# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3a
_database_code_depnum_ccdc_archive 'CCDC 1422957'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H48 N6 O3'
_chemical_formula_weight         684.86
_chemical_absolute_configuration rm

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.489(8)
_cell_length_b                   16.788(10)
_cell_length_c                   15.691(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.627(9)
_cell_angle_gamma                90.00
_cell_volume                     3783(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3024
_cell_measurement_theta_min      1.31
_cell_measurement_theta_max      23.37

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9682
_exptl_absorpt_correction_T_max  0.9846
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,Version 1.171.35.4
in SCALE3 ABSPACK
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33895
_diffrn_reflns_av_R_equivalents  0.1734
_diffrn_reflns_av_sigmaI/netI    0.1805
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         23.37
_reflns_number_total             10962
_reflns_number_gt                5885
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0483P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3(2)
_refine_ls_number_reflns         10962
_refine_ls_number_parameters     925
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.0674
_refine_ls_wR_factor_ref         0.1585
_refine_ls_wR_factor_gt          0.1246
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_restrained_S_all      0.962
_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 0.3770(3) 0.3082(3) 0.3812(3) 0.0374(13) Uani 1 1 d . . .
H1O H 0.4298 0.3139 0.4065 0.045 Uiso 1 1 d R . .
O2 O 0.2151(3) 0.3457(3) 0.0260(3) 0.0256(11) Uani 1 1 d . . .
H2O H 0.1639 0.3415 0.0594 0.031 Uiso 1 1 d R . .
O3 O 0.6032(3) 0.3362(3) 0.0991(3) 0.0307(12) Uani 1 1 d . . .
H3O H 0.5942 0.3486 0.0382 0.037 Uiso 1 1 d R . .
O4 O 0.2228(3) 0.0046(3) -0.0022(3) 0.0275(12) Uani 1 1 d . . .
H4O H 0.1772 0.0000 0.0381 0.033 Uiso 1 1 d R . .
O5 O 0.2292(3) 0.0566(3) -0.3535(3) 0.0337(13) Uani 1 1 d . . .
H5O H 0.2912 0.0449 -0.3341 0.040 Uiso 1 1 d R . .
O6 O -0.1179(3) 0.0234(3) -0.1988(3) 0.0283(12) Uani 1 1 d . . .
H6O H -0.1192 0.0308 -0.2480 0.034 Uiso 1 1 d R . .
N1 N 0.6796(4) 0.2466(3) 0.3381(4) 0.0303(15) Uani 1 1 d . . .
N2 N 0.5391(4) 0.2608(4) 0.4513(4) 0.0319(15) Uani 1 1 d . . .
N3 N 0.1117(4) 0.2607(3) 0.2802(4) 0.0283(15) Uani 1 1 d . . .
N4 N 0.0719(4) 0.2972(3) 0.0942(4) 0.0270(14) Uani 1 1 d . . .
N5 N 0.3855(3) 0.3298(3) -0.1588(3) 0.0246(14) Uani 1 1 d . . .
N6 N 0.5768(4) 0.3204(3) -0.0660(3) 0.0258(14) Uani 1 1 d . . .
N11 N -0.0750(3) 0.0493(3) 0.0608(3) 0.0215(13) Uani 1 1 d . . .
N12 N 0.1212(4) 0.0240(3) 0.1204(3) 0.0226(14) Uani 1 1 d . . .
N13 N 0.4538(4) 0.0631(3) -0.1118(3) 0.0260(14) Uani 1 1 d . . .
N14 N 0.4023(4) 0.0850(4) -0.2982(4) 0.0299(15) Uani 1 1 d . . .
N15 N -0.0240(4) 0.1303(3) -0.4656(4) 0.0310(15) Uani 1 1 d . . .
N16 N -0.1614(4) 0.0851(4) -0.3534(3) 0.0265(14) Uani 1 1 d . . .
C1 C 0.6869(5) 0.3068(4) 0.4073(4) 0.0303(18) Uani 1 1 d . . .
H1 H 0.6557 0.3571 0.3846 0.036 Uiso 1 1 calc R . .
C2 C 0.6379(5) 0.2749(4) 0.4816(4) 0.0292(18) Uani 1 1 d . . .
H2 H 0.6678 0.2238 0.5032 0.035 Uiso 1 1 calc R . .
C3 C 0.6460(6) 0.3359(4) 0.5551(4) 0.040(2) Uani 1 1 d . . .
H3A H 0.6099 0.3842 0.5357 0.048 Uiso 1 1 calc R . .
H3B H 0.6190 0.3131 0.6045 0.048 Uiso 1 1 calc R . .
C4 C 0.7474(5) 0.3592(4) 0.5841(5) 0.041(2) Uani 1 1 d . . .
H4A H 0.7811 0.3128 0.6122 0.049 Uiso 1 1 calc R . .
H4B H 0.7494 0.4026 0.6271 0.049 Uiso 1 1 calc R . .
C5 C 0.7967(6) 0.3869(4) 0.5084(5) 0.044(2) Uani 1 1 d . . .
H5A H 0.7685 0.4373 0.4849 0.052 Uiso 1 1 calc R . .
H5B H 0.8633 0.3968 0.5286 0.052 Uiso 1 1 calc R . .
C6 C 0.7874(6) 0.3235(5) 0.4386(6) 0.044(2) Uani 1 1 d . . .
H6A H 0.822(5) 0.349(4) 0.391(4) 0.052 Uiso 1 1 d . . .
H6B H 0.820(5) 0.274(5) 0.454(5) 0.052 Uiso 1 1 d . . .
C7 C 0.5055(5) 0.1912(5) 0.4571(4) 0.035(2) Uani 1 1 d . . .
H7 H 0.5453 0.1497 0.4810 0.042 Uiso 1 1 calc R . .
C8 C 0.4080(5) 0.1732(4) 0.4281(4) 0.0316(19) Uani 1 1 d . . .
C9 C 0.3479(5) 0.2320(4) 0.3916(5) 0.0327(19) Uani 1 1 d . . .
C10 C 0.2538(5) 0.2156(4) 0.3619(4) 0.0265(18) Uani 1 1 d . . .
C11 C 0.2204(6) 0.1389(4) 0.3744(4) 0.038(2) Uani 1 1 d . . .
H11 H 0.1567 0.1266 0.3569 0.045 Uiso 1 1 calc R . .
C12 C 0.2809(6) 0.0804(4) 0.4127(5) 0.038(2) Uani 1 1 d . . .
H12 H 0.2579 0.0284 0.4215 0.046 Uiso 1 1 calc R . .
C13 C 0.3730(6) 0.0972(4) 0.4377(5) 0.037(2) Uani 1 1 d . . .
H13 H 0.4135 0.0562 0.4620 0.045 Uiso 1 1 calc R . .
C14 C 0.1912(5) 0.2769(4) 0.3190(4) 0.0327(19) Uani 1 1 d . . .
H14 H 0.2117 0.3307 0.3207 0.039 Uiso 1 1 calc R . .
C15 C 0.0549(5) 0.3287(4) 0.2432(4) 0.0293(18) Uani 1 1 d . . .
H15 H 0.0967 0.3751 0.2368 0.035 Uiso 1 1 calc R . .
C16 C 0.0049(5) 0.3054(4) 0.1549(5) 0.0314(19) Uani 1 1 d . . .
H16 H -0.0281 0.2536 0.1595 0.038 Uiso 1 1 calc R . .
C17 C -0.0655(5) 0.3690(4) 0.1193(5) 0.039(2) Uani 1 1 d . . .
H17A H -0.0317 0.4180 0.1068 0.047 Uiso 1 1 calc R . .
H17B H -0.1004 0.3499 0.0646 0.047 Uiso 1 1 calc R . .
C18 C -0.1339(5) 0.3886(5) 0.1824(5) 0.042(2) Uani 1 1 d . . .
H18B H -0.1772 0.4309 0.1581 0.051 Uiso 1 1 calc R . .
H18A H -0.1711 0.3407 0.1920 0.051 Uiso 1 1 calc R . .
C19 C -0.0809(6) 0.4164(5) 0.2673(5) 0.046(2) Uani 1 1 d . . .
H19B H -0.1252 0.4290 0.3082 0.055 Uiso 1 1 calc R . .
H19A H -0.0455 0.4654 0.2580 0.055 Uiso 1 1 calc R . .
C20 C -0.0134(5) 0.3506(4) 0.3051(5) 0.038(2) Uani 1 1 d . . .
H20B H 0.0215 0.3693 0.3600 0.046 Uiso 1 1 calc R . .
H20A H -0.0494 0.3028 0.3173 0.046 Uiso 1 1 calc R . .
C21 C 0.0646(5) 0.2399(4) 0.0390(4) 0.0285(18) Uani 1 1 d . . .
H21 H 0.0182 0.2005 0.0429 0.034 Uiso 1 1 calc R . .
C22 C 0.1231(5) 0.2324(4) -0.0283(4) 0.0268(18) Uani 1 1 d . . .
C23 C 0.1982(5) 0.2855(4) -0.0323(4) 0.0250(17) Uani 1 1 d . . .
C24 C 0.2551(4) 0.2773(4) -0.0971(4) 0.0220(16) Uani 1 1 d . . .
C25 C 0.2370(5) 0.2162(4) -0.1561(4) 0.0253(17) Uani 1 1 d . . .
H25 H 0.2764 0.2094 -0.1993 0.030 Uiso 1 1 calc R . .
C26 C 0.1634(5) 0.1652(4) -0.1536(4) 0.0304(18) Uani 1 1 d . . .
H26 H 0.1512 0.1249 -0.1962 0.037 Uiso 1 1 calc R . .
C27 C 0.1074(5) 0.1719(4) -0.0900(4) 0.0293(18) Uani 1 1 d . . .
H27 H 0.0578 0.1353 -0.0878 0.035 Uiso 1 1 calc R . .
C28 C 0.3331(4) 0.3350(4) -0.1000(4) 0.0242(17) Uani 1 1 d . . .
H28 H 0.3435 0.3758 -0.0578 0.029 Uiso 1 1 calc R . .
C29 C 0.4566(5) 0.3925(4) -0.1574(4) 0.0250(17) Uani 1 1 d . . .
H29 H 0.4537 0.4282 -0.1068 0.030 Uiso 1 1 calc R . .
C30 C 0.5528(4) 0.3558(4) -0.1524(4) 0.0228(17) Uani 1 1 d . . .
H30 H 0.5525 0.3133 -0.1971 0.027 Uiso 1 1 calc R . .
C31 C 0.6280(4) 0.4171(4) -0.1639(4) 0.0250(18) Uani 1 1 d . . .
H31A H 0.6880 0.3894 -0.1657 0.030 Uiso 1 1 calc R . .
H31B H 0.6355 0.4537 -0.1140 0.030 Uiso 1 1 calc R . .
C32 C 0.6032(5) 0.4656(4) -0.2471(4) 0.0331(19) Uani 1 1 d . . .
H32A H 0.6507 0.5075 -0.2505 0.040 Uiso 1 1 calc R . .
H32B H 0.6033 0.4301 -0.2976 0.040 Uiso 1 1 calc R . .
C33 C 0.5083(4) 0.5037(4) -0.2491(4) 0.0300(18) Uani 1 1 d . . .
H33B H 0.4926 0.5334 -0.3035 0.036 Uiso 1 1 calc R . .
H33A H 0.5096 0.5420 -0.2009 0.036 Uiso 1 1 calc R . .
C34 C 0.4347(5) 0.4409(4) -0.2416(4) 0.0292(18) Uani 1 1 d . . .
H34B H 0.4314 0.4043 -0.2914 0.035 Uiso 1 1 calc R . .
H34A H 0.3733 0.4669 -0.2429 0.035 Uiso 1 1 calc R . .
C35 C 0.5998(4) 0.2476(4) -0.0565(4) 0.0233(17) Uani 1 1 d . . .
H35 H 0.5993 0.2147 -0.1058 0.028 Uiso 1 1 calc R . .
C36 C 0.6272(4) 0.2136(4) 0.0294(4) 0.0242(17) Uani 1 1 d . . .
C37 C 0.6281(4) 0.2590(4) 0.1026(4) 0.0231(17) Uani 1 1 d . . .
C38 C 0.6528(4) 0.2246(4) 0.1842(4) 0.0255(17) Uani 1 1 d . . .
C39 C 0.6785(5) 0.1436(4) 0.1899(5) 0.0288(18) Uani 1 1 d . . .
H39 H 0.6960 0.1200 0.2447 0.035 Uiso 1 1 calc R . .
C40 C 0.6786(5) 0.0982(4) 0.1163(5) 0.0302(18) Uani 1 1 d . . .
H40 H 0.6963 0.0437 0.1203 0.036 Uiso 1 1 calc R . .
C41 C 0.6522(4) 0.1333(4) 0.0362(4) 0.0264(18) Uani 1 1 d . . .
H41 H 0.6512 0.1022 -0.0144 0.032 Uiso 1 1 calc R . .
C42 C 0.6557(4) 0.2730(4) 0.2618(4) 0.0266(17) Uani 1 1 d . . .
H42 H 0.6388 0.3276 0.2553 0.032 Uiso 1 1 calc R . .
C43 C -0.0404(4) -0.0218(4) 0.1122(4) 0.0219(16) Uani 1 1 d . . .
H43 H -0.0257 -0.0657 0.0732 0.026 Uiso 1 1 calc R . .
C44 C 0.0469(4) 0.0025(4) 0.1712(4) 0.0212(16) Uani 1 1 d . . .
H44 H 0.0328 0.0487 0.2077 0.025 Uiso 1 1 calc R . .
C45 C 0.0824(5) -0.0675(4) 0.2282(4) 0.0331(19) Uani 1 1 d . . .
H45B H 0.1379 -0.0504 0.2675 0.040 Uiso 1 1 calc R . .
H45A H 0.1016 -0.1109 0.1916 0.040 Uiso 1 1 calc R . .
C46 C 0.0088(5) -0.0996(4) 0.2815(5) 0.037(2) Uani 1 1 d . . .
H46B H 0.0328 -0.1482 0.3126 0.044 Uiso 1 1 calc R . .
H46A H -0.0036 -0.0592 0.3246 0.044 Uiso 1 1 calc R . .
C47 C -0.0816(5) -0.1190(4) 0.2235(4) 0.0308(18) Uani 1 1 d . . .
H47B H -0.0713 -0.1656 0.1871 0.037 Uiso 1 1 calc R . .
H47A H -0.1301 -0.1336 0.2596 0.037 Uiso 1 1 calc R . .
C48 C -0.1159(4) -0.0490(4) 0.1659(4) 0.0276(18) Uani 1 1 d . . .
H48A H -0.1328 -0.0042 0.2018 0.033 Uiso 1 1 calc R . .
H48B H -0.1724 -0.0650 0.1270 0.033 Uiso 1 1 calc R . .
C49 C 0.1700(5) 0.0858(4) 0.1448(4) 0.0270(17) Uani 1 1 d . . .
H49 H 0.1540 0.1166 0.1914 0.032 Uiso 1 1 calc R . .
C50 C 0.2496(4) 0.1097(4) 0.1026(4) 0.0209(16) Uani 1 1 d . . .
C51 C 0.2735(4) 0.0676(4) 0.0323(4) 0.0246(17) Uani 1 1 d . . .
C52 C 0.3511(4) 0.0909(4) -0.0058(4) 0.0239(17) Uani 1 1 d . . .
C53 C 0.4025(5) 0.1551(4) 0.0278(4) 0.0336(19) Uani 1 1 d . . .
H53 H 0.4546 0.1715 0.0013 0.040 Uiso 1 1 calc R . .
C54 C 0.3811(5) 0.1970(4) 0.0989(4) 0.0288(18) Uani 1 1 d . . .
H54 H 0.4186 0.2406 0.1210 0.035 Uiso 1 1 calc R . .
C55 C 0.3038(5) 0.1743(4) 0.1374(4) 0.0298(18) Uani 1 1 d . . .
H55 H 0.2881 0.2020 0.1863 0.036 Uiso 1 1 calc R . .
C56 C 0.3817(4) 0.0444(4) -0.0775(4) 0.0247(17) Uani 1 1 d . . .
H56 H 0.3464 -0.0008 -0.0987 0.030 Uiso 1 1 calc R . .
C57 C 0.4827(5) 0.0114(4) -0.1769(4) 0.0279(18) Uani 1 1 d . . .
H57 H 0.4341 -0.0304 -0.1918 0.033 Uiso 1 1 calc R . .
C58 C 0.4937(5) 0.0594(4) -0.2574(4) 0.0297(18) Uani 1 1 d . . .
H58 H 0.5331 0.1073 -0.2410 0.036 Uiso 1 1 calc R . .
C59 C 0.5385(4) 0.0096(4) -0.3232(4) 0.0285(18) Uani 1 1 d . . .
H59B H 0.4958 -0.0338 -0.3455 0.034 Uiso 1 1 calc R . .
H59A H 0.5500 0.0437 -0.3723 0.034 Uiso 1 1 calc R . .
C60 C 0.6309(5) -0.0258(4) -0.2803(4) 0.0310(18) Uani 1 1 d . . .
H60B H 0.6597 -0.0575 -0.3230 0.037 Uiso 1 1 calc R . .
H60A H 0.6743 0.0179 -0.2601 0.037 Uiso 1 1 calc R . .
C61 C 0.6160(5) -0.0784(4) -0.2049(5) 0.037(2) Uani 1 1 d . . .
H61B H 0.6762 -0.1013 -0.1789 0.044 Uiso 1 1 calc R . .
H61A H 0.5737 -0.1228 -0.2249 0.044 Uiso 1 1 calc R . .
C62 C 0.5736(5) -0.0288(4) -0.1378(4) 0.0335(19) Uani 1 1 d . . .
H62A H 0.6187 0.0125 -0.1142 0.040 Uiso 1 1 calc R . .
H62B H 0.5611 -0.0637 -0.0898 0.040 Uiso 1 1 calc R . .
C63 C 0.3900(5) 0.1569(4) -0.3232(4) 0.0263(18) Uani 1 1 d . . .
H63 H 0.4405 0.1933 -0.3135 0.032 Uiso 1 1 calc R . .
C64 C 0.3008(5) 0.1846(4) -0.3664(4) 0.0279(18) Uani 1 1 d . . .
C65 C 0.2227(5) 0.1336(4) -0.3796(4) 0.0267(18) Uani 1 1 d . . .
C66 C 0.1366(5) 0.1613(4) -0.4211(4) 0.0281(18) Uani 1 1 d . . .
C67 C 0.1289(5) 0.2397(4) -0.4498(5) 0.036(2) Uani 1 1 d . . .
H67 H 0.0706 0.2590 -0.4768 0.043 Uiso 1 1 calc R . .
C68 C 0.2064(5) 0.2903(4) -0.4393(5) 0.037(2) Uani 1 1 d . . .
H68 H 0.2017 0.3431 -0.4613 0.044 Uiso 1 1 calc R . .
C69 C 0.2896(5) 0.2629(4) -0.3966(4) 0.0330(19) Uani 1 1 d . . .
H69 H 0.3411 0.2983 -0.3874 0.040 Uiso 1 1 calc R . .
C70 C 0.0579(5) 0.1068(4) -0.4378(4) 0.0297(18) Uani 1 1 d . . .
H70 H 0.0683 0.0515 -0.4276 0.036 Uiso 1 1 calc R . .
C71 C -0.0951(5) 0.0681(4) -0.4897(4) 0.0277(18) Uani 1 1 d . . .
H71 H -0.0695 0.0145 -0.4715 0.033 Uiso 1 1 calc R . .
C72 C -0.1816(4) 0.0853(4) -0.4479(4) 0.0255(17) Uani 1 1 d . . .
H72 H -0.2058 0.1391 -0.4670 0.031 Uiso 1 1 calc R . .
C73 C -0.2569(4) 0.0230(4) -0.4765(4) 0.0288(18) Uani 1 1 d . . .
H73B H -0.2345 -0.0303 -0.4564 0.035 Uiso 1 1 calc R . .
H73A H -0.3136 0.0353 -0.4500 0.035 Uiso 1 1 calc R . .
C74 C -0.2810(5) 0.0220(4) -0.5741(4) 0.0351(19) Uani 1 1 d . . .
H74B H -0.3107 0.0732 -0.5934 0.042 Uiso 1 1 calc R . .
H74A H -0.3264 -0.0211 -0.5908 0.042 Uiso 1 1 calc R . .
C75 C -0.1947(5) 0.0093(4) -0.6187(4) 0.0332(19) Uani 1 1 d . . .
H75B H -0.2117 0.0142 -0.6817 0.040 Uiso 1 1 calc R . .
H75A H -0.1698 -0.0450 -0.6062 0.040 Uiso 1 1 calc R . .
C76 C -0.1201(5) 0.0709(4) -0.5874(4) 0.0295(18) Uani 1 1 d . . .
H76B H -0.0636 0.0605 -0.6149 0.035 Uiso 1 1 calc R . .
H76A H -0.1432 0.1247 -0.6049 0.035 Uiso 1 1 calc R . .
C77 C -0.1828(5) 0.1483(4) -0.3145(4) 0.0298(18) Uani 1 1 d . . .
H77 H -0.2053 0.1927 -0.3487 0.036 Uiso 1 1 calc R . .
C78 C -0.1748(4) 0.1567(4) -0.2213(4) 0.0239(17) Uani 1 1 d . . .
C79 C -0.1421(4) 0.0939(4) -0.1667(4) 0.0234(17) Uani 1 1 d . . .
C80 C -0.1347(4) 0.1032(4) -0.0779(4) 0.0197(16) Uani 1 1 d . . .
C81 C -0.1575(4) 0.1760(4) -0.0448(4) 0.0280(18) Uani 1 1 d . . .
H81 H -0.1526 0.1825 0.0158 0.034 Uiso 1 1 calc R . .
C82 C -0.1875(5) 0.2399(4) -0.0978(5) 0.0300(18) Uani 1 1 d . . .
H82 H -0.2026 0.2895 -0.0741 0.036 Uiso 1 1 calc R . .
C83 C -0.1947(5) 0.2295(4) -0.1860(4) 0.0261(17) Uani 1 1 d . . .
H83 H -0.2135 0.2730 -0.2230 0.031 Uiso 1 1 calc R . .
C84 C -0.0998(4) 0.0377(4) -0.0203(4) 0.0206(16) Uani 1 1 d . . .
H84 H -0.0954 -0.0143 -0.0433 0.025 Uiso 1 1 calc R . .


_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 C9 1.363(8) . ?
O2 C23 1.365(7) . ?
O3 C37 1.345(7) . ?
O4 C51 1.358(7) . ?
O5 C65 1.356(8) . ?
O6 C79 1.351(8) . ?
N1 C42 1.280(8) . ?
N1 C1 1.477(8) . ?
N2 C7 1.273(9) . ?
N2 C2 1.467(8) . ?
N3 C14 1.260(8) . ?
N3 C15 1.480(8) . ?
N4 C21 1.289(8) . ?
N4 C16 1.454(8) . ?
N5 C28 1.273(8) . ?
N5 C29 1.472(8) . ?
N6 C35 1.270(8) . ?
N6 C30 1.479(8) . ?
N11 C84 1.290(7) . ?
N11 C43 1.490(8) . ?
N12 C49 1.284(8) . ?
N12 C44 1.468(8) . ?
N13 C56 1.275(8) . ?
N13 C57 1.445(8) . ?
N14 C63 1.275(8) . ?
N14 C58 1.457(8) . ?
N15 C70 1.272(8) . ?
N15 C71 1.480(8) . ?
N16 C77 1.282(8) . ?
N16 C72 1.472(7) . ?
C1 C6 1.501(10) . ?
C1 C2 1.540(9) . ?
C2 C3 1.536(9) . ?
C3 C4 1.530(10) . ?
C4 C5 1.536(10) . ?
C5 C6 1.520(10) . ?
C7 C8 1.457(10) . ?
C8 C9 1.388(10) . ?
C8 C13 1.389(10) . ?
C9 C10 1.408(9) . ?
C10 C11 1.399(9) . ?
C10 C14 1.473(9) . ?
C11 C12 1.399(10) . ?
C12 C13 1.369(10) . ?
C15 C20 1.521(9) . ?
C15 C16 1.526(9) . ?
C16 C17 1.530(9) . ?
C17 C18 1.528(9) . ?
C18 C19 1.521(10) . ?
C19 C20 1.541(10) . ?
C21 C22 1.445(9) . ?
C22 C27 1.400(9) . ?
C22 C23 1.415(9) . ?
C23 C24 1.399(9) . ?
C24 C25 1.383(9) . ?
C24 C28 1.493(9) . ?
C25 C26 1.372(9) . ?
C26 C27 1.372(9) . ?
C29 C30 1.516(9) . ?
C29 C34 1.547(9) . ?
C30 C31 1.526(8) . ?
C31 C32 1.541(8) . ?
C32 C33 1.514(9) . ?
C33 C34 1.515(9) . ?
C35 C36 1.469(9) . ?
C36 C37 1.377(9) . ?
C36 C41 1.396(9) . ?
C37 C38 1.407(9) . ?
C38 C39 1.410(9) . ?
C38 C42 1.459(9) . ?
C39 C40 1.384(9) . ?
C40 C41 1.395(9) . ?
C43 C44 1.520(8) . ?
C43 C48 1.536(9) . ?
C44 C45 1.524(8) . ?
C45 C46 1.537(9) . ?
C46 C47 1.528(9) . ?
C47 C48 1.525(9) . ?
C49 C50 1.460(9) . ?
C50 C51 1.392(9) . ?
C50 C55 1.406(9) . ?
C51 C52 1.398(9) . ?
C52 C53 1.374(9) . ?
C52 C56 1.486(9) . ?
C53 C54 1.387(9) . ?
C54 C55 1.394(9) . ?
C57 C58 1.524(9) . ?
C57 C62 1.533(9) . ?
C58 C59 1.539(8) . ?
C59 C60 1.536(9) . ?
C60 C61 1.515(9) . ?
C61 C62 1.533(9) . ?
C63 C64 1.454(9) . ?
C64 C69 1.398(9) . ?
C64 C65 1.413(9) . ?
C65 C66 1.407(9) . ?
C66 C67 1.390(9) . ?
C66 C70 1.459(9) . ?
C67 C68 1.401(10) . ?
C68 C69 1.378(9) . ?
C71 C72 1.518(9) . ?
C71 C76 1.528(8) . ?
C72 C73 1.536(9) . ?
C73 C74 1.524(9) . ?
C74 C75 1.528(9) . ?
C75 C76 1.529(9) . ?
C77 C78 1.458(9) . ?
C78 C83 1.388(9) . ?
C78 C79 1.401(9) . ?
C79 C80 1.393(8) . ?
C80 C81 1.386(9) . ?
C80 C84 1.469(9) . ?
C81 C82 1.391(9) . ?
C82 C83 1.385(9) . ?

