# 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,   
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data_110520d
_database_code_depnum_ccdc_archive 'CCDC 895105'
#TrackingRef '4q.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H24 N2 O'
_chemical_formula_weight         404.49
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'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   8.0693(8)
_cell_length_b                   14.7370(13)
_cell_length_c                   18.6512(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.6200(10)
_cell_angle_gamma                90.00
_cell_volume                     2213.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2921
_cell_measurement_theta_min      2.589
_cell_measurement_theta_max      23.384
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9640
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10918
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3908
_reflns_number_gt                2523
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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.
;
_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^)+(0.0577P)^2^+0.7176P] 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         3908
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1461
_refine_ls_wR_factor_gt          0.1154
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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
N1 N 0.3134(2) 0.62912(12) 0.60564(10) 0.0369(5) Uani 1 1 d . . .
N2 N 0.8343(3) 0.69783(14) 0.82263(11) 0.0503(6) Uani 1 1 d . . .
H2 H 0.9070 0.7366 0.8389 0.060 Uiso 1 1 calc R . .
O1 O 0.5407(2) 0.37301(11) 0.62207(10) 0.0530(5) Uani 1 1 d . . .
C1 C 0.4110(3) 0.67057(15) 0.66045(12) 0.0370(5) Uani 1 1 d . . .
C2 C 0.5298(3) 0.61017(14) 0.68507(12) 0.0366(5) Uani 1 1 d . . .
C3 C 0.5026(3) 0.52771(14) 0.64397(12) 0.0349(5) Uani 1 1 d . . .
C4 C 0.3665(3) 0.54219(15) 0.59609(12) 0.0373(5) Uani 1 1 d . . .
C5 C 0.2834(3) 0.48213(16) 0.54064(14) 0.0497(7) Uani 1 1 d . . .
H5A H 0.1970 0.4483 0.5616 0.074 Uiso 1 1 calc R . .
H5B H 0.3633 0.4410 0.5228 0.074 Uiso 1 1 calc R . .
H5C H 0.2362 0.5184 0.5018 0.074 Uiso 1 1 calc R . .
C6 C 0.1681(3) 0.66822(14) 0.56907(12) 0.0364(5) Uani 1 1 d . . .
C7 C 0.0217(3) 0.67110(18) 0.60272(14) 0.0528(7) Uani 1 1 d . . .
H7 H 0.0167 0.6487 0.6491 0.063 Uiso 1 1 calc R . .
C8 C -0.1178(3) 0.7075(2) 0.56707(16) 0.0598(8) Uani 1 1 d . . .
H8 H -0.2169 0.7089 0.5900 0.072 Uiso 1 1 calc R . .
C9 C -0.1146(3) 0.74165(16) 0.49859(15) 0.0487(7) Uani 1 1 d . . .
C10 C 0.0330(3) 0.73746(18) 0.46574(15) 0.0553(7) Uani 1 1 d . . .
H10 H 0.0381 0.7594 0.4192 0.066 Uiso 1 1 calc R . .
C11 C 0.1744(3) 0.70114(17) 0.50083(13) 0.0483(6) Uani 1 1 d . . .
H11 H 0.2734 0.6992 0.4779 0.058 Uiso 1 1 calc R . .
C12 C -0.2676(4) 0.7820(2) 0.46030(18) 0.0750(9) Uani 1 1 d . . .
H12A H -0.3382 0.8067 0.4950 0.113 Uiso 1 1 calc R . .
H12B H -0.3264 0.7356 0.4329 0.113 Uiso 1 1 calc R . .
H12C H -0.2355 0.8293 0.4286 0.113 Uiso 1 1 calc R . .
C13 C 0.3797(3) 0.76424(15) 0.68447(13) 0.0393(6) Uani 1 1 d . . .
C14 C 0.4183(4) 0.83837(18) 0.64401(16) 0.0643(8) Uani 1 1 d . . .
H14 H 0.4608 0.8299 0.5993 0.077 Uiso 1 1 calc R . .
C15 C 0.3945(5) 0.9256(2) 0.6690(2) 0.0776(10) Uani 1 1 d . . .
H15 H 0.4227 0.9751 0.6414 0.093 Uiso 1 1 calc R . .
C16 C 0.3302(4) 0.9390(2) 0.7337(2) 0.0696(9) Uani 1 1 d . . .
H16 H 0.3130 0.9976 0.7502 0.084 Uiso 1 1 calc R . .
C17 C 0.2914(4) 0.8670(2) 0.77387(19) 0.0749(9) Uani 1 1 d . . .
H17 H 0.2477 0.8760 0.8183 0.090 Uiso 1 1 calc R . .
C18 C 0.3158(4) 0.78021(19) 0.74964(15) 0.0605(8) Uani 1 1 d . . .
H18 H 0.2884 0.7313 0.7781 0.073 Uiso 1 1 calc R . .
C19 C 0.7518(3) 0.70026(16) 0.75656(13) 0.0455(6) Uani 1 1 d . . .
H19 H 0.7642 0.7457 0.7227 0.055 Uiso 1 1 calc R . .
C20 C 0.6488(3) 0.62763(14) 0.74661(12) 0.0375(6) Uani 1 1 d . . .
C21 C 0.6656(3) 0.57752(15) 0.81265(12) 0.0389(6) Uani 1 1 d . . .
C22 C 0.7818(3) 0.62308(15) 0.85867(13) 0.0415(6) Uani 1 1 d . . .
C23 C 0.8238(4) 0.59380(19) 0.92797(15) 0.0581(7) Uani 1 1 d . . .
H23 H 0.9029 0.6243 0.9573 0.070 Uiso 1 1 calc R . .
C24 C 0.7450(4) 0.5185(2) 0.95167(17) 0.0756(9) Uani 1 1 d . . .
H24 H 0.7689 0.4981 0.9984 0.091 Uiso 1 1 calc R . .
C25 C 0.6299(4) 0.4718(2) 0.90705(17) 0.0762(10) Uani 1 1 d . . .
H25 H 0.5791 0.4203 0.9244 0.091 Uiso 1 1 calc R . .
C26 C 0.5891(4) 0.49983(18) 0.83804(15) 0.0587(8) Uani 1 1 d . . .
H26 H 0.5121 0.4678 0.8087 0.070 Uiso 1 1 calc R . .
C27 C 0.6005(3) 0.44475(16) 0.64580(12) 0.0404(6) Uani 1 1 d . . .
C28 C 0.7780(3) 0.44652(18) 0.67364(16) 0.0602(8) Uani 1 1 d . . .
H28A H 0.7839 0.4435 0.7252 0.090 Uiso 1 1 calc R . .
H28B H 0.8290 0.5017 0.6587 0.090 Uiso 1 1 calc R . .
H28C H 0.8353 0.3955 0.6549 0.090 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
N1 0.0427(11) 0.0317(11) 0.0356(11) -0.0005(8) -0.0027(9) 0.0050(8)
N2 0.0571(13) 0.0405(12) 0.0515(14) -0.0044(10) -0.0109(11) -0.0137(10)
O1 0.0595(11) 0.0305(9) 0.0676(12) -0.0061(8) -0.0080(9) 0.0060(8)
C1 0.0447(13) 0.0326(13) 0.0336(13) -0.0010(10) 0.0013(10) 0.0012(10)
C2 0.0415(13) 0.0307(12) 0.0371(13) -0.0008(10) -0.0005(10) -0.0001(10)
C3 0.0419(13) 0.0304(12) 0.0323(13) 0.0012(10) 0.0012(10) 0.0006(10)
C4 0.0435(13) 0.0323(13) 0.0358(13) -0.0010(10) 0.0006(10) -0.0001(10)
C5 0.0609(16) 0.0375(14) 0.0489(16) -0.0053(12) -0.0104(13) 0.0028(12)
C6 0.0400(13) 0.0318(12) 0.0369(13) -0.0012(10) -0.0014(10) 0.0014(10)
C7 0.0527(16) 0.0646(18) 0.0417(15) 0.0025(13) 0.0077(13) 0.0053(13)
C8 0.0434(15) 0.079(2) 0.0570(18) -0.0073(16) 0.0047(13) 0.0119(14)
C9 0.0496(16) 0.0391(14) 0.0554(17) -0.0119(12) -0.0113(13) 0.0088(11)
C10 0.0608(17) 0.0571(17) 0.0468(16) 0.0130(13) -0.0071(13) 0.0013(13)
C11 0.0412(14) 0.0575(16) 0.0464(15) 0.0092(13) 0.0039(11) 0.0034(12)
C12 0.0651(19) 0.069(2) 0.088(2) -0.0156(18) -0.0259(17) 0.0205(16)
C13 0.0430(13) 0.0340(13) 0.0401(14) -0.0036(11) -0.0026(11) 0.0050(10)
C14 0.100(2) 0.0401(16) 0.0544(18) 0.0007(13) 0.0137(16) 0.0015(15)
C15 0.107(3) 0.0361(17) 0.088(3) 0.0076(16) -0.005(2) 0.0025(16)
C16 0.0632(19) 0.0468(18) 0.096(3) -0.0285(18) -0.0175(18) 0.0139(14)
C17 0.081(2) 0.066(2) 0.080(2) -0.0279(19) 0.0196(18) 0.0094(17)
C18 0.077(2) 0.0484(17) 0.0580(18) -0.0062(14) 0.0213(15) 0.0017(14)
C19 0.0564(15) 0.0361(14) 0.0434(15) 0.0021(11) -0.0009(12) -0.0055(12)
C20 0.0422(13) 0.0305(12) 0.0393(14) -0.0024(10) -0.0019(10) 0.0030(10)
C21 0.0433(14) 0.0315(13) 0.0410(14) 0.0001(10) -0.0046(11) 0.0019(10)
C22 0.0466(14) 0.0343(13) 0.0425(15) -0.0034(11) -0.0071(11) 0.0014(11)
C23 0.0687(18) 0.0524(17) 0.0504(17) -0.0044(14) -0.0173(14) -0.0001(14)
C24 0.106(3) 0.068(2) 0.0502(19) 0.0155(16) -0.0185(18) -0.0088(19)
C25 0.101(3) 0.061(2) 0.064(2) 0.0247(16) -0.0128(18) -0.0227(18)
C26 0.0688(19) 0.0457(16) 0.0595(19) 0.0068(13) -0.0125(15) -0.0147(13)
C27 0.0474(14) 0.0360(14) 0.0378(14) -0.0001(11) 0.0018(11) 0.0039(11)
C28 0.0527(17) 0.0526(17) 0.074(2) -0.0117(14) -0.0073(14) 0.0124(13)
_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 C4 1.366(3) . ?
N1 C1 1.392(3) . ?
N1 C6 1.439(3) . ?
N2 C19 1.364(3) . ?
N2 C22 1.372(3) . ?
N2 H2 0.8600 . ?
O1 C27 1.233(3) . ?
C1 C2 1.366(3) . ?
C1 C13 1.478(3) . ?
C2 C3 1.446(3) . ?
C2 C20 1.472(3) . ?
C3 C4 1.387(3) . ?
C3 C27 1.455(3) . ?
C4 C5 1.488(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C11 1.366(3) . ?
C6 C7 1.373(3) . ?
C7 C8 1.379(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.375(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.374(4) . ?
C9 C12 1.509(3) . ?
C10 C11 1.386(3) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C18 1.371(3) . ?
C13 C14 1.374(3) . ?
C14 C15 1.384(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.357(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.347(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.374(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.361(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.435(3) . ?
C21 C26 1.397(3) . ?
C21 C22 1.402(3) . ?
C22 C23 1.384(3) . ?
C23 C24 1.366(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.390(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.372(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.492(3) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
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
C4 N1 C1 109.85(18) . . ?
