# Electronic Supplementary Material (ESI) for Faraday Discussions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_PERE37
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_Int_Tables_number      4
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,-z
_cell_length_a                   14.4962(5)
_cell_length_b                   5.1115(3)
_cell_length_c                   23.0047(8)
_cell_angle_alpha                90
_cell_angle_beta                 104.217(2)
_cell_angle_gamma                90
_cell_volume                     1652.38
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
O1 O 0.9344(2) 0.6597(12) 0.19987(13)
O2 O 1.1430(2) 0.6197(9) 0.08167(11)
O3 O 1.17423(18) -0.3907(10) 0.37418(11)
O4 O 1.38876(18) -0.4037(9) 0.26030(11)
N1 N 1.0363(2) 0.6337(12) 0.13910(13)
N2 N 1.2819(2) -0.3856(12) 0.31728(13)
H2 H 1.3119 -0.5161 0.3389
C1 C 1.0031(3) 0.5573(16) 0.18870(16)
C2 C 1.1180(3) 0.5347(13) 0.12451(15)
C3 C 1.1707(3) 0.3278(13) 0.16345(15)
C4 C 1.2513(3) 0.2188(12) 0.15147(16)
H4 H 1.2734 0.2809 0.1184
C5 C 1.3007(3) 0.0190(13) 0.18721(16)
H5 H 1.3570 -0.0498 0.1788
C6 C 1.2692(3) -0.0799(13) 0.23457(15)
C7 C 1.3189(3) -0.2972(13) 0.27096(15)
C8 C 1.2021(3) -0.2891(14) 0.33314(15)
C9 C 1.1524(3) -0.0663(14) 0.29729(16)
C10 C 1.0726(3) 0.0433(16) 0.30963(16)
H10 H 1.0500 -0.0200 0.3424
C11 C 1.0241(3) 0.2485(16) 0.27405(16)
H11 H 0.9695 0.3242 0.2832
C12 C 1.0555(3) 0.3397(15) 0.22608(16)
C13 C 1.1374(3) 0.2309(14) 0.21271(15)
C14 C 1.1861(3) 0.0292(13) 0.24815(15)
C15 C 0.9811(3) 0.8367(16) 0.09885(17)
H15A H 1.0236 0.9630 0.0857
H15B H 0.9378 0.9326 0.1186
C16A C 0.9184(9) 0.652(3) 0.0398(5)
H16A H 0.8852 0.7739 0.0080
H16B H 0.9649 0.5527 0.0234
C17A C 0.8453(6) 0.460(3) 0.0517(4)
H17A H 0.8770 0.3430 0.0850
H17B H 0.8227 0.3497 0.0156
C18A C 0.7591(5) 0.584(2) 0.0677(3)
H18A H 0.7813 0.7268 0.0969
H18B H 0.7277 0.4511 0.0875
C19A C 0.6857(5) 0.695(2) 0.0137(3)
H19A H 0.7188 0.8060 -0.0101
H19B H 0.6407 0.8083 0.0283
C20A C 0.6295(6) 0.482(2) -0.0269(4)
H20A H 0.6040 0.3573 -0.0018
H20B H 0.6737 0.3840 -0.0456
C21A C 0.5465(6) 0.585(3) -0.0768(4)
H21A H 0.5715 0.6955 -0.1049
H21B H 0.5039 0.6938 -0.0591
C22A C 0.4880(10) 0.342(4) -0.1125(6)
H22A H 0.4657 0.2298 -0.0843
H22B H 0.5294 0.2415 -0.1320
H22C H 0.4332 0.4081 -0.1429
O1 O 0.0656(2) 1.1597(12) 0.80013(13)
O2 O -0.1430(2) 1.1197(9) 0.91833(11)
O3 O -0.17423(18) 0.1093(10) 0.62582(11)
O4 O -0.38876(18) 0.0963(9) 0.73970(11)
N1 N -0.0363(2) 1.1337(12) 0.86090(13)
N2 N -0.2819(2) 0.1144(12) 0.68272(13)
H2 H -0.3119 -0.0161 0.6611
C1 C -0.0031(3) 1.0573(16) 0.81130(16)
C2 C -0.1180(3) 1.0347(13) 0.87549(15)
C3 C -0.1707(3) 0.8278(13) 0.83655(15)
C4 C -0.2513(3) 0.7188(12) 0.84853(16)
H4 H -0.2734 0.7809 0.8816
C5 C -0.3007(3) 0.5190(13) 0.81279(16)
H5 H -0.3570 0.4502 0.8212
C6 C -0.2692(3) 0.4201(13) 0.76543(15)
C7 C -0.3189(3) 0.2028(13) 0.72904(15)
C8 C -0.2021(3) 0.2109(14) 0.66686(15)
C9 C -0.1524(3) 0.4337(14) 0.70271(16)
C10 C -0.0726(3) 0.5433(16) 0.69037(16)
H10 H -0.0500 0.4800 0.6576
C11 C -0.0241(3) 0.7485(16) 0.72595(16)
H11 H 0.0305 0.8242 0.7168
C12 C -0.0555(3) 0.8397(15) 0.77392(16)
C13 C -0.1374(3) 0.7309(14) 0.78729(15)
C14 C -0.1861(3) 0.5292(13) 0.75185(15)
C15 C 0.0189(3) 1.3367(16) 0.90115(17)
H15A H -0.0236 1.4630 0.9143
H15B H 0.0622 1.4326 0.8814
C16A C 0.0816(9) 1.152(3) 0.9602(5)
H16A H 0.1148 1.2739 0.9920
H16B H 0.0351 1.0527 0.9766
C17A C 0.1547(6) 0.960(3) 0.9483(4)
H17A H 0.1230 0.8430 0.9150
H17B H 0.1773 0.8497 0.9844
C18A C 0.2409(5) 1.084(2) 0.9323(3)
H18A H 0.2187 1.2268 0.9031
H18B H 0.2723 0.9511 0.9125
C19A C 0.3143(5) 1.195(2) 0.9863(3)
H19A H 0.2812 1.3060 1.0101
H19B H 0.3593 1.3083 0.9717
C20A C 0.3705(6) 0.982(2) 1.0269(4)
H20A H 0.3960 0.8573 1.0018
H20B H 0.3263 0.8840 1.0456
C21A C 0.4535(6) 1.085(3) 1.0768(4)
H21A H 0.4285 1.1955 1.1049
H21B H 0.4961 1.1938 1.0591
C22A C 0.5120(10) 0.842(4) 1.1125(6)
H22A H 0.5343 0.7298 1.0843
H22B H 0.4706 0.7415 1.1320
H22C H 0.5668 0.9081 1.1429
N31 N 0.5059(2) 0.6605(11) 0.67297(13)
H31 H 0.5231 0.7969 0.6965
N32 N 0.6272(2) 0.6841(11) 0.61897(13)
N33 N 0.7286(2) 0.6410(12) 0.55124(13)
H33 H 0.7655 0.7772 0.5632
C31 C 0.5510(3) 0.5724(14) 0.63145(15)
C32 C 0.6555(2) 0.5601(14) 0.57485(15)
C33 C 0.7345(3) 0.4707(14) 0.50502(15)
C34 C 0.6679(3) 0.2812(15) 0.49996(15)
H34 H 0.6578 0.1404 0.4722
C35 C 0.6148(3) 0.3308(14) 0.54429(15)
C36 C 0.5356(3) 0.2176(15) 0.55892(15)
H36 H 0.5061 0.0639 0.5397
C37 C 0.5026(3) 0.3456(14) 0.60385(16)
C38 C 0.4242(3) 0.3067(15) 0.63115(16)
H38 H 0.3783 0.1706 0.6220
C39 C 0.4276(3) 0.4989(14) 0.67221(16)
C40 C 0.8055(3) 0.5101(14) 0.46968(16)
C41 C 0.8064(3) 0.3399(16) 0.42194(17)
H41 H 0.7602 0.2046 0.4121
C42 C 0.8740(3) 0.3673(17) 0.38901(18)
H42 H 0.8738 0.2510 0.3568
C43 C 0.9415(3) 0.5623(16) 0.40274(17)
H43 H 0.9889 0.5770 0.3808
C44 C 0.9401(3) 0.7368(16) 0.44858(19)
H44 H 0.9855 0.8744 0.4574
C45 C 0.8724(3) 0.7104(15) 0.48160(18)
H45 H 0.8717 0.8312 0.5129
C46 C 0.3642(3) 0.5535(16) 0.71178(17)
C47 C 0.2858(3) 0.3913(16) 0.70900(19)
H47 H 0.2744 0.2492 0.6815
C48 C 0.2242(3) 0.4339(17) 0.7456(2)
H48 H 0.1712 0.3215 0.7432
C49 C 0.2404(3) 0.6424(17) 0.78578(18)
H49 H 0.1988 0.6726 0.8112
C50 C 0.3169(3) 0.8038(18) 0.78851(19)
H50 H 0.3276 0.9469 0.8157
C51 C 0.3792(3) 0.7607(16) 0.75187(18)
H51 H 0.4321 0.8737 0.7544
N31 N 0.4941(2) 0.1605(11) 0.32703(13)
H31 H 0.4769 0.2969 0.3035
N32 N 0.3728(2) 0.1841(11) 0.38103(13)
N33 N 0.2714(2) 0.1410(12) 0.44876(13)
H33 H 0.2345 0.2772 0.4368
C31 C 0.4490(3) 0.0724(14) 0.36855(15)
C32 C 0.3445(2) 0.0601(14) 0.42515(15)
C33 C 0.2655(3) -0.0293(14) 0.49498(15)
C34 C 0.3321(3) -0.2188(15) 0.50004(15)
H34 H 0.3422 -0.3596 0.5278
C35 C 0.3852(3) -0.1692(14) 0.45571(15)
C36 C 0.4644(3) -0.2824(15) 0.44108(15)
H36 H 0.4939 -0.4361 0.4603
C37 C 0.4974(3) -0.1544(14) 0.39615(16)
C38 C 0.5758(3) -0.1933(15) 0.36885(16)
H38 H 0.6217 -0.3294 0.3780
C39 C 0.5724(3) -0.0011(14) 0.32779(16)
C40 C 0.1945(3) 0.0101(14) 0.53032(16)
C41 C 0.1936(3) -0.1601(16) 0.57806(17)
H41 H 0.2398 -0.2954 0.5879
C42 C 0.1260(3) -0.1327(17) 0.61099(18)
H42 H 0.1262 -0.2490 0.6432
C43 C 0.0585(3) 0.0623(16) 0.59726(17)
H43 H 0.0111 0.0770 0.6192
C44 C 0.0599(3) 0.2368(16) 0.55142(19)
H44 H 0.0145 0.3744 0.5426
C45 C 0.1276(3) 0.2104(15) 0.51840(18)
H45 H 0.1283 0.3312 0.4871
C46 C 0.6358(3) 0.0535(16) 0.28822(17)
C47 C 0.7142(3) -0.1087(16) 0.29100(19)
H47 H 0.7256 -0.2508 0.3185
C48 C 0.7758(3) -0.0661(17) 0.2544(2)
H48 H 0.8288 -0.1785 0.2568
C49 C 0.7596(3) 0.1424(17) 0.21422(18)
H49 H 0.8012 0.1726 0.1888
C50 C 0.6831(3) 0.3038(18) 0.21149(19)
H50 H 0.6724 0.4469 0.1843
C51 C 0.6208(3) 0.2607(16) 0.24813(18)
H51 H 0.5679 0.3737 0.2456
H15C H 0.9516 0.9506 1.1241
H15D H 1.0277 0.9459 1.0849
C16B C 0.9088(8) 0.772(3) 1.0477(6)
H16C H 0.9368 0.6783 1.0184
H16D H 0.8781 0.9333 1.0285
C17B C 0.8341(6) 0.597(3) 1.0657(4)
H17C H 0.8662 0.4468 1.0894
H17D H 0.8010 0.6983 1.0912
C18B C 0.7612(5) 0.496(2) 1.0104(3)
H18C H 0.7250 0.6465 0.9890
H18D H 0.7952 0.4122 0.9830
C19B C 0.6917(5) 0.300(2) 1.0261(3)
H19C H 0.7285 0.1628 1.0521
H19D H 0.6524 0.3914 1.0494
C20B C 0.6259(5) 0.170(2) 0.9719(3)
H20C H 0.5899 0.0291 0.9862
H20D H 0.6650 0.0874 0.9472
C21B C 0.5547(6) 0.360(3) 0.9323(3)
H21C H 0.5897 0.4948 0.9153
H21D H 0.5169 0.4500 0.9568
C22B C 0.4864(14) 0.204(4) 0.8800(8)
H22D H 0.4501 0.0755 0.8971
H22E H 0.5242 0.1124 0.8564
H22F H 0.4424 0.3252 0.8542
H15C H 0.0484 1.4506 -0.1241
H15D H -0.0277 1.4459 -0.0849
C16B C 0.0912(8) 1.272(3) -0.0477(6)
H16C H 0.0632 1.1783 -0.0184
H16D H 0.1219 1.4333 -0.0285
C17B C 0.1659(6) 1.097(3) -0.0657(4)
H17C H 0.1338 0.9468 -0.0894
H17D H 0.1990 1.1983 -0.0912
C18B C 0.2388(5) 0.996(2) -0.0104(3)
H18C H 0.2750 1.1465 0.0110
H18D H 0.2048 0.9122 0.0170
C19B C 0.3083(5) 0.800(2) -0.0261(3)
H19C H 0.2715 0.6628 -0.0521
H19D H 0.3476 0.8914 -0.0494
C20B C 0.3741(5) 0.670(2) 0.0281(3)
H20C H 0.4101 0.5291 0.0138
H20D H 0.3350 0.5874 0.0528
C21B C 0.4453(6) 0.860(3) 0.0677(3)
H21C H 0.4103 0.9948 0.0847
H21D H 0.4831 0.9500 0.0432
C22B C 0.5136(14) 0.704(4) 0.1200(8)
H22D H 0.5499 0.5755 0.1029
H22E H 0.4758 0.6124 0.1436
H22F H 0.5576 0.8252 0.1458

