# Electronic Supplementary Material (ESI) for RSC Advances
# This journal is © The Royal Society of Chemistry 2013


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#  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. 
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#  fide research purposes only. It may contain copyright material 
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data_n1545
_database_code_depnum_ccdc_archive 'CCDC 894064'
#TrackingRef '- CIF Files of X-Ray Structures.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H30 N4, 2(Br), 2(O) '
_chemical_formula_sum            'C38 H30 Br2 N4 O2'
_chemical_formula_weight         734.48
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'
_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                   8.3588(2)
_cell_length_b                   10.3505(3)
_cell_length_c                   10.9632(3)
_cell_angle_alpha                63.8699(15)
_cell_angle_beta                 84.6098(15)
_cell_angle_gamma                83.0969(16)
_cell_volume                     844.50(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2515
_cell_measurement_theta_min      4.78
_cell_measurement_theta_max      66.37
_exptl_crystal_description       palte
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             372
_exptl_absorpt_coefficient_mu    3.355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6089
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_process_details   'Twinabs, Bruker'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         microsource
_diffrn_radiation_monochromator  'MX optics'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2927
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.50
_diffrn_reflns_theta_max         67.02
_reflns_number_total             2927
_reflns_number_gt                2529
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of 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.
The crystal under investigation was found to be non-merohedrally twinned.
The orientation matrices for the two components were identified using the
program Cell_Now (Sheldrick, 2005), and the data were processed using both
orientation matrices with SAINT, The exact twin matrix identified
by the integration program was found to be
(1.00010 -0.15803 -0.07668 / 0.00058 -1.00056 0.00109
/ 0.00138 -0.00136 -0.99953). The second domain is rotated from first
domain by 179.9 \% about the real lattice a axis. The absorption correction
was carried out using TWINABS V2008/4 (Sheldrick, 2008) to create an hklf5
file which was used in all refinements; the structure was solved using direct
methods with only the non-overlapping reflections of component 1. The twin
fraction refined to a value of 0.4990(39).
;
_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^)+(0.1882P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2927
_refine_ls_number_parameters     212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0786
_refine_ls_wR_factor_ref         0.2278
_refine_ls_wR_factor_gt          0.2179
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.0000 0.0000 0.5000 0.0314(3) Uani 1 2 d S . .
Br2 Br 0.0000 0.5000 0.5000 0.0304(3) Uani 1 2 d S . .
O1 O 0.1895(5) 0.3122(5) 0.3371(4) 0.0435(10) Uani 1 1 d . . .
N1 N 0.5610(5) 0.8327(4) 0.3602(4) 0.0262(9) Uani 1 1 d . . .
N2 N 0.3123(5) 0.8162(4) 0.3307(4) 0.0265(9) Uani 1 1 d . . .
C1 C 0.4479(5) 0.8747(5) 0.2694(5) 0.0247(10) Uani 1 1 d . . .
H1 H 0.4619 0.9369 0.1753 0.030 Uiso 1 1 calc R . .
C2 C 0.4929(6) 0.7454(6) 0.4862(5) 0.0417(18) Uani 1 1 d . . .
H2 H 0.5448 0.7004 0.5702 0.050 Uiso 1 1 calc R . .
C3 C 0.3376(6) 0.7368(7) 0.4661(5) 0.0430(15) Uani 1 1 d . . .
H3 H 0.2603 0.6847 0.5340 0.052 Uiso 1 1 calc R . .
C4 C 0.7297(5) 0.8719(5) 0.3292(5) 0.0258(10) Uani 1 1 d . . .
H4A H 0.8048 0.7837 0.3683 0.031 Uiso 1 1 calc R . .
H4B H 0.7484 0.9362 0.3707 0.031 Uiso 1 1 calc R . .
C5 C 0.1596(5) 0.8405(5) 0.2616(5) 0.0248(10) Uani 1 1 d . . .
H5A H 0.0795 0.9013 0.2906 0.030 Uiso 1 1 calc R . .
H5B H 0.1154 0.7466 0.2886 0.030 Uiso 1 1 calc R . .
C6 C 0.1872(5) 0.9136(5) 0.1092(5) 0.0224(10) Uani 1 1 d . . .
C7 C 0.1708(5) 1.0664(5) 0.0393(5) 0.0221(9) Uani 1 1 d . . .
C8 C 0.1325(6) 1.1537(6) 0.1113(5) 0.0291(11) Uani 1 1 d . . .
H8 H 0.1169 1.1089 0.2075 0.035 Uiso 1 1 calc R . .
C9 C 0.1184(6) 1.3007(6) 0.0425(5) 0.0319(11) Uani 1 1 d . . .
H9 H 0.0927 1.3575 0.0913 0.038 Uiso 1 1 calc R . .
C10 C 0.1417(6) 1.3693(5) -0.1006(5) 0.0332(12) Uani 1 1 d . . .
H10 H 0.1294 1.4717 -0.1475 0.040 Uiso 1 1 calc R . .
C11 C 0.1813(6) 1.2897(5) -0.1709(5) 0.0277(11) Uani 1 1 d . . .
H11 H 0.1994 1.3377 -0.2668 0.033 Uiso 1 1 calc R . .
C12 C 0.1969(5) 1.1346(5) -0.1045(5) 0.0226(10) Uani 1 1 d . . .
C13 C 0.2388(5) 1.0526(5) -0.1779(5) 0.0218(9) Uani 1 1 d . . .
C14 C 0.2607(5) 0.9000(5) -0.1076(5) 0.0244(10) Uani 1 1 d . . .
C15 C 0.3142(6) 0.8123(6) -0.1766(6) 0.0330(11) Uani 1 1 d . . .
H15 H 0.3322 0.8568 -0.2726 0.040 Uiso 1 1 calc R . .
C16 C 0.3398(7) 0.6662(6) -0.1071(6) 0.0384(12) Uani 1 1 d . . .
H16 H 0.3760 0.6102 -0.1553 0.046 Uiso 1 1 calc R . .
C17 C 0.3133(6) 0.5965(6) 0.0356(6) 0.0364(12) Uani 1 1 d . . .
H17 H 0.3305 0.4944 0.0829 0.044 Uiso 1 1 calc R . .
C18 C 0.2632(5) 0.6761(5) 0.1045(5) 0.0294(11) Uani 1 1 d . . .
H18 H 0.2464 0.6283 0.2005 0.035 Uiso 1 1 calc R . .
C19 C 0.2346(5) 0.8303(5) 0.0372(5) 0.0244(10) Uani 1 1 d . . .
