B 123.2(6) . . ?
C2B C3B Br3B 117.2(6) . . ?
C5B C4B C3B 123.2(7) . . ?
C5B C4B Br4B 117.3(6) . . ?
C3B C4B Br4B 119.6(6) . . ?
C4B C5B C6B 119.0(7) . . ?
C5B C6B C3 135.4(8) . . ?
C5B C6B C1B 117.7(7) . . ?
C3 C6B C1B 106.9(7) . . ?
C2C C1C N6 128.9(7) . . ?
C2C C1C C6C 123.2(7) . . ?
N6 C1C C6C 107.9(7) . . ?
C1C C2C C3C 116.8(8) . . ?
C2C C3C C4C 121.5(7) . . ?
C2C C3C Br3C 117.5(6) . . ?
C4C C3C Br3C 120.9(6) . . ?
C5C C4C C3C 121.3(7) . . ?
C5C C4C Br4C 117.2(6) . . ?
C3C C4C Br4C 121.4(6) . . ?
C4C C5C C6C 117.5(7) . . ?
C1C C6C C5C 119.6(7) . . ?
C1C C6C C5 107.6(7) . . ?
C5C C6C C5 132.7(7) . . ?
C1A N2 C2 108.3(6) . . ?
C1B N4 C4 109.8(6) . . ?
C6 N6 C1C 109.7(6) . . ?
C53 N52 C50 124.8(15) . . ?
C53 N52 C51 115.9(13) . . ?
C50 N52 C51 119.2(14) . . ?
O54 C53 N52 134.4(16) . . ?
O60 C61 C63 120.8(11) . . ?
O60 C61 C62 121.3(10) . . ?
C63 C61 C62 117.7(10) . . ?
O70 C71 N72 139(2) . . ?
C71 N72 C74 132.7(19) . . ?
C71 N72 C73 107.7(16) . . ?
C74 N72 C73 119.0(14) . . ?

_diffrn_measured_fraction_theta_max    0.990
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.990
_refine_diff_density_max    1.168
_refine_diff_density_min   -0.881
_refine_diff_density_rms    0.156

#===END

data_nrbrcn 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C56 H41 Br6 N11 O4 S4' 
_chemical_formula_weight          1539.70 
loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0181   0.0091 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0311   0.0180 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Br'  'Br'  -0.6763   1.2805 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0492   0.0322 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'S'  'S'   0.3331   0.5567 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
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                    14.455(3) 
_cell_length_b                    25.371(5) 
_cell_length_c                    16.719(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.24(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      6122(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     220(2) 
_cell_measurement_reflns_used     55 
_cell_measurement_theta_min       5 
_cell_measurement_theta_max       90 
_exptl_crystal_description        Needle 
_exptl_crystal_colour             Red 
_exptl_crystal_size_max           0.74 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.671 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3040 
_exptl_absorpt_coefficient_mu     6.460 
_exptl_absorpt_correction_type    'Optimised numerical'
_exptl_absorpt_correction_T_min   0.0871 
_exptl_absorpt_correction_T_max   0.5186 
_exptl_absorpt_process_details    ? 
_exptl_special_details 
; 
? 
; 
_diffrn_ambient_temperature       220(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        Omega-theta 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             8438 
_diffrn_reflns_av_R_equivalents   0.0906 
_diffrn_reflns_av_sigmaI/netI     0.1215 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -8 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -6 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.17 
_diffrn_reflns_theta_max          52.58 
_reflns_number_total              6965 
_reflns_number_gt                 2916 
_reflns_threshold_expression      >2sigma(I) 
_computing_data_collection        'Stoe DIF4' 
_computing_cell_refinement        'Stoe DIF4' 
_computing_data_reduction         'Stoe REDU4'  
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     SHELXTL 
_computing_publication_material   ? 
_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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/[\s^2^(Fo^2^)+(0.1227P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     Riding 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          6965 
_refine_ls_number_parameters      704 
_refine_ls_number_restraints      69 
_refine_ls_R_factor_all           0.1807 
_refine_ls_R_factor_gt            0.0868 
_refine_ls_wR_factor_ref          0.2476 
_refine_ls_wR_factor_gt           0.2021 
_refine_ls_goodness_of_fit_ref    0.955 
_refine_ls_restrained_S_all       0.962 
_refine_ls_shift/su_max           0.013 
_refine_ls_shift/su_mean          0.001 
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 -0.7056(9) 0.4832(5) 0.8555(9) 0.051(4) Uani 1 1 d . . . 
C2 C -0.7393(10) 0.5184(7) 0.9140(11) 0.065(4) Uani 1 1 d . . . 