C4 N1 C6 124.52(18) . . ?
C1 N1 C6 125.37(18) . . ?
C19 N2 C22 108.4(2) . . ?
C19 N2 H2 125.8 . . ?
C22 N2 H2 125.8 . . ?
C2 C1 N1 108.27(19) . . ?
C2 C1 C13 129.5(2) . . ?
N1 C1 C13 122.19(19) . . ?
C1 C2 C3 106.8(2) . . ?
C1 C2 C20 123.9(2) . . ?
C3 C2 C20 129.1(2) . . ?
C4 C3 C2 107.43(19) . . ?
C4 C3 C27 123.4(2) . . ?
C2 C3 C27 129.0(2) . . ?
N1 C4 C3 107.60(19) . . ?
N1 C4 C5 121.1(2) . . ?
C3 C4 C5 131.3(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 119.9(2) . . ?
C11 C6 N1 120.5(2) . . ?
C7 C6 N1 119.6(2) . . ?
C6 C7 C8 119.4(2) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C9 C8 C7 121.8(2) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C10 C9 C8 117.8(2) . . ?
C10 C9 C12 120.8(3) . . ?
C8 C9 C12 121.4(3) . . ?
C9 C10 C11 121.1(2) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C6 C11 C10 120.0(2) . . ?
C6 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 117.5(2) . . ?
C18 C13 C1 120.7(2) . . ?
C14 C13 C1 121.8(2) . . ?
C13 C14 C15 120.8(3) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 119.7(3) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 120.4(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 121.4(3) . . ?
C13 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C20 C19 N2 111.2(2) . . ?
C20 C19 H19 124.4 . . ?
N2 C19 H19 124.4 . . ?
C19 C20 C21 105.3(2) . . ?
C19 C20 C2 127.4(2) . . ?
C21 C20 C2 126.9(2) . . ?
C26 C21 C22 118.5(2) . . ?
C26 C21 C20 133.8(2) . . ?
C22 C21 C20 107.6(2) . . ?
N2 C22 C23 130.0(2) . . ?
N2 C22 C21 107.5(2) . . ?
C23 C22 C21 122.5(2) . . ?
C24 C23 C22 117.6(3) . . ?
C24 C23 H23 121.2 . . ?
C22 C23 H23 121.2 . . ?
C23 C24 C25 121.0(3) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C26 C25 C24 121.7(3) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C25 C26 C21 118.7(3) . . ?
C25 C26 H26 120.7 . . ?
C21 C26 H26 120.7 . . ?
O1 C27 C3 120.8(2) . . ?
O1 C27 C28 119.0(2) . . ?
C3 C27 C28 120.1(2) . . ?
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 . . ?
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
C4 N1 C1 C2 1.3(2) . . . . ?
C6 N1 C1 C2 175.6(2) . . . . ?
C4 N1 C1 C13 -178.1(2) . . . . ?
C6 N1 C1 C13 -3.7(3) . . . . ?
N1 C1 C2 C3 -0.6(2) . . . . ?
C13 C1 C2 C3 178.7(2) . . . . ?
N1 C1 C2 C20 -175.46(19) . . . . ?
C13 C1 C2 C20 3.9(4) . . . . ?
C1 C2 C3 C4 -0.3(2) . . . . ?
C20 C2 C3 C4 174.2(2) . . . . ?
C1 C2 C3 C27 175.7(2) . . . . ?
C20 C2 C3 C27 -9.8(4) . . . . ?
C1 N1 C4 C3 -1.4(2) . . . . ?
C6 N1 C4 C3 -175.85(19) . . . . ?
C1 N1 C4 C5 179.9(2) . . . . ?
C6 N1 C4 C5 5.5(3) . . . . ?
C2 C3 C4 N1 1.0(2) . . . . ?
C27 C3 C4 N1 -175.2(2) . . . . ?
C2 C3 C4 C5 179.5(2) . . . . ?
C27 C3 C4 C5 3.2(4) . . . . ?
C4 N1 C6 C11 -81.4(3) . . . . ?
C1 N1 C6 C11 105.0(3) . . . . ?
C4 N1 C6 C7 97.6(3) . . . . ?
C1 N1 C6 C7 -76.0(3) . . . . ?
C11 C6 C7 C8 -0.1(4) . . . . ?
N1 C6 C7 C8 -179.1(2) . . . . ?
C6 C7 C8 C9 -0.4(4) . . . . ?
C7 C8 C9 C10 0.9(4) . . . . ?
C7 C8 C9 C12 -179.5(3) . . . . ?
C8 C9 C10 C11 -0.9(4) . . . . ?
C12 C9 C10 C11 179.5(2) . . . . ?
C7 C6 C11 C10 0.1(4) . . . . ?
N1 C6 C11 C10 179.1(2) . . . . ?
C9 C10 C11 C6 0.4(4) . . . . ?
C2 C1 C13 C18 -71.0(3) . . . . ?
N1 C1 C13 C18 108.2(3) . . . . ?
C2 C1 C13 C14 106.7(3) . . . . ?
N1 C1 C13 C14 -74.0(3) . . . . ?
C18 C13 C14 C15 0.7(4) . . . . ?
C1 C13 C14 C15 -177.2(3) . . . . ?
C13 C14 C15 C16 -1.0(5) . . . . ?
C14 C15 C16 C17 0.8(5) . . . . ?
C15 C16 C17 C18 -0.3(5) . . . . ?
C14 C13 C18 C17 -0.1(4) . . . . ?
C1 C13 C18 C17 177.7(3) . . . . ?
C16 C17 C18 C13 -0.1(5) . . . . ?
C22 N2 C19 C20 -1.8(3) . . . . ?
N2 C19 C20 C21 1.7(3) . . . . ?
N2 C19 C20 C2 174.7(2) . . . . ?
C1 C2 C20 C19 -53.2(3) . . . . ?
C3 C2 C20 C19 133.2(3) . . . . ?
C1 C2 C20 C21 118.3(3) . . . . ?
C3 C2 C20 C21 -55.3(3) . . . . ?
C19 C20 C21 C26 176.6(3) . . . . ?
C2 C20 C21 C26 3.5(4) . . . . ?
C19 C20 C21 C22 -1.0(3) . . . . ?
C2 C20 C21 C22 -174.0(2) . . . . ?
C19 N2 C22 C23 -177.0(3) . . . . ?
C19 N2 C22 C21 1.1(3) . . . . ?
C26 C21 C22 N2 -178.0(2) . . . . ?
C20 C21 C22 N2 0.0(3) . . . . ?
C26 C21 C22 C23 0.3(4) . . . . ?
C20 C21 C22 C23 178.2(2) . . . . ?
N2 C22 C23 C24 176.6(3) . . . . ?
C21 C22 C23 C24 -1.3(4) . . . . ?
C22 C23 C24 C25 1.5(5) . . . . ?
C23 C24 C25 C26 -0.8(5) . . . . ?
C24 C25 C26 C21 -0.3(5) . . . . ?
C22 C21 C26 C25 0.5(4) . . . . ?
C20 C21 C26 C25 -176.8(3) . . . . ?
C4 C3 C27 O1 -23.5(3) . . . . ?
C2 C3 C27 O1 161.1(2) . . . . ?
C4 C3 C27 C28 153.8(2) . . . . ?
C2 C3 C27 C28 -21.6(4) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.047


data_110704b
_database_code_depnum_ccdc_archive 'CCDC 895106'
#TrackingRef '6y.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H25 N O2 S'
_chemical_formula_weight         427.54
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'
S S 0.1246 0.1234 '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                   10.5132(11)
_cell_length_b                   10.6040(12)
_cell_length_c                   22.086(2)
_cell_angle_alpha                78.6820(10)
_cell_angle_beta                 84.544(2)
_cell_angle_gamma                72.6060(10)
_cell_volume                     2302.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1504
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      20.697
_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9344
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11743
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.1266
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         25.02
_reflns_number_total             8021
_reflns_number_gt                3349
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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.
;
_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^)+(0.0369P)^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         8021
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1522
_refine_ls_wR_factor_gt          0.1345
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.7550(3) 0.9844(4) -0.00644(14) 0.0524(9) Uani 1 1 d . . .
N2 N 0.2384(3) 0.4880(4) 0.50562(15) 0.0541(9) Uani 1 1 d . . .
O1 O 0.6971(4) 1.3958(3) -0.06325(15) 0.0910(11) Uani 1 1 d . . .
O2 O 0.8187(4) 0.6460(4) 0.23938(16) 0.1002(12) Uani 1 1 d . . .
O3 O 0.1913(4) 0.8481(3) 0.56702(16) 0.0971(12) Uani 1 1 d . . .
O4 O 0.2945(4) 0.4009(4) 0.24378(15) 0.0985(12) Uani 1 1 d . . .
S1 S 0.57721(12) 1.16662(12) 0.12859(5) 0.0653(4) Uani 1 1 d . . .
S2 S 0.10160(13) 0.78656(12) 0.37210(5) 0.0716(4) Uani 1 1 d . . .
C1 C 0.7561(4) 1.1114(4) -0.03513(18) 0.0518(11) Uani 1 1 d . . .
C2 C 0.7013(4) 1.1977(4) 0.00606(18) 0.0513(11) Uani 1 1 d . . .
C3 C 0.6667(4) 1.1173(5) 0.06165(18) 0.0547(12) Uani 1 1 d . . .
C4 C 0.6999(4) 0.9872(4) 0.05327(18) 0.0513(11) Uani 1 1 d . . .
C5 C 0.8066(4) 0.8653(4) -0.03300(17) 0.0486(11) Uani 1 1 d . . .
C6 C 0.9274(5) 0.7783(5) -0.01774(19) 0.0635(13) Uani 1 1 d . . .
H6 H 0.9770 0.7945 0.0110 0.076 Uiso 1 1 calc R . .
C7 C 0.9770(5) 0.6653(5) -0.0449(2) 0.0711(14) Uani 1 1 d . . .
H7 H 1.0602 0.6066 -0.0341 0.085 Uiso 1 1 calc R . .
C8 C 0.9066(5) 0.6375(5) -0.0874(2) 0.0604(12) Uani 1 1 d . . .
C9 C 0.7821(5) 0.7271(5) -0.10168(19) 0.0643(13) Uani 1 1 d . . .
H9 H 0.7308 0.7112 -0.1298 0.077 Uiso 1 1 calc R . .
C10 C 0.7343(4) 0.8390(4) -0.07454(18) 0.0594(12) Uani 1 1 d . . .
H10 H 0.6509 0.8981 -0.0847 0.071 Uiso 1 1 calc R . .
C11 C 0.9630(5) 0.5189(4) -0.1191(2) 0.0946(17) Uani 1 1 d . . .
H11A H 0.8983 0.4704 -0.1168 0.142 Uiso 1 1 calc R . .
H11B H 1.0422 0.4612 -0.0992 0.142 Uiso 1 1 calc R . .
H11C H 0.9845 0.5493 -0.1616 0.142 Uiso 1 1 calc R . .
C12 C 0.8168(5) 1.1335(4) -0.09875(18) 0.0796(15) Uani 1 1 d . . .
H12A H 0.8813 1.0519 -0.1063 0.119 Uiso 1 1 calc R . .
H12B H 0.8598 1.2030 -0.1025 0.119 Uiso 1 1 calc R . .
H12C H 0.7483 1.1599 -0.1284 0.119 Uiso 1 1 calc R . .
C13 C 0.6838(4) 1.3420(5) -0.0099(2) 0.0607(13) Uani 1 1 d . . .
C14 C 0.6494(4) 1.4278(4) 0.03926(19) 0.0724(14) Uani 1 1 d . . .
