# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics
# This journal is © The Owner Societies 2012


data_global
_journal_name_full               Phys.Chem.Chem.Phys.(PCCP)
_journal_coden_cambridge         1326
#TrackingRef '- product1.cif'

#===================================================================
_audit_creation_date             2011/12/23
_audit_creation_method           'from SHELXL97'

#===================================================================
# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Dr. Jiro Abe'
_publ_contact_author_address     
;
Department of Chemistry
School of Science and Engineering
Aoyama Gakuin University
5-10-1 Fuchinobe, Chuo-ku, Sagamihara
Kanagawa 252-5258, Japan
;
_publ_contact_author_phone       '81 42 759 6225'
_publ_contact_author_fax         '81 42 759 6225'
_publ_contact_author_email       'jiro abe@chem.aoyama.ac.jp'
_publ_requested_category         EM
_publ_requested_coeditor_name    ?

_publ_contact_letter             
;
Please consider this as part of our Electronic Supporting Information
;

#=====================================================================
# 2. TITLE AND AUTHOR LIST

_publ_section_title              
;
Peroxide-Bridged Imidazole Dimer Formed from a Photochromic
Naphthalene-Bridged Imidazole Dimer
;

# _publ_section_title_footnote
# ;
# ;

loop_
_publ_author_name
_publ_author_address
# ''
S.Hatano
;
Department of Chemistry
School of Science and Engineering
Aoyama Gakuin University
5-10-1 Fuchinobe, Chuo-ku, Sagamihara
Kanagawa 252-5258, Japan
;
j.Abe
;
Department of Chemistry
School of Science and Engineering
Aoyama Gakuin University
5-10-1 Fuchinobe, Chuo-ku, Sagamihara
Kanagawa 252-5258, Japan
;
#======================================================================
# 3. TEXT

_publ_section_abstract           
;
2,4,5-Triphenylimidazole (lophine) is well known
as the first chemiluminescence
substrate discovered in 1877, and its oxidized derivative,
2,4,5-triphenylimidazolyl
radical, corresponds to the colored species in the photochromic reaction of
hexaarylbiimidazole (HABI). We report the first direct
observation of the O2 adduct
of the imidazolyl radical that forms the end-on peroxide-bridged
imidazole dimer.
The ring-opening reaction of the peroxide-bridged
imidazole dimer leading to the
formation of an N-benzoylbenzamidine
derivative supports the presence of
the 4,5-epidioxide of lophine as a reaction intermediate
of its chemiluminescence.
This study sheds light on the
long standing problem of the presence of
the 4,5-epidioxide of lophine.
;

#===================================================================
data_p_1
_database_code_depnum_ccdc_archive 'CCDC 859985'
#TrackingRef '- product1.cif'

#===================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H42 N4 O4'
_chemical_formula_weight         834.94

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.544(3)
_cell_length_b                   15.291(4)
_cell_length_c                   15.387(4)
_cell_angle_alpha                64.648(3)
_cell_angle_beta                 74.579(3)
_cell_angle_gamma                83.447(3)
_cell_volume                     2161.3(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    90
_cell_measurement_reflns_used    4540
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.17