C3 C -0.7510(9) 0.5023(6) 0.9926(10) 0.057(4) Uani 1 1 d . . . 
C4 C -0.7244(10) 0.4524(8) 1.0172(12) 0.078(5) Uani 1 1 d . . . 
C5 C -0.6891(10) 0.4142(7) 0.9618(9) 0.066(5) Uani 1 1 d . . . 
C6 C -0.6814(9) 0.4305(6) 0.8831(10) 0.061(4) Uani 1 1 d . . . 
N2 N -0.7573(8) 0.5647(5) 0.8752(8) 0.066(3) Uani 1 1 d . . . 
H2A H -0.7806 0.5921 0.8967 0.080 Uiso 1 1 calc R . . 
C1A C -0.7335(10) 0.5619(6) 0.7970(10) 0.060(4) Uani 1 1 d . . . 
C2A C -0.7360(10) 0.5995(6) 0.7400(12) 0.073(5) Uani 1 1 d . . . 
H2AA H -0.7574 0.6331 0.7515 0.088 Uiso 1 1 calc R . . 
C3A C -0.7071(12) 0.5884(9) 0.6653(12) 0.098(6) Uani 1 1 d . . . 
C4A C -0.6770(11) 0.5360(8) 0.6490(11) 0.081(5) Uani 1 1 d . . . 
C5A C -0.6718(11) 0.4969(6) 0.7097(10) 0.074(5) Uani 1 1 d . . . 
H5AA H -0.6474 0.4636 0.7010 0.088 Uiso 1 1 calc R . . 
C6A C -0.7036(9) 0.5104(6) 0.7791(9) 0.053(4) Uani 1 1 d . . . 
N4 N -0.7383(8) 0.4464(5) 1.0958(9) 0.071(4) Uani 1 1 d . . . 
H4A H -0.7288 0.4173 1.1213 0.085 Uiso 1 1 calc R . . 
C1B C -0.7693(10) 0.4917(7) 1.1310(11) 0.066(5) Uani 1 1 d . . . 
C2B C -0.7926(10) 0.5053(8) 1.2072(11) 0.077(5) Uani 1 1 d . . . 
H2BA H -0.7890 0.4810 1.2490 0.092 Uiso 1 1 calc R . . 
C3B C -0.8208(12) 0.5554(8) 1.2182(11) 0.081(5) Uani 1 1 d . . . 
C4B C -0.8370(11) 0.5924(7) 1.1560(14) 0.085(6) Uani 1 1 d . . . 
C5B C -0.8120(11) 0.5790(7) 1.0805(10) 0.076(5) Uani 1 1 d . . . 
H5BA H -0.8160 0.6039 1.0396 0.091 Uiso 1 1 calc R . . 
C6B C -0.7801(9) 0.5275(7) 1.0649(11) 0.066(5) Uani 1 1 d . . . 
N6 N -0.6467(8) 0.3909(6) 0.8390(8) 0.072(4) Uani 1 1 d . . . 
H6A H -0.6351 0.3928 0.7892 0.087 Uiso 1 1 calc R . . 
C1C C -0.6326(12) 0.3455(8) 0.8888(10) 0.076(5) Uani 1 1 d . . . 
C2C C -0.5979(10) 0.2971(7) 0.8685(13) 0.082(5) Uani 1 1 d . . . 
H2CA H -0.5821 0.2893 0.8166 0.098 Uiso 1 1 calc R . . 
C3C C -0.5883(11) 0.2613(7) 0.9288(15) 0.088(6) Uani 1 1 d . . . 
C4C C -0.6188(10) 0.2724(6) 1.0065(13) 0.079(5) Uani 1 1 d . . . 
C5C C -0.6512(10) 0.3224(7) 1.0295(11) 0.076(5) Uani 1 1 d . . . 
H5CA H -0.6656 0.3307 1.0815 0.091 Uiso 1 1 calc R . . 
C6C C -0.6593(10) 0.3588(6) 0.9648(12) 0.069(5) Uani 1 1 d . . . 
Br3A Br -0.71033(18) 0.64055(9) 0.58516(15) 0.1295(10) Uani 1 1 d . . . 
Br4A Br -0.63141(19) 0.51892(10) 0.54759(14) 0.1320(10) Uani 1 1 d . . . 
Br3B Br -0.85172(15) 0.57062(9) 1.32511(13) 0.1117(8) Uani 1 1 d . . . 
Br4B Br -0.87706(12) 0.66090(8) 1.17821(13) 0.0965(7) Uani 1 1 d . . . 
Br3C Br -0.54465(16) 0.19475(8) 0.90335(16) 0.1202(9) Uani 1 1 d . . . 
Br4C Br -0.60831(15) 0.22199(8) 1.08978(15) 0.1152(8) Uani 1 1 d . . . 
