# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is (c) The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2006

data_global
_journal_name_full               'New J.Chem.(Nouv.J.Chim.)'

_journal_coden_Cambridge         0440

_publ_contact_author_name        K.V.Radhakrishnan
_publ_contact_author_address     
;
Organic division, Chemical sciences section
RRL(CSIR)
Scientist C, Organic division
RRL (CSIR)
Trivandrum
Kerala
695019
INDIA
;

_publ_contact_author_email       RADHUPREETHI@REDIFFMAIL.COM

_publ_section_title              
;
Interplay of dual reactivity in the reaction of
pentafulvenes with 1,2,4-triazoline-3,5-diones: Experimental and
theoretical investigations
;
loop_
_publ_author_name
K.V.Radhakrishnan
S.Anas
K.S.Anju
'K.Syam Krishnan'
V.S.Sajisha
;
E.Suresh
;
'Cherumuttathu Suresh'

# Attachment 'Cif_file_final_revision_-NJC-B614533.CIF'

data_radh2m
_database_code_depnum_ccdc_archive 'CCDC 275653'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C52 H38 N6 O4, C4 H8 O2'
_chemical_formula_sum            'C56 H46 N6 O6'
_chemical_formula_weight         898.99

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           TRICLINC
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   12.2707(13)
_cell_length_b                   13.5989(15)
_cell_length_c                   15.4906(17)
_cell_angle_alpha                71.100(2)
_cell_angle_beta                 73.300(2)
_cell_angle_gamma                72.169(2)
_cell_volume                     2276.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plates
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.98.29
_exptl_absorpt_correction_T_max  0.99.31
_exptl_absorpt_process_details   BRUKER-SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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 CCD diffractometer'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13579
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0964
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         28.26
_reflns_number_total             9964
_reflns_number_gt                5156
_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    'ORTEP, MERCURY'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.1133P)^2^+0.0785P] 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         9964
_refine_ls_number_parameters     615
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1444
_refine_ls_R_factor_gt           0.0738
_refine_ls_wR_factor_ref         0.2350
_refine_ls_wR_factor_gt          0.1924
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5514(2) 0.49206(18) 0.08678(15) 0.0450(6) Uani 1 d . . .
O2 O 0.4321(2) 0.85271(18) -0.04208(16) 0.0565(7) Uani 1 d . . .
O3 O 0.4364(2) 0.34679(18) 0.56760(17) 0.0506(7) Uani 1 d . . .
O4 O 0.0597(2) 0.46514(19) 0.71534(17) 0.0569(7) Uani 1 d . . .
N1 N 0.5234(2) 0.6712(2) 0.00111(17) 0.0384(7) Uani 1 d . . .
N2 N 0.4299(2) 0.63087(19) 0.14768(17) 0.0346(6) Uani 1 d . . .
N3 N 0.3850(2) 0.74267(19) 0.10515(17) 0.0359(6) Uani 1 d . . .
N4 N 0.2829(2) 0.48259(19) 0.52004(17) 0.0334(6) Uani 1 d . . .
N5 N 0.1677(2) 0.52789(19) 0.56780(17) 0.0337(6) Uani 1 d . . .
N6 N 0.2483(2) 0.3751(2) 0.66026(18) 0.0393(7) Uani 1 d . . .
C1 C 0.5874(3) 0.7175(3) -0.1686(2) 0.0486(9) Uani 1 d . . .
H1 H 0.5126 0.7589 -0.1741 0.058 Uiso 1 calc R . .
C2 C 0.6752(4) 0.7101(3) -0.2469(2) 0.0575(11) Uani 1 d . . .
H2 H 0.6597 0.7474 -0.3057 0.069 Uiso 1 calc R . .
C3 C 0.7858(4) 0.6477(3) -0.2386(3) 0.0618(12) Uani 1 d . . .
H3 H 0.8446 0.6430 -0.2916 0.074 Uiso 1 calc R . .
C4 C 0.8089(3) 0.5927(3) -0.1523(3) 0.0593(11) Uani 1 d . . .
H4 H 0.8832 0.5499 -0.1469 0.071 Uiso 1 calc R . .