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             876
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9605
_exptl_absorpt_correction_T_max  0.9919
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90
_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 APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            12022
_diffrn_reflns_av_R_equivalents  0.0131
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         27.18
_reflns_number_total             9125
_reflns_number_gt                7142
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_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^)+(0.0520P)^2^+0.7828P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9125
_refine_ls_number_parameters     579
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.1124
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.08968(15) 0.05754(11) 0.86499(11) 0.0186(3) Uani 1 1 d . . .
H1 H -0.1641 0.0878 0.8914 0.022 Uiso 1 1 calc R . .
C2 C 0.09989(14) 0.34314(10) 0.40490(10) 0.0157(3) Uani 1 1 d . . .
C3 C 0.12585(14) 0.07026(10) 0.75538(11) 0.0171(3) Uani 1 1 d . . .
C4 C -0.08643(14) -0.04329(11) 0.89858(11) 0.0181(3) Uani 1 1 d . . .
C5 C -0.36657(14) -0.03334(11) 0.85947(11) 0.0177(3) Uani 1 1 d . . .
C6 C -0.27252(14) 0.02685(11) 0.76530(10) 0.0171(3) Uani 1 1 d . . .
C7 C 0.00411(14) 0.20579(10) 0.50566(11) 0.0160(3) Uani 1 1 d . . .
C8 C -0.09662(14) 0.14453(10) 0.59011(10) 0.0165(3) Uani 1 1 d . . .
C9 C -0.17120(14) -0.01468(11) 0.71521(11) 0.0177(3) Uani 1 1 d . . .
H9 H -0.1618 -0.0831 0.7407 0.021 Uiso 1 1 calc R . .
C10 C 0.04188(15) 0.51297(11) 0.37440(11) 0.0195(3) Uani 1 1 d . . .
H10 H -0.0354 0.4899 0.4262 0.023 Uiso 1 1 calc R . .
C11 C -0.33059(14) -0.09489(10) 0.95149(11) 0.0171(3) Uani 1 1 d . . .
C12 C 0.22692(14) 0.13240(11) 0.67160(11) 0.0169(3) Uani 1 1 d . . .
C13 C -0.20156(14) 0.18586(11) 0.63682(11) 0.0178(3) Uani 1 1 d . . .
H13 H -0.2131 0.2541 0.6098 0.021 Uiso 1 1 calc R . .
C14 C 0.13463(15) -0.03062(11) 0.79438(11) 0.0194(3) Uani 1 1 d . . .
H14 H 0.2125 -0.0609 0.7724 0.023 Uiso 1 1 calc R . .
C15 C -0.08484(14) 0.04334(11) 0.62890(11) 0.0179(3) Uani 1 1 d . . .
H15 H -0.0167 0.0144 0.5955 0.021 Uiso 1 1 calc R . .
C16 C 0.32179(15) 0.25895(12) 0.22466(12) 0.0230(3) Uani 1 1 d . . .
H16 H 0.3975 0.2440 0.2509 0.028 Uiso 1 1 calc R . .
C17 C 0.38397(14) 0.33078(10) 0.57840(11) 0.0173(3) Uani 1 1 d . . .
C18 C -0.43305(15) -0.15442(11) 1.03155(11) 0.0196(3) Uani 1 1 d . . .
C19 C 0.33514(14) 0.25823(10) 0.55100(11) 0.0167(3) Uani 1 1 d . . .
C20 C -0.20213(15) -0.10361(11) 0.97046(11) 0.0184(3) Uani 1 1 d . . .
C21 C 0.02930(15) -0.08658(11) 0.86545(11) 0.0202(3) Uani 1 1 d . . .
H21 H 0.0359 -0.1551 0.8919 0.024 Uiso 1 1 calc R . .
C22 C 0.50356(15) 0.32124(11) 0.60297(11) 0.0197(3) Uani 1 1 d . . .
H22 H 0.5605 0.2689 0.6012 0.024 Uiso 1 1 calc R . .
C23 C 0.41634(14) 0.16486(10) 0.56668(11) 0.0168(3) Uani 1 1 d . . .
C24 C -0.40508(16) -0.22059(11) 1.12249(11) 0.0222(3) Uani 1 1 d . . .
H24 H -0.4736 -0.2603 1.1740 0.027 Uiso 1 1 calc R . .
C25 C 0.17810(16) 0.64536(11) 0.24804(12) 0.0228(3) Uani 1 1 d . . .
H25 H 0.1943 0.7130 0.2129 0.027 Uiso 1 1 calc R . .
C26 C 0.54622(14) 0.15626(11) 0.50580(11) 0.0178(3) Uani 1 1 d . . .
C27 C 0.19992(14) 0.26869(10) 0.28286(11) 0.0165(3) Uani 1 1 d . . .
C28 C 0.12984(14) 0.44686(10) 0.34933(11) 0.0163(3) Uani 1 1 d . . .
C29 C -0.28925(14) 0.12719(11) 0.72287(11) 0.0186(3) Uani 1 1 d . . .
H29 H -0.3617 0.1558 0.7533 0.022 Uiso 1 1 calc R . .
C30 C -0.28210(16) -0.22847(12) 1.13767(11) 0.0239(3) Uani 1 1 d . . .
H30 H -0.2647 -0.2729 1.1991 0.029 Uiso 1 1 calc R . .
C31 C 0.01432(15) 0.11334(11) 0.79387(11) 0.0187(3) Uani 1 1 d . . .
H31 H 0.0101 0.1818 0.7708 0.022 Uiso 1 1 calc R . .
C32 C 0.18371(14) 0.25982(10) 0.38799(11) 0.0165(3) Uani 1 1 d . . .
C33 C 0.30179(15) 0.40859(11) 0.58018(11) 0.0220(3) Uani 1 1 d . . .
H33 H 0.2201 0.4156 0.5628 0.026 Uiso 1 1 calc R . .
C34 C 0.53991(16) 0.38882(12) 0.63027(11) 0.0243(3) Uani 1 1 d . . .
H34 H 0.6221 0.3823 0.6469 0.029 Uiso 1 1 calc R . .
C35 C 0.60811(15) 0.06533(11) 0.53014(12) 0.0216(3) Uani 1 1 d . . .
H35 H 0.5672 0.0109 0.5871 0.026 Uiso 1 1 calc R . .
C36 C 0.24347(15) 0.48151(11) 0.27320(11) 0.0193(3) Uani 1 1 d . . .
H36 H 0.3047 0.4374 0.2561 0.023 Uiso 1 1 calc R . .
C37 C -0.18109(16) -0.16957(11) 1.06076(11) 0.0223(3) Uani 1 1 d . . .
H37 H -0.0952 -0.1754 1.0713 0.027 Uiso 1 1 calc R . .
C38 C -0.49575(15) -0.02926(11) 0.85428(12) 0.0226(3) Uani 1 1 d . . .
H38 H -0.5183 0.0133 0.7941 0.027 Uiso 1 1 calc R . .
C39 C 0.06604(16) 0.61168(11) 0.32461(12) 0.0229(3) Uani 1 1 d . . .
H39 H 0.0064 0.6559 0.3428 0.027 Uiso 1 1 calc R . .