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
C42 N1 C1 115.7(6) . . ?
C7 N2 C2 119.5(6) . . ?
C14 N3 C15 116.6(6) . . ?
C21 N4 C16 120.5(6) . . ?
C28 N5 C29 115.1(6) . . ?
C35 N6 C30 121.3(6) . . ?
C84 N11 C43 116.3(5) . . ?
C49 N12 C44 116.9(5) . . ?
C56 N13 C57 118.7(6) . . ?
C63 N14 C58 119.7(6) . . ?
C70 N15 C71 117.1(6) . . ?
C77 N16 C72 116.7(6) . . ?
N1 C1 C6 109.9(6) . . ?
N1 C1 C2 108.9(5) . . ?
C6 C1 C2 110.0(6) . . ?
N2 C2 C3 109.0(6) . . ?
N2 C2 C1 109.8(6) . . ?
C3 C2 C1 109.9(6) . . ?
C4 C3 C2 111.6(6) . . ?
C3 C4 C5 111.9(6) . . ?
C6 C5 C4 109.9(7) . . ?
C1 C6 C5 110.9(7) . . ?
N2 C7 C8 122.2(7) . . ?
C9 C8 C13 118.7(7) . . ?
C9 C8 C7 120.7(7) . . ?
C13 C8 C7 120.6(7) . . ?
O1 C9 C8 122.0(7) . . ?
O1 C9 C10 116.4(7) . . ?
C8 C9 C10 121.6(7) . . ?
C11 C10 C9 118.1(7) . . ?
C11 C10 C14 120.2(7) . . ?
C9 C10 C14 121.7(7) . . ?
C12 C11 C10 119.9(7) . . ?
C13 C12 C11 120.7(7) . . ?
C12 C13 C8 120.9(7) . . ?
N3 C14 C10 122.6(7) . . ?
N3 C15 C20 108.2(5) . . ?
N3 C15 C16 109.3(6) . . ?
C20 C15 C16 111.8(6) . . ?
N4 C16 C15 110.0(6) . . ?
N4 C16 C17 107.3(6) . . ?
C15 C16 C17 111.5(6) . . ?
C18 C17 C16 111.9(6) . . ?
C19 C18 C17 109.7(6) . . ?
C18 C19 C20 109.8(6) . . ?
C15 C20 C19 111.2(6) . . ?
N4 C21 C22 123.5(7) . . ?
C27 C22 C23 118.7(6) . . ?
C27 C22 C21 120.8(6) . . ?
C23 C22 C21 120.5(6) . . ?
O2 C23 C24 119.3(6) . . ?
O2 C23 C22 120.5(6) . . ?
C24 C23 C22 120.1(6) . . ?
C25 C24 C23 118.8(6) . . ?
C25 C24 C28 122.6(6) . . ?
C23 C24 C28 118.7(6) . . ?
C26 C25 C24 121.5(7) . . ?
C27 C26 C25 120.4(7) . . ?
C26 C27 C22 120.4(7) . . ?
N5 C28 C24 120.2(6) . . ?
N5 C29 C30 110.3(5) . . ?
N5 C29 C34 107.4(5) . . ?
C30 C29 C34 109.9(5) . . ?
N6 C30 C29 108.3(5) . . ?
N6 C30 C31 107.1(5) . . ?
C29 C30 C31 112.7(5) . . ?
C30 C31 C32 111.5(5) . . ?
C33 C32 C31 110.4(6) . . ?
C32 C33 C34 110.6(6) . . ?
C33 C34 C29 111.4(5) . . ?
N6 C35 C36 121.1(6) . . ?
C37 C36 C41 119.8(7) . . ?
C37 C36 C35 121.5(6) . . ?
C41 C36 C35 118.8(6) . . ?
O3 C37 C36 121.8(6) . . ?
O3 C37 C38 117.9(6) . . ?
C36 C37 C38 120.3(6) . . ?
C37 C38 C39 119.1(6) . . ?
C37 C38 C42 120.4(6) . . ?
C39 C38 C42 120.4(6) . . ?
C40 C39 C38 120.6(7) . . ?
C39 C40 C41 119.2(7) . . ?
C40 C41 C36 121.0(6) . . ?
N1 C42 C38 124.1(7) . . ?
N11 C43 C44 107.9(5) . . ?
N11 C43 C48 108.8(5) . . ?
C44 C43 C48 110.0(5) . . ?
N12 C44 C43 110.3(5) . . ?
N12 C44 C45 107.1(5) . . ?
C43 C44 C45 109.8(5) . . ?
C44 C45 C46 112.7(6) . . ?
C47 C46 C45 110.6(6) . . ?
C48 C47 C46 112.0(6) . . ?
C47 C48 C43 110.7(5) . . ?
N12 C49 C50 121.6(6) . . ?
C51 C50 C55 121.0(6) . . ?
C51 C50 C49 120.9(6) . . ?
C55 C50 C49 118.1(6) . . ?
O4 C51 C50 122.2(6) . . ?
O4 C51 C52 118.1(6) . . ?
C50 C51 C52 119.7(6) . . ?
C53 C52 C51 118.8(6) . . ?
C53 C52 C56 120.1(6) . . ?
C51 C52 C56 120.9(6) . . ?
C52 C53 C54 122.5(6) . . ?
C53 C54 C55 119.2(7) . . ?
C54 C55 C50 118.8(6) . . ?
N13 C56 C52 122.2(6) . . ?
N13 C57 C58 109.9(5) . . ?
N13 C57 C62 107.2(5) . . ?
C58 C57 C62 112.7(5) . . ?
N14 C58 C57 109.3(5) . . ?
N14 C58 C59 107.8(6) . . ?
C57 C58 C59 111.6(5) . . ?
C60 C59 C58 109.7(6) . . ?
C61 C60 C59 111.2(6) . . ?
C60 C61 C62 109.4(6) . . ?
C61 C62 C57 111.4(6) . . ?
N14 C63 C64 121.7(6) . . ?
C69 C64 C65 117.7(6) . . ?
C69 C64 C63 121.0(6) . . ?
C65 C64 C63 121.3(6) . . ?
O5 C65 C66 118.5(6) . . ?
O5 C65 C64 120.8(6) . . ?
C66 C65 C64 120.8(7) . . ?
C67 C66 C65 119.4(7) . . ?
C67 C66 C70 120.6(7) . . ?
C65 C66 C70 120.0(7) . . ?
C66 C67 C68 120.5(7) . . ?
C69 C68 C67 119.4(7) . . ?
C68 C69 C64 122.2(7) . . ?
N15 C70 C66 122.6(7) . . ?
N15 C71 C72 110.0(5) . . ?
N15 C71 C76 107.5(5) . . ?
C72 C71 C76 109.2(5) . . ?
N16 C72 C71 111.8(5) . . ?
N16 C72 C73 109.3(5) . . ?
C71 C72 C73 109.9(6) . . ?
C74 C73 C72 111.1(6) . . ?
C73 C74 C75 111.7(6) . . ?
C74 C75 C76 110.1(6) . . ?
C71 C76 C75 111.5(6) . . ?
N16 C77 C78 124.4(7) . . ?
C83 C78 C79 119.3(6) . . ?
C83 C78 C77 119.5(6) . . ?
C79 C78 C77 121.0(6) . . ?
O6 C79 C80 118.8(6) . . ?
O6 C79 C78 121.0(6) . . ?
C80 C79 C78 120.2(6) . . ?
C81 C80 C79 118.9(6) . . ?
C81 C80 C84 120.6(6) . . ?
C79 C80 C84 120.4(6) . . ?
C80 C81 C82 121.8(6) . . ?
C83 C82 C81 118.5(7) . . ?
C82 C83 C78 121.2(6) . . ?
N11 C84 C80 121.4(6) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        23.37
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.056
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3b
_database_code_depnum_ccdc_archive 'CCDC 1422958'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H45 F3 N6 O3'
_chemical_formula_sum            'C42 H45 F3 N6 O3'
_chemical_formula_weight         738.84
_chemical_absolute_configuration rm

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.6367(4)
_cell_length_b                   17.6967(4)
_cell_length_c                   15.0640(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.450(2)
_cell_angle_gamma                90.00
_cell_volume                     3890.13(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(1)
_cell_measurement_reflns_used    8075
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      28.81

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9395
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro (Agilent Technologies, 2011)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;


_diffrn_ambient_temperature      120(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_standards_number         31888
_diffrn_standards_interval_count 4
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31842
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         28.81
_reflns_number_total             17092
_reflns_number_gt                12811
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0523P)²+0.3534P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(5)
_refine_ls_number_reflns         17092
_refine_ls_number_parameters     973
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1214
_refine_ls_wR_factor_gt          0.1087
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
N1 N 0.53167(15) 0.10408(13) 0.61910(14) 0.0377(5) Uani 1 1 d . . .
N2 N 0.57082(15) 0.12601(12) 0.80865(14) 0.0349(5) Uani 1 1 d . . .
C1 C 0.49616(19) 0.05419(15) 0.68533(17) 0.0357(6) Uani 1 1 d . . .
H1A H 0.5410 0.0141 0.7000 0.043 Uiso 1 1 calc R . .
C2 C 0.48226(17) 0.09989(14) 0.76973(17) 0.0332(6) Uani 1 1 d . . .
H2A H 0.4437 0.1438 0.7537 0.040 Uiso 1 1 calc R . .
C3 C 0.4357(2) 0.05226(16) 0.83742(19) 0.0409(7) Uani 1 1 d . . .
H3A H 0.4762 0.0115 0.8579 0.049 Uiso 1 1 calc R . .
H3B H 0.4242 0.0833 0.8884 0.049 Uiso 1 1 calc R . .
C4 C 0.3459(2) 0.01948(16) 0.79790(19) 0.0425(7) Uani 1 1 d . . .
H4A H 0.3036 0.0602 0.7815 0.051 Uiso 1 1 calc R . .
H4B H 0.3190 -0.0115 0.8421 0.051 Uiso 1 1 calc R . .
C5 C 0.3607(2) -0.02819(16) 0.71613(19) 0.0459(7) Uani 1 1 d . . .
H5A H 0.3988 -0.0714 0.7334 0.055 Uiso 1 1 calc R . .
H5B H 0.3022 -0.0468 0.6904 0.055 Uiso 1 1 calc R . .
C6 C 0.4065(2) 0.01833(16) 0.64732(18) 0.0403(7) Uani 1 1 d . . .
H6A H 0.3649 0.0579 0.6251 0.048 Uiso 1 1 calc R . .
H6B H 0.4189 -0.0139 0.5975 0.048 Uiso 1 1 calc R . .
C7 C 0.58687(18) 0.19684(15) 0.81588(16) 0.0336(6) Uani 1 1 d . . .
H7A H 0.5410 0.2306 0.7959 0.040 Uiso 1 1 calc R . .
C8 C 0.67325(18) 0.22686(14) 0.85379(16) 0.0315(6) Uani 1 1 d . . .
C9 C 0.6840(2) 0.30482(15) 0.86458(17) 0.0372(6) Uani 1 1 d . . .
H9A H 0.6358 0.3374 0.8480 0.045 Uiso 1 1 calc R . .
C10 C 0.7659(2) 0.33291(15) 0.89967(18) 0.0417(7) Uani 1 1 d . . .
C11 C 0.8400(2) 0.28683(15) 0.92320(18) 0.0391(6) Uani 1 1 d . . .
H11A H 0.8952 0.3078 0.9459 0.047 Uiso 1 1 calc R . .
C12 C 0.83189(18) 0.20964(15) 0.91294(17) 0.0352(6) Uani 1 1 d . . .
C13 C 0.74742(19) 0.17867(14) 0.87878(16) 0.0349(6) Uani 1 1 d . . .
C14 C 0.90943(19) 0.15939(16) 0.93818(17) 0.0381(6) Uani 1 1 d . . .
H14A H 0.9010 0.1074 0.9345 0.046 Uiso 1 1 calc R . .
F1 F 0.77515(12) 0.40859(9) 0.91167(13) 0.0576(5) Uani 1 1 d . . .
O1 O 0.73913(13) 0.10315(10) 0.87184(12) 0.0393(4) Uani 1 1 d . . .
H1O H 0.6785 0.0924 0.8466 0.059 Uiso 1 1 d R . .
N3 N 0.98787(16) 0.18532(13) 0.96497(15) 0.0419(6) Uani 1 1 d . . .
N4 N 1.13177(15) 0.14564(13) 0.85134(15) 0.0400(5) Uani 1 1 d . . .
C15 C 1.05999(19) 0.13227(16) 0.99328(18) 0.0414(7) Uani 1 1 d . . .
H15A H 1.0404 0.0808 0.9771 0.050 Uiso 1 1 calc R . .
C16 C 1.14611(18) 0.15173(16) 0.94795(17) 0.0397(6) Uani 1 1 d . . .
H16A H 1.1625 0.2042 0.9627 0.048 Uiso 1 1 calc R . .
C17 C 1.22652(19) 0.10169(18) 0.98018(19) 0.0460(7) Uani 1 1 d . . .
H17A H 1.2125 0.0495 0.9647 0.055 Uiso 1 1 calc R . .
H17B H 1.2803 0.1164 0.9506 0.055 Uiso 1 1 calc R . .
C18 C 1.2467(2) 0.10818(18) 1.0796(2) 0.0519(8) Uani 1 1 d . . .
H18A H 1.2673 0.1590 1.0945 0.062 Uiso 1 1 calc R . .
H18B H 1.2955 0.0734 1.0990 0.062 Uiso 1 1 calc R . .
C19 C 1.1618(2) 0.09029(19) 1.1279(2) 0.0520(8) Uani 1 1 d . . .
H19A H 1.1468 0.0372 1.1201 0.062 Uiso 1 1 calc R . .
H19B H 1.1748 0.0995 1.1911 0.062 Uiso 1 1 calc R . .
C20 C 1.0801(2) 0.13773(17) 1.09382(19) 0.0490(7) Uani 1 1 d . . .
H20A H 1.0917 0.1901 1.1099 0.059 Uiso 1 1 calc R . .
H20B H 1.0265 0.1213 1.1227 0.059 Uiso 1 1 calc R . .
C21 C 1.14814(19) 0.20410(16) 0.8058(2) 0.0441(7) Uani 1 1 d . . .
H21A H 1.1626 0.2487 0.8364 0.053 Uiso 1 1 calc R . .
C22 C 1.14566(19) 0.20549(15) 0.70986(19) 0.0393(6) Uani 1 1 d . . .
C23 C 1.1702(2) 0.27089(16) 0.6659(2) 0.0473(7) Uani 1 1 d . . .
H23A H 1.1881 0.3139 0.6983 0.057 Uiso 1 1 calc R . .
C24 C 1.16777(19) 0.27156(16) 0.5754(2) 0.0442(7) Uani 1 1 d . . .
C25 C 1.14278(17) 0.20984(16) 0.52506(19) 0.0398(7) Uani 1 1 d . . .
H25A H 1.1428 0.2122 0.4634 0.048 Uiso 1 1 calc R . .
C26 C 1.11740(17) 0.14354(15) 0.56563(18) 0.0351(6) Uani 1 1 d . . .
C27 C 1.12006(17) 0.14084(15) 0.65888(18) 0.0353(6) Uani 1 1 d . . .
C28 C 1.08406(17) 0.07813(16) 0.51308(17) 0.0350(6) Uani 1 1 d . . .
H28A H 1.0795 0.0315 0.5409 0.042 Uiso 1 1 calc R . .
F2 F 1.19210(13) 0.33633(9) 0.53425(13) 0.0619(5) Uani 1 1 d . . .
O2 O 1.09704(13) 0.07612(10) 0.69921(12) 0.0418(5) Uani 1 1 d . . .
H2O H 1.0996 0.0910 0.7618 0.063 Uiso 1 1 d R . .
N5 N 1.06139(15) 0.08368(13) 0.43071(15) 0.0392(5) Uani 1 1 d . . .
N6 N 0.87016(15) 0.05525(14) 0.37735(14) 0.0404(6) Uani 1 1 d . . .
C29 C 1.03047(19) 0.01409(16) 0.38516(18) 0.0390(6) Uani 1 1 d . . .
H29A H 1.0166 -0.0241 0.4292 0.047 Uiso 1 1 calc R . .
N15 N 0.50253(16) 0.29540(13) 0.04718(14) 0.0390(5) Uani 1 1 d . . .
N16 N 0.35239(15) 0.29289(11) 0.16245(14) 0.0326(5) Uani 1 1 d . . .
C79 C 0.4076(2) 0.30538(17) 0.01364(17) 0.0420(7) Uani 1 1 d . . .
H79A H 0.3805 0.2560 -0.0016 0.050 Uiso 1 1 calc R . .
C30 C 0.94410(19) 0.03097(17) 0.32416(18) 0.0411(7) Uani 1 1 d . . .
H30A H 0.9574 0.0712 0.2824 0.049 Uiso 1 1 calc R . .
C31 C 0.9136(2) -0.03918(18) 0.27235(19) 0.0476(7) Uani 1 1 d . . .
H31A H 0.8597 -0.0272 0.2332 0.057 Uiso 1 1 calc R . .
H31B H 0.8965 -0.0778 0.3137 0.057 Uiso 1 1 calc R . .
C32 C 0.9879(2) -0.07019(19) 0.21698(19) 0.0535(8) Uani 1 1 d . . .
H32A H 0.9670 -0.1169 0.1884 0.064 Uiso 1 1 calc R . .
H32B H 1.0002 -0.0342 0.1708 0.064 Uiso 1 1 calc R . .
C33 C 1.0751(2) -0.08472(19) 0.27599(19) 0.0521(8) Uani 1 1 d . . .
H33A H 1.0647 -0.1259 0.3165 0.062 Uiso 1 1 calc R . .
H33B H 1.1235 -0.0999 0.2392 0.062 Uiso 1 1 calc R . .
C34 C 1.1054(2) -0.01511(18) 0.32928(19) 0.0455(7) Uani 1 1 d . . .
H34A H 1.1221 0.0243 0.2888 0.055 Uiso 1 1 calc R . .
H34B H 1.1594 -0.0273 0.3682 0.055 Uiso 1 1 calc R . .
C35 C 0.83000(18) 0.11793(16) 0.35856(18) 0.0380(6) Uani 1 1 d . . .
H35A H 0.8519 0.1479 0.3141 0.046 Uiso 1 1 calc R . .
C36 C 0.75178(18) 0.14472(14) 0.40337(17) 0.0337(6) Uani 1 1 d . . .
C37 C 0.70928(18) 0.21155(15) 0.37455(19) 0.0396(6) Uani 1 1 d . . .
H37A H 0.7311 0.2390 0.3280 0.047 Uiso 1 1 calc R . .
C38 C 0.6344(2) 0.23634(15) 0.4162(2) 0.0438(7) Uani 1 1 d . . .
C39 C 0.60124(19) 0.19593(15) 0.4853(2) 0.0416(7) Uani 1 1 d . . .
H39A H 0.5507 0.2139 0.5127 0.050 Uiso 1 1 calc R . .
C40 C 0.64217(17) 0.12922(14) 0.51419(17) 0.0335(6) Uani 1 1 d . . .
C41 C 0.71934(17) 0.10340(15) 0.47366(17) 0.0341(6) Uani 1 1 d . . .
C42 C 0.60446(18) 0.08457(15) 0.58532(17) 0.0341(6) Uani 1 1 d . . .
H42A H 0.6349 0.0411 0.6058 0.041 Uiso 1 1 calc R . .
F3 F 0.59515(13) 0.30252(9) 0.39083(14) 0.0656(5) Uani 1 1 d . . .
O3 O 0.75948(12) 0.03845(10) 0.50265(12) 0.0406(5) Uani 1 1 d . . .
H3O H 0.8159 0.0414 0.4714 0.061 Uiso 1 1 d R . .
N11 N 0.43468(13) 0.38078(11) 0.57393(13) 0.0285(4) Uani 1 1 d . . .
N12 N 0.62153(13) 0.38847(12) 0.65426(13) 0.0305(5) Uani 1 1 d . . .
C51 C 0.45878(16) 0.41605(13) 0.65959(15) 0.0272(5) Uani 1 1 d . . .
H51A H 0.4575 0.3781 0.7069 0.033 Uiso 1 1 calc R . .
C52 C 0.55543(17) 0.44935(14) 0.65947(15) 0.0287(5) Uani 1 1 d . . .
H52A H 0.5582 0.4820 0.6072 0.034 Uiso 1 1 calc R . .
C53 C 0.57893(18) 0.49609(14) 0.74323(17) 0.0340(6) Uani 1 1 d . . .
H53A H 0.5807 0.4633 0.7950 0.041 Uiso 1 1 calc R . .
H53B H 0.6393 0.5182 0.7404 0.041 Uiso 1 1 calc R . .
C54 C 0.50937(19) 0.55844(15) 0.75324(18) 0.0392(6) Uani 1 1 d . . .
H54A H 0.5105 0.5932 0.7036 0.047 Uiso 1 1 calc R . .
H54B H 0.5255 0.5864 0.8076 0.047 Uiso 1 1 calc R . .
C55 C 0.41337(19) 0.52573(15) 0.75616(17) 0.0364(6) Uani 1 1 d . . .
H55A H 0.3694 0.5665 0.7587 0.044 Uiso 1 1 calc R . .
H55B H 0.4105 0.4952 0.8094 0.044 Uiso 1 1 calc R . .
C56 C 0.38877(18) 0.47731(15) 0.67403(17) 0.0337(6) Uani 1 1 d . . .
H56A H 0.3296 0.4538 0.6799 0.040 Uiso 1 1 calc R . .
H56B H 0.3830 0.5097 0.6220 0.040 Uiso 1 1 calc R . .
C57 C 0.67587(16) 0.39304(14) 0.59320(16) 0.0301(5) Uani 1 1 d . . .
H57A H 0.6694 0.4332 0.5534 0.036 Uiso 1 1 calc R . .
C58 C 0.74906(17) 0.33724(14) 0.58266(16) 0.0308(6) Uani 1 1 d . . .
C59 C 0.75928(18) 0.27458(15) 0.63751(17) 0.0341(6) Uani 1 1 d . . .
H59A H 0.7189 0.2668 0.6813 0.041 Uiso 1 1 calc R . .
C60 C 0.82880(19) 0.22379(14) 0.62759(18) 0.0368(6) Uani 1 1 d . . .
C61 C 0.89020(19) 0.23336(15) 0.56370(18) 0.0384(6) Uani 1 1 d . . .
H61A H 0.9366 0.1982 0.5579 0.046 Uiso 1 1 calc R . .
C62 C 0.88232(17) 0.29603(15) 0.50785(16) 0.0317(6) Uani 1 1 d . . .
C63 C 0.81093(17) 0.34796(15) 0.51706(16) 0.0320(6) Uani 1 1 d . . .
C64 C 0.94760(17) 0.30675(16) 0.44075(17) 0.0357(6) Uani 1 1 d . . .
H64A H 0.9904 0.2690 0.4327 0.043 Uiso 1 1 calc R . .
F11 F 0.83631(12) 0.16234(9) 0.68147(11) 0.0529(4) Uani 1 1 d . . .
O11 O 0.80176(12) 0.40956(10) 0.46393(11) 0.0372(4) Uani 1 1 d . . .
H11O H 0.8432 0.4097 0.4204 0.056 Uiso 1 1 d R . .
N13 N 0.94841(14) 0.36600(13) 0.39252(14) 0.0363(5) Uani 1 1 d . . .
N14 N 0.91984(16) 0.32336(13) 0.20757(15) 0.0395(5) Uani 1 1 d . . .
C65 C 1.01797(18) 0.37530(16) 0.32904(18) 0.0390(6) Uani 1 1 d . . .
H65A H 1.0535 0.3285 0.3270 0.047 Uiso 1 1 calc R . .
C66 C 0.97140(18) 0.39034(15) 0.23780(17) 0.0369(6) Uani 1 1 d . . .
H66A H 0.9293 0.4332 0.2410 0.044 Uiso 1 1 calc R . .
C67 C 1.0418(2) 0.40809(17) 0.17072(19) 0.0471(7) Uani 1 1 d . . .
H67A H 1.0785 0.3635 0.1618 0.057 Uiso 1 1 calc R . .
H67B H 1.0102 0.4216 0.1140 0.057 Uiso 1 1 calc R . .
C68 C 1.1039(2) 0.47253(17) 0.2032(2) 0.0503(8) Uani 1 1 d . . .
H68A H 1.0678 0.5182 0.2071 0.060 Uiso 1 1 calc R . .
H68B H 1.1491 0.4814 0.1606 0.060 Uiso 1 1 calc R . .
C69 C 1.1527(2) 0.45577(18) 0.2937(2) 0.0493(7) Uani 1 1 d . . .
H69A H 1.1901 0.4987 0.3135 0.059 Uiso 1 1 calc R . .
H69B H 1.1926 0.4124 0.2894 0.059 Uiso 1 1 calc R . .
C70 C 1.08228(19) 0.43969(17) 0.36037(19) 0.0449(7) Uani 1 1 d . . .
H70A H 1.0466 0.4850 0.3687 0.054 Uiso 1 1 calc R . .
H70B H 1.1137 0.4264 0.4173 0.054 Uiso 1 1 calc R . .
C71 C 0.83819(19) 0.33274(15) 0.17469(16) 0.0349(6) Uani 1 1 d . . .
H71A H 0.8138 0.3813 0.1717 0.042 Uiso 1 1 calc R . .
C72 C 0.7812(2) 0.26921(14) 0.14119(17) 0.0347(6) Uani 1 1 d . . .
C73 C 0.8176(2) 0.19668(15) 0.13977(18) 0.0418(7) Uani 1 1 d . . .
H73A H 0.8789 0.1886 0.1584 0.050 Uiso 1 1 calc R . .
C74 C 0.7636(2) 0.13750(16) 0.1112(2) 0.0474(8) Uani 1 1 d . . .
C75 C 0.6736(2) 0.14665(16) 0.08223(18) 0.0459(8) Uani 1 1 d . . .
H75A H 0.6387 0.1051 0.0629 0.055 Uiso 1 1 calc R . .
C76 C 0.6340(2) 0.21848(15) 0.08158(17) 0.0366(6) Uani 1 1 d . . .
C77 C 0.6896(2) 0.28043(14) 0.11112(17) 0.0362(6) Uani 1 1 d . . .
C78 C 0.5391(2) 0.23008(16) 0.05069(17) 0.0410(7) Uani 1 1 d . . .
H78A H 0.5035 0.1884 0.0328 0.049 Uiso 1 1 calc R . .
F12 F 0.80107(15) 0.06752(9) 0.11051(14) 0.0722(6) Uani 1 1 d . . .
O12 O 0.65582(13) 0.35111(10) 0.11027(13) 0.0442(5) Uani 1 1 d . . .
H12O H 0.5988 0.3479 0.0819 0.066 Uiso 1 1 d R . .
C80 C 0.35444(18) 0.34259(15) 0.08513(17) 0.0360(6) Uani 1 1 d . . .
H80A H 0.3845 0.3902 0.1035 0.043 Uiso 1 1 calc R . .
C81 C 0.2568(2) 0.35878(19) 0.0493(2) 0.0540(8) Uani 1 1 d . . .
H81A H 0.2251 0.3114 0.0367 0.065 Uiso 1 1 calc R . .
H81B H 0.2252 0.3851 0.0945 0.065 Uiso 1 1 calc R . .
C82 C 0.2526(3) 0.4060(3) -0.0342(3) 0.0932(16) Uani 1 1 d . . .
H82A H 0.2770 0.4559 -0.0201 0.112 Uiso 1 1 calc R . .
H82B H 0.1892 0.4117 -0.0573 0.112 Uiso 1 1 calc R . .
C83 C 0.3066(3) 0.3703(3) -0.1046(3) 0.107(2) Uani 1 1 d . . .
H83A H 0.2775 0.3233 -0.1243 0.129 Uiso 1 1 calc R . .
H83B H 0.3066 0.4038 -0.1555 0.129 Uiso 1 1 calc R . .
C84 C 0.4041(2) 0.3548(2) -0.06930(19) 0.0661(11) Uani 1 1 d . . .
H84A H 0.4349 0.4022 -0.0551 0.079 Uiso 1 1 calc R . .
H84B H 0.4362 0.3297 -0.1149 0.079 Uiso 1 1 calc R . .
C85 C 0.36809(16) 0.32278(14) 0.23828(15) 0.0282(5) Uani 1 1 d . . .
H85A H 0.3836 0.3737 0.2413 0.034 Uiso 1 1 calc R . .
C86 C 0.36291(16) 0.28090(13) 0.32142(16) 0.0277(5) Uani 1 1 d . . .
C87 C 0.33598(17) 0.20520(13) 0.32141(17) 0.0305(5) Uani 1 1 d . . .
H87A H 0.3200 0.1806 0.2679 0.037 Uiso 1 1 calc R . .
C88 C 0.33321(17) 0.16733(13) 0.40018(18) 0.0312(6) Uani 1 1 d . . .
C89 C 0.35666(16) 0.20073(14) 0.48070(17) 0.0297(5) Uani 1 1 d . . .
H89A H 0.3549 0.1731 0.5331 0.036 Uiso 1 1 calc R . .
C90 C 0.38318(16) 0.27639(13) 0.48362(16) 0.0274(5) Uani 1 1 d . . .
C91 C 0.38525(16) 0.31713(13) 0.40282(16) 0.0273(5) Uani 1 1 d . . .
C92 C 0.40894(16) 0.31214(14) 0.56864(16) 0.0285(5) Uani 1 1 d . . .
H92A H 0.4066 0.2841 0.6206 0.034 Uiso 1 1 calc R . .
F13 F 0.30629(11) 0.09353(8) 0.39903(10) 0.0437(4) Uani 1 1 d . . .
O13 O 0.40983(12) 0.39013(9) 0.40269(11) 0.0328(4) Uani 1 1 d . . .
H13O H 0.4214 0.4050 0.4623 0.049 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C42 1.264(3) . ?
N1 C1 1.458(3) . ?
N2 C7 1.278(3) . ?
N2 C2 1.456(3) . ?
C1 C6 1.528(4) . ?
C1 C2 1.534(4) . ?
C1 H1A 0.9800 . ?
C2 C3 1.524(4) . ?
C2 H2A 0.9800 . ?
C3 C4 1.515(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.522(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.520(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.447(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.397(3) . ?
C8 C13 1.409(4) . ?
C9 C10 1.365(4) . ?
C9 H9A 0.9300 . ?
C10 F1 1.357(3) . ?
C10 C11 1.381(4) . ?
C11 C12 1.379(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.412(4) . ?
C12 C14 1.468(4) . ?
C13 O1 1.345(3) . ?
C14 N3 1.273(3) . ?
C14 H14A 0.9300 . ?
O1 H1O 0.9576 . ?
N3 C15 1.452(4) . ?
N4 C21 1.274(4) . ?
N4 C16 1.458(3) . ?
C15 C16 1.519(4) . ?
C15 C20 1.523(4) . ?
C15 H15A 0.9800 . ?
C16 C17 1.522(4) . ?
C16 H16A 0.9800 . ?
C17 C18 1.508(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.521(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.518(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.443(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.394(4) . ?
C22 C27 1.412(4) . ?
C23 C24 1.361(4) . ?
C23 H23A 0.9300 . ?
C24 C25 1.364(4) . ?
C24 F2 1.364(3) . ?
C25 C26 1.387(4) . ?
C25 H25A 0.9300 . ?
C26 C27 1.403(4) . ?
C26 C28 1.464(4) . ?
C27 O2 1.351(3) . ?
C28 N5 1.263(3) . ?
C28 H28A 0.9300 . ?
O2 H2O 0.9765 . ?
N5 C29 1.464(4) . ?
N6 C35 1.277(3) . ?
N6 C30 1.460(3) . ?
C29 C34 1.524(4) . ?
C29 C30 1.533(4) . ?
C29 H29A 0.9800 . ?
N15 C78 1.273(4) . ?
N15 C79 1.452(4) . ?
N16 C85 1.263(3) . ?
N16 C80 1.462(3) . ?
C79 C84 1.522(4) . ?
C79 C80 1.526(4) . ?
C79 H79A 0.9800 . ?
C30 C31 1.515(4) . ?
C30 H30A 0.9800 . ?
C31 C32 1.524(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.520(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.518(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.453(4) . ?
C35 H35A 0.9300 . ?
C36 C37 1.390(4) . ?
C36 C41 1.400(4) . ?
C37 C38 1.376(4) . ?
C37 H37A 0.9300 . ?
C38 F3 1.347(3) . ?
C38 C39 1.382(4) . ?
C39 C40 1.379(4) . ?
C39 H39A 0.9300 . ?
C40 C41 1.402(4) . ?
C40 C42 1.473(4) . ?
C41 O3 1.348(3) . ?
C42 H42A 0.9300 . ?
O3 H3O 0.9825 . ?
N11 C92 1.273(3) . ?
N11 C51 1.452(3) . ?
N12 C57 1.264(3) . ?
N12 C52 1.454(3) . ?
C51 C56 1.519(3) . ?
C51 C52 1.533(3) . ?
C51 H51A 0.9800 . ?
C52 C53 1.525(3) . ?
C52 H52A 0.9800 . ?
C53 C54 1.517(4) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.523(4) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.525(4) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 C58 1.475(3) . ?
C57 H57A 0.9300 . ?
C58 C59 1.384(3) . ?
C58 C63 1.404(3) . ?
C59 C60 1.374(4) . ?
C59 H59A 0.9300 . ?
C60 F11 1.356(3) . ?
C60 C61 1.377(4) . ?
C61 C62 1.391(4) . ?
C61 H61A 0.9300 . ?
C62 C63 1.406(3) . ?
C62 C64 1.456(4) . ?
C63 O11 1.353(3) . ?
C64 N13 1.276(3) . ?
C64 H64A 0.9300 . ?
O11 H11O 0.9278 . ?
N13 C65 1.459(3) . ?
N14 C71 1.269(3) . ?
N14 C66 1.459(3) . ?
C65 C66 1.510(4) . ?
C65 C70 1.529(4) . ?
C65 H65A 0.9800 . ?
C66 C67 1.531(4) . ?
C66 H66A 0.9800 . ?
C67 C68 1.516(4) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C68 C69 1.517(4) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C69 C70 1.521(4) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C71 C72 1.466(4) . ?
C71 H71A 0.9300 . ?
C72 C73 1.391(4) . ?
C72 C77 1.396(4) . ?
C73 C74 1.362(4) . ?
C73 H73A 0.9300 . ?
C74 F12 1.355(3) . ?
C74 C75 1.365(4) . ?
C75 C76 1.397(4) . ?
C75 H75A 0.9300 . ?
C76 C77 1.416(4) . ?
C76 C78 1.445(4) . ?
C77 O12 1.345(3) . ?
C78 H78A 0.9300 . ?
O12 H12O 0.9095 . ?
C80 C81 1.516(4) . ?
C80 H80A 0.9800 . ?
C81 C82 1.508(5) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C82 C83 1.509(7) . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C83 C84 1.508(5) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C84 H84A 0.9700 . ?
C84 H84B 0.9700 . ?
C85 C86 1.462(3) . ?
C85 H85A 0.9300 . ?
C86 C87 1.397(3) . ?
C86 C91 1.400(3) . ?
C87 C88 1.366(4) . ?
C87 H87A 0.9300 . ?
C88 F13 1.364(3) . ?
C88 C89 1.369(4) . ?
C89 C90 1.394(3) . ?
C89 H89A 0.9300 . ?
C90 C91 1.417(3) . ?
C90 C92 1.452(3) . ?
C91 O13 1.341(3) . ?
C92 H92A 0.9300 . ?
O13 H13O 0.9388 . ?