#END
_database_code_depnum_ccdc_archive 'CCDC 990641'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_PERE34
_vrf_PLAT088_PERE34              
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.07    
RESPONSE: All the molecule C21H15N3 is disordered over 2 sites. 
Each model were refined anisotropically with SIMU restraints. 
To help to keep good geometry, SAME restraint was used.
A limit on data / parameter ratio's that
properly takes into account these number of restraints  
would be more appropriate.
;
_vrf_PLAT220_PERE34              
;
PROBLEM:Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        4.9 Ratio
RESPONSE: Disorder, see above.
;

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H30 N6, C14 H6 N2 O4'
_chemical_formula_sum            'C56 H36 N8 O4'
_chemical_formula_weight         884.93
_chemical_compound_source        'Synthesized by the authors. See text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_symmetry_space_group_name_H-M   P21/n
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   18.8301(4)
_cell_length_b                   5.1118(1)
_cell_length_c                   21.2931(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.929(1)
_cell_angle_gamma                90
_cell_volume                     2048.42(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    7257
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      70.45

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.748
_shelx_estimated_absorpt_T_min   0.865
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_Type   multi-scan
_exptl_absorpt_correction_T_min  0.6004
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'

_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker smart diffractometer equiped with an APEX II CCD Detector,
a Incoatec IMuS source and a Quazar MX mirror. The crystal-to-detector distance 
5.0 cm, and the data collection was carried out in 512 x 512 pixel mode.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 180.0 degree
scan in 180 frames over three different parts of the reciprocal space


;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\muS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            26966
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.082
_diffrn_reflns_theta_max         70.761
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             3838
_reflns_number_gt                3036
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2010 )'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2010)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL  (Bruker AXS, 2003)'
_computing_publication_material  'UdMX (Maris, 2004)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0898P)²+0.1985P]
 where P=(Fo²+2Fc²)/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         3838
_refine_ls_number_parameters     543
_refine_ls_number_restraints     158
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1321
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.049