C7A C 0.0096(12) 0.1249(8) 0.7047(14) 0.086(5) Uani 1 1 d . . . 
C8A C 0.0005(10) 0.0776(7) 0.6589(12) 0.073(5) Uani 1 1 d . . . 
H8AA H -0.0227 0.0474 0.6822 0.087 Uiso 1 1 calc R . . 
C9A C 0.0255(10) 0.0760(6) 0.5809(14) 0.081(6) Uani 1 1 d . . . 
H9AA H 0.0167 0.0453 0.5511 0.097 Uiso 1 1 calc R . . 
C10A C 0.0647(9) 0.1210(7) 0.5456(13) 0.070(5) Uani 1 1 d . . . 
C11A C 0.0800(12) 0.1687(8) 0.5962(13) 0.093(6) Uani 1 1 d . . . 
H11A H 0.1101 0.1980 0.5764 0.111 Uiso 1 1 calc R . . 
C12A C 0.0512(11) 0.1691(7) 0.6676(14) 0.087(6) Uani 1 1 d . . . 
H12A H 0.0579 0.2001 0.6970 0.104 Uiso 1 1 calc R . . 
C13A C -0.0236(13) 0.1289(10) 0.7752(15) 0.102(7) Uani 1 1 d . . . 
C14A C -0.0245(15) 0.1760(10) 0.8246(13) 0.108(7) Uani 1 1 d . . . 
C15A C -0.0667(16) 0.0854(12) 0.8150(14) 0.122(10) Uani 1 1 d . . . 
N7A N -0.0251(13) 0.2162(8) 0.8557(13) 0.145(8) Uani 1 1 d . . . 
N7B N -0.1071(12) 0.0522(9) 0.8417(12) 0.138(8) Uani 1 1 d . . . 
C16A C 0.0880(11) 0.1231(7) 0.4666(13) 0.083(6) Uani 1 1 d . . . 
C17A C 0.1241(12) 0.1704(9) 0.4272(11) 0.082(6) Uani 1 1 d . . . 
C18A C 0.0702(10) 0.0780(8) 0.4141(10) 0.072(5) Uani 1 1 d . . . 
N7C N 0.1502(12) 0.2060(7) 0.3979(11) 0.111(6) Uani 1 1 d . . . 
N7D N 0.0504(9) 0.0450(6) 0.3730(10) 0.090(5) Uani 1 1 d . . . 
C7B C 0.3741(9) -0.1389(8) 0.6474(9) 0.064(4) Uani 1 1 d . . . 
C8B C 0.3691(11) -0.1166(7) 0.7254(10) 0.072(5) Uani 1 1 d . . . 
H8BA H 0.3503 -0.1380 0.7665 0.086 Uiso 1 1 calc R . . 
C9B C 0.3901(10) -0.0666(8) 0.7423(10) 0.075(5) Uani 1 1 d . . . 
H9BA H 0.3785 -0.0532 0.7926 0.089 Uiso 1 1 calc R . . 
C10B C 0.4306(11) -0.0325(7) 0.6841(10) 0.070(5) Uani 1 1 d . . . 
C11B C 0.4342(10) -0.0540(6) 0.6036(11) 0.071(5) Uani 1 1 d . . . 
H11B H 0.4539 -0.0327 0.5626 0.085 Uiso 1 1 calc R . . 
C12B C 0.4093(8) -0.1048(7) 0.5875(9) 0.063(4) Uani 1 1 d . . . 
H12B H 0.4152 -0.1178 0.5360 0.076 Uiso 1 1 calc R . . 
C13B C 0.3532(11) -0.1910(8) 0.6319(12) 0.073(5) Uani 1 1 d . . . 
C14B C 0.3635(12) -0.2133(6) 0.5544(13) 0.068(5) Uani 1 1 d . . . 
C15B C 0.3199(11) -0.2233(7) 0.6927(12) 0.077(5) Uani 1 1 d . . . 
N8A N 0.3708(13) -0.2326(6) 0.4932(11) 0.118(6) Uani 1 1 d . . . 
N8B N 0.2939(11) -0.2499(6) 0.7407(12) 0.118(6) Uani 1 1 d . . . 
C16B C 0.4558(11) 0.0182(7) 0.7008(11) 0.068(4) Uani 1 1 d . . . 
C17B C 0.4916(10) 0.0527(7) 0.6390(12) 0.072(5) Uani 1 1 d . . . 
C18B C 0.4543(12) 0.0391(7) 0.7776(14) 0.081(6) Uani 1 1 d . . . 
N8C N 0.5188(11) 0.0788(7) 0.5915(10) 0.105(6) Uani 1 1 d . . . 