C40 C 0.22366(18) 0.29391(12) 0.08883(12) 0.0281(4) Uani 1 1 d . . .
H40 H 0.2322 0.3032 0.0224 0.034 Uiso 1 1 calc R . .
C41 C 0.09004(16) 0.28997(11) 0.24361(12) 0.0223(3) Uani 1 1 d . . .
H41 H 0.0062 0.2955 0.2834 0.027 Uiso 1 1 calc R . .
C42 C 0.26682(15) 0.58054(11) 0.22246(11) 0.0217(3) Uani 1 1 d . . .
H42 H 0.3435 0.6040 0.1702 0.026 Uiso 1 1 calc R . .
C43 C -0.56328(15) -0.14811(11) 1.02048(12) 0.0229(3) Uani 1 1 d . . .
H43 H -0.6296 -0.1882 1.0740 0.028 Uiso 1 1 calc R . .
C44 C 0.33888(17) 0.47575(12) 0.60726(12) 0.0255(4) Uani 1 1 d . . .
H44 H 0.2829 0.5289 0.6079 0.031 Uiso 1 1 calc R . .
C45 C 0.72711(16) 0.22418(12) 0.36300(12) 0.0266(4) Uani 1 1 d . . .
H45 H 0.7680 0.2781 0.3055 0.032 Uiso 1 1 calc R . .
C46 C 0.45803(17) 0.46517(12) 0.63342(12) 0.0260(4) Uani 1 1 d . . .
H46 H 0.4830 0.5102 0.6533 0.031 Uiso 1 1 calc R . .
C47 C -0.59544(16) -0.08551(12) 0.93446(12) 0.0257(4) Uani 1 1 d . . .
H47 H -0.6839 -0.0800 0.9289 0.031 Uiso 1 1 calc R . .
C48 C 0.10180(17) 0.30318(12) 0.14660(12) 0.0276(4) Uani 1 1 d . . .
H48 H 0.0264 0.3185 0.1200 0.033 Uiso 1 1 calc R . .
C49 C 0.72833(16) 0.05468(12) 0.47157(13) 0.0248(3) Uani 1 1 d . . .
H49 H 0.7701 -0.0068 0.4884 0.030 Uiso 1 1 calc R . .
C50 C 0.60703(15) 0.23565(11) 0.42164(12) 0.0229(3) Uani 1 1 d . . .
H50 H 0.5662 0.2975 0.4046 0.027 Uiso 1 1 calc R . .
C51 C 0.78771(16) 0.13416(12) 0.38810(12) 0.0266(4) Uani 1 1 d . . .
H51 H 0.8703 0.1269 0.3479 0.032 Uiso 1 1 calc R . .
C52 C 0.33270(17) 0.27109(12) 0.12830(12) 0.0283(4) Uani 1 1 d . . .
H52 H 0.4160 0.2636 0.0890 0.034 Uiso 1 1 calc R . .
C53 C 0.6689(3) 0.4258(3) 0.0211(3) 0.0979(12) Uani 1 1 d . . .
H53A H 0.5777 0.4268 0.0166 0.147 Uiso 1 1 calc R . .
H53B H 0.7038 0.3599 0.0384 0.147 Uiso 1 1 calc R . .
H53C H 0.7223 0.4695 -0.0428 0.147 Uiso 1 1 calc R . .
C54 C 0.9497(2) 0.55195(16) 0.12904(17) 0.0492(6) Uani 1 1 d . . .
H54A H 1.0142 0.5017 0.1244 0.074 Uiso 1 1 calc R . .
H54B H 0.9648 0.5748 0.1760 0.074 Uiso 1 1 calc R . .
H54C H 0.9591 0.6061 0.0637 0.074 Uiso 1 1 calc R . .
C55 C 0.8136(2) 0.51097(16) 0.16429(15) 0.0482(5) Uani 1 1 d . . .
H55A H 0.8012 0.4589 0.2321 0.058 Uiso 1 1 calc R . .
H55B H 0.7476 0.5622 0.1657 0.058 Uiso 1 1 calc R . .
C56 C 0.6730(3) 0.4581(2) 0.0992(2) 0.0644(7) Uani 1 1 d . . .
N1 N -0.00724(12) 0.30967(9) 0.47161(9) 0.0169(3) Uani 1 1 d . . .
N2 N 0.35200(12) 0.09261(9) 0.64104(9) 0.0185(3) Uani 1 1 d . . .
N3 N 0.10713(12) 0.17366(9) 0.46161(9) 0.0182(3) Uani 1 1 d . . .
N4 N 0.20755(12) 0.22272(9) 0.62043(9) 0.0179(3) Uani 1 1 d . . .
O1 O 0.32573(10) 0.31563(7) 0.45127(7) 0.0183(2) Uani 1 1 d . . .
O2 O 0.31300(10) 0.25177(8) 0.40439(8) 0.0203(2) Uani 1 1 d . . .
O3 O 0.79710(15) 0.47270(12) 0.09693(11) 0.0500(4) Uani 1 1 d . . .
O4 O 0.5801(2) 0.4701(2) 0.15583(18) 0.1030(8) 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 0.0173(7) 0.0201(7) 0.0185(7) -0.0088(6) -0.0038(6) 0.0014(6)
C2 0.0149(7) 0.0192(7) 0.0149(7) -0.0076(6) -0.0058(6) 0.0006(6)
C3 0.0152(7) 0.0191(7) 0.0168(7) -0.0062(6) -0.0050(6) -0.0021(6)
C4 0.0180(7) 0.0210(8) 0.0156(7) -0.0064(6) -0.0055(6) -0.0027(6)
C5 0.0173(7) 0.0177(7) 0.0166(7) -0.0070(6) -0.0018(6) -0.0001(6)
C6 0.0164(7) 0.0188(7) 0.0142(7) -0.0051(6) -0.0034(6) -0.0011(6)
C7 0.0158(7) 0.0159(7) 0.0157(7) -0.0050(6) -0.0061(6) 0.0016(5)
C8 0.0160(7) 0.0180(7) 0.0145(7) -0.0053(6) -0.0043(6) -0.0008(6)
C9 0.0183(7) 0.0156(7) 0.0180(7) -0.0055(6) -0.0050(6) 0.0000(6)
C10 0.0173(7) 0.0192(7) 0.0188(7) -0.0062(6) -0.0020(6) 0.0002(6)
C11 0.0191(7) 0.0152(7) 0.0162(7) -0.0072(6) -0.0016(6) -0.0001(6)
C12 0.0149(7) 0.0192(7) 0.0179(7) -0.0082(6) -0.0054(6) 0.0003(6)
C13 0.0171(7) 0.0174(7) 0.0178(7) -0.0063(6) -0.0047(6) 0.0011(6)
C14 0.0156(7) 0.0204(8) 0.0215(8) -0.0079(6) -0.0051(6) 0.0015(6)
C15 0.0171(7) 0.0196(7) 0.0173(7) -0.0086(6) -0.0037(6) 0.0020(6)
C16 0.0189(8) 0.0287(9) 0.0242(8) -0.0155(7) -0.0014(6) -0.0010(6)
C17 0.0182(7) 0.0166(7) 0.0135(7) -0.0039(6) -0.0016(6) -0.0019(6)
C18 0.0218(8) 0.0181(7) 0.0173(7) -0.0083(6) 0.0002(6) -0.0013(6)
C19 0.0142(7) 0.0173(7) 0.0160(7) -0.0047(6) -0.0034(6) 0.0003(5)
C20 0.0196(8) 0.0177(7) 0.0175(7) -0.0078(6) -0.0022(6) -0.0023(6)
C21 0.0216(8) 0.0159(7) 0.0219(8) -0.0055(6) -0.0077(6) 0.0003(6)
C22 0.0199(8) 0.0204(8) 0.0165(7) -0.0056(6) -0.0042(6) -0.0007(6)
C23 0.0170(7) 0.0181(7) 0.0178(7) -0.0086(6) -0.0067(6) 0.0007(6)
C24 0.0242(8) 0.0219(8) 0.0159(7) -0.0064(6) 0.0021(6) -0.0050(6)
C25 0.0254(8) 0.0159(7) 0.0233(8) -0.0045(6) -0.0052(7) -0.0029(6)
C26 0.0150(7) 0.0201(7) 0.0200(7) -0.0098(6) -0.0047(6) 0.0010(6)
C27 0.0189(7) 0.0131(7) 0.0163(7) -0.0057(6) -0.0022(6) -0.0013(5)
C28 0.0172(7) 0.0167(7) 0.0160(7) -0.0068(6) -0.0056(6) 0.0000(6)