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
Br1 0.0357(5) 0.0391(5) 0.0217(5) -0.0135(4) -0.0011(4) -0.0110(4)
Br2 0.0330(5) 0.0263(5) 0.0211(5) 0.0010(3) -0.0059(4) -0.0044(3)
O1 0.049(2) 0.045(2) 0.031(2) -0.0103(19) -0.004(2) -0.0089(19)
N1 0.0232(19) 0.030(2) 0.020(2) -0.0048(17) -0.0032(16) -0.0061(16)
N2 0.022(2) 0.030(2) 0.019(2) -0.0015(17) -0.0029(16) -0.0064(16)
C1 0.018(2) 0.031(2) 0.021(2) -0.005(2) -0.0018(17) -0.0071(17)
C2 0.033(3) 0.057(5) 0.019(3) 0.001(3) -0.005(3) -0.011(3)
C3 0.024(2) 0.062(4) 0.023(3) 0.002(3) -0.002(2) -0.013(2)
C4 0.020(2) 0.032(2) 0.024(3) -0.010(2) -0.0047(18) -0.0048(18)
C5 0.016(2) 0.030(2) 0.024(3) -0.006(2) -0.0020(19) -0.0058(17)
C6 0.0100(17) 0.031(2) 0.022(2) -0.006(2) -0.0031(16) -0.0052(16)
C7 0.0140(18) 0.028(2) 0.021(2) -0.0068(19) -0.0022(17) -0.0047(16)
C8 0.026(2) 0.035(3) 0.023(3) -0.008(2) -0.0057(19) -0.0071(19)
C9 0.032(3) 0.034(3) 0.032(3) -0.017(2) -0.004(2) -0.001(2)
C10 0.036(3) 0.025(2) 0.033(3) -0.007(2) -0.009(2) -0.003(2)
C11 0.029(2) 0.029(2) 0.019(3) -0.002(2) -0.0058(19) -0.0078(19)
C12 0.016(2) 0.027(2) 0.019(2) -0.0035(19) -0.0052(17) -0.0048(17)
C13 0.0131(19) 0.029(2) 0.021(2) -0.0066(19) -0.0046(17) -0.0054(16)
C14 0.018(2) 0.030(2) 0.022(2) -0.008(2) -0.0009(18) -0.0071(18)
C15 0.028(2) 0.037(3) 0.035(3) -0.017(2) 0.000(2) -0.005(2)
C16 0.033(3) 0.039(3) 0.047(3) -0.023(3) -0.001(2) -0.001(2)
C17 0.028(2) 0.032(3) 0.044(3) -0.011(2) -0.005(2) 0.000(2)
C18 0.025(2) 0.028(3) 0.025(3) -0.001(2) -0.003(2) -0.0043(19)
C19 0.014(2) 0.029(2) 0.027(3) -0.008(2) -0.0043(18) -0.0049(17)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.331(6) . ?
N1 C2 1.388(6) . ?
N1 C4 1.481(6) . ?
N2 C1 1.329(6) . ?
N2 C3 1.366(7) . ?
N2 C5 1.484(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.356(7) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C13 1.503(6) 2_675 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.509(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C19 1.408(7) . ?
C6 C7 1.416(7) . ?
C7 C12 1.422(7) . ?
C7 C8 1.433(7) . ?
C8 C9 1.364(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.413(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.352(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.437(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.402(7) . ?
C13 C14 1.417(7) . ?
C13 C4 1.503(6) 2_675 ?
C14 C15 1.428(7) . ?
C14 C19 1.432(7) . ?
C15 C16 1.361(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.413(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.353(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.433(7) . ?
C18 H18 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 107.8(4) . . ?
C1 N1 C4 125.2(4) . . ?
C2 N1 C4 127.0(4) . . ?
C1 N2 C3 108.2(4) . . ?
C1 N2 C5 124.6(4) . . ?
C3 N2 C5 127.1(4) . . ?
N2 C1 N1 109.5(4) . . ?
N2 C1 H1 125.3 . . ?
N1 C1 H1 125.3 . . ?
C3 C2 N1 106.6(5) . . ?
C3 C2 H2 126.7 . . ?
N1 C2 H2 126.7 . . ?
C2 C3 N2 107.8(5) . . ?
C2 C3 H3 126.1 . . ?
N2 C3 H3 126.1 . . ?
N1 C4 C13 109.9(4) . 2_675 ?
N1 C4 H4A 109.7 . . ?
C13 C4 H4A 109.7 2_675 . ?
N1 C4 H4B 109.7 . . ?
C13 C4 H4B 109.7 2_675 . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 110.9(4) . . ?
N2 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.0 . . ?
C19 C6 C7 120.1(4) . . ?
C19 C6 C5 120.0(4) . . ?
C7 C6 C5 119.8(4) . . ?
C6 C7 C12 119.5(4) . . ?
C6 C7 C8 121.2(5) . . ?
C12 C7 C8 119.3(4) . . ?
C9 C8 C7 120.4(5) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 120.6(5) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 120.3(5) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 121.7(5) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C13 C12 C7 120.9(4) . . ?
C13 C12 C11 121.5(4) . . ?
C7 C12 C11 117.6(4) . . ?
C12 C13 C14 119.7(4) . . ?
C12 C13 C4 119.6(4) . 2_675 ?
C14 C13 C4 120.7(4) . 2_675 ?
C13 C14 C15 121.8(5) . . ?
C13 C14 C19 119.8(4) . . ?
C15 C14 C19 118.3(4) . . ?
C16 C15 C14 121.1(5) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 120.9(5) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 119.7(5) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 122.0(5) . . ?
C17 C18 H18 119.0 . . ?
C19 C18 H18 119.0 . . ?
C6 C19 C14 119.9(4) . . ?
C6 C19 C18 122.1(5) . . ?
C14 C19 C18 118.0(4) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 1.5(6) . . . . ?
C5 N2 C1 N1 179.2(4) . . . . ?
C2 N1 C1 N2 -1.3(6) . . . . ?
C4 N1 C1 N2 177.9(4) . . . . ?
C1 N1 C2 C3 0.5(7) . . . . ?
C4 N1 C2 C3 -178.6(5) . . . . ?
N1 C2 C3 N2 0.4(7) . . . . ?
C1 N2 C3 C2 -1.2(7) . . . . ?
C5 N2 C3 C2 -178.8(5) . . . . ?
C1 N1 C4 C13 -8.4(6) . . . 2_675 ?
C2 N1 C4 C13 170.6(5) . . . 2_675 ?
C1 N2 C5 C6 12.0(7) . . . . ?
C3 N2 C5 C6 -170.8(5) . . . . ?
N2 C5 C6 C19 87.1(5) . . . . ?
N2 C5 C6 C7 -90.7(5) . . . . ?
C19 C6 C7 C12 2.3(6) . . . . ?
C5 C6 C7 C12 -179.9(4) . . . . ?
C19 C6 C7 C8 -176.1(4) . . . . ?
C5 C6 C7 C8 1.7(6) . . . . ?
C6 C7 C8 C9 179.5(4) . . . . ?
C12 C7 C8 C9 1.1(7) . . . . ?
C7 C8 C9 C10 -0.2(7) . . . . ?
C8 C9 C10 C11 -1.3(8) . . . . ?
C9 C10 C11 C12 1.7(7) . . . . ?
C6 C7 C12 C13 -0.1(6) . . . . ?
C8 C7 C12 C13 178.3(4) . . . . ?
C6 C7 C12 C11 -179.1(4) . . . . ?
C8 C7 C12 C11 -0.7(6) . . . . ?
C10 C11 C12 C13 -179.7(4) . . . . ?
C10 C11 C12 C7 -0.7(7) . . . . ?
C7 C12 C13 C14 -2.1(6) . . . . ?
C11 C12 C13 C14 176.9(4) . . . . ?
C7 C12 C13 C4 -178.2(4) . . . 2_675 ?
C11 C12 C13 C4 0.8(6) . . . 2_675 ?
C12 C13 C14 C15 -175.6(4) . . . . ?
C4 C13 C14 C15 0.5(6) 2_675 . . . ?
C12 C13 C14 C19 2.1(6) . . . . ?
C4 C13 C14 C19 178.1(4) 2_675 . . . ?
C13 C14 C15 C16 177.8(5) . . . . ?
C19 C14 C15 C16 0.1(7) . . . . ?
C14 C15 C16 C17 0.4(8) . . . . ?
C15 C16 C17 C18 -0.6(8) . . . . ?
C16 C17 C18 C19 0.4(7) . . . . ?
C7 C6 C19 C14 -2.3(6) . . . . ?
C5 C6 C19 C14 180.0(4) . . . . ?
C7 C6 C19 C18 175.7(4) . . . . ?
C5 C6 C19 C18 -2.0(6) . . . . ?
C13 C14 C19 C6 0.1(6) . . . . ?
C15 C14 C19 C6 177.8(4) . . . . ?
C13 C14 C19 C18 -178.0(4) . . . . ?
C15 C14 C19 C18 -0.3(6) . . . . ?
C17 C18 C19 C6 -178.1(4) . . . . ?
C17 C18 C19 C14 0.0(7) . . . . ?
