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


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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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_compound2
_database_code_depnum_ccdc_archive 'CCDC 917193'
#TrackingRef '16371_web_deposit_cif_file_0_DattatrayaH.Dethe_1356085110.dethe.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H27 Br N2 O2, C H2 Cl2 '
_chemical_formula_sum            'C31 H29 Br Cl2 N2 O2'
_chemical_formula_weight         612.37
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P n 21 a '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, y, -z+1/2'
_cell_length_a                   11.149(5)
_cell_length_b                   19.600(5)
_cell_length_c                   25.468(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     5565(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4413
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      24.42
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2512
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            29575
_diffrn_reflns_av_R_equivalents  0.1094
_diffrn_reflns_av_sigmaI/netI    0.0996
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8083
_reflns_number_gt                5359
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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^)+(0.1165P)^2^+21.4862P] 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   0.00
_refine_ls_number_reflns         8083
_refine_ls_number_parameters     691
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0747
_refine_ls_wR_factor_ref         0.2300
_refine_ls_wR_factor_gt          0.1845
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3222(10) 0.7664(8) 0.7300(4) 0.036(4) Uani 1 1 d . . .
C2 C 0.4238(10) 0.7315(8) 0.7431(4) 0.033(3) Uani 1 1 d . . .
H2 H 0.4747 0.7160 0.7168 0.040 Uiso 1 1 calc R . .
C3 C 0.4523(10) 0.7188(8) 0.7949(5) 0.033(3) Uani 1 1 d . . .
H3 H 0.5197 0.6940 0.8047 0.039 Uiso 1 1 calc R . .
C4 C 0.3707(10) 0.7466(7) 0.8325(4) 0.025(3) Uani 1 1 d . . .
C5 C 0.2709(9) 0.7824(8) 0.8195(4) 0.025(3) Uani 1 1 d . . .
C6 C 0.2402(10) 0.7932(8) 0.7651(4) 0.029(3) Uani 1 1 d . . .
H6 H 0.1713 0.8162 0.7546 0.034 Uiso 1 1 calc R . .
C7 C 0.4738(10) 0.7123(8) 0.9173(4) 0.036(3) Uani 1 1 d . . .
H7A H 0.4531 0.7121 0.9539 0.054 Uiso 1 1 calc R . .
H7B H 0.5471 0.7372 0.9124 0.054 Uiso 1 1 calc R . .
H7C H 0.4843 0.6662 0.9053 0.054 Uiso 1 1 calc R . .
C8 C 0.2824(9) 0.7795(8) 0.9067(4) 0.029(3) Uani 1 1 d . . .
H8 H 0.2675 0.7862 0.9423 0.034 Uiso 1 1 calc R . .
C9 C 0.2116(10) 0.8032(7) 0.8674(4) 0.031(3) Uani 1 1 d . . .
C10 C 0.1002(10) 0.8461(7) 0.8712(4) 0.029(3) Uani 1 1 d . . .
H10 H 0.0371 0.8265 0.8490 0.035 Uiso 1 1 calc R . .
C11 C 0.1152(10) 0.9229(8) 0.8585(4) 0.032(3) Uani 1 1 d . . .
H11 H 0.1943 0.9303 0.8428 0.039 Uiso 1 1 calc R . .
C12 C 0.0200(10) 0.9426(7) 0.8196(5) 0.029(3) Uani 1 1 d . . .
C13 C -0.0403(10) 0.9347(9) 0.7281(4) 0.041(4) Uani 1 1 d . . .
H13A H -0.0584 0.9830 0.7262 0.049 Uiso 1 1 calc R . .
H13B H -0.1143 0.9105 0.7355 0.049 Uiso 1 1 calc R . .
C14 C 0.0089(14) 0.9115(10) 0.6778(5) 0.055(5) Uani 1 1 d . . .
H14A H 0.0235 0.8633 0.6793 0.082 Uiso 1 1 calc R . .
H14B H 0.0828 0.9349 0.6709 0.082 Uiso 1 1 calc R . .
H14C H -0.0474 0.9211 0.6502 0.082 Uiso 1 1 calc R . .
C15 C 0.1055(10) 0.9652(7) 0.9102(4) 0.029(3) Uani 1 1 d . . .
H15 H 0.0421 0.9993 0.9059 0.035 Uiso 1 1 calc R . .
C16 C 0.2238(10) 1.0022(8) 0.9228(4) 0.027(3) Uani 1 1 d . . .
C17 C 0.2277(10) 1.0727(8) 0.9193(4) 0.033(3) Uani 1 1 d . . .
H17 H 0.1592 1.0968 0.9097 0.040 Uiso 1 1 calc R . .
C18 C 0.3329(13) 1.1074(9) 0.9299(5) 0.047(4) Uani 1 1 d . . .
H18 H 0.3342 1.1548 0.9275 0.056 Uiso 1 1 calc R . .
C19 C 0.4359(10) 1.0730(9) 0.9439(4) 0.033(3) Uani 1 1 d . . .
H19 H 0.5062 1.0968 0.9511 0.040 Uiso 1 1 calc R . .
C20 C 0.4331(10) 1.0027(9) 0.9473(4) 0.037(4) Uani 1 1 d . . .
H20 H 0.5027 0.9788 0.9554 0.045 Uiso 1 1 calc R . .
C21 C 0.3234(10) 0.9663(8) 0.9381(4) 0.032(3) Uani 1 1 d . . .
H21 H 0.3199 0.9193 0.9425 0.038 Uiso 1 1 calc R . .
C22 C 0.0652(9) 0.9143(7) 0.9477(4) 0.023(3) Uani 1 1 d . . .
C23 C 0.0264(9) 0.9116(7) 0.9998(4) 0.025(3) Uani 1 1 d . . .
C24 C 0.0236(11) 0.9693(8) 1.0390(5) 0.038(4) Uani 1 1 d . . .
H24A H 0.0321 1.0120 1.0209 0.058 Uiso 1 1 calc R . .
H24B H 0.0883 0.9640 1.0635 0.058 Uiso 1 1 calc R . .
H24C H -0.0514 0.9687 1.0575 0.058 Uiso 1 1 calc R . .
C25 C -0.0078(10) 0.8433(7) 1.0085(4) 0.025(3) Uani 1 1 d . . .
C26 C 0.0127(9) 0.8043(7) 0.9619(4) 0.024(3) Uani 1 1 d . . .