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
C42 N1 C1 117.8(2) . . ?
C7 N2 C2 119.8(2) . . ?
N1 C1 C6 109.7(2) . . ?
N1 C1 C2 109.0(2) . . ?
C6 C1 C2 111.4(2) . . ?
N1 C1 H1A 108.9 . . ?
C6 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N2 C2 C3 109.7(2) . . ?
N2 C2 C1 109.3(2) . . ?
C3 C2 C1 111.0(2) . . ?
N2 C2 H2A 109.0 . . ?
C3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C4 C3 C2 111.6(2) . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C3 C4 C5 110.9(2) . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
C6 C5 C4 110.5(2) . . ?
C6 C5 H5A 109.6 . . ?
C4 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C5 C6 C1 112.4(2) . . ?
C5 C6 H6A 109.1 . . ?
C1 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
C1 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 C8 122.9(2) . . ?
N2 C7 H7A 118.6 . . ?
C8 C7 H7A 118.6 . . ?
C9 C8 C13 119.3(2) . . ?
C9 C8 C7 119.7(2) . . ?
C13 C8 C7 121.0(2) . . ?
C10 C9 C8 119.5(3) . . ?
C10 C9 H9A 120.2 . . ?
C8 C9 H9A 120.2 . . ?
F1 C10 C9 119.1(3) . . ?
F1 C10 C11 118.7(3) . . ?
C9 C10 C11 122.2(2) . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C11 C12 C13 119.4(2) . . ?
C11 C12 C14 120.9(3) . . ?
C13 C12 C14 119.8(2) . . ?
O1 C13 C8 121.2(2) . . ?
O1 C13 C12 119.0(2) . . ?
C8 C13 C12 119.8(2) . . ?
N3 C14 C12 121.6(3) . . ?
N3 C14 H14A 119.2 . . ?
C12 C14 H14A 119.2 . . ?
C13 O1 H1O 107.6 . . ?
C14 N3 C15 118.5(2) . . ?
C21 N4 C16 117.3(2) . . ?
N3 C15 C16 109.3(2) . . ?
N3 C15 C20 109.3(2) . . ?
C16 C15 C20 109.2(2) . . ?
N3 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
C20 C15 H15A 109.6 . . ?
N4 C16 C15 111.8(2) . . ?
N4 C16 C17 108.9(2) . . ?
C15 C16 C17 111.9(2) . . ?
N4 C16 H16A 108.0 . . ?
C15 C16 H16A 108.0 . . ?
C17 C16 H16A 108.0 . . ?
C18 C17 C16 111.1(2) . . ?
C18 C17 H17A 109.4 . . ?
C16 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
C16 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C17 C18 C19 110.8(2) . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 112.0(3) . . ?
C20 C19 H19A 109.2 . . ?
C18 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C18 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C19 C20 C15 112.8(2) . . ?
C19 C20 H20A 109.0 . . ?
C15 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
C15 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
N4 C21 C22 124.2(3) . . ?
N4 C21 H21A 117.9 . . ?
C22 C21 H21A 117.9 . . ?
C23 C22 C27 118.8(3) . . ?
C23 C22 C21 120.2(3) . . ?
C27 C22 C21 121.0(3) . . ?
C24 C23 C22 119.7(3) . . ?
C24 C23 H23A 120.2 . . ?
C22 C23 H23A 120.2 . . ?
C23 C24 C25 122.4(3) . . ?
C23 C24 F2 118.4(3) . . ?
C25 C24 F2 119.2(3) . . ?
C24 C25 C26 120.1(3) . . ?
C24 C25 H25A 119.9 . . ?
C26 C25 H25A 119.9 . . ?
C25 C26 C27 118.8(3) . . ?
C25 C26 C28 121.3(2) . . ?
C27 C26 C28 119.8(2) . . ?
O2 C27 C26 119.4(2) . . ?
O2 C27 C22 120.5(2) . . ?
C26 C27 C22 120.2(2) . . ?
N5 C28 C26 121.4(3) . . ?
N5 C28 H28A 119.3 . . ?
C26 C28 H28A 119.3 . . ?
C27 O2 H2O 102.3 . . ?
C28 N5 C29 116.3(2) . . ?
C35 N6 C30 118.8(2) . . ?
N5 C29 C34 109.5(2) . . ?
N5 C29 C30 109.1(2) . . ?
C34 C29 C30 109.3(2) . . ?
N5 C29 H29A 109.6 . . ?
C34 C29 H29A 109.6 . . ?
C30 C29 H29A 109.6 . . ?
C78 N15 C79 120.8(2) . . ?
C85 N16 C80 117.1(2) . . ?
N15 C79 C84 109.0(2) . . ?
N15 C79 C80 109.5(2) . . ?
C84 C79 C80 110.2(3) . . ?
N15 C79 H79A 109.4 . . ?
C84 C79 H79A 109.4 . . ?
C80 C79 H79A 109.4 . . ?
N6 C30 C31 108.8(2) . . ?
N6 C30 C29 109.9(2) . . ?
C31 C30 C29 110.2(2) . . ?
N6 C30 H30A 109.3 . . ?
C31 C30 H30A 109.3 . . ?
C29 C30 H30A 109.3 . . ?
C30 C31 C32 112.5(3) . . ?
C30 C31 H31A 109.1 . . ?
C32 C31 H31A 109.1 . . ?
C30 C31 H31B 109.1 . . ?
C32 C31 H31B 109.1 . . ?
H31A C31 H31B 107.8 . . ?
C33 C32 C31 110.1(2) . . ?
C33 C32 H32A 109.6 . . ?
C31 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.2 . . ?
C34 C33 C32 111.7(3) . . ?
C34 C33 H33A 109.3 . . ?
C32 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C32 C33 H33B 109.3 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 C29 111.9(2) . . ?
C33 C34 H34A 109.2 . . ?
C29 C34 H34A 109.2 . . ?
C33 C34 H34B 109.2 . . ?
C29 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
N6 C35 C36 123.1(3) . . ?
N6 C35 H35A 118.4 . . ?
C36 C35 H35A 118.4 . . ?
C37 C36 C41 120.7(3) . . ?
C37 C36 C35 118.8(2) . . ?
C41 C36 C35 120.4(2) . . ?
C38 C37 C36 118.8(3) . . ?
C38 C37 H37A 120.6 . . ?
C36 C37 H37A 120.6 . . ?
F3 C38 C37 119.0(3) . . ?
F3 C38 C39 119.8(3) . . ?
C37 C38 C39 121.1(3) . . ?
C40 C39 C38 120.7(3) . . ?
C40 C39 H39A 119.6 . . ?
C38 C39 H39A 119.6 . . ?
C39 C40 C41 119.1(2) . . ?
C39 C40 C42 120.7(2) . . ?
C41 C40 C42 120.1(2) . . ?
O3 C41 C36 121.7(2) . . ?
O3 C41 C40 118.9(2) . . ?
C36 C41 C40 119.4(2) . . ?
N1 C42 C40 121.4(2) . . ?
N1 C42 H42A 119.3 . . ?
C40 C42 H42A 119.3 . . ?
C41 O3 H3O 99.2 . . ?
C92 N11 C51 121.1(2) . . ?
C57 N12 C52 116.8(2) . . ?
N11 C51 C56 108.30(19) . . ?
N11 C51 C52 108.95(19) . . ?
C56 C51 C52 111.0(2) . . ?
N11 C51 H51A 109.5 . . ?
C56 C51 H51A 109.5 . . ?
C52 C51 H51A 109.5 . . ?
N12 C52 C53 109.76(19) . . ?
N12 C52 C51 109.46(19) . . ?
C53 C52 C51 110.9(2) . . ?
N12 C52 H52A 108.9 . . ?
C53 C52 H52A 108.9 . . ?
C51 C52 H52A 108.9 . . ?
C54 C53 C52 111.5(2) . . ?
C54 C53 H53A 109.3 . . ?
C52 C53 H53A 109.3 . . ?
C54 C53 H53B 109.3 . . ?
C52 C53 H53B 109.3 . . ?
H53A C53 H53B 108.0 . . ?
C53 C54 C55 110.7(2) . . ?
C53 C54 H54A 109.5 . . ?
C55 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C55 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
C54 C55 C56 110.5(2) . . ?
C54 C55 H55A 109.5 . . ?
C56 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 108.1 . . ?
C51 C56 C55 113.4(2) . . ?
C51 C56 H56A 108.9 . . ?
C55 C56 H56A 108.9 . . ?
C51 C56 H56B 108.9 . . ?
C55 C56 H56B 108.9 . . ?
H56A C56 H56B 107.7 . . ?
N12 C57 C58 122.6(2) . . ?
N12 C57 H57A 118.7 . . ?
C58 C57 H57A 118.7 . . ?
C59 C58 C63 118.9(2) . . ?
C59 C58 C57 121.2(2) . . ?
C63 C58 C57 119.9(2) . . ?
C60 C59 C58 120.4(2) . . ?
C60 C59 H59A 119.8 . . ?
C58 C59 H59A 119.8 . . ?
F11 C60 C59 119.1(2) . . ?
F11 C60 C61 119.3(2) . . ?
C59 C60 C61 121.6(2) . . ?
C60 C61 C62 119.5(2) . . ?
C60 C61 H61A 120.2 . . ?
C62 C61 H61A 120.2 . . ?
C61 C62 C63 119.2(2) . . ?
C61 C62 C64 119.7(2) . . ?
C63 C62 C64 121.1(2) . . ?
O11 C63 C58 119.0(2) . . ?
O11 C63 C62 120.6(2) . . ?
C58 C63 C62 120.4(2) . . ?
N13 C64 C62 122.5(2) . . ?
N13 C64 H64A 118.7 . . ?
C62 C64 H64A 118.7 . . ?
C63 O11 H11O 112.3 . . ?
C64 N13 C65 120.2(2) . . ?
C71 N14 C66 117.7(2) . . ?
N13 C65 C66 109.1(2) . . ?
N13 C65 C70 109.0(2) . . ?
C66 C65 C70 111.9(2) . . ?
N13 C65 H65A 108.9 . . ?
C66 C65 H65A 108.9 . . ?
C70 C65 H65A 108.9 . . ?
N14 C66 C65 109.1(2) . . ?
N14 C66 C67 108.6(2) . . ?
C65 C66 C67 111.0(2) . . ?
N14 C66 H66A 109.4 . . ?
C65 C66 H66A 109.4 . . ?
C67 C66 H66A 109.4 . . ?
C68 C67 C66 111.0(2) . . ?
C68 C67 H67A 109.4 . . ?
C66 C67 H67A 109.4 . . ?
C68 C67 H67B 109.4 . . ?
C66 C67 H67B 109.4 . . ?
H67A C67 H67B 108.0 . . ?
C67 C68 C69 111.8(2) . . ?
C67 C68 H68A 109.3 . . ?
C69 C68 H68A 109.3 . . ?
C67 C68 H68B 109.3 . . ?
C69 C68 H68B 109.3 . . ?
H68A C68 H68B 107.9 . . ?
C68 C69 C70 109.5(2) . . ?
C68 C69 H69A 109.8 . . ?
C70 C69 H69A 109.8 . . ?
C68 C69 H69B 109.8 . . ?
C70 C69 H69B 109.8 . . ?
H69A C69 H69B 108.2 . . ?
C69 C70 C65 111.6(2) . . ?
C69 C70 H70A 109.3 . . ?
C65 C70 H70A 109.3 . . ?
C69 C70 H70B 109.3 . . ?
C65 C70 H70B 109.3 . . ?
H70A C70 H70B 108.0 . . ?
N14 C71 C72 121.8(2) . . ?
N14 C71 H71A 119.1 . . ?
C72 C71 H71A 119.1 . . ?
C73 C72 C77 119.1(3) . . ?
C73 C72 C71 120.3(3) . . ?
C77 C72 C71 120.6(2) . . ?
C74 C73 C72 120.1(3) . . ?
C74 C73 H73A 120.0 . . ?
C72 C73 H73A 120.0 . . ?
F12 C74 C73 118.7(3) . . ?
F12 C74 C75 119.1(3) . . ?
C73 C74 C75 122.1(3) . . ?
C74 C75 C76 120.0(3) . . ?
C74 C75 H75A 120.0 . . ?
C76 C75 H75A 120.0 . . ?
C75 C76 C77 118.3(3) . . ?
C75 C76 C78 121.3(3) . . ?
C77 C76 C78 120.4(2) . . ?
O12 C77 C72 118.6(2) . . ?
O12 C77 C76 121.0(3) . . ?
C72 C77 C76 120.4(2) . . ?
N15 C78 C76 122.2(3) . . ?
N15 C78 H78A 118.9 . . ?
C76 C78 H78A 118.9 . . ?
C77 O12 H12O 105.7 . . ?
N16 C80 C81 108.7(2) . . ?
N16 C80 C79 110.2(2) . . ?
C81 C80 C79 110.4(2) . . ?
N16 C80 H80A 109.2 . . ?
C81 C80 H80A 109.2 . . ?
C79 C80 H80A 109.2 . . ?
C82 C81 C80 112.2(3) . . ?
C82 C81 H81A 109.2 . . ?
C80 C81 H81A 109.2 . . ?
C82 C81 H81B 109.2 . . ?
C80 C81 H81B 109.2 . . ?
H81A C81 H81B 107.9 . . ?
C81 C82 C83 111.4(4) . . ?
C81 C82 H82A 109.3 . . ?
C83 C82 H82A 109.3 . . ?
C81 C82 H82B 109.3 . . ?
C83 C82 H82B 109.3 . . ?
H82A C82 H82B 108.0 . . ?
C84 C83 C82 111.2(3) . . ?
C84 C83 H83A 109.4 . . ?
C82 C83 H83A 109.4 . . ?
C84 C83 H83B 109.4 . . ?
C82 C83 H83B 109.4 . . ?
H83A C83 H83B 108.0 . . ?
C83 C84 C79 111.4(3) . . ?
C83 C84 H84A 109.3 . . ?
C79 C84 H84A 109.3 . . ?
C83 C84 H84B 109.3 . . ?
C79 C84 H84B 109.3 . . ?
H84A C84 H84B 108.0 . . ?
N16 C85 C86 123.0(2) . . ?
N16 C85 H85A 118.5 . . ?
C86 C85 H85A 118.5 . . ?
C87 C86 C91 119.1(2) . . ?
C87 C86 C85 121.3(2) . . ?
C91 C86 C85 119.6(2) . . ?
C88 C87 C86 119.9(2) . . ?
C88 C87 H87A 120.1 . . ?
C86 C87 H87A 120.1 . . ?
F13 C88 C87 119.1(2) . . ?
F13 C88 C89 118.5(2) . . ?
C87 C88 C89 122.4(2) . . ?
C88 C89 C90 119.5(2) . . ?
C88 C89 H89A 120.2 . . ?
C90 C89 H89A 120.2 . . ?
C89 C90 C91 119.1(2) . . ?
C89 C90 C92 119.9(2) . . ?
C91 C90 C92 121.0(2) . . ?
O13 C91 C86 119.0(2) . . ?
O13 C91 C90 121.0(2) . . ?
C86 C91 C90 120.0(2) . . ?
N11 C92 C90 121.8(2) . . ?
N11 C92 H92A 119.1 . . ?
C90 C92 H92A 119.1 . . ?
C91 O13 H13O 107.3 . . ?

_diffrn_measured_fraction_theta_max 0.874
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.042
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3c
_database_code_depnum_ccdc_archive 'CCDC 1422959'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H45 Cl3 N6 O3'
_chemical_formula_sum            'C42 H45 Cl3 N6 O3'
_chemical_formula_weight         788.19
_chemical_absolute_configuration rm


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.6060(4)
_cell_length_b                   18.7364(5)
_cell_length_c                   14.7922(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.420(2)
_cell_angle_gamma                90.00
_cell_volume                     4044.48(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(1)
_cell_measurement_reflns_used    10919
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      28.73