H14A H 0.6562 1.5161 0.0219 0.109 Uiso 1 1 calc R . .
H14B H 0.7101 1.3885 0.0722 0.109 Uiso 1 1 calc R . .
H14C H 0.5599 1.4339 0.0550 0.109 Uiso 1 1 calc R . .
C15 C 0.6980(5) 1.1760(4) 0.17612(18) 0.0536(12) Uani 1 1 d . . .
C16 C 0.6527(5) 1.2074(5) 0.2328(2) 0.0905(17) Uani 1 1 d . . .
H16 H 0.5627 1.2217 0.2442 0.109 Uiso 1 1 calc R . .
C17 C 0.7398(7) 1.2180(7) 0.2734(2) 0.124(2) Uani 1 1 d . . .
H17 H 0.7092 1.2360 0.3126 0.149 Uiso 1 1 calc R . .
C18 C 0.8714(7) 1.2018(6) 0.2555(3) 0.114(2) Uani 1 1 d . . .
H18 H 0.9296 1.2114 0.2823 0.137 Uiso 1 1 calc R . .
C19 C 0.9170(5) 1.1719(5) 0.1992(2) 0.0856(16) Uani 1 1 d . . .
H19 H 1.0064 1.1612 0.1873 0.103 Uiso 1 1 calc R . .
C20 C 0.8302(5) 1.1574(4) 0.1591(2) 0.0677(13) Uani 1 1 d . . .
H20 H 0.8619 1.1350 0.1206 0.081 Uiso 1 1 calc R . .
C21 C 0.6862(4) 0.8649(4) 0.09515(18) 0.0521(11) Uani 1 1 d . . .
C22 C 0.7610(4) 0.8166(5) 0.14761(19) 0.0626(13) Uani 1 1 d . . .
H22 H 0.8194 0.8613 0.1560 0.075 Uiso 1 1 calc R . .
C23 C 0.7492(5) 0.7028(5) 0.1872(2) 0.0699(14) Uani 1 1 d . . .
C24 C 0.6607(6) 0.6391(5) 0.1748(2) 0.0770(15) Uani 1 1 d . . .
H24 H 0.6526 0.5619 0.2014 0.092 Uiso 1 1 calc R . .
C25 C 0.5844(5) 0.6880(5) 0.1238(2) 0.0731(14) Uani 1 1 d . . .
H25 H 0.5239 0.6448 0.1163 0.088 Uiso 1 1 calc R . .
C26 C 0.5967(4) 0.7996(5) 0.0839(2) 0.0628(13) Uani 1 1 d . . .
H26 H 0.5452 0.8321 0.0492 0.075 Uiso 1 1 calc R . .
C27 C 0.9164(6) 0.7001(6) 0.2521(2) 0.118(2) Uani 1 1 d . . .
H27A H 0.9782 0.7027 0.2173 0.177 Uiso 1 1 calc R . .
H27B H 0.9630 0.6454 0.2878 0.177 Uiso 1 1 calc R . .
H27C H 0.8754 0.7895 0.2600 0.177 Uiso 1 1 calc R . .
C28 C 0.2387(4) 0.5876(5) 0.53598(19) 0.0535(12) Uani 1 1 d . . .
C29 C 0.1977(4) 0.7085(5) 0.49581(19) 0.0545(12) Uani 1 1 d . . .
C30 C 0.1712(4) 0.6780(4) 0.43876(18) 0.0531(11) Uani 1 1 d . . .
C31 C 0.1963(4) 0.5420(5) 0.44548(18) 0.0545(12) Uani 1 1 d . . .
C32 C 0.2931(5) 0.3472(5) 0.52963(18) 0.0515(11) Uani 1 1 d . . .
C33 C 0.4181(5) 0.2822(5) 0.51144(19) 0.0658(13) Uani 1 1 d . . .
H33 H 0.4663 0.3271 0.4821 0.079 Uiso 1 1 calc R . .
C34 C 0.4742(5) 0.1483(5) 0.5367(2) 0.0733(14) Uani 1 1 d . . .
H34 H 0.5594 0.1037 0.5234 0.088 Uiso 1 1 calc R . .
C35 C 0.4062(6) 0.0802(5) 0.5812(2) 0.0668(14) Uani 1 1 d . . .
C36 C 0.2797(6) 0.1465(6) 0.5975(2) 0.0759(15) Uani 1 1 d . . .
H36 H 0.2305 0.1012 0.6261 0.091 Uiso 1 1 calc R . .
C37 C 0.2219(5) 0.2802(5) 0.57250(19) 0.0676(13) Uani 1 1 d . . .
H37 H 0.1355 0.3241 0.5847 0.081 Uiso 1 1 calc R . .
C38 C 0.4726(5) -0.0622(5) 0.6114(2) 0.1013(19) Uani 1 1 d . . .
H38A H 0.4830 -0.0650 0.6544 0.152 Uiso 1 1 calc R . .
H38B H 0.5586 -0.0939 0.5916 0.152 Uiso 1 1 calc R . .
H38C H 0.4184 -0.1184 0.6073 0.152 Uiso 1 1 calc R . .
C39 C 0.2870(5) 0.5563(4) 0.60011(18) 0.0762(15) Uani 1 1 d . . .
H39A H 0.2124 0.5614 0.6291 0.114 Uiso 1 1 calc R . .
H39B H 0.3319 0.6200 0.6051 0.114 Uiso 1 1 calc R . .
H39C H 0.3477 0.4675 0.6073 0.114 Uiso 1 1 calc R . .
C40 C 0.1833(5) 0.8393(5) 0.5136(2) 0.0670(13) Uani 1 1 d . . .
C41 C 0.1593(5) 0.9642(4) 0.4661(2) 0.0791(15) Uani 1 1 d . . .
H41A H 0.1558 1.0389 0.4854 0.119 Uiso 1 1 calc R . .
H41B H 0.0762 0.9800 0.4471 0.119 Uiso 1 1 calc R . .
H41C H 0.2305 0.9542 0.4351 0.119 Uiso 1 1 calc R . .
C42 C 0.2386(5) 0.8253(4) 0.32859(18) 0.0555(12) Uani 1 1 d . . .
C43 C 0.3704(5) 0.7638(4) 0.34221(19) 0.0633(13) Uani 1 1 d . . .
H43 H 0.3919 0.6977 0.3772 0.076 Uiso 1 1 calc R . .
C44 C 0.4706(5) 0.7996(5) 0.3045(2) 0.0730(14) Uani 1 1 d . . .
H44 H 0.5591 0.7557 0.3139 0.088 Uiso 1 1 calc R . .
C45 C 0.4428(7) 0.8975(6) 0.2539(2) 0.0917(18) Uani 1 1 d . . .
H45 H 0.5108 0.9218 0.2287 0.110 Uiso 1 1 calc R . .
C46 C 0.3105(8) 0.9603(6) 0.2408(2) 0.101(2) Uani 1 1 d . . .
H46 H 0.2891 1.0279 0.2064 0.122 Uiso 1 1 calc R . .
C47 C 0.2106(6) 0.9244(5) 0.2777(2) 0.0886(17) Uani 1 1 d . . .
H47 H 0.1222 0.9681 0.2681 0.106 Uiso 1 1 calc R . .
C48 C 0.1852(4) 0.4568(4) 0.40175(19) 0.0545(12) Uani 1 1 d . . .
C49 C 0.2502(4) 0.4702(4) 0.34420(19) 0.0598(12) Uani 1 1 d . . .
H49 H 0.3020 0.5293 0.3341 0.072 Uiso 1 1 calc R . .
C50 C 0.2368(5) 0.3939(5) 0.3016(2) 0.0692(14) Uani 1 1 d . . .
C51 C 0.1620(5) 0.3047(5) 0.3174(2) 0.0754(15) Uani 1 1 d . . .
H51 H 0.1555 0.2518 0.2896 0.091 Uiso 1 1 calc R . .
C52 C 0.0972(5) 0.2942(5) 0.3742(2) 0.0780(15) Uani 1 1 d . . .
H52 H 0.0453 0.2352 0.3840 0.094 Uiso 1 1 calc R . .
C53 C 0.1073(5) 0.3693(5) 0.41735(19) 0.0643(13) Uani 1 1 d . . .
H53 H 0.0629 0.3612 0.4558 0.077 Uiso 1 1 calc R . .
C54 C 0.3536(6) 0.5052(6) 0.2218(2) 0.116(2) Uani 1 1 d . . .
H54A H 0.2940 0.5886 0.2303 0.174 Uiso 1 1 calc R . .
H54B H 0.3715 0.5114 0.1781 0.174 Uiso 1 1 calc R . .