C29 0.0161(7) 0.0201(8) 0.0182(7) -0.0077(6) -0.0036(6) 0.0027(6)
C30 0.0311(9) 0.0227(8) 0.0144(7) -0.0046(6) -0.0044(6) -0.0015(7)
C31 0.0205(8) 0.0163(7) 0.0183(7) -0.0059(6) -0.0055(6) -0.0006(6)
C32 0.0131(7) 0.0169(7) 0.0172(7) -0.0059(6) -0.0022(6) 0.0003(5)
C33 0.0195(8) 0.0207(8) 0.0208(8) -0.0063(6) -0.0008(6) -0.0003(6)
C34 0.0261(9) 0.0261(8) 0.0190(8) -0.0060(7) -0.0060(7) -0.0060(7)
C35 0.0199(8) 0.0208(8) 0.0240(8) -0.0088(7) -0.0067(6) 0.0015(6)
C36 0.0173(7) 0.0212(8) 0.0204(8) -0.0103(6) -0.0036(6) 0.0005(6)
C37 0.0230(8) 0.0235(8) 0.0196(8) -0.0072(7) -0.0062(6) -0.0017(6)
C38 0.0205(8) 0.0239(8) 0.0190(8) -0.0056(7) -0.0038(6) 0.0007(6)
C39 0.0226(8) 0.0191(8) 0.0252(8) -0.0095(7) -0.0036(6) 0.0029(6)
C40 0.0423(10) 0.0243(8) 0.0186(8) -0.0105(7) -0.0049(7) -0.0027(7)
C41 0.0213(8) 0.0238(8) 0.0231(8) -0.0116(7) -0.0050(6) 0.0022(6)
C42 0.0195(8) 0.0232(8) 0.0190(8) -0.0073(6) -0.0002(6) -0.0041(6)
C43 0.0190(8) 0.0240(8) 0.0194(8) -0.0069(7) 0.0038(6) -0.0047(6)
C44 0.0306(9) 0.0198(8) 0.0223(8) -0.0094(7) 0.0013(7) -0.0010(7)
C45 0.0202(8) 0.0261(9) 0.0246(8) -0.0057(7) 0.0007(7) -0.0005(6)
C46 0.0354(10) 0.0229(8) 0.0186(8) -0.0088(7) -0.0007(7) -0.0091(7)
C47 0.0163(8) 0.0316(9) 0.0259(8) -0.0104(7) -0.0015(6) -0.0016(6)
C48 0.0334(9) 0.0286(9) 0.0267(9) -0.0143(7) -0.0142(7) 0.0050(7)
C49 0.0222(8) 0.0220(8) 0.0321(9) -0.0139(7) -0.0073(7) 0.0056(6)
C50 0.0177(8) 0.0208(8) 0.0266(8) -0.0073(7) -0.0051(6) 0.0030(6)
C51 0.0184(8) 0.0331(9) 0.0288(9) -0.0165(8) -0.0019(7) 0.0035(7)
C52 0.0279(9) 0.0336(9) 0.0253(9) -0.0187(8) 0.0041(7) -0.0064(7)
C53 0.0651(19) 0.161(3) 0.111(3) -0.103(3) 0.0020(18) -0.030(2)
C54 0.0666(15) 0.0428(12) 0.0492(13) -0.0214(10) -0.0324(12) 0.0118(11)
C55 0.0784(16) 0.0379(11) 0.0290(10) -0.0174(9) -0.0086(10) 0.0007(11)
C56 0.0492(15) 0.088(2) 0.0668(17) -0.0503(16) 0.0068(13) -0.0149(13)
N1 0.0161(6) 0.0160(6) 0.0166(6) -0.0050(5) -0.0037(5) 0.0000(5)
N2 0.0155(6) 0.0199(6) 0.0200(6) -0.0079(5) -0.0051(5) 0.0002(5)
N3 0.0168(6) 0.0172(6) 0.0163(6) -0.0042(5) -0.0018(5) 0.0000(5)
N4 0.0151(6) 0.0199(6) 0.0174(6) -0.0065(5) -0.0035(5) -0.0013(5)
O1 0.0207(5) 0.0169(5) 0.0181(5) -0.0070(4) -0.0060(4) -0.0004(4)
O2 0.0170(5) 0.0267(6) 0.0229(6) -0.0157(5) -0.0068(4) 0.0048(4)
O3 0.0479(9) 0.0663(10) 0.0475(9) -0.0386(8) -0.0027(7) -0.0043(7)
O4 0.0554(12) 0.170(2) 0.1099(18) -0.1024(18) 0.0239(12) -0.0253(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
C1 C31 1.380(2) . ?
C1 C4 1.400(2) . ?
C1 H1 0.9500 . ?
C2 N1 1.2873(19) . ?
C2 C28 1.468(2) . ?
C2 C32 1.542(2) . ?
C3 C14 1.397(2) . ?
C3 C31 1.398(2) . ?
C3 C12 1.467(2) . ?
C4 C21 1.400(2) . ?
C4 C20 1.493(2) . ?
C5 C38 1.378(2) . ?
C5 C11 1.448(2) . ?
C5 C6 1.494(2) . ?
C6 C29 1.398(2) . ?
C6 C9 1.402(2) . ?
C7 N3 1.2856(19) . ?
C7 N1 1.4453(19) . ?
C7 C8 1.465(2) . ?
C8 C13 1.395(2) . ?
C8 C15 1.404(2) . ?
C9 C15 1.383(2) . ?
C9 H9 0.9500 . ?
C10 C39 1.387(2) . ?
C10 C28 1.400(2) . ?
C10 H10 0.9500 . ?
C11 C18 1.439(2) . ?
C11 C20 1.440(2) . ?
C12 N4 1.2880(19) . ?
C12 N2 1.4362(19) . ?
C13 C29 1.391(2) . ?
C13 H13 0.9500 . ?
C14 C21 1.390(2) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C52 1.387(2) . ?
C16 C27 1.391(2) . ?
C16 H16 0.9500 . ?
C17 C22 1.385(2) . ?
C17 C33 1.395(2) . ?
C17 C19 1.523(2) . ?
C18 C43 1.416(2) . ?
C18 C24 1.417(2) . ?
C19 O1 1.4292(17) . ?
C19 N4 1.4669(19) . ?
C19 C23 1.538(2) . ?
C20 C37 1.382(2) . ?
C21 H21 0.9500 . ?
C22 C34 1.392(2) . ?
C22 H22 0.9500 . ?
C23 N2 1.2906(19) . ?
C23 C26 1.467(2) . ?
C24 C30 1.361(2) . ?
C24 H24 0.9500 . ?
C25 C39 1.389(2) . ?
C25 C42 1.393(2) . ?
C25 H25 0.9500 . ?
C26 C50 1.397(2) . ?
C26 C35 1.406(2) . ?
C27 C41 1.390(2) . ?
C27 C32 1.528(2) . ?
C28 C36 1.398(2) . ?
C29 H29 0.9500 . ?
C30 C37 1.408(2) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 O2 1.4338(17) . ?
C32 N3 1.4661(18) . ?
C33 C44 1.388(2) . ?
C33 H33 0.9500 . ?
C34 C46 1.381(2) . ?
C34 H34 0.9500 . ?
C35 C49 1.384(2) . ?
C35 H35 0.9500 . ?
C36 C42 1.390(2) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C47 1.405(2) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C52 1.382(2) . ?
C40 C48 1.386(2) . ?
C40 H40 0.9500 . ?
C41 C48 1.390(2) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C47 1.365(2) . ?
C43 H43 0.9500 . ?
C44 C46 1.391(2) . ?
C44 H44 0.9500 . ?
C45 C50 1.387(2) . ?
C45 C51 1.388(2) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C51 1.388(2) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C56 1.493(4) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.499(3) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 O3 1.444(2) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 O4 1.181(3) . ?
C56 O3 1.341(3) . ?
O1 O2 1.4751(14) . ?