_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        67.02
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         4.904
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.309
_vrf_PLAT306_I                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1
RESPONSE: Hydrogen atoms on the water molecule were not found.
;


data_prg111
_database_code_depnum_ccdc_archive 'CCDC 894065'
#TrackingRef '- CIF Files of X-Ray Structures.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H58 Br2 N8 O3'
_chemical_formula_weight         1098.96
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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                   10.3953(4)
_cell_length_b                   17.2537(6)
_cell_length_c                   16.1405(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.491(2)
_cell_angle_gamma                90.00
_cell_volume                     2846.53(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6426
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      21.0
_exptl_crystal_description       needle
_exptl_crystal_colour            'Pale brown'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_process_details   'SADABS(Bruker, 1999)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            25966
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9821
_reflns_number_gt                7012
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.1266P)^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    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   0.045(12)
_refine_ls_number_reflns         9821
_refine_ls_number_parameters     681
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1974
_refine_ls_wR_factor_gt          0.1719
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_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 0.8601(7) 0.5936(5) 0.0472(6) 0.057(2) Uani 1 1 d . . .
H1 H 0.9082 0.5483 0.0599 0.069 Uiso 1 1 calc R . .
C2 C 0.8421(7) 0.6334(5) -0.0272(6) 0.054(2) Uani 1 1 d . . .
H2 H 0.8767 0.6208 -0.0747 0.065 Uiso 1 1 calc R . .
C3 C 0.7107(7) 0.7515(5) -0.0830(5) 0.0530(18) Uani 1 1 d . . .
H3A H 0.7328 0.7366 -0.1366 0.064 Uiso 1 1 calc R . .
H3B H 0.7488 0.8019 -0.0678 0.064 Uiso 1 1 calc R . .
C4 C 0.5636(6) 0.7560(4) -0.0912(4) 0.0394(15) Uani 1 1 d . . .
C5 C 0.4875(7) 0.6970(4) -0.1327(5) 0.0431(17) Uani 1 1 d . . .
C6 C 0.5434(8) 0.6333(5) -0.1705(5) 0.0527(19) Uani 1 1 d . . .
H6 H 0.6326 0.6338 -0.1714 0.063 Uiso 1 1 calc R . .
C7 C 0.4719(11) 0.5728(5) -0.2049(6) 0.068(2) Uani 1 1 d . . .
H7 H 0.5116 0.5319 -0.2281 0.081 Uiso 1 1 calc R . .
C8 C 0.3375(11) 0.5717(6) -0.2056(6) 0.072(3) Uani 1 1 d . . .
H8 H 0.2882 0.5300 -0.2305 0.086 Uiso 1 1 calc R . .
C9 C 0.2775(9) 0.6289(6) -0.1713(6) 0.068(3) Uani 1 1 d . . .
H9 H 0.1880 0.6258 -0.1721 0.082 Uiso 1 1 calc R . .
C10 C 0.3493(7) 0.6952(5) -0.1331(5) 0.0467(17) Uani 1 1 d . . .
C11 C 0.2937(6) 0.7538(5) -0.0973(5) 0.0494(18) Uani 1 1 d . . .
C12 C 0.3662(7) 0.8185(4) -0.0562(5) 0.0460(18) Uani 1 1 d . . .
C13 C 0.3138(8) 0.8793(6) -0.0178(6) 0.060(2) Uani 1 1 d . . .
H13 H 0.2236 0.8808 -0.0209 0.072 Uiso 1 1 calc R . .
C14 C 0.3852(9) 0.9356(5) 0.0233(6) 0.061(2) Uani 1 1 d . . .
H14 H 0.3456 0.9746 0.0495 0.073 Uiso 1 1 calc R . .
C15 C 0.5212(9) 0.9358(5) 0.0270(5) 0.061(2) Uani 1 1 d . . .
H15 H 0.5716 0.9754 0.0554 0.073 Uiso 1 1 calc R . .
C16 C 0.5778(8) 0.8807(5) -0.0093(5) 0.0526(19) Uani 1 1 d . . .
H16 H 0.6680 0.8825 -0.0061 0.063 Uiso 1 1 calc R . .
C17 C 0.5061(6) 0.8178(4) -0.0537(4) 0.0395(16) Uani 1 1 d . . .
C18 C 0.1488(7) 0.7518(6) -0.0887(6) 0.065(2) Uani 1 1 d . . .
H18A H 0.1097 0.8025 -0.1016 0.078 Uiso 1 1 calc R . .
H18B H 0.1018 0.7146 -0.1280 0.078 Uiso 1 1 calc R . .
C19 C 0.2005(7) 0.6690(5) 0.0399(5) 0.052(2) Uani 1 1 d . . .
H19 H 0.2513 0.6328 0.0179 0.063 Uiso 1 1 calc R . .
C20 C 0.0723(8) 0.7702(6) 0.0510(7) 0.068(2) Uani 1 1 d . . .
H20 H 0.0201 0.8138 0.0374 0.081 Uiso 1 1 calc R . .
C21 C 0.0979(8) 0.7335(6) 0.1263(7) 0.066(2) Uani 1 1 d . . .
H21 H 0.0689 0.7482 0.1752 0.080 Uiso 1 1 calc R . .
C22 C 0.2291(9) 0.6157(5) 0.1846(6) 0.064(2) Uani 1 1 d . . .
H22A H 0.1904 0.5648 0.1728 0.077 Uiso 1 1 calc R . .
H22B H 0.2082 0.6339 0.2375 0.077 Uiso 1 1 calc R . .
C23 C 0.3717(8) 0.6110(4) 0.1911(5) 0.0514(19) Uani 1 1 d . . .
C24 C 0.4550(10) 0.6713(5) 0.2245(6) 0.064(2) Uani 1 1 d . . .
H24 H 0.4192 0.7143 0.2466 0.077 Uiso 1 1 calc R . .
C25 C 0.5823(10) 0.6699(5) 0.2261(6) 0.064(2) Uani 1 1 d . . .
H25 H 0.6336 0.7114 0.2494 0.077 Uiso 1 1 calc R . .
C26 C 0.6413(8) 0.6069(4) 0.1932(5) 0.0496(19) Uani 1 1 d . . .
C27 C 0.5664(9) 0.5450(5) 0.1644(6) 0.065(2) Uani 1 1 d . . .
H27 H 0.6049 0.5013 0.1457 0.078 Uiso 1 1 calc R . .
C28 C 0.4308(10) 0.5464(5) 0.1624(6) 0.068(3) Uani 1 1 d . . .
H28 H 0.3801 0.5038 0.1419 0.081 Uiso 1 1 calc R . .
C29 C 0.7823(8) 0.6102(5) 0.1835(6) 0.063(2) Uani 1 1 d . . .
H29A H 0.8287 0.6472 0.2234 0.076 Uiso 1 1 calc R . .
H29B H 0.8222 0.5598 0.1961 0.076 Uiso 1 1 calc R . .
C30 C 0.7399(8) 0.6944(5) 0.0605(5) 0.052(2) Uani 1 1 d . . .
H30 H 0.6925 0.7317 0.0838 0.063 Uiso 1 1 calc R . .
C31 C 0.8460(9) 0.5709(6) 0.4414(6) 0.064(2) Uani 1 1 d . . .
H31 H 0.8753 0.6061 0.4054 0.077 Uiso 1 1 calc R . .
C32 C 0.8513(8) 0.4912(5) 0.4378(6) 0.057(2) Uani 1 1 d . . .
H32 H 0.8891 0.4620 0.4002 0.069 Uiso 1 1 calc R . .
C33 C 0.7628(7) 0.3803(4) 0.5154(5) 0.0458(17) Uani 1 1 d . . .
H33A H 0.8155 0.3637 0.5683 0.055 Uiso 1 1 calc R . .
H33B H 0.7845 0.3480 0.4708 0.055 Uiso 1 1 calc R . .