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.64724(6) 0.5892(2) 0.04913(5) 0.0336(3) Uani 1 1 d . . . . .
O2 O 0.44570(6) 0.4599(2) 0.15493(5) 0.0348(3) Uani 1 1 d . . . . .
N1 N 0.54709(7) 0.5117(2) 0.10226(6) 0.0269(3) Uani 1 1 d . . . . .
H1 H 0.5590(9) 0.653(4) 0.1284(9) 0.034(5) Uiso 1 1 d . . . . .
C1 C 0.59349(8) 0.4585(3) 0.05509(7) 0.0263(3) Uani 1 1 d . . . . .
C2 C 0.48412(8) 0.3854(3) 0.11331(6) 0.0269(3) Uani 1 1 d . . . . .
C3 C 0.46498(7) 0.1638(3) 0.07102(6) 0.0232(3) Uani 1 1 d . . . . .
C4 C 0.50984(7) 0.1017(3) 0.02094(6) 0.0214(3) Uani 1 1 d . . . . .
C5 C 0.57349(7) 0.2417(3) 0.01173(6) 0.0234(3) Uani 1 1 d . . . . .
C6 C 0.61594(7) 0.1796(3) -0.03784(7) 0.0273(3) Uani 1 1 d . . . . .
H6 H 0.6586 0.2743 -0.0438 0.033 Uiso 1 1 calc R U . . .
C7 C 0.59630(7) -0.0230(3) -0.07950(7) 0.0270(3) Uani 1 1 d . . . . .
H7 H 0.6255 -0.0630 -0.1137 0.032 Uiso 1 1 calc R U . . .
N11 N 0.7046(4) 0.018(2) 0.1292(6) 0.0235(16) Uani 0.5 1 d D U P A 1
H11 H 0.706(2) -0.130(9) 0.103(2) 0.026(10) Uiso 0.5 1 d . . P B 1
N12 N 0.5914(6) -0.066(2) 0.1730(5) 0.0243(16) Uani 0.5 1 d D U P A 1
N13 N 0.4843(3) -0.0617(11) 0.2298(2) 0.0276(11) Uani 0.5 1 d D U P A 1
H13 H 0.465(3) -0.219(11) 0.203(2) 0.055(14) Uiso 0.5 1 d . . P C 1
C11 C 0.6506(5) 0.069(2) 0.1686(5) 0.0159(15) Uani 0.5 1 d D U P A 1
C12 C 0.5495(5) 0.0351(17) 0.2159(3) 0.0217(14) Uani 0.5 1 d D U P A 1
C13 C 0.4535(2) 0.0932(8) 0.2753(2) 0.0279(9) Uani 0.5 1 d D U P A 1
C14 C 0.5003(3) 0.2904(11) 0.2919(2) 0.0267(10) Uani 0.5 1 d D U P A 1
H14 H 0.4932 0.4231 0.3223 0.032 Uiso 0.5 1 calc R U P A 1
C15 C 0.5620(5) 0.2577(18) 0.2546(3) 0.0259(16) Uani 0.5 1 d D U P A 1
C16 C 0.6250(6) 0.394(3) 0.2487(6) 0.0223(16) Uani 0.5 1 d D U P A 1
H16 H 0.6367 0.5417 0.2741 0.027 Uiso 0.5 1 calc R U P A 1
C17 C 0.6702(7) 0.301(3) 0.2030(6) 0.0218(18) Uani 0.5 1 d D U P A 1
C18 C 0.7387(7) 0.377(3) 0.1825(7) 0.0234(15) Uani 0.5 1 d D U P A 1
H18 H 0.7657 0.5217 0.1979 0.028 Uiso 0.5 1 calc R U P A 1
C19 C 0.7587(4) 0.205(2) 0.1367(5) 0.0244(16) Uani 0.5 1 d D U P A 1
C20 C 0.8242(2) 0.1868(9) 0.1017(2) 0.0257(10) Uani 0.5 1 d D U P A 1
C21 C 0.8784(2) 0.3673(9) 0.1139(2) 0.0310(9) Uani 0.5 1 d D U P A 1
H21 H 0.8722 0.5010 0.1443 0.037 Uiso 0.5 1 calc R U P A 1
C22 C 0.9412(2) 0.3527(7) 0.08210(17) 0.0376(7) Uani 0.5 1 d D . P A 1
H22 H 0.9779 0.4756 0.0911 0.045 Uiso 0.5 1 calc R U P A 1
C23 C 0.95097(18) 0.1603(7) 0.03711(16) 0.0364(7) Uani 0.5 1 d D . P A 1
H23 H 0.9939 0.1526 0.0150 0.044 Uiso 0.5 1 calc R U P A 1
C24 C 0.8970(2) -0.0212(7) 0.02485(16) 0.0370(7) Uani 0.5 1 d D . P A 1
H24 H 0.9033 -0.1541 -0.0056 0.044 Uiso 0.5 1 calc R U P A 1
C25 C 0.8345(2) -0.0087(7) 0.05680(16) 0.0325(7) Uani 0.5 1 d D U P A 1
H25 H 0.7982 -0.1339 0.0483 0.039 Uiso 0.5 1 calc R U P A 1
C26 C 0.38179(16) 0.0352(6) 0.29656(18) 0.0304(6) Uani 0.5 1 d D . P A 1
C27 C 0.3520(2) 0.1889(9) 0.3421(2) 0.0619(13) Uani 0.5 1 d D . P A 1
H27 H 0.3790 0.3271 0.3608 0.074 Uiso 0.5 1 calc R U P A 1
C28 C 0.2829(3) 0.1439(10) 0.3608(3) 0.0779(17) Uani 0.5 1 d D . P A 1
H28 H 0.2636 0.2503 0.3925 0.094 Uiso 0.5 1 calc R U P A 1
C29 C 0.24256(19) -0.0518(8) 0.3340(2) 0.0524(10) Uani 0.5 1 d D . P A 1
H29 H 0.1952 -0.0796 0.3465 0.063 Uiso 0.5 1 calc R U P A 1
C30 C 0.2711(2) -0.2068(9) 0.28909(19) 0.0521(10) Uani 0.5 1 d D . P A 1
H30 H 0.2436 -0.3437 0.2705 0.063 Uiso 0.5 1 calc R U P A 1
C31 C 0.34066(19) -0.1652(8) 0.2703(2) 0.0455(8) Uani 0.5 1 d D . P A 1
H31 H 0.3600 -0.2752 0.2393 0.055 Uiso 0.5 1 calc R U P A 1
N41 N 0.6840(4) 0.027(2) 0.1347(6) 0.026(2) Uani 0.5 1 d D U P D 2
H41 H 0.678(2) -0.097(9) 0.108(2) 0.022(10) Uiso 0.5 1 d . . P E 2
N42 N 0.5781(5) -0.063(2) 0.1872(5) 0.0233(16) Uani 0.5 1 d D U P D 2
N43 N 0.4777(3) -0.0891(10) 0.2526(2) 0.0279(10) Uani 0.5 1 d D U P D 2
H43 H 0.4616(18) -0.233(7) 0.2361(19) 0.016(8) Uiso 0.5 1 d . . P F 2
C41 C 0.6360(6) 0.081(3) 0.1811(6) 0.029(2) Uani 0.5 1 d D U P D 2
C42 C 0.5389(5) 0.0232(17) 0.2341(3) 0.0224(15) Uani 0.5 1 d D U P D 2
C43 C 0.4521(2) 0.0534(8) 0.3030(2) 0.0313(9) Uani 0.5 1 d D U P D 2
C44 C 0.4969(4) 0.2600(11) 0.3153(2) 0.0322(12) Uani 0.5 1 d D U P D 2
H44 H 0.4911 0.3892 0.3468 0.039 Uiso 0.5 1 calc R U P D 2
C45 C 0.5536(5) 0.2475(17) 0.2727(3) 0.0271(16) Uani 0.5 1 d D U P D 2
C46 C 0.6152(7) 0.391(3) 0.2626(7) 0.035(2) Uani 0.5 1 d D U P D 2
H46 H 0.6261 0.5446 0.2862 0.042 Uiso 0.5 1 calc R U P D 2
C47 C 0.6600(7) 0.302(3) 0.2164(6) 0.030(2) Uani 0.5 1 d D U P D 2
C48 C 0.7243(8) 0.380(3) 0.1878(8) 0.037(3) Uani 0.5 1 d D U P D 2
H48 H 0.7530 0.5253 0.2001 0.044 Uiso 0.5 1 calc R U P D 2
C49 C 0.7380(4) 0.209(3) 0.1395(6) 0.0307(19) Uani 0.5 1 d D U P D 2
C50 C 0.7961(3) 0.2147(9) 0.0953(3) 0.0307(11) Uani 0.5 1 d D U P D 2
C51 C 0.8504(3) 0.3971(12) 0.1016(2) 0.0469(13) Uani 0.5 1 d D U P D 2
H51 H 0.8499 0.5173 0.1356 0.056 Uiso 0.5 1 calc R U P D 2
C52 C 0.9053(2) 0.4100(9) 0.0601(2) 0.0521(11) Uani 0.5 1 d D . P D 2
H52 H 0.9417 0.5371 0.0658 0.062 Uiso 0.5 1 calc R U P D 2
C53 C 0.9067(2) 0.2375(8) 0.0105(2) 0.0522(10) Uani 0.5 1 d D . P D 2
H53 H 0.9439 0.2456 -0.0185 0.063 Uiso 0.5 1 calc R U P D 2
C54 C 0.8535(2) 0.0525(8) 0.0032(2) 0.0569(11) Uani 0.5 1 d D . P D 2
H54 H 0.8547 -0.0682 -0.0307 0.068 Uiso 0.5 1 calc R U P D 2
C55 C 0.7987(2) 0.0411(8) 0.0446(2) 0.0470(10) Uani 0.5 1 d D U P D 2
H55 H 0.7623 -0.0861 0.0385 0.056 Uiso 0.5 1 calc R U P D 2
C56 C 0.38813(17) -0.0221(6) 0.33556(17) 0.0313(6) Uani 0.5 1 d D . P D 2
C57 C 0.3706(2) 0.1062(8) 0.39111(17) 0.0428(8) Uani 0.5 1 d D . P D 2
H57 H 0.3999 0.2453 0.4063 0.051 Uiso 0.5 1 calc R U P D 2
C58 C 0.3118(2) 0.0357(7) 0.42437(17) 0.0437(8) Uani 0.5 1 d D . P D 2
H58 H 0.3014 0.1249 0.4621 0.052 Uiso 0.5 1 calc R U P D 2
C59 C 0.26843(19) -0.1627(8) 0.40294(18) 0.0459(8) Uani 0.5 1 d D . P D 2
H59 H 0.2279 -0.2115 0.4256 0.055 Uiso 0.5 1 calc R U P D 2
C60 C 0.2842(2) -0.2912(9) 0.3480(2) 0.0572(11) Uani 0.5 1 d D . P D 2
H60 H 0.2539 -0.4271 0.3327 0.069 Uiso 0.5 1 calc R U P D 2
C61 C 0.34407(19) -0.2238(8) 0.3149(2) 0.0459(9) Uani 0.5 1 d D . P D 2
H61 H 0.3548 -0.3169 0.2778 0.055 Uiso 0.5 1 calc R U P D 2