C27 C -0.0103(10) 0.7369(8) 0.9579(4) 0.030(3) Uani 1 1 d . . .
H27 H 0.0078 0.7130 0.9274 0.036 Uiso 1 1 calc R . .
C28 C -0.0629(10) 0.7036(8) 1.0018(5) 0.034(3) Uani 1 1 d . . .
H28 H -0.0832 0.6577 1.0004 0.041 Uiso 1 1 calc R . .
C29 C -0.0839(10) 0.7433(8) 1.0487(4) 0.034(4) Uani 1 1 d . . .
H29 H -0.1175 0.7218 1.0778 0.041 Uiso 1 1 calc R . .
C30 C -0.0580(10) 0.8073(7) 1.0520(5) 0.025(3) Uani 1 1 d U . .
H30 H -0.0723 0.8305 1.0833 0.031 Uiso 1 1 calc R . .
C31 C 0.4117(9) 1.0685(8) 0.2693(4) 0.029(3) Uani 1 1 d . . .
C32 C 0.3083(9) 1.1003(7) 0.2528(4) 0.029(3) Uani 1 1 d . . .
H32 H 0.2580 1.1206 0.2774 0.035 Uiso 1 1 calc R . .
C33 C 0.2781(10) 1.1025(7) 0.1997(4) 0.029(3) Uani 1 1 d . . .
H33 H 0.2077 1.1230 0.1881 0.034 Uiso 1 1 calc R . .
C34 C 0.3586(9) 1.0725(8) 0.1649(3) 0.024(3) Uani 1 1 d . . .
C35 C 0.4638(9) 1.0402(6) 0.1818(4) 0.018(2) Uani 1 1 d U . .
C36 C 0.4924(9) 1.0367(7) 0.2359(4) 0.025(3) Uani 1 1 d . . .
H36 H 0.5606 1.0145 0.2481 0.030 Uiso 1 1 calc R . .
C37 C 0.2579(9) 1.0980(8) 0.0783(4) 0.030(3) Uani 1 1 d . . .
H37A H 0.2742 1.0882 0.0420 0.045 Uiso 1 1 calc R . .
H37B H 0.2590 1.1465 0.0836 0.045 Uiso 1 1 calc R . .
H37C H 0.1805 1.0804 0.0875 0.045 Uiso 1 1 calc R . .
C38 C 0.4488(9) 1.0325(7) 0.0948(4) 0.029(3) Uani 1 1 d . . .
H38 H 0.4658 1.0231 0.0598 0.034 Uiso 1 1 calc R . .
C39 C 0.5217(9) 1.0137(7) 0.1352(4) 0.025(3) Uani 1 1 d . . .
C40 C 0.6362(9) 0.9731(7) 0.1335(4) 0.026(3) Uani 1 1 d . . .
H40 H 0.6974 0.9946 0.1555 0.031 Uiso 1 1 calc R . .
C41 C 0.6212(10) 0.8976(8) 0.1486(4) 0.026(3) Uani 1 1 d . . .
H41 H 0.5444 0.8921 0.1668 0.032 Uiso 1 1 calc R . .
C42 C 0.7222(13) 0.8777(8) 0.1861(4) 0.036(3) Uani 1 1 d . . .
C43 C 0.7863(13) 0.8873(10) 0.2750(4) 0.052(5) Uani 1 1 d . . .
H43A H 0.8595 0.9129 0.2690 0.062 Uiso 1 1 calc R . .
H43B H 0.8052 0.8390 0.2756 0.062 Uiso 1 1 calc R . .
C44 C 0.7272(13) 0.9089(9) 0.3254(5) 0.044(4) Uani 1 1 d . . .
H44A H 0.6496 0.8879 0.3280 0.065 Uiso 1 1 calc R . .
H44B H 0.7184 0.9576 0.3257 0.065 Uiso 1 1 calc R . .
H44C H 0.7758 0.8950 0.3546 0.065 Uiso 1 1 calc R . .
C45 C 0.6189(9) 0.8536(8) 0.0972(4) 0.032(3) Uani 1 1 d . . .
H45 H 0.6759 0.8158 0.1008 0.038 Uiso 1 1 calc R . .
C46 C 0.4974(10) 0.8253(7) 0.0857(4) 0.026(3) Uani 1 1 d U . .
C47 C 0.4617(11) 0.7675(8) 0.1097(5) 0.042(4) Uani 1 1 d . . .
H47 H 0.5153 0.7446 0.1314 0.051 Uiso 1 1 calc R . .
C48 C 0.3436(12) 0.7403(9) 0.1028(6) 0.050(4) Uani 1 1 d . . .
H48 H 0.3203 0.7004 0.1197 0.060 Uiso 1 1 calc R . .
C49 C 0.2659(11) 0.7746(9) 0.0706(5) 0.038(3) Uani 1 1 d . . .
H49 H 0.1884 0.7582 0.0656 0.045 Uiso 1 1 calc R . .
C50 C 0.3009(10) 0.8311(8) 0.0463(5) 0.036(4) Uani 1 1 d . . .
H50 H 0.2474 0.8542 0.0247 0.043 Uiso 1 1 calc R . .
C51 C 0.4149(10) 0.8559(8) 0.0528(5) 0.035(3) Uani 1 1 d . . .
H51 H 0.4375 0.8948 0.0343 0.042 Uiso 1 1 calc R . .
C52 C 0.6660(10) 0.9032(7) 0.0571(4) 0.029(3) Uani 1 1 d . . .
C53 C 0.6973(9) 0.9053(7) 0.0054(4) 0.028(3) Uani 1 1 d . . .
C54 C 0.6946(11) 0.8476(9) -0.0331(5) 0.046(4) Uani 1 1 d . . .
H54A H 0.6969 0.8050 -0.0144 0.069 Uiso 1 1 calc R . .
H54B H 0.7628 0.8507 -0.0559 0.069 Uiso 1 1 calc R . .
H54C H 0.6223 0.8500 -0.0535 0.069 Uiso 1 1 calc R . .
C55 C 0.7305(9) 0.9736(8) -0.0049(4) 0.031(3) Uani 1 1 d . . .
C56 C 0.7731(10) 1.0088(9) -0.0497(4) 0.036(4) Uani 1 1 d . . .
H56 H 0.7841 0.9856 -0.0812 0.043 Uiso 1 1 calc R . .