C5 C 0.7227(3) 0.6002(3) -0.0728(3) 0.0487(9) Uani 1 d . . .
H5 H 0.7391 0.5635 -0.0141 0.058 Uiso 1 calc R . .
C6 C 0.6127(3) 0.6621(3) -0.0813(2) 0.0390(8) Uani 1 d . . .
C7 C 0.4436(3) 0.7663(3) 0.0149(2) 0.0387(8) Uani 1 d . . .
C8 C 0.5072(3) 0.5856(3) 0.0787(2) 0.0344(7) Uani 1 d . . .
C9 C 0.2586(3) 0.7825(2) 0.1476(2) 0.0326(7) Uani 1 d . . .
C10 C 0.2536(3) 0.6914(2) 0.2388(2) 0.0306(7) Uani 1 d . . .
C11 C 0.3297(3) 0.5902(2) 0.2097(2) 0.0321(7) Uani 1 d . . .
H11 H 0.2905 0.5659 0.1763 0.039 Uiso 1 calc R . .
C12 C 0.3277(3) 0.5197(2) 0.3102(2) 0.0333(7) Uani 1 d . . .
H12 H 0.3662 0.4438 0.3163 0.040 Uiso 1 calc R . .
C13 C 0.3781(3) 0.5800(2) 0.35201(19) 0.0318(7) Uani 1 d . . .
H13 H 0.4636 0.5650 0.3320 0.038 Uiso 1 calc R . .
C14 C 0.3231(3) 0.6993(2) 0.3083(2) 0.0310(7) Uani 1 d . . .
H14 H 0.3825 0.7407 0.2757 0.037 Uiso 1 calc R . .
C15 C 0.1957(3) 0.5451(3) 0.3421(2) 0.0376(8) Uani 1 d . . .
H15 H 0.1524 0.4974 0.3841 0.045 Uiso 1 calc R . .
C16 C 0.1512(3) 0.6464(3) 0.3008(2) 0.0365(8) Uani 1 d . . .
H16 H 0.0726 0.6822 0.3086 0.044 Uiso 1 calc R . .
C17 C 0.2424(3) 0.7393(2) 0.3887(2) 0.0320(7) Uani 1 d . . .
H17 H 0.1937 0.8076 0.3830 0.038 Uiso 1 calc R . .
C18 C 0.2482(3) 0.6663(2) 0.4691(2) 0.0286(7) Uani 1 d . . .
C19 C 0.3417(3) 0.5671(2) 0.45896(19) 0.0307(7) Uani 1 d . . .
H19 H 0.4085 0.5648 0.4829 0.037 Uiso 1 calc R . .
C20 C 0.1595(3) 0.6458(2) 0.5599(2) 0.0325(7) Uani 1 d . . .
C21 C 0.1475(3) 0.4569(2) 0.6560(2) 0.0375(8) Uani 1 d . . .
C22 C 0.3354(3) 0.3961(2) 0.5810(2) 0.0347(7) Uani 1 d . . .
C23 C 0.1768(3) 0.7918(3) 0.0854(2) 0.0387(8) Uani 1 d . . .
C24 C 0.1110(3) 0.7187(3) 0.1015(3) 0.0529(10) Uani 1 d . . .
H24 H 0.1195 0.6574 0.1505 0.064 Uiso 1 calc R . .
C25 C 0.0326(4) 0.7348(4) 0.0464(3) 0.0690(12) Uani 1 d . . .
H25 H -0.0118 0.6853 0.0595 0.083 Uiso 1 calc R . .
C26 C 0.0204(4) 0.8239(4) -0.0274(3) 0.0713(13) Uani 1 d . . .
H26 H -0.0320 0.8348 -0.0645 0.086 Uiso 1 calc R . .
C27 C 0.0859(4) 0.8963(4) -0.0458(3) 0.0664(12) Uani 1 d . . .
H27 H 0.0785 0.9562 -0.0961 0.080 Uiso 1 calc R . .
C28 C 0.1631(3) 0.8814(3) 0.0097(2) 0.0512(9) Uani 1 d . . .
H28 H 0.2064 0.9318 -0.0036 0.061 Uiso 1 calc R . .
C29 C 0.2386(3) 0.8908(2) 0.1683(2) 0.0359(8) Uani 1 d . . .