_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_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 . . 1.2230(18) y
O2 C2 . . 1.2236(19) y
N1 C2 . . 1.377(2) y
N1 C1 . . 1.380(2) y
N1 H1 . . 0.94(2) ?
C1 C5 . . 1.4831(19) y
C2 C3 . . 1.4839(19) y
C3 C7 . 3_655 1.377(2) y
C3 C4 . . 1.4185(19) y
C4 C4 . 3_655 1.411(3) y
C4 C5 . . 1.4152(19) y
C5 C6 . . 1.382(2) y
C6 C7 . . 1.405(2) y
C6 H6 . . 0.9500 ?
C7 C3 . 3_655 1.377(2) y
C7 H7 . . 0.9500 ?
N11 C11 . . 1.366(7) y
N11 C19 . . 1.403(9) y
N11 H11 . . 0.94(5) ?
N12 C11 . . 1.318(9) y
N12 C12 . . 1.333(7) y
N13 C12 . . 1.365(8) y
N13 C13 . . 1.391(6) y
N13 H13 . . 1.04(5) ?
C11 C17 . . 1.434(9) y
C12 C15 . . 1.421(9) y
C13 C14 . . 1.377(6) y
C13 C26 . . 1.469(5) y
C14 C15 . . 1.438(7) y
C14 H14 . . 0.9500 ?
C15 C16 . . 1.385(9) y
C16 C17 . . 1.398(9) y
C16 H16 . . 0.9500 ?
C17 C18 . . 1.429(10) y
C18 C19 . . 1.376(9) y
C18 H18 . . 0.9500 ?
C19 C20 . . 1.465(7) y
C20 C21 . . 1.394(6) y
C20 C25 . . 1.401(5) y
C21 C22 . . 1.384(6) y
C21 H21 . . 0.9500 ?
C22 C23 . . 1.390(5) y
C22 H22 . . 0.9500 ?
C23 C24 . . 1.394(5) y
C23 H23 . . 0.9500 ?
C24 C25 . . 1.381(5) y
C24 H24 . . 0.9500 ?
C25 H25 . . 0.9500 ?
C26 C27 . . 1.381(5) y
C26 C31 . . 1.390(5) y
C27 C28 . . 1.392(5) y
C27 H27 . . 0.9500 ?
C28 C29 . . 1.369(6) y
C28 H28 . . 0.9500 ?
C29 C30 . . 1.366(6) y
C29 H29 . . 0.9500 ?
C30 C31 . . 1.397(5) y
C30 H30 . . 0.9500 ?
C31 H31 . . 0.9500 ?
N41 C49 . . 1.379(9) y
N41 C41 . . 1.389(9) y
N41 H41 . . 0.86(5) ?
N42 C41 . . 1.323(10) y
N42 C42 . . 1.337(7) y
N43 C42 . . 1.358(8) y
N43 C43 . . 1.395(6) y
N43 H43 . . 0.86(4) ?
C41 C47 . . 1.423(10) y
C42 C45 . . 1.432(9) y
C43 C44 . . 1.371(6) y
C43 C56 . . 1.462(5) y
C44 C45 . . 1.426(8) y
C44 H44 . . 0.9500 ?
C45 C46 . . 1.396(10) y
C46 C47 . . 1.393(9) y
C46 H46 . . 0.9500 ?
C47 C48 . . 1.432(10) y
C48 C49 . . 1.379(10) y
C48 H48 . . 0.9500 ?
C49 C50 . . 1.467(8) y
C50 C51 . . 1.387(7) y
C50 C55 . . 1.400(6) y
C51 C52 . . 1.383(7) y
C51 H51 . . 0.9500 ?
C52 C53 . . 1.377(6) y
C52 H52 . . 0.9500 ?
C53 C54 . . 1.382(5) y
C53 H53 . . 0.9500 ?
C54 C55 . . 1.382(5) y
C54 H54 . . 0.9500 ?
C55 H55 . . 0.9500 ?
C56 C61 . . 1.386(5) y
C56 C57 . . 1.402(5) y
C57 C58 . . 1.382(5) y
C57 H57 . . 0.9500 ?
C58 C59 . . 1.371(5) y
C58 H58 . . 0.9500 ?
C59 C60 . . 1.382(5) y
C59 H59 . . 0.9500 ?
C60 C61 . . 1.393(5) y
C60 H60 . . 0.9500 ?
C61 H61 . . 0.9500 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 N1 C1 . . . 126.99(12) y
C2 N1 H1 . . . 116.9(11) ?
C1 N1 H1 . . . 116.1(11) ?
O1 C1 N1 . . . 120.95(14) y
O1 C1 C5 . . . 122.50(14) y
N1 C1 C5 . . . 116.53(12) y
O2 C2 N1 . . . 120.75(14) y
O2 C2 C3 . . . 122.66(14) y
N1 C2 C3 . . . 116.56(12) y
C7 C3 C4 3_655 . . 120.29(13) y
C7 C3 C2 3_655 . . 120.46(13) y
C4 C3 C2 . . . 119.24(13) y
C4 C4 C5 3_655 . . 119.38(16) y
C4 C4 C3 3_655 . . 119.32(16) y
C5 C4 C3 . . . 121.30(13) y
C6 C5 C4 . . . 120.26(13) y
C6 C5 C1 . . . 120.39(13) y
C4 C5 C1 . . . 119.34(13) y
C5 C6 C7 . . . 120.32(13) y
C5 C6 H6 . . . 119.8 ?
C7 C6 H6 . . . 119.8 ?
C3 C7 C6 3_655 . . 120.42(13) y
C3 C7 H7 3_655 . . 119.8 ?
C6 C7 H7 . . . 119.8 ?
C11 N11 C19 . . . 110.5(8) y
C11 N11 H11 . . . 124(3) ?
C19 N11 H11 . . . 126(3) ?
C11 N12 C12 . . . 111.4(8) y
C12 N13 C13 . . . 110.1(5) y
C12 N13 H13 . . . 117(3) ?
C13 N13 H13 . . . 133(3) ?
N12 C11 N11 . . . 126.1(7) y
N12 C11 C17 . . . 127.1(8) y
N11 C11 C17 . . . 106.9(7) y
N12 C12 N13 . . . 124.5(7) y
N12 C12 C15 . . . 128.2(8) y
N13 C12 C15 . . . 107.3(6) y
C14 C13 N13 . . . 108.5(4) y
C14 C13 C26 . . . 131.0(4) y
N13 C13 C26 . . . 120.5(4) y
C13 C14 C15 . . . 107.2(5) y
C13 C14 H14 . . . 126.4 ?
C15 C14 H14 . . . 126.4 ?
C16 C15 C12 . . . 118.5(7) y
C16 C15 C14 . . . 134.6(8) y
C12 C15 C14 . . . 107.0(6) y
C15 C16 C17 . . . 115.8(9) y
C15 C16 H16 . . . 122.1 ?
C17 C16 H16 . . . 122.1 ?
C16 C17 C18 . . . 134.2(9) y
C16 C17 C11 . . . 118.9(9) y
C18 C17 C11 . . . 106.7(8) y
C19 C18 C17 . . . 108.3(8) y
C19 C18 H18 . . . 125.9 ?
C17 C18 H18 . . . 125.9 ?
C18 C19 N11 . . . 107.6(8) y
C18 C19 C20 . . . 131.0(8) y
N11 C19 C20 . . . 121.3(7) y
C21 C20 C25 . . . 118.8(4) y
C21 C20 C19 . . . 119.2(5) y
C25 C20 C19 . . . 122.1(5) y
C22 C21 C20 . . . 120.3(4) y
C22 C21 H21 . . . 119.8 ?
C20 C21 H21 . . . 119.8 ?
C21 C22 C23 . . . 120.7(4) y
C21 C22 H22 . . . 119.6 ?
C23 C22 H22 . . . 119.6 ?
C22 C23 C24 . . . 119.2(3) y
C22 C23 H23 . . . 120.4 ?
C24 C23 H23 . . . 120.4 ?
C25 C24 C23 . . . 120.3(3) y
C25 C24 H24 . . . 119.8 ?
C23 C24 H24 . . . 119.8 ?
C24 C25 C20 . . . 120.6(4) y
C24 C25 H25 . . . 119.7 ?
C20 C25 H25 . . . 119.7 ?
C27 C26 C31 . . . 117.8(3) y
C27 C26 C13 . . . 120.0(3) y
C31 C26 C13 . . . 122.0(3) y
C26 C27 C28 . . . 120.8(4) y
C26 C27 H27 . . . 119.6 ?
C28 C27 H27 . . . 119.6 ?
C29 C28 C27 . . . 120.8(4) y
C29 C28 H28 . . . 119.6 ?
C27 C28 H28 . . . 119.6 ?
C30 C29 C28 . . . 119.2(4) y
C30 C29 H29 . . . 120.4 ?
C28 C29 H29 . . . 120.4 ?
C29 C30 C31 . . . 120.4(4) y
C29 C30 H30 . . . 119.8 ?
C31 C30 H30 . . . 119.8 ?
C26 C31 C30 . . . 120.8(4) y
C26 C31 H31 . . . 119.6 ?
C30 C31 H31 . . . 119.6 ?
C49 N41 C41 . . . 108.2(8) y
C49 N41 H41 . . . 129(3) ?
C41 N41 H41 . . . 123(3) ?
C41 N42 C42 . . . 111.7(8) y
C42 N43 C43 . . . 108.7(5) y
C42 N43 H43 . . . 122(2) ?
C43 N43 H43 . . . 129(2) ?
N42 C41 N41 . . . 121.3(8) y
N42 C41 C47 . . . 129.5(8) y
N41 C41 C47 . . . 109.2(8) y
N42 C42 N43 . . . 125.0(7) y
N42 C42 C45 . . . 126.1(7) y
N43 C42 C45 . . . 108.8(6) y
C44 C43 N43 . . . 108.8(5) y
C44 C43 C56 . . . 128.6(4) y
N43 C43 C56 . . . 122.6(4) y
C43 C44 C45 . . . 108.3(5) y
C43 C44 H44 . . . 125.9 ?
C45 C44 H44 . . . 125.9 ?
C46 C45 C44 . . . 135.9(7) y
C46 C45 C42 . . . 118.7(8) y
C44 C45 C42 . . . 105.4(6) y
C47 C46 C45 . . . 117.5(10) y
C47 C46 H46 . . . 121.3 ?
C45 C46 H46 . . . 121.3 ?
C46 C47 C41 . . . 116.4(9) y
C46 C47 C48 . . . 138.6(9) y
C41 C47 C48 . . . 104.7(8) y