C57 C 0.7975(10) 1.0763(9) -0.0466(5) 0.041(4) Uani 1 1 d . . .
H57 H 0.8265 1.0988 -0.0762 0.049 Uiso 1 1 calc R . .
C58 C 0.7808(11) 1.1124(9) -0.0010(5) 0.042(4) Uani 1 1 d . . .
H58 H 0.7969 1.1589 -0.0006 0.050 Uiso 1 1 calc R . .
C59 C 0.7405(9) 1.0811(8) 0.0440(4) 0.035(4) Uani 1 1 d . . .
H59 H 0.7293 1.1055 0.0749 0.042 Uiso 1 1 calc R . .
C60 C 0.7175(10) 1.0123(7) 0.0416(4) 0.022(2) Uani 1 1 d U . .
C61 C 0.2243(13) 0.0605(12) 0.7214(6) 0.074(6) Uani 1 1 d . . .
H61A H 0.2289 0.0122 0.7135 0.088 Uiso 1 1 calc R . .
H61B H 0.2942 0.0825 0.7063 0.088 Uiso 1 1 calc R . .
C62 C -0.007(2) 0.7238(14) 0.2072(10) 0.116(9) Uani 1 1 d . . .
H62A H -0.0790 0.7072 0.2247 0.139 Uiso 1 1 calc R . .
H62B H -0.0268 0.7664 0.1898 0.139 Uiso 1 1 calc R . .
N1 N 0.3777(8) 0.7449(6) 0.8873(3) 0.029(3) Uani 1 1 d . . .
N2 N 0.0573(7) 0.8508(5) 0.9261(3) 0.021(2) Uani 1 1 d . . .
N3 N 0.6787(9) 0.9678(6) 0.0791(3) 0.028(3) Uani 1 1 d . . .
N4 N 0.3482(7) 1.0666(6) 0.1107(3) 0.026(2) Uani 1 1 d . . .
O1 O -0.0754(8) 0.9713(6) 0.8294(3) 0.044(3) Uani 1 1 d . . .
O2 O 0.0450(7) 0.9224(5) 0.7695(3) 0.032(2) Uani 1 1 d U . .
O3 O 0.6961(8) 0.9025(5) 0.2341(3) 0.039(2) Uani 1 1 d . . .
O4 O 0.8082(7) 0.8429(6) 0.1759(3) 0.044(3) Uani 1 1 d . . .
Cl1 Cl 0.2260(4) 0.0719(3) 0.79018(15) 0.0704(12) Uani 1 1 d . . .
Cl2 Cl 0.0928(4) 0.0951(3) 0.69246(18) 0.0783(15) Uani 1 1 d . . .
Cl3 Cl 0.1109(5) 0.7374(3) 0.2549(2) 0.0930(17) Uani 1 1 d . . .
Cl4 Cl 0.0414(4) 0.6649(4) 0.16207(17) 0.094(2) Uani 1 1 d . . .
Br1 Br 0.28691(10) 0.78055(8) 0.65662(4) 0.0361(4) Uani 1 1 d . . .
Br2 Br 0.44450(9) 1.06713(8) 0.34283(4) 0.0346(4) 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 0.028(6) 0.064(12) 0.016(5) -0.003(6) -0.002(5) -0.020(7)
C2 0.025(6) 0.058(10) 0.016(5) -0.006(6) 0.004(5) -0.013(6)
C3 0.019(6) 0.046(10) 0.033(7) -0.012(6) 0.007(5) -0.003(6)
C4 0.019(5) 0.049(9) 0.008(5) -0.010(5) 0.005(4) -0.006(6)
C5 0.017(5) 0.047(8) 0.011(4) 0.003(6) 0.002(4) -0.011(6)
C6 0.022(6) 0.055(10) 0.009(4) -0.001(6) 0.004(4) -0.014(6)
C7 0.028(6) 0.059(11) 0.021(6) 0.000(6) -0.003(5) 0.008(6)
C8 0.022(5) 0.034(8) 0.030(5) 0.004(7) 0.009(5) 0.002(6)
C9 0.031(6) 0.049(10) 0.012(5) 0.005(5) -0.003(5) 0.001(6)
C10 0.023(5) 0.058(10) 0.006(5) 0.002(5) -0.001(4) -0.009(6)
C11 0.019(6) 0.060(11) 0.017(5) 0.000(6) -0.003(4) 0.006(6)
C12 0.011(5) 0.046(10) 0.030(6) 0.007(6) -0.006(5) 0.003(6)
C13 0.021(6) 0.081(13) 0.021(6) 0.017(7) -0.004(5) -0.006(7)
C14 0.060(9) 0.074(13) 0.030(7) -0.006(8) -0.013(7) -0.026(9)
C15 0.014(5) 0.051(10) 0.022(6) -0.001(6) 0.002(4) -0.001(6)
C16 0.024(6) 0.049(10) 0.007(5) -0.001(5) -0.003(4) -0.005(6)
C17 0.033(6) 0.042(10) 0.025(6) -0.004(7) -0.006(5) 0.000(7)
C18 0.055(9) 0.054(11) 0.030(7) 0.003(7) 0.015(6) -0.004(8)
C19 0.033(6) 0.041(10) 0.026(6) -0.010(7) 0.005(5) -0.008(7)
C20 0.023(6) 0.072(13) 0.017(6) -0.007(7) -0.002(5) 0.006(7)
C21 0.029(6) 0.052(10) 0.014(5) -0.005(6) 0.005(5) 0.003(6)
C22 0.008(5) 0.034(9) 0.027(6) -0.004(6) 0.004(4) 0.007(5)
C23 0.014(5) 0.041(9) 0.018(5) -0.004(6) 0.002(4) 0.004(6)
C24 0.034(7) 0.054(11) 0.028(6) -0.012(7) 0.002(5) 0.008(7)
C25 0.011(5) 0.049(10) 0.016(5) -0.002(5) 0.002(4) 0.002(6)
C26 0.009(5) 0.041(9) 0.021(5) 0.003(5) -0.003(4) -0.006(5)
C27 0.022(6) 0.054(11) 0.013(5) 0.007(6) -0.004(4) 0.004(6)
C28 0.023(6) 0.044(9) 0.036(7) 0.007(6) -0.003(5) 0.005(6)