C34 C 0.6190(6) 0.3717(4) 0.5192(5) 0.0363(15) Uani 1 1 d . . .
C35 C 0.5780(7) 0.3703(4) 0.5965(5) 0.0401(17) Uani 1 1 d . . .
C36 C 0.6653(8) 0.3736(5) 0.6753(5) 0.0527(19) Uani 1 1 d . . .
H36 H 0.7549 0.3767 0.6762 0.063 Uiso 1 1 calc R . .
C37 C 0.6189(9) 0.3722(5) 0.7511(6) 0.061(2) Uani 1 1 d . . .
H37 H 0.6781 0.3732 0.8018 0.073 Uiso 1 1 calc R . .
C38 C 0.4909(9) 0.3695(4) 0.7518(5) 0.053(2) Uani 1 1 d . . .
H38 H 0.4627 0.3689 0.8033 0.064 Uiso 1 1 calc R . .
C39 C 0.4013(9) 0.3674(4) 0.6803(5) 0.0508(19) Uani 1 1 d . . .
H39 H 0.3127 0.3657 0.6830 0.061 Uiso 1 1 calc R . .
C40 C 0.4422(7) 0.3679(4) 0.5991(5) 0.0426(17) Uani 1 1 d . . .
C41 C 0.3491(6) 0.3686(3) 0.5225(5) 0.0375(15) Uani 1 1 d . . .
C42 C 0.3922(7) 0.3695(4) 0.4458(5) 0.0411(16) Uani 1 1 d . . .
C43 C 0.3008(8) 0.3716(5) 0.3680(6) 0.056(2) Uani 1 1 d . . .
H43 H 0.2115 0.3731 0.3685 0.068 Uiso 1 1 calc R . .
C44 C 0.3433(10) 0.3714(6) 0.2948(6) 0.072(3) Uani 1 1 d . . .
H44 H 0.2831 0.3717 0.2445 0.086 Uiso 1 1 calc R . .
C45 C 0.4812(10) 0.3708(5) 0.2926(6) 0.066(2) Uani 1 1 d . . .
H45 H 0.5089 0.3702 0.2410 0.080 Uiso 1 1 calc R . .
C46 C 0.5697(8) 0.3709(4) 0.3638(5) 0.0496(18) Uani 1 1 d . . .
H46 H 0.6583 0.3708 0.3610 0.059 Uiso 1 1 calc R . .
C47 C 0.5306(7) 0.3712(4) 0.4440(5) 0.0376(15) Uani 1 1 d . . .
C48 C 0.2084(7) 0.3739(4) 0.5294(6) 0.053(2) Uani 1 1 d . . .
H48A H 0.1544 0.3586 0.4764 0.064 Uiso 1 1 calc R . .
H48B H 0.1906 0.3388 0.5729 0.064 Uiso 1 1 calc R . .
C49 C 0.1031(7) 0.4771(6) 0.6076(6) 0.058(2) Uani 1 1 d . . .
H49 H 0.0599 0.4445 0.6393 0.070 Uiso 1 1 calc R . .
C50 C 0.1035(7) 0.5524(5) 0.6110(5) 0.054(2) Uani 1 1 d . . .
H50 H 0.0634 0.5833 0.6460 0.064 Uiso 1 1 calc R . .
C51 C 0.2177(8) 0.5185(5) 0.5203(6) 0.056(2) Uani 1 1 d . . .
H51 H 0.2719 0.5206 0.4804 0.067 Uiso 1 1 calc R . .
C52 C 0.2071(9) 0.6589(5) 0.5331(7) 0.066(3) Uani 1 1 d . . .
H52A H 0.1587 0.6728 0.4780 0.079 Uiso 1 1 calc R . .
H52B H 0.1803 0.6936 0.5741 0.079 Uiso 1 1 calc R . .
C53 C 0.3485(9) 0.6689(4) 0.5341(6) 0.055(2) Uani 1 1 d . . .
C54 C 0.4329(9) 0.6753(5) 0.6059(6) 0.055(2) Uani 1 1 d . . .
H54 H 0.4025 0.6792 0.6564 0.066 Uiso 1 1 calc R . .
C55 C 0.5695(9) 0.6761(4) 0.6062(6) 0.057(2) Uani 1 1 d . . .
H55 H 0.6283 0.6802 0.6568 0.068 Uiso 1 1 calc R . .
C56 C 0.6144(8) 0.6709(4) 0.5320(6) 0.050(2) Uani 1 1 d . . .
C57 C 0.5280(9) 0.6664(5) 0.4604(6) 0.061(2) Uani 1 1 d . . .
H57 H 0.5581 0.6630 0.4096 0.073 Uiso 1 1 calc R . .
C58 C 0.3956(9) 0.6667(5) 0.4595(6) 0.057(2) Uani 1 1 d . . .
H58 H 0.3375 0.6654 0.4084 0.068 Uiso 1 1 calc R . .
C59 C 0.7567(9) 0.6654(5) 0.5336(7) 0.066(2) Uani 1 1 d . . .
H59A H 0.7826 0.7036 0.4957 0.079 Uiso 1 1 calc R . .
H59B H 0.8039 0.6761 0.5900 0.079 Uiso 1 1 calc R . .
C60 C 0.7567(7) 0.5212(5) 0.5417(5) 0.0476(17) Uani 1 1 d . . .
H60 H 0.7158 0.5173 0.5883 0.057 Uiso 1 1 calc R . .
N1 N 0.7642(5) 0.6946(3) -0.0185(4) 0.0411(14) Uani 1 1 d . . .
N2 N 0.7942(6) 0.6328(4) 0.0988(4) 0.0495(15) Uani 1 1 d . . .
N3 N 0.1395(6) 0.7298(5) -0.0017(5) 0.0630(19) Uani 1 1 d . . .
N4 N 0.1762(7) 0.6693(4) 0.1169(5) 0.0623(19) Uani 1 1 d . . .
N5 N 0.7912(6) 0.4635(4) 0.4991(4) 0.0429(14) Uani 1 1 d . . .
N6 N 0.7897(6) 0.5872(4) 0.5077(4) 0.0493(15) Uani 1 1 d . . .
N7 N 0.1757(5) 0.4539(3) 0.5503(4) 0.0431(14) Uani 1 1 d . . .
N8 N 0.1745(6) 0.5767(4) 0.5531(4) 0.0510(16) Uani 1 1 d . . .
Br1 Br 0.06502(10) 0.79952(6) 0.65992(7) 0.0773(3) Uani 1 1 d . . .
Br2 Br 0.98150(9) 0.75046(5) 0.34031(6) 0.0649(3) Uani 1 1 d . . .
Br3 Br 0.08653(10) 0.43127(6) 0.07572(8) 0.0845(4) Uani 1 1 d . . .
Br4 Br 0.8823(2) 0.53351(17) 0.75928(13) 0.1138(8) Uani 0.702(3) 1 d P . .
Br4' Br 0.8833(6) 0.5892(4) 0.7657(3) 0.1138(8) Uani 0.297(3) 1 d P . .
O1 O 0.8073(10) 0.8351(7) 0.1753(7) 0.130(3) Uani 1 1 d . . .
O2 O 0.9762(11) 0.4609(5) 0.2440(7) 0.128(4) Uani 1 1 d . . .
O3 O 0.1073(9) 0.5684(6) 0.3463(5) 0.114(3) Uani 1 1 d . . .