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
C31 C1 C4 120.53(14) . . ?
C31 C1 H1 119.7 . . ?
C4 C1 H1 119.7 . . ?
N1 C2 C28 123.44(13) . . ?
N1 C2 C32 110.17(12) . . ?
C28 C2 C32 126.24(13) . . ?
C14 C3 C31 119.12(13) . . ?
C14 C3 C12 121.93(14) . . ?
C31 C3 C12 118.86(13) . . ?
C1 C4 C21 118.47(13) . . ?
C1 C4 C20 120.84(14) . . ?
C21 C4 C20 120.67(13) . . ?
C38 C5 C11 119.75(14) . . ?
C38 C5 C6 115.30(13) . . ?
C11 C5 C6 124.93(13) . . ?
C29 C6 C9 118.60(13) . . ?
C29 C6 C5 119.39(13) . . ?
C9 C6 C5 121.93(13) . . ?
N3 C7 N1 116.61(13) . . ?
N3 C7 C8 124.47(13) . . ?
N1 C7 C8 118.83(12) . . ?
C13 C8 C15 118.97(13) . . ?
C13 C8 C7 120.49(13) . . ?
C15 C8 C7 120.44(13) . . ?
C15 C9 C6 120.36(14) . . ?
C15 C9 H9 119.8 . . ?
C6 C9 H9 119.8 . . ?
C39 C10 C28 120.86(14) . . ?
C39 C10 H10 119.6 . . ?
C28 C10 H10 119.6 . . ?
C18 C11 C20 116.71(13) . . ?
C18 C11 C5 116.72(13) . . ?
C20 C11 C5 126.57(13) . . ?
N4 C12 N2 117.04(13) . . ?
N4 C12 C3 122.66(13) . . ?
N2 C12 C3 120.27(13) . . ?
C29 C13 C8 120.01(14) . . ?
C29 C13 H13 120.0 . . ?
C8 C13 H13 120.0 . . ?
C21 C14 C3 119.88(14) . . ?
C21 C14 H14 120.1 . . ?
C3 C14 H14 120.1 . . ?
C9 C15 C8 120.77(14) . . ?
C9 C15 H15 119.6 . . ?
C8 C15 H15 119.6 . . ?
C52 C16 C27 119.93(15) . . ?
C52 C16 H16 120.0 . . ?
C27 C16 H16 120.0 . . ?
C22 C17 C33 119.69(14) . . ?
C22 C17 C19 122.85(13) . . ?
C33 C17 C19 117.45(13) . . ?
C43 C18 C24 118.98(14) . . ?
C43 C18 C11 120.48(14) . . ?
C24 C18 C11 120.54(14) . . ?
O1 C19 N4 113.38(11) . . ?
O1 C19 C17 102.66(11) . . ?
N4 C19 C17 106.70(12) . . ?
O1 C19 C23 115.12(12) . . ?
N4 C19 C23 102.93(11) . . ?
C17 C19 C23 116.11(12) . . ?
C37 C20 C11 119.95(14) . . ?
C37 C20 C4 115.92(14) . . ?
C11 C20 C4 124.11(13) . . ?
C14 C21 C4 120.90(14) . . ?
C14 C21 H21 119.5 . . ?
C4 C21 H21 119.5 . . ?
C17 C22 C34 119.65(15) . . ?
C17 C22 H22 120.2 . . ?
C34 C22 H22 120.2 . . ?
N2 C23 C26 123.82(13) . . ?
N2 C23 C19 109.99(13) . . ?
C26 C23 C19 126.17(13) . . ?
C30 C24 C18 121.41(14) . . ?
C30 C24 H24 119.3 . . ?
C18 C24 H24 119.3 . . ?
C39 C25 C42 120.32(14) . . ?
C39 C25 H25 119.8 . . ?
C42 C25 H25 119.8 . . ?
C50 C26 C35 119.30(14) . . ?
C50 C26 C23 121.35(13) . . ?
C35 C26 C23 119.29(13) . . ?
C41 C27 C16 119.30(14) . . ?
C41 C27 C32 118.77(13) . . ?
C16 C27 C32 121.90(13) . . ?
C36 C28 C10 119.13(14) . . ?
C36 C28 C2 122.26(13) . . ?
C10 C28 C2 118.61(13) . . ?
C13 C29 C6 121.05(14) . . ?
C13 C29 H29 119.5 . . ?
C6 C29 H29 119.5 . . ?
C24 C30 C37 118.84(15) . . ?
C24 C30 H30 120.6 . . ?
C37 C30 H30 120.6 . . ?
C1 C31 C3 120.71(14) . . ?
C1 C31 H31 119.6 . . ?
C3 C31 H31 119.6 . . ?
O2 C32 N3 109.21(11) . . ?
O2 C32 C27 107.22(11) . . ?
N3 C32 C27 111.21(12) . . ?
O2 C32 C2 114.78(12) . . ?
N3 C32 C2 102.93(11) . . ?
C27 C32 C2 111.51(11) . . ?
C44 C33 C17 120.30(15) . . ?
C44 C33 H33 119.8 . . ?
C17 C33 H33 119.8 . . ?
C46 C34 C22 120.82(15) . . ?
C46 C34 H34 119.6 . . ?
C22 C34 H34 119.6 . . ?
C49 C35 C26 120.34(15) . . ?
C49 C35 H35 119.8 . . ?
C26 C35 H35 119.8 . . ?
C42 C36 C28 119.98(14) . . ?
C42 C36 H36 120.0 . . ?
C28 C36 H36 120.0 . . ?
C20 C37 C30 122.51(15) . . ?
C20 C37 H37 118.7 . . ?
C30 C37 H37 118.7 . . ?
C5 C38 C47 122.61(15) . . ?
C5 C38 H38 118.7 . . ?
C47 C38 H38 118.7 . . ?
C10 C39 C25 119.51(14) . . ?
C10 C39 H39 120.2 . . ?
C25 C39 H39 120.2 . . ?
C52 C40 C48 119.69(15) . . ?
C52 C40 H40 120.2 . . ?
C48 C40 H40 120.2 . . ?
C27 C41 C48 120.52(15) . . ?
C27 C41 H41 119.7 . . ?
C48 C41 H41 119.7 . . ?
C36 C42 C25 120.17(14) . . ?
C36 C42 H42 119.9 . . ?
C25 C42 H42 119.9 . . ?
C47 C43 C18 121.31(14) . . ?
C47 C43 H43 119.3 . . ?
C18 C43 H43 119.3 . . ?
C33 C44 C46 119.91(15) . . ?
C33 C44 H44 120.0 . . ?
C46 C44 H44 120.0 . . ?
C50 C45 C51 120.23(15) . . ?
C50 C45 H45 119.9 . . ?
C51 C45 H45 119.9 . . ?
C34 C46 C44 119.62(15) . . ?
C34 C46 H46 120.2 . . ?
C44 C46 H46 120.2 . . ?
C43 C47 C38 118.99(15) . . ?
C43 C47 H47 120.5 . . ?
C38 C47 H47 120.5 . . ?
C40 C48 C41 119.87(16) . . ?
C40 C48 H48 120.1 . . ?
C41 C48 H48 120.1 . . ?
C35 C49 C51 119.79(15) . . ?
C35 C49 H49 120.1 . . ?
C51 C49 H49 120.1 . . ?
C45 C50 C26 119.97(15) . . ?
C45 C50 H50 120.0 . . ?
C26 C50 H50 120.0 . . ?
C49 C51 C45 120.37(15) . . ?
C49 C51 H51 119.8 . . ?
C45 C51 H51 119.8 . . ?
C40 C52 C16 120.67(16) . . ?
C40 C52 H52 119.7 . . ?
C16 C52 H52 119.7 . . ?
C56 C53 H53A 109.5 . . ?
C56 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C56 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 H54A 109.5 . . ?
C55 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C55 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O3 C55 C54 108.16(17) . . ?
O3 C55 H55A 110.1 . . ?
C54 C55 H55A 110.1 . . ?
O3 C55 H55B 110.1 . . ?
C54 C55 H55B 110.1 . . ?
H55A C55 H55B 108.4 . . ?
O4 C56 O3 123.6(2) . . ?
O4 C56 C53 125.2(3) . . ?
O3 C56 C53 111.2(2) . . ?
C2 N1 C7 104.81(12) . . ?
C23 N2 C12 104.67(12) . . ?
C7 N3 C32 105.35(12) . . ?
C12 N4 C19 104.63(12) . . ?
C19 O1 O2 109.54(10) . . ?
C32 O2 O1 110.28(10) . . ?
C56 O3 C55 116.46(18) . . ?