C30 C 0.1282(3) 0.9352(3) 0.2122(2) 0.0444(9) Uani 1 d . . .
H30 H 0.0679 0.9010 0.2262 0.053 Uiso 1 calc R . .
C31 C 0.1066(4) 1.0305(3) 0.2355(3) 0.0620(11) Uani 1 d . . .
H31 H 0.0320 1.0594 0.2659 0.074 Uiso 1 calc R . .
C32 C 0.1944(5) 1.0824(3) 0.2141(3) 0.0665(12) Uani 1 d . . .
H32 H 0.1793 1.1468 0.2292 0.080 Uiso 1 calc R . .
C33 C 0.3042(4) 1.0390(3) 0.1705(3) 0.0625(11) Uani 1 d . . .
H33 H 0.3640 1.0740 0.1561 0.075 Uiso 1 calc R . .
C34 C 0.3270(3) 0.9428(3) 0.1474(2) 0.0472(9) Uani 1 d . . .
H34 H 0.4019 0.9135 0.1180 0.057 Uiso 1 calc R . .
C35 C 0.0384(3) 0.7139(2) 0.5444(2) 0.0322(7) Uani 1 d . . .
C36 C -0.0359(3) 0.6755(3) 0.5188(2) 0.0416(8) Uani 1 d . . .
H36 H -0.0147 0.6053 0.5141 0.050 Uiso 1 calc R . .
C37 C -0.1426(3) 0.7412(3) 0.5000(3) 0.0534(10) Uani 1 d . . .
H37 H -0.1928 0.7147 0.4833 0.064 Uiso 1 calc R . .
C38 C -0.1740(4) 0.8442(4) 0.5060(3) 0.0658(12) Uani 1 d . . .
H38 H -0.2457 0.8878 0.4938 0.079 Uiso 1 calc R . .
C39 C -0.0991(4) 0.8836(3) 0.5302(3) 0.0659(12) Uani 1 d . . .
H39 H -0.1200 0.9543 0.5334 0.079 Uiso 1 calc R . .
C40 C 0.0065(3) 0.8187(3) 0.5497(3) 0.0514(9) Uani 1 d . . .
H40 H 0.0564 0.8455 0.5664 0.062 Uiso 1 calc R . .
C41 C 0.1908(3) 0.6532(2) 0.6458(2) 0.0368(8) Uani 1 d . . .
C42 C 0.3053(3) 0.6391(3) 0.6508(3) 0.0514(10) Uani 1 d . . .
H42 H 0.3648 0.6336 0.5983 0.062 Uiso 1 calc R . .
C43 C 0.3321(4) 0.6331(4) 0.7335(3) 0.0679(12) Uani 1 d . . .
H43 H 0.4097 0.6223 0.7364 0.081 Uiso 1 calc R . .
C44 C 0.2448(4) 0.6429(4) 0.8116(3) 0.0733(13) Uani 1 d . . .
H44 H 0.2633 0.6388 0.8670 0.088 Uiso 1 calc R . .
C45 C 0.1316(4) 0.6587(4) 0.8071(3) 0.0660(12) Uani 1 d . . .
H45 H 0.0723 0.6667 0.8592 0.079 Uiso 1 calc R . .
C46 C 0.1044(3) 0.6627(3) 0.7255(2) 0.0506(9) Uani 1 d . . .
H46 H 0.0266 0.6721 0.7238 0.061 Uiso 1 calc R . .
C47 C 0.2698(3) 0.2908(3) 0.7435(2) 0.0423(8) Uani 1 d . . .
C48 C 0.2874(5) 0.1872(3) 0.7441(3) 0.0807(15) Uani 1 d . . .
H48 H 0.2818 0.1698 0.6925 0.097 Uiso 1 calc R . .
C49 C 0.3138(5) 0.1080(4) 0.8224(3) 0.0978(19) Uani 1 d . . .
H49 H 0.3281 0.0367 0.8225 0.117 Uiso 1 calc R . .
C50 C 0.3192(4) 0.1316(4) 0.8982(3) 0.0728(13) Uani 1 d . . .
H50 H 0.3345 0.0772 0.9511 0.087 Uiso 1 calc R . .