_exptl_crystal_description       plate
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_min  0.9896
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro (Agilent Technologies, 2011)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      130(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_standards_number         45070
_diffrn_standards_interval_count 4
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            45026
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         28.73
_reflns_number_total             18081
_reflns_number_gt                14047
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0533P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_number_reflns         18081
_refine_ls_number_parameters     997
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1088
_refine_ls_wR_factor_gt          0.0997
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_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
N1 N 0.62599(17) 0.49916(12) 0.62519(15) 0.0248(5) Uani 1 1 d . . .
N2 N 0.57282(17) 0.46829(12) 0.43946(15) 0.0248(5) Uani 1 1 d . . .
C1 C 0.67689(19) 0.52556(15) 0.54965(18) 0.0243(6) Uani 1 1 d . . .
H1 H 0.7237 0.4904 0.5350 0.029 Uiso 1 1 calc R . .
C2 C 0.6136(2) 0.53710(14) 0.46739(19) 0.0242(6) Uani 1 1 d . . .
H2 H 0.5647 0.5702 0.4828 0.029 Uiso 1 1 calc R . .
C3 C 0.6671(2) 0.56862(16) 0.3905(2) 0.0290(7) Uani 1 1 d . . .
H3A H 0.7129 0.5346 0.3725 0.035 Uiso 1 1 calc R . .
H3B H 0.6256 0.5773 0.3387 0.035 Uiso 1 1 calc R . .
C4 C 0.7139(2) 0.63819(16) 0.4188(2) 0.0348(7) Uani 1 1 d . . .
H4A H 0.6677 0.6735 0.4320 0.042 Uiso 1 1 calc R . .
H4B H 0.7487 0.6560 0.3692 0.042 Uiso 1 1 calc R . .
C5 C 0.7778(2) 0.62787(16) 0.5021(2) 0.0352(8) Uani 1 1 d . . .
H5A H 0.8278 0.5964 0.4876 0.042 Uiso 1 1 calc R . .
H5B H 0.8036 0.6734 0.5211 0.042 Uiso 1 1 calc R . .
C6 C 0.7242(2) 0.59570(15) 0.5785(2) 0.0291(7) Uani 1 1 d . . .
H6A H 0.6783 0.6296 0.5967 0.035 Uiso 1 1 calc R . .
H6B H 0.7656 0.5868 0.6302 0.035 Uiso 1 1 calc R . .
C7 C 0.4876(2) 0.46700(15) 0.42356(18) 0.0240(6) Uani 1 1 d . . .
H7 H 0.4543 0.5088 0.4309 0.029 Uiso 1 1 calc R . .
C8 C 0.4384(2) 0.40211(14) 0.39381(17) 0.0231(6) Uani 1 1 d . . .
C9 C 0.4870(2) 0.33987(15) 0.37428(17) 0.0238(6) Uani 1 1 d . . .
H9 H 0.5508 0.3404 0.3773 0.029 Uiso 1 1 calc R . .
C10 C 0.4411(2) 0.27789(15) 0.35064(19) 0.0277(7) Uani 1 1 d . . .
C11 C 0.3473(2) 0.27604(15) 0.34643(19) 0.0270(7) Uani 1 1 d . . .
H11 H 0.3173 0.2337 0.3309 0.032 Uiso 1 1 calc R . .
C12 C 0.2965(2) 0.33608(14) 0.36487(19) 0.0247(6) Uani 1 1 d . . .
C13 C 0.3430(2) 0.40061(15) 0.38806(18) 0.0243(6) Uani 1 1 d . . .
C14 C 0.1972(2) 0.33260(16) 0.36160(19) 0.0288(7) Uani 1 1 d . . .
H14 H 0.1696 0.2885 0.3507 0.035 Uiso 1 1 calc R . .
Cl1 Cl 0.50275(6) 0.20092(4) 0.32709(5) 0.03381(18) Uani 1 1 d . . .
O1 O 0.29548(16) 0.46061(11) 0.40374(14) 0.0319(5) Uani 1 1 d . . .
H1O H 0.237(2) 0.4482(18) 0.398(2) 0.040(10) Uiso 1 1 d . . .
N3 N 0.14527(17) 0.38673(14) 0.37285(15) 0.0288(6) Uani 1 1 d . . .
N4 N 0.03375(17) 0.34301(13) 0.52036(16) 0.0294(6) Uani 1 1 d . . .
C15 C 0.04595(19) 0.37678(16) 0.36294(19) 0.0272(6) Uani 1 1 d . . .
H15 H 0.0337 0.3268 0.3472 0.033 Uiso 1 1 calc R . .
C16 C 0.0006(2) 0.39316(16) 0.45122(19) 0.0276(7) Uani 1 1 d . . .
H16 H 0.0155 0.4420 0.4703 0.033 Uiso 1 1 calc R . .
C17 C -0.1041(2) 0.38495(18) 0.4376(2) 0.0344(7) Uani 1 1 d . . .
H17A H -0.1188 0.3352 0.4258 0.041 Uiso 1 1 calc R . .
H17B H -0.1331 0.3989 0.4926 0.041 Uiso 1 1 calc R . .
C18 C -0.1420(2) 0.43024(16) 0.3595(2) 0.0350(8) Uani 1 1 d . . .
H18A H -0.2072 0.4212 0.3508 0.042 Uiso 1 1 calc R . .
H18B H -0.1340 0.4803 0.3747 0.042 Uiso 1 1 calc R . .
C19 C -0.0961(2) 0.41502(18) 0.2735(2) 0.0398(8) Uani 1 1 d . . .
H19A H -0.1189 0.4476 0.2268 0.048 Uiso 1 1 calc R . .
H19B H -0.1105 0.3668 0.2538 0.048 Uiso 1 1 calc R . .
C20 C 0.0080(2) 0.42333(17) 0.2863(2) 0.0336(7) Uani 1 1 d . . .
H20A H 0.0367 0.4103 0.2307 0.040 Uiso 1 1 calc R . .
H20B H 0.0227 0.4729 0.2993 0.040 Uiso 1 1 calc R . .
C21 C 0.06179(19) 0.36825(15) 0.59595(19) 0.0255(6) Uani 1 1 d . . .
H21 H 0.0648 0.4175 0.6032 0.031 Uiso 1 1 calc R . .
C22 C 0.08963(19) 0.32224(15) 0.67218(19) 0.0246(6) Uani 1 1 d . . .
C23 C 0.0817(2) 0.24914(15) 0.6670(2) 0.0265(6) Uani 1 1 d . . .
H23 H 0.0600 0.2283 0.6132 0.032 Uiso 1 1 calc R . .
C24 C 0.10527(19) 0.20621(15) 0.73979(19) 0.0262(6) Uani 1 1 d . . .
C25 C 0.13965(19) 0.23512(15) 0.81917(19) 0.0256(6) Uani 1 1 d . . .
H25 H 0.1568 0.2054 0.8673 0.031 Uiso 1 1 calc R . .
C26 C 0.14915(19) 0.30880(15) 0.82832(19) 0.0230(6) Uani 1 1 d . . .
C27 C 0.12215(19) 0.35314(15) 0.75414(19) 0.0239(6) Uani 1 1 d . . .
C28 C 0.18377(19) 0.33883(15) 0.91322(19) 0.0238(6) Uani 1 1 d . . .
H28 H 0.2059 0.3082 0.9585 0.029 Uiso 1 1 calc R . .
Cl2 Cl 0.08813(6) 0.11383(4) 0.73048(5) 0.03572(19) Uani 1 1 d . . .
O2 O 0.12697(14) 0.42469(10) 0.76129(14) 0.0294(5) Uani 1 1 d . . .
H2O H 0.140(3) 0.444(2) 0.823(3) 0.089(15) Uiso 1 1 d . . .
N5 N 0.18495(17) 0.40631(13) 0.92826(15) 0.0265(6) Uani 1 1 d . . .
N6 N 0.37842(16) 0.43413(13) 0.96567(16) 0.0269(5) Uani 1 1 d . . .
C29 C 0.2210(2) 0.43327(15) 1.01560(18) 0.0261(6) Uani 1 1 d . . .
H29 H 0.2381 0.3926 1.0544 0.031 Uiso 1 1 calc R . .
C30 C 0.3065(2) 0.47889(15) 1.00182(19) 0.0267(7) Uani 1 1 d . . .
H30 H 0.2911 0.5171 0.9585 0.032 Uiso 1 1 calc R . .
C31 C 0.3417(2) 0.51192(17) 1.0909(2) 0.0348(7) Uani 1 1 d . . .
H31A H 0.3933 0.5429 1.0797 0.042 Uiso 1 1 calc R . .
H31B H 0.3631 0.4744 1.1317 0.042 Uiso 1 1 calc R . .
C32 C 0.2669(2) 0.55507(18) 1.1356(2) 0.0397(8) Uani 1 1 d . . .
H32A H 0.2903 0.5729 1.1937 0.048 Uiso 1 1 calc R . .
H32B H 0.2502 0.5957 1.0978 0.048 Uiso 1 1 calc R . .
C33 C 0.1829(2) 0.50943(18) 1.1493(2) 0.0377(8) Uani 1 1 d . . .
H33A H 0.1353 0.5386 1.1742 0.045 Uiso 1 1 calc R . .
H33B H 0.1983 0.4718 1.1924 0.045 Uiso 1 1 calc R . .
C34 C 0.1470(2) 0.47625(17) 1.0607(2) 0.0326(7) Uani 1 1 d . . .
H34A H 0.1252 0.5137 1.0199 0.039 Uiso 1 1 calc R . .
H34B H 0.0956 0.4453 1.0724 0.039 Uiso 1 1 calc R . .
C35 C 0.4145(2) 0.45579(15) 0.89436(18) 0.0255(6) Uani 1 1 d . . .
H35 H 0.3927 0.4977 0.8674 0.031 Uiso 1 1 calc R . .
C36 C 0.4892(2) 0.41734(14) 0.85267(18) 0.0243(6) Uani 1 1 d . . .
C37 C 0.5220(2) 0.35283(15) 0.88814(19) 0.0261(6) Uani 1 1 d . . .
H37 H 0.4960 0.3336 0.9391 0.031 Uiso 1 1 calc R . .
C38 C 0.5927(2) 0.31713(14) 0.8483(2) 0.0273(7) Uani 1 1 d . . .
C39 C 0.6323(2) 0.34441(15) 0.77441(19) 0.0254(6) Uani 1 1 d . . .
H39 H 0.6799 0.3197 0.7485 0.030 Uiso 1 1 calc R . .
C40 C 0.6021(2) 0.40976(15) 0.73655(18) 0.0230(6) Uani 1 1 d . . .
C41 C 0.53008(19) 0.44569(15) 0.77670(18) 0.0241(6) Uani 1 1 d . . .
C42 C 0.6465(2) 0.43830(15) 0.65860(19) 0.0256(6) Uani 1 1 d . . .
H42 H 0.6916 0.4113 0.6321 0.031 Uiso 1 1 calc R . .
Cl3 Cl 0.63187(6) 0.23564(4) 0.89205(5) 0.03703(19) Uani 1 1 d . . .
O3 O 0.49900(14) 0.50896(10) 0.74336(14) 0.0280(5) Uani 1 1 d . . .
H3O H 0.536(2) 0.5166(17) 0.692(2) 0.038(9) Uiso 1 1 d . . .
N11 N 0.81743(16) 0.20170(12) 0.58856(15) 0.0267(5) Uani 1 1 d . . .
N12 N 0.63207(16) 0.15765(12) 0.55549(14) 0.0238(5) Uani 1 1 d . . .
C51 C 0.7942(2) 0.13682(14) 0.53801(18) 0.0261(7) Uani 1 1 d . . .
H51 H 0.7900 0.0967 0.5801 0.031 Uiso 1 1 calc R . .
C52 C 0.7017(2) 0.14788(15) 0.48827(18) 0.0263(6) Uani 1 1 d . . .
H52 H 0.7045 0.1911 0.4512 0.032 Uiso 1 1 calc R . .
C53 C 0.6774(2) 0.08469(15) 0.42716(19) 0.0278(7) Uani 1 1 d . . .
H53A H 0.6708 0.0422 0.4637 0.033 Uiso 1 1 calc R . .
H53B H 0.6194 0.0937 0.3949 0.033 Uiso 1 1 calc R . .
C54 C 0.7513(2) 0.07247(16) 0.3597(2) 0.0352(8) Uani 1 1 d . . .
H54A H 0.7354 0.0314 0.3222 0.042 Uiso 1 1 calc R . .
H54B H 0.7554 0.1138 0.3205 0.042 Uiso 1 1 calc R . .
C55 C 0.8431(2) 0.05983(17) 0.4087(2) 0.0366(8) Uani 1 1 d . . .
H55A H 0.8900 0.0541 0.3647 0.044 Uiso 1 1 calc R . .
H55B H 0.8404 0.0162 0.4437 0.044 Uiso 1 1 calc R . .
C56 C 0.8685(2) 0.12152(17) 0.4712(2) 0.0342(7) Uani 1 1 d . . .
H56A H 0.8785 0.1639 0.4352 0.041 Uiso 1 1 calc R . .
H56B H 0.9254 0.1105 0.5044 0.041 Uiso 1 1 calc R . .
C57 C 0.58636(19) 0.21600(15) 0.55623(18) 0.0236(6) Uani 1 1 d . . .
H57 H 0.5979 0.2507 0.5132 0.028 Uiso 1 1 calc R . .
C58 C 0.51721(19) 0.23014(14) 0.62173(18) 0.0223(6) Uani 1 1 d . . .
C59 C 0.4641(2) 0.29180(15) 0.61322(19) 0.0257(6) Uani 1 1 d . . .
H59 H 0.4738 0.3239 0.5667 0.031 Uiso 1 1 calc R . .
C60 C 0.3966(2) 0.30505(14) 0.67436(19) 0.0257(6) Uani 1 1 d . . .
C61 C 0.3820(2) 0.25820(14) 0.74382(18) 0.0230(6) Uani 1 1 d . . .
H61 H 0.3367 0.2680 0.7844 0.028 Uiso 1 1 calc R . .
C62 C 0.43391(19) 0.19648(15) 0.75428(17) 0.0216(6) Uani 1 1 d . . .
C63 C 0.50209(19) 0.18212(14) 0.69265(18) 0.0222(6) Uani 1 1 d . . .
C64 C 0.4165(2) 0.14439(14) 0.82610(17) 0.0223(6) Uani 1 1 d . . .
H64 H 0.4578 0.1070 0.8353 0.027 Uiso 1 1 calc R . .
Cl11 Cl 0.33061(5) 0.38200(4) 0.66154(5) 0.03437(18) Uani 1 1 d . . .
O11 O 0.55062(15) 0.12120(11) 0.70195(14) 0.0260(5) Uani 1 1 d . . .
H11O H 0.584(2) 0.122(2) 0.664(2) 0.044(12) Uiso 1 1 d . . .
N13 N 0.34805(16) 0.14795(12) 0.87611(15) 0.0241(5) Uani 1 1 d . . .
N14 N 0.42293(16) 0.15299(12) 1.06012(14) 0.0225(5) Uani 1 1 d . . .
C65 C 0.33780(19) 0.08904(14) 0.94072(18) 0.0218(6) Uani 1 1 d . . .
H65 H 0.3904 0.0568 0.9370 0.026 Uiso 1 1 calc R . .
C66 C 0.33537(18) 0.11847(15) 1.03650(17) 0.0220(6) Uani 1 1 d . . .
H66 H 0.2853 0.1530 1.0404 0.026 Uiso 1 1 calc R . .
C67 C 0.3223(2) 0.05749(16) 1.10363(19) 0.0293(7) Uani 1 1 d . . .
H67A H 0.3760 0.0270 1.1045 0.035 Uiso 1 1 calc R . .
H67B H 0.3173 0.0773 1.1638 0.035 Uiso 1 1 calc R . .
C68 C 0.2374(2) 0.01244(17) 1.0806(2) 0.0330(7) Uani 1 1 d . . .
H68A H 0.2357 -0.0279 1.1216 0.040 Uiso 1 1 calc R . .
H68B H 0.1828 0.0408 1.0884 0.040 Uiso 1 1 calc R . .
C69 C 0.2388(2) -0.01424(16) 0.9835(2) 0.0344(8) Uani 1 1 d . . .
H69A H 0.1820 -0.0392 0.9683 0.041 Uiso 1 1 calc R . .
H69B H 0.2889 -0.0477 0.9780 0.041 Uiso 1 1 calc R . .
C70 C 0.2502(2) 0.04735(15) 0.9173(2) 0.0291(7) Uani 1 1 d . . .
H70A H 0.2525 0.0287 0.8562 0.035 Uiso 1 1 calc R . .
H70B H 0.1978 0.0790 0.9195 0.035 Uiso 1 1 calc R . .
C71 C 0.42503(19) 0.21827(15) 1.08279(17) 0.0224(6) Uani 1 1 d . . .
H71 H 0.3706 0.2441 1.0822 0.027 Uiso 1 1 calc R . .
C72 C 0.5107(2) 0.25390(14) 1.10974(18) 0.0222(6) Uani 1 1 d . . .
C73 C 0.5095(2) 0.32487(15) 1.13661(18) 0.0241(6) Uani 1 1 d . . .
H73 H 0.4544 0.3498 1.1366 0.029 Uiso 1 1 calc R . .
C74 C 0.5902(2) 0.35812(15) 1.16326(18) 0.0266(7) Uani 1 1 d . . .
C75 C 0.6730(2) 0.32246(15) 1.16261(18) 0.0252(6) Uani 1 1 d . . .
H75 H 0.7268 0.3461 1.1805 0.030 Uiso 1 1 calc R . .
C76 C 0.6765(2) 0.25140(15) 1.13527(18) 0.0245(6) Uani 1 1 d . . .
C77 C 0.5947(2) 0.21662(14) 1.10962(18) 0.0241(6) Uani 1 1 d . . .
C78 C 0.7640(2) 0.21338(16) 1.13201(18) 0.0255(6) Uani 1 1 d . . .
H78 H 0.7635 0.1659 1.1136 0.031 Uiso 1 1 calc R . .
Cl12 Cl 0.58719(6) 0.44560(4) 1.20284(5) 0.03605(19) Uani 1 1 d . . .
O12 O 0.59828(15) 0.14728(10) 1.08558(14) 0.0292(5) Uani 1 1 d . . .
H12O H 0.536(3) 0.130(2) 1.067(2) 0.064(12) Uiso 1 1 d . . .
N15 N 0.84012(16) 0.24225(13) 1.15309(16) 0.0261(5) Uani 1 1 d . . .
N16 N 0.95829(16) 0.24157(13) 1.00096(16) 0.0274(5) Uani 1 1 d . . .
C79 C 0.92211(19) 0.19806(16) 1.14986(19) 0.0268(6) Uani 1 1 d . . .
H79 H 0.9063 0.1520 1.1220 0.032 Uiso 1 1 calc R . .
C80 C 0.9933(2) 0.23555(16) 1.09462(19) 0.0274(7) Uani 1 1 d . . .
H80 H 1.0050 0.2833 1.1194 0.033 Uiso 1 1 calc R . .
C81 C 1.0830(2) 0.1932(2) 1.0959(2) 0.0393(8) Uani 1 1 d . . .
H81A H 1.0723 0.1473 1.0671 0.047 Uiso 1 1 calc R . .
H81B H 1.1278 0.2188 1.0617 0.047 Uiso 1 1 calc R . .
C82 C 1.1203(2) 0.1820(2) 1.1914(2) 0.0521(10) Uani 1 1 d . . .
H82A H 1.1374 0.2277 1.2178 0.063 Uiso 1 1 calc R . .
H82B H 1.1749 0.1526 1.1904 0.063 Uiso 1 1 calc R . .
C83 C 1.0505(3) 0.1463(2) 1.2493(2) 0.0492(10) Uani 1 1 d . . .
H83A H 1.0401 0.0978 1.2281 0.059 Uiso 1 1 calc R . .
H83B H 1.0746 0.1439 1.3114 0.059 Uiso 1 1 calc R . .
C84 C 0.9602(2) 0.18618(18) 1.2464(2) 0.0357(8) Uani 1 1 d . . .
H84A H 0.9690 0.2321 1.2759 0.043 Uiso 1 1 calc R . .
H84B H 0.9160 0.1594 1.2798 0.043 Uiso 1 1 calc R . .
C85 C 0.9481(2) 0.30278(16) 0.9649(2) 0.0270(7) Uani 1 1 d . . .
H85 H 0.9617 0.3433 0.9991 0.032 Uiso 1 1 calc R . .
C86 C 0.91545(19) 0.31070(15) 0.87100(18) 0.0227(6) Uani 1 1 d . . .
C87 C 0.91183(19) 0.37800(15) 0.83101(19) 0.0259(6) Uani 1 1 d . . .
H87 H 0.9278 0.4182 0.8649 0.031 Uiso 1 1 calc R . .
C88 C 0.8847(2) 0.38480(15) 0.7419(2) 0.0256(6) Uani 1 1 d . . .
C89 C 0.8608(2) 0.32614(15) 0.69007(19) 0.0247(6) Uani 1 1 d . . .
H89 H 0.8431 0.3320 0.6294 0.030 Uiso 1 1 calc R . .
C90 C 0.86287(19) 0.25815(14) 0.72777(19) 0.0224(6) Uani 1 1 d . . .
C91 C 0.89093(19) 0.25038(14) 0.81832(19) 0.0235(6) Uani 1 1 d . . .
C92 C 0.83802(18) 0.19570(15) 0.67207(18) 0.0240(6) Uani 1 1 d . . .
H92 H 0.8374 0.1508 0.6988 0.029 Uiso 1 1 calc R . .
Cl13 Cl 0.88322(6) 0.46946(4) 0.69245(5) 0.03716(19) Uani 1 1 d . . .
O13 O 0.89551(14) 0.18411(10) 0.85328(14) 0.0297(5) Uani 1 1 d . . .
H13O H 0.925(2) 0.1908(19) 0.917(3) 0.060(11) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C42 1.273(3) . ?
N1 C1 1.455(4) . ?
N2 C7 1.258(4) . ?
N2 C2 1.472(3) . ?
C1 C2 1.512(4) . ?
C1 C6 1.536(4) . ?
C1 H1 0.9800 . ?
C2 C3 1.526(4) . ?
C2 H2 0.9800 . ?
C3 C4 1.522(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.527(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.525(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.470(4) . ?
C7 H7 0.9300 . ?
C8 C13 1.393(4) . ?
C8 C9 1.402(4) . ?
C9 C10 1.379(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.370(4) . ?
C10 Cl1 1.743(3) . ?
C11 C12 1.381(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.422(4) . ?
C12 C14 1.451(4) . ?
C13 O1 1.346(3) . ?
C14 N3 1.281(4) . ?
C14 H14 0.9300 . ?
O1 H1O 0.89(4) . ?
N3 C15 1.464(4) . ?
N4 C21 1.266(4) . ?
N4 C16 1.456(4) . ?
C15 C20 1.517(4) . ?
C15 C16 1.520(4) . ?
C15 H15 0.9800 . ?
C16 C17 1.542(4) . ?
C16 H16 0.9800 . ?
C17 C18 1.519(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.492(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.532(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.463(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.376(4) . ?
C22 C27 1.408(4) . ?
C23 C24 1.376(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.369(4) . ?
C24 Cl2 1.753(3) . ?
C25 C26 1.393(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.419(4) . ?
C26 C28 1.448(4) . ?
C27 O2 1.346(3) . ?
C28 N5 1.284(4) . ?
C28 H28 0.9300 . ?
O2 H2O 0.99(5) . ?
N5 C29 1.464(4) . ?
N6 C35 1.265(3) . ?
N6 C30 1.463(4) . ?
C29 C34 1.524(4) . ?
C29 C30 1.534(4) . ?
C29 H29 0.9800 . ?
C30 C31 1.526(4) . ?
C30 H30 0.9800 . ?
C31 C32 1.531(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.516(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.524(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.465(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.394(4) . ?
C36 C41 1.399(4) . ?
C37 C38 1.384(4) . ?
C37 H37 0.9300 . ?
C38 C39 1.358(4) . ?
C38 Cl3 1.745(3) . ?
C39 C40 1.410(4) . ?
C39 H39 0.9300 . ?
C40 C41 1.402(4) . ?
C40 C42 1.449(4) . ?
C41 O3 1.355(3) . ?
C42 H42 0.9300 . ?
O3 H3O 0.96(3) . ?
N11 C92 1.264(3) . ?
N11 C51 1.460(3) . ?
N12 C57 1.281(3) . ?
N12 C52 1.463(4) . ?
C51 C52 1.525(4) . ?
C51 C56 1.526(4) . ?
C51 H51 0.9800 . ?
C52 C53 1.522(4) . ?
C52 H52 0.9800 . ?
C53 C54 1.519(4) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.515(5) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.516(4) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 C58 1.453(4) . ?
C57 H57 0.9300 . ?
C58 C59 1.395(4) . ?
C58 C63 1.407(4) . ?
C59 C60 1.387(4) . ?
C59 H59 0.9300 . ?
C60 C61 1.375(4) . ?
C60 Cl11 1.740(3) . ?
C61 C62 1.388(4) . ?
C61 H61 0.9300 . ?
C62 C63 1.404(4) . ?
C62 C64 1.472(4) . ?
C63 O11 1.348(3) . ?
C64 N13 1.271(3) . ?
C64 H64 0.9300 . ?
O11 H11O 0.76(3) . ?
N13 C65 1.472(3) . ?
N14 C71 1.268(3) . ?
N14 C66 1.462(3) . ?
C65 C66 1.522(4) . ?
C65 C70 1.527(4) . ?
C65 H65 0.9800 . ?
C66 C67 1.531(4) . ?
C66 H66 0.9800 . ?
C67 C68 1.526(4) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C68 C69 1.522(4) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C69 C70 1.527(4) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C71 C72 1.459(4) . ?
C71 H71 0.9300 . ?
C72 C73 1.388(4) . ?
C72 C77 1.412(4) . ?
C73 C74 1.376(4) . ?
C73 H73 0.9300 . ?
C74 C75 1.383(4) . ?
C74 Cl12 1.742(3) . ?
C75 C76 1.393(4) . ?
C75 H75 0.9300 . ?
C76 C77 1.400(4) . ?
C76 C78 1.466(4) . ?
C77 O12 1.349(3) . ?
C78 N15 1.263(3) . ?
C78 H78 0.9300 . ?
O12 H12O 0.99(4) . ?
N15 C79 1.458(4) . ?
N16 C85 1.271(4) . ?
N16 C80 1.461(4) . ?
C79 C80 1.521(4) . ?
C79 C84 1.527(4) . ?
C79 H79 0.9800 . ?
C80 C81 1.531(4) . ?
C80 H80 0.9800 . ?
C81 C82 1.507(5) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C82 C83 1.516(5) . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C83 C84 1.514(5) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C84 H84A 0.9700 . ?
C84 H84B 0.9700 . ?
C85 C86 1.457(4) . ?
C85 H85 0.9300 . ?
C86 C87 1.393(4) . ?
C86 C91 1.410(4) . ?
C87 C88 1.367(4) . ?
C87 H87 0.9300 . ?
C88 C89 1.376(4) . ?
C88 Cl13 1.746(3) . ?
C89 C90 1.391(4) . ?
C89 H89 0.9300 . ?
C90 C91 1.392(4) . ?
C90 C92 1.468(4) . ?
C91 O13 1.346(3) . ?
C92 H92 0.9300 . ?
O13 H13O 1.03(4) . ?

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
C42 N1 C1 118.9(2) . . ?
C7 N2 C2 117.1(2) . . ?
N1 C1 C2 110.6(2) . . ?
N1 C1 C6 108.4(2) . . ?
C2 C1 C6 110.7(2) . . ?
N1 C1 H1 109.0 . . ?
C2 C1 H1 109.0 . . ?
C6 C1 H1 109.0 . . ?
N2 C2 C1 109.1(2) . . ?
N2 C2 C3 110.1(2) . . ?
C1 C2 C3 109.9(2) . . ?
N2 C2 H2 109.3 . . ?
C1 C2 H2 109.3 . . ?
C3 C2 H2 109.3 . . ?
C4 C3 C2 111.4(2) . . ?
C4 C3 H3A 109.4 . . ?
C2 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C3 C4 C5 111.5(2) . . ?
C3 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
C6 C5 C4 109.4(3) . . ?
C6 C5 H5A 109.8 . . ?
C4 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
C4 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
C5 C6 C1 111.8(2) . . ?
C5 C6 H6A 109.3 . . ?
C1 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
C1 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 C8 122.6(3) . . ?
N2 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C13 C8 C9 119.0(3) . . ?
C13 C8 C7 120.6(3) . . ?
C9 C8 C7 120.3(3) . . ?
C10 C9 C8 120.5(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 120.5(3) . . ?
C11 C10 Cl1 119.6(2) . . ?
C9 C10 Cl1 119.9(2) . . ?
C10 C11 C12 121.0(3) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C13 119.0(3) . . ?
C11 C12 C14 120.1(3) . . ?
C13 C12 C14 120.9(3) . . ?
O1 C13 C8 119.6(3) . . ?
O1 C13 C12 120.5(3) . . ?
C8 C13 C12 119.9(3) . . ?
N3 C14 C12 123.8(3) . . ?
N3 C14 H14 118.1 . . ?
C12 C14 H14 118.1 . . ?
C13 O1 H1O 106(2) . . ?
C14 N3 C15 118.4(3) . . ?
C21 N4 C16 117.7(2) . . ?
N3 C15 C20 109.3(2) . . ?
N3 C15 C16 110.7(2) . . ?
C20 C15 C16 111.6(3) . . ?
N3 C15 H15 108.4 . . ?
C20 C15 H15 108.4 . . ?
C16 C15 H15 108.4 . . ?
N4 C16 C15 109.2(2) . . ?
N4 C16 C17 109.0(2) . . ?
C15 C16 C17 109.4(2) . . ?
N4 C16 H16 109.7 . . ?
C15 C16 H16 109.7 . . ?
C17 C16 H16 109.7 . . ?
C18 C17 C16 111.8(3) . . ?
C18 C17 H17A 109.3 . . ?
C16 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 107.9 . . ?
C19 C18 C17 112.3(3) . . ?
C19 C18 H18A 109.1 . . ?
C17 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
C17 C18 H18B 109.1 . . ?
H18A C18 H18B 107.9 . . ?
C18 C19 C20 110.8(3) . . ?
C18 C19 H19A 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C15 C20 C19 111.3(3) . . ?
C15 C20 H20A 109.4 . . ?
C19 C20 H20A 109.4 . . ?
C15 C20 H20B 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
N4 C21 C22 122.0(3) . . ?
N4 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
C23 C22 C27 118.8(3) . . ?
C23 C22 C21 121.6(3) . . ?
C27 C22 C21 119.6(3) . . ?
C24 C23 C22 121.4(3) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C25 C24 C23 120.7(3) . . ?
C25 C24 Cl2 120.3(2) . . ?
C23 C24 Cl2 119.1(2) . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C27 118.8(3) . . ?
C25 C26 C28 119.9(3) . . ?
C27 C26 C28 121.3(3) . . ?
O2 C27 C22 119.5(3) . . ?
O2 C27 C26 120.7(3) . . ?
C22 C27 C26 119.9(3) . . ?
N5 C28 C26 122.3(3) . . ?
N5 C28 H28 118.8 . . ?
C26 C28 H28 118.8 . . ?
C27 O2 H2O 116(3) . . ?
C28 N5 C29 119.6(2) . . ?
C35 N6 C30 116.8(2) . . ?
N5 C29 C34 109.4(2) . . ?
N5 C29 C30 109.9(2) . . ?
C34 C29 C30 111.1(2) . . ?
N5 C29 H29 108.8 . . ?
C34 C29 H29 108.8 . . ?
C30 C29 H29 108.8 . . ?
N6 C30 C31 109.1(2) . . ?
N6 C30 C29 109.3(2) . . ?
C31 C30 C29 111.0(2) . . ?
N6 C30 H30 109.2 . . ?
C31 C30 H30 109.2 . . ?
C29 C30 H30 109.2 . . ?
C30 C31 C32 111.5(3) . . ?
C30 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
C33 C32 C31 110.9(3) . . ?
C33 C32 H32A 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
C32 C33 C34 111.5(3) . . ?
C32 C33 H33A 109.3 . . ?
C34 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
C34 C33 H33B 109.3 . . ?
H33A C33 H33B 108.0 . . ?
C33 C34 C29 111.5(3) . . ?
C33 C34 H34A 109.3 . . ?
C29 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
C29 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
N6 C35 C36 122.5(3) . . ?
N6 C35 H35 118.8 . . ?
C36 C35 H35 118.8 . . ?
C37 C36 C41 118.7(3) . . ?
C37 C36 C35 121.2(3) . . ?
C41 C36 C35 120.1(3) . . ?
C38 C37 C36 120.6(3) . . ?
C38 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
C39 C38 C37 120.8(3) . . ?
C39 C38 Cl3 118.9(2) . . ?
C37 C38 Cl3 120.2(2) . . ?
C38 C39 C40 120.6(3) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
C41 C40 C39 118.5(3) . . ?
C41 C40 C42 121.9(3) . . ?
C39 C40 C42 119.5(3) . . ?
O3 C41 C36 118.5(3) . . ?
O3 C41 C40 120.8(2) . . ?
C36 C41 C40 120.7(3) . . ?
N1 C42 C40 122.2(3) . . ?
N1 C42 H42 118.9 . . ?
C40 C42 H42 118.9 . . ?
C41 O3 H3O 103.0(19) . . ?
C92 N11 C51 117.9(2) . . ?
C57 N12 C52 119.3(2) . . ?
N11 C51 C52 108.4(2) . . ?
N11 C51 C56 109.4(2) . . ?
C52 C51 C56 110.7(2) . . ?
N11 C51 H51 109.4 . . ?
C52 C51 H51 109.4 . . ?
C56 C51 H51 109.4 . . ?
N12 C52 C53 110.5(2) . . ?
N12 C52 C51 108.4(2) . . ?
C53 C52 C51 111.1(2) . . ?
N12 C52 H52 108.9 . . ?
C53 C52 H52 108.9 . . ?
C51 C52 H52 108.9 . . ?
C54 C53 C52 110.7(2) . . ?
C54 C53 H53A 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C54 C53 H53B 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 108.1 . . ?
C55 C54 C53 110.4(3) . . ?
C55 C54 H54A 109.6 . . ?
C53 C54 H54A 109.6 . . ?
C55 C54 H54B 109.6 . . ?
C53 C54 H54B 109.6 . . ?
H54A C54 H54B 108.1 . . ?
C54 C55 C56 111.2(3) . . ?
C54 C55 H55A 109.4 . . ?
C56 C55 H55A 109.4 . . ?
C54 C55 H55B 109.4 . . ?
C56 C55 H55B 109.4 . . ?
H55A C55 H55B 108.0 . . ?
C55 C56 C51 112.1(3) . . ?
C55 C56 H56A 109.2 . . ?
C51 C56 H56A 109.2 . . ?
C55 C56 H56B 109.2 . . ?
C51 C56 H56B 109.2 . . ?
H56A C56 H56B 107.9 . . ?
N12 C57 C58 122.6(2) . . ?
N12 C57 H57 118.7 . . ?
C58 C57 H57 118.7 . . ?
C59 C58 C63 119.5(3) . . ?
C59 C58 C57 119.4(2) . . ?
C63 C58 C57 121.1(2) . . ?
C60 C59 C58 119.8(3) . . ?
C60 C59 H59 120.1 . . ?
C58 C59 H59 120.1 . . ?
C61 C60 C59 120.7(3) . . ?
C61 C60 Cl11 120.5(2) . . ?
C59 C60 Cl11 118.8(2) . . ?
C60 C61 C62 120.9(3) . . ?
C60 C61 H61 119.5 . . ?
C62 C61 H61 119.5 . . ?
C61 C62 C63 119.1(2) . . ?
C61 C62 C64 121.5(2) . . ?
C63 C62 C64 119.3(2) . . ?
O11 C63 C62 118.7(2) . . ?
O11 C63 C58 121.3(3) . . ?
C62 C63 C58 120.0(2) . . ?
N13 C64 C62 123.3(3) . . ?
N13 C64 H64 118.3 . . ?
C62 C64 H64 118.3 . . ?
C63 O11 H11O 105(3) . . ?
C64 N13 C65 116.3(2) . . ?
C71 N14 C66 120.1(2) . . ?
N13 C65 C66 109.9(2) . . ?
N13 C65 C70 110.1(2) . . ?
C66 C65 C70 110.2(2) . . ?
N13 C65 H65 108.9 . . ?
C66 C65 H65 108.9 . . ?
C70 C65 H65 108.9 . . ?
N14 C66 C65 109.2(2) . . ?
N14 C66 C67 107.9(2) . . ?
C65 C66 C67 110.0(2) . . ?
N14 C66 H66 109.9 . . ?
C65 C66 H66 109.9 . . ?
C67 C66 H66 109.9 . . ?
C68 C67 C66 113.0(2) . . ?
C68 C67 H67A 109.0 . . ?
C66 C67 H67A 109.0 . . ?
C68 C67 H67B 109.0 . . ?
C66 C67 H67B 109.0 . . ?
H67A C67 H67B 107.8 . . ?
C69 C68 C67 110.4(2) . . ?
C69 C68 H68A 109.6 . . ?
C67 C68 H68A 109.6 . . ?
C69 C68 H68B 109.6 . . ?
C67 C68 H68B 109.6 . . ?
H68A C68 H68B 108.1 . . ?
C68 C69 C70 111.3(2) . . ?
C68 C69 H69A 109.4 . . ?
C70 C69 H69A 109.4 . . ?
C68 C69 H69B 109.4 . . ?
C70 C69 H69B 109.4 . . ?
H69A C69 H69B 108.0 . . ?
C65 C70 C69 110.7(2) . . ?
C65 C70 H70A 109.5 . . ?
C69 C70 H70A 109.5 . . ?
C65 C70 H70B 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 108.1 . . ?
N14 C71 C72 121.6(3) . . ?
N14 C71 H71 119.2 . . ?
C72 C71 H71 119.2 . . ?
C73 C72 C77 119.7(3) . . ?
C73 C72 C71 119.7(3) . . ?
C77 C72 C71 120.6(2) . . ?
C74 C73 C72 119.6(3) . . ?
C74 C73 H73 120.2 . . ?
C72 C73 H73 120.2 . . ?
C73 C74 C75 121.2(3) . . ?
C73 C74 Cl12 119.3(2) . . ?
C75 C74 Cl12 119.4(2) . . ?
C74 C75 C76 120.4(3) . . ?
C74 C75 H75 119.8 . . ?
C76 C75 H75 119.8 . . ?
C75 C76 C77 118.8(3) . . ?
C75 C76 C78 121.1(3) . . ?
C77 C76 C78 120.0(3) . . ?
O12 C77 C76 118.5(3) . . ?
O12 C77 C72 121.4(3) . . ?
C76 C77 C72 120.1(3) . . ?
N15 C78 C76 122.9(3) . . ?
N15 C78 H78 118.6 . . ?
C76 C78 H78 118.6 . . ?
C77 O12 H12O 110(2) . . ?
C78 N15 C79 117.6(2) . . ?
C85 N16 C80 119.9(3) . . ?
N15 C79 C80 109.7(2) . . ?
N15 C79 C84 108.6(2) . . ?
C80 C79 C84 109.8(2) . . ?
N15 C79 H79 109.6 . . ?
C80 C79 H79 109.6 . . ?
C84 C79 H79 109.6 . . ?
N16 C80 C79 109.0(2) . . ?
N16 C80 C81 108.5(2) . . ?
C79 C80 C81 111.0(3) . . ?
N16 C80 H80 109.5 . . ?
C79 C80 H80 109.5 . . ?
C81 C80 H80 109.5 . . ?
C82 C81 C80 111.0(3) . . ?
C82 C81 H81A 109.4 . . ?
C80 C81 H81A 109.4 . . ?
C82 C81 H81B 109.4 . . ?
C80 C81 H81B 109.4 . . ?
H81A C81 H81B 108.0 . . ?
C81 C82 C83 111.5(3) . . ?
C81 C82 H82A 109.3 . . ?
C83 C82 H82A 109.3 . . ?
C81 C82 H82B 109.3 . . ?
C83 C82 H82B 109.3 . . ?
H82A C82 H82B 108.0 . . ?
C84 C83 C82 111.8(3) . . ?
C84 C83 H83A 109.3 . . ?
C82 C83 H83A 109.3 . . ?
C84 C83 H83B 109.3 . . ?
C82 C83 H83B 109.3 . . ?
H83A C83 H83B 107.9 . . ?
C83 C84 C79 112.4(3) . . ?
C83 C84 H84A 109.1 . . ?
C79 C84 H84A 109.1 . . ?
C83 C84 H84B 109.1 . . ?
C79 C84 H84B 109.1 . . ?
H84A C84 H84B 107.9 . . ?
N16 C85 C86 121.3(3) . . ?
N16 C85 H85 119.3 . . ?
C86 C85 H85 119.3 . . ?
C87 C86 C91 119.1(3) . . ?
C87 C86 C85 120.1(3) . . ?
C91 C86 C85 120.7(3) . . ?
C88 C87 C86 119.9(3) . . ?
C88 C87 H87 120.1 . . ?
C86 C87 H87 120.1 . . ?
C87 C88 C89 121.3(3) . . ?
C87 C88 Cl13 119.1(2) . . ?
C89 C88 Cl13 119.6(2) . . ?
C88 C89 C90 120.5(3) . . ?
C88 C89 H89 119.7 . . ?
C90 C89 H89 119.7 . . ?
C89 C90 C91 118.8(3) . . ?
C89 C90 C92 120.3(3) . . ?
C91 C90 C92 120.9(2) . . ?
O13 C91 C90 118.3(2) . . ?
O13 C91 C86 121.3(2) . . ?
C90 C91 C86 120.4(2) . . ?
N11 C92 C90 121.4(3) . . ?
N11 C92 H92 119.3 . . ?
C90 C92 H92 119.3 . . ?
C91 O13 H13O 105(2) . . ?