C29 0.024(6) 0.069(12) 0.009(5) 0.007(6) -0.002(4) -0.007(6)
C30 0.026(3) 0.026(3) 0.025(3) -0.0003(10) 0.0006(10) -0.0002(10)
C31 0.019(5) 0.050(9) 0.017(5) 0.003(7) 0.005(4) 0.000(7)
C32 0.018(5) 0.049(9) 0.019(6) -0.001(6) 0.003(4) -0.006(6)
C33 0.024(6) 0.043(9) 0.019(6) -0.013(6) 0.003(5) 0.009(6)
C34 0.022(5) 0.042(8) 0.008(4) -0.004(6) -0.005(4) -0.001(6)
C35 0.018(2) 0.019(3) 0.017(2) -0.0005(10) 0.0002(10) -0.0003(10)
C36 0.009(5) 0.046(9) 0.020(5) 0.000(6) -0.006(4) 0.001(5)
C37 0.017(5) 0.055(10) 0.018(5) 0.010(6) -0.004(4) 0.001(6)
C38 0.021(6) 0.050(9) 0.015(5) -0.003(6) 0.003(4) 0.001(6)
C39 0.013(5) 0.049(9) 0.013(5) -0.005(6) 0.003(4) 0.003(5)
C40 0.016(5) 0.040(9) 0.021(5) -0.009(6) 0.002(4) 0.000(5)
C41 0.014(5) 0.057(10) 0.008(5) -0.003(5) -0.001(4) -0.002(6)
C42 0.046(8) 0.046(10) 0.015(6) 0.002(6) -0.013(5) -0.005(7)
C43 0.051(9) 0.088(14) 0.017(6) 0.009(7) -0.021(6) -0.003(9)
C44 0.057(9) 0.057(11) 0.017(6) 0.011(7) -0.007(6) -0.009(8)
C45 0.013(5) 0.059(10) 0.023(6) 0.006(6) -0.001(4) 0.005(6)
C46 0.026(3) 0.026(3) 0.025(3) -0.0004(10) 0.0000(10) 0.0001(10)
C47 0.030(6) 0.057(11) 0.041(7) -0.007(7) -0.017(5) -0.003(7)
C48 0.034(7) 0.063(12) 0.054(9) -0.001(8) -0.008(7) -0.013(7)
C49 0.030(6) 0.049(11) 0.034(6) -0.005(8) -0.007(5) -0.004(7)
C50 0.022(6) 0.058(11) 0.026(6) -0.019(7) -0.004(5) -0.006(6)
C51 0.018(6) 0.049(10) 0.038(7) -0.012(7) -0.001(5) 0.004(6)
C52 0.022(6) 0.047(9) 0.018(5) -0.010(6) 0.002(5) 0.009(6)
C53 0.012(5) 0.045(10) 0.028(6) -0.001(6) -0.005(5) 0.009(6)
C54 0.025(6) 0.087(13) 0.027(6) -0.029(8) -0.011(5) 0.003(7)
C55 0.014(5) 0.066(11) 0.011(5) -0.002(6) 0.000(4) 0.001(6)
C56 0.019(6) 0.069(12) 0.020(6) 0.008(7) -0.003(5) 0.002(7)
C57 0.030(6) 0.065(13) 0.027(6) 0.019(8) -0.006(5) 0.004(8)
C58 0.036(7) 0.069(12) 0.020(6) 0.005(7) -0.007(5) -0.010(7)
C59 0.019(5) 0.072(13) 0.014(5) 0.003(6) -0.003(4) 0.009(7)
C60 0.021(3) 0.022(3) 0.022(3) 0.0005(10) -0.0004(10) 0.0000(10)
C61 0.050(9) 0.103(18) 0.068(11) -0.008(12) 0.014(8) 0.005(11)
C62 0.115(19) 0.086(19) 0.15(2) 0.012(18) -0.023(17) 0.036(16)
N1 0.019(4) 0.053(8) 0.017(5) 0.001(5) 0.007(4) 0.007(5)
N2 0.015(4) 0.035(7) 0.012(4) 0.000(4) 0.000(3) -0.006(4)
N3 0.029(5) 0.040(8) 0.014(4) -0.006(5) 0.006(4) 0.002(5)
N4 0.020(4) 0.044(7) 0.014(4) 0.004(5) 0.001(3) 0.001(5)
O1 0.034(5) 0.077(9) 0.021(4) 0.011(5) 0.003(4) 0.018(5)
O2 0.033(2) 0.033(2) 0.031(2) -0.0001(10) -0.0011(10) 0.0001(10)
O3 0.042(5) 0.058(7) 0.015(4) -0.006(4) -0.008(3) 0.008(5)
O4 0.024(5) 0.079(8) 0.028(4) 0.003(5) 0.002(4) 0.024(5)
Cl1 0.086(3) 0.078(3) 0.047(2) 0.001(3) 0.0118(19) 0.001(3)
Cl2 0.076(3) 0.083(4) 0.075(3) 0.023(3) -0.006(2) 0.004(3)
Cl3 0.099(4) 0.099(5) 0.081(3) -0.020(3) 0.018(3) -0.029(3)
Cl4 0.060(3) 0.175(7) 0.047(2) -0.007(3) -0.0009(19) 0.011(3)
Br1 0.0287(6) 0.0682(10) 0.0115(5) -0.0020(7) 0.0028(4) -0.0104(7)
Br2 0.0220(5) 0.0714(10) 0.0105(5) -0.0001(7) 0.0007(4) -0.0021(7)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.366(18) . ?
C1 C6 1.383(17) . ?
C1 Br1 1.929(11) . ?
C2 C3 1.378(17) . ?
C3 C4 1.427(16) . ?
C4 C5 1.357(17) . ?
C4 N1 1.398(12) . ?
C5 C6 1.441(13) . ?
C5 C9 1.447(15) . ?
C7 N1 1.463(15) . ?
C8 C9 1.357(16) . ?
C8 N1 1.355(15) . ?
C9 C10 1.503(17) . ?
C10 N2 1.482(12) . ?
C10 C11 1.55(2) . ?
C11 C12 1.503(15) . ?
C11 C15 1.559(16) . ?
C12 O1 1.229(14) . ?
C12 O2 1.364(15) . ?
C13 O2 1.441(14) . ?
C13 C14 1.466(19) . ?
C15 C22 1.452(18) . ?