_diffrn_measured_fraction_theta_max 0.949
_diffrn_reflns_theta_full        27.18
_diffrn_measured_fraction_theta_full 0.949
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.045

#===================================================================
data_p_1_2
_database_code_depnum_ccdc_archive 'CCDC 859986'
#TrackingRef '- product2.cif'

#===================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H34 N4 O2'
_chemical_formula_weight         746.83

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.462(9)
_cell_length_b                   10.806(9)
_cell_length_c                   17.637(15)
_cell_angle_alpha                86.158(11)
_cell_angle_beta                 74.173(13)
_cell_angle_gamma                73.868(12)
_cell_volume                     1843(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    90
_cell_measurement_reflns_used    1410
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      23.85

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9836
_exptl_absorpt_correction_T_max  0.9959
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90
_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 APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            8427
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.1236
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         24.99
_reflns_number_total             6210
_reflns_number_gt                3680
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_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^)+(0.0725P)^2^+12.6970P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6210
_refine_ls_number_parameters     524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0917
_refine_ls_wR_factor_ref         0.2740
_refine_ls_wR_factor_gt          0.2496
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.3458(4) 0.9653(4) 0.3346(2) 0.0194(10) Uani 1 1 d . . .
O2 O 0.6909(5) 0.7204(5) 0.4617(3) 0.0328(12) Uani 1 1 d . . .
N3 N 0.3763(6) 0.9588(5) 0.1970(3) 0.0204(12) Uani 1 1 d . . .
N1 N 0.7576(6) 0.6889(5) 0.3278(3) 0.0204(12) Uani 1 1 d . . .
N2 N 0.5617(5) 0.8295(5) 0.2997(3) 0.0191(12) Uani 1 1 d . . .
N4 N 0.5707(5) 1.0335(5) 0.1632(3) 0.0198(12) Uani 1 1 d . . .
C1 C 0.7000(6) 0.6455(6) 0.2122(4) 0.0168(14) Uani 1 1 d . . .
C2 C 0.2480(6) 1.1585(6) 0.2751(4) 0.0173(14) Uani 1 1 d . . .
C3 C 0.6698(6) 0.7199(5) 0.2872(4) 0.0173(14) Uani 1 1 d . . .
C4 C 0.6443(7) 0.6816(6) -0.0383(4) 0.0197(14) Uani 1 1 d . . .
C5 C 0.8076(7) 0.8652(6) 0.3851(4) 0.0216(15) Uani 1 1 d . . .
C6 C 0.1016(7) 1.3442(6) 0.3524(4) 0.0230(15) Uani 1 1 d . . .
H6 H 0.0790 1.3974 0.3975 0.028 Uiso 1 1 calc R . .
C7 C 0.2134(7) 1.2367(6) 0.3409(4) 0.0239(15) Uani 1 1 d . . .
H7 H 0.2667 1.2162 0.3781 0.029 Uiso 1 1 calc R . .
C8 C 0.7434(6) 0.7560(6) 0.3950(4) 0.0215(15) Uani 1 1 d . . .
C9 C 0.5383(7) 0.8812(6) 0.0728(4) 0.0202(14) Uani 1 1 d . . .
C10 C 0.4882(7) 0.9624(6) 0.1441(4) 0.0211(15) Uani 1 1 d . . .
C11 C 0.4344(7) 0.8444(6) 0.3339(4) 0.0187(14) Uani 1 1 d . . .
C12 C 0.7714(7) 0.4405(6) -0.0682(4) 0.0216(15) Uani 1 1 d . . .
C13 C 0.6287(7) 0.5491(6) 0.1179(4) 0.0229(15) Uani 1 1 d . . .
H13 H 0.5561 0.5328 0.1009 0.027 Uiso 1 1 calc R . .
C14 C 0.6804(7) 0.8381(6) 0.0382(4) 0.0202(14) Uani 1 1 d . . .
H14 H 0.7416 0.8773 0.0522 0.024 Uiso 1 1 calc R . .
C15 C 0.7310(7) 0.7397(6) -0.0155(4) 0.0196(14) Uani 1 1 d . . .
H15 H 0.8279 0.7101 -0.0379 0.024 Uiso 1 1 calc R . .
C16 C 0.3631(6) 0.7500(6) 0.3767(3) 0.0169(14) Uani 1 1 d . . .
C17 C 0.7656(6) 0.4961(6) 0.0749(4) 0.0187(14) Uani 1 1 d . . .
C18 C 0.5012(7) 0.7355(6) -0.0095(4) 0.0228(15) Uani 1 1 d . . .
H18 H 0.4393 0.7042 -0.0286 0.027 Uiso 1 1 calc R . .
C19 C 0.8686(7) 0.5196(6) 0.1040(4) 0.0230(15) Uani 1 1 d . . .
H19 H 0.9626 0.4848 0.0766 0.028 Uiso 1 1 calc R . .
C20 C 0.6962(6) 0.5638(6) -0.0899(4) 0.0214(15) Uani 1 1 d . . .
C21 C 0.7837(7) 0.3589(7) -0.1993(4) 0.0263(16) Uani 1 1 d . . .
H21 H 0.8146 0.2907 -0.2368 0.032 Uiso 1 1 calc R . .
C22 C 0.4311(7) 0.6398(6) 0.4082(4) 0.0210(14) Uani 1 1 d . . .
H22 H 0.5272 0.6234 0.4029 0.025 Uiso 1 1 calc R . .
C23 C 0.4505(7) 0.8317(6) 0.0453(4) 0.0220(15) Uani 1 1 d . . .
H23 H 0.3535 0.8654 0.0650 0.026 Uiso 1 1 calc R . .
C24 C 0.8178(7) 0.3376(6) -0.1260(4) 0.0228(15) Uani 1 1 d . . .
C25 C 0.0218(7) 1.3758(6) 0.2991(4) 0.0253(16) Uani 1 1 d . . .
H25 H -0.0564 1.4487 0.3078 0.030 Uiso 1 1 calc R . .
C26 C 0.8372(7) 0.5919(6) 0.1713(4) 0.0195(14) Uani 1 1 d . . .
H26 H 0.9094 0.6053 0.1900 0.023 Uiso 1 1 calc R . .
C27 C 0.5089(6) 1.0731(6) 0.2346(4) 0.0181(14) Uani 1 1 d . . .
C28 C 0.5603(6) 1.1537(6) 0.2763(4) 0.0195(14) Uani 1 1 d . . .
C29 C 0.1695(7) 1.1887(6) 0.2216(4) 0.0226(15) Uani 1 1 d . . .
H29 H 0.1911 1.1346 0.1770 0.027 Uiso 1 1 calc R . .
C30 C 0.5966(7) 0.6247(6) 0.1843(4) 0.0216(15) Uani 1 1 d . . .
H30 H 0.5027 0.6625 0.2109 0.026 Uiso 1 1 calc R . .
C31 C 0.2228(7) 0.5741(6) 0.4539(4) 0.0236(15) Uani 1 1 d . . .
H31 H 0.1754 0.5137 0.4804 0.028 Uiso 1 1 calc R . .
C32 C 0.8750(7) 1.0223(6) 0.4444(4) 0.0263(16) Uani 1 1 d . . .
H32 H 0.8797 1.0612 0.4900 0.032 Uiso 1 1 calc R . .
C33 C 0.8060(7) 0.4089(6) 0.0062(4) 0.0209(15) Uani 1 1 d . . .
C34 C 0.8835(7) 0.2877(6) 0.0171(4) 0.0243(15) Uani 1 1 d . . .
H34 H 0.9066 0.2685 0.0658 0.029 Uiso 1 1 calc R . .
C35 C 0.7066(7) 0.4773(7) -0.2165(4) 0.0264(16) Uani 1 1 d . . .
H35 H 0.6830 0.4902 -0.2653 0.032 Uiso 1 1 calc R . .
C36 C 0.8649(7) 0.9068(6) 0.3111(4) 0.0223(15) Uani 1 1 d . . .
H36 H 0.8623 0.8666 0.2655 0.027 Uiso 1 1 calc R . .
C37 C 0.8955(7) 0.2152(6) -0.1102(4) 0.0253(16) Uani 1 1 d . . .
H37 H 0.9237 0.1489 -0.1487 0.030 Uiso 1 1 calc R . .
C38 C 0.9318(7) 1.0635(6) 0.3702(4) 0.0256(16) Uani 1 1 d . . .