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 0.037(4) 0.050(5) 0.085(7) -0.016(5) 0.011(4) 0.007(3)
C2 0.041(4) 0.062(5) 0.063(6) -0.006(4) 0.017(4) 0.009(4)
C3 0.050(4) 0.053(4) 0.060(5) 0.003(4) 0.022(4) -0.005(4)
C4 0.045(4) 0.045(4) 0.031(3) 0.014(3) 0.011(3) -0.001(3)
C5 0.045(4) 0.048(4) 0.036(4) 0.014(3) 0.005(3) 0.001(3)
C6 0.057(5) 0.059(5) 0.040(5) 0.000(4) 0.001(4) 0.006(4)
C7 0.092(7) 0.057(5) 0.052(5) 0.008(5) 0.005(5) 0.005(5)
C8 0.094(8) 0.060(6) 0.054(6) -0.011(5) -0.007(5) -0.016(5)
C9 0.058(5) 0.073(6) 0.063(6) 0.021(5) -0.017(4) -0.021(5)
C10 0.047(4) 0.062(5) 0.029(4) 0.009(3) 0.000(3) 0.000(4)
C11 0.030(3) 0.074(5) 0.044(4) 0.013(4) 0.007(3) -0.001(4)
C12 0.037(4) 0.055(5) 0.045(4) 0.012(4) 0.005(3) 0.010(3)
C13 0.042(4) 0.076(6) 0.066(6) 0.017(5) 0.021(4) 0.015(4)
C14 0.068(6) 0.059(5) 0.059(6) -0.002(4) 0.019(4) 0.019(4)
C15 0.077(6) 0.054(5) 0.051(5) -0.013(4) 0.011(4) -0.002(4)
C16 0.053(5) 0.055(4) 0.047(5) 0.005(4) 0.000(4) -0.003(4)
C17 0.035(4) 0.053(4) 0.028(4) 0.010(3) -0.001(3) 0.002(3)
C18 0.033(4) 0.092(6) 0.070(6) 0.011(5) 0.007(4) 0.001(4)
C19 0.041(4) 0.066(5) 0.054(5) 0.017(4) 0.020(4) 0.010(4)
C20 0.043(5) 0.076(6) 0.084(7) 0.006(5) 0.014(4) -0.008(4)
C21 0.047(5) 0.076(6) 0.077(7) -0.016(5) 0.016(4) -0.007(4)
C22 0.075(6) 0.067(5) 0.059(6) 0.002(4) 0.035(4) -0.018(4)
C23 0.075(5) 0.043(4) 0.039(4) 0.009(3) 0.016(4) -0.009(4)
C24 0.076(6) 0.044(5) 0.077(7) -0.002(4) 0.028(5) -0.001(4)
C25 0.084(7) 0.042(4) 0.063(6) -0.012(4) 0.002(5) -0.010(4)
C26 0.066(5) 0.047(4) 0.030(4) 0.007(3) -0.007(3) 0.010(4)
C27 0.074(7) 0.055(6) 0.064(6) -0.008(4) 0.007(5) -0.001(4)
C28 0.074(7) 0.055(5) 0.077(6) -0.010(4) 0.019(5) -0.022(4)
C29 0.068(6) 0.062(5) 0.051(5) 0.001(4) -0.012(4) 0.013(4)
C30 0.053(5) 0.048(4) 0.053(5) -0.005(4) 0.001(4) 0.018(4)
C31 0.063(5) 0.084(7) 0.054(5) 0.007(5) 0.029(4) -0.027(5)
C32 0.064(5) 0.057(5) 0.057(5) 0.009(4) 0.031(4) 0.003(4)
C33 0.046(4) 0.038(4) 0.054(5) 0.001(3) 0.011(3) 0.013(3)
C34 0.041(4) 0.025(3) 0.046(4) 0.001(3) 0.018(3) 0.004(3)
C35 0.047(4) 0.021(3) 0.052(5) 0.003(3) 0.008(3) 0.002(3)
C36 0.065(5) 0.049(4) 0.043(5) 0.006(4) 0.006(4) 0.004(4)
C37 0.070(6) 0.057(5) 0.050(5) -0.008(4) -0.005(4) 0.004(4)
C38 0.076(6) 0.045(4) 0.044(5) -0.003(4) 0.025(4) 0.006(4)
C39 0.069(5) 0.036(4) 0.053(5) -0.003(4) 0.025(4) -0.005(3)
C40 0.062(5) 0.020(3) 0.051(5) 0.001(3) 0.025(4) 0.001(3)
C41 0.044(4) 0.019(3) 0.049(4) 0.004(3) 0.007(3) -0.002(3)
C42 0.046(4) 0.031(3) 0.046(4) 0.002(3) 0.008(3) 0.002(3)
C43 0.053(5) 0.054(5) 0.056(5) 0.005(4) -0.005(4) -0.008(4)
C44 0.078(6) 0.089(7) 0.046(5) 0.000(5) 0.004(5) -0.003(5)
C45 0.086(7) 0.067(5) 0.049(5) 0.000(4) 0.019(5) 0.001(5)
C46 0.055(4) 0.050(4) 0.046(5) -0.005(4) 0.015(4) 0.000(3)
C47 0.048(4) 0.026(3) 0.040(4) -0.001(3) 0.009(3) 0.001(3)
C48 0.048(4) 0.045(4) 0.072(6) -0.005(4) 0.026(4) -0.012(3)
C49 0.030(4) 0.082(7) 0.062(6) 0.000(5) 0.005(4) -0.001(4)
C50 0.028(4) 0.075(6) 0.060(5) -0.011(4) 0.012(3) 0.008(3)
C51 0.050(5) 0.058(5) 0.066(5) -0.005(5) 0.032(4) 0.002(4)
C52 0.066(6) 0.042(4) 0.088(7) -0.005(4) 0.011(5) 0.022(4)
C53 0.072(6) 0.029(4) 0.064(6) 0.004(4) 0.010(5) 0.014(3)
C54 0.067(5) 0.050(5) 0.049(5) 0.011(4) 0.016(4) -0.002(4)
C55 0.080(6) 0.036(4) 0.053(5) -0.008(4) 0.009(4) -0.010(4)
C56 0.068(5) 0.022(3) 0.062(6) 0.000(3) 0.016(4) -0.006(3)
C57 0.077(7) 0.060(5) 0.043(5) 0.004(4) 0.005(4) -0.001(4)
C58 0.070(6) 0.055(5) 0.040(5) 0.003(4) -0.005(4) 0.004(4)
C59 0.078(6) 0.041(4) 0.080(7) 0.001(4) 0.021(5) -0.023(4)
C60 0.049(5) 0.045(4) 0.053(4) 0.001(4) 0.020(4) -0.005(3)
N1 0.032(3) 0.045(3) 0.048(4) -0.003(3) 0.012(3) 0.002(2)
N2 0.040(3) 0.051(4) 0.055(4) 0.001(3) 0.003(3) 0.007(3)
N3 0.037(3) 0.087(5) 0.069(5) -0.003(4) 0.019(3) -0.006(3)
N4 0.053(4) 0.067(4) 0.073(5) 0.007(4) 0.030(4) -0.013(3)
N5 0.038(3) 0.051(4) 0.043(4) 0.007(3) 0.014(3) -0.001(3)
N6 0.048(4) 0.044(3) 0.058(4) 0.005(3) 0.015(3) -0.008(3)
N7 0.032(3) 0.045(3) 0.055(4) 0.008(3) 0.015(3) 0.009(2)
N8 0.040(3) 0.054(4) 0.060(4) 0.003(3) 0.010(3) 0.025(3)
Br1 0.0776(6) 0.0726(6) 0.0934(8) 0.0035(5) 0.0470(5) 0.0109(5)
Br2 0.0723(6) 0.0613(5) 0.0601(5) -0.0073(4) 0.0095(4) -0.0054(4)
Br3 0.0592(5) 0.0739(6) 0.1133(9) -0.0186(6) -0.0028(5) 0.0201(4)
Br4 0.1354(14) 0.136(2) 0.0800(10) -0.0253(14) 0.0467(10) -0.0574(16)
Br4' 0.1354(14) 0.136(2) 0.0800(10) -0.0253(14) 0.0467(10) -0.0574(16)
O1 0.129(8) 0.141(8) 0.110(7) -0.011(6) -0.001(6) 0.011(6)
O2 0.180(10) 0.092(6) 0.129(8) 0.018(5) 0.071(7) 0.044(6)
O3 0.111(6) 0.147(7) 0.093(6) 0.016(6) 0.044(5) 0.002(6)
_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 N2 1.353(10) . ?