C15 C16 1.539(16) . ?
C16 C21 1.371(17) . ?
C16 C17 1.38(2) . ?
C17 C18 1.384(19) . ?
C18 C19 1.38(2) . ?
C19 C20 1.38(2) . ?
C20 C21 1.435(18) . ?
C22 N2 1.365(16) . ?
C22 C23 1.396(15) . ?
C23 C25 1.409(18) . ?
C23 C24 1.509(18) . ?
C25 C30 1.427(17) . ?
C25 C26 1.432(16) . ?
C26 C27 1.348(18) . ?
C26 N2 1.381(15) . ?
C27 C28 1.421(17) . ?
C28 C29 1.445(18) . ?
C29 C30 1.291(19) . ?
C31 C32 1.375(16) . ?
C31 C36 1.386(16) . ?
C31 Br2 1.909(10) . ?
C32 C33 1.395(15) . ?
C33 C34 1.391(15) . ?
C34 N4 1.390(11) . ?
C34 C35 1.400(15) . ?
C35 C36 1.415(14) . ?
C35 C39 1.448(14) . ?
C37 N4 1.440(14) . ?
C38 C39 1.362(15) . ?
C38 N4 1.367(14) . ?
C39 C40 1.505(15) . ?
C40 N3 1.467(13) . ?
C40 C41 1.538(19) . ?
C41 C42 1.527(16) . ?
C41 C45 1.569(17) . ?
C42 O4 1.206(16) . ?
C42 O3 1.347(15) . ?
C43 O3 1.478(14) . ?
C43 C44 1.504(19) . ?
C45 C46 1.492(16) . ?
C45 C52 1.504(18) . ?
C46 C47 1.346(19) . ?
C46 C51 1.383(17) . ?
C47 C48 1.431(18) . ?
C48 C49 1.37(2) . ?
C49 C50 1.33(2) . ?
C50 C51 1.370(17) . ?
C52 C53 1.364(15) . ?
C52 N3 1.390(17) . ?
C53 C55 1.41(2) . ?
C53 C54 1.497(18) . ?
C55 C60 1.414(16) . ?
C55 C56 1.416(17) . ?
C56 C57 1.35(2) . ?
C57 C58 1.373(19) . ?
C58 C59 1.377(17) . ?
C59 C60 1.37(2) . ?
C60 N3 1.365(15) . ?
C61 Cl1 1.766(16) . ?
C61 Cl2 1.775(17) . ?
C62 Cl4 1.72(3) . ?
C62 Cl3 1.81(2) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 125.4(10) . . ?
C2 C1 Br1 118.6(9) . . ?
C6 C1 Br1 116.0(9) . . ?
C1 C2 C3 121.0(11) . . ?
C2 C3 C4 115.2(12) . . ?
C5 C4 N1 107.5(9) . . ?
C5 C4 C3 123.8(10) . . ?
N1 C4 C3 128.7(11) . . ?
C4 C5 C6 120.3(10) . . ?
C4 C5 C9 108.3(9) . . ?
C6 C5 C9 131.3(11) . . ?
C1 C6 C5 114.2(11) . . ?
C9 C8 N1 111.0(10) . . ?
C8 C9 C5 105.1(10) . . ?
C8 C9 C10 128.7(10) . . ?
C5 C9 C10 126.1(10) . . ?
N2 C10 C9 111.2(9) . . ?
N2 C10 C11 99.9(10) . . ?
C9 C10 C11 116.1(10) . . ?
C12 C11 C10 108.2(10) . . ?
C12 C11 C15 111.8(11) . . ?
C10 C11 C15 109.5(9) . . ?
O1 C12 O2 120.0(10) . . ?
O1 C12 C11 126.5(11) . . ?
O2 C12 C11 113.4(10) . . ?
O2 C13 C14 109.9(11) . . ?
C22 C15 C16 116.8(10) . . ?
C22 C15 C11 102.2(11) . . ?
C16 C15 C11 111.6(9) . . ?
C21 C16 C17 120.3(12) . . ?
C21 C16 C15 120.8(13) . . ?
C17 C16 C15 118.9(11) . . ?
C18 C17 C16 120.3(12) . . ?
C17 C18 C19 121.0(16) . . ?
C18 C19 C20 119.1(13) . . ?
C19 C20 C21 120.3(12) . . ?
C16 C21 C20 118.8(14) . . ?
N2 C22 C23 109.1(11) . . ?
N2 C22 C15 112.4(10) . . ?
C23 C22 C15 138.4(12) . . ?
C22 C23 C25 105.7(11) . . ?
C22 C23 C24 127.3(13) . . ?
C25 C23 C24 127.0(10) . . ?
C23 C25 C30 134.3(11) . . ?
C23 C25 C26 109.5(10) . . ?
C30 C25 C26 116.2(12) . . ?
C27 C26 N2 131.7(11) . . ?
C27 C26 C25 123.7(12) . . ?
N2 C26 C25 104.6(11) . . ?
C26 C27 C28 118.0(12) . . ?
C27 C28 C29 118.1(14) . . ?
C30 C29 C28 122.7(13) . . ?
C29 C30 C25 121.2(13) . . ?
C32 C31 C36 124.1(10) . . ?
C32 C31 Br2 117.8(8) . . ?
C36 C31 Br2 118.1(8) . . ?
C31 C32 C33 120.7(11) . . ?
C34 C33 C32 116.7(10) . . ?
C33 C34 N4 127.9(10) . . ?
C33 C34 C35 122.4(9) . . ?
N4 C34 C35 109.7(9) . . ?
C34 C35 C36 120.6(9) . . ?
C34 C35 C39 106.5(9) . . ?
C36 C35 C39 132.8(10) . . ?
C31 C36 C35 115.4(10) . . ?
C39 C38 N4 113.4(9) . . ?
C38 C39 C35 104.8(9) . . ?
C38 C39 C40 128.9(10) . . ?
C35 C39 C40 126.3(9) . . ?
N3 C40 C39 109.8(9) . . ?
N3 C40 C41 101.7(9) . . ?
C39 C40 C41 114.2(9) . . ?
C42 C41 C40 108.8(10) . . ?
C42 C41 C45 113.2(11) . . ?
C40 C41 C45 108.8(9) . . ?
O4 C42 O3 124.9(11) . . ?
O4 C42 C41 126.6(11) . . ?