C51 C 0.3024(4) 0.2345(4) 0.8979(3) 0.0783(14) Uani 1 d . . .
H51 H 0.3073 0.2510 0.9502 0.094 Uiso 1 calc R . .
C52 C 0.2777(4) 0.3157(3) 0.8196(3) 0.0674(12) Uani 1 d . . .
H52 H 0.2667 0.3867 0.8190 0.081 Uiso 1 calc R . .
O5 O 0.4551(6) 0.1296(5) 0.5033(6) 0.220(3) Uani 1 d . . .
O6 O 0.6469(3) 0.0936(3) 0.4490(3) 0.0989(11) Uani 1 d . . .
C53 C 0.5862(6) 0.0786(5) 0.6114(5) 0.115(2) Uani 1 d . . .
H53A H 0.5254 0.1159 0.6523 0.172 Uiso 1 calc R . .
H53B H 0.6584 0.0972 0.6039 0.172 Uiso 1 calc R . .
H53C H 0.5953 0.0029 0.6376 0.172 Uiso 1 calc R . .
C54 C 0.5553(6) 0.1082(4) 0.5218(6) 0.102(2) Uani 1 d . . .
C55 C 0.6084(10) 0.1165(6) 0.3603(4) 0.167(4) Uani 1 d . . .
H55A H 0.5688 0.1908 0.3395 0.200 Uiso 1 calc R . .
H55B H 0.5594 0.0704 0.3644 0.200 Uiso 1 calc R . .
C56 C 0.7349(10) 0.0874(6) 0.2975(5) 0.186(4) Uani 1 d . . .
H56A H 0.7857 0.1227 0.3071 0.278 Uiso 1 calc R . .
H56B H 0.7298 0.1105 0.2330 0.278 Uiso 1 calc R . .
H56C H 0.7659 0.0115 0.3145 0.278 Uiso 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 0.0508(15) 0.0355(14) 0.0364(13) -0.0063(10) -0.0052(11) 0.0000(11)
O2 0.0676(17) 0.0377(14) 0.0360(13) 0.0031(11) 0.0089(12) -0.0049(12)
O3 0.0401(15) 0.0371(13) 0.0520(15) 0.0022(11) -0.0026(12) 0.0013(11)
O4 0.0438(15) 0.0542(16) 0.0456(15) 0.0017(12) 0.0112(13) -0.0085(12)
N1 0.0396(16) 0.0374(15) 0.0268(13) -0.0031(11) 0.0018(12) -0.0068(12)
N2 0.0369(15) 0.0280(14) 0.0273(13) -0.0018(11) -0.0004(12) -0.0028(11)
N3 0.0367(15) 0.0285(14) 0.0286(14) -0.0001(11) 0.0010(12) -0.0033(11)
N4 0.0306(15) 0.0326(14) 0.0262(13) -0.0019(11) -0.0005(11) -0.0036(11)
N5 0.0313(15) 0.0287(14) 0.0305(14) -0.0010(11) -0.0032(11) -0.0024(11)
N6 0.0419(16) 0.0317(15) 0.0308(14) 0.0031(11) -0.0035(12) -0.0055(12)
C1 0.058(2) 0.051(2) 0.0326(18) -0.0086(16) -0.0002(17) -0.0174(18)
C2 0.080(3) 0.069(3) 0.0300(19) -0.0207(18) 0.010(2) -0.039(2)
C3 0.066(3) 0.075(3) 0.050(2) -0.039(2) 0.029(2) -0.038(2)
C4 0.044(2) 0.068(3) 0.062(3) -0.030(2) 0.015(2) -0.0187(19)
C5 0.043(2) 0.052(2) 0.046(2) -0.0163(17) 0.0009(17) -0.0105(18)
C6 0.045(2) 0.0404(19) 0.0310(17) -0.0126(14) 0.0030(15) -0.0159(16)
C7 0.042(2) 0.0341(18) 0.0290(17) -0.0035(14) 0.0029(15) -0.0081(15)
C8 0.0347(18) 0.0401(19) 0.0250(15) -0.0059(13) -0.0044(14) -0.0086(15)
C9 0.0358(18) 0.0304(16) 0.0241(15) -0.0043(12) -0.0020(13) -0.0043(13)
C10 0.0340(18) 0.0311(16) 0.0239(14) -0.0053(12) -0.0047(13) -0.0071(13)
C11 0.0397(18) 0.0314(17) 0.0240(15) -0.0056(12) -0.0036(13) -0.0112(14)
C12 0.0437(19) 0.0260(16) 0.0272(15) -0.0041(12) -0.0051(14) -0.0091(13)
C13 0.0284(17) 0.0358(17) 0.0233(15) -0.0031(12) -0.0002(13) -0.0060(13)