C49 C48 C47 . . . 108.9(9) y
C49 C48 H48 . . . 125.5 ?
C47 C48 H48 . . . 125.5 ?
C48 C49 N41 . . . 109.0(8) y
C48 C49 C50 . . . 129.0(9) y
N41 C49 C50 . . . 121.9(9) y
C51 C50 C55 . . . 117.1(5) y
C51 C50 C49 . . . 120.9(6) y
C55 C50 C49 . . . 122.0(6) y
C52 C51 C50 . . . 122.3(5) y
C52 C51 H51 . . . 118.8 ?
C50 C51 H51 . . . 118.8 ?
C53 C52 C51 . . . 119.6(4) y
C53 C52 H52 . . . 120.2 ?
C51 C52 H52 . . . 120.2 ?
C52 C53 C54 . . . 119.5(4) y
C52 C53 H53 . . . 120.3 ?
C54 C53 H53 . . . 120.3 ?
C55 C54 C53 . . . 120.7(4) y
C55 C54 H54 . . . 119.6 ?
C53 C54 H54 . . . 119.6 ?
C54 C55 C50 . . . 120.8(4) y
C54 C55 H55 . . . 119.6 ?
C50 C55 H55 . . . 119.6 ?
C61 C56 C57 . . . 117.4(3) y
C61 C56 C43 . . . 122.7(3) y
C57 C56 C43 . . . 119.9(3) y
C58 C57 C56 . . . 121.7(3) y
C58 C57 H57 . . . 119.1 ?
C56 C57 H57 . . . 119.1 ?
C59 C58 C57 . . . 120.1(3) y
C59 C58 H58 . . . 120.0 ?
C57 C58 H58 . . . 120.0 ?
C58 C59 C60 . . . 119.4(4) y
C58 C59 H59 . . . 120.3 ?
C60 C59 H59 . . . 120.3 ?
C59 C60 C61 . . . 120.8(4) y
C59 C60 H60 . . . 119.6 ?
C61 C60 H60 . . . 119.6 ?
C56 C61 C60 . . . 120.6(3) y
C56 C61 H61 . . . 119.7 ?
C60 C61 H61 . . . 119.7 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 N1 C1 O1 . . . . 178.20(13) y
C2 N1 C1 C5 . . . . -0.2(2) y
C1 N1 C2 O2 . . . . -176.22(13) y
C1 N1 C2 C3 . . . . 1.8(2) y
O2 C2 C3 C7 . . . 3_655 -3.4(2) y
N1 C2 C3 C7 . . . 3_655 178.62(13) y
O2 C2 C3 C4 . . . . 175.34(13) y
N1 C2 C3 C4 . . . . -2.60(18) y
C7 C3 C4 C4 3_655 . . 3_655 1.5(2) y
C2 C3 C4 C4 . . . 3_655 -177.30(14) y
C7 C3 C4 C5 3_655 . . . -179.25(12) y
C2 C3 C4 C5 . . . . 1.97(19) y
C4 C4 C5 C6 3_655 . . . 0.0(2) y
C3 C4 C5 C6 . . . . -179.25(12) y
C4 C4 C5 C1 3_655 . . . 178.92(14) y
C3 C4 C5 C1 . . . . -0.35(19) y
O1 C1 C5 C6 . . . . -0.1(2) y
N1 C1 C5 C6 . . . . 178.30(12) y
O1 C1 C5 C4 . . . . -178.95(13) y
N1 C1 C5 C4 . . . . -0.60(18) y
C4 C5 C6 C7 . . . . 0.0(2) y
C1 C5 C6 C7 . . . . -178.91(13) y
C5 C6 C7 C3 . . . 3_655 -0.8(2) y
C12 N12 C11 N11 . . . . -179.9(12) y
C12 N12 C11 C17 . . . . -1(2) y
C19 N11 C11 N12 . . . . 179.2(14) y
C19 N11 C11 C17 . . . . 0.4(15) y
C11 N12 C12 N13 . . . . 178.9(10) y
C11 N12 C12 C15 . . . . 0(2) y
C13 N13 C12 N12 . . . . -178.3(11) y
C13 N13 C12 C15 . . . . 1.2(8) y
C12 N13 C13 C14 . . . . -1.2(6) y
C12 N13 C13 C26 . . . . 177.6(5) y
N13 C13 C14 C15 . . . . 0.7(6) y
C26 C13 C14 C15 . . . . -177.9(5) y
N12 C12 C15 C16 . . . . 0.3(18) y
N13 C12 C15 C16 . . . . -179.2(11) y
N12 C12 C15 C14 . . . . 178.7(11) y
N13 C12 C15 C14 . . . . -0.7(9) y
C13 C14 C15 C16 . . . . 178.1(13) y
C13 C14 C15 C12 . . . . 0.0(8) y
C12 C15 C16 C17 . . . . 2(2) y
C14 C15 C16 C17 . . . . -176.3(11) y
C15 C16 C17 C18 . . . . -178.7(17) y
C15 C16 C17 C11 . . . . -3(2) y
N12 C11 C17 C16 . . . . 3(2) y
N11 C11 C17 C16 . . . . -177.9(14) y
N12 C11 C17 C18 . . . . 180.0(16) y
N11 C11 C17 C18 . . . . -1.3(16) y
C16 C17 C18 C19 . . . . 177.6(18) y
C11 C17 C18 C19 . . . . 1.7(19) y
C17 C18 C19 N11 . . . . -1.4(18) y
C17 C18 C19 C20 . . . . -177.7(13) y
C11 N11 C19 C18 . . . . 0.6(16) y
C11 N11 C19 C20 . . . . 177.3(10) y
C18 C19 C20 C21 . . . . 0.1(18) y
N11 C19 C20 C21 . . . . -175.7(9) y
C18 C19 C20 C25 . . . . 179.2(14) y
N11 C19 C20 C25 . . . . 3.4(14) y
C25 C20 C21 C22 . . . . 0.1(6) y
C19 C20 C21 C22 . . . . 179.2(7) y
C20 C21 C22 C23 . . . . 0.6(6) y
C21 C22 C23 C24 . . . . -0.9(6) y
C22 C23 C24 C25 . . . . 0.4(5) y
C23 C24 C25 C20 . . . . 0.3(6) y
C21 C20 C25 C24 . . . . -0.5(6) y
C19 C20 C25 C24 . . . . -179.6(7) y
C14 C13 C26 C27 . . . . -2.0(7) y
N13 C13 C26 C27 . . . . 179.5(4) y
C14 C13 C26 C31 . . . . 175.2(5) y
N13 C13 C26 C31 . . . . -3.4(6) y
C31 C26 C27 C28 . . . . -0.1(8) y
C13 C26 C27 C28 . . . . 177.2(5) y
C26 C27 C28 C29 . . . . -0.8(9) y
C27 C28 C29 C30 . . . . 1.1(8) y
C28 C29 C30 C31 . . . . -0.4(7) y
C27 C26 C31 C30 . . . . 0.7(6) y
C13 C26 C31 C30 . . . . -176.5(4) y
C29 C30 C31 C26 . . . . -0.5(7) y
C42 N42 C41 N41 . . . . -179.4(12) y
C42 N42 C41 C47 . . . . 0(2) y
C49 N41 C41 N42 . . . . 179.4(15) y
C49 N41 C41 C47 . . . . -0.2(16) y
C41 N42 C42 N43 . . . . -178.1(11) y
C41 N42 C42 C45 . . . . 2.6(19) y
C43 N43 C42 N42 . . . . 179.8(10) y
C43 N43 C42 C45 . . . . -0.8(8) y
C42 N43 C43 C44 . . . . 1.3(6) y
C42 N43 C43 C56 . . . . -177.6(5) y
N43 C43 C44 C45 . . . . -1.2(7) y
C56 C43 C44 C45 . . . . 177.5(6) y
C43 C44 C45 C46 . . . . -177.9(15) y
C43 C44 C45 C42 . . . . 0.7(8) y
N42 C42 C45 C46 . . . . -1.6(18) y
N43 C42 C45 C46 . . . . 178.9(11) y
N42 C42 C45 C44 . . . . 179.5(10) y
N43 C42 C45 C44 . . . . 0.1(9) y
C44 C45 C46 C47 . . . . 176.4(13) y
C42 C45 C46 C47 . . . . -2(2) y
C45 C46 C47 C41 . . . . 4(3) y
C45 C46 C47 C48 . . . . 177(2) y
N42 C41 C47 C46 . . . . -3(3) y
N41 C41 C47 C46 . . . . 176.1(15) y
N42 C41 C47 C48 . . . . -178.5(18) y
N41 C41 C47 C48 . . . . 1.0(19) y
C46 C47 C48 C49 . . . . -175(2) y
C41 C47 C48 C49 . . . . -1(2) y
C47 C48 C49 N41 . . . . 1(2) y
C47 C48 C49 C50 . . . . 177.6(13) y
C41 N41 C49 C48 . . . . -0.8(17) y
C41 N41 C49 C50 . . . . -177.3(11) y
C48 C49 C50 C51 . . . . 5.3(19) y
N41 C49 C50 C51 . . . . -179.0(9) y
C48 C49 C50 C55 . . . . -173.5(15) y
N41 C49 C50 C55 . . . . 2.2(15) y
C55 C50 C51 C52 . . . . 0.0(8) y
C49 C50 C51 C52 . . . . -178.9(7) y
C50 C51 C52 C53 . . . . 0.1(8) y
C51 C52 C53 C54 . . . . -0.5(7) y
C52 C53 C54 C55 . . . . 0.8(8) y
C53 C54 C55 C50 . . . . -0.7(8) y
C51 C50 C55 C54 . . . . 0.3(8) y
C49 C50 C55 C54 . . . . 179.2(7) y
C44 C43 C56 C61 . . . . 174.4(5) y
N43 C43 C56 C61 . . . . -7.0(6) y
C44 C43 C56 C57 . . . . -7.6(7) y
N43 C43 C56 C57 . . . . 171.0(4) y
C61 C56 C57 C58 . . . . 0.0(6) y
C43 C56 C57 C58 . . . . -178.1(4) y
C56 C57 C58 C59 . . . . -0.6(6) y
C57 C58 C59 C60 . . . . 0.1(6) y
C58 C59 C60 C61 . . . . 0.9(7) y
C57 C56 C61 C60 . . . . 1.0(6) y
C43 C56 C61 C60 . . . . 179.1(4) y
C59 C60 C61 C56 . . . . -1.5(7) y