_diffrn_measured_fraction_theta_max 0.908
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.055
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3d
_database_code_depnum_ccdc_archive 'CCDC 1422960'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H45 Br3 N6 O3'
_chemical_formula_sum            'C42 H45 Br3 N6 O3'
_chemical_formula_weight         921.57
_chemical_absolute_configuration rm

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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.5208(2)
_cell_length_b                   19.0262(3)
_cell_length_c                   14.9678(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.8320(10)
_cell_angle_gamma                90.00
_cell_volume                     4133.13(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(1)
_cell_measurement_reflns_used    50674
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      76.55

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1872
_exptl_absorpt_coefficient_mu    3.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.4 (release 09-12-2010 CrysAlis171 .NET)
(compiled Dec  9 2010,10:47:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      130(1)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5357
_diffrn_standards_number         61611
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            61556
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0125
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         76.55
_reflns_number_total             17091
_reflns_number_gt                17015
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0317P)²+3.9677P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(7)
_refine_ls_number_reflns         17091
_refine_ls_number_parameters     973
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0255
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0672
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_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 1.30535(19) 0.59062(14) 0.54411(17) 0.0261(5) Uani 1 1 d . . .
H1 H 1.3012 0.5508 0.5853 0.031 Uiso 1 1 calc R . .
C2 C 1.21309(19) 0.60057(14) 0.49341(17) 0.0244(5) Uani 1 1 d . . .
H2 H 1.2162 0.6431 0.4567 0.029 Uiso 1 1 calc R . .
C3 C 1.1914(2) 0.53808(15) 0.43283(18) 0.0286(6) Uani 1 1 d . . .
H3A H 1.1335 0.5463 0.4003 0.034 Uiso 1 1 calc R . .
H3B H 1.1846 0.4962 0.4689 0.034 Uiso 1 1 calc R . .
C4 C 1.2677(2) 0.52676(16) 0.3668(2) 0.0342(6) Uani 1 1 d . . .
H4A H 1.2536 0.4859 0.3302 0.041 Uiso 1 1 calc R . .
H4B H 1.2715 0.5673 0.3277 0.041 Uiso 1 1 calc R . .
C5 C 1.3592(2) 0.51612(17) 0.4166(2) 0.0379(7) Uani 1 1 d . . .
H5A H 1.4076 0.5112 0.3738 0.046 Uiso 1 1 calc R . .
H5B H 1.3569 0.4731 0.4512 0.046 Uiso 1 1 calc R . .
C6 C 1.3816(2) 0.57722(17) 0.4785(2) 0.0351(6) Uani 1 1 d . . .
H6A H 1.3908 0.6192 0.4432 0.042 Uiso 1 1 calc R . .
H6B H 1.4387 0.5674 0.5117 0.042 Uiso 1 1 calc R . .
N1 N 1.32621(15) 0.65452(13) 0.59449(15) 0.0275(5) Uani 1 1 d . . .
N2 N 1.14089(15) 0.60971(12) 0.55915(14) 0.0246(4) Uani 1 1 d . . .
C7 C 1.09676(17) 0.66744(14) 0.55971(16) 0.0236(5) Uani 1 1 d . . .
H7 H 1.1105 0.7018 0.5180 0.028 Uiso 1 1 calc R . .
C8 C 1.02509(16) 0.68161(14) 0.62394(16) 0.0221(5) Uani 1 1 d . . .
C9 C 1.00770(17) 0.63428(13) 0.69386(17) 0.0216(5) Uani 1 1 d . . .
C10 C 0.93789(16) 0.64936(14) 0.75441(16) 0.0221(5) Uani 1 1 d . . .
C11 C 0.88691(19) 0.71059(14) 0.74367(17) 0.0243(5) Uani 1 1 d . . .
H11 H 0.8410 0.7211 0.7835 0.029 Uiso 1 1 calc R . .
C12 C 0.90376(18) 0.75588(14) 0.67444(18) 0.0251(5) Uani 1 1 d . . .
C13 C 0.97290(18) 0.74259(14) 0.61489(17) 0.0242(5) Uani 1 1 d . . .
H13 H 0.9843 0.7743 0.5692 0.029 Uiso 1 1 calc R . .
C14 C 0.91926(17) 0.59795(13) 0.82598(17) 0.0221(5) Uani 1 1 d . . .
H14 H 0.9601 0.5608 0.8348 0.027 Uiso 1 1 calc R . .
Br1 Br 0.832067(19) 0.838969(15) 0.65763(2) 0.03107(6) Uani 1 1 d . . .
O1 O 1.05543(13) 0.57378(10) 0.70307(12) 0.0264(4) Uani 1 1 d . . .
H1O H 1.0976 0.5689 0.6550 0.034 Uiso 1 1 d R . .
C15 C 0.83951(18) 0.54420(14) 0.93912(17) 0.0236(5) Uani 1 1 d . . .
H15 H 0.8917 0.5119 0.9346 0.028 Uiso 1 1 calc R . .
C16 C 0.83688(17) 0.57251(14) 1.03517(17) 0.0239(5) Uani 1 1 d . . .
H16 H 0.7868 0.6067 1.0398 0.029 Uiso 1 1 calc R . .
C17 C 0.8227(2) 0.51191(16) 1.10055(19) 0.0308(6) Uani 1 1 d . . .
H17A H 0.8763 0.4815 1.1005 0.037 Uiso 1 1 calc R . .
H17B H 0.8178 0.5309 1.1604 0.037 Uiso 1 1 calc R . .
C18 C 0.7373(2) 0.46853(17) 1.0778(2) 0.0358(7) Uani 1 1 d . . .
H18A H 0.6827 0.4968 1.0862 0.043 Uiso 1 1 calc R . .
H18B H 0.7349 0.4285 1.1178 0.043 Uiso 1 1 calc R . .
C19 C 0.7384(2) 0.44279(17) 0.9810(2) 0.0361(7) Uani 1 1 d . . .
H19A H 0.7885 0.4097 0.9745 0.043 Uiso 1 1 calc R . .
H19B H 0.6811 0.4187 0.9662 0.043 Uiso 1 1 calc R . .
C20 C 0.75042(19) 0.50433(16) 0.91703(19) 0.0298(6) Uani 1 1 d . . .
H20A H 0.6984 0.5361 0.9211 0.036 Uiso 1 1 calc R . .
H20B H 0.7516 0.4869 0.8562 0.036 Uiso 1 1 calc R . .
N3 N 0.85052(15) 0.60203(12) 0.87576(14) 0.0246(4) Uani 1 1 d . . .
N4 N 0.92454(15) 0.60593(12) 1.05824(14) 0.0250(4) Uani 1 1 d . . .
C21 C 0.92670(18) 0.67043(14) 1.08087(17) 0.0251(5) Uani 1 1 d . . .
H21 H 0.8721 0.6961 1.0801 0.030 Uiso 1 1 calc R . .
C22 C 1.01232(19) 0.70488(15) 1.10789(17) 0.0255(5) Uani 1 1 d . . .
C23 C 1.09638(18) 0.66823(14) 1.10970(17) 0.0246(5) Uani 1 1 d . . .
C24 C 1.17801(19) 0.70287(15) 1.13605(17) 0.0270(5) Uani 1 1 d . . .
C25 C 1.1737(2) 0.77281(15) 1.16360(18) 0.0288(6) Uani 1 1 d . . .
H25 H 1.2274 0.7961 1.1820 0.035 Uiso 1 1 calc R . .
C26 C 1.0908(2) 0.80749(15) 1.16376(18) 0.0291(6) Uani 1 1 d . . .
C27 C 1.01021(19) 0.77520(15) 1.13564(17) 0.0267(5) Uani 1 1 d . . .
H27 H 0.9549 0.7998 1.1350 0.032 Uiso 1 1 calc R . .
C28 C 1.26691(18) 0.66542(15) 1.13380(18) 0.0275(5) Uani 1 1 d . . .
H28 H 1.2675 0.6187 1.1156 0.033 Uiso 1 1 calc R . .
Br2 Br 1.08576(2) 0.900787(16) 1.20779(2) 0.03734(7) Uani 1 1 d . . .
O2 O 1.10118(13) 0.60040(10) 1.08554(13) 0.0290(4) Uani 1 1 d . . .
H2O H 1.0431 0.5807 1.0738 0.038 Uiso 1 1 d R . .
C29 C 1.42587(18) 0.65297(16) 1.15285(17) 0.0276(5) Uani 1 1 d . . .
H29 H 1.4115 0.6068 1.1270 0.033 Uiso 1 1 calc R . .
C30 C 1.49587(18) 0.69099(16) 1.09570(18) 0.0291(6) Uani 1 1 d . . .
H30 H 1.5063 0.7385 1.1193 0.035 Uiso 1 1 calc R . .
C31 C 1.5873(2) 0.6512(2) 1.0960(2) 0.0399(7) Uani 1 1 d . . .
H31A H 1.5778 0.6051 1.0695 0.048 Uiso 1 1 calc R . .
H31B H 1.6309 0.6765 1.0601 0.048 Uiso 1 1 calc R . .
C32 C 1.6269(2) 0.6430(2) 1.1910(2) 0.0473(9) Uani 1 1 d . . .
H32A H 1.6832 0.6157 1.1901 0.057 Uiso 1 1 calc R . .
H32B H 1.6418 0.6890 1.2155 0.057 Uiso 1 1 calc R . .
C33 C 1.5578(3) 0.6066(2) 1.2499(2) 0.0473(8) Uani 1 1 d . . .
H33A H 1.5490 0.5586 1.2296 0.057 Uiso 1 1 calc R . .
H33B H 1.5823 0.6051 1.3110 0.057 Uiso 1 1 calc R . .
C34 C 1.4660(2) 0.64418(18) 1.24783(19) 0.0350(6) Uani 1 1 d . . .
H34A H 1.4737 0.6902 1.2751 0.042 Uiso 1 1 calc R . .
H34B H 1.4229 0.6178 1.2830 0.042 Uiso 1 1 calc R . .
N5 N 1.34255(15) 0.69503(13) 1.15588(15) 0.0284(5) Uani 1 1 d . . .
N6 N 1.45943(15) 0.69548(13) 1.00389(15) 0.0281(5) Uani 1 1 d . . .
C35 C 1.44778(18) 0.75563(15) 0.96801(19) 0.0272(5) Uani 1 1 d . . .
H35 H 1.4599 0.7958 1.0018 0.033 Uiso 1 1 calc R . .
C36 C 1.41581(17) 0.76292(14) 0.87498(18) 0.0244(5) Uani 1 1 d . . .
C37 C 1.39230(18) 0.70282(14) 0.82301(18) 0.0247(5) Uani 1 1 d . . .
C38 C 1.36492(18) 0.71090(15) 0.73291(18) 0.0254(5) Uani 1 1 d . . .
C39 C 1.36233(18) 0.77805(15) 0.69602(18) 0.0257(5) Uani 1 1 d . . .
H39 H 1.3449 0.7839 0.6362 0.031 Uiso 1 1 calc R . .
C40 C 1.38533(18) 0.83581(15) 0.74737(19) 0.0280(5) Uani 1 1 d . . .
C41 C 1.41131(18) 0.82957(15) 0.83631(19) 0.0278(5) Uani 1 1 d . . .
H41 H 1.4257 0.8693 0.8702 0.033 Uiso 1 1 calc R . .
C42 C 1.34276(17) 0.64854(15) 0.67741(17) 0.0249(5) Uani 1 1 d . . .
H42 H 1.3410 0.6044 0.7039 0.030 Uiso 1 1 calc R . .
Br3 Br 1.38401(2) 0.926978(15) 0.69462(2) 0.03520(7) Uani 1 1 d . . .
O3 O 1.39756(14) 0.63776(10) 0.85772(13) 0.0293(4) Uani 1 1 d . . .
H3O H 1.4235 0.6458 0.9135 0.038 Uiso 1 1 d R . .
C51A C 1.10805(17) 0.99259(13) 0.46858(17) 0.0231(5) Uani 1 1 d . . .
H51 H 1.0584 1.0247 0.4845 0.028 Uiso 1 1 calc R . .
C52 C 1.17370(17) 0.98180(14) 0.54947(17) 0.0235(5) Uani 1 1 d . . .
H52 H 1.2215 0.9478 0.5343 0.028 Uiso 1 1 calc R . .
C53 C 1.21920(19) 1.05194(15) 0.57667(19) 0.0293(6) Uani 1 1 d . . .
H53A H 1.1722 1.0846 0.5950 0.035 Uiso 1 1 calc R . .
H53B H 1.2614 1.0442 0.6273 0.035 Uiso 1 1 calc R . .
C54 C 1.2717(2) 1.08394(16) 0.4996(2) 0.0332(6) Uani 1 1 d . . .
H54A H 1.2968 1.1292 0.5176 0.040 Uiso 1 1 calc R . .
H54B H 1.3225 1.0535 0.4847 0.040 Uiso 1 1 calc R . .
C55 C 1.2074(2) 1.09299(16) 0.4186(2) 0.0323(6) Uani 1 1 d . . .
H55A H 1.2419 1.1107 0.3690 0.039 Uiso 1 1 calc R . .
H55B H 1.1603 1.1273 0.4319 0.039 Uiso 1 1 calc R . .
C56 C 1.1616(2) 1.02377(15) 0.39182(19) 0.0285(6) Uani 1 1 d . . .
H56A H 1.2084 0.9906 0.3741 0.034 Uiso 1 1 calc R . .
H56B H 1.1199 1.0316 0.3408 0.034 Uiso 1 1 calc R . .
N11 N 1.06909(15) 0.92460(12) 0.44245(14) 0.0254(4) Uani 1 1 d . . .
N12 N 1.12330(15) 0.95564(12) 0.62538(15) 0.0247(4) Uani 1 1 d . . .
C57 C 1.14478(18) 0.89527(15) 0.65651(18) 0.0252(5) Uani 1 1 d . . .
H57 H 1.1894 0.8690 0.6282 0.030 Uiso 1 1 calc R . .
C58 C 1.10169(18) 0.86583(14) 0.73518(17) 0.0243(5) Uani 1 1 d . . .
C59 C 1.03000(17) 0.90188(14) 0.77706(17) 0.0233(5) Uani 1 1 d . . .
C60 C 0.99040(18) 0.87252(14) 0.85303(17) 0.0249(5) Uani 1 1 d . . .
C61 C 1.02383(18) 0.80910(15) 0.88652(18) 0.0260(5) Uani 1 1 d . . .
H61 H 0.9983 0.7894 0.9369 0.031 Uiso 1 1 calc R . .
C62 C 1.09534(19) 0.77494(14) 0.84497(18) 0.0261(5) Uani 1 1 d . . .
C63 C 1.13317(18) 0.80241(14) 0.77000(19) 0.0259(5) Uani 1 1 d . . .
H63 H 1.1802 0.7784 0.7423 0.031 Uiso 1 1 calc R . .
C64 C 0.91399(18) 0.90958(14) 0.89501(18) 0.0259(5) Uani 1 1 d . . .
H64 H 0.8925 0.9514 0.8698 0.031 Uiso 1 1 calc R . .
Br4 Br 1.14136(2) 0.687623(16) 0.890131(19) 0.03240(7) Uani 1 1 d . . .
O4 O 0.99853(13) 0.96429(10) 0.74656(13) 0.0276(4) Uani 1 1 d . . .
H4O H 1.0306 0.9700 0.7015 0.036 Uiso 1 1 d R . .
C65 C 0.80324(18) 0.92977(15) 1.00070(18) 0.0276(5) Uani 1 1 d . . .
H65 H 0.7873 0.9676 0.9586 0.033 Uiso 1 1 calc R . .
C66 C 0.71856(19) 0.88331(16) 1.01407(18) 0.0291(6) Uani 1 1 d . . .
H66 H 0.7359 0.8432 1.0522 0.035 Uiso 1 1 calc R . .
C67 C 0.6429(2) 0.92635(19) 1.0589(2) 0.0367(7) Uani 1 1 d . . .
H67A H 0.6222 0.9636 1.0188 0.044 Uiso 1 1 calc R . .
H67B H 0.5906 0.8961 1.0697 0.044 Uiso 1 1 calc R . .
C68 C 0.6770(2) 0.95858(19) 1.1474(2) 0.0414(7) Uani 1 1 d . . .
H68A H 0.6286 0.9871 1.1719 0.050 Uiso 1 1 calc R . .
H68B H 0.6919 0.9214 1.1898 0.050 Uiso 1 1 calc R . .
C69 C 0.7615(2) 1.00356(19) 1.1339(2) 0.0427(8) Uani 1 1 d . . .
H69A H 0.7842 1.0212 1.1912 0.051 Uiso 1 1 calc R . .
H69B H 0.7448 1.0435 1.0966 0.051 Uiso 1 1 calc R . .
C70 C 0.8377(2) 0.96142(18) 1.0898(2) 0.0373(7) Uani 1 1 d . . .
H70A H 0.8583 0.9240 1.1297 0.045 Uiso 1 1 calc R . .
H70B H 0.8898 0.9920 1.0796 0.045 Uiso 1 1 calc R . .
N13 N 0.87658(16) 0.88631(13) 0.96425(16) 0.0287(5) Uani 1 1 d . . .
N14 N 0.68374(16) 0.85778(13) 0.92740(15) 0.0282(5) Uani 1 1 d . . .
C71 C 0.68369(18) 0.79170(15) 0.91178(18) 0.0256(5) Uani 1 1 d . . .
H71 H 0.7063 0.7613 0.9559 0.031 Uiso 1 1 calc R . .
C72 C 0.64933(17) 0.76227(14) 0.82697(17) 0.0233(5) Uani 1 1 d . . .
C73 C 0.62235(18) 0.80604(14) 0.75463(18) 0.0242(5) Uani 1 1 d . . .
C74 C 0.59030(17) 0.77584(14) 0.67331(18) 0.0244(5) Uani 1 1 d . . .
C75 C 0.58224(18) 0.70305(14) 0.66646(18) 0.0269(5) Uani 1 1 d . . .
H75 H 0.5611 0.6828 0.6131 0.032 Uiso 1 1 calc R . .
C76 C 0.60567(18) 0.66109(14) 0.73880(18) 0.0253(5) Uani 1 1 d . . .
C77 C 0.64075(17) 0.68948(14) 0.81817(17) 0.0244(5) Uani 1 1 d . . .
H77 H 0.6585 0.6601 0.8653 0.029 Uiso 1 1 calc R . .
C78 C 0.56168(18) 0.82129(14) 0.59806(18) 0.0257(5) Uani 1 1 d . . .
H78 H 0.5667 0.8698 0.6044 0.031 Uiso 1 1 calc R . .
Br5 Br 0.58676(2) 0.562350(15) 0.72848(2) 0.03361(7) Uani 1 1 d . . .
O5 O 0.62586(14) 0.87646(10) 0.76175(13) 0.0289(4) Uani 1 1 d . . .
H5O H 0.6467 0.8894 0.8198 0.035 Uiso 1 1 d R . .
C79 C 0.49673(18) 0.84535(15) 0.45649(18) 0.0275(5) Uani 1 1 d . . .
H79 H 0.5112 0.8937 0.4746 0.033 Uiso 1 1 calc R . .
C80 C 0.54200(18) 0.82851(15) 0.36866(19) 0.0277(5) Uani 1 1 d . . .
H80 H 0.5304 0.7790 0.3542 0.033 Uiso 1 1 calc R . .
C81 C 0.5032(2) 0.87347(17) 0.29219(19) 0.0319(6) Uani 1 1 d . . .
H81A H 0.5320 0.8601 0.2371 0.038 Uiso 1 1 calc R . .
H81B H 0.5176 0.9225 0.3038 0.038 Uiso 1 1 calc R . .
C82 C 0.3988(2) 0.86468(17) 0.2812(2) 0.0361(7) Uani 1 1 d . . .
H82A H 0.3753 0.8959 0.2345 0.043 Uiso 1 1 calc R . .
H82B H 0.3845 0.8168 0.2634 0.043 Uiso 1 1 calc R . .
C83 C 0.3526(2) 0.88120(16) 0.3676(2) 0.0345(6) Uani 1 1 d . . .
H83A H 0.2869 0.8726 0.3604 0.041 Uiso 1 1 calc R . .
H83B H 0.3613 0.9305 0.3819 0.041 Uiso 1 1 calc R . .
C84 C 0.39199(19) 0.83621(16) 0.4448(2) 0.0327(6) Uani 1 1 d . . .
H84A H 0.3780 0.7871 0.4331 0.039 Uiso 1 1 calc R . .
H84B H 0.3629 0.8495 0.4997 0.039 Uiso 1 1 calc R . .
N15 N 0.53048(16) 0.79629(12) 0.52501(16) 0.0290(5) Uani 1 1 d . . .
N16 N 0.64159(15) 0.83933(13) 0.37703(15) 0.0279(5) Uani 1 1 d . . .
C85 C 0.69359(19) 0.78604(15) 0.36636(18) 0.0274(5) Uani 1 1 d . . .
H85 H 0.6664 0.7424 0.3558 0.033 Uiso 1 1 calc R . .
C86 C 0.79440(18) 0.79095(14) 0.37016(18) 0.0259(5) Uani 1 1 d . . .
C87 C 0.83942(18) 0.85454(14) 0.39213(17) 0.0251(5) Uani 1 1 d . . .
C88 C 0.93589(18) 0.85667(14) 0.39928(17) 0.0237(5) Uani 1 1 d . . .
C89 C 0.98589(18) 0.79607(14) 0.38007(17) 0.0248(5) Uani 1 1 d . . .
H89 H 1.0499 0.7972 0.3835 0.030 Uiso 1 1 calc R . .
C90 C 0.94135(19) 0.73494(14) 0.35626(17) 0.0258(5) Uani 1 1 d . . .
C91 C 0.84582(19) 0.73174(15) 0.35140(18) 0.0271(5) Uani 1 1 d . . .
H91 H 0.8164 0.6899 0.3356 0.033 Uiso 1 1 calc R . .
C92 C 0.98282(17) 0.92186(14) 0.42797(17) 0.0242(5) Uani 1 1 d . . .
H92 H 0.9480 0.9623 0.4357 0.029 Uiso 1 1 calc R . .
Br6 Br 1.00989(2) 0.652692(15) 0.330500(19) 0.03142(6) Uani 1 1 d . . .
O6 O 0.79067(13) 0.91343(10) 0.40706(14) 0.0321(4) Uani 1 1 d . . .
H6O H 0.7270 0.9013 0.3938 0.042 Uiso 1 1 d R . .