C1 C2 1.366(13) . ?
C1 H1 0.9300 . ?
C2 N1 1.354(10) . ?
C2 H2 0.9300 . ?
C3 N1 1.464(10) . ?
C3 C4 1.512(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.385(11) . ?
C4 C17 1.412(10) . ?
C5 C6 1.431(11) . ?
C5 C10 1.436(10) . ?
C6 C7 1.341(13) . ?
C6 H6 0.9300 . ?
C7 C8 1.395(15) . ?
C7 H7 0.9300 . ?
C8 C9 1.341(15) . ?
C8 H8 0.9300 . ?
C9 C10 1.441(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.345(11) . ?
C11 C12 1.441(12) . ?
C11 C18 1.539(10) . ?
C12 C13 1.378(12) . ?
C12 C17 1.448(10) . ?
C13 C14 1.325(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.405(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.311(12) . ?
C15 H15 0.9300 . ?
C16 C17 1.432(11) . ?
C16 H16 0.9300 . ?
C18 N3 1.475(12) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N4 1.313(11) . ?
C19 N3 1.341(11) . ?
C19 H19 0.9300 . ?
C20 C21 1.354(14) . ?
C20 N3 1.383(12) . ?
C20 H20 0.9300 . ?
C21 N4 1.399(12) . ?
C21 H21 0.9300 . ?
C22 N4 1.460(12) . ?
C22 C23 1.469(13) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C28 1.391(12) . ?
C23 C24 1.399(12) . ?
C24 C25 1.319(14) . ?
C24 H24 0.9300 . ?
C25 C26 1.398(12) . ?
C25 H25 0.9300 . ?
C26 C27 1.353(12) . ?
C26 C29 1.504(13) . ?
C27 C28 1.404(13) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 N2 1.448(12) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N2 1.305(10) . ?
C30 N1 1.344(10) . ?
C30 H30 0.9300 . ?
C31 N6 1.339(11) . ?
C31 C32 1.378(13) . ?
C31 H31 0.9300 . ?
C32 N5 1.350(10) . ?
C32 H32 0.9300 . ?
C33 N5 1.500(9) . ?
C33 C34 1.514(10) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C47 1.383(10) . ?
C34 C35 1.390(10) . ?
C35 C36 1.422(11) . ?
C35 C40 1.421(10) . ?
C36 C37 1.394(12) . ?
C36 H36 0.9300 . ?
C37 C38 1.335(13) . ?
C37 H37 0.9300 . ?
C38 C39 1.344(12) . ?
C38 H38 0.9300 . ?
C39 C40 1.450(11) . ?
C39 H39 0.9300 . ?
C40 C41 1.426(11) . ?
C41 C42 1.391(10) . ?
C41 C48 1.490(10) . ?
C42 C43 1.430(11) . ?
C42 C47 1.444(10) . ?
C43 C44 1.335(13) . ?
C43 H43 0.9300 . ?
C44 C45 1.440(14) . ?
C44 H44 0.9300 . ?
C45 C46 1.335(12) . ?
C45 H45 0.9300 . ?
C46 C47 1.425(11) . ?
C46 H46 0.9300 . ?
C48 N7 1.475(10) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 C50 1.299(12) . ?
C49 N7 1.357(11) . ?
C49 H49 0.9300 . ?
C50 N8 1.357(11) . ?
C50 H50 0.9300 . ?
C51 N8 1.256(10) . ?
C51 N7 1.320(11) . ?
C51 H51 0.9300 . ?
C52 C53 1.477(13) . ?
C52 N8 1.507(11) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 C54 1.325(12) . ?
C53 C58 1.380(13) . ?
C54 C55 1.419(13) . ?
C54 H54 0.9300 . ?
C55 C56 1.365(13) . ?
C55 H55 0.9300 . ?
C56 C57 1.331(12) . ?
C56 C59 1.478(13) . ?
C57 C58 1.374(13) . ?
C57 H57 0.9300 . ?
C58 H58 0.9300 . ?
C59 N6 1.472(11) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 N5 1.297(10) . ?
C60 N6 1.337(10) . ?
C60 H60 0.9300 . ?
Br4 Br4' 0.967(6) . ?
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
N2 C1 C2 106.6(7) . . ?
N2 C1 H1 126.7 . . ?
C2 C1 H1 126.7 . . ?
N1 C2 C1 106.9(7) . . ?
N1 C2 H2 126.6 . . ?
C1 C2 H2 126.6 . . ?
N1 C3 C4 110.2(6) . . ?
N1 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C17 120.9(6) . . ?
C5 C4 C3 118.9(7) . . ?
C17 C4 C3 120.2(7) . . ?
C4 C5 C6 122.0(7) . . ?
C4 C5 C10 120.0(7) . . ?
C6 C5 C10 117.7(7) . . ?
C7 C6 C5 122.4(8) . . ?
C7 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C6 C7 C8 119.6(9) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C9 C8 C7 121.8(8) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C10 121.2(9) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C11 C10 C5 119.3(7) . . ?
C11 C10 C9 123.4(8) . . ?
C5 C10 C9 117.3(8) . . ?
C10 C11 C12 123.4(6) . . ?
C10 C11 C18 121.8(8) . . ?
C12 C11 C18 114.4(7) . . ?
C13 C12 C11 125.5(7) . . ?
C13 C12 C17 118.1(7) . . ?
C11 C12 C17 116.4(6) . . ?
C14 C13 C12 123.5(8) . . ?
C14 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
C13 C14 C15 119.4(8) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C16 C15 C14 120.6(8) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 122.5(8) . . ?
C15 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
C4 C17 C16 124.3(6) . . ?
C4 C17 C12 119.8(6) . . ?
C16 C17 C12 115.9(7) . . ?
N3 C18 C11 109.1(6) . . ?
N3 C18 H18A 109.9 . . ?
C11 C18 H18A 109.9 . . ?
N3 C18 H18B 109.9 . . ?
C11 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
N4 C19 N3 108.4(7) . . ?
N4 C19 H19 125.8 . . ?
N3 C19 H19 125.8 . . ?
C21 C20 N3 106.1(9) . . ?
C21 C20 H20 127.0 . . ?
N3 C20 H20 127.0 . . ?
C20 C21 N4 107.3(8) . . ?
C20 C21 H21 126.4 . . ?
N4 C21 H21 126.4 . . ?
N4 C22 C23 109.0(6) . . ?
N4 C22 H22A 109.9 . . ?
C23 C22 H22A 109.9 . . ?
N4 C22 H22B 109.9 . . ?
C23 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C28 C23 C24 116.4(8) . . ?
C28 C23 C22 121.5(8) . . ?
C24 C23 C22 122.1(8) . . ?
C25 C24 C23 122.8(8) . . ?
C25 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
C24 C25 C26 121.0(8) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C27 C26 C25 118.6(8) . . ?
C27 C26 C29 120.3(8) . . ?
C25 C26 C29 120.9(8) . . ?
C26 C27 C28 120.5(8) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C23 C28 C27 120.5(8) . . ?
C23 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
N2 C29 C26 111.1(6) . . ?
N2 C29 H29A 109.4 . . ?
C26 C29 H29A 109.4 . . ?
N2 C29 H29B 109.4 . . ?
C26 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
N2 C30 N1 108.2(7) . . ?
N2 C30 H30 125.9 . . ?
N1 C30 H30 125.9 . . ?
N6 C31 C32 105.7(7) . . ?
N6 C31 H31 127.2 . . ?
C32 C31 H31 127.2 . . ?