C14 0.0343(17) 0.0256(16) 0.0276(15) 0.0003(12) -0.0034(13) -0.0100(13)
C15 0.0417(19) 0.045(2) 0.0286(16) -0.0067(14) -0.0016(15) -0.0219(16)
C16 0.0347(18) 0.048(2) 0.0272(16) -0.0088(14) -0.0028(14) -0.0156(15)
C17 0.0375(18) 0.0254(15) 0.0312(16) -0.0058(12) -0.0048(14) -0.0087(13)
C18 0.0320(17) 0.0287(16) 0.0267(15) -0.0077(12) -0.0057(13) -0.0092(13)
C19 0.0328(17) 0.0327(16) 0.0228(14) -0.0031(12) -0.0042(13) -0.0081(13)
C20 0.0340(18) 0.0314(17) 0.0245(15) -0.0008(12) -0.0039(13) -0.0060(13)
C21 0.0363(19) 0.0338(18) 0.0326(17) -0.0018(13) -0.0006(15) -0.0081(15)
C22 0.039(2) 0.0294(17) 0.0316(17) -0.0047(13) -0.0052(15) -0.0069(15)
C23 0.042(2) 0.0395(19) 0.0271(16) -0.0081(14) -0.0072(14) -0.0005(15)
C24 0.063(3) 0.055(2) 0.043(2) -0.0097(18) -0.0199(19) -0.0122(19)
C25 0.077(3) 0.080(3) 0.068(3) -0.024(2) -0.037(3) -0.019(2)
C26 0.076(3) 0.078(3) 0.062(3) -0.023(2) -0.039(2) 0.007(3)
C27 0.086(3) 0.064(3) 0.041(2) -0.0093(19) -0.030(2) 0.006(2)
C28 0.060(2) 0.051(2) 0.0349(19) -0.0046(16) -0.0121(18) -0.0063(18)
C29 0.045(2) 0.0288(17) 0.0252(15) -0.0007(12) -0.0092(14) -0.0007(14)
C30 0.046(2) 0.0353(19) 0.043(2) -0.0094(15) -0.0090(17) 0.0018(16)
C31 0.071(3) 0.051(2) 0.052(2) -0.019(2) -0.018(2) 0.013(2)
C32 0.101(4) 0.039(2) 0.063(3) -0.015(2) -0.031(3) -0.007(2)
C33 0.084(3) 0.044(2) 0.063(3) -0.011(2) -0.014(2) -0.023(2)
C34 0.061(2) 0.038(2) 0.0399(19) -0.0050(15) -0.0067(17) -0.0167(17)
C35 0.0291(17) 0.0368(18) 0.0225(15) -0.0039(12) -0.0020(13) -0.0034(14)
C36 0.038(2) 0.0419(19) 0.0350(18) -0.0055(15) -0.0031(15) -0.0047(16)
C37 0.041(2) 0.065(3) 0.048(2) -0.0067(19) -0.0126(18) -0.0077(19)
C38 0.044(2) 0.062(3) 0.068(3) -0.003(2) -0.017(2) 0.011(2)
C39 0.063(3) 0.047(2) 0.077(3) -0.016(2) -0.018(2) 0.006(2)
C40 0.046(2) 0.044(2) 0.057(2) -0.0114(18) -0.0130(19) -0.0004(17)
C41 0.041(2) 0.0380(18) 0.0268(16) -0.0039(13) -0.0095(14) -0.0052(15)
C42 0.045(2) 0.062(2) 0.044(2) -0.0202(18) -0.0100(18) -0.0011(18)
C43 0.066(3) 0.086(3) 0.060(3) -0.030(2) -0.034(2) 0.001(2)
C44 0.087(4) 0.087(3) 0.041(2) -0.024(2) -0.024(2) 0.003(3)
C45 0.067(3) 0.086(3) 0.036(2) -0.020(2) -0.006(2) -0.006(2)
C46 0.051(2) 0.059(2) 0.0351(19) -0.0112(17) -0.0055(17) -0.0084(18)
C47 0.045(2) 0.0349(19) 0.0327(18) 0.0053(14) -0.0052(16) -0.0075(15)
C48 0.153(5) 0.035(2) 0.044(2) 0.0009(18) -0.023(3) -0.019(3)
C49 0.174(6) 0.039(2) 0.059(3) 0.009(2) -0.027(3) -0.015(3)
C50 0.088(3) 0.059(3) 0.047(3) 0.020(2) -0.018(2) -0.014(2)
C51 0.110(4) 0.070(3) 0.059(3) 0.012(2) -0.043(3) -0.034(3)
C52 0.105(4) 0.051(2) 0.051(2) 0.0063(19) -0.034(2) -0.030(2)
O5 0.150(5) 0.204(6) 0.343(10) -0.110(7) -0.074(6) -0.028(5)