H38 H 0.9752 1.1313 0.3650 0.031 Uiso 1 1 calc R . .
C39 C 0.2219(7) 0.7716(6) 0.3838(4) 0.0253(15) Uani 1 1 d . . .
H39 H 0.1729 0.8472 0.3625 0.030 Uiso 1 1 calc R . .
C40 C 0.3699(7) 1.0390(6) 0.2617(4) 0.0200(14) Uani 1 1 d . . .
C41 C 0.6627(7) 0.5789(6) -0.1620(4) 0.0232(15) Uani 1 1 d . . .
H41 H 0.6088 0.6601 -0.1743 0.028 Uiso 1 1 calc R . .
C42 C 0.0586(7) 1.2987(6) 0.2331(4) 0.0256(16) Uani 1 1 d . . .
H42 H 0.0075 1.3210 0.1948 0.031 Uiso 1 1 calc R . .
C43 C 0.8120(7) 0.9251(6) 0.4519(4) 0.0247(15) Uani 1 1 d . . .
H43 H 0.7709 0.8981 0.5028 0.030 Uiso 1 1 calc R . .
C44 C 0.9312(7) 0.1890(6) -0.0417(4) 0.0286(16) Uani 1 1 d . . .
H44 H 0.9870 0.1064 -0.0329 0.034 Uiso 1 1 calc R . .
C45 C 0.9264(7) 1.0072(7) 0.3033(4) 0.0287(16) Uani 1 1 d . . .
H45 H 0.9643 1.0371 0.2525 0.034 Uiso 1 1 calc R . .
C46 C 0.3624(7) 0.5529(6) 0.4475(4) 0.0236(15) Uani 1 1 d . . .
H46 H 0.4105 0.4784 0.4702 0.028 Uiso 1 1 calc R . .
C47 C 0.5379(7) 1.1502(6) 0.3586(4) 0.0235(15) Uani 1 1 d . . .
H47 H 0.4857 1.0964 0.3893 0.028 Uiso 1 1 calc R . .
C48 C 0.6348(7) 1.2355(6) 0.2329(4) 0.0226(15) Uani 1 1 d . . .
H48 H 0.6513 1.2384 0.1772 0.027 Uiso 1 1 calc R . .
C49 C 0.6854(7) 1.3130(6) 0.2708(4) 0.0259(16) Uani 1 1 d . . .
H49 H 0.7355 1.3692 0.2410 0.031 Uiso 1 1 calc R . .
C50 C 0.1536(7) 0.6823(7) 0.4221(4) 0.0280(16) Uani 1 1 d . . .
H50 H 0.0581 0.6965 0.4261 0.034 Uiso 1 1 calc R . .
C51 C 0.6626(7) 1.3080(6) 0.3516(4) 0.0273(16) Uani 1 1 d . . .
H51 H 0.6955 1.3618 0.3777 0.033 Uiso 1 1 calc R . .
C52 C 0.5918(7) 1.2247(6) 0.3946(4) 0.0259(16) Uani 1 1 d . . .
H52 H 0.5803 1.2188 0.4499 0.031 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
O1 0.023(2) 0.011(2) 0.018(2) 0.0058(17) -0.0030(19) -0.0004(19)
O2 0.043(3) 0.033(3) 0.025(3) 0.008(2) -0.010(2) -0.015(2)
N3 0.025(3) 0.012(3) 0.026(3) 0.004(2) -0.010(3) -0.006(2)
N1 0.024(3) 0.018(3) 0.019(3) 0.002(2) -0.006(2) -0.005(2)
N2 0.020(3) 0.017(3) 0.020(3) 0.005(2) -0.007(2) -0.005(2)
N4 0.021(3) 0.013(3) 0.023(3) 0.002(2) -0.007(2) 0.000(2)
C1 0.018(3) 0.014(3) 0.019(3) 0.006(3) -0.006(3) -0.005(3)
C2 0.019(3) 0.013(3) 0.021(3) 0.005(3) -0.005(3) -0.008(3)
C3 0.021(3) 0.009(3) 0.023(3) 0.004(2) -0.007(3) -0.005(3)
C4 0.022(3) 0.018(3) 0.020(3) 0.008(3) -0.007(3) -0.007(3)
C5 0.020(3) 0.023(4) 0.023(4) 0.000(3) -0.010(3) -0.004(3)
C6 0.024(4) 0.016(3) 0.026(4) 0.005(3) -0.002(3) -0.007(3)
C7 0.026(4) 0.024(4) 0.025(4) 0.008(3) -0.008(3) -0.012(3)
C8 0.016(3) 0.023(4) 0.024(4) 0.003(3) -0.007(3) -0.004(3)
C9 0.022(3) 0.016(3) 0.022(3) 0.012(3) -0.008(3) -0.005(3)
C10 0.020(3) 0.016(3) 0.030(4) 0.012(3) -0.014(3) -0.005(3)
C11 0.024(4) 0.014(3) 0.020(3) 0.000(3) -0.010(3) -0.003(3)
C12 0.020(3) 0.024(4) 0.025(4) 0.007(3) -0.008(3) -0.013(3)
C13 0.023(4) 0.022(3) 0.027(4) 0.006(3) -0.009(3) -0.009(3)
C14 0.019(3) 0.019(3) 0.022(3) -0.002(3) -0.003(3) -0.007(3)
C15 0.016(3) 0.022(3) 0.021(3) 0.006(3) -0.007(3) -0.006(3)
C16 0.019(3) 0.012(3) 0.016(3) -0.003(2) -0.001(3) -0.001(3)
C17 0.020(3) 0.020(3) 0.017(3) 0.005(3) -0.002(3) -0.009(3)
C18 0.024(4) 0.020(3) 0.026(4) 0.005(3) -0.007(3) -0.009(3)
C19 0.020(3) 0.018(3) 0.029(4) 0.004(3) -0.004(3) -0.006(3)
C20 0.017(3) 0.024(4) 0.027(4) 0.002(3) -0.006(3) -0.013(3)
C21 0.026(4) 0.030(4) 0.023(4) -0.007(3) 0.002(3) -0.015(3)
C22 0.021(3) 0.020(3) 0.023(3) 0.004(3) -0.008(3) -0.006(3)
C23 0.016(3) 0.020(3) 0.030(4) 0.008(3) -0.008(3) -0.005(3)
C24 0.026(4) 0.022(4) 0.023(4) 0.000(3) -0.003(3) -0.013(3)
C25 0.020(3) 0.016(3) 0.036(4) 0.003(3) 0.000(3) -0.006(3)
C26 0.022(3) 0.017(3) 0.022(3) 0.006(3) -0.007(3) -0.009(3)
C27 0.016(3) 0.013(3) 0.025(4) 0.007(3) -0.012(3) 0.001(3)
C28 0.017(3) 0.017(3) 0.027(4) 0.003(3) -0.008(3) -0.006(3)
C29 0.022(3) 0.023(4) 0.024(4) 0.004(3) -0.004(3) -0.010(3)
C30 0.025(4) 0.017(3) 0.021(3) 0.005(3) -0.004(3) -0.006(3)
C31 0.027(4) 0.020(3) 0.026(4) 0.002(3) -0.006(3) -0.012(3)
C32 0.022(4) 0.025(4) 0.036(4) -0.003(3) -0.012(3) -0.008(3)
C33 0.021(3) 0.023(4) 0.024(4) 0.006(3) -0.004(3) -0.015(3)
C34 0.029(4) 0.020(4) 0.025(4) 0.002(3) -0.007(3) -0.009(3)
C35 0.027(4) 0.036(4) 0.025(4) 0.006(3) -0.009(3) -0.021(3)
C36 0.023(4) 0.019(3) 0.024(4) -0.001(3) -0.006(3) -0.004(3)
C37 0.031(4) 0.020(4) 0.023(4) -0.005(3) 0.000(3) -0.009(3)
C38 0.027(4) 0.019(3) 0.033(4) 0.004(3) -0.011(3) -0.008(3)
C39 0.029(4) 0.023(4) 0.026(4) -0.001(3) -0.009(3) -0.007(3)
C40 0.030(4) 0.018(3) 0.013(3) 0.008(3) -0.006(3) -0.010(3)
C41 0.020(4) 0.025(4) 0.025(4) 0.004(3) -0.005(3) -0.010(3)
C42 0.026(4) 0.025(4) 0.028(4) 0.009(3) -0.009(3) -0.011(3)
C43 0.028(4) 0.027(4) 0.020(4) 0.006(3) -0.009(3) -0.006(3)
C44 0.030(4) 0.020(4) 0.032(4) -0.001(3) -0.001(3) -0.007(3)
C45 0.029(4) 0.027(4) 0.028(4) 0.002(3) -0.001(3) -0.011(3)
C46 0.029(4) 0.018(3) 0.022(4) 0.006(3) -0.009(3) -0.004(3)
C47 0.018(3) 0.027(4) 0.024(4) 0.004(3) -0.003(3) -0.007(3)
C48 0.023(4) 0.021(3) 0.024(4) 0.001(3) -0.009(3) -0.004(3)
C49 0.022(4) 0.019(3) 0.039(4) 0.006(3) -0.011(3) -0.008(3)
C50 0.021(4) 0.032(4) 0.036(4) 0.009(3) -0.012(3) -0.014(3)
C51 0.030(4) 0.020(4) 0.032(4) -0.008(3) -0.011(3) -0.002(3)
C52 0.024(4) 0.026(4) 0.025(4) -0.007(3) -0.004(3) -0.004(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C11 1.375(7) . ?
O1 C40 1.465(7) . ?
O2 C8 1.240(8) . ?
N3 C10 1.291(8) . ?
N3 C40 1.455(8) . ?
N1 C3 1.275(8) . ?
N1 C8 1.384(8) . ?
N2 C11 1.273(8) . ?
N2 C3 1.373(8) . ?
N4 C27 1.288(8) . ?
N4 C10 1.418(8) . ?
C1 C26 1.394(9) . ?
C1 C30 1.379(9) . ?
C1 C3 1.507(9) . ?
C2 C29 1.379(9) . ?
C2 C7 1.388(9) . ?
C2 C40 1.519(9) . ?
C4 C18 1.407(9) . ?
C4 C15 1.389(9) . ?
C4 C20 1.498(9) . ?
C5 C36 1.381(9) . ?
C5 C43 1.399(9) . ?
C5 C8 1.490(9) . ?
C6 C25 1.388(9) . ?