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 N12 0.94(2) 1.81(2) 2.744(11) 173(17) 1_565 y
N1 H1 N42 0.94(2) 1.94(2) 2.877(10) 175.4(17) 1_565 y
N11 H11 O1 0.94(5) 2.12(5) 2.957(11) 147(4) 1_545 y
N13 H13 O2 1.04(5) 1.97(5) 2.996(6) 171(4) 1_545 y
N41 H41 O1 0.86(5) 2.10(5) 2.956(11) 171(4) 1_545 y
N43 H43 O2 0.86(4) 2.35(4) 3.149(5) 154(3) 1_545 y





#=== END OF THE CIF FILE
_database_code_depnum_ccdc_archive 'CCDC 990642'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
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#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_PERE38

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H15 N3, C20 H16 N2 O4'
_chemical_formula_sum            'C41 H31 N5 O4'
_chemical_formula_weight         657.71
_chemical_compound_source        'Synthesized by the authors. See text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_symmetry_space_group_name_H-M   P-1
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.9141(13)
_cell_length_b                   13.008(2)
_cell_length_c                   19.433(4)
_cell_angle_alpha                96.403(4)
_cell_angle_beta                 94.854(4)
_cell_angle_gamma                97.233(4)
_cell_volume                     1714.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.433
_shelx_estimated_absorpt_T_min   0.911
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_Type   none
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_T_max  0.0000
_exptl_absorpt_process_details   'No absorption correction applied'

_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker Platform diffractometer, equipped with a Bruker SMART 2K
Charged-Coupled Device (CCD) Area Detector using the program SMART and
normal focus sealed tube source graphite monochromated Cu-Kα radiation.
The crystal-to-detector distance was 4.908 cm, and the data collection
was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 9.0 degree
scan in 30 frames over four different parts of the reciprocal space
(120 frames total).  One complete sphere of data was collected, to
better than 0.8Å resolution.  Upon completion of the data collection,
the first 101 frames were recollected in order to improve the decay
correction analysis.
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.34138
_diffrn_radiation_type           GaK\a
_diffrn_measurement_device_type  'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.6
_diffrn_reflns_number            0
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         3.002
_diffrn_reflns_theta_max         55.894
_diffrn_reflns_theta_full        53.594
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6771
_reflns_number_gt                5608
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1068P)²+2.6616P] where P=(Fo²+2Fc²)/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         6771
_refine_ls_number_parameters     458
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0874
_refine_ls_wR_factor_ref         0.2517
_refine_ls_wR_factor_gt          0.2467
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.082

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.002 0.500 1.000 222.3 40.7

_platon_squeeze_details          
;
Attempts to  model disordered solvent molecules
were unsuccessful. PLATON/SQUEEZE  was used to correct
the data for the presence of the disordered solvent.
A potential solvent volume of 222.6 Å³, 
13.0 % of the total unit-cell volume, was found.
41 electrons per unit cell worth of scattering were located
in the void. The reported structure is based on the 
PLATON/SQUEEZE corrected data. The actual solvent content is
unknown, so several quantities calculated like empirical formula, density, 
absorption coefficient, F(000) etc. may be incorrect.

Ref:  Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201.
;