O3 C42 C41 108.4(11) . . ?
O3 C43 C44 104.3(11) . . ?
C46 C45 C52 115.1(9) . . ?
C46 C45 C41 112.5(9) . . ?
C52 C45 C41 101.8(11) . . ?
C47 C46 C51 116.3(11) . . ?
C47 C46 C45 119.5(11) . . ?
C51 C46 C45 124.2(12) . . ?
C46 C47 C48 122.0(13) . . ?
C49 C48 C47 118.2(15) . . ?
C50 C49 C48 120.1(13) . . ?
C49 C50 C51 120.9(13) . . ?
C50 C51 C46 122.4(14) . . ?
C53 C52 N3 109.6(12) . . ?
C53 C52 C45 139.8(13) . . ?
N3 C52 C45 110.6(9) . . ?
C52 C53 C55 106.0(11) . . ?
C52 C53 C54 127.2(13) . . ?
C55 C53 C54 126.8(11) . . ?
C60 C55 C53 109.0(10) . . ?
C60 C55 C56 116.6(14) . . ?
C53 C55 C56 134.3(12) . . ?
C57 C56 C55 119.8(13) . . ?
C56 C57 C58 121.8(13) . . ?
C57 C58 C59 121.3(16) . . ?
C60 C59 C58 117.4(12) . . ?
N3 C60 C59 131.0(10) . . ?
N3 C60 C55 106.0(11) . . ?
C59 C60 C55 123.1(11) . . ?
Cl1 C61 Cl2 111.9(9) . . ?
Cl4 C62 Cl3 108.4(13) . . ?
C8 N1 C4 108.0(9) . . ?
C8 N1 C7 127.0(9) . . ?
C4 N1 C7 125.0(9) . . ?
C22 N2 C26 111.1(9) . . ?
C22 N2 C10 114.6(10) . . ?
C26 N2 C10 134.3(11) . . ?
C60 N3 C52 109.5(9) . . ?
C60 N3 C40 135.8(11) . . ?
C52 N3 C40 114.3(10) . . ?
C38 N4 C34 105.5(9) . . ?
C38 N4 C37 127.7(9) . . ?
C34 N4 C37 126.3(10) . . ?
C12 O2 C13 120.0(9) . . ?
C42 O3 C43 114.8(11) . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.898
_refine_diff_density_min         -1.417
_refine_diff_density_rms         0.159


data_compound3
_database_code_depnum_ccdc_archive 'CCDC 917194'
#TrackingRef '16371_web_deposit_cif_file_0_DattatrayaH.Dethe_1356085110.dethe.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H28 N2 O2'
_chemical_formula_sum            'C30 H28 N2 O2'
_chemical_formula_weight         448.54
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'
O O 0.0106 0.0060 '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'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   11.4304(7)
_cell_length_b                   12.7197(7)
_cell_length_c                   16.8479(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.853(5)
_cell_angle_gamma                90.00
_cell_volume                     2432.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2304
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.12
_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_process_details   SADABS
_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 SMART APEX'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12200
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.62
_reflns_number_total             5599
_reflns_number_gt                3360
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ciftab
_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^ > 2\s(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^)+(0.0602P)^2^+0.4556P] 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     SHELXL
_refine_ls_extinction_coef       0.0062(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5599
_refine_ls_number_parameters     311
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1745
_refine_ls_wR_factor_gt          0.1429
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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 0.04573(14) 0.17032(13) 0.06594(9) 0.0497(4) Uani 1 1 d . . .
C11 C -0.07946(16) 0.27183(16) 0.13636(11) 0.0483(5) Uani 1 1 d . . .
H2 H -0.1431 0.2292 0.1539 0.058 Uiso 1 1 calc R . .
C12 C -0.11266(16) 0.38627(16) 0.13992(11) 0.0482(5) Uani 1 1 d . . .
C10 C 0.03807(16) 0.24498(15) 0.18998(11) 0.0460(5) Uani 1 1 d . . .
H4 H 0.0903 0.3062 0.1914 0.055 Uiso 1 1 calc R . .
C1 C -0.05302(17) 0.23259(16) 0.05656(12) 0.0489(5) Uani 1 1 d . . .
C26 C 0.01487(19) 0.22032(18) 0.27357(12) 0.0561(5) Uani 1 1 d . . .
C7 C 0.06667(18) 0.13170(16) -0.00706(12) 0.0514(5) Uani 1 1 d . . .
C8 C -0.02068(19) 0.17522(16) -0.06368(12) 0.0539(5) Uani 1 1 d . . .
O2 O 0.01561(16) 0.30554(13) 0.31758(9) 0.0771(5) Uani 1 1 d . . .
C9 C 0.09564(17) 0.15351(16) 0.14869(11) 0.0477(5) Uani 1 1 d . . .
H10 H 0.0671 0.0865 0.1677 0.057 Uiso 1 1 calc R . .
C2 C -0.09713(18) 0.23861(17) -0.02192(12) 0.0555(5) Uani 1 1 d . . .
C19 C 0.22643(18) 0.15477(17) 0.16124(12) 0.0523(5) Uani 1 1 d . . .
C25 C 0.30295(19) 0.22904(19) 0.12937(12) 0.0570(6) Uani 1 1 d . . .
C13 C -0.05648(19) 0.46172(18) 0.09925(13) 0.0585(6) Uani 1 1 d . . .
H14 H 0.0022 0.4412 0.0687 0.070 Uiso 1 1 calc R . .
C18 C 0.2952(2) 0.08637(19) 0.20837(14) 0.0640(6) Uani 1 1 d . . .
N2 N 0.41132(18) 0.11431(19) 0.20755(13) 0.0802(7) Uani 1 1 d . . .
H16 H 0.4705 0.0820 0.2329 0.096 Uiso 1 1 calc R . .
C3 C -0.0164(2) 0.1524(2) -0.14437(13) 0.0686(7) Uani 1 1 d . . .
H17 H -0.0720 0.1808 -0.1833 0.082 Uiso 1 1 calc R . .
O1 O -0.0054(2) 0.13521(15) 0.29767(11) 0.1034(7) Uani 1 1 d . . .
C24 C 0.4187(2) 0.2012(2) 0.16036(15) 0.0710(7) Uani 1 1 d . . .
C17 C -0.19831(19) 0.4200(2) 0.18535(14) 0.0655(6) Uani 1 1 d . . .