H54C H 0.4357 0.4865 0.2422 0.174 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
N1 0.056(2) 0.064(3) 0.042(2) -0.0187(19) -0.0003(18) -0.018(2)
N2 0.061(3) 0.056(3) 0.044(2) 0.000(2) -0.0027(18) -0.020(2)
O1 0.130(3) 0.074(2) 0.070(2) -0.0131(19) 0.003(2) -0.032(2)
O2 0.109(3) 0.116(3) 0.069(2) 0.009(2) -0.018(2) -0.035(3)
O3 0.142(4) 0.080(3) 0.074(2) -0.021(2) -0.008(2) -0.034(2)
O4 0.122(3) 0.136(3) 0.066(2) -0.036(2) 0.022(2) -0.077(3)
S1 0.0523(8) 0.0922(10) 0.0602(7) -0.0353(6) 0.0042(6) -0.0219(7)
S2 0.0619(9) 0.0801(9) 0.0681(8) 0.0070(7) -0.0145(7) -0.0224(7)
C1 0.058(3) 0.055(3) 0.045(3) -0.008(2) -0.003(2) -0.020(3)
C2 0.055(3) 0.056(3) 0.048(3) -0.014(2) -0.003(2) -0.020(2)
C3 0.048(3) 0.071(3) 0.053(3) -0.021(2) -0.003(2) -0.022(3)
C4 0.051(3) 0.066(3) 0.044(3) -0.014(2) -0.003(2) -0.024(3)
C5 0.051(3) 0.053(3) 0.044(3) -0.017(2) 0.000(2) -0.013(3)
C6 0.056(3) 0.069(4) 0.069(3) -0.022(3) -0.014(3) -0.013(3)
C7 0.050(3) 0.071(4) 0.086(4) -0.021(3) -0.007(3) -0.001(3)
C8 0.062(4) 0.065(3) 0.058(3) -0.027(3) 0.012(3) -0.018(3)
C9 0.068(4) 0.069(4) 0.061(3) -0.024(3) -0.002(3) -0.020(3)
C10 0.052(3) 0.071(3) 0.056(3) -0.023(2) -0.004(2) -0.010(3)
C11 0.105(4) 0.067(4) 0.106(4) -0.040(3) 0.013(3) -0.003(3)
C12 0.105(4) 0.082(4) 0.056(3) -0.020(2) 0.012(3) -0.033(3)
C13 0.062(3) 0.060(4) 0.058(3) -0.012(3) -0.002(3) -0.014(3)
C14 0.075(4) 0.070(3) 0.071(3) -0.028(3) -0.004(3) -0.010(3)
C15 0.056(3) 0.062(3) 0.046(3) -0.018(2) 0.001(2) -0.017(2)
C16 0.081(4) 0.149(5) 0.063(3) -0.050(3) 0.013(3) -0.050(4)
C17 0.131(6) 0.223(7) 0.065(4) -0.062(4) 0.016(4) -0.102(6)
C18 0.111(6) 0.190(7) 0.074(4) -0.031(4) -0.023(4) -0.082(5)
C19 0.064(4) 0.125(5) 0.069(4) 0.001(3) -0.015(3) -0.037(3)
C20 0.061(4) 0.089(4) 0.054(3) -0.011(2) -0.008(3) -0.021(3)
C21 0.056(3) 0.064(3) 0.045(3) -0.020(2) 0.007(2) -0.026(3)
C22 0.056(3) 0.086(4) 0.053(3) -0.021(3) -0.002(3) -0.025(3)
C23 0.084(4) 0.079(4) 0.047(3) -0.008(3) -0.001(3) -0.025(3)
C24 0.095(4) 0.065(4) 0.076(4) -0.014(3) 0.014(3) -0.034(3)
C25 0.082(4) 0.090(4) 0.065(3) -0.030(3) 0.013(3) -0.047(3)
C26 0.063(3) 0.084(4) 0.052(3) -0.019(3) 0.002(2) -0.034(3)
C27 0.118(6) 0.148(6) 0.084(4) -0.008(4) -0.038(4) -0.029(5)
C28 0.056(3) 0.057(3) 0.048(3) -0.011(3) 0.003(2) -0.017(3)
C29 0.054(3) 0.063(3) 0.049(3) -0.013(3) 0.007(2) -0.022(3)
C30 0.045(3) 0.055(3) 0.057(3) -0.001(2) 0.003(2) -0.017(2)
C31 0.043(3) 0.068(4) 0.048(3) -0.001(3) 0.002(2) -0.016(3)
C32 0.054(3) 0.058(3) 0.043(3) -0.003(2) -0.002(2) -0.020(3)
C33 0.055(4) 0.081(4) 0.060(3) -0.003(3) 0.007(3) -0.026(3)
C34 0.062(4) 0.074(4) 0.076(3) -0.012(3) -0.002(3) -0.009(3)
C35 0.078(4) 0.067(4) 0.054(3) -0.004(3) -0.013(3) -0.019(3)
C36 0.079(4) 0.080(4) 0.065(3) 0.011(3) 0.001(3) -0.034(3)
C37 0.058(3) 0.081(4) 0.060(3) 0.001(3) 0.006(3) -0.025(3)
C38 0.139(5) 0.069(4) 0.087(4) 0.015(3) -0.039(4) -0.023(4)
C39 0.097(4) 0.075(3) 0.056(3) -0.015(2) -0.008(3) -0.020(3)
C40 0.061(3) 0.074(4) 0.064(3) -0.013(3) 0.001(3) -0.019(3)
C41 0.084(4) 0.063(3) 0.088(4) -0.013(3) 0.005(3) -0.019(3)
C42 0.072(4) 0.057(3) 0.042(3) -0.009(2) -0.006(2) -0.022(3)
C43 0.068(4) 0.075(4) 0.047(3) 0.001(2) -0.003(3) -0.029(3)
C44 0.075(4) 0.078(4) 0.072(3) -0.019(3) 0.011(3) -0.030(3)
C45 0.120(6) 0.088(5) 0.069(4) -0.017(3) 0.036(4) -0.042(4)
C46 0.146(7) 0.085(5) 0.055(3) 0.013(3) 0.014(4) -0.028(5)
C47 0.101(5) 0.091(4) 0.059(3) 0.008(3) 0.001(3) -0.020(3)
C48 0.060(3) 0.060(3) 0.047(3) -0.002(2) -0.010(2) -0.025(3)
C49 0.065(3) 0.071(3) 0.051(3) -0.005(2) 0.003(2) -0.036(3)
C50 0.080(4) 0.085(4) 0.049(3) -0.009(3) 0.002(3) -0.036(3)
C51 0.092(4) 0.086(4) 0.066(3) -0.021(3) -0.002(3) -0.047(3)
C52 0.087(4) 0.090(4) 0.071(3) 0.002(3) -0.005(3) -0.056(3)
C53 0.080(4) 0.078(3) 0.046(3) -0.008(2) -0.004(2) -0.040(3)
C54 0.147(6) 0.147(6) 0.073(4) -0.023(4) 0.037(4) -0.080(5)
_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 1.374(5) . ?
N1 C4 1.391(5) . ?
N1 C5 1.433(5) . ?
N2 C28 1.358(5) . ?
N2 C31 1.396(4) . ?
N2 C32 1.441(5) . ?
O1 C13 1.219(4) . ?
O2 C23 1.360(5) . ?
O2 C27 1.391(6) . ?
O3 C40 1.215(5) . ?
O4 C50 1.360(5) . ?
O4 C54 1.410(5) . ?
S1 C3 1.758(4) . ?
S1 C15 1.759(4) . ?
S2 C30 1.750(4) . ?
S2 C42 1.761(5) . ?
C1 C2 1.382(5) . ?
C1 C12 1.492(5) . ?
C2 C3 1.434(5) . ?
C2 C13 1.459(5) . ?
C3 C4 1.364(5) . ?
C4 C21 1.474(5) . ?
C5 C6 1.355(5) . ?
C5 C10 1.363(5) . ?
C6 C7 1.385(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.373(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.391(5) . ?
C8 C11 1.498(5) . ?
C9 C10 1.373(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.502(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.363(5) . ?
C15 C20 1.371(5) . ?
C16 C17 1.384(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.372(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.352(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.391(5) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.387(5) . ?
C21 C26 1.388(5) . ?
C22 C23 1.375(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.377(6) . ?
C24 C25 1.370(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.361(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.383(5) . ?
C28 C39 1.492(5) . ?
C29 C30 1.432(5) . ?
C29 C40 1.476(6) . ?
C30 C31 1.366(5) . ?
C31 C48 1.480(5) . ?
C32 C33 1.353(5) . ?
C32 C37 1.371(5) . ?
C33 C34 1.388(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.376(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.358(6) . ?
C35 C38 1.509(6) . ?
C36 C37 1.388(5) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 C41 1.491(5) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C47 1.366(5) . ?
C42 C43 1.377(5) . ?
C43 C44 1.377(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.356(6) . ?
C44 H44 0.9300 . ?
C45 C46 1.381(7) . ?
C45 H45 0.9300 . ?
C46 C47 1.367(7) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 C49 1.387(5) . ?
C48 C53 1.388(5) . ?
C49 C50 1.396(6) . ?
C49 H49 0.9300 . ?
C50 C51 1.377(6) . ?
C51 C52 1.370(6) . ?
C51 H51 0.9300 . ?
C52 C53 1.385(6) . ?
C52 H52 0.9300 . ?
C53 H53 0.9300 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
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 C4 110.0(3) . . ?
C1 N1 C5 125.4(3) . . ?
C4 N1 C5 124.6(4) . . ?
C28 N2 C31 110.2(4) . . ?
C28 N2 C32 123.8(3) . . ?
C31 N2 C32 125.3(4) . . ?
C23 O2 C27 118.3(4) . . ?
C50 O4 C54 118.2(4) . . ?
C3 S1 C15 105.0(2) . . ?
C30 S2 C42 104.4(2) . . ?
N1 C1 C2 107.9(4) . . ?
N1 C1 C12 120.2(4) . . ?
C2 C1 C12 131.8(4) . . ?
C1 C2 C3 106.5(4) . . ?
C1 C2 C13 122.5(4) . . ?
C3 C2 C13 130.9(4) . . ?
C4 C3 C2 108.8(4) . . ?
C4 C3 S1 121.0(3) . . ?
C2 C3 S1 129.7(4) . . ?
C3 C4 N1 106.8(4) . . ?
C3 C4 C21 131.1(4) . . ?
N1 C4 C21 122.1(4) . . ?
C6 C5 C10 119.2(4) . . ?
C6 C5 N1 120.8(4) . . ?
C10 C5 N1 119.9(4) . . ?
C5 C6 C7 120.1(4) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 121.7(4) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C7 C8 C9 117.2(4) . . ?
C7 C8 C11 121.8(5) . . ?
C9 C8 C11 121.0(4) . . ?
C10 C9 C8 120.5(4) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C5 C10 C9 121.3(4) . . ?
C5 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C1 C12 H12A 109.5 . . ?
C1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 C2 121.1(4) . . ?
O1 C13 C14 118.3(4) . . ?
C2 C13 C14 120.7(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 119.7(4) . . ?
C16 C15 S1 116.0(4) . . ?
C20 C15 S1 124.4(3) . . ?
C15 C16 C17 120.4(5) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C18 C17 C16 119.5(5) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C19 C18 C17 120.5(5) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 119.9(5) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C15 C20 C19 120.0(4) . . ?
C15 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C26 119.4(4) . . ?
C22 C21 C4 119.4(4) . . ?
C26 C21 C4 121.1(4) . . ?
C23 C22 C21 120.1(4) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
O2 C23 C22 125.0(5) . . ?
O2 C23 C24 115.6(5) . . ?
C22 C23 C24 119.3(5) . . ?
C25 C24 C23 120.8(5) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C26 C25 C24 120.3(5) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C21 120.0(4) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
O2 C27 H27A 109.5 . . ?
O2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N2 C28 C29 108.0(4) . . ?
N2 C28 C39 121.0(4) . . ?
C29 C28 C39 130.9(4) . . ?
C28 C29 C30 106.8(4) . . ?
C28 C29 C40 123.0(4) . . ?
C30 C29 C40 130.1(4) . . ?
C31 C30 C29 108.2(4) . . ?
C31 C30 S2 121.9(3) . . ?
C29 C30 S2 129.6(4) . . ?
C30 C31 N2 106.8(4) . . ?
C30 C31 C48 131.1(4) . . ?
N2 C31 C48 122.1(4) . . ?
C33 C32 C37 119.9(4) . . ?
C33 C32 N2 119.4(4) . . ?
C37 C32 N2 120.7(4) . . ?
C32 C33 C34 119.8(4) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C35 C34 C33 121.3(5) . . ?
C35 C34 H34 119.3 . . ?
C33 C34 H34 119.3 . . ?
C36 C35 C34 117.7(5) . . ?
C36 C35 C38 121.8(5) . . ?
C34 C35 C38 120.5(5) . . ?
C35 C36 C37 121.6(5) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 H36 119.2 . . ?
C32 C37 C36 119.5(4) . . ?
C32 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C28 C39 H39A 109.5 . . ?
C28 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C28 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O3 C40 C29 121.1(4) . . ?
O3 C40 C41 118.3(5) . . ?
C29 C40 C41 120.6(4) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C47 C42 C43 118.2(5) . . ?
C47 C42 S2 116.9(4) . . ?
C43 C42 S2 125.0(3) . . ?
C44 C43 C42 120.5(4) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C45 C44 C43 121.3(5) . . ?
C45 C44 H44 119.4 . . ?
C43 C44 H44 119.4 . . ?
C44 C45 C46 118.1(6) . . ?
C44 C45 H45 121.0 . . ?
C46 C45 H45 121.0 . . ?
C47 C46 C45 120.9(5) . . ?
C47 C46 H46 119.5 . . ?
C45 C46 H46 119.5 . . ?
C42 C47 C46 121.0(5) . . ?
C42 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
C49 C48 C53 121.0(4) . . ?
C49 C48 C31 118.5(4) . . ?
C53 C48 C31 120.5(4) . . ?
C48 C49 C50 119.2(4) . . ?
C48 C49 H49 120.4 . . ?
C50 C49 H49 120.4 . . ?
O4 C50 C51 116.1(5) . . ?
O4 C50 C49 123.9(5) . . ?
C51 C50 C49 120.0(4) . . ?
C52 C51 C50 119.9(5) . . ?
C52 C51 H51 120.1 . . ?
C50 C51 H51 120.1 . . ?
C51 C52 C53 121.6(4) . . ?
C51 C52 H52 119.2 . . ?
C53 C52 H52 119.2 . . ?
C52 C53 C48 118.3(4) . . ?
C52 C53 H53 120.9 . . ?
C48 C53 H53 120.9 . . ?