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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.9282(4) 1.01915(19) 0.11993(11) 0.0452(6) Uani 1 1 d . . . . .
O2 O 0.7427(4) 0.6923(2) 0.17623(12) 0.0525(7) Uani 1 1 d . . . . .
O3 O 1.1494(3) 0.85492(18) 0.52192(11) 0.0413(5) Uani 1 1 d . . . . .
O4 O 1.3740(3) 1.17100(18) 0.46125(12) 0.0437(6) Uani 1 1 d . . . . .
N1 N 0.8412(4) 0.8542(2) 0.14577(13) 0.0404(6) Uani 1 1 d . . . . .
N2 N 1.2520(4) 1.0127(2) 0.48929(14) 0.0386(6) Uani 1 1 d . . . . .
H2 H 1.301(7) 1.034(3) 0.532(3) 0.063(13) Uiso 1 1 d . . . . .
C1 C 0.9233(5) 0.9590(3) 0.16298(16) 0.0403(7) Uani 1 1 d . . . . .
C2 C 0.8192(5) 0.7819(3) 0.19356(17) 0.0430(8) Uani 1 1 d . . . . .
C3 C 0.8972(5) 0.8181(3) 0.26732(16) 0.0398(7) Uani 1 1 d . . . . .
C4 C 0.8822(5) 0.7489(3) 0.31563(16) 0.0393(7) Uani 1 1 d . . . . .
H4 H 0.8168 0.6799 0.3023 0.047 Uiso 1 1 calc R U . . .
C5 C 0.9635(5) 0.7799(3) 0.38501(16) 0.0394(7) Uani 1 1 d . . . . .
H5 H 0.9519 0.7323 0.4186 0.047 Uiso 1 1 calc R U . . .
C6 C 1.0603(5) 0.8802(3) 0.40388(16) 0.0379(7) Uani 1 1 d . . . . .
C7 C 1.1562(5) 0.9120(3) 0.47600(16) 0.0377(7) Uani 1 1 d . . . . .
C8 C 1.2743(5) 1.0865(3) 0.44351(17) 0.0392(7) Uani 1 1 d . . . . .
C9 C 1.1747(5) 1.0553(3) 0.37237(16) 0.0381(7) Uani 1 1 d . . . . .
C10 C 1.1871(5) 1.1241(3) 0.32347(17) 0.0405(7) Uani 1 1 d . . . . .
H10 H 1.2539 1.1929 0.3360 0.049 Uiso 1 1 calc R U . . .
C11 C 1.1008(5) 1.0925(3) 0.25479(17) 0.0403(7) Uani 1 1 d . . . . .
H11 H 1.1076 1.1404 0.2213 0.048 Uiso 1 1 calc R U . . .
C12 C 1.0070(5) 0.9925(3) 0.23645(16) 0.0394(7) Uani 1 1 d . . . . .
C13 C 0.9901(4) 0.9209(3) 0.28597(16) 0.0366(7) Uani 1 1 d . . . . .
C14 C 1.0747(5) 0.9525(3) 0.35497(16) 0.0377(7) Uani 1 1 d . . . . .
C15 C 0.7699(5) 0.8157(3) 0.07121(16) 0.0430(8) Uani 1 1 d . . . . .
H15 H 0.7189 0.7400 0.0699 0.052 Uiso 1 1 calc R U . . .
C16 C 0.5986(5) 0.8672(3) 0.04416(17) 0.0482(8) Uani 1 1 d . . . . .
H16A H 0.6413 0.9425 0.0433 0.058 Uiso 1 1 calc R U . . .
H16B H 0.4931 0.8601 0.0754 0.058 Uiso 1 1 calc R U . . .
C17 C 0.5209(6) 0.8154(3) -0.02937(17) 0.0509(9) Uani 1 1 d . . . . .
H17A H 0.4145 0.8519 -0.0481 0.061 Uiso 1 1 calc R U . . .
H17B H 0.4660 0.7418 -0.0276 0.061 Uiso 1 1 calc R U . . .
C18 C 0.6860(6) 0.8195(3) -0.07750(18) 0.0512(9) Uani 1 1 d . . . . .
H18A H 0.6348 0.7825 -0.1240 0.061 Uiso 1 1 calc R U . . .
H18B H 0.7310 0.8932 -0.0830 0.061 Uiso 1 1 calc R U . . .
C19 C 0.8588(6) 0.7698(3) -0.04907(17) 0.0507(9) Uani 1 1 d . . . . .
H19A H 0.9648 0.7774 -0.0801 0.061 Uiso 1 1 calc R U . . .
H19B H 0.8175 0.6943 -0.0483 0.061 Uiso 1 1 calc R U . . .
C20 C 0.9366(5) 0.8205(3) 0.02436(17) 0.0468(8) Uani 1 1 d . . . . .
H20A H 0.9921 0.8941 0.0231 0.056 Uiso 1 1 calc R U . . .
H20B H 1.0420 0.7834 0.0431 0.056 Uiso 1 1 calc R U . . .
N21 N 0.4417(4) 0.7483(2) 0.39762(15) 0.0394(6) Uani 1 1 d . . . . .
H21 H 0.481(8) 0.755(4) 0.441(3) 0.082(16) Uiso 1 1 d . . . . .
N22 N 0.5566(4) 0.9223(2) 0.37658(13) 0.0376(6) Uani 1 1 d . . . . .
N23 N 0.6363(4) 1.0848(2) 0.33220(14) 0.0382(6) Uani 1 1 d . . . . .
H23 H 0.697(7) 1.118(4) 0.370(3) 0.076(15) Uiso 1 1 d . . . . .
C21 C 0.4726(4) 0.8239(3) 0.35544(16) 0.0366(7) Uani 1 1 d . . . . .
C22 C 0.5651(4) 0.9817(3) 0.32487(16) 0.0360(7) Uani 1 1 d . . . . .
C23 C 0.6201(5) 1.1222(3) 0.26771(16) 0.0386(7) Uani 1 1 d . . . . .
C24 C 0.5364(5) 1.0396(3) 0.21890(16) 0.0398(7) Uani 1 1 d . . . . .
H24 H 0.5096 1.0427 0.1705 0.048 Uiso 1 1 calc R U . . .
C25 C 0.4971(5) 0.9498(3) 0.25294(16) 0.0392(7) Uani 1 1 d . . . . .
C26 C 0.4112(5) 0.8454(3) 0.23369(16) 0.0406(7) Uani 1 1 d . . . . .
H26 H 0.3639 0.8201 0.1868 0.049 Uiso 1 1 calc R U . . .
C27 C 0.3981(5) 0.7809(3) 0.28599(16) 0.0391(7) Uani 1 1 d . . . . .
C28 C 0.3220(5) 0.6756(3) 0.29014(17) 0.0427(8) Uani 1 1 d . . . . .
H28 H 0.2625 0.6263 0.2522 0.051 Uiso 1 1 calc R U . . .
C29 C 0.3488(5) 0.6568(3) 0.35842(17) 0.0403(7) Uani 1 1 d D . . . .
C30 C 0.6716(5) 1.2313(3) 0.25888(16) 0.0399(7) Uani 1 1 d . . . . .
C31 C 0.7506(5) 1.2583(3) 0.19812(17) 0.0436(8) Uani 1 1 d . . . . .
H31 H 0.7819 1.2048 0.1652 0.052 Uiso 1 1 calc R U . . .
C32 C 0.7836(6) 1.3600(3) 0.18542(19) 0.0530(9) Uani 1 1 d . . . . .
H32 H 0.8371 1.3767 0.1440 0.064 Uiso 1 1 calc R U . . .
C33 C 0.7387(6) 1.4390(3) 0.2333(2) 0.0553(10) Uani 1 1 d . . . . .
H33 H 0.7603 1.5097 0.2244 0.066 Uiso 1 1 calc R U . . .
C34 C 0.6622(6) 1.4144(3) 0.2942(2) 0.0542(9) Uani 1 1 d . . . . .
H34 H 0.6306 1.4683 0.3268 0.065 Uiso 1 1 calc R U . . .
C35 C 0.6318(5) 1.3120(3) 0.30771(18) 0.0466(8) Uani 1 1 d . . . . .
H35 H 0.5838 1.2960 0.3502 0.056 Uiso 1 1 calc R U . . .
C36A C 0.2901(17) 0.5616(9) 0.3896(5) 0.0431(10) Uani 0.504(7) 1 d DG . P A 1
C37A C 0.176(2) 0.4784(12) 0.3480(4) 0.0454(19) Uani 0.504(7) 1 d G . P A 1
H37A H 0.1407 0.4834 0.3003 0.054 Uiso 0.504(7) 1 calc R U P A 1
C38A C 0.112(2) 0.3880(10) 0.3762(6) 0.0517(13) Uani 0.504(7) 1 d G . P A 1
H38A H 0.0336 0.3312 0.3478 0.062 Uiso 0.504(7) 1 calc R U P A 1
C39A C 0.1629(17) 0.3807(5) 0.4461(6) 0.064(2) Uani 0.504(7) 1 d G . P A 1
H39A H 0.1195 0.3189 0.4654 0.077 Uiso 0.504(7) 1 calc R U P A 1
C40A C 0.2775(13) 0.4639(6) 0.4877(4) 0.0600(18) Uani 0.504(7) 1 d G . P A 1
H40A H 0.3123 0.4589 0.5355 0.072 Uiso 0.504(7) 1 calc R U P A 1
C41A C 0.3411(11) 0.5543(5) 0.4595(5) 0.0517(19) Uani 0.504(7) 1 d G . P A 1
H41A H 0.4194 0.6111 0.4879 0.062 Uiso 0.504(7) 1 calc R U P A 1
C36B C 0.2702(17) 0.5639(9) 0.3914(5) 0.0431(10) Uani 0.496(7) 1 d DG . P A 2
C37B C 0.208(3) 0.4707(12) 0.3486(4) 0.0454(19) Uani 0.496(7) 1 d G . P A 2
H37B H 0.2191 0.4669 0.3001 0.054 Uiso 0.496(7) 1 calc R U P A 2
C38B C 0.130(2) 0.3829(9) 0.3769(6) 0.0517(13) Uani 0.496(7) 1 d G . P A 2
H38B H 0.0875 0.3192 0.3477 0.062 Uiso 0.496(7) 1 calc R U P A 2
C39B C 0.1137(17) 0.3885(6) 0.4480(6) 0.064(2) Uani 0.496(7) 1 d G . P A 2
H39B H 0.0603 0.3285 0.4673 0.077 Uiso 0.496(7) 1 calc R U P A 2
C40B C 0.1758(13) 0.4817(6) 0.4908(4) 0.0600(18) Uani 0.496(7) 1 d G . P A 2
H40B H 0.1648 0.4855 0.5394 0.072 Uiso 0.496(7) 1 calc R U P A 2
C41B C 0.2540(11) 0.5695(5) 0.4625(5) 0.0517(19) Uani 0.496(7) 1 d G . P A 2
H41B H 0.2965 0.6332 0.4918 0.062 Uiso 0.496(7) 1 calc R U P A 2