_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 N1 1.457(4) . ?
C1 C6 1.525(4) . ?
C1 C2 1.530(4) . ?
C1 H1 0.9800 . ?
C2 N2 1.471(3) . ?
C2 C3 1.522(4) . ?
C2 H2 0.9800 . ?
C3 C4 1.523(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.516(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.516(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N1 C42 1.262(3) . ?
N2 C7 1.272(3) . ?
C7 C8 1.464(3) . ?
C7 H7 0.9300 . ?
C8 C13 1.390(4) . ?
C8 C9 1.410(4) . ?
C9 O1 1.348(3) . ?
C9 C10 1.411(3) . ?
C10 C11 1.387(4) . ?
C10 C14 1.482(3) . ?
C11 C12 1.376(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(4) . ?
C12 Br1 1.905(3) . ?
C13 H13 0.9300 . ?
C14 N3 1.267(3) . ?
C14 H14 0.9300 . ?
O1 H1O 0.9633 . ?
C15 N3 1.465(3) . ?
C15 C20 1.527(4) . ?
C15 C16 1.537(3) . ?
C15 H15 0.9800 . ?
C16 N4 1.455(3) . ?
C16 C17 1.530(4) . ?
C16 H16 0.9800 . ?
C17 C18 1.519(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.530(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.526(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
N4 C21 1.273(4) . ?
C21 C22 1.452(4) . ?
C21 H21 0.9300 . ?
C22 C27 1.401(4) . ?
C22 C23 1.405(4) . ?
C23 O2 1.343(3) . ?
C23 C24 1.402(4) . ?
C24 C25 1.395(4) . ?
C24 C28 1.476(4) . ?
C25 C26 1.374(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.375(4) . ?
C26 Br2 1.896(3) . ?
C27 H27 0.9300 . ?
C28 N5 1.269(4) . ?
C28 H28 0.9300 . ?
O2 H2O 0.9349 . ?
C29 N5 1.453(3) . ?
C29 C34 1.528(4) . ?
C29 C30 1.531(4) . ?
C29 H29 0.9800 . ?
C30 N6 1.459(3) . ?
C30 C31 1.529(4) . ?
C30 H30 0.9800 . ?
C31 C32 1.525(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.523(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.513(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
N6 C35 1.273(4) . ?
C35 C36 1.460(4) . ?
C35 H35 0.9300 . ?
C36 C41 1.394(4) . ?
C36 C37 1.419(4) . ?
C37 O3 1.344(3) . ?
C37 C38 1.402(4) . ?
C38 C39 1.392(4) . ?
C38 C42 1.478(4) . ?
C39 C40 1.376(4) . ?
C39 H39 0.9300 . ?
C40 C41 1.377(4) . ?
C40 Br3 1.906(3) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
O3 H3O 0.9182 . ?
C51A N11 1.460(3) . ?
C51A C56 1.528(4) . ?
C51A C52 1.531(4) . ?
C51A H51 0.9800 . ?
C52 N12 1.459(3) . ?
C52 C53 1.538(4) . ?
C52 H52 0.9800 . ?
C53 C54 1.528(4) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.517(4) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.523(4) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
N11 C92 1.265(3) . ?
N12 C57 1.274(4) . ?
C57 C58 1.463(4) . ?
C57 H57 0.9300 . ?
C58 C63 1.386(4) . ?
C58 C59 1.410(4) . ?
C59 O4 1.347(3) . ?
C59 C60 1.406(4) . ?
C60 C61 1.388(4) . ?
C60 C64 1.472(4) . ?
C61 C62 1.389(4) . ?
C61 H61 0.9300 . ?
C62 C63 1.369(4) . ?
C62 Br4 1.906(3) . ?
C63 H63 0.9300 . ?
C64 N13 1.265(4) . ?
C64 H64 0.9300 . ?
O4 H4O 0.8387 . ?
C65 N13 1.467(3) . ?
C65 C66 1.533(4) . ?
C65 C70 1.533(4) . ?
C65 H65 0.9800 . ?
C66 N14 1.460(4) . ?
C66 C67 1.542(4) . ?
C66 H66 0.9800 . ?
C67 C68 1.527(4) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C68 C69 1.514(5) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C69 C70 1.533(4) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
N14 C71 1.279(4) . ?
C71 C72 1.461(4) . ?
C71 H71 0.9300 . ?
C72 C77 1.396(4) . ?
C72 C73 1.412(4) . ?
C73 O5 1.345(3) . ?
C73 C74 1.411(4) . ?
C74 C75 1.393(4) . ?
C74 C78 1.469(4) . ?
C75 C76 1.379(4) . ?
C75 H75 0.9300 . ?
C76 C77 1.387(4) . ?
C76 Br5 1.904(3) . ?
C77 H77 0.9300 . ?
C78 N15 1.263(4) . ?
C78 H78 0.9300 . ?
O5 H5O 0.9431 . ?
C79 N15 1.460(3) . ?
C79 C80 1.523(4) . ?
C79 C84 1.535(4) . ?
C79 H79 0.9800 . ?
C80 N16 1.462(3) . ?
C80 C81 1.522(4) . ?
C80 H80 0.9800 . ?
C81 C82 1.530(4) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C82 C83 1.509(5) . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C83 C84 1.533(4) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C84 H84A 0.9700 . ?
C84 H84B 0.9700 . ?
N16 C85 1.277(4) . ?
C85 C86 1.466(4) . ?
C85 H85 0.9300 . ?
C86 C91 1.385(4) . ?
C86 C87 1.409(4) . ?
C87 O6 1.348(3) . ?
C87 C88 1.402(4) . ?
C88 C89 1.397(4) . ?
C88 C92 1.473(4) . ?
C89 C90 1.372(4) . ?
C89 H89 0.9300 . ?
C90 C91 1.388(4) . ?
C90 Br6 1.901(3) . ?
C91 H91 0.9300 . ?
C92 H92 0.9300 . ?
O6 H6O 0.9672 . ?

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
N1 C1 C6 109.2(2) . . ?
N1 C1 C2 108.5(2) . . ?
C6 C1 C2 110.1(2) . . ?
N1 C1 H1 109.7 . . ?
C6 C1 H1 109.7 . . ?
C2 C1 H1 109.7 . . ?
N2 C2 C3 110.6(2) . . ?
N2 C2 C1 108.3(2) . . ?
C3 C2 C1 111.1(2) . . ?
N2 C2 H2 108.9 . . ?
C3 C2 H2 108.9 . . ?
C1 C2 H2 108.9 . . ?
C2 C3 C4 110.8(2) . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C3 110.1(2) . . ?
C5 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
C5 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C4 C5 C6 111.5(3) . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 C1 112.0(3) . . ?
C5 C6 H6A 109.2 . . ?
C1 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
C1 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C42 N1 C1 117.6(2) . . ?
C7 N2 C2 118.5(2) . . ?
N2 C7 C8 122.2(2) . . ?
N2 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C13 C8 C9 119.7(2) . . ?
C13 C8 C7 119.1(2) . . ?
C9 C8 C7 121.2(2) . . ?
O1 C9 C8 121.2(2) . . ?
O1 C9 C10 119.1(2) . . ?
C8 C9 C10 119.8(2) . . ?
C11 C10 C9 119.2(2) . . ?
C11 C10 C14 121.9(2) . . ?
C9 C10 C14 118.8(2) . . ?
C12 C11 C10 120.4(2) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 121.3(2) . . ?
C11 C12 Br1 120.6(2) . . ?
C13 C12 Br1 118.0(2) . . ?
C12 C13 C8 119.6(2) . . ?
C12 C13 H13 120.2 . . ?
C8 C13 H13 120.2 . . ?
N3 C14 C10 123.4(2) . . ?
N3 C14 H14 118.3 . . ?
C10 C14 H14 118.3 . . ?
C9 O1 H1O 110.0 . . ?
N3 C15 C20 110.0(2) . . ?
N3 C15 C16 110.4(2) . . ?
C20 C15 C16 109.3(2) . . ?
N3 C15 H15 109.0 . . ?
C20 C15 H15 109.0 . . ?
C16 C15 H15 109.0 . . ?
N4 C16 C17 108.2(2) . . ?
N4 C16 C15 109.1(2) . . ?
C17 C16 C15 110.0(2) . . ?
N4 C16 H16 109.8 . . ?
C17 C16 H16 109.8 . . ?
C15 C16 H16 109.8 . . ?
C18 C17 C16 113.1(2) . . ?
C18 C17 H17A 109.0 . . ?
C16 C17 H17A 109.0 . . ?
C18 C17 H17B 109.0 . . ?
C16 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 C19 110.7(2) . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 110.7(3) . . ?
C20 C19 H19A 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C19 C20 C15 111.0(2) . . ?
C19 C20 H20A 109.4 . . ?
C15 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
C15 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C14 N3 C15 116.0(2) . . ?
C21 N4 C16 119.9(2) . . ?
N4 C21 C22 121.5(2) . . ?
N4 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C27 C22 C23 119.7(3) . . ?
C27 C22 C21 119.1(2) . . ?
C23 C22 C21 121.1(2) . . ?
O2 C23 C24 118.5(2) . . ?
O2 C23 C22 121.6(2) . . ?
C24 C23 C22 119.9(2) . . ?
C25 C24 C23 119.1(3) . . ?
C25 C24 C28 121.0(2) . . ?
C23 C24 C28 119.9(3) . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 121.5(3) . . ?
C25 C26 Br2 119.6(2) . . ?
C27 C26 Br2 118.9(2) . . ?
C26 C27 C22 119.4(3) . . ?
C26 C27 H27 120.3 . . ?
C22 C27 H27 120.3 . . ?
N5 C28 C24 122.0(3) . . ?
N5 C28 H28 119.0 . . ?
C24 C28 H28 119.0 . . ?
C23 O2 H2O 112.5 . . ?
N5 C29 C34 108.9(2) . . ?
N5 C29 C30 109.0(2) . . ?
C34 C29 C30 109.4(2) . . ?
N5 C29 H29 109.8 . . ?
C34 C29 H29 109.8 . . ?
C30 C29 H29 109.8 . . ?
N6 C30 C31 108.7(2) . . ?
N6 C30 C29 109.1(2) . . ?
C31 C30 C29 110.9(3) . . ?
N6 C30 H30 109.4 . . ?
C31 C30 H30 109.4 . . ?
C29 C30 H30 109.4 . . ?
C32 C31 C30 110.7(3) . . ?
C32 C31 H31A 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 108.1 . . ?
C33 C32 C31 110.6(3) . . ?
C33 C32 H32A 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
C34 C33 C32 111.7(3) . . ?
C34 C33 H33A 109.3 . . ?
C32 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C32 C33 H33B 109.3 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 C29 112.4(3) . . ?
C33 C34 H34A 109.1 . . ?
C29 C34 H34A 109.1 . . ?
C33 C34 H34B 109.1 . . ?
C29 C34 H34B 109.1 . . ?
H34A C34 H34B 107.9 . . ?
C28 N5 C29 117.5(2) . . ?
C35 N6 C30 119.3(3) . . ?
N6 C35 C36 121.4(3) . . ?
N6 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C41 C36 C37 119.9(2) . . ?
C41 C36 C35 119.4(2) . . ?
C37 C36 C35 120.7(2) . . ?
O3 C37 C38 118.9(2) . . ?
O3 C37 C36 121.4(2) . . ?
C38 C37 C36 119.7(2) . . ?
C39 C38 C37 119.0(3) . . ?
C39 C38 C42 120.7(2) . . ?
C37 C38 C42 120.2(2) . . ?
C40 C39 C38 120.6(3) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C39 C40 C41 121.7(3) . . ?
C39 C40 Br3 119.8(2) . . ?
C41 C40 Br3 118.5(2) . . ?
C40 C41 C36 119.2(3) . . ?
C40 C41 H41 120.4 . . ?
C36 C41 H41 120.4 . . ?
N1 C42 C38 120.8(3) . . ?
N1 C42 H42 119.6 . . ?
C38 C42 H42 119.6 . . ?
C37 O3 H3O 102.4 . . ?
N11 C51A C56 110.2(2) . . ?
N11 C51A C52 108.6(2) . . ?
C56 C51A C52 109.1(2) . . ?
N11 C51A H51 109.6 . . ?
C56 C51A H51 109.6 . . ?
C52 C51A H51 109.6 . . ?
N12 C52 C51A 110.3(2) . . ?
N12 C52 C53 108.2(2) . . ?
C51A C52 C53 110.1(2) . . ?
N12 C52 H52 109.4 . . ?
C51A C52 H52 109.4 . . ?
C53 C52 H52 109.4 . . ?
C54 C53 C52 111.5(2) . . ?
C54 C53 H53A 109.3 . . ?
C52 C53 H53A 109.3 . . ?
C54 C53 H53B 109.3 . . ?
C52 C53 H53B 109.3 . . ?
H53A C53 H53B 108.0 . . ?
C55 C54 C53 109.9(2) . . ?
C55 C54 H54A 109.7 . . ?
C53 C54 H54A 109.7 . . ?
C55 C54 H54B 109.7 . . ?
C53 C54 H54B 109.7 . . ?
H54A C54 H54B 108.2 . . ?
C54 C55 C56 111.4(2) . . ?
C54 C55 H55A 109.4 . . ?
C56 C55 H55A 109.4 . . ?
C54 C55 H55B 109.4 . . ?
C56 C55 H55B 109.4 . . ?
H55A C55 H55B 108.0 . . ?
C55 C56 C51A 111.5(2) . . ?
C55 C56 H56A 109.3 . . ?
C51A C56 H56A 109.3 . . ?
C55 C56 H56B 109.3 . . ?
C51A C56 H56B 109.3 . . ?
H56A C56 H56B 108.0 . . ?
C92 N11 C51A 117.1(2) . . ?
C57 N12 C52 118.0(2) . . ?
N12 C57 C58 122.2(2) . . ?
N12 C57 H57 118.9 . . ?
C58 C57 H57 118.9 . . ?
C63 C58 C59 119.7(2) . . ?
C63 C58 C57 119.4(2) . . ?
C59 C58 C57 120.8(2) . . ?
O4 C59 C60 118.8(2) . . ?
O4 C59 C58 121.7(2) . . ?
C60 C59 C58 119.5(2) . . ?
C61 C60 C59 119.3(2) . . ?
C61 C60 C64 121.4(2) . . ?
C59 C60 C64 119.2(2) . . ?
C60 C61 C62 120.2(3) . . ?
C60 C61 H61 119.9 . . ?
C62 C61 H61 119.9 . . ?
C63 C62 C61 120.9(3) . . ?
C63 C62 Br4 118.6(2) . . ?
C61 C62 Br4 120.5(2) . . ?
C62 C63 C58 120.3(3) . . ?
C62 C63 H63 119.9 . . ?
C58 C63 H63 119.9 . . ?
N13 C64 C60 122.1(3) . . ?
N13 C64 H64 119.0 . . ?
C60 C64 H64 119.0 . . ?
C59 O4 H4O 101.3 . . ?
N13 C65 C66 108.6(2) . . ?
N13 C65 C70 108.9(2) . . ?
C66 C65 C70 110.7(2) . . ?
N13 C65 H65 109.5 . . ?
C66 C65 H65 109.5 . . ?
C70 C65 H65 109.5 . . ?
N14 C66 C65 109.4(2) . . ?
N14 C66 C67 109.4(2) . . ?
C65 C66 C67 109.7(2) . . ?
N14 C66 H66 109.4 . . ?
C65 C66 H66 109.4 . . ?
C67 C66 H66 109.4 . . ?
C68 C67 C66 112.0(3) . . ?
C68 C67 H67A 109.2 . . ?
C66 C67 H67A 109.2 . . ?
C68 C67 H67B 109.2 . . ?
C66 C67 H67B 109.2 . . ?
H67A C67 H67B 107.9 . . ?
C69 C68 C67 110.7(3) . . ?
C69 C68 H68A 109.5 . . ?
C67 C68 H68A 109.5 . . ?
C69 C68 H68B 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 108.1 . . ?
C68 C69 C70 111.2(3) . . ?
C68 C69 H69A 109.4 . . ?
C70 C69 H69A 109.4 . . ?
C68 C69 H69B 109.4 . . ?
C70 C69 H69B 109.4 . . ?
H69A C69 H69B 108.0 . . ?
C69 C70 C65 111.1(3) . . ?
C69 C70 H70A 109.4 . . ?
C65 C70 H70A 109.4 . . ?
C69 C70 H70B 109.4 . . ?
C65 C70 H70B 109.4 . . ?
H70A C70 H70B 108.0 . . ?
C64 N13 C65 116.3(2) . . ?
C71 N14 C66 119.2(2) . . ?
N14 C71 C72 122.3(3) . . ?
N14 C71 H71 118.9 . . ?
C72 C71 H71 118.9 . . ?
C77 C72 C73 119.4(2) . . ?
C77 C72 C71 119.3(2) . . ?
C73 C72 C71 121.3(2) . . ?
O5 C73 C74 119.0(2) . . ?
O5 C73 C72 121.2(2) . . ?
C74 C73 C72 119.8(2) . . ?
C75 C74 C73 119.5(2) . . ?
C75 C74 C78 120.5(2) . . ?
C73 C74 C78 119.9(2) . . ?
C76 C75 C74 120.0(3) . . ?
C76 C75 H75 120.0 . . ?
C74 C75 H75 120.0 . . ?
C75 C76 C77 121.4(3) . . ?
C75 C76 Br5 118.4(2) . . ?
C77 C76 Br5 120.1(2) . . ?
C76 C77 C72 119.8(2) . . ?
C76 C77 H77 120.1 . . ?
C72 C77 H77 120.1 . . ?
N15 C78 C74 121.8(2) . . ?
N15 C78 H78 119.1 . . ?
C74 C78 H78 119.1 . . ?
C73 O5 H5O 110.1 . . ?
N15 C79 C80 109.1(2) . . ?
N15 C79 C84 108.5(2) . . ?
C80 C79 C84 109.3(2) . . ?
N15 C79 H79 110.0 . . ?
C80 C79 H79 110.0 . . ?
C84 C79 H79 110.0 . . ?
N16 C80 C79 110.5(2) . . ?
N16 C80 C81 109.1(2) . . ?
C79 C80 C81 111.8(2) . . ?
N16 C80 H80 108.5 . . ?
C79 C80 H80 108.5 . . ?
C81 C80 H80 108.5 . . ?
C80 C81 C82 111.2(2) . . ?
C80 C81 H81A 109.4 . . ?
C82 C81 H81A 109.4 . . ?
C80 C81 H81B 109.4 . . ?
C82 C81 H81B 109.4 . . ?
H81A C81 H81B 108.0 . . ?
C83 C82 C81 110.6(2) . . ?
C83 C82 H82A 109.5 . . ?
C81 C82 H82A 109.5 . . ?
C83 C82 H82B 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 108.1 . . ?
C82 C83 C84 111.3(2) . . ?
C82 C83 H83A 109.4 . . ?
C84 C83 H83A 109.4 . . ?
C82 C83 H83B 109.4 . . ?
C84 C83 H83B 109.4 . . ?
H83A C83 H83B 108.0 . . ?
C83 C84 C79 111.5(2) . . ?
C83 C84 H84A 109.3 . . ?
C79 C84 H84A 109.3 . . ?
C83 C84 H84B 109.3 . . ?
C79 C84 H84B 109.3 . . ?
H84A C84 H84B 108.0 . . ?
C78 N15 C79 118.1(2) . . ?
C85 N16 C80 117.7(2) . . ?
N16 C85 C86 122.5(3) . . ?
N16 C85 H85 118.7 . . ?
C86 C85 H85 118.7 . . ?
C91 C86 C87 119.8(2) . . ?
C91 C86 C85 119.0(2) . . ?
C87 C86 C85 121.3(2) . . ?
O6 C87 C88 119.5(2) . . ?
O6 C87 C86 120.7(2) . . ?
C88 C87 C86 119.8(2) . . ?
C89 C88 C87 119.0(2) . . ?
C89 C88 C92 121.1(2) . . ?
C87 C88 C92 119.9(2) . . ?
C90 C89 C88 120.6(2) . . ?
C90 C89 H89 119.7 . . ?
C88 C89 H89 119.7 . . ?
C89 C90 C91 120.8(3) . . ?
C89 C90 Br6 120.3(2) . . ?
C91 C90 Br6 118.8(2) . . ?
C86 C91 C90 119.9(3) . . ?
C86 C91 H91 120.1 . . ?
C90 C91 H91 120.1 . . ?
N11 C92 C88 122.1(2) . . ?
N11 C92 H92 119.0 . . ?
C88 C92 H92 119.0 . . ?
C87 O6 H6O 105.8 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        76.55
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.058
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3e
_database_code_depnum_ccdc_archive 'CCDC 1422961'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C94 H118 N12 O13'
_chemical_formula_weight         1624.00
_chemical_absolute_configuration rm

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   11.2310(3)
_cell_length_b                   16.5478(4)
_cell_length_c                   16.6580(4)
_cell_angle_alpha                60.773(2)
_cell_angle_beta                 70.814(2)
_cell_angle_gamma                73.664(2)
_cell_volume                     2524.11(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    31750
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      76.50