O6 0.086(3) 0.080(2) 0.117(3) -0.017(2) -0.017(3) -0.014(2)
C53 0.124(5) 0.124(5) 0.118(5) -0.059(4) -0.023(4) -0.031(4)
C54 0.065(4) 0.078(4) 0.158(7) -0.032(4) -0.031(4) 0.000(3)
C55 0.343(13) 0.132(6) 0.061(4) 0.008(4) -0.028(6) -0.152(8)
C56 0.344(14) 0.115(6) 0.094(6) -0.011(5) -0.036(8) -0.075(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
O1 C8 1.200(4) . ?
O2 C7 1.216(4) . ?
O3 C22 1.209(4) . ?
O4 C21 1.201(4) . ?
N1 C8 1.392(4) . ?
N1 C7 1.399(4) . ?
N1 C6 1.436(4) . ?
N2 C8 1.381(4) . ?
N2 N3 1.448(3) . ?
N2 C11 1.461(4) . ?
N3 C7 1.359(4) . ?
N3 C9 1.504(4) . ?
N4 C22 1.363(4) . ?
N4 N5 1.444(3) . ?
N4 C19 1.466(4) . ?
N5 C21 1.399(4) . ?
N5 C20 1.542(4) . ?
N6 C21 1.390(4) . ?
N6 C22 1.392(4) . ?
N6 C47 1.449(4) . ?
C1 C2 1.381(5) . ?
C1 C6 1.390(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.380(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.366(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.371(5) . ?
C5 H5 0.9300 . ?
C9 C23 1.532(4) . ?
C9 C29 1.540(4) . ?
C9 C10 1.549(4) . ?
C10 C16 1.507(4) . ?
C10 C11 1.531(4) . ?
C10 C14 1.599(4) . ?
C11 C12 1.539(4) . ?
C11 H11 0.9800 . ?
C12 C15 1.515(4) . ?
C12 C13 1.537(4) . ?
C12 H12 0.9800 . ?
C13 C19 1.552(4) . ?
C13 C14 1.558(4) . ?
C13 H13 0.9800 . ?
C14 C17 1.493(4) . ?
C14 H14 0.9800 . ?
C15 C16 1.332(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.322(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.499(4) . ?
C18 C20 1.514(4) . ?
C19 H19 0.9800 . ?
C20 C41 1.528(4) . ?
C20 C35 1.530(4) . ?
C23 C24 1.385(5) . ?
C23 C28 1.396(4) . ?
C24 C25 1.387(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.374(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.367(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.384(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C30 1.377(4) . ?
C29 C34 1.378(5) . ?
C30 C31 1.384(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.371(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.367(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.393(5) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.377(5) . ?
C35 C40 1.380(5) . ?
C36 C37 1.390(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.361(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.380(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.380(5) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.380(5) . ?
C41 C46 1.391(5) . ?
C42 C43 1.383(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.378(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.358(6) . ?
C44 H44 0.9300 . ?
C45 C46 1.377(5) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C47 C48 1.356(5) . ?