N8D N 0.4619(11) 0.0563(7) 0.8376(10) 0.103(5) Uani 1 1 d . . . 
S1S S 0.3752(6) 0.2004(3) 0.5679(5) 0.190(3) Uani 1 1 d U . . 
C1S C 0.4077(19) 0.2131(9) 0.6580(15) 0.177(7) Uani 1 1 d U . . 
H1SA H 0.4329 0.1819 0.6832 0.266 Uiso 1 1 calc R . . 
H1SB H 0.3556 0.2250 0.6863 0.266 Uiso 1 1 calc R . . 
H1SC H 0.4542 0.2402 0.6591 0.266 Uiso 1 1 calc R . . 
C2S C 0.337(2) 0.2587(9) 0.5328(18) 0.218(8) Uani 1 1 d U . . 
H2SA H 0.3222 0.2561 0.4762 0.327 Uiso 1 1 calc R . . 
H2SB H 0.3838 0.2850 0.5428 0.327 Uiso 1 1 calc R . . 
H2SC H 0.2821 0.2686 0.5594 0.327 Uiso 1 1 calc R . . 
O1S O 0.2951(9) 0.1632(4) 0.5717(8) 0.114(4) Uani 1 1 d U . . 
S2S S -0.8094(5) 0.3396(3) 1.2454(5) 0.178(3) Uani 1 1 d U . . 
C3S C -0.7739(18) 0.3317(10) 1.3425(16) 0.192(7) Uani 1 1 d U . . 
H3SA H -0.7646 0.3656 1.3671 0.288 Uiso 1 1 calc R . . 
H3SB H -0.7168 0.3123 1.3460 0.288 Uiso 1 1 calc R . . 
H3SC H -0.8202 0.3126 1.3697 0.288 Uiso 1 1 calc R . . 
C4S C -0.8203(18) 0.2755(10) 1.2200(17) 0.198(7) Uani 1 1 d U . . 
H4SA H -0.8434 0.2728 1.1652 0.296 Uiso 1 1 calc R . . 
H4SB H -0.8627 0.2587 1.2541 0.296 Uiso 1 1 calc R . . 
H4SC H -0.7609 0.2586 1.2263 0.296 Uiso 1 1 calc R . . 
O2S O -0.7242(9) 0.3615(5) 1.2074(9) 0.131(4) Uani 1 1 d U . . 
S3S S 0.1402(7) 0.3968(4) 0.5149(5) 0.204(4) Uani 1 1 d U . . 
C5SA C 0.157(5) 0.469(3) 0.504(4) 0.208(15) Uani 0.46(5) 1 d PU A 1 
H5SA H 0.2192 0.4761 0.4888 0.312 Uiso 0.46(5) 1 calc PR A 1 
H5SB H 0.1482 0.4863 0.5546 0.312 Uiso 0.46(5) 1 calc PR A 1 
H5SC H 0.1136 0.4828 0.4641 0.312 Uiso 0.46(5) 1 calc PR A 1 
C5SB C 0.168(4) 0.449(3) 0.450(4) 0.215(14) Uani 0.54(5) 1 d PU A 2 
H5SD H 0.1957 0.4344 0.4040 0.322 Uiso 0.54(5) 1 calc PR A 2 
H5SE H 0.2103 0.4723 0.4776 0.322 Uiso 0.54(5) 1 calc PR A 2 
H5SF H 0.1122 0.4673 0.4333 0.322 Uiso 0.54(5) 1 calc PR A 2 
C6S C 0.0235(17) 0.4147(11) 0.5381(15) 0.198(11) Uani 1 1 d U A . 
H6SA H -0.0086 0.3840 0.5554 0.296 Uiso 1 1 calc R . . 
H6SB H -0.0087 0.4290 0.4911 0.296 Uiso 1 1 calc R . . 
H6SC H 0.0257 0.4406 0.5800 0.296 Uiso 1 1 calc R . . 
O3S O 0.1965(15) 0.3887(10) 0.5900(11) 0.229(7) Uani 1 1 d U A . 
loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
C1 0.042(9) 0.045(9) 0.064(10) -0.009(9) -0.007(8) 0.022(7) 
C2 0.045(10) 0.060(12) 0.091(14) 0.011(11) 0.007(9) -0.017(8) 
C3 0.035(9) 0.061(11) 0.073(12) 0.006(10) -0.016(8) 0.018(8) 
C4 0.040(10) 0.120(18) 0.074(14) 0.013(13) -0.002(10) -0.011(10) 
C5 0.064(11) 0.079(13) 0.056(11) -0.002(10) 0.009(9) -0.032(10) 
C6 0.039(9) 0.065(11) 0.078(12) 0.021(10) 0.003(8) 0.023(8) 
N2 0.066(9) 0.056(9) 0.078(10) 0.001(8) 0.014(7) -0.002(7) 
C1A 0.060(10) 0.048(11) 0.072(12) 0.011(10) -0.002(9) 0.008(8) 
C2A 0.049(10) 0.043(10) 0.128(16) 0.008(11) 0.016(11) 0.009(8) 
C3A 0.063(12) 0.137(19) 0.096(15) -0.013(14) 0.020(11) -0.003(12) 
C4A 0.064(11) 0.094(14) 0.085(13) -0.024(12) 0.016(10) 0.009(10) 
C5A 0.101(14) 0.059(11) 0.066(11) 0.002(10) 0.043(10) 0.014(9) 
C6A 0.046(9) 0.048(10) 0.065(11) 0.016(9) -0.002(8) -0.001(8) 
N4 0.059(9) 0.049(9) 0.106(12) 0.008(9) 0.010(8) 0.008(7) 
C1B 0.040(10) 0.072(13) 0.087(13) 0.020(12) 0.006(9) -0.008(9) 
C2B 0.052(11) 0.100(16) 0.081(13) 0.005(12) 0.019(9) -0.008(10) 
C3B 0.068(12) 0.078(14) 0.100(15) -0.027(12) 0.017(11) 0.002(11) 
C4B 0.058(11) 0.058(12) 0.135(18) -0.015(13) -0.029(12) -0.004(9) 
C5B 0.091(13) 0.071(13) 0.065(12) -0.026(10) -0.003(10) -0.041(10) 
C6B 0.023(8) 0.061(11) 0.114(15) -0.052(12) 0.001(9) -0.008(8) 
N6 0.038(7) 0.085(10) 0.097(11) -0.036(10) 0.020(7) -0.016(7) 
C1C 0.087(13) 0.084(15) 0.060(12) -0.010(11) 0.032(10) -0.007(11) 
C2C 0.059(11) 0.055(12) 0.131(17) -0.033(13) 0.010(11) 0.011(9) 
C3C 0.057(11) 0.071(13) 0.137(18) 0.011(14) 0.013(12) 0.022(10) 
C4C 0.047(10) 0.050(12) 0.141(18) 0.016(12) 0.003(11) -0.002(8) 
C5C 0.060(11) 0.061(12) 0.105(14) 0.002(11) -0.005(10) -0.010(9) 
C6C 0.048(10) 0.045(11) 0.116(16) 0.017(11) 0.014(10) 0.002(8) 
Br3A 0.153(2) 0.1077(17) 0.132(2) 0.0433(15) 0.0500(17) 0.0245(15) 
Br4A 0.163(2) 0.130(2) 0.1083(17) 0.0134(15) 0.0545(16) 0.0217(17) 
Br3B 0.0963(16) 0.145(2) 0.0970(15) -0.0191(14) 0.0310(12) -0.0115(14) 
Br4B 0.0714(13) 0.0911(14) 0.1292(17) -0.0306(13) 0.0236(12) -0.0075(11) 
Br3C 0.1191(18) 0.0720(14) 0.171(2) 0.0109(14) 0.0239(16) 0.0257(13) 
Br4C 0.1137(18) 0.0857(15) 0.147(2) 0.0337(14) 0.0115(15) 0.0086(13) 
C7A 0.053(12) 0.090(16) 0.115(17) -0.022(15) 0.001(12) -0.016(11) 
C8A 0.050(11) 0.088(15) 0.081(13) 0.010(12) 0.005(10) -0.006(9) 
C9A 0.029(9) 0.051(11) 0.16(2) -0.003(12) -0.021(11) 0.002(8) 
C10A 0.029(9) 0.066(13) 0.115(16) -0.007(12) -0.003(10) -0.001(8) 
C11A 0.074(13) 0.089(16) 0.116(17) 0.004(14) 0.023(13) -0.009(11) 
C12A 0.054(11) 0.070(13) 0.139(19) -0.016(13) 0.021(12) -0.001(10) 
C13A 0.055(13) 0.14(2) 0.114(19) 0.016(18) 0.008(13) -0.018(13) 
C14A 0.121(18) 0.109(19) 0.099(17) -0.019(15) 0.051(14) -0.017(15) 