H20 H -0.2370 0.3712 0.2140 0.079 Uiso 1 1 calc R . .
C14 C -0.0853(2) 0.56636(18) 0.10290(14) 0.0652(6) Uani 1 1 d . . .
H21 H -0.0463 0.6157 0.0749 0.078 Uiso 1 1 calc R . .
C15 C -0.1712(2) 0.5981(2) 0.14772(15) 0.0716(7) Uani 1 1 d . . .
H22 H -0.1911 0.6688 0.1502 0.086 Uiso 1 1 calc R . .
C6 C 0.1535(2) 0.06534(19) -0.02842(14) 0.0658(6) Uani 1 1 d . . .
H23 H 0.2095 0.0361 0.0098 0.079 Uiso 1 1 calc R . .
C5 C 0.1534(3) 0.0444(2) -0.10849(16) 0.0778(7) Uani 1 1 d . . .
H24 H 0.2106 -0.0002 -0.1246 0.093 Uiso 1 1 calc R . .
C4 C 0.0705(3) 0.0880(2) -0.16566(15) 0.0764(7) Uani 1 1 d . . .
H25 H 0.0739 0.0732 -0.2194 0.092 Uiso 1 1 calc R . .
C20 C 0.2872(2) 0.3150(2) 0.07832(14) 0.0718(7) Uani 1 1 d . . .
H26 H 0.2118 0.3344 0.0563 0.086 Uiso 1 1 calc R . .
C23 C 0.5158(2) 0.2569(3) 0.14238(19) 0.0976(11) Uani 1 1 d . . .
H27 H 0.5916 0.2372 0.1633 0.117 Uiso 1 1 calc R . .
C29 C -0.2020(2) 0.2994(2) -0.05827(16) 0.0865(8) Uani 1 1 d . . .
H28A H -0.2549 0.3106 -0.0189 0.130 Uiso 1 1 calc R . .
H28B H -0.2417 0.2607 -0.1024 0.130 Uiso 1 1 calc R . .
H28C H -0.1767 0.3661 -0.0768 0.130 Uiso 1 1 calc R . .
C16 C -0.2273(2) 0.5248(2) 0.18877(17) 0.0803(8) Uani 1 1 d . . .
H29 H -0.2856 0.5459 0.2194 0.096 Uiso 1 1 calc R . .
C21 C 0.3832(3) 0.3711(3) 0.06058(17) 0.0939(9) Uani 1 1 d . . .
H30 H 0.3725 0.4290 0.0268 0.113 Uiso 1 1 calc R . .
C30 C 0.2635(3) -0.0053(2) 0.25635(18) 0.0900(9) Uani 1 1 d . . .
H31A H 0.2735 -0.0690 0.2274 0.135 Uiso 1 1 calc R . .
H31B H 0.1828 0.0008 0.2663 0.135 Uiso 1 1 calc R . .
H31C H 0.3136 -0.0068 0.3063 0.135 Uiso 1 1 calc R . .
C27 C -0.0228(3) 0.2936(3) 0.39689(15) 0.0972(10) Uani 1 1 d . . .
H32A H -0.1064 0.2780 0.3921 0.117 Uiso 1 1 calc R . .
H32B H 0.0196 0.2363 0.4254 0.117 Uiso 1 1 calc R . .
C22 C 0.4969(3) 0.3420(4) 0.0928(2) 0.1099(12) Uani 1 1 d . . .
H33 H 0.5609 0.3811 0.0803 0.132 Uiso 1 1 calc R . .
C28 C 0.0011(5) 0.3905(3) 0.4393(2) 0.1574(19) Uani 1 1 d . . .
H1A1 H 0.0842 0.4046 0.4444 0.236 Uiso 1 1 calc R . .
H1A2 H -0.0242 0.3850 0.4914 0.236 Uiso 1 1 calc R . .
H1A3 H -0.0407 0.4467 0.4103 0.236 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 0.0523(9) 0.0515(10) 0.0441(9) -0.0046(8) 0.0008(7) 0.0009(8)
C11 0.0411(9) 0.0505(11) 0.0537(11) 0.0023(9) 0.0081(8) -0.0064(9)
C12 0.0398(9) 0.0532(12) 0.0515(11) 0.0015(9) 0.0053(8) -0.0022(9)
C10 0.0473(10) 0.0450(11) 0.0456(11) 0.0001(9) 0.0054(8) -0.0069(9)
C1 0.0444(10) 0.0475(11) 0.0542(12) -0.0017(10) 0.0025(8) -0.0059(9)
C26 0.0592(12) 0.0582(13) 0.0515(12) 0.0012(11) 0.0099(10) -0.0044(11)
C7 0.0578(12) 0.0453(11) 0.0508(11) -0.0062(9) 0.0058(9) -0.0107(10)
C8 0.0612(12) 0.0502(12) 0.0490(12) -0.0018(10) 0.0018(9) -0.0142(10)
O2 0.1118(14) 0.0734(11) 0.0488(9) -0.0046(8) 0.0198(9) 0.0060(10)
C9 0.0513(10) 0.0439(10) 0.0469(11) 0.0011(9) 0.0016(8) -0.0035(9)
C2 0.0532(11) 0.0580(13) 0.0523(12) 0.0011(10) -0.0064(9) -0.0086(10)
C19 0.0506(11) 0.0566(12) 0.0487(11) -0.0060(10) 0.0015(9) 0.0016(10)
C25 0.0549(12) 0.0693(14) 0.0474(11) -0.0116(11) 0.0085(9) -0.0048(11)
C13 0.0590(12) 0.0574(13) 0.0616(13) 0.0009(11) 0.0175(10) -0.0010(11)
C18 0.0622(13) 0.0672(15) 0.0597(13) -0.0074(12) -0.0045(11) 0.0097(12)
N2 0.0565(11) 0.1022(18) 0.0770(14) -0.0093(13) -0.0120(10) 0.0163(12)
C3 0.0881(17) 0.0662(15) 0.0500(13) -0.0010(11) 0.0016(12) -0.0210(14)
O1 0.169(2) 0.0757(13) 0.0737(12) 0.0047(10) 0.0465(12) -0.0307(13)
C24 0.0509(12) 0.104(2) 0.0569(14) -0.0205(14) 0.0032(10) -0.0045(14)
C17 0.0529(12) 0.0686(15) 0.0787(15) 0.0043(12) 0.0229(11) 0.0021(12)
C14 0.0729(15) 0.0539(13) 0.0693(14) 0.0089(12) 0.0114(12) -0.0008(12)
C15 0.0734(16) 0.0571(14) 0.0827(17) 0.0014(13) 0.0023(13) 0.0148(13)
C6 0.0726(15) 0.0615(14) 0.0638(14) -0.0110(12) 0.0105(11) -0.0010(12)
C5 0.0898(18) 0.0707(16) 0.0767(17) -0.0237(14) 0.0255(14) -0.0083(15)
C4 0.101(2) 0.0717(17) 0.0588(15) -0.0141(13) 0.0187(14) -0.0198(16)
C20 0.0698(15) 0.0818(17) 0.0655(15) -0.0009(13) 0.0151(12) -0.0163(14)
C23 0.0582(15) 0.154(3) 0.081(2) -0.026(2) 0.0084(14) -0.0203(18)
C29 0.0712(16) 0.109(2) 0.0741(17) 0.0075(16) -0.0143(13) 0.0125(16)
C16 0.0664(15) 0.0787(18) 0.101(2) -0.0006(16) 0.0315(14) 0.0150(14)
C21 0.100(2) 0.107(2) 0.0779(18) 0.0010(17) 0.0234(16) -0.0368(19)
C30 0.104(2) 0.0702(18) 0.0890(19) 0.0148(15) -0.0187(16) 0.0155(16)
C27 0.123(2) 0.120(3) 0.0522(15) -0.0039(16) 0.0265(15) 0.008(2)
C22 0.083(2) 0.167(4) 0.084(2) -0.025(2) 0.0279(17) -0.053(2)
C28 0.287(6) 0.119(3) 0.072(2) -0.025(2) 0.047(3) 0.015(3)
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 C7 1.372(2) . ?