C47 C52 1.363(5) . ?
C48 C49 1.379(6) . ?
C48 H48 0.9300 . ?
C49 C50 1.338(6) . ?
C49 H49 0.9300 . ?
C50 C51 1.349(6) . ?
C50 H50 0.9300 . ?
C51 C52 1.385(5) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
O5 C54 1.268(7) . ?
O6 C54 1.362(7) . ?
O6 C55 1.488(7) . ?
C53 C54 1.442(8) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C55 C56 1.587(12) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 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
C8 N1 C7 111.4(2) . . ?
C8 N1 C6 123.6(3) . . ?
C7 N1 C6 125.0(3) . . ?
C8 N2 N3 107.9(2) . . ?
C8 N2 C11 124.5(3) . . ?
N3 N2 C11 106.6(2) . . ?
C7 N3 N2 108.4(2) . . ?
C7 N3 C9 129.9(2) . . ?
N2 N3 C9 112.4(2) . . ?
C22 N4 N5 109.2(2) . . ?
C22 N4 C19 122.7(3) . . ?
N5 N4 C19 110.7(2) . . ?
C21 N5 N4 106.4(2) . . ?
C21 N5 C20 119.6(2) . . ?
N4 N5 C20 108.7(2) . . ?
C21 N6 C22 111.2(2) . . ?
C21 N6 C47 124.4(3) . . ?
C22 N6 C47 123.2(3) . . ?
C2 C1 C6 118.9(4) . . ?
C2 C1 H1 120.6 . . ?
C6 C1 H1 120.6 . . ?
C3 C2 C1 120.4(4) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.6(4) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 119.4(4) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 120.8(3) . . ?
C5 C6 N1 119.6(3) . . ?
C1 C6 N1 119.6(3) . . ?
O2 C7 N3 127.5(3) . . ?
O2 C7 N1 126.5(3) . . ?
N3 C7 N1 106.0(3) . . ?
O1 C8 N2 126.0(3) . . ?
O1 C8 N1 128.7(3) . . ?
N2 C8 N1 105.2(3) . . ?
N3 C9 C23 112.0(2) . . ?
N3 C9 C29 111.0(2) . . ?
C23 C9 C29 110.0(2) . . ?
N3 C9 C10 96.8(2) . . ?
C23 C9 C10 115.5(3) . . ?
C29 C9 C10 110.9(2) . . ?
C16 C10 C11 98.2(2) . . ?
C16 C10 C9 129.6(3) . . ?
C11 C10 C9 105.2(2) . . ?
C16 C10 C14 105.4(2) . . ?
C11 C10 C14 101.3(2) . . ?
C9 C10 C14 112.7(2) . . ?
N2 C11 C10 100.1(2) . . ?
N2 C11 C12 125.0(3) . . ?
C10 C11 C12 94.9(2) . . ?
N2 C11 H11 111.4 . . ?
C10 C11 H11 111.4 . . ?
C12 C11 H11 111.4 . . ?
C15 C12 C13 108.8(2) . . ?
C15 C12 C11 96.0(2) . . ?
C13 C12 C11 102.3(2) . . ?
C15 C12 H12 115.8 . . ?
C13 C12 H12 115.8 . . ?
C11 C12 H12 115.8 . . ?
C12 C13 C19 118.1(2) . . ?
C12 C13 C14 102.7(2) . . ?
C19 C13 C14 104.8(2) . . ?
C12 C13 H13 110.3 . . ?
C19 C13 H13 110.3 . . ?
C14 C13 H13 110.3 . . ?
C17 C14 C13 104.7(2) . . ?
C17 C14 C10 112.1(2) . . ?
C13 C14 C10 103.0(2) . . ?
C17 C14 H14 112.1 . . ?
C13 C14 H14 112.1 . . ?
C10 C14 H14 112.1 . . ?
C16 C15 C12 109.5(3) . . ?
C16 C15 H15 125.3 . . ?
C12 C15 H15 125.3 . . ?
C15 C16 C10 106.3(3) . . ?
C15 C16 H16 126.9 . . ?
C10 C16 H16 126.9 . . ?
C18 C17 C14 112.1(3) . . ?