C15A 0.072(17) 0.20(3) 0.102(17) -0.068(19) 0.038(13) -0.032(16) 
N7A 0.124(15) 0.136(17) 0.18(2) -0.071(15) 0.051(13) -0.031(13) 
N7B 0.062(12) 0.21(2) 0.144(17) -0.056(16) 0.034(11) -0.034(12) 
C16A 0.055(11) 0.095(15) 0.094(15) 0.040(14) -0.025(11) -0.012(10) 
C17A 0.061(12) 0.099(16) 0.087(14) 0.023(12) 0.002(10) 0.029(12) 
C18A 0.032(9) 0.105(16) 0.075(13) -0.027(11) -0.022(8) -0.007(10) 
N7C 0.090(12) 0.112(15) 0.133(15) 0.041(12) 0.009(11) 0.005(11) 
N7D 0.056(9) 0.101(12) 0.113(13) -0.021(10) -0.007(9) -0.020(9) 
C7B 0.039(9) 0.110(15) 0.042(10) 0.019(11) -0.004(7) 0.009(10) 
C8B 0.079(12) 0.069(13) 0.068(13) 0.018(10) 0.014(9) 0.034(10) 
C9B 0.051(10) 0.094(14) 0.082(12) 0.021(12) 0.035(9) 0.017(10) 
C10B 0.065(11) 0.076(13) 0.068(12) -0.009(11) 0.000(9) 0.017(10) 
C11B 0.061(11) 0.038(10) 0.110(15) 0.007(10) -0.017(10) -0.014(8) 
C12B 0.027(8) 0.092(13) 0.071(11) 0.007(10) -0.001(8) 0.004(8) 
C13B 0.062(11) 0.064(12) 0.091(15) 0.030(12) -0.006(10) -0.010(10) 
C14B 0.078(12) 0.044(11) 0.082(15) 0.010(10) 0.000(12) 0.009(9) 
C15B 0.055(11) 0.057(12) 0.119(16) 0.019(12) 0.003(11) 0.021(9) 
N8A 0.140(16) 0.090(13) 0.121(16) -0.019(11) -0.006(13) 0.023(11) 
N8B 0.089(12) 0.089(12) 0.178(18) 0.075(12) 0.011(12) 0.010(9) 
C16B 0.059(11) 0.051(11) 0.095(15) -0.001(11) 0.010(10) 0.015(9) 
C17B 0.028(10) 0.083(14) 0.105(16) -0.017(12) 0.004(10) 0.007(9) 
C18B 0.076(13) 0.079(14) 0.085(15) -0.022(12) -0.012(13) -0.013(10) 
N8C 0.084(12) 0.118(14) 0.116(14) 0.018(11) 0.034(10) 0.004(10) 
N8D 0.108(13) 0.112(14) 0.086(12) -0.006(11) -0.011(11) 0.012(10) 
S1S 0.220(7) 0.133(5) 0.208(7) 0.046(5) -0.072(6) -0.088(5) 
C1S 0.228(17) 0.116(14) 0.185(11) 0.006(11) -0.014(13) -0.064(12) 
C2S 0.268(18) 0.119(10) 0.258(17) 0.056(13) -0.069(16) -0.101(10) 
O1S 0.126(9) 0.075(7) 0.142(9) 0.021(7) 0.011(8) -0.007(6) 
S2S 0.147(6) 0.173(6) 0.218(7) 0.076(6) 0.052(5) -0.025(5) 
C3S 0.184(16) 0.195(16) 0.203(9) 0.067(12) 0.067(11) -0.056(14) 
C4S 0.172(16) 0.189(10) 0.235(16) 0.058(13) 0.045(15) -0.076(12) 
O2S 0.107(8) 0.120(9) 0.168(10) 0.061(9) 0.021(8) -0.008(7) 
S3S 0.215(9) 0.284(10) 0.119(5) -0.005(7) 0.058(6) -0.028(8) 
C5SA 0.18(3) 0.323(15) 0.11(3) 0.00(2) -0.06(3) -0.18(2) 
C5SB 0.19(3) 0.34(3) 0.11(3) -0.01(2) -0.02(2) -0.18(3) 
C6S 0.161(12) 0.25(3) 0.18(2) -0.06(2) 0.035(12) -0.113(15) 
O3S 0.222(14) 0.351(17) 0.120(9) -0.010(13) 0.060(9) 0.017(14) 
_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 1.431(19) . ? 
C1 C6 1.451(18) . ? 
C1 C6A 1.454(18) . ? 
C2 N2 1.359(18) . ? 
C2 C3 1.39(2) . ? 
C3 C4 1.38(2) . ? 
C3 C6B 1.45(2) . ? 
C4 N4 1.349(19) . ? 
C4 C5 1.45(2) . ? 
C5 C6 1.389(19) . ? 
C5 C6C 1.47(2) . ? 
C6 N6 1.359(17) . ? 
N2 C1A 1.373(17) . ? 
C1A C2A 1.35(2) . ? 
C1A C6A 1.412(19) . ? 
C2A C3A 1.37(2) . ? 