_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_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 . . 1.208(4) y
O2 C2 . . 1.216(4) y
O3 C7 . . 1.223(4) y
O4 C8 . . 1.219(4) y
N1 C2 . . 1.397(4) y
N1 C1 . . 1.401(4) y
N1 C15 . . 1.500(4) y
N2 C7 . . 1.377(4) y
N2 C8 . . 1.384(4) y
N2 H2 . . 0.87(5) ?
C1 C12 . . 1.490(4) y
C2 C3 . . 1.491(4) y
C3 C4 . . 1.373(5) y
C3 C13 . . 1.403(5) y
C4 C5 . . 1.411(4) y
C4 H4 . . 0.9500 ?
C5 C6 . . 1.384(5) y
C5 H5 . . 0.9500 ?
C6 C14 . . 1.410(5) y
C6 C7 . . 1.490(4) y
C8 C9 . . 1.481(4) y
C9 C10 . . 1.377(5) y
C9 C14 . . 1.417(5) y
C10 C11 . . 1.410(4) y
C10 H10 . . 0.9500 ?
C11 C12 . . 1.373(5) y
C11 H11 . . 0.9500 ?
C12 C13 . . 1.413(5) y
C13 C14 . . 1.412(4) y
C15 C16 . . 1.517(5) y
C15 C20 . . 1.528(5) y
C15 H15 . . 1.0000 ?
C16 C17 . . 1.532(4) y
C16 H16a . . 0.9900 ?
C16 H16b . . 0.9900 ?
C17 C18 . . 1.536(5) y
C17 H17a . . 0.9900 ?
C17 H17b . . 0.9900 ?
C18 C19 . . 1.521(5) y
C18 H18a . . 0.9900 ?
C18 H18b . . 0.9900 ?
C19 C20 . . 1.527(5) y
C19 H19a . . 0.9900 ?
C19 H19b . . 0.9900 ?
C20 H20a . . 0.9900 ?
C20 H20b . . 0.9900 ?
N21 C21 . . 1.356(4) y
N21 C29 . . 1.391(4) y
N21 H21 . . 0.85(6) ?
N22 C22 . . 1.335(4) y
N22 C21 . . 1.342(4) y
N23 C22 . . 1.357(4) y
N23 C23 . . 1.395(4) y
N23 H23 . . 0.85(5) ?
C21 C27 . . 1.428(4) y
C22 C25 . . 1.434(4) y
C23 C24 . . 1.383(4) y
C23 C30 . . 1.452(5) y
C24 C25 . . 1.413(5) y
C24 H24 . . 0.9500 ?
C25 C26 . . 1.408(5) y
C26 C27 . . 1.390(5) y
C26 H26 . . 0.9500 ?
C27 C28 . . 1.417(5) y
C28 C29 . . 1.377(5) y
C28 H28 . . 0.9500 ?
C29 C36a . . 1.466(9) y
C29 C36b . . 1.494(9) y
C30 C31 . . 1.404(5) y
C30 C35 . . 1.405(5) y
C31 C32 . . 1.367(5) y
C31 H31 . . 0.9500 ?
C32 C33 . . 1.391(6) y
C32 H32 . . 0.9500 ?
C33 C34 . . 1.390(6) y
C33 H33 . . 0.9500 ?
C34 C35 . . 1.380(5) y
C34 H34 . . 0.9500 ?
C35 H35 . . 0.9500 ?
C36a C37a . . 1.3900 y
C36a C41a . . 1.3900 y
C37a C38a . . 1.3900 y
C37a H37a . . 0.9500 ?
C38a C39a . . 1.3900 y
C38a H38a . . 0.9500 ?
C39a C40a . . 1.3900 y
C39a H39a . . 0.9500 ?
C40a C41a . . 1.3900 y
C40a H40a . . 0.9500 ?
C41a H41a . . 0.9500 ?
C36b C37b . . 1.3900 y
C36b C41b . . 1.3900 y
C37b C38b . . 1.3900 y
C37b H37b . . 0.9500 ?
C38b C39b . . 1.3900 y
C38b H38b . . 0.9500 ?
C39b C40b . . 1.3900 y
C39b H39b . . 0.9500 ?
C40b C41b . . 1.3900 y
C40b H40b . . 0.9500 ?
C41b H41b . . 0.9500 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 N1 C1 . . . 124.6(3) y
C2 N1 C15 . . . 116.9(3) y
C1 N1 C15 . . . 118.6(3) y
C7 N2 C8 . . . 128.0(3) y
C7 N2 H2 . . . 116(3) ?
C8 N2 H2 . . . 116(3) ?
O1 C1 N1 . . . 121.4(3) y
O1 C1 C12 . . . 121.5(3) y
N1 C1 C12 . . . 117.1(3) y
O2 C2 N1 . . . 122.0(3) y
O2 C2 C3 . . . 120.6(3) y
N1 C2 C3 . . . 117.3(3) y
C4 C3 C13 . . . 121.0(3) y
C4 C3 C2 . . . 119.2(3) y
C13 C3 C2 . . . 119.8(3) y
C3 C4 C5 . . . 120.2(3) y
C3 C4 H4 . . . 119.9 ?
C5 C4 H4 . . . 119.9 ?
C6 C5 C4 . . . 119.6(3) y
C6 C5 H5 . . . 120.2 ?
C4 C5 H5 . . . 120.2 ?
C5 C6 C14 . . . 120.8(3) y
C5 C6 C7 . . . 120.1(3) y
C14 C6 C7 . . . 119.1(3) y
O3 C7 N2 . . . 120.8(3) y
O3 C7 C6 . . . 123.5(3) y
N2 C7 C6 . . . 115.7(3) y
O4 C8 N2 . . . 121.0(3) y
O4 C8 C9 . . . 122.9(3) y
N2 C8 C9 . . . 116.0(3) y
C10 C9 C14 . . . 121.0(3) y
C10 C9 C8 . . . 120.1(3) y
C14 C9 C8 . . . 118.9(3) y
C9 C10 C11 . . . 120.1(3) y
C9 C10 H10 . . . 119.9 ?
C11 C10 H10 . . . 119.9 ?
C12 C11 C10 . . . 119.9(3) y
C12 C11 H11 . . . 120.1 ?
C10 C11 H11 . . . 120.1 ?
C11 C12 C13 . . . 121.0(3) y
C11 C12 C1 . . . 119.3(3) y
C13 C12 C1 . . . 119.7(3) y
C3 C13 C14 . . . 119.4(3) y
C3 C13 C12 . . . 121.3(3) y
C14 C13 C12 . . . 119.3(3) y
C6 C14 C13 . . . 119.1(3) y
C6 C14 C9 . . . 122.2(3) y
C13 C14 C9 . . . 118.7(3) y
N1 C15 C16 . . . 113.0(3) y
N1 C15 C20 . . . 112.0(3) y
C16 C15 C20 . . . 112.9(3) y
N1 C15 H15 . . . 106.1 ?
C16 C15 H15 . . . 106.1 ?
C20 C15 H15 . . . 106.1 ?
C15 C16 C17 . . . 109.6(3) y
C15 C16 H16A . . . 109.7 ?
C17 C16 H16A . . . 109.7 ?
C15 C16 H16B . . . 109.7 ?
C17 C16 H16B . . . 109.7 ?
H16A C16 H16B . . . 108.2 ?
C16 C17 C18 . . . 110.4(3) y
C16 C17 H17A . . . 109.6 ?
C18 C17 H17A . . . 109.6 ?
C16 C17 H17B . . . 109.6 ?
C18 C17 H17B . . . 109.6 ?
H17A C17 H17B . . . 108.1 ?
C19 C18 C17 . . . 111.8(3) y
C19 C18 H18A . . . 109.2 ?
C17 C18 H18A . . . 109.2 ?
C19 C18 H18B . . . 109.2 ?
C17 C18 H18B . . . 109.2 ?
H18A C18 H18B . . . 107.9 ?
C18 C19 C20 . . . 111.3(3) y
C18 C19 H19A . . . 109.4 ?
C20 C19 H19A . . . 109.4 ?
C18 C19 H19B . . . 109.4 ?
C20 C19 H19B . . . 109.4 ?
H19A C19 H19B . . . 108.0 ?
C19 C20 C15 . . . 109.5(3) y
C19 C20 H20A . . . 109.8 ?
C15 C20 H20A . . . 109.8 ?
C19 C20 H20B . . . 109.8 ?
C15 C20 H20B . . . 109.8 ?
H20A C20 H20B . . . 108.2 ?
C21 N21 C29 . . . 109.4(3) y
C21 N21 H21 . . . 125(4) ?
C29 N21 H21 . . . 125(3) ?
C22 N22 C21 . . . 113.0(3) y
C22 N23 C23 . . . 109.8(3) y
C22 N23 H23 . . . 124(3) ?
C23 N23 H23 . . . 126(3) ?
N22 C21 N21 . . . 125.0(3) y
N22 C21 C27 . . . 126.6(3) y
N21 C21 C27 . . . 108.4(3) y
N22 C22 N23 . . . 125.1(3) y
N22 C22 C25 . . . 126.8(3) y
N23 C22 C25 . . . 108.0(3) y
C24 C23 N23 . . . 107.6(3) y
C24 C23 C30 . . . 129.1(3) y
N23 C23 C30 . . . 123.1(3) y
C23 C24 C25 . . . 108.7(3) y
C23 C24 H24 . . . 125.6 ?
C25 C24 H24 . . . 125.6 ?
C26 C25 C24 . . . 136.4(3) y
C26 C25 C22 . . . 117.7(3) y
C24 C25 C22 . . . 105.9(3) y
C27 C26 C25 . . . 117.4(3) y
C27 C26 H26 . . . 121.3 ?
C25 C26 H26 . . . 121.3 ?
C26 C27 C28 . . . 136.0(3) y
C26 C27 C21 . . . 118.5(3) y
C28 C27 C21 . . . 105.6(3) y
C29 C28 C27 . . . 108.6(3) y
C29 C28 H28 . . . 125.7 ?
C27 C28 H28 . . . 125.7 ?
C28 C29 N21 . . . 107.9(3) y
C28 C29 C36A . . . 129.5(6) y
N21 C29 C36A . . . 122.5(6) y
C28 C29 C36B . . . 129.4(6) y
N21 C29 C36B . . . 122.0(6) y
C31 C30 C35 . . . 118.2(3) y
C31 C30 C23 . . . 120.0(3) y
C35 C30 C23 . . . 121.6(3) y
C32 C31 C30 . . . 121.3(3) y
C32 C31 H31 . . . 119.3 ?
C30 C31 H31 . . . 119.3 ?
C31 C32 C33 . . . 119.9(4) y
C31 C32 H32 . . . 120.0 ?
C33 C32 H32 . . . 120.0 ?
C34 C33 C32 . . . 119.8(4) y
C34 C33 H33 . . . 120.1 ?
C32 C33 H33 . . . 120.1 ?
C35 C34 C33 . . . 120.4(4) y
C35 C34 H34 . . . 119.8 ?
C33 C34 H34 . . . 119.8 ?
C34 C35 C30 . . . 120.3(3) y
C34 C35 H35 . . . 119.9 ?
C30 C35 H35 . . . 119.9 ?
C37A C36A C41A . . . 120.0 y
C37A C36A C29 . . . 118.3(8) y
C41A C36A C29 . . . 121.7(8) y
C38A C37A C36A . . . 120.0 y
C38A C37A H37A . . . 120.0 ?
C36A C37A H37A . . . 120.0 ?
C37A C38A C39A . . . 120.0 y
C37A C38A H38A . . . 120.0 ?
C39A C38A H38A . . . 120.0 ?
C40A C39A C38A . . . 120.0 y
C40A C39A H39A . . . 120.0 ?
C38A C39A H39A . . . 120.0 ?
C41A C40A C39A . . . 120.0 y
C41A C40A H40A . . . 120.0 ?
C39A C40A H40A . . . 120.0 ?
C40A C41A C36A . . . 120.0 y
C40A C41A H41A . . . 120.0 ?
C36A C41A H41A . . . 120.0 ?
C37B C36B C41B . . . 120.0 y
C37B C36B C29 . . . 118.0(8) y
C41B C36B C29 . . . 121.9(8) y
C38B C37B C36B . . . 120.0 y
C38B C37B H37B . . . 120.0 ?
C36B C37B H37B . . . 120.0 ?
C39B C38B C37B . . . 120.0 y
C39B C38B H38B . . . 120.0 ?
C37B C38B H38B . . . 120.0 ?
C38B C39B C40B . . . 120.0 y
C38B C39B H39B . . . 120.0 ?
C40B C39B H39B . . . 120.0 ?
C39B C40B C41B . . . 120.0 y
C39B C40B H40B . . . 120.0 ?
C41B C40B H40B . . . 120.0 ?
C40B C41B C36B . . . 120.0 y
C40B C41B H41B . . . 120.0 ?
C36B C41B H41B . . . 120.0 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N23 H23 O3 0.85(5) 2.25(5) 3.057(3) 158(4) 2_776 y
N21 H21 O4 0.85(6) 2.14(6) 2.946(4) 158(5) 2_776 y
N2 H2 N22 0.87(5) 1.95(5) 2.811(4) 172(4) 2_776 y





#=== END OF THE CIF FILE
_database_code_depnum_ccdc_archive 'CCDC 990643'