N5 C32 C31 107.2(8) . . ?
N5 C32 H32 126.4 . . ?
C31 C32 H32 126.4 . . ?
N5 C33 C34 109.1(5) . . ?
N5 C33 H33A 109.9 . . ?
C34 C33 H33A 109.9 . . ?
N5 C33 H33B 109.9 . . ?
C34 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
C47 C34 C35 121.7(6) . . ?
C47 C34 C33 117.9(6) . . ?
C35 C34 C33 120.3(7) . . ?
C34 C35 C36 123.5(7) . . ?
C34 C35 C40 119.7(7) . . ?
C36 C35 C40 116.8(7) . . ?
C37 C36 C35 121.2(8) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C38 C37 C36 120.9(8) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C37 C38 C39 122.0(8) . . ?
C37 C38 H38 119.0 . . ?
C39 C38 H38 119.0 . . ?
C38 C39 C40 120.2(8) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C35 C40 C41 119.7(7) . . ?
C35 C40 C39 119.0(7) . . ?
C41 C40 C39 121.3(7) . . ?
C42 C41 C40 119.6(6) . . ?
C42 C41 C48 123.1(7) . . ?
C40 C41 C48 117.1(7) . . ?
C41 C42 C43 120.7(7) . . ?
C41 C42 C47 120.1(6) . . ?
C43 C42 C47 119.1(7) . . ?
C44 C43 C42 120.2(8) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 120.8(9) . . ?
C43 C44 H44 119.6 . . ?
C45 C44 H44 119.6 . . ?
C46 C45 C44 120.8(9) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C47 121.0(8) . . ?
C45 C46 H46 119.5 . . ?
C47 C46 H46 119.5 . . ?
C34 C47 C46 122.9(6) . . ?
C34 C47 C42 119.1(7) . . ?
C46 C47 C42 117.9(7) . . ?
N7 C48 C41 110.2(6) . . ?
N7 C48 H48A 109.6 . . ?
C41 C48 H48A 109.6 . . ?
N7 C48 H48B 109.6 . . ?
C41 C48 H48B 109.6 . . ?
H48A C48 H48B 108.1 . . ?
C50 C49 N7 109.0(8) . . ?
C50 C49 H49 125.5 . . ?
N7 C49 H49 125.5 . . ?
C49 C50 N8 106.1(7) . . ?
C49 C50 H50 126.9 . . ?
N8 C50 H50 126.9 . . ?
N8 C51 N7 110.7(7) . . ?
N8 C51 H51 124.7 . . ?
N7 C51 H51 124.7 . . ?
C53 C52 N8 111.8(6) . . ?
C53 C52 H52A 109.3 . . ?
N8 C52 H52A 109.3 . . ?
C53 C52 H52B 109.3 . . ?
N8 C52 H52B 109.3 . . ?
H52A C52 H52B 107.9 . . ?
C54 C53 C58 118.8(9) . . ?
C54 C53 C52 121.2(9) . . ?
C58 C53 C52 119.9(9) . . ?
C53 C54 C55 120.5(9) . . ?
C53 C54 H54 119.8 . . ?
C55 C54 H54 119.8 . . ?
C56 C55 C54 119.9(9) . . ?
C56 C55 H55 120.1 . . ?
C54 C55 H55 120.1 . . ?
C57 C56 C55 118.8(9) . . ?
C57 C56 C59 121.7(9) . . ?
C55 C56 C59 119.4(9) . . ?
C56 C57 C58 121.6(9) . . ?
C56 C57 H57 119.2 . . ?
C58 C57 H57 119.2 . . ?
C57 C58 C53 120.4(8) . . ?
C57 C58 H58 119.8 . . ?
C53 C58 H58 119.8 . . ?
N6 C59 C56 109.8(6) . . ?
N6 C59 H59A 109.7 . . ?
C56 C59 H59A 109.7 . . ?
N6 C59 H59B 109.7 . . ?
C56 C59 H59B 109.7 . . ?
H59A C59 H59B 108.2 . . ?
N5 C60 N6 108.6(6) . . ?
N5 C60 H60 125.7 . . ?
N6 C60 H60 125.7 . . ?
C30 N1 C2 108.4(7) . . ?
C30 N1 C3 124.3(6) . . ?
C2 N1 C3 127.3(7) . . ?
C30 N2 C1 109.9(8) . . ?
C30 N2 C29 124.3(7) . . ?
C1 N2 C29 125.9(7) . . ?
C19 N3 C20 109.5(8) . . ?
C19 N3 C18 124.8(7) . . ?
C20 N3 C18 125.7(8) . . ?
C19 N4 C21 108.7(8) . . ?
C19 N4 C22 126.5(7) . . ?
C21 N4 C22 124.6(8) . . ?
C60 N5 C32 109.1(7) . . ?
C60 N5 C33 124.0(6) . . ?
C32 N5 C33 126.9(7) . . ?
C60 N6 C31 109.4(7) . . ?
C60 N6 C59 125.0(7) . . ?
C31 N6 C59 125.3(7) . . ?
C51 N7 C49 105.2(7) . . ?
C51 N7 C48 126.9(6) . . ?
C49 N7 C48 127.8(7) . . ?
C51 N8 C50 108.9(7) . . ?
C51 N8 C52 123.4(7) . . ?
C50 N8 C52 127.6(7) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N1 -1.0(9) . . . . ?
N1 C3 C4 C5 -75.5(8) . . . . ?
N1 C3 C4 C17 101.6(7) . . . . ?
C17 C4 C5 C6 -179.4(7) . . . . ?
C3 C4 C5 C6 -2.3(10) . . . . ?
C17 C4 C5 C10 -4.2(10) . . . . ?
C3 C4 C5 C10 172.9(6) . . . . ?
C4 C5 C6 C7 174.6(8) . . . . ?
C10 C5 C6 C7 -0.7(11) . . . . ?
C5 C6 C7 C8 1.1(14) . . . . ?
C6 C7 C8 C9 -1.3(15) . . . . ?
C7 C8 C9 C10 1.0(15) . . . . ?
C4 C5 C10 C11 4.0(10) . . . . ?
C6 C5 C10 C11 179.4(7) . . . . ?
C4 C5 C10 C9 -175.0(7) . . . . ?
C6 C5 C10 C9 0.4(10) . . . . ?
C8 C9 C10 C11 -179.5(8) . . . . ?
C8 C9 C10 C5 -0.5(12) . . . . ?
C5 C10 C11 C12 -1.5(11) . . . . ?
C9 C10 C11 C12 177.4(7) . . . . ?
C5 C10 C11 C18 -174.5(7) . . . . ?
C9 C10 C11 C18 4.5(12) . . . . ?
C10 C11 C12 C13 -179.1(8) . . . . ?
C18 C11 C12 C13 -5.7(11) . . . . ?
C10 C11 C12 C17 -0.7(11) . . . . ?
C18 C11 C12 C17 172.7(6) . . . . ?
C11 C12 C13 C14 176.2(8) . . . . ?
C17 C12 C13 C14 -2.1(12) . . . . ?
C12 C13 C14 C15 1.7(13) . . . . ?
C13 C14 C15 C16 -0.5(13) . . . . ?
C14 C15 C16 C17 -0.3(13) . . . . ?
C5 C4 C17 C16 179.6(7) . . . . ?
C3 C4 C17 C16 2.6(10) . . . . ?
C5 C4 C17 C12 1.9(10) . . . . ?
C3 C4 C17 C12 -175.1(6) . . . . ?
C15 C16 C17 C4 -177.8(7) . . . . ?
C15 C16 C17 C12 -0.1(11) . . . . ?
C13 C12 C17 C4 179.1(7) . . . . ?
C11 C12 C17 C4 0.6(10) . . . . ?
C13 C12 C17 C16 1.2(10) . . . . ?