C3A C4A 1.43(2) . ? 
C3A Br3A 1.88(2) . ? 
C4A C5A 1.42(2) . ? 
C4A Br4A 1.904(16) . ? 
C5A C6A 1.318(18) . ? 
N4 C1B 1.378(19) . ? 
C1B C2B 1.38(2) . ? 
C1B C6B 1.43(2) . ? 
C2B C3B 1.35(2) . ? 
C3B C4B 1.41(2) . ? 
C3B Br3B 1.907(17) . ? 
C4B C5B 1.37(2) . ? 
C4B Br4B 1.875(17) . ? 
C5B C6B 1.42(2) . ? 
N6 C1C 1.430(19) . ? 
C1C C2C 1.38(2) . ? 
C1C C6C 1.39(2) . ? 
C2C C3C 1.36(2) . ? 
C3C C4C 1.42(2) . ? 
C3C Br3C 1.860(18) . ? 
C4C C5C 1.41(2) . ? 
C4C Br4C 1.891(17) . ? 
C5C C6C 1.42(2) . ? 
C7A C13A 1.30(2) . ? 
C7A C8A 1.43(2) . ? 
C7A C12A 1.43(2) . ? 
C8A C9A 1.37(2) . ? 
C9A C10A 1.42(2) . ? 
C10A C16A 1.38(2) . ? 
C10A C11A 1.49(2) . ? 
C11A C12A 1.29(2) . ? 
C13A C15A 1.45(3) . ? 
C13A C14A 1.45(3) . ? 
C14A N7A 1.15(2) . ? 
C15A N7B 1.13(3) . ? 
C16A C18A 1.46(2) . ? 
C16A C17A 1.48(3) . ? 
C17A N7C 1.10(2) . ? 
C18A N7D 1.111(18) . ? 
C7B C13B 1.38(2) . ? 
C7B C8B 1.43(2) . ? 
C7B C12B 1.438(19) . ? 
C8B C9B 1.33(2) . ? 
C9B C10B 1.45(2) . ? 
C10B C16B 1.36(2) . ? 
C10B C11B 1.46(2) . ? 
C11B C12B 1.361(18) . ? 
C13B C15B 1.41(2) . ? 
C13B C14B 1.43(2) . ? 
C14B N8A 1.14(2) . ? 
C15B N8B 1.13(2) . ? 
C16B C18B 1.39(2) . ? 
C16B C17B 1.47(2) . ? 
C17B N8C 1.12(2) . ? 
C18B N8D 1.09(2) . ? 
S1S O1S 1.498(13) . ? 
S1S C1S 1.59(2) . ? 
S1S C2S 1.68(3) . ? 
S2S O2S 1.523(13) . ? 
S2S C4S 1.68(3) . ? 
S2S C3S 1.69(3) . ? 
S3S O3S 1.47(2) . ? 
S3S C5SB 1.76(5) . ? 
S3S C6S 1.81(3) . ? 
S3S C5SA 1.87(7) . ? 
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 C6 116.3(14) . . ? 
C2 C1 C6A 109.1(13) . . ? 
C6 C1 C6A 134.6(14) . . ? 
N2 C2 C3 132.2(16) . . ? 
N2 C2 C1 106.0(14) . . ? 
C3 C2 C1 121.7(15) . . ? 
C4 C3 C2 120.2(16) . . ? 
C4 C3 C6B 104.2(15) . . ? 
C2 C3 C6B 135.4(16) . . ? 
N4 C4 C3 109.9(17) . . ? 
N4 C4 C5 128.5(18) . . ? 
C3 C4 C5 121.6(17) . . ? 
C6 C5 C4 117.1(16) . . ? 
C6 C5 C6C 106.1(15) . . ? 
C4 C5 C6C 136.8(16) . . ? 
N6 C6 C5 110.3(14) . . ? 
N6 C6 C1 126.7(15) . . ? 
C5 C6 C1 123.0(15) . . ? 
C2 N2 C1A 111.0(13) . . ? 
C2A C1A N2 129.7(16) . . ? 
C2A C1A C6A 120.1(15) . . ? 
N2 C1A C6A 110.2(14) . . ? 
C1A C2A C3A 120.2(16) . . ? 
C2A C3A C4A 118.4(18) . . ? 
C2A C3A Br3A 120.7(16) . . ? 
C4A C3A Br3A 120.9(15) . . ? 
C5A C4A C3A 121.3(15) . . ? 
C5A C4A Br4A 118.1(13) . . ? 
C3A C4A Br4A 120.4(15) . . ? 
C6A C5A C4A 116.1(14) . . ? 
C5A C6A C1A 123.6(14) . . ? 