O4 C54 H54A 109.5 . . ?
O4 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
O4 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
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
C4 N1 C1 C2 0.0(5) . . . . ?
C5 N1 C1 C2 -178.3(4) . . . . ?
C4 N1 C1 C12 177.0(4) . . . . ?
C5 N1 C1 C12 -1.2(6) . . . . ?
N1 C1 C2 C3 0.2(5) . . . . ?
C12 C1 C2 C3 -176.4(4) . . . . ?
N1 C1 C2 C13 -178.4(4) . . . . ?
C12 C1 C2 C13 5.0(7) . . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
C13 C2 C3 C4 178.1(4) . . . . ?
C1 C2 C3 S1 -172.2(3) . . . . ?
C13 C2 C3 S1 6.2(7) . . . . ?
C15 S1 C3 C4 100.4(4) . . . . ?
C15 S1 C3 C2 -88.5(4) . . . . ?
C2 C3 C4 N1 0.2(5) . . . . ?
S1 C3 C4 N1 173.0(3) . . . . ?
C2 C3 C4 C21 179.9(4) . . . . ?
S1 C3 C4 C21 -7.4(6) . . . . ?
C1 N1 C4 C3 -0.1(5) . . . . ?
C5 N1 C4 C3 178.1(4) . . . . ?
C1 N1 C4 C21 -179.8(4) . . . . ?
C5 N1 C4 C21 -1.6(6) . . . . ?
C1 N1 C5 C6 101.2(5) . . . . ?
C4 N1 C5 C6 -76.8(5) . . . . ?
C1 N1 C5 C10 -78.3(5) . . . . ?
C4 N1 C5 C10 103.7(5) . . . . ?
C10 C5 C6 C7 1.0(6) . . . . ?
N1 C5 C6 C7 -178.5(4) . . . . ?
C5 C6 C7 C8 -0.2(7) . . . . ?
C6 C7 C8 C9 -0.7(7) . . . . ?
C6 C7 C8 C11 177.0(4) . . . . ?
C7 C8 C9 C10 0.9(6) . . . . ?
C11 C8 C9 C10 -176.8(4) . . . . ?
C6 C5 C10 C9 -0.7(6) . . . . ?
N1 C5 C10 C9 178.7(4) . . . . ?
C8 C9 C10 C5 -0.2(7) . . . . ?
C1 C2 C13 O1 11.8(7) . . . . ?
C3 C2 C13 O1 -166.4(5) . . . . ?
C1 C2 C13 C14 -167.9(4) . . . . ?
C3 C2 C13 C14 13.9(7) . . . . ?
C3 S1 C15 C16 -177.3(4) . . . . ?
C3 S1 C15 C20 4.4(4) . . . . ?
C20 C15 C16 C17 -1.2(8) . . . . ?
S1 C15 C16 C17 -179.6(4) . . . . ?
C15 C16 C17 C18 2.4(9) . . . . ?
C16 C17 C18 C19 -1.8(10) . . . . ?
C17 C18 C19 C20 -0.1(9) . . . . ?
C16 C15 C20 C19 -0.7(7) . . . . ?
S1 C15 C20 C19 177.6(3) . . . . ?
C18 C19 C20 C15 1.4(7) . . . . ?
C3 C4 C21 C22 -66.5(6) . . . . ?
N1 C4 C21 C22 113.1(4) . . . . ?
C3 C4 C21 C26 111.5(5) . . . . ?
N1 C4 C21 C26 -68.9(6) . . . . ?
C26 C21 C22 C23 1.8(7) . . . . ?
C4 C21 C22 C23 179.9(4) . . . . ?
C27 O2 C23 C22 -4.8(8) . . . . ?
C27 O2 C23 C24 175.5(5) . . . . ?
C21 C22 C23 O2 179.1(4) . . . . ?
C21 C22 C23 C24 -1.2(7) . . . . ?
O2 C23 C24 C25 179.5(4) . . . . ?
C22 C23 C24 C25 -0.2(8) . . . . ?
C23 C24 C25 C26 1.1(8) . . . . ?
C24 C25 C26 C21 -0.5(7) . . . . ?
C22 C21 C26 C25 -0.9(7) . . . . ?
C4 C21 C26 C25 -179.0(4) . . . . ?
C31 N2 C28 C29 -0.4(5) . . . . ?
C32 N2 C28 C29 170.9(4) . . . . ?
C31 N2 C28 C39 -176.6(4) . . . . ?
C32 N2 C28 C39 -5.2(6) . . . . ?
N2 C28 C29 C30 0.3(5) . . . . ?
C39 C28 C29 C30 175.9(4) . . . . ?
N2 C28 C29 C40 178.7(4) . . . . ?
C39 C28 C29 C40 -5.7(7) . . . . ?
C28 C29 C30 C31 0.0(5) . . . . ?
C40 C29 C30 C31 -178.3(4) . . . . ?
C28 C29 C30 S2 173.3(3) . . . . ?
C40 C29 C30 S2 -5.0(7) . . . . ?
C42 S2 C30 C31 -100.0(4) . . . . ?
C42 S2 C30 C29 87.4(4) . . . . ?
C29 C30 C31 N2 -0.2(4) . . . . ?
S2 C30 C31 N2 -174.2(3) . . . . ?
C29 C30 C31 C48 179.7(4) . . . . ?
S2 C30 C31 C48 5.7(6) . . . . ?
C28 N2 C31 C30 0.4(5) . . . . ?
C32 N2 C31 C30 -170.8(4) . . . . ?
C28 N2 C31 C48 -179.5(4) . . . . ?
C32 N2 C31 C48 9.3(6) . . . . ?
C28 N2 C32 C33 -97.2(5) . . . . ?
C31 N2 C32 C33 72.9(5) . . . . ?
C28 N2 C32 C37 80.1(5) . . . . ?
C31 N2 C32 C37 -109.9(5) . . . . ?
C37 C32 C33 C34 -0.6(6) . . . . ?
N2 C32 C33 C34 176.7(4) . . . . ?
C32 C33 C34 C35 -1.4(7) . . . . ?
C33 C34 C35 C36 3.1(7) . . . . ?
C33 C34 C35 C38 -175.6(4) . . . . ?
C34 C35 C36 C37 -2.9(7) . . . . ?
C38 C35 C36 C37 175.9(4) . . . . ?
C33 C32 C37 C36 0.9(6) . . . . ?
N2 C32 C37 C36 -176.4(4) . . . . ?
C35 C36 C37 C32 0.9(7) . . . . ?
C28 C29 C40 O3 -9.2(7) . . . . ?
C30 C29 C40 O3 168.8(4) . . . . ?
C28 C29 C40 C41 170.5(4) . . . . ?
C30 C29 C40 C41 -11.5(7) . . . . ?
C30 S2 C42 C47 -170.8(4) . . . . ?
C30 S2 C42 C43 8.8(4) . . . . ?
C47 C42 C43 C44 -1.7(6) . . . . ?
S2 C42 C43 C44 178.7(3) . . . . ?
C42 C43 C44 C45 1.4(7) . . . . ?
C43 C44 C45 C46 -0.5(8) . . . . ?
C44 C45 C46 C47 -0.2(8) . . . . ?
C43 C42 C47 C46 1.0(7) . . . . ?
S2 C42 C47 C46 -179.3(4) . . . . ?
C45 C46 C47 C42 -0.1(9) . . . . ?
C30 C31 C48 C49 53.4(6) . . . . ?
N2 C31 C48 C49 -126.7(4) . . . . ?
C30 C31 C48 C53 -124.2(5) . . . . ?
N2 C31 C48 C53 55.7(6) . . . . ?
C53 C48 C49 C50 -0.2(6) . . . . ?
C31 C48 C49 C50 -177.8(4) . . . . ?
C54 O4 C50 C51 169.9(5) . . . . ?
C54 O4 C50 C49 -10.3(7) . . . . ?
C48 C49 C50 O4 179.0(4) . . . . ?
C48 C49 C50 C51 -1.3(7) . . . . ?
O4 C50 C51 C52 -178.1(4) . . . . ?
C49 C50 C51 C52 2.1(7) . . . . ?
C50 C51 C52 C53 -1.5(7) . . . . ?
C51 C52 C53 C48 0.1(7) . . . . ?
C49 C48 C53 C52 0.8(7) . . . . ?
C31 C48 C53 C52 178.3(4) . . . . ?
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.045


data_121119f
_database_code_depnum_ccdc_archive 'CCDC 916139'
#TrackingRef 'web_deposit_cif_file_0_Shu-JiangTu_1355746000.8c.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H21 Br2 Cl N2 O2'
_chemical_formula_weight         576.71
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'
Cl Cl 0.1484 0.1585 '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                   11.9309(11)
_cell_length_b                   14.0473(13)
_cell_length_c                   15.0113(15)
_cell_angle_alpha                100.801(2)
_cell_angle_beta                 90.9050(10)
_cell_angle_gamma                97.8560(10)
_cell_volume                     2445.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1473
_cell_measurement_theta_min      2.407
_cell_measurement_theta_max      26.068
_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_exptl_absorpt_coefficient_mu    3.448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5044
_exptl_absorpt_correction_T_max  0.7243
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12419
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_sigmaI/netI    0.2540
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         25.02
_reflns_number_total             8464
_reflns_number_gt                2500
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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.
;
_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^)+(0.1980P)^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         8464
_refine_ls_number_parameters     583
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2959
_refine_ls_R_factor_gt           0.1442
_refine_ls_wR_factor_ref         0.4226
_refine_ls_wR_factor_gt          0.3698
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.0568(2) 0.28000(16) 0.35384(19) 0.1030(10) Uani 1 1 d . . .
Br2 Br 0.6745(2) 1.1580(2) 0.3650(2) 0.1217(12) Uani 1 1 d . . .
Br3 Br -0.0897(2) 0.1056(2) 0.0634(2) 0.1413(14) Uani 1 1 d . . .
Br4 Br 0.7985(4) 0.8631(3) 0.1459(3) 0.1777(17) Uani 1 1 d . . .
Cl1 Cl 0.6402(5) 0.0733(4) -0.0665(4) 0.099(2) Uani 1 1 d . . .
Cl2 Cl 0.1540(6) 0.5663(4) -0.0666(3) 0.098(2) Uani 1 1 d . . .
N1 N 0.0529(9) 0.7161(8) 0.3652(7) 0.032(3) Uani 1 1 d . . .
N2 N 0.2229(10) 0.9280(8) 0.4186(8) 0.035(3) Uani 1 1 d . . .
H2 H 0.2050 0.9289 0.4740 0.042 Uiso 1 1 calc R . .
N3 N 0.3517(10) 0.3296(9) 0.2431(8) 0.041(3) Uani 1 1 d . . .
N4 N 0.5095(10) 0.5430(9) 0.2942(8) 0.039(3) Uani 1 1 d . . .
H4 H 0.4567 0.5614 0.3289 0.047 Uiso 1 1 calc R . .
O1 O 0.2562(8) 0.7438(7) 0.3760(6) 0.034(2) Uani 1 1 d . . .
H1 H 0.2725 0.7882 0.4201 0.051 Uiso 1 1 calc R . .
O2 O -0.1307(9) 0.9569(7) 0.4195(7) 0.048(3) Uani 1 1 d . . .
O3 O 0.3950(9) 0.4460(7) 0.1465(6) 0.041(3) Uani 1 1 d . . .
H3 H 0.3979 0.5002 0.1791 0.062 Uiso 1 1 calc R . .
O4 O 0.5145(8) 0.3712(7) 0.5048(6) 0.038(3) Uani 1 1 d . . .
C1 C 0.1614(12) 0.7609(10) 0.3289(9) 0.034(4) Uani 1 1 d . . .