C18 C17 H17 123.9 . . ?
C14 C17 H17 123.9 . . ?
C17 C18 C19 112.6(3) . . ?
C17 C18 C20 132.4(3) . . ?
C19 C18 C20 111.4(2) . . ?
N4 C19 C18 102.0(2) . . ?
N4 C19 C13 120.4(3) . . ?
C18 C19 C13 104.0(2) . . ?
N4 C19 H19 109.9 . . ?
C18 C19 H19 109.9 . . ?
C13 C19 H19 109.9 . . ?
C18 C20 C41 116.2(3) . . ?
C18 C20 C35 109.1(2) . . ?
C41 C20 C35 113.6(3) . . ?
C18 C20 N5 97.3(2) . . ?
C41 C20 N5 109.3(2) . . ?
C35 C20 N5 110.0(2) . . ?
O4 C21 N6 127.3(3) . . ?
O4 C21 N5 126.5(3) . . ?
N6 C21 N5 106.2(3) . . ?
O3 C22 N4 126.7(3) . . ?
O3 C22 N6 127.4(3) . . ?
N4 C22 N6 105.8(3) . . ?
C24 C23 C28 117.1(3) . . ?
C24 C23 C9 124.1(3) . . ?
C28 C23 C9 118.7(3) . . ?
C23 C24 C25 121.6(4) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C26 C25 C24 120.1(4) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C27 C26 C25 119.5(4) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C26 C27 C28 120.7(4) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C27 C28 C23 121.0(4) . . ?
C27 C28 H28 119.5 . . ?
C23 C28 H28 119.5 . . ?
C30 C29 C34 119.1(3) . . ?
C30 C29 C9 118.1(3) . . ?
C34 C29 C9 122.8(3) . . ?
C29 C30 C31 120.4(4) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C32 C31 C30 120.4(4) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C31 119.7(4) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C32 C33 C34 120.3(4) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C29 C34 C33 120.1(4) . . ?
C29 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C36 C35 C40 119.3(3) . . ?
C36 C35 C20 121.4(3) . . ?
C40 C35 C20 119.1(3) . . ?
C35 C36 C37 120.2(3) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C38 C37 C36 120.3(4) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C39 119.8(4) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
C40 C39 C38 120.3(4) . . ?
C40 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C39 C40 C35 120.2(4) . . ?
C39 C40 H40 119.9 . . ?
C35 C40 H40 119.9 . . ?
C42 C41 C46 118.0(3) . . ?
C42 C41 C20 121.8(3) . . ?
C46 C41 C20 119.9(3) . . ?
C41 C42 C43 120.4(4) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
C44 C43 C42 120.5(4) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C45 C44 C43 119.6(4) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C44 C45 C46 120.2(4) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C45 C46 C41 121.2(4) . . ?
C45 C46 H46 119.4 . . ?
C41 C46 H46 119.4 . . ?
C48 C47 C52 120.1(3) . . ?
C48 C47 N6 120.0(3) . . ?
C52 C47 N6 119.8(3) . . ?
C47 C48 C49 119.1(4) . . ?
C47 C48 H48 120.5 . . ?
C49 C48 H48 120.5 . . ?
C50 C49 C48 121.3(4) . . ?
C50 C49 H49 119.4 . . ?
C48 C49 H49 119.4 . . ?
C49 C50 C51 119.9(4) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C50 C51 C52 120.0(4) . . ?
C50 C51 H51 120.0 . . ?
C52 C51 H51 120.0 . . ?
C47 C52 C51 119.5(4) . . ?
C47 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
C54 O6 C55 112.5(6) . . ?
C54 C53 H53A 109.5 . . ?
C54 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C54 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O5 C54 O6 114.8(8) . . ?
O5 C54 C53 128.9(8) . . ?
O6 C54 C53 115.3(5) . . ?
O6 C55 C56 96.8(7) . . ?
O6 C55 H55A 112.4 . . ?
C56 C55 H55A 112.4 . . ?
O6 C55 H55B 112.4 . . ?
C56 C55 H55B 112.4 . . ?
H55A C55 H55B 109.9 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.883
_diffrn_reflns_theta_full        28.26
_diffrn_measured_fraction_theta_full 0.883
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.064