C5A C6A C1 132.4(14) . . ? 
C1A C6A C1 103.4(13) . . ? 
C4 N4 C1B 113.0(15) . . ? 
N4 C1B C2B 134.8(18) . . ? 
N4 C1B C6B 102.9(15) . . ? 
C2B C1B C6B 122.2(17) . . ? 
C3B C2B C1B 116.8(17) . . ? 
C2B C3B C4B 124.4(17) . . ? 
C2B C3B Br3B 114.0(16) . . ? 
C4B C3B Br3B 121.2(15) . . ? 
C5B C4B C3B 118.1(16) . . ? 
C5B C4B Br4B 120.7(16) . . ? 
C3B C4B Br4B 120.7(17) . . ? 
C4B C5B C6B 120.2(17) . . ? 
C5B C6B C1B 117.8(16) . . ? 
C5B C6B C3 132.3(19) . . ? 
C1B C6B C3 109.8(14) . . ? 
C6 N6 C1C 108.9(13) . . ? 
C2C C1C C6C 124.6(19) . . ? 
C2C C1C N6 128.1(16) . . ? 
C6C C1C N6 107.3(15) . . ? 
C3C C2C C1C 115.9(18) . . ? 
C2C C3C C4C 121.4(16) . . ? 
C2C C3C Br3C 117.3(17) . . ? 
C4C C3C Br3C 121.0(16) . . ? 
C5C C4C C3C 123.4(16) . . ? 
C5C C4C Br4C 115.0(16) . . ? 
C3C C4C Br4C 121.4(14) . . ? 
C4C C5C C6C 113.0(16) . . ? 
C1C C6C C5C 121.4(16) . . ? 
C1C C6C C5 107.4(15) . . ? 
C5C C6C C5 131.2(17) . . ? 
C13A C7A C8A 122(2) . . ? 
C13A C7A C12A 121(2) . . ? 
C8A C7A C12A 117.1(19) . . ? 
C9A C8A C7A 120.8(18) . . ? 
C8A C9A C10A 120.4(17) . . ? 
C16A C10A C9A 123.6(18) . . ? 
C16A C10A C11A 118.4(17) . . ? 
C9A C10A C11A 118.0(18) . . ? 
C12A C11A C10A 119.3(18) . . ? 
C11A C12A C7A 124.2(19) . . ? 
C7A C13A C15A 123(2) . . ? 
C7A C13A C14A 127(2) . . ? 
C15A C13A C14A 110(2) . . ? 
N7A C14A C13A 172(2) . . ? 
N7B C15A C13A 174(3) . . ? 
C10A C16A C18A 120.0(16) . . ? 
C10A C16A C17A 124.7(18) . . ? 
C18A C16A C17A 115.1(18) . . ? 
N7C C17A C16A 179(2) . . ? 
N7D C18A C16A 174.9(18) . . ? 
C13B C7B C8B 122.1(16) . . ? 
C13B C7B C12B 122.0(16) . . ? 
C8B C7B C12B 115.8(17) . . ? 
C9B C8B C7B 123.4(17) . . ? 
C8B C9B C10B 121.4(16) . . ? 
C16B C10B C9B 122.6(17) . . ? 
C16B C10B C11B 121.3(16) . . ? 
C9B C10B C11B 115.8(16) . . ? 
C12B C11B C10B 121.0(16) . . ? 
C11B C12B C7B 122.1(16) . . ? 
C7B C13B C15B 120.1(18) . . ? 
C7B C13B C14B 121.2(16) . . ? 
C15B C13B C14B 118.7(17) . . ? 
N8A C14B C13B 178(2) . . ? 
N8B C15B C13B 179(2) . . ? 
C10B C16B C18B 122.2(17) . . ? 
C10B C16B C17B 121.2(17) . . ? 
C18B C16B C17B 116.5(16) . . ? 
N8C C17B C16B 180(2) . . ? 
N8D C18B C16B 173(2) . . ? 
O1S S1S C1S 106.0(12) . . ? 
O1S S1S C2S 109.2(11) . . ? 
C1S S1S C2S 103.1(14) . . ? 
O2S S2S C4S 108.2(11) . . ? 
O2S S2S C3S 103.6(11) . . ? 
C4S S2S C3S 98.4(14) . . ? 
O3S S3S C5SB 120(2) . . ? 
O3S S3S C6S 109.2(12) . . ? 
C5SB S3S C6S 101(3) . . ? 
O3S S3S C5SA 99(2) . . ? 
C5SB S3S C5SA 34(2) . . ? 
C6S S3S C5SA 85(3) . . ? 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              52.58 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.892 
_refine_diff_density_min   -0.632 
_refine_diff_density_rms    0.095