C2 C 0.1430(12) 0.8698(10) 0.3456(10) 0.035(4) Uani 1 1 d . . .
H2A H 0.1533 0.8958 0.2896 0.042 Uiso 1 1 calc R . .
C3 C 0.0235(12) 0.8705(10) 0.3741(9) 0.033(4) Uani 1 1 d . . .
C4 C -0.0217(12) 0.7802(11) 0.3876(9) 0.035(4) Uani 1 1 d . . .
C5 C -0.1323(12) 0.7526(11) 0.4220(10) 0.039(4) Uani 1 1 d . . .
H5A H -0.1863 0.7289 0.3720 0.059 Uiso 1 1 calc R . .
H5B H -0.1557 0.8086 0.4602 0.059 Uiso 1 1 calc R . .
H5C H -0.1280 0.7020 0.4564 0.059 Uiso 1 1 calc R . .
C6 C 0.0239(13) 0.6120(11) 0.3603(10) 0.036(4) Uani 1 1 d . . .
C7 C -0.0614(13) 0.5564(11) 0.3063(10) 0.037(4) Uani 1 1 d . . .
H7 H -0.1032 0.5860 0.2693 0.045 Uiso 1 1 calc R . .
C8 C -0.0890(13) 0.4569(11) 0.3040(10) 0.041(4) Uani 1 1 d . . .
H8 H -0.1524 0.4219 0.2702 0.049 Uiso 1 1 calc R . .
C9 C -0.0231(13) 0.4108(11) 0.3513(10) 0.043(4) Uani 1 1 d . . .
C10 C 0.0699(13) 0.4624(11) 0.4055(10) 0.042(4) Uani 1 1 d . . .
H10 H 0.1143 0.4307 0.4387 0.050 Uiso 1 1 calc R . .
C11 C 0.0952(13) 0.5672(11) 0.4085(10) 0.040(4) Uani 1 1 d . . .
H11 H 0.1580 0.6038 0.4420 0.047 Uiso 1 1 calc R . .
C12 C 0.1627(13) 0.7155(10) 0.2293(10) 0.035(4) Uani 1 1 d . . .
C13 C 0.0777(13) 0.7208(11) 0.1703(10) 0.040(4) Uani 1 1 d . . .
H13 H 0.0218 0.7584 0.1915 0.048 Uiso 1 1 calc R . .
C14 C 0.0692(14) 0.6739(11) 0.0807(10) 0.046(4) Uani 1 1 d . . .
H14 H 0.0066 0.6740 0.0429 0.055 Uiso 1 1 calc R . .
C15 C 0.1609(15) 0.6262(12) 0.0504(10) 0.048(4) Uani 1 1 d . . .
C16 C 0.2429(14) 0.6188(11) 0.1033(10) 0.046(4) Uani 1 1 d . . .
H16 H 0.2999 0.5836 0.0799 0.055 Uiso 1 1 calc R . .
C17 C 0.2492(13) 0.6619(11) 0.1948(10) 0.041(4) Uani 1 1 d . . .
H17 H 0.3093 0.6555 0.2325 0.049 Uiso 1 1 calc R . .
C18 C 0.3258(13) 0.9814(10) 0.4022(10) 0.034(4) Uani 1 1 d . . .
C19 C 0.3790(13) 0.9611(11) 0.3222(10) 0.039(4) Uani 1 1 d . . .
H19 H 0.3440 0.9122 0.2758 0.047 Uiso 1 1 calc R . .
C20 C 0.4857(13) 1.0123(11) 0.3080(11) 0.044(4) Uani 1 1 d . . .
H20 H 0.5228 0.9947 0.2547 0.052 Uiso 1 1 calc R . .
C21 C 0.5343(13) 1.0899(11) 0.3756(10) 0.041(4) Uani 1 1 d . . .
C22 C 0.4815(13) 1.1122(11) 0.4558(10) 0.041(4) Uani 1 1 d . . .
H22 H 0.5154 1.1629 0.5012 0.049 Uiso 1 1 calc R . .
C23 C 0.3778(13) 1.0597(10) 0.4700(10) 0.037(4) Uani 1 1 d . . .
H23 H 0.3423 1.0762 0.5243 0.044 Uiso 1 1 calc R . .
C24 C -0.0336(14) 0.9571(11) 0.3865(10) 0.037(4) Uani 1 1 d . . .
C25 C 0.0203(14) 1.0444(11) 0.3574(11) 0.052(4) Uani 1 1 d . . .
H25A H 0.0455 1.0271 0.2968 0.078 Uiso 1 1 calc R . .
H25B H 0.0841 1.0739 0.3976 0.078 Uiso 1 1 calc R . .
H25C H -0.0329 1.0900 0.3584 0.078 Uiso 1 1 calc R . .
C26 C 0.4428(12) 0.3828(11) 0.1946(10) 0.039(4) Uani 1 1 d . . .
C27 C 0.5227(13) 0.4401(11) 0.2750(9) 0.038(4) Uani 1 1 d . . .
H27 H 0.6015 0.4331 0.2612 0.046 Uiso 1 1 calc R . .
C28 C 0.4883(12) 0.3913(11) 0.3557(9) 0.037(4) Uani 1 1 d . . .
C29 C 0.3854(12) 0.3343(11) 0.3292(10) 0.038(4) Uani 1 1 d . . .
C30 C 0.3129(12) 0.2751(11) 0.3858(9) 0.040(4) Uani 1 1 d . . .
H30A H 0.2357 0.2650 0.3631 0.061 Uiso 1 1 calc R . .
H30B H 0.3178 0.3095 0.4477 0.061 Uiso 1 1 calc R . .
H30C H 0.3389 0.2129 0.3829 0.061 Uiso 1 1 calc R . .
C31 C 0.2519(13) 0.2783(12) 0.1962(10) 0.043(4) Uani 1 1 d . . .
C32 C 0.2398(13) 0.1771(13) 0.1747(10) 0.047(4) Uani 1 1 d . . .
H32 H 0.2987 0.1446 0.1887 0.056 Uiso 1 1 calc R . .
C33 C 0.1399(14) 0.1237(13) 0.1324(11) 0.054(5) Uani 1 1 d . . .
H33 H 0.1329 0.0558 0.1161 0.065 Uiso 1 1 calc R . .
C34 C 0.0501(14) 0.1730(14) 0.1147(11) 0.056(5) Uani 1 1 d . . .
C35 C 0.0627(14) 0.2736(13) 0.1349(11) 0.053(5) Uani 1 1 d . . .
H35 H 0.0042 0.3066 0.1211 0.063 Uiso 1 1 calc R . .
C36 C 0.1637(13) 0.3258(12) 0.1763(10) 0.046(4) Uani 1 1 d . . .
H36 H 0.1718 0.3938 0.1906 0.055 Uiso 1 1 calc R . .
C37 C 0.4974(13) 0.3075(12) 0.1285(10) 0.042(4) Uani 1 1 d . . .
C38 C 0.5557(13) 0.2435(12) 0.1562(11) 0.045(4) Uani 1 1 d . . .
H38 H 0.5682 0.2480 0.2183 0.054 Uiso 1 1 calc R . .
C39 C 0.5978(13) 0.1724(13) 0.0986(11) 0.051(4) Uani 1 1 d . . .
H39 H 0.6367 0.1285 0.1213 0.062 Uiso 1 1 calc R . .
C40 C 0.5831(14) 0.1651(13) 0.0070(11) 0.051(5) Uani 1 1 d . . .
C41 C 0.5262(14) 0.2268(13) -0.0247(11) 0.054(5) Uani 1 1 d . . .
H41 H 0.5157 0.2215 -0.0870 0.065 Uiso 1 1 calc R . .
C42 C 0.4829(13) 0.2978(12) 0.0330(10) 0.046(4) Uani 1 1 d . . .
H42 H 0.4432 0.3408 0.0096 0.056 Uiso 1 1 calc R . .
C43 C 0.5814(13) 0.6148(12) 0.2574(10) 0.040(4) Uani 1 1 d . . .
C44 C 0.5788(13) 0.7165(12) 0.3015(10) 0.043(4) Uani 1 1 d . . .
H44 H 0.5338 0.7331 0.3505 0.052 Uiso 1 1 calc R . .
C45 C 0.6486(14) 0.7877(13) 0.2653(11) 0.050(4) Uani 1 1 d . . .
H45 H 0.6504 0.8533 0.2918 0.061 Uiso 1 1 calc R . .
C46 C 0.7140(14) 0.7641(13) 0.1926(11) 0.050(4) Uani 1 1 d . . .
C47 C 0.7107(14) 0.6664(13) 0.1507(11) 0.051(4) Uani 1 1 d . . .
H47 H 0.7516 0.6494 0.0994 0.061 Uiso 1 1 calc R . .
C48 C 0.6453(13) 0.5954(12) 0.1870(10) 0.045(4) Uani 1 1 d . . .
H48 H 0.6463 0.5302 0.1605 0.054 Uiso 1 1 calc R . .
C49 C 0.5483(12) 0.4050(11) 0.4394(11) 0.037(4) Uani 1 1 d . . .
C50 C 0.6624(12) 0.4685(11) 0.4479(10) 0.042(4) Uani 1 1 d . . .
H50A H 0.6794 0.4987 0.5103 0.063 Uiso 1 1 calc R . .
H50B H 0.6607 0.5183 0.4121 0.063 Uiso 1 1 calc R . .