_exptl_crystal_description       needle
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             870
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.51875
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28, SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.2679
_diffrn_standards_number         20997
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            56259
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         76.50
_reflns_number_total             19930
_reflns_number_gt                18377
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1108P)²+0.1613P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(12)
_refine_ls_number_reflns         19930
_refine_ls_number_parameters     1080
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1559
_refine_ls_wR_factor_gt          0.1516
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2418(2) 0.53472(14) 0.24381(16) 0.0442(5) Uani 1 1 d . . .
H1A H 0.1679 0.4992 0.2810 0.053 Uiso 1 1 calc R . .
C2 C 0.3092(2) 0.53048(13) 0.31228(15) 0.0414(4) Uani 1 1 d . . .
H2A H 0.3876 0.5612 0.2759 0.050 Uiso 1 1 calc R . .
C3 C 0.2203(3) 0.57996(15) 0.37205(17) 0.0477(5) Uani 1 1 d . . .
H3A H 0.2666 0.5791 0.4139 0.057 Uiso 1 1 calc R . .
H3B H 0.1470 0.5456 0.4125 0.057 Uiso 1 1 calc R . .
C4 C 0.1713(3) 0.68143(16) 0.31035(19) 0.0555(6) Uani 1 1 d . . .
H4A H 0.1103 0.7100 0.3512 0.067 Uiso 1 1 calc R . .
H4B H 0.2436 0.7177 0.2751 0.067 Uiso 1 1 calc R . .
C5 C 0.1066(3) 0.68651(17) 0.2415(2) 0.0603(7) Uani 1 1 d . . .
H5A H 0.0820 0.7529 0.1994 0.072 Uiso 1 1 calc R . .
H5B H 0.0279 0.6574 0.2767 0.072 Uiso 1 1 calc R . .
C6 C 0.1925(3) 0.63704(16) 0.18213(17) 0.0555(6) Uani 1 1 d . . .
H6A H 0.2660 0.6710 0.1409 0.067 Uiso 1 1 calc R . .
H6B H 0.1447 0.6381 0.1411 0.067 Uiso 1 1 calc R . .
N1 N 0.3292(2) 0.49235(13) 0.18327(14) 0.0510(5) Uani 1 1 d . . .
N2 N 0.34407(18) 0.43326(11) 0.37714(12) 0.0405(4) Uani 1 1 d . . .
C7 C 0.4575(2) 0.40449(14) 0.38866(16) 0.0438(5) Uani 1 1 d . . .
H7A H 0.5196 0.4455 0.3519 0.053 Uiso 1 1 calc R . .
C8 C 0.4941(2) 0.30973(14) 0.45719(15) 0.0408(4) Uani 1 1 d . . .
C9 C 0.4035(2) 0.24776(14) 0.51429(15) 0.0396(4) Uani 1 1 d . . .
C10 C 0.4420(2) 0.15722(14) 0.58107(14) 0.0388(4) Uani 1 1 d . . .
C11 C 0.5676(2) 0.12993(15) 0.58805(16) 0.0435(5) Uani 1 1 d . . .
H11A H 0.5929 0.0683 0.6322 0.052 Uiso 1 1 calc R . .
C12 C 0.6588(2) 0.19065(15) 0.53181(16) 0.0434(4) Uani 1 1 d . . .
C13 C 0.6209(2) 0.28102(15) 0.46686(16) 0.0445(5) Uani 1 1 d . . .
H13A H 0.6812 0.3233 0.4290 0.053 Uiso 1 1 calc R . .
O1 O 0.28166(15) 0.27310(10) 0.50621(11) 0.0430(3) Uani 1 1 d . . .
H1B H 0.2710 0.3289 0.4638 0.064 Uiso 1 1 d R . .
O1R O 0.77894(17) 0.15462(12) 0.54424(14) 0.0529(4) Uani 1 1 d . . .
C1R C 0.8698(2) 0.21779(19) 0.4986(2) 0.0541(6) Uani 1 1 d . . .
H1RA H 0.9490 0.1855 0.5201 0.081 Uiso 1 1 calc R . .
H1RB H 0.8359 0.2711 0.5143 0.081 Uiso 1 1 calc R . .
H1RC H 0.8869 0.2403 0.4301 0.081 Uiso 1 1 calc R . .
C14 C 0.3468(2) 0.09274(14) 0.64053(15) 0.0401(4) Uani 1 1 d . . .
H14A H 0.2681 0.1069 0.6234 0.048 Uiso 1 1 calc R . .
N3 N 0.36743(19) 0.01867(13) 0.71415(13) 0.0434(4) Uani 1 1 d . . .
N4 N 0.3268(2) -0.11780(13) 0.66661(13) 0.0463(4) Uani 1 1 d . . .
C15 C 0.2641(2) -0.03920(15) 0.76849(15) 0.0435(5) Uani 1 1 d . . .
H15A H 0.1871 -0.0065 0.7414 0.052 Uiso 1 1 calc R . .
C16 C 0.3095(3) -0.13334(16) 0.76341(15) 0.0485(5) Uani 1 1 d . . .
H16A H 0.3920 -0.1626 0.7836 0.058 Uiso 1 1 calc R . .
C17 C 0.2095(3) -0.19826(17) 0.82783(18) 0.0587(7) Uani 1 1 d . . .
H17A H 0.2410 -0.2598 0.8262 0.070 Uiso 1 1 calc R . .
H17B H 0.1305 -0.1716 0.8040 0.070 Uiso 1 1 calc R . .
C18 C 0.1791(4) -0.2121(2) 0.92979(19) 0.0731(9) Uani 1 1 d . . .
H18A H 0.2568 -0.2417 0.9552 0.088 Uiso 1 1 calc R . .
H18B H 0.1136 -0.2542 0.9694 0.088 Uiso 1 1 calc R . .
C19 C 0.1302(4) -0.1176(2) 0.9334(2) 0.0754(10) Uani 1 1 d . . .
H19A H 0.1119 -0.1262 0.9992 0.090 Uiso 1 1 calc R . .
H19B H 0.0504 -0.0890 0.9106 0.090 Uiso 1 1 calc R . .
C20 C 0.2327(3) -0.0535(2) 0.87046(17) 0.0592(7) Uani 1 1 d . . .
H20A H 0.2021 0.0080 0.8723 0.071 Uiso 1 1 calc R . .
H20B H 0.3109 -0.0815 0.8953 0.071 Uiso 1 1 calc R . .
C21 C 0.4361(2) -0.14281(15) 0.62269(17) 0.0457(5) Uani 1 1 d . . .
H21A H 0.5057 -0.1691 0.6526 0.055 Uiso 1 1 calc R . .
C22 C 0.4549(2) -0.13130(15) 0.52645(16) 0.0450(5) Uani 1 1 d . . .
C23 C 0.3551(2) -0.08994(16) 0.47940(16) 0.0451(5) Uani 1 1 d . . .
C24 C 0.3750(2) -0.08138(17) 0.38765(16) 0.0465(5) Uani 1 1 d . . .
C25 C 0.4957(3) -0.1125(2) 0.34472(18) 0.0524(5) Uani 1 1 d . . .
H25A H 0.5097 -0.1074 0.2831 0.063 Uiso 1 1 calc R . .
C26 C 0.5955(3) -0.1507(2) 0.3899(2) 0.0543(6) Uani 1 1 d . . .
C27 C 0.5759(2) -0.16136(17) 0.48121(18) 0.0501(5) Uani 1 1 d . . .
H27A H 0.6438 -0.1888 0.5128 0.060 Uiso 1 1 calc R . .
O2 O 0.23832(16) -0.05828(12) 0.52007(11) 0.0478(4) Uani 1 1 d . . .
H2B H 0.2389 -0.0677 0.5749 0.072 Uiso 1 1 d R . .
O2R O 0.7099(2) -0.17644(19) 0.33883(17) 0.0721(6) Uani 1 1 d . . .
C2R C 0.8165(3) -0.2081(3) 0.3791(3) 0.0753(9) Uani 1 1 d . . .
H2RA H 0.8926 -0.2216 0.3350 0.113 Uiso 1 1 calc R . .
H2RB H 0.8023 -0.2652 0.4382 0.113 Uiso 1 1 calc R . .
H2RC H 0.8286 -0.1596 0.3921 0.113 Uiso 1 1 calc R . .
C28 C 0.2704(2) -0.03797(16) 0.33853(15) 0.0441(5) Uani 1 1 d . . .
H28A H 0.1946 -0.0081 0.3657 0.053 Uiso 1 1 calc R . .
N5 N 0.2766(2) -0.03858(13) 0.26107(13) 0.0453(4) Uani 1 1 d . . .
N6 N 0.2512(2) 0.15609(12) 0.12484(13) 0.0433(4) Uani 1 1 d . . .
C29 C 0.1646(2) 0.00802(15) 0.21969(15) 0.0434(5) Uani 1 1 d . . .
H29A H 0.0995 0.0375 0.2591 0.052 Uiso 1 1 calc R . .
C30 C 0.2071(2) 0.08441(14) 0.11930(15) 0.0429(5) Uani 1 1 d . . .
H30A H 0.2782 0.0558 0.0818 0.051 Uiso 1 1 calc R . .
C31 C 0.0965(3) 0.12991(16) 0.07039(17) 0.0497(5) Uani 1 1 d . . .
H31A H 0.1264 0.1769 0.0052 0.060 Uiso 1 1 calc R . .
H31B H 0.0292 0.1628 0.1045 0.060 Uiso 1 1 calc R . .
C32 C 0.0399(3) 0.05758(19) 0.0669(2) 0.0586(6) Uani 1 1 d . . .
H32A H -0.0337 0.0892 0.0369 0.070 Uiso 1 1 calc R . .
H32B H 0.1047 0.0281 0.0283 0.070 Uiso 1 1 calc R . .
C33 C -0.0033(3) -0.01782(18) 0.1669(2) 0.0599(7) Uani 1 1 d . . .
H33A H -0.0735 0.0109 0.2038 0.072 Uiso 1 1 calc R . .
H33B H -0.0357 -0.0657 0.1637 0.072 Uiso 1 1 calc R . .
C34 C 0.1071(3) -0.06399(17) 0.21604(18) 0.0540(6) Uani 1 1 d . . .
H34A H 0.1741 -0.0971 0.1819 0.065 Uiso 1 1 calc R . .
H34B H 0.0768 -0.1109 0.2812 0.065 Uiso 1 1 calc R . .
C35 C 0.3584(2) 0.18178(15) 0.07426(15) 0.0423(4) Uani 1 1 d . . .
H35A H 0.4100 0.1514 0.0359 0.051 Uiso 1 1 calc R . .
C36 C 0.4054(2) 0.25685(15) 0.07302(15) 0.0422(4) Uani 1 1 d . . .
C37 C 0.3311(2) 0.30157(14) 0.13112(14) 0.0389(4) Uani 1 1 d . . .
C38 C 0.3769(2) 0.37441(14) 0.12819(14) 0.0399(4) Uani 1 1 d . . .
C39 C 0.4935(2) 0.39965(15) 0.06945(16) 0.0437(4) Uani 1 1 d . . .
H39A H 0.5235 0.4496 0.0664 0.052 Uiso 1 1 calc R . .
C40 C 0.5669(2) 0.35375(18) 0.01542(18) 0.0489(5) Uani 1 1 d . . .
C41 C 0.5217(2) 0.28198(18) 0.01666(18) 0.0491(5) Uani 1 1 d . . .
H41A H 0.5716 0.2510 -0.0214 0.059 Uiso 1 1 calc R . .
O3 O 0.21826(15) 0.27675(10) 0.18898(11) 0.0430(3) Uani 1 1 d . . .
H3D H 0.1837 0.2336 0.1957 0.052 Uiso 1 1 d R . .
O3R O 0.68356(19) 0.38325(15) -0.03829(15) 0.0633(5) Uani 1 1 d . . .
C3R C 0.7673(3) 0.3320(3) -0.0877(3) 0.0720(8) Uani 1 1 d . . .
H3RA H 0.8460 0.3599 -0.1222 0.108 Uiso 1 1 calc R . .
H3RB H 0.7265 0.3338 -0.1324 0.108 Uiso 1 1 calc R . .
H3RC H 0.7875 0.2669 -0.0426 0.108 Uiso 1 1 calc R . .
C42 C 0.2987(2) 0.42227(14) 0.18765(15) 0.0399(4) Uani 1 1 d . . .
H42A H 0.2226 0.3994 0.2308 0.048 Uiso 1 1 calc R . .
C51 C 0.9222(3) 0.41157(15) 0.08306(16) 0.0487(5) Uani 1 1 d . . .
H51A H 0.8444 0.4511 0.0594 0.058 Uiso 1 1 calc R . .
C52 C 0.9813(3) 0.46457(15) 0.11031(15) 0.0487(5) Uani 1 1 d . . .
H52A H 1.0540 0.4219 0.1393 0.058 Uiso 1 1 calc R . .
C53 C 1.0317(4) 0.55081(18) 0.02399(19) 0.0650(8) Uani 1 1 d . . .
H53A H 0.9597 0.5955 -0.0030 0.078 Uiso 1 1 calc R . .
H53B H 1.0721 0.5823 0.0436 0.078 Uiso 1 1 calc R . .
C54 C 1.1282(4) 0.52401(19) -0.05067(17) 0.0640(7) Uani 1 1 d . . .
H54A H 1.1565 0.5812 -0.1068 0.077 Uiso 1 1 calc R . .
H54B H 1.2038 0.4839 -0.0256 0.077 Uiso 1 1 calc R . .
C55 C 1.0711(3) 0.47206(18) -0.07933(17) 0.0605(7) Uani 1 1 d . . .
H55A H 1.1371 0.4522 -0.1253 0.073 Uiso 1 1 calc R . .
H55B H 1.0013 0.5145 -0.1105 0.073 Uiso 1 1 calc R . .
C56 C 1.0191(3) 0.38588(16) 0.00646(16) 0.0527(6) Uani 1 1 d . . .
H56A H 1.0907 0.3402 0.0332 0.063 Uiso 1 1 calc R . .
H56B H 0.9779 0.3557 -0.0140 0.063 Uiso 1 1 calc R . .
N11 N 0.8884(2) 0.32517(12) 0.16553(13) 0.0449(4) Uani 1 1 d . . .
N12 N 0.8885(3) 0.49500(14) 0.17875(16) 0.0584(5) Uani 1 1 d . . .
C57 C 0.9158(3) 0.46520(15) 0.25742(16) 0.0459(5) Uani 1 1 d . . .
H57A H 0.9921 0.4227 0.2687 0.055 Uiso 1 1 calc R . .
C58 C 0.8365(2) 0.49253(16) 0.33185(17) 0.0474(5) Uani 1 1 d . . .
C59 C 0.8843(2) 0.46196(16) 0.41248(16) 0.0447(5) Uani 1 1 d . . .
C60 C 0.8091(2) 0.49049(16) 0.48325(17) 0.0478(5) Uani 1 1 d . . .
C61 C 0.6904(3) 0.5460(2) 0.4744(2) 0.0561(6) Uani 1 1 d . . .
H61A H 0.6406 0.5642 0.5230 0.067 Uiso 1 1 calc R . .
C62 C 0.6441(3) 0.5753(2) 0.3943(2) 0.0580(6) Uani 1 1 d . . .
C63 C 0.7188(3) 0.54872(19) 0.32406(18) 0.0536(6) Uani 1 1 d . . .
H63A H 0.6888 0.5695 0.2690 0.064 Uiso 1 1 calc R . .
O4 O 0.99808(16) 0.40771(12) 0.41947(11) 0.0461(3) Uani 1 1 d . . .
H4C H 1.0327 0.3873 0.4655 0.055 Uiso 1 1 d R . .
O4R O 0.5287(2) 0.62743(19) 0.37893(18) 0.0745(6) Uani 1 1 d . . .
C4R C 0.4463(3) 0.6498(3) 0.4520(3) 0.0728(8) Uani 1 1 d . . .
H4RA H 0.3687 0.6895 0.4317 0.109 Uiso 1 1 calc R . .
H4RB H 0.4890 0.6834 0.4668 0.109 Uiso 1 1 calc R . .
H4RC H 0.4240 0.5921 0.5083 0.109 Uiso 1 1 calc R . .
C64 C 0.8549(3) 0.46129(17) 0.56806(17) 0.0497(5) Uani 1 1 d . . .
H64A H 0.8027 0.4797 0.6159 0.060 Uiso 1 1 calc R . .
N13 N 0.9646(2) 0.41112(14) 0.57855(13) 0.0476(4) Uani 1 1 d . . .
N14 N 0.9370(2) 0.23392(13) 0.74742(14) 0.0452(4) Uani 1 1 d . . .
C65 C 1.0095(3) 0.38746(17) 0.66077(16) 0.0487(5) Uani 1 1 d . . .
H65A H 0.9396 0.4087 0.7050 0.058 Uiso 1 1 calc R . .
C66 C 1.0486(2) 0.28125(15) 0.71177(16) 0.0441(5) Uani 1 1 d . . .
H66A H 1.1138 0.2594 0.6660 0.053 Uiso 1 1 calc R . .
C67 C 1.1049(3) 0.25556(18) 0.79477(19) 0.0527(5) Uani 1 1 d . . .
H67A H 1.0378 0.2710 0.8433 0.063 Uiso 1 1 calc R . .
H67B H 1.1341 0.1873 0.8236 0.063 Uiso 1 1 calc R . .
C68 C 1.2161(3) 0.3070(2) 0.7644(2) 0.0612(7) Uani 1 1 d . . .
H68A H 1.2883 0.2850 0.7229 0.073 Uiso 1 1 calc R . .
H68B H 1.2444 0.2932 0.8208 0.073 Uiso 1 1 calc R . .
C69 C 1.1772(4) 0.4137(2) 0.7111(2) 0.0652(7) Uani 1 1 d . . .
H69A H 1.1129 0.4368 0.7553 0.078 Uiso 1 1 calc R . .
H69B H 1.2527 0.4455 0.6874 0.078 Uiso 1 1 calc R . .
C70 C 1.1228(3) 0.43770(18) 0.62919(19) 0.0584(7) Uani 1 1 d . . .
H70A H 1.1898 0.4200 0.5820 0.070 Uiso 1 1 calc R . .
H70B H 1.0957 0.5061 0.5984 0.070 Uiso 1 1 calc R . .
C71 C 0.9498(2) 0.16829(15) 0.72569(16) 0.0415(4) Uani 1 1 d . . .
H71A H 1.0289 0.1540 0.6879 0.050 Uiso 1 1 calc R . .
C72 C 0.8477(2) 0.11277(16) 0.75620(18) 0.0446(5) Uani 1 1 d . . .
C73 C 0.8703(2) 0.03873(15) 0.73300(17) 0.0428(4) Uani 1 1 d . . .
C74 C 0.7712(2) -0.01220(15) 0.75989(17) 0.0443(5) Uani 1 1 d . . .
C75 C 0.6502(2) 0.01285(18) 0.80833(18) 0.0489(5) Uani 1 1 d . . .
H75A H 0.5830 -0.0212 0.8262 0.059 Uiso 1 1 calc R . .
C76 C 0.6282(2) 0.08737(19) 0.83029(19) 0.0496(5) Uani 1 1 d . . .
C77 C 0.7261(2) 0.13640(19) 0.8055(2) 0.0523(6) Uani 1 1 d . . .
H77A H 0.7109 0.1865 0.8220 0.063 Uiso 1 1 calc R . .
O5 O 0.98735(15) 0.01916(11) 0.68334(13) 0.0472(4) Uani 1 1 d . . .
H5C H 1.0089 -0.0236 0.6647 0.057 Uiso 1 1 d R . .
O5R O 0.51173(17) 0.11937(15) 0.87529(16) 0.0603(5) Uani 1 1 d . . .
C5R C 0.4067(3) 0.0820(2) 0.8851(2) 0.0609(7) Uani 1 1 d . . .
H5RA H 0.3281 0.1130 0.9125 0.091 Uiso 1 1 calc R . .
H5RB H 0.4166 0.0147 0.9268 0.091 Uiso 1 1 calc R . .
H5RC H 0.4024 0.0922 0.8230 0.091 Uiso 1 1 calc R . .
C78 C 0.7931(2) -0.08927(16) 0.73398(17) 0.0454(5) Uani 1 1 d . . .
H78A H 0.7255 -0.1230 0.7518 0.055 Uiso 1 1 calc R . .
N15 N 0.90144(19) -0.11105(12) 0.68802(13) 0.0426(4) Uani 1 1 d . . .
N16 N 0.86821(19) -0.08550(12) 0.50948(14) 0.0435(4) Uani 1 1 d . . .
C79 C 0.9250(2) -0.18757(14) 0.66259(15) 0.0428(5) Uani 1 1 d . . .
H79A H 0.8444 -0.2140 0.6832 0.051 Uiso 1 1 calc R . .
C80 C 0.9726(2) -0.14915(13) 0.55449(15) 0.0404(4) Uani 1 1 d . . .
H80A H 1.0445 -0.1137 0.5335 0.048 Uiso 1 1 calc R . .
C81 C 1.0191(3) -0.22890(15) 0.52464(17) 0.0497(5) Uani 1 1 d . . .
H81A H 0.9467 -0.2614 0.5413 0.060 Uiso 1 1 calc R . .
H81B H 1.0519 -0.2027 0.4552 0.060 Uiso 1 1 calc R . .
C82 C 1.1240(3) -0.29900(16) 0.57280(18) 0.0527(6) Uani 1 1 d . . .
H82A H 1.1976 -0.2673 0.5553 0.063 Uiso 1 1 calc R . .
H82B H 1.1533 -0.3493 0.5517 0.063 Uiso 1 1 calc R . .
C83 C 1.0725(3) -0.34106(16) 0.68008(18) 0.0578(7) Uani 1 1 d . . .
H83A H 1.0014 -0.3753 0.6978 0.069 Uiso 1 1 calc R . .
H83B H 1.1405 -0.3860 0.7119 0.069 Uiso 1 1 calc R . .
C84 C 1.0257(3) -0.26329(15) 0.71183(17) 0.0524(6) Uani 1 1 d . . .
H84A H 1.0993 -0.2339 0.6995 0.063 Uiso 1 1 calc R . .
H84B H 0.9896 -0.2910 0.7809 0.063 Uiso 1 1 calc R . .
C85 C 0.8876(2) -0.00176(14) 0.45384(15) 0.0403(4) Uani 1 1 d . . .
H85A H 0.9656 0.0162 0.4456 0.048 Uiso 1 1 calc R . .
C86 C 0.7927(2) 0.06828(13) 0.40173(15) 0.0402(4) Uani 1 1 d . . .
C87 C 0.8285(2) 0.15355(14) 0.32430(15) 0.0410(4) Uani 1 1 d . . .
C88 C 0.7389(2) 0.21901(14) 0.27439(16) 0.0430(5) Uani 1 1 d . . .
C89 C 0.6117(2) 0.20264(16) 0.30205(17) 0.0478(5) Uani 1 1 d . . .
H89A H 0.5508 0.2477 0.2678 0.057 Uiso 1 1 calc R . .
C90 C 0.5755(2) 0.12003(16) 0.37985(18) 0.0478(5) Uani 1 1 d . . .
C91 C 0.6680(2) 0.05439(15) 0.42704(16) 0.0441(5) Uani 1 1 d . . .
H91A H 0.6437 -0.0025 0.4790 0.053 Uiso 1 1 calc R . .
O6 O 0.95153(15) 0.16757(10) 0.30057(11) 0.0445(3) Uani 1 1 d . . .
H6C H 0.9606 0.2207 0.2535 0.067 Uiso 1 1 d R . .
O6R O 0.45514(18) 0.09770(13) 0.41561(13) 0.0560(4) Uani 1 1 d . . .
C6R C 0.3630(3) 0.15584(19) 0.3600(2) 0.0598(6) Uani 1 1 d . . .
H6RA H 0.2827 0.1298 0.3902 0.090 Uiso 1 1 calc R . .
H6RB H 0.3947 0.1583 0.2967 0.090 Uiso 1 1 calc R . .
H6RC H 0.3485 0.2192 0.3550 0.090 Uiso 1 1 calc R . .
C92 C 0.7742(2) 0.30711(15) 0.19329(16) 0.0462(5) Uani 1 1 d . . .
H92A H 0.7112 0.3514 0.1609 0.055 Uiso 1 1 calc R . .
C1S C 0.5477(5) 0.3427(3) 0.6539(4) 0.0960(13) Uani 1 1 d . . .
H1SA H 0.5453 0.2754 0.6822 0.144 Uiso 1 1 calc R . .
H1SB H 0.6309 0.3566 0.6109 0.144 Uiso 1 1 calc R . .
H1SC H 0.4805 0.3772 0.6188 0.144 Uiso 1 1 calc R . .
C2S C 0.5269(4) 0.3716(2) 0.7304(3) 0.0872(11) Uani 1 1 d . . .
H2SA H 0.4564 0.3423 0.7834 0.105 Uiso 1 1 calc R . .
H2SB H 0.6050 0.3510 0.7548 0.105 Uiso 1 1 calc R . .
O3S O 0.4965(3) 0.47025(18) 0.6922(2) 0.0868(7) Uani 1 1 d . . .
C4S C 0.4665(5) 0.5031(3) 0.7618(3) 0.0919(11) Uani 1 1 d . . .
H4SA H 0.5398 0.4853 0.7905 0.110 Uiso 1 1 calc R . .
H4SB H 0.3923 0.4764 0.8122 0.110 Uiso 1 1 calc R . .
C5S C 0.4371(4) 0.6043(3) 0.7126(3) 0.0880(11) Uani 1 1 d . . .
H5SA H 0.4297 0.6319 0.7547 0.132 Uiso 1 1 calc R . .
H5SB H 0.3563 0.6208 0.6937 0.132 Uiso 1 1 calc R . .
H5SC H 0.5053 0.6283 0.6563 0.132 Uiso 1 1 calc R . .


_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 N1 1.458(3) . ?
C1 C2 1.529(3) . ?
C1 C6 1.542(3) . ?
C2 N2 1.461(3) . ?
C2 C3 1.530(3) . ?
C3 C4 1.531(3) . ?
C4 C5 1.507(4) . ?
C5 C6 1.515(4) . ?
N1 C42 1.262(3) . ?
N2 C7 1.271(3) . ?
C7 C8 1.459(3) . ?
C8 C13 1.405(3) . ?
C8 C9 1.411(3) . ?
C9 O1 1.345(3) . ?
C9 C10 1.412(3) . ?
C10 C11 1.380(3) . ?
C10 C14 1.475(3) . ?
C11 C12 1.402(3) . ?
C12 O1R 1.353(3) . ?
C12 C13 1.397(3) . ?
O1R C1R 1.423(3) . ?
C14 N3 1.272(3) . ?
N3 C15 1.474(3) . ?
N4 C21 1.278(3) . ?
N4 C16 1.456(3) . ?
C15 C20 1.525(3) . ?
C15 C16 1.532(3) . ?
C16 C17 1.526(3) . ?
C17 C18 1.529(4) . ?
C18 C19 1.530(5) . ?
C19 C20 1.535(4) . ?
C21 C22 1.467(3) . ?
C22 C23 1.400(3) . ?
C22 C27 1.405(4) . ?
C23 O2 1.353(3) . ?
C23 C24 1.410(3) . ?
C24 C25 1.394(4) . ?
C24 C28 1.466(3) . ?
C25 C26 1.384(4) . ?
C26 O2R 1.372(3) . ?
C26 C27 1.391(4) . ?
O2R C2R 1.411(4) . ?
C28 N5 1.274(3) . ?
N5 C29 1.469(3) . ?
N6 C35 1.269(3) . ?
N6 C30 1.459(3) . ?
C29 C34 1.540(3) . ?
C29 C30 1.540(3) . ?
C30 C31 1.522(3) . ?
C31 C32 1.536(3) . ?
C32 C33 1.532(4) . ?
C33 C34 1.521(4) . ?
C35 C36 1.469(3) . ?
C36 C41 1.371(4) . ?
C36 C37 1.415(3) . ?
C37 O3 1.344(3) . ?
C37 C38 1.412(3) . ?
C38 C39 1.384(3) . ?
C38 C42 1.477(3) . ?
C39 C40 1.376(3) . ?
C40 O3R 1.385(3) . ?
C40 C41 1.406(4) . ?
O3R C3R 1.415(4) . ?
C51 N11 1.456(3) . ?
C51 C52 1.527(3) . ?
C51 C56 1.533(4) . ?
C52 N12 1.457(3) . ?
C52 C53 1.530(3) . ?
C53 C54 1.517(5) . ?
C54 C55 1.513(4) . ?
C55 C56 1.532(3) . ?
N11 C92 1.280(3) . ?
N12 C57 1.266(3) . ?
C57 C58 1.459(4) . ?
C58 C63 1.390(4) . ?
C58 C59 1.416(3) . ?
C59 O4 1.343(3) . ?
C59 C60 1.411(3) . ?
C60 C61 1.397(4) . ?
C60 C64 1.471(4) . ?
C61 C62 1.404(4) . ?
C62 O4R 1.365(4) . ?
C62 C63 1.384(4) . ?
O4R C4R 1.408(4) . ?
C64 N13 1.290(4) . ?
N13 C65 1.450(3) . ?
N14 C71 1.262(3) . ?
N14 C66 1.464(3) . ?
C65 C70 1.522(4) . ?
C65 C66 1.535(3) . ?
C66 C67 1.531(4) . ?
C67 C68 1.518(4) . ?
C68 C69 1.544(4) . ?
C69 C70 1.508(4) . ?
C71 C72 1.473(3) . ?
C72 C73 1.392(3) . ?
C72 C77 1.403(3) . ?
C73 O5 1.351(3) . ?
C73 C74 1.408(3) . ?
C74 C75 1.400(3) . ?
C74 C78 1.471(3) . ?
C75 C76 1.387(3) . ?
C76 O5R 1.381(3) . ?
C76 C77 1.384(4) . ?
O5R C5R 1.409(3) . ?
C78 N15 1.268(3) . ?
N15 C79 1.454(3) . ?
N16 C85 1.269(3) . ?
N16 C80 1.469(3) . ?
C79 C84 1.526(3) . ?
C79 C80 1.540(3) . ?
C80 C81 1.531(3) . ?
C81 C82 1.524(3) . ?
C82 C83 1.531(4) . ?
C83 C84 1.521(3) . ?
C85 C86 1.471(3) . ?
C86 C91 1.375(3) . ?
C86 C87 1.420(3) . ?
C87 O6 1.361(3) . ?
C87 C88 1.391(3) . ?
C88 C89 1.411(3) . ?
C88 C92 1.469(3) . ?
C89 C90 1.396(3) . ?
C90 O6R 1.362(3) . ?
C90 C91 1.395(3) . ?
O6R C6R 1.434(3) . ?
C1S C2S 1.498(7) . ?
C2S O3S 1.414(4) . ?
O3S C4S 1.416(5) . ?
C4S C5S 1.453(6) . ?

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
N1 C1 C2 110.1(2) . . ?
N1 C1 C6 109.43(19) . . ?
C2 C1 C6 110.46(18) . . ?
N2 C2 C1 110.26(16) . . ?
N2 C2 C3 107.35(17) . . ?
C1 C2 C3 110.30(19) . . ?
C2 C3 C4 111.67(19) . . ?
C5 C4 C3 111.18(19) . . ?
C4 C5 C6 111.7(2) . . ?
C5 C6 C1 111.86(19) . . ?
C42 N1 C1 117.0(2) . . ?
C7 N2 C2 119.61(18) . . ?
N2 C7 C8 121.3(2) . . ?
C13 C8 C9 120.08(19) . . ?
C13 C8 C7 119.19(19) . . ?
C9 C8 C7 120.7(2) . . ?
O1 C9 C8 121.41(18) . . ?
O1 C9 C10 119.50(19) . . ?
C8 C9 C10 119.1(2) . . ?
C11 C10 C9 119.80(19) . . ?
C11 C10 C14 121.33(18) . . ?
C9 C10 C14 118.8(2) . . ?
C10 C11 C12 121.78(19) . . ?
O1R C12 C13 125.4(2) . . ?
O1R C12 C11 115.9(2) . . ?
C13 C12 C11 118.8(2) . . ?
C12 C13 C8 120.5(2) . . ?
C12 O1R C1R 117.24(19) . . ?
N3 C14 C10 121.7(2) . . ?
C14 N3 C15 116.59(19) . . ?
C21 N4 C16 119.4(2) . . ?
N3 C15 C20 107.99(18) . . ?
N3 C15 C16 108.9(2) . . ?
C20 C15 C16 110.61(18) . . ?
N4 C16 C17 108.9(2) . . ?
N4 C16 C15 109.01(17) . . ?
C17 C16 C15 109.7(2) . . ?
C16 C17 C18 111.9(2) . . ?
C17 C18 C19 109.8(2) . . ?
C18 C19 C20 108.6(3) . . ?
C15 C20 C19 111.4(2) . . ?
N4 C21 C22 120.6(2) . . ?
C23 C22 C27 120.1(2) . . ?
C23 C22 C21 121.0(2) . . ?
C27 C22 C21 118.8(2) . . ?
O2 C23 C22 121.7(2) . . ?
O2 C23 C24 118.5(2) . . ?
C22 C23 C24 119.9(2) . . ?
C25 C24 C23 118.8(2) . . ?
C25 C24 C28 121.5(2) . . ?
C23 C24 C28 119.7(2) . . ?
C26 C25 C24 121.5(2) . . ?
O2R C26 C25 115.5(2) . . ?
O2R C26 C27 124.4(2) . . ?
C25 C26 C27 120.1(2) . . ?
C26 C27 C22 119.6(2) . . ?
C26 O2R C2R 117.2(2) . . ?
N5 C28 C24 122.9(2) . . ?
C28 N5 C29 116.9(2) . . ?
C35 N6 C30 119.59(19) . . ?
N5 C29 C34 109.81(18) . . ?
N5 C29 C30 108.3(2) . . ?
C34 C29 C30 110.27(18) . . ?
N6 C30 C31 108.82(17) . . ?
N6 C30 C29 109.43(17) . . ?
C31 C30 C29 110.4(2) . . ?
C30 C31 C32 111.82(19) . . ?
C33 C32 C31 110.2(2) . . ?
C34 C33 C32 110.4(2) . . ?
C33 C34 C29 111.8(2) . . ?
N6 C35 C36 122.2(2) . . ?
C41 C36 C37 120.6(2) . . ?
C41 C36 C35 119.7(2) . . ?
C37 C36 C35 119.7(2) . . ?
O3 C37 C38 119.08(19) . . ?
O3 C37 C36 121.93(19) . . ?
C38 C37 C36 119.0(2) . . ?
C39 C38 C37 119.3(2) . . ?
C39 C38 C42 121.5(2) . . ?
C37 C38 C42 119.2(2) . . ?
C40 C39 C38 121.2(2) . . ?
C39 C40 O3R 116.0(2) . . ?
C39 C40 C41 120.0(2) . . ?
O3R C40 C41 124.0(2) . . ?
C36 C41 C40 119.8(2) . . ?
C40 O3R C3R 117.8(2) . . ?
N1 C42 C38 122.5(2) . . ?
N11 C51 C52 109.14(17) . . ?
N11 C51 C56 108.13(19) . . ?
C52 C51 C56 109.9(2) . . ?
N12 C52 C51 111.0(2) . . ?
N12 C52 C53 108.4(2) . . ?
C51 C52 C53 111.39(19) . . ?
C54 C53 C52 111.1(2) . . ?
C55 C54 C53 110.8(3) . . ?
C54 C55 C56 111.2(2) . . ?
C55 C56 C51 111.8(2) . . ?
C92 N11 C51 120.20(19) . . ?
C57 N12 C52 116.7(2) . . ?
N12 C57 C58 123.7(3) . . ?
C63 C58 C59 120.2(2) . . ?
C63 C58 C57 121.8(2) . . ?
C59 C58 C57 118.0(2) . . ?
O4 C59 C60 122.2(2) . . ?
O4 C59 C58 119.8(2) . . ?
C60 C59 C58 117.9(2) . . ?
C61 C60 C59 120.9(2) . . ?
C61 C60 C64 119.1(2) . . ?
C59 C60 C64 120.1(2) . . ?
C60 C61 C62 120.5(2) . . ?
O4R C62 C63 115.5(3) . . ?
O4R C62 C61 125.8(3) . . ?
C63 C62 C61 118.7(3) . . ?
C62 C63 C58 121.8(2) . . ?
C62 O4R C4R 117.1(3) . . ?
N13 C64 C60 121.2(2) . . ?
C64 N13 C65 119.7(2) . . ?
C71 N14 C66 115.9(2) . . ?
N13 C65 C70 108.9(2) . . ?
N13 C65 C66 110.40(18) . . ?
C70 C65 C66 110.0(2) . . ?
N14 C66 C67 108.91(19) . . ?
N14 C66 C65 109.6(2) . . ?
C67 C66 C65 111.15(18) . . ?
C68 C67 C66 112.1(2) . . ?
C67 C68 C69 110.6(3) . . ?
C70 C69 C68 111.5(2) . . ?
C69 C70 C65 111.7(2) . . ?
N14 C71 C72 123.1(2) . . ?
C73 C72 C77 119.7(2) . . ?
C73 C72 C71 120.0(2) . . ?
C77 C72 C71 120.3(2) . . ?
O5 C73 C72 118.4(2) . . ?
O5 C73 C74 121.92(19) . . ?
C72 C73 C74 119.7(2) . . ?
C75 C74 C73 119.9(2) . . ?
C75 C74 C78 119.9(2) . . ?
C73 C74 C78 120.2(2) . . ?
C76 C75 C74 120.1(2) . . ?
O5R C76 C77 115.2(2) . . ?
O5R C76 C75 124.6(2) . . ?
C77 C76 C75 120.2(2) . . ?
C76 C77 C72 120.5(2) . . ?
C76 O5R C5R 115.7(2) . . ?
N15 C78 C74 120.5(2) . . ?
C78 N15 C79 121.2(2) . . ?
C85 N16 C80 116.35(19) . . ?
N15 C79 C84 108.62(18) . . ?
N15 C79 C80 108.40(16) . . ?
C84 C79 C80 110.5(2) . . ?
N16 C80 C81 109.49(18) . . ?
N16 C80 C79 109.25(19) . . ?
C81 C80 C79 110.87(16) . . ?
C82 C81 C80 111.37(19) . . ?
C81 C82 C83 109.3(2) . . ?
C84 C83 C82 109.6(2) . . ?
C83 C84 C79 113.7(2) . . ?
N16 C85 C86 121.9(2) . . ?
C91 C86 C87 118.40(19) . . ?
C91 C86 C85 121.62(19) . . ?
C87 C86 C85 120.0(2) . . ?
O6 C87 C88 122.08(19) . . ?
O6 C87 C86 118.13(19) . . ?
C88 C87 C86 119.8(2) . . ?
C87 C88 C89 120.4(2) . . ?
C87 C88 C92 120.8(2) . . ?
C89 C88 C92 118.8(2) . . ?
C90 C89 C88 119.8(2) . . ?
O6R C90 C91 116.0(2) . . ?
O6R C90 C89 125.4(2) . . ?
C91 C90 C89 118.6(2) . . ?
C86 C91 C90 122.9(2) . . ?
C90 O6R C6R 117.1(2) . . ?
N11 C92 C88 121.12(19) . . ?
O3S C2S C1S 108.4(4) . . ?
C2S O3S C4S 112.0(3) . . ?
O3S C4S C5S 105.7(4) . . ?