C6 C7 1.381(9) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C9 C23 1.384(9) . ?
C9 C14 1.399(9) . ?
C9 C10 1.470(9) . ?
C11 C16 1.476(9) . ?
C12 C20 1.433(9) . ?
C12 C33 1.450(9) . ?
C12 C24 1.446(9) . ?
C13 C30 1.383(9) . ?
C13 C17 1.401(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.363(9) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C22 1.374(8) . ?
C16 C39 1.401(9) . ?
C17 C19 1.400(9) . ?
C17 C33 1.478(9) . ?
C18 C23 1.358(9) . ?
C18 H18 0.9500 . ?
C19 C26 1.377(9) . ?
C19 H19 0.9500 . ?
C20 C41 1.395(9) . ?
C21 C35 1.374(10) . ?
C21 C24 1.420(9) . ?
C21 H21 0.9500 . ?
C22 C46 1.377(9) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C37 1.402(9) . ?
C25 C42 1.381(10) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.466(9) . ?
C27 C40 1.541(9) . ?
C28 C48 1.394(9) . ?
C28 C47 1.406(9) . ?
C29 C42 1.392(9) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C50 1.368(9) . ?
C31 C46 1.387(9) . ?
C31 H31 0.9500 . ?
C32 C43 1.369(9) . ?
C32 C38 1.382(10) . ?
C32 H32 0.9500 . ?
C33 C34 1.368(9) . ?
C34 C44 1.426(9) . ?
C34 H34 0.9500 . ?
C35 C41 1.400(10) . ?
C35 H35 0.9500 . ?
C36 C45 1.390(9) . ?
C36 H36 0.9500 . ?
C37 C44 1.348(10) . ?
C37 H37 0.9500 . ?
C38 C45 1.385(10) . ?
C38 H38 0.9500 . ?
C39 C50 1.389(9) . ?
C39 H39 0.9500 . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C52 1.373(9) . ?
C47 H47 0.9500 . ?
C48 C49 1.394(9) . ?
C48 H48 0.9500 . ?
C49 C51 1.380(10) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 C52 1.380(10) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 O1 C40 116.3(5) . . ?
C10 N3 C40 105.3(5) . . ?
C3 N1 C8 122.4(6) . . ?
C11 N2 C3 130.0(5) . . ?
C27 N4 C10 105.0(5) . . ?
C26 C1 C30 119.1(6) . . ?
C26 C1 C3 118.8(6) . . ?
C30 C1 C3 122.1(6) . . ?
C29 C2 C7 119.5(6) . . ?
C29 C2 C40 119.6(6) . . ?
C7 C2 C40 120.9(6) . . ?
N1 C3 N2 124.2(6) . . ?
N1 C3 C1 118.0(6) . . ?
N2 C3 C1 116.9(5) . . ?
C18 C4 C15 117.6(6) . . ?
C18 C4 C20 119.3(6) . . ?
C15 C4 C20 123.1(6) . . ?
C36 C5 C43 119.4(6) . . ?
C36 C5 C8 121.2(6) . . ?
C43 C5 C8 119.4(6) . . ?
C25 C6 C7 121.0(6) . . ?
C25 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C2 120.1(6) . . ?
C6 C7 H7 119.9 . . ?
C2 C7 H7 119.9 . . ?
O2 C8 N1 121.8(6) . . ?
O2 C8 C5 120.7(6) . . ?
N1 C8 C5 117.2(6) . . ?
C23 C9 C14 118.7(6) . . ?
C23 C9 C10 121.5(6) . . ?
C14 C9 C10 119.1(6) . . ?
N3 C10 N4 116.8(6) . . ?
N3 C10 C9 121.4(6) . . ?
N4 C10 C9 121.1(6) . . ?
N2 C11 O1 118.0(5) . . ?
N2 C11 C16 129.7(6) . . ?
O1 C11 C16 112.3(5) . . ?
C20 C12 C33 126.2(6) . . ?
C20 C12 C24 117.1(6) . . ?
C33 C12 C24 116.7(6) . . ?
C30 C13 C17 121.7(6) . . ?
C30 C13 H13 119.1 . . ?
C17 C13 H13 119.1 . . ?
C15 C14 C9 120.0(6) . . ?
C15 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
C14 C15 C4 121.5(6) . . ?
C14 C15 H15 119.2 . . ?
C4 C15 H15 119.2 . . ?
C22 C16 C39 118.7(6) . . ?
C22 C16 C11 122.3(6) . . ?
C39 C16 C11 119.0(6) . . ?
C19 C17 C13 116.7(6) . . ?
C19 C17 C33 119.2(6) . . ?
C13 C17 C33 123.9(6) . . ?
C23 C18 C4 120.8(6) . . ?
C23 C18 H18 119.6 . . ?
C4 C18 H18 119.6 . . ?
C26 C19 C17 121.8(6) . . ?
C26 C19 H19 119.1 . . ?
C17 C19 H19 119.1 . . ?
C41 C20 C12 120.2(6) . . ?
C41 C20 C4 115.6(6) . . ?
C12 C20 C4 124.1(6) . . ?
C35 C21 C24 120.6(6) . . ?
C35 C21 H21 119.7 . . ?
C24 C21 H21 119.7 . . ?
C16 C22 C46 121.2(6) . . ?
C16 C22 H22 119.4 . . ?
C46 C22 H22 119.4 . . ?
C18 C23 C9 120.8(6) . . ?
C18 C23 H23 119.6 . . ?
C9 C23 H23 119.6 . . ?
C37 C24 C21 119.0(6) . . ?
C37 C24 C12 120.6(6) . . ?
C21 C24 C12 120.3(6) . . ?
C6 C25 C42 118.4(6) . . ?
C6 C25 H25 120.8 . . ?
C42 C25 H25 120.8 . . ?
C1 C26 C19 120.3(6) . . ?
C1 C26 H26 119.8 . . ?
C19 C26 H26 119.8 . . ?
N4 C27 C28 122.3(6) . . ?
N4 C27 C40 109.9(5) . . ?
C28 C27 C40 127.3(6) . . ?
C48 C28 C47 118.9(6) . . ?
C48 C28 C27 119.0(6) . . ?
C47 C28 C27 122.1(6) . . ?
C2 C29 C42 119.9(6) . . ?
C2 C29 H29 120.1 . . ?
C42 C29 H29 120.1 . . ?
C13 C30 C1 120.4(6) . . ?
C13 C30 H30 119.8 . . ?
C1 C30 H30 119.8 . . ?
C50 C31 C46 119.8(6) . . ?
C50 C31 H31 120.1 . . ?
C46 C31 H31 120.1 . . ?
C43 C32 C38 119.6(6) . . ?
C43 C32 H32 120.2 . . ?
C38 C32 H32 120.2 . . ?
C34 C33 C12 119.4(6) . . ?
C34 C33 C17 114.1(6) . . ?
C12 C33 C17 126.5(6) . . ?
C33 C34 C44 122.8(6) . . ?
C33 C34 H34 118.6 . . ?
C44 C34 H34 118.6 . . ?
C21 C35 C41 119.9(6) . . ?
C21 C35 H35 120.0 . . ?
C41 C35 H35 120.0 . . ?
C5 C36 C45 120.2(6) . . ?
C5 C36 H36 119.9 . . ?
C45 C36 H36 119.9 . . ?
C44 C37 C24 121.9(6) . . ?
C44 C37 H37 119.1 . . ?
C24 C37 H37 119.1 . . ?
C45 C38 C32 120.8(6) . . ?
C45 C38 H38 119.6 . . ?
C32 C38 H38 119.6 . . ?
C50 C39 C16 119.9(6) . . ?
C50 C39 H39 120.0 . . ?
C16 C39 H39 120.0 . . ?
N3 C40 O1 108.0(5) . . ?
N3 C40 C2 112.7(5) . . ?
O1 C40 C2 105.0(5) . . ?
N3 C40 C27 102.4(5) . . ?
O1 C40 C27 116.9(5) . . ?
C2 C40 C27 112.0(5) . . ?
C35 C41 C20 121.7(6) . . ?
C35 C41 H41 119.2 . . ?
C20 C41 H41 119.2 . . ?
C25 C42 C29 121.1(6) . . ?
C25 C42 H42 119.5 . . ?
C29 C42 H42 119.5 . . ?
C32 C43 C5 120.6(6) . . ?
C32 C43 H43 119.7 . . ?
C5 C43 H43 119.7 . . ?
C37 C44 C34 118.6(6) . . ?
C37 C44 H44 120.7 . . ?
C34 C44 H44 120.7 . . ?
C36 C45 C38 119.4(6) . . ?
C36 C45 H45 120.3 . . ?
C38 C45 H45 120.3 . . ?
C22 C46 C31 120.0(6) . . ?
C22 C46 H46 120.0 . . ?
C31 C46 H46 120.0 . . ?
C52 C47 C28 119.8(6) . . ?
C52 C47 H47 120.1 . . ?
C28 C47 H47 120.1 . . ?
C28 C48 C49 120.4(6) . . ?
C28 C48 H48 119.8 . . ?
C49 C48 H48 119.8 . . ?
C51 C49 C48 119.8(6) . . ?
C51 C49 H49 120.1 . . ?
C48 C49 H49 120.1 . . ?
C31 C50 C39 120.4(6) . . ?
C31 C50 H50 119.8 . . ?
C39 C50 H50 119.8 . . ?
C52 C51 C49 120.0(6) . . ?
C52 C51 H51 120.0 . . ?
C49 C51 H51 120.0 . . ?
C47 C52 C51 121.0(6) . . ?
C47 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?

_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.097