H50C H 0.7196 0.4289 0.4266 0.063 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
Br1 0.112(2) 0.0499(14) 0.145(2) 0.0248(15) 0.0199(17) -0.0064(13)
Br2 0.092(2) 0.135(3) 0.137(2) 0.043(2) -0.0055(17) -0.0080(17)
Br3 0.0768(18) 0.160(3) 0.153(3) -0.028(2) -0.0227(18) -0.0198(18)
Br4 0.184(4) 0.158(4) 0.192(4) 0.067(3) -0.001(3) -0.019(3)
Cl1 0.089(4) 0.117(5) 0.071(3) -0.052(3) 0.000(3) 0.038(4)
Cl2 0.149(5) 0.106(5) 0.038(3) -0.019(3) 0.005(3) 0.058(4)
N1 0.039(8) 0.026(7) 0.034(7) 0.007(6) 0.004(6) 0.010(6)
N2 0.042(8) 0.030(7) 0.034(7) 0.005(6) 0.002(6) 0.009(6)
N3 0.039(8) 0.046(8) 0.036(8) 0.003(7) 0.001(7) 0.008(7)
N4 0.038(8) 0.044(9) 0.037(7) 0.006(7) 0.002(6) 0.011(6)
O1 0.038(6) 0.028(6) 0.036(6) 0.007(5) -0.001(5) 0.005(5)
O2 0.055(7) 0.041(7) 0.050(7) 0.003(5) 0.002(6) 0.019(6)
O3 0.042(6) 0.042(7) 0.039(6) 0.007(5) -0.005(5) 0.008(6)
O4 0.042(6) 0.040(6) 0.033(6) 0.005(5) -0.004(5) 0.014(5)
C1 0.041(9) 0.029(9) 0.033(8) 0.005(7) 0.003(7) 0.010(7)
C2 0.043(10) 0.029(9) 0.035(8) 0.006(7) 0.003(7) 0.010(7)
C3 0.040(9) 0.029(9) 0.033(8) 0.006(7) 0.002(7) 0.012(7)
C4 0.042(10) 0.030(9) 0.034(8) 0.005(7) 0.001(7) 0.009(8)
C5 0.041(10) 0.033(9) 0.044(9) 0.007(8) 0.011(8) 0.005(7)
C6 0.042(10) 0.029(9) 0.037(9) 0.007(8) 0.007(8) 0.008(8)
C7 0.043(10) 0.031(10) 0.038(9) 0.006(8) 0.004(8) 0.008(8)
C8 0.045(10) 0.032(10) 0.044(9) 0.004(8) 0.007(8) 0.005(8)
C9 0.046(10) 0.035(9) 0.046(10) 0.005(8) 0.009(8) 0.005(8)
C10 0.047(10) 0.030(10) 0.050(10) 0.009(8) 0.004(9) 0.009(8)
C11 0.045(10) 0.031(9) 0.042(9) 0.004(8) 0.004(8) 0.007(8)
C12 0.041(9) 0.031(9) 0.034(9) 0.004(7) 0.006(8) 0.009(7)
C13 0.046(10) 0.037(9) 0.037(9) 0.000(8) 0.005(8) 0.012(8)
C14 0.055(11) 0.045(10) 0.036(10) -0.003(8) 0.003(8) 0.014(9)
C15 0.058(12) 0.047(11) 0.035(10) -0.006(8) 0.007(9) 0.010(9)
C16 0.055(11) 0.045(11) 0.038(10) -0.002(8) 0.006(9) 0.021(9)
C17 0.046(10) 0.037(10) 0.037(9) 0.000(8) 0.003(8) 0.014(8)
C18 0.041(10) 0.028(9) 0.036(9) 0.006(7) 0.001(8) 0.012(8)
C19 0.046(10) 0.034(9) 0.038(9) 0.007(8) 0.001(8) 0.010(8)
C20 0.049(11) 0.040(10) 0.044(10) 0.008(9) 0.000(8) 0.010(8)
C21 0.046(10) 0.035(10) 0.043(10) 0.010(8) 0.000(8) 0.007(8)
C22 0.047(11) 0.032(9) 0.046(10) 0.010(8) -0.004(8) 0.013(8)
C23 0.043(10) 0.030(9) 0.040(9) 0.007(8) 0.001(8) 0.013(8)
C24 0.045(10) 0.030(9) 0.037(9) 0.005(7) 0.001(8) 0.011(8)
C25 0.065(12) 0.036(10) 0.055(11) 0.005(9) -0.002(9) 0.014(9)
C26 0.039(9) 0.045(10) 0.034(9) 0.005(8) 0.000(8) 0.011(8)
C27 0.038(9) 0.043(10) 0.034(9) 0.006(8) 0.000(7) 0.009(8)
C28 0.037(9) 0.042(10) 0.032(9) 0.005(8) 0.001(8) 0.010(8)
C29 0.036(9) 0.043(10) 0.036(9) 0.002(8) 0.002(8) 0.011(8)
C30 0.040(9) 0.048(10) 0.030(8) 0.004(8) -0.003(7) 0.001(8)
C31 0.038(10) 0.049(12) 0.038(9) 0.000(8) 0.001(8) 0.007(9)
C32 0.042(10) 0.052(12) 0.043(10) 0.000(9) 0.000(8) 0.006(9)
C33 0.046(11) 0.057(12) 0.054(11) -0.002(9) -0.002(9) 0.005(10)
C34 0.046(11) 0.063(13) 0.051(11) -0.003(10) -0.003(9) -0.002(10)
C35 0.046(11) 0.057(13) 0.052(11) 0.003(10) 0.000(9) 0.004(9)
C36 0.042(10) 0.049(11) 0.042(10) 0.002(9) 0.000(8) 0.004(9)
C37 0.042(10) 0.049(11) 0.035(9) 0.003(8) 0.001(8) 0.010(8)
C38 0.045(10) 0.051(11) 0.037(9) 0.000(9) 0.001(8) 0.010(9)
C39 0.050(11) 0.058(12) 0.042(10) -0.004(9) 0.003(9) 0.012(9)
C40 0.049(11) 0.058(12) 0.042(11) -0.007(9) 0.004(8) 0.012(9)
C41 0.053(11) 0.064(13) 0.040(10) -0.005(10) 0.000(9) 0.009(10)
C42 0.046(10) 0.053(11) 0.038(10) 0.001(9) 0.001(8) 0.010(9)
C43 0.040(10) 0.044(11) 0.036(9) 0.010(8) -0.002(8) 0.009(8)
C44 0.042(10) 0.046(11) 0.043(9) 0.012(9) 0.000(8) 0.010(8)
C45 0.053(11) 0.050(11) 0.051(11) 0.012(9) -0.005(9) 0.012(9)
C46 0.054(11) 0.050(12) 0.049(11) 0.019(10) 0.000(9) 0.005(9)
C47 0.050(11) 0.054(12) 0.048(10) 0.012(10) 0.000(9) 0.005(9)
C48 0.046(10) 0.047(11) 0.042(10) 0.009(9) 0.000(9) 0.009(9)
C49 0.034(9) 0.041(10) 0.036(10) 0.000(8) -0.001(8) 0.012(8)
C50 0.043(10) 0.041(10) 0.038(9) -0.003(8) -0.007(7) 0.007(8)
_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 C9 1.833(16) . ?
Br2 C21 1.835(16) . ?
Br3 C34 1.878(17) . ?
Br4 C46 1.857(17) . ?
Cl1 C40 1.753(17) . ?
Cl2 C15 1.796(16) . ?
N1 C4 1.353(17) . ?
N1 C6 1.443(17) . ?
N1 C1 1.516(18) . ?
N2 C18 1.400(18) . ?
N2 C2 1.482(17) . ?
N2 H2 0.8600 . ?
N3 C29 1.335(17) . ?
N3 C31 1.408(19) . ?
N3 C26 1.509(19) . ?
N4 C43 1.431(18) . ?
N4 C27 1.450(18) . ?
N4 H4 0.8600 . ?
O1 C1 1.396(16) . ?
O1 H1 0.8200 . ?
O2 C24 1.267(16) . ?
O3 C26 1.414(17) . ?
O3 H3 0.8200 . ?
O4 C49 1.220(17) . ?
C1 C12 1.513(19) . ?
C1 C2 1.549(19) . ?
C2 C3 1.495(19) . ?
C2 H2A 0.9800 . ?
C3 C4 1.361(19) . ?
C3 C24 1.458(19) . ?
C4 C5 1.454(19) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.35(2) . ?
C6 C11 1.393(19) . ?
C7 C8 1.39(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.35(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.40(2) . ?
C10 C11 1.45(2) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.354(19) . ?
C12 C17 1.409(19) . ?
C13 C14 1.378(19) . ?
C13 H13 0.9300 . ?
C14 C15 1.40(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.28(2) . ?
C16 C17 1.39(2) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.367(19) . ?
C18 C23 1.42(2) . ?
C19 C20 1.41(2) . ?
C19 H19 0.9300 . ?
C20 C21 1.40(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.37(2) . ?
C22 C23 1.39(2) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.45(2) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C37 1.53(2) . ?
C26 C27 1.55(2) . ?
C27 C28 1.535(19) . ?
C27 H27 0.9800 . ?
C28 C29 1.38(2) . ?
C28 C49 1.40(2) . ?
C29 C30 1.50(2) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C36 1.38(2) . ?
C31 C32 1.38(2) . ?
C32 C33 1.39(2) . ?
C32 H32 0.9300 . ?
C33 C34 1.40(2) . ?
C33 H33 0.9300 . ?
C34 C35 1.38(2) . ?
C35 C36 1.39(2) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C38 1.33(2) . ?
C37 C42 1.42(2) . ?
C38 C39 1.35(2) . ?
C38 H38 0.9300 . ?
C39 C40 1.37(2) . ?
C39 H39 0.9300 . ?
C40 C41 1.32(2) . ?
C41 C42 1.36(2) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C48 1.32(2) . ?
C43 C44 1.46(2) . ?
C44 C45 1.41(2) . ?
C44 H44 0.9300 . ?
C45 C46 1.37(2) . ?
C45 H45 0.9300 . ?
C46 C47 1.39(2) . ?
C47 C48 1.38(2) . ?
C47 H47 0.9300 . ?
C48 H48 0.9300 . ?
C49 C50 1.51(2) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
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
C4 N1 C6 123.0(12) . . ?
C4 N1 C1 113.3(11) . . ?
C6 N1 C1 122.7(10) . . ?
C18 N2 C2 123.5(11) . . ?
C18 N2 H2 118.3 . . ?
C2 N2 H2 118.3 . . ?
C29 N3 C31 128.6(13) . . ?
C29 N3 C26 110.2(12) . . ?
C31 N3 C26 121.0(12) . . ?
C43 N4 C27 122.2(12) . . ?
C43 N4 H4 118.9 . . ?
C27 N4 H4 118.9 . . ?
C1 O1 H1 109.5 . . ?
C26 O3 H3 109.5 . . ?
O1 C1 C12 110.6(11) . . ?
O1 C1 N1 111.1(11) . . ?
C12 C1 N1 107.4(11) . . ?
O1 C1 C2 113.9(12) . . ?
C12 C1 C2 113.1(12) . . ?
N1 C1 C2 100.1(10) . . ?
N2 C2 C3 110.4(11) . . ?
N2 C2 C1 110.0(11) . . ?
C3 C2 C1 105.4(12) . . ?
N2 C2 H2A 110.3 . . ?
C3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
C4 C3 C24 125.9(14) . . ?
C4 C3 C2 110.3(12) . . ?
C24 C3 C2 123.8(13) . . ?
N1 C4 C3 110.0(13) . . ?
N1 C4 C5 122.8(13) . . ?
C3 C4 C5 127.2(13) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 119.4(14) . . ?
C7 C6 N1 123.5(14) . . ?
C11 C6 N1 116.8(13) . . ?
C6 C7 C8 122.5(15) . . ?
C6 C7 H7 118.8 . . ?
C8 C7 H7 118.8 . . ?
C9 C8 C7 119.7(15) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 121.2(15) . . ?
C8 C9 Br1 122.0(12) . . ?
C10 C9 Br1 116.7(12) . . ?
C9 C10 C11 117.9(14) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
C6 C11 C10 119.0(14) . . ?
C6 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C13 C12 C17 117.2(13) . . ?
C13 C12 C1 121.3(12) . . ?
C17 C12 C1 121.5(13) . . ?
C12 C13 C14 123.9(14) . . ?
C12 C13 H13 118.0 . . ?
C14 C13 H13 118.0 . . ?
C13 C14 C15 115.4(15) . . ?
C13 C14 H14 122.3 . . ?
C15 C14 H14 122.3 . . ?
C16 C15 C14 122.8(15) . . ?
C16 C15 Cl2 120.3(13) . . ?
C14 C15 Cl2 116.7(13) . . ?
C15 C16 C17 121.8(15) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C16 C17 C12 118.5(14) . . ?
C16 C17 H17 120.7 . . ?
C12 C17 H17 120.7 . . ?
C19 C18 N2 122.4(14) . . ?
C19 C18 C23 118.0(15) . . ?
N2 C18 C23 119.6(13) . . ?
C18 C19 C20 121.9(14) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 H19 119.0 . . ?
C21 C20 C19 118.7(14) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C22 C21 C20 120.1(15) . . ?
C22 C21 Br2 117.8(12) . . ?
C20 C21 Br2 121.8(12) . . ?
C21 C22 C23 120.6(15) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C18 120.5(14) . . ?
C22 C23 H23 119.8 . . ?
C18 C23 H23 119.8 . . ?
O2 C24 C25 119.3(13) . . ?
O2 C24 C3 121.5(14) . . ?
C25 C24 C3 119.2(14) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O3 C26 N3 109.8(11) . . ?
O3 C26 C37 109.9(11) . . ?
N3 C26 C37 109.0(12) . . ?
O3 C26 C27 112.0(12) . . ?
N3 C26 C27 101.7(11) . . ?