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
_platon_squeeze_void_content
1 0.657 0.783 0.010 445 137 ' '
_platon_squeeze_details          
;
The unit cell contains 3 molecules of any combination
of methylene chloride and ethyl diether which have
been treated as a diffuse contribution to 
the overall scattering without
specific atom positions by SQUEEZE in PLATON.
;

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        76.50
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.040
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3f
_database_code_depnum_ccdc_archive 'CCDC 1422962'
_audit_update_record             
;
2015-10-29 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H72 N6 O3'
_chemical_formula_sum            'C54 H72 N6 O3'
_chemical_formula_weight         853.18
_chemical_absolute_configuration rm

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           hexagonal
_symmetry_space_group_name_H-M   'P 63 2 2'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   18.740(3)
_cell_length_b                   18.740(3)
_cell_length_c                   22.056(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6708.3(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9998
_cell_measurement_theta_min      1.85
_cell_measurement_theta_max      25.65

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7021
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36164
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.65
_reflns_number_total             4243
_reflns_number_gt                3903
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2012.10-0 (Bruker AXS, 2005-2012)'
_computing_cell_refinement       'APEX2 v2012.10-0 (Bruker AXS, 2005-2012)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0598P)²+1.0891P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(17)
_refine_ls_number_reflns         4243
_refine_ls_number_parameters     193
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1172
_refine_ls_wR_factor_gt          0.1151
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_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 0.50299(9) 0.37870(8) 0.32070(5) 0.0505(4) Uani 1 1 d . . .
N2 N 0.58545(10) 0.53178(9) 0.35129(6) 0.0393(3) Uani 1 1 d . . .
C8 C 0.52691(11) 0.42327(10) 0.42486(7) 0.0360(4) Uani 1 1 d . . .
C11 C 0.44046(11) 0.25972(11) 0.46035(8) 0.0403(4) Uani 1 1 d . . .
H11 H 0.4107 0.2036 0.4725 0.048 Uiso 1 1 calc R . .
C7 C 0.57373(11) 0.50976(10) 0.40755(7) 0.0357(4) Uani 1 1 d . . .
H7 H 0.5961 0.5508 0.4382 0.043 Uiso 1 1 calc R . .
C9 C 0.51500(11) 0.40193(10) 0.48613(7) 0.0366(4) Uani 1 1 d . . .
H9 H 0.5375 0.4443 0.5158 0.044 Uiso 1 1 calc R . .
C18 C 0.42431(11) 0.21229(11) 0.35334(7) 0.0436(4) Uani 1 1 d . . .
H18 H 0.4439 0.2272 0.3130 0.052 Uiso 1 1 calc R . .
C10 C 0.47107(11) 0.32015(11) 0.50481(7) 0.0371(4) Uani 1 1 d . . .
C13 C 0.49465(11) 0.36110(10) 0.38028(7) 0.0383(4) Uani 1 1 d . . .
C12 C 0.45167(12) 0.27806(11) 0.39828(8) 0.0411(4) Uani 1 1 d . . .
N1 N 0.76074(11) 0.62317(10) 0.36444(6) 0.0454(4) Uani 1 1 d . . .
C14 C 0.45565(12) 0.29454(11) 0.57241(8) 0.0441(4) Uani 1 1 d . . .
C4 C 0.63776(15) 0.72817(12) 0.26770(8) 0.0517(5) Uani 1 1 d . . .
H4A H 0.6089 0.7386 0.2343 0.062 Uiso 1 1 calc R . .
H4B H 0.6422 0.7639 0.3022 0.062 Uiso 1 1 calc R . .
C1 C 0.71792(12) 0.63948(11) 0.31493(7) 0.0421(4) Uani 1 1 d . . .
H1 H 0.7125 0.6043 0.2792 0.050 Uiso 1 1 calc R . .
C2 C 0.63264(12) 0.61889(10) 0.33678(7) 0.0380(4) Uani 1 1 d . . .
H2 H 0.6379 0.6521 0.3737 0.046 Uiso 1 1 calc R . .
C3 C 0.58733(13) 0.63743(11) 0.28715(8) 0.0444(5) Uani 1 1 d . . .
H3A H 0.5328 0.6257 0.3024 0.053 Uiso 1 1 calc R . .
H3B H 0.5783 0.6014 0.2517 0.053 Uiso 1 1 calc R . .
C17 C 0.36215(14) 0.24677(17) 0.58332(10) 0.0694(7) Uani 1 1 d . . .
H17A H 0.3512 0.2318 0.6263 0.104 Uiso 1 1 calc R . .
H17B H 0.3370 0.1967 0.5585 0.104 Uiso 1 1 calc R . .
H17C H 0.3387 0.2814 0.5721 0.104 Uiso 1 1 calc R . .
C15 C 0.49643(14) 0.36855(12) 0.61421(8) 0.0522(5) Uani 1 1 d . . .
H15A H 0.4707 0.4026 0.6087 0.078 Uiso 1 1 calc R . .
H15B H 0.5553 0.4011 0.6045 0.078 Uiso 1 1 calc R . .
H15C H 0.4897 0.3498 0.6564 0.078 Uiso 1 1 calc R . .
C16 C 0.49227(15) 0.23882(13) 0.58633(8) 0.0583(6) Uani 1 1 d . . .
H16A H 0.4796 0.2194 0.6283 0.087 Uiso 1 1 calc R . .
H16B H 0.5522 0.2702 0.5808 0.087 Uiso 1 1 calc R . .
H16C H 0.4684 0.1915 0.5588 0.087 Uiso 1 1 calc R . .
C6 C 0.76816(16) 0.73079(14) 0.29698(10) 0.0634(6) Uani 1 1 d . . .
H6A H 0.8229 0.7434 0.2816 0.076 Uiso 1 1 calc R . .
H6B H 0.7766 0.7658 0.3329 0.076 Uiso 1 1 calc R . .
C5 C 0.72157(16) 0.74940(13) 0.24732(9) 0.0625(6) Uani 1 1 d . . .
H5A H 0.7532 0.8086 0.2368 0.075 Uiso 1 1 calc R . .
H5B H 0.7172 0.7174 0.2104 0.075 Uiso 1 1 calc R . .
H10 H 0.5388 0.4310 0.3221 0.075 Uiso 1 1 d R . .


_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 C13 1.345(2) . ?
N2 C7 1.2914(19) . ?
N2 C2 1.451(2) . ?
C8 C9 1.395(2) . ?
C8 C13 1.409(2) . ?
C8 C7 1.456(2) . ?
C11 C10 1.387(2) . ?
C11 C12 1.401(2) . ?
C9 C10 1.391(2) . ?
C18 N1 1.252(2) 3_655 ?
C18 C12 1.460(3) . ?
C10 C14 1.549(2) . ?
C13 C12 1.405(2) . ?
N1 C18 1.252(2) 5_665 ?
N1 C1 1.475(2) . ?
C14 C15 1.516(3) . ?
C14 C17 1.537(3) . ?
C14 C16 1.540(3) . ?
C4 C5 1.484(3) . ?
C4 C3 1.537(3) . ?
C1 C2 1.523(3) . ?
C1 C6 1.536(3) . ?
C2 C3 1.528(2) . ?
C6 C5 1.545(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N2 C2 118.82(14) . . ?
C9 C8 C13 119.86(15) . . ?
C9 C8 C7 119.60(15) . . ?
C13 C8 C7 120.53(14) . . ?
C10 C11 C12 122.70(15) . . ?
N2 C7 C8 121.28(15) . . ?
C10 C9 C8 121.64(15) . . ?
N1 C18 C12 124.38(16) 3_655 . ?
C11 C10 C9 117.74(14) . . ?
C11 C10 C14 119.39(15) . . ?
C9 C10 C14 122.87(15) . . ?
O1 C13 C12 118.67(15) . . ?
O1 C13 C8 122.00(15) . . ?
C12 C13 C8 119.33(15) . . ?
C11 C12 C13 118.71(15) . . ?
C11 C12 C18 120.64(15) . . ?
C13 C12 C18 120.51(15) . . ?
C18 N1 C1 117.39(15) 5_665 . ?
C15 C14 C17 110.14(17) . . ?
C15 C14 C16 107.90(17) . . ?
C17 C14 C16 109.79(17) . . ?
C15 C14 C10 111.80(14) . . ?
C17 C14 C10 108.25(16) . . ?
C16 C14 C10 108.95(15) . . ?
C5 C4 C3 111.34(15) . . ?
N1 C1 C2 108.91(13) . . ?
N1 C1 C6 109.13(17) . . ?
C2 C1 C6 110.17(14) . . ?
N2 C2 C1 109.08(12) . . ?
N2 C2 C3 108.56(15) . . ?
C1 C2 C3 110.35(13) . . ?
C2 C3 C4 110.33(16) . . ?
C1 C6 C5 109.47(19) . . ?
C4 C5 C6 111.50(16) . . ?

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
_platon_squeeze_void_content
1 0.000 0.000 -0.006 1549 160 ' '
2 0.333 0.667 0.250 132 22 ' '
3 0.333 0.667 0.750 192 40 ' '
4 0.667 0.333 0.750 132 21 ' '
5 0.666 0.333 0.250 192 40 ' '
_platon_squeeze_details          
;
283 electrons - approx. 16 molecules of methanol squeezed
;


_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.65
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.137
_refine_diff_density_rms         0.030
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3fsCO2
_database_code_depnum_ccdc_archive 'CCDC 1422963'
_audit_update_record             
;
2015-10-29 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H72 N6 O3'
_chemical_formula_weight         853.18
_chemical_absolute_configuration rm

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           hexagonal
_symmetry_space_group_name_H-M   'P 63 2 2'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   18.640(3)
_cell_length_b                   18.640
_cell_length_c                   22.083(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6644.8(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8415
_cell_measurement_theta_min      1.84
_cell_measurement_theta_max      25.39

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6512
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34249
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         25.39
_reflns_number_total             4090
_reflns_number_gt                3218
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0700P)²+0.2762P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.8(19)
_refine_ls_number_reflns         4090
_refine_ls_number_parameters     193
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1271
_refine_ls_wR_factor_gt          0.1206
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.38427(12) 0.37210(14) 0.16669(8) 0.0383(5) Uani 1 1 d . . .
H1 H 0.3511 0.3668 0.1296 0.046 Uiso 1 1 calc R . .
C2 C 0.36209(13) 0.28682(15) 0.18855(9) 0.0415(5) Uani 1 1 d . . .
H2 H 0.3975 0.2921 0.2242 0.050 Uiso 1 1 calc R . .
C3 C 0.27025(15) 0.23787(19) 0.20747(11) 0.0609(7) Uani 1 1 d . . .
H3B H 0.2346 0.2291 0.1718 0.073 Uiso 1 1 calc R . .
H3A H 0.2570 0.1829 0.2234 0.073 Uiso 1 1 calc R . .
C4 C 0.25325(16) 0.28557(18) 0.25602(11) 0.0620(8) Uani 1 1 d . . .
H4B H 0.1937 0.2549 0.2667 0.074 Uiso 1 1 calc R . .
H4A H 0.2853 0.2897 0.2929 0.074 Uiso 1 1 calc R . .
C5 C 0.27642(14) 0.37084(17) 0.23484(9) 0.0536(7) Uani 1 1 d . . .
H5B H 0.2671 0.4010 0.2680 0.064 Uiso 1 1 calc R . .
H5A H 0.2404 0.3666 0.2005 0.064 Uiso 1 1 calc R . .
C6 C 0.36621(14) 0.41903(15) 0.21515(9) 0.0465(6) Uani 1 1 d . . .
H6B H 0.4025 0.4287 0.2506 0.056 Uiso 1 1 calc R . .
H6A H 0.3786 0.4736 0.1990 0.056 Uiso 1 1 calc R . .
N1 N 0.47149(10) 0.41740(11) 0.15167(7) 0.0366(4) Uani 1 1 d . . .
N2 N 0.37692(12) 0.24253(13) 0.14035(8) 0.0460(5) Uani 1 1 d . . .
C7 C 0.42904(13) 0.21957(14) 0.15049(9) 0.0399(5) Uani 1 1 d . . .
H7 H 0.4526 0.2282 0.1898 0.048 Uiso 1 1 calc R . .
C8 C 0.45496(14) 0.18031(13) 0.10478(9) 0.0383(5) Uani 1 1 d . . .
C9 C 0.49645(13) 0.13909(12) 0.12276(8) 0.0353(5) Uani 1 1 d . . .
C10 C 0.52591(13) 0.10615(12) 0.07911(9) 0.0354(5) Uani 1 1 d . . .
C11 C 0.51241(14) 0.11431(12) 0.01757(9) 0.0389(5) Uani 1 1 d . . .
H11 H 0.5325 0.0917 -0.0120 0.047 Uiso 1 1 calc R . .
C12 C 0.47080(14) 0.15434(13) -0.00120(9) 0.0407(5) Uani 1 1 d . . .
C13 C 0.44242(14) 0.18680(13) 0.04347(9) 0.0411(5) Uani 1 1 d . . .
H13 H 0.4134 0.2144 0.0316 0.049 Uiso 1 1 calc R . .
C14 C 0.45490(16) 0.16461(15) -0.06840(10) 0.0480(6) Uani 1 1 d . . .
C15 C 0.4956(2) 0.25727(17) -0.08265(10) 0.0652(8) Uani 1 1 d . . .
H15A H 0.5551 0.2842 -0.0741 0.098 Uiso 1 1 calc R . .
H15B H 0.4706 0.2822 -0.0575 0.098 Uiso 1 1 calc R . .
H15C H 0.4872 0.2647 -0.1255 0.098 Uiso 1 1 calc R . .
C16 C 0.49284(18) 0.12759(18) -0.11046(10) 0.0588(7) Uani 1 1 d . . .
H16A H 0.4665 0.0678 -0.1033 0.088 Uiso 1 1 calc R . .
H16B H 0.5524 0.1536 -0.1025 0.088 Uiso 1 1 calc R . .
H16C H 0.4840 0.1376 -0.1527 0.088 Uiso 1 1 calc R . .
C17 C 0.36191(18) 0.1222(2) -0.07908(11) 0.0725(9) Uani 1 1 d . . .
H17A H 0.3512 0.1283 -0.1217 0.109 Uiso 1 1 calc R . .
H17B H 0.3381 0.1478 -0.0533 0.109 Uiso 1 1 calc R . .
H17C H 0.3365 0.0633 -0.0691 0.109 Uiso 1 1 calc R . .
C18 C 0.57009(14) 0.06359(12) 0.09612(9) 0.0360(5) Uani 1 1 d . . .
H18 H 0.5901 0.0424 0.0654 0.043 Uiso 1 1 calc R . .
O1 O 0.50764(9) 0.13243(9) 0.18251(6) 0.0409(4) Uani 1 1 d . . .
H1O H 0.5388 0.1019 0.1841 0.049 Uiso 1 1 d R . .


_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 N1 1.447(3) . ?
C1 C2 1.508(3) . ?
C1 C6 1.523(3) . ?
C2 N2 1.456(3) . ?
C2 C3 1.541(3) . ?
C3 C4 1.524(4) . ?
C4 C5 1.498(4) . ?
C5 C6 1.515(3) . ?
N1 C18 1.277(2) 5_665 ?
N2 C7 1.262(3) . ?
C7 C8 1.463(3) . ?
C8 C13 1.389(3) . ?
C8 C9 1.393(3) . ?
C9 O1 1.351(2) . ?
C9 C10 1.395(3) . ?
C10 C11 1.404(3) . ?
C10 C18 1.450(3) . ?
C11 C12 1.382(3) . ?
C12 C13 1.393(3) . ?
C12 C14 1.544(3) . ?
C14 C17 1.521(4) . ?
C14 C16 1.525(3) . ?
C14 C15 1.532(4) . ?
C18 N1 1.278(2) 3_655 ?

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
N1 C1 C2 108.93(15) . . ?
N1 C1 C6 109.42(18) . . ?
C2 C1 C6 110.97(16) . . ?
N2 C2 C1 109.51(17) . . ?
N2 C2 C3 109.40(19) . . ?
C1 C2 C3 110.41(18) . . ?
C4 C3 C2 109.8(2) . . ?
C5 C4 C3 111.4(2) . . ?
C4 C5 C6 111.44(19) . . ?
C5 C6 C1 110.9(2) . . ?
C18 N1 C1 119.42(17) 5_665 . ?
C7 N2 C2 117.34(17) . . ?
N2 C7 C8 123.36(19) . . ?
C13 C8 C9 119.33(19) . . ?
C13 C8 C7 121.09(19) . . ?
C9 C8 C7 119.51(18) . . ?
O1 C9 C8 118.87(17) . . ?
O1 C9 C10 121.44(18) . . ?
C8 C9 C10 119.69(18) . . ?
C9 C10 C11 119.34(18) . . ?
C9 C10 C18 121.22(18) . . ?
C11 C10 C18 119.44(18) . . ?
C12 C11 C10 121.88(19) . . ?
C11 C12 C13 117.38(18) . . ?
C11 C12 C14 123.34(19) . . ?
C13 C12 C14 119.28(19) . . ?
C8 C13 C12 122.38(19) . . ?
C17 C14 C16 109.7(2) . . ?
C17 C14 C15 110.3(2) . . ?
C16 C14 C15 107.7(2) . . ?
C17 C14 C12 108.9(2) . . ?
C16 C14 C12 111.60(18) . . ?
C15 C14 C12 108.64(18) . . ?
N1 C18 C10 121.18(18) 3_655 . ?

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
_platon_squeeze_void_content
1 0.000 0.000 -0.006 1584 92 ' '
2 0.333 0.667 0.250 132 8 ' '
3 0.333 0.667 0.750 165 11 ' '
4 0.667 0.333 0.750 132 8 ' '
5 0.667 0.333 0.250 165 11 ' '
_platon_squeeze_details          ?


_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.39
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.033
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3g
_database_code_depnum_ccdc_archive 'CCDC 1422964'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C99 H90 N6 O3, 4(C H2 Cl2), C H4 O'
_chemical_formula_sum            'C104 H102 Cl8 N6 O4'
_chemical_formula_weight         1783.52
_chemical_absolute_configuration rm

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   14.177(2)
_cell_length_b                   21.094(3)
_cell_length_c                   32.557(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9736(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    30861
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      66.60

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3744
_exptl_absorpt_coefficient_mu    2.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.49489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.4 Empirical absorption correction 
using spherical harmonics, implemented 
in SCALE3 ABSPACK scaling algorithm.
;


_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Atlas detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            51554
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         66.60
_reflns_number_total             17185
_reflns_number_gt                15826
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,v. 1.171.35.4 
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,v. 1.171.35.4 
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies, v. 1.171.35.4
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1220P)²+1.9807P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.060(12)
_refine_ls_number_reflns         17185
_refine_ls_number_parameters     1120
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1755
_refine_ls_wR_factor_gt          0.1704
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.047
_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 0.9918(2) 0.71512(15) 1.15683(11) 0.0422(7) Uani 1 1 d . . .
H1 H 0.9675 0.6911 1.1325 0.051 Uiso 1 1 calc R . .
C2 C 1.0922(2) 0.73887(14) 1.14797(10) 0.0379(6) Uani 1 1 d . . .
H2 H 1.1155 0.7644 1.1718 0.045 Uiso 1 1 calc R . .
C3 C 1.1578(3) 0.68281(18) 1.14078(12) 0.0509(8) Uani 1 1 d . . .
H3A H 1.2225 0.6985 1.1355 0.061 Uiso 1 1 calc R . .
H3B H 1.1367 0.6590 1.1162 0.061 Uiso 1 1 calc R . .
C4 C 1.1586(3) 0.6386(2) 1.17799(14) 0.0629(10) Uani 1 1 d . . .
H4A H 1.1993 0.6016 1.1720 0.076 Uiso 1 1 calc R . .
H4B H 1.1861 0.6613 1.2018 0.076 Uiso 1 1 calc R . .
C5 C 1.0621(4) 0.6159(2) 1.18906(18) 0.0747(13) Uani 1 1 d . . .
H5A H 1.0653 0.5914 1.2150 0.090 Uiso 1 1 calc R . .
H5B H 1.0385 0.5873 1.1672 0.090 Uiso 1 1 calc R . .
C6 C 0.9926(3) 0.67186(19) 1.19442(14) 0.0602(10) Uani 1 1 d . . .
H6A H 0.9283 0.6550 1.1991 0.072 Uiso 1 1 calc R . .
H6B H 1.0109 0.6968 1.2189 0.072 Uiso 1 1 calc R . .
N1 N 0.92853(18) 0.76818(12) 1.16582(8) 0.0394(5) Uani 1 1 d . . .
N2 N 1.08912(17) 0.77845(12) 1.11131(8) 0.0365(5) Uani 1 1 d . . .
C7 C 1.1129(2) 0.83657(14) 1.11383(9) 0.0350(6) Uani 1 1 d . . .
H7 H 1.1320 0.8533 1.1396 0.042 Uiso 1 1 calc R . .
C8 C 1.1112(2) 0.87793(13) 1.07805(9) 0.0336(6) Uani 1 1 d . . .
C9 C 1.08656(19) 0.85467(13) 1.03908(9) 0.0313(5) Uani 1 1 d . . .
C10 C 1.0923(2) 0.89418(13) 1.00435(9) 0.0332(6) Uani 1 1 d . . .
C11 C 1.1143(2) 0.95840(14) 1.01072(9) 0.0355(6) Uani 1 1 d . . .
H11 H 1.1165 0.9859 0.9876 0.043 Uiso 1 1 calc R . .
C12 C 1.1329(2) 0.98341(14) 1.04933(10) 0.0365(6) Uani 1 1 d . . .
C13 C 1.1355(2) 0.94181(14) 1.08219(10) 0.0378(6) Uani 1 1 d . . .
H13 H 1.1545 0.9572 1.1083 0.045 Uiso 1 1 calc R . .
C14 C 1.1594(2) 1.05400(13) 1.05641(10) 0.0391(7) Uani 1 1 d . . .
C15 C 1.1019(2) 1.08455(14) 1.09143(11) 0.0403(7) Uani 1 1 d . . .
C16 C 1.0294(2) 1.05501(16) 1.11305(11) 0.0452(7) Uani 1 1 d . . .
H16 H 1.0117 1.0129 1.1061 0.054 Uiso 1 1 calc R . .
C17 C 0.9823(3) 1.08633(18) 1.14468(11) 0.0505(8) Uani 1 1 d . . .
H17 H 0.9343 1.0651 1.1597 0.061 Uiso 1 1 calc R . .
C18 C 1.0055(3) 1.14892(18) 1.15435(12) 0.0544(9) Uani 1 1 d . . .
H18 H 0.9742 1.1703 1.1761 0.065 Uiso 1 1 calc R . .
C19 C 1.0739(3) 1.17887(17) 1.13214(12) 0.0559(9) Uani 1 1 d . . .
H19 H 1.0887 1.2218 1.1382 0.067 Uiso 1 1 calc R . .
C20 C 1.1221(3) 1.14829(15) 1.10110(12) 0.0492(8) Uani 1 1 d . . .
H20 H 1.1693 1.1704 1.0861 0.059 Uiso 1 1 calc R . .
C21 C 1.2664(2) 1.05167(14) 1.06754(13) 0.0490(8) Uani 1 1 d . . .
C22 C 1.2997(3) 1.06785(18) 1.10593(15) 0.0586(10) Uani 1 1 d . . .
H22 H 1.2576 1.0843 1.1260 0.070 Uiso 1 1 calc R . .
C23 C 1.3966(3) 1.0600(2) 1.1156(2) 0.0772(15) Uani 1 1 d . . .
H23 H 1.4183 1.0709 1.1423 0.093 Uiso 1 1 calc R . .
C24 C 1.4582(3) 1.03761(19) 1.0878(3) 0.091(2) Uani 1 1 d . . .
H24 H 1.5229 1.0329 1.0948 0.110 Uiso 1 1 calc R . .
C25 C 1.4261(3) 1.02136(18) 1.0488(2) 0.090(2) Uani 1 1 d . . .
H25 H 1.4690 1.0059 1.0287 0.108 Uiso 1 1 calc R . .
C26 C 1.3298(3) 1.02793(18) 1.03917(19) 0.0702(13) Uani 1 1 d . . .
H26 H 1.3080 1.0158 1.0127 0.084 Uiso 1 1 calc R . .
C27 C 1.1366(2) 1.09396(14) 1.01792(11) 0.0410(7) Uani 1 1 d . . .
C28 C 1.2021(3) 1.13238(16) 0.99807(11) 0.0483(8) Uani 1 1 d . . .
H28 H 1.2658 1.1326 1.0070 0.058 Uiso 1 1 calc R . .
C29 C 1.1751(3) 1.17053(18) 0.96526(12) 0.0549(9) Uani 1 1 d . . .
H29 H 1.2205 1.1971 0.9525 0.066 Uiso 1 1 calc R . .
C30 C 1.0841(3) 1.17039(17) 0.95111(11) 0.0553(9) Uani 1 1