N1 C1 1.373(2) . ?
N1 C9 1.458(2) . ?
C11 C1 1.498(3) . ?
C11 C12 1.507(3) . ?
C11 C10 1.564(3) . ?
C12 C17 1.381(3) . ?
C12 C13 1.381(3) . ?
C10 C26 1.497(3) . ?
C10 C9 1.543(3) . ?
C1 C2 1.360(3) . ?
C26 O1 1.189(3) . ?
C26 O2 1.313(3) . ?
C7 C6 1.383(3) . ?
C7 C8 1.409(3) . ?
C8 C3 1.397(3) . ?
C8 C2 1.434(3) . ?
O2 C27 1.463(3) . ?
C9 C19 1.485(3) . ?
C2 C29 1.495(3) . ?
C19 C18 1.363(3) . ?
C19 C25 1.435(3) . ?
C25 C20 1.390(3) . ?
C25 C24 1.408(3) . ?
C13 C14 1.374(3) . ?
C18 N2 1.375(3) . ?
C18 C30 1.488(4) . ?
N2 C24 1.370(3) . ?
C3 C4 1.368(4) . ?
C24 C23 1.380(4) . ?
C17 C16 1.377(3) . ?
C14 C15 1.369(3) . ?
C15 C16 1.365(3) . ?
C6 C5 1.375(3) . ?
C5 C4 1.384(4) . ?
C20 C21 1.371(3) . ?
C23 C22 1.369(5) . ?
C21 C22 1.397(5) . ?
C27 C28 1.434(5) . ?
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
C7 N1 C1 109.42(16) . . ?
C7 N1 C9 135.62(17) . . ?
C1 N1 C9 114.67(16) . . ?
C1 C11 C12 115.85(16) . . ?
C1 C11 C10 101.20(15) . . ?
C12 C11 C10 113.00(16) . . ?
C17 C12 C13 117.5(2) . . ?
C17 C12 C11 121.36(19) . . ?
C13 C12 C11 121.14(17) . . ?
C26 C10 C9 113.53(16) . . ?
C26 C10 C11 110.65(16) . . ?
C9 C10 C11 106.70(15) . . ?
C2 C1 N1 110.41(18) . . ?
C2 C1 C11 139.70(19) . . ?
N1 C1 C11 109.88(16) . . ?
O1 C26 O2 123.2(2) . . ?
O1 C26 C10 125.1(2) . . ?
O2 C26 C10 111.62(19) . . ?
N1 C7 C6 131.3(2) . . ?
N1 C7 C8 106.32(18) . . ?
C6 C7 C8 122.41(19) . . ?
C3 C8 C7 118.2(2) . . ?
C3 C8 C2 133.5(2) . . ?
C7 C8 C2 108.22(17) . . ?
C26 O2 C27 116.6(2) . . ?
N1 C9 C19 114.03(16) . . ?
N1 C9 C10 100.45(15) . . ?
C19 C9 C10 113.83(16) . . ?
C1 C2 C8 105.58(18) . . ?
C1 C2 C29 127.8(2) . . ?
C8 C2 C29 126.6(2) . . ?
C18 C19 C25 107.65(19) . . ?
C18 C19 C9 125.3(2) . . ?
C25 C19 C9 127.03(19) . . ?
C20 C25 C24 118.3(2) . . ?
C20 C25 C19 135.2(2) . . ?
C24 C25 C19 106.5(2) . . ?
C14 C13 C12 121.5(2) . . ?
C19 C18 N2 108.6(2) . . ?
C19 C18 C30 131.0(2) . . ?
N2 C18 C30 120.4(2) . . ?
C24 N2 C18 109.9(2) . . ?
C4 C3 C8 119.4(2) . . ?
N2 C24 C23 130.4(3) . . ?
N2 C24 C25 107.3(2) . . ?
C23 C24 C25 122.3(3) . . ?
C16 C17 C12 120.9(2) . . ?
C15 C14 C13 120.1(2) . . ?
C16 C15 C14 119.3(2) . . ?
C5 C6 C7 117.2(2) . . ?
C6 C5 C4 121.7(3) . . ?
C3 C4 C5 121.1(2) . . ?
C21 C20 C25 119.7(3) . . ?
C22 C23 C24 117.9(3) . . ?
C15 C16 C17 120.7(2) . . ?
C20 C21 C22 120.6(3) . . ?
C28 C27 O2 107.8(3) . . ?
C23 C22 C21 121.2(3) . . ?
_diffrn_measured_fraction_theta_max 0.99
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.99
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.037
#===END