C37 C26 C27 114.2(12) . . ?
N4 C27 C28 111.0(12) . . ?
N4 C27 C26 111.4(12) . . ?
C28 C27 C26 105.0(12) . . ?
N4 C27 H27 109.8 . . ?
C28 C27 H27 109.8 . . ?
C26 C27 H27 109.8 . . ?
C29 C28 C49 127.9(14) . . ?
C29 C28 C27 105.4(12) . . ?
C49 C28 C27 126.7(14) . . ?
N3 C29 C28 115.0(14) . . ?
N3 C29 C30 118.4(13) . . ?
C28 C29 C30 126.5(13) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 119.4(15) . . ?
C36 C31 N3 121.6(15) . . ?
C32 C31 N3 118.8(14) . . ?
C31 C32 C33 120.4(16) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C32 C33 C34 119.4(17) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C35 C34 C33 120.1(16) . . ?
C35 C34 Br3 118.1(14) . . ?
C33 C34 Br3 121.8(14) . . ?
C34 C35 C36 119.5(16) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C31 C36 C35 121.0(16) . . ?
C31 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
C38 C37 C42 115.7(15) . . ?
C38 C37 C26 122.5(13) . . ?
C42 C37 C26 121.7(14) . . ?
C37 C38 C39 123.2(15) . . ?
C37 C38 H38 118.4 . . ?
C39 C38 H38 118.4 . . ?
C38 C39 C40 119.9(17) . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C41 C40 C39 119.7(16) . . ?
C41 C40 Cl1 121.1(13) . . ?
C39 C40 Cl1 119.1(15) . . ?
C40 C41 C42 120.5(16) . . ?
C40 C41 H41 119.7 . . ?
C42 C41 H41 119.7 . . ?
C41 C42 C37 121.0(16) . . ?
C41 C42 H42 119.5 . . ?
C37 C42 H42 119.5 . . ?
C48 C43 N4 124.9(15) . . ?
C48 C43 C44 119.6(15) . . ?
N4 C43 C44 115.4(13) . . ?
C45 C44 C43 115.8(15) . . ?
C45 C44 H44 122.1 . . ?
C43 C44 H44 122.1 . . ?
C46 C45 C44 122.4(16) . . ?
C46 C45 H45 118.8 . . ?
C44 C45 H45 118.8 . . ?
C45 C46 C47 119.7(16) . . ?
C45 C46 Br4 119.6(14) . . ?
C47 C46 Br4 120.6(13) . . ?
C48 C47 C46 118.6(16) . . ?
C48 C47 H47 120.7 . . ?
C46 C47 H47 120.7 . . ?
C43 C48 C47 123.7(16) . . ?
C43 C48 H48 118.1 . . ?
C47 C48 H48 118.1 . . ?
O4 C49 C28 125.1(14) . . ?
O4 C49 C50 118.6(13) . . ?
C28 C49 C50 116.3(14) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
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
C4 N1 C1 O1 127.4(12) . . . . ?
C6 N1 C1 O1 -63.3(16) . . . . ?
C4 N1 C1 C12 -111.5(13) . . . . ?
C6 N1 C1 C12 57.7(16) . . . . ?
C4 N1 C1 C2 6.8(14) . . . . ?
C6 N1 C1 C2 176.0(12) . . . . ?
C18 N2 C2 C3 -147.2(12) . . . . ?
C18 N2 C2 C1 96.8(15) . . . . ?
O1 C1 C2 N2 -8.0(16) . . . . ?
C12 C1 C2 N2 -135.5(12) . . . . ?
N1 C1 C2 N2 110.6(12) . . . . ?
O1 C1 C2 C3 -127.0(12) . . . . ?
C12 C1 C2 C3 105.5(14) . . . . ?
N1 C1 C2 C3 -8.4(13) . . . . ?
N2 C2 C3 C4 -110.6(13) . . . . ?
C1 C2 C3 C4 8.2(16) . . . . ?
N2 C2 C3 C24 68.6(17) . . . . ?
C1 C2 C3 C24 -172.6(13) . . . . ?
C6 N1 C4 C3 -171.3(12) . . . . ?
C1 N1 C4 C3 -2.1(16) . . . . ?
C6 N1 C4 C5 9(2) . . . . ?
C1 N1 C4 C5 178.7(12) . . . . ?
C24 C3 C4 N1 176.8(13) . . . . ?
C2 C3 C4 N1 -4.0(17) . . . . ?
C24 C3 C4 C5 -4(2) . . . . ?
C2 C3 C4 C5 175.1(13) . . . . ?
C4 N1 C6 C7 57.4(19) . . . . ?
C1 N1 C6 C7 -110.8(16) . . . . ?
C4 N1 C6 C11 -128.3(14) . . . . ?
C1 N1 C6 C11 63.5(17) . . . . ?
C11 C6 C7 C8 7(2) . . . . ?
N1 C6 C7 C8 -178.8(13) . . . . ?
C6 C7 C8 C9 -6(2) . . . . ?
C7 C8 C9 C10 3(2) . . . . ?
C7 C8 C9 Br1 178.3(11) . . . . ?
C8 C9 C10 C11 -1(2) . . . . ?
Br1 C9 C10 C11 -176.9(10) . . . . ?
C7 C6 C11 C10 -5(2) . . . . ?
N1 C6 C11 C10 -179.8(12) . . . . ?
C9 C10 C11 C6 2(2) . . . . ?
O1 C1 C12 C13 178.6(13) . . . . ?
N1 C1 C12 C13 57.3(17) . . . . ?
C2 C1 C12 C13 -52.2(19) . . . . ?
O1 C1 C12 C17 1.7(19) . . . . ?
N1 C1 C12 C17 -119.7(14) . . . . ?
C2 C1 C12 C17 130.9(14) . . . . ?
C17 C12 C13 C14 3(2) . . . . ?
C1 C12 C13 C14 -174.2(14) . . . . ?
C12 C13 C14 C15 -6(2) . . . . ?
C13 C14 C15 C16 6(2) . . . . ?
C13 C14 C15 Cl2 -178.8(12) . . . . ?
C14 C15 C16 C17 -3(3) . . . . ?
Cl2 C15 C16 C17 -178.2(13) . . . . ?
C15 C16 C17 C12 0(2) . . . . ?
C13 C12 C17 C16 0(2) . . . . ?
C1 C12 C17 C16 177.5(14) . . . . ?
C2 N2 C18 C19 -22(2) . . . . ?
C2 N2 C18 C23 158.2(12) . . . . ?
N2 C18 C19 C20 -176.8(12) . . . . ?
C23 C18 C19 C20 3(2) . . . . ?
C18 C19 C20 C21 -4(2) . . . . ?
C19 C20 C21 C22 3(2) . . . . ?
C19 C20 C21 Br2 177.9(11) . . . . ?
C20 C21 C22 C23 -2(2) . . . . ?
Br2 C21 C22 C23 -176.6(10) . . . . ?
C21 C22 C23 C18 1(2) . . . . ?
C19 C18 C23 C22 -1.8(19) . . . . ?
N2 C18 C23 C22 178.4(12) . . . . ?
C4 C3 C24 O2 6(2) . . . . ?
C2 C3 C24 O2 -172.8(13) . . . . ?
C4 C3 C24 C25 -171.5(14) . . . . ?
C2 C3 C24 C25 9(2) . . . . ?
C29 N3 C26 O3 -132.1(12) . . . . ?
C31 N3 C26 O3 52.4(17) . . . . ?
C29 N3 C26 C37 107.5(13) . . . . ?
C31 N3 C26 C37 -68.0(17) . . . . ?
C29 N3 C26 C27 -13.3(15) . . . . ?
C31 N3 C26 C27 171.1(13) . . . . ?
C43 N4 C27 C28 148.4(13) . . . . ?
C43 N4 C27 C26 -95.0(15) . . . . ?
O3 C26 C27 N4 13.0(17) . . . . ?
N3 C26 C27 N4 -104.1(13) . . . . ?
C37 C26 C27 N4 138.7(13) . . . . ?
O3 C26 C27 C28 133.2(12) . . . . ?
N3 C26 C27 C28 16.1(14) . . . . ?
C37 C26 C27 C28 -101.1(14) . . . . ?
N4 C27 C28 C29 106.4(13) . . . . ?
C26 C27 C28 C29 -14.1(15) . . . . ?
N4 C27 C28 C49 -71.8(18) . . . . ?
C26 C27 C28 C49 167.7(14) . . . . ?
C31 N3 C29 C28 -179.9(14) . . . . ?
C26 N3 C29 C28 4.9(17) . . . . ?
C31 N3 C29 C30 3(2) . . . . ?
C26 N3 C29 C30 -172.4(12) . . . . ?
C49 C28 C29 N3 -175.7(14) . . . . ?
C27 C28 C29 N3 6.1(17) . . . . ?
C49 C28 C29 C30 1(3) . . . . ?
C27 C28 C29 C30 -176.8(13) . . . . ?
C29 N3 C31 C36 105.5(19) . . . . ?
C26 N3 C31 C36 -79.8(18) . . . . ?
C29 N3 C31 C32 -71(2) . . . . ?
C26 N3 C31 C32 104.1(17) . . . . ?
C36 C31 C32 C33 1(2) . . . . ?
N3 C31 C32 C33 176.8(13) . . . . ?
C31 C32 C33 C34 -2(2) . . . . ?
C32 C33 C34 C35 3(3) . . . . ?
C32 C33 C34 Br3 -176.8(12) . . . . ?
C33 C34 C35 C36 -2(3) . . . . ?
Br3 C34 C35 C36 177.5(11) . . . . ?
C32 C31 C36 C35 0(2) . . . . ?
N3 C31 C36 C35 -176.0(14) . . . . ?
C34 C35 C36 C31 1(2) . . . . ?
O3 C26 C37 C38 175.0(15) . . . . ?
N3 C26 C37 C38 -64.7(18) . . . . ?
C27 C26 C37 C38 48(2) . . . . ?
O3 C26 C37 C42 -9(2) . . . . ?
N3 C26 C37 C42 111.5(16) . . . . ?
C27 C26 C37 C42 -135.7(15) . . . . ?
C42 C37 C38 C39 -1(2) . . . . ?
C26 C37 C38 C39 175.4(15) . . . . ?
C37 C38 C39 C40 1(3) . . . . ?
C38 C39 C40 C41 -1(3) . . . . ?
C38 C39 C40 Cl1 179.1(13) . . . . ?
C39 C40 C41 C42 0(3) . . . . ?
Cl1 C40 C41 C42 -179.7(13) . . . . ?
C40 C41 C42 C37 0(3) . . . . ?
C38 C37 C42 C41 0(2) . . . . ?
C26 C37 C42 C41 -176.0(14) . . . . ?
C27 N4 C43 C48 18(2) . . . . ?
C27 N4 C43 C44 -163.8(12) . . . . ?
C48 C43 C44 C45 -1(2) . . . . ?
N4 C43 C44 C45 -179.5(12) . . . . ?
C43 C44 C45 C46 1(2) . . . . ?
C44 C45 C46 C47 1(2) . . . . ?
C44 C45 C46 Br4 177.2(11) . . . . ?
C45 C46 C47 C48 -3(2) . . . . ?
Br4 C46 C47 C48 -179.0(12) . . . . ?
N4 C43 C48 C47 177.4(14) . . . . ?
C44 C43 C48 C47 -1(2) . . . . ?
C46 C47 C48 C43 3(2) . . . . ?
C29 C28 C49 O4 -4(3) . . . . ?
C27 C28 C49 O4 173.9(14) . . . . ?
C29 C28 C49 C50 177.3(14) . . . . ?
C27 C28 C49 C50 -5(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.065
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.199