C11 C12 C17 C16 -177.3(7) . . . . ?
C10 C11 C18 N3 100.8(9) . . . . ?
C12 C11 C18 N3 -72.8(9) . . . . ?
N3 C20 C21 N4 -2.4(9) . . . . ?
N4 C22 C23 C28 -105.6(9) . . . . ?
N4 C22 C23 C24 73.1(10) . . . . ?
C28 C23 C24 C25 2.9(13) . . . . ?
C22 C23 C24 C25 -175.8(9) . . . . ?
C23 C24 C25 C26 0.4(15) . . . . ?
C24 C25 C26 C27 -4.1(13) . . . . ?
C24 C25 C26 C29 171.1(9) . . . . ?
C25 C26 C27 C28 4.2(13) . . . . ?
C29 C26 C27 C28 -171.0(8) . . . . ?
C24 C23 C28 C27 -2.7(13) . . . . ?
C22 C23 C28 C27 176.0(9) . . . . ?
C26 C27 C28 C23 -0.8(14) . . . . ?
C27 C26 C29 N2 79.2(9) . . . . ?
C25 C26 C29 N2 -95.9(9) . . . . ?
N6 C31 C32 N5 3.5(10) . . . . ?
N5 C33 C34 C47 77.5(8) . . . . ?
N5 C33 C34 C35 -97.9(7) . . . . ?
C47 C34 C35 C36 -177.7(7) . . . . ?
C33 C34 C35 C36 -2.4(10) . . . . ?
C47 C34 C35 C40 0.2(9) . . . . ?
C33 C34 C35 C40 175.4(6) . . . . ?
C34 C35 C36 C37 179.8(7) . . . . ?
C40 C35 C36 C37 1.9(11) . . . . ?
C35 C36 C37 C38 -1.5(12) . . . . ?
C36 C37 C38 C39 0.4(13) . . . . ?
C37 C38 C39 C40 0.2(12) . . . . ?
C34 C35 C40 C41 -1.2(9) . . . . ?
C36 C35 C40 C41 176.8(6) . . . . ?
C34 C35 C40 C39 -179.2(6) . . . . ?
C36 C35 C40 C39 -1.3(9) . . . . ?
C38 C39 C40 C35 0.3(10) . . . . ?
C38 C39 C40 C41 -177.7(6) . . . . ?
C35 C40 C41 C42 1.7(9) . . . . ?
C39 C40 C41 C42 179.6(6) . . . . ?
C35 C40 C41 C48 -174.1(5) . . . . ?
C39 C40 C41 C48 3.8(9) . . . . ?
C40 C41 C42 C43 -178.9(6) . . . . ?
C48 C41 C42 C43 -3.3(10) . . . . ?
C40 C41 C42 C47 -1.1(9) . . . . ?
C48 C41 C42 C47 174.5(6) . . . . ?
C41 C42 C43 C44 -179.1(8) . . . . ?
C47 C42 C43 C44 3.1(11) . . . . ?
C42 C43 C44 C45 -1.3(14) . . . . ?
C43 C44 C45 C46 -0.5(15) . . . . ?
C44 C45 C46 C47 0.5(13) . . . . ?
C35 C34 C47 C46 -178.6(6) . . . . ?
C33 C34 C47 C46 6.1(10) . . . . ?
C35 C34 C47 C42 0.4(9) . . . . ?
C33 C34 C47 C42 -174.9(6) . . . . ?
C45 C46 C47 C34 -179.7(8) . . . . ?
C45 C46 C47 C42 1.3(11) . . . . ?
C41 C42 C47 C34 0.1(9) . . . . ?
C43 C42 C47 C34 177.9(6) . . . . ?
C41 C42 C47 C46 179.1(6) . . . . ?
C43 C42 C47 C46 -3.1(9) . . . . ?
C42 C41 C48 N7 -99.5(8) . . . . ?
C40 C41 C48 N7 76.2(8) . . . . ?
N7 C49 C50 N8 1.7(9) . . . . ?
N8 C52 C53 C54 -78.2(10) . . . . ?
N8 C52 C53 C58 97.5(10) . . . . ?
C58 C53 C54 C55 -2.9(11) . . . . ?
C52 C53 C54 C55 172.9(7) . . . . ?
C53 C54 C55 C56 0.4(11) . . . . ?
C54 C55 C56 C57 1.1(11) . . . . ?
C54 C55 C56 C59 -175.0(7) . . . . ?
C55 C56 C57 C58 -0.2(12) . . . . ?
C59 C56 C57 C58 175.9(7) . . . . ?
C56 C57 C58 C53 -2.4(13) . . . . ?
C54 C53 C58 C57 3.8(12) . . . . ?
C52 C53 C58 C57 -172.0(7) . . . . ?
C57 C56 C59 N6 -66.2(10) . . . . ?
C55 C56 C59 N6 109.9(8) . . . . ?
N2 C30 N1 C2 -3.4(8) . . . . ?
N2 C30 N1 C3 175.1(6) . . . . ?
C1 C2 N1 C30 2.7(8) . . . . ?
C1 C2 N1 C3 -175.8(7) . . . . ?
C4 C3 N1 C30 -52.4(10) . . . . ?
C4 C3 N1 C2 125.8(7) . . . . ?
N1 C30 N2 C1 2.8(9) . . . . ?
N1 C30 N2 C29 -176.1(7) . . . . ?
C2 C1 N2 C30 -1.2(9) . . . . ?
C2 C1 N2 C29 177.8(7) . . . . ?
C26 C29 N2 C30 52.6(10) . . . . ?
C26 C29 N2 C1 -126.2(8) . . . . ?
N4 C19 N3 C20 -0.6(9) . . . . ?
N4 C19 N3 C18 176.6(7) . . . . ?
C21 C20 N3 C19 1.9(10) . . . . ?
C21 C20 N3 C18 -175.2(8) . . . . ?
C11 C18 N3 C19 -49.3(12) . . . . ?
C11 C18 N3 C20 127.4(9) . . . . ?
N3 C19 N4 C21 -0.9(9) . . . . ?
N3 C19 N4 C22 -176.5(7) . . . . ?
C20 C21 N4 C19 2.1(9) . . . . ?
C20 C21 N4 C22 177.8(7) . . . . ?
C23 C22 N4 C19 49.6(11) . . . . ?
C23 C22 N4 C21 -125.4(8) . . . . ?
N6 C60 N5 C32 1.9(9) . . . . ?
N6 C60 N5 C33 -176.2(7) . . . . ?
C31 C32 N5 C60 -3.4(10) . . . . ?
C31 C32 N5 C33 174.7(7) . . . . ?
C34 C33 N5 C60 50.3(10) . . . . ?
C34 C33 N5 C32 -127.5(8) . . . . ?
N5 C60 N6 C31 0.4(9) . . . . ?
N5 C60 N6 C59 174.4(8) . . . . ?
C32 C31 N6 C60 -2.4(10) . . . . ?
C32 C31 N6 C59 -176.4(8) . . . . ?
C56 C59 N6 C60 -53.0(11) . . . . ?
C56 C59 N6 C31 120.1(9) . . . . ?
N8 C51 N7 C49 -1.4(9) . . . . ?
N8 C51 N7 C48 -177.9(7) . . . . ?
C50 C49 N7 C51 -0.3(9) . . . . ?
C50 C49 N7 C48 176.1(8) . . . . ?
C41 C48 N7 C51 39.7(11) . . . . ?
C41 C48 N7 C49 -136.0(8) . . . . ?
N7 C51 N8 C50 2.6(10) . . . . ?
N7 C51 N8 C52 178.8(8) . . . . ?
C49 C50 N8 C51 -2.6(9) . . . . ?
C49 C50 N8 C52 -178.7(8) . . . . ?
C53 C52 N8 C51 -46.1(12) . . . . ?
C53 C52 N8 C50 129.4(9) . . . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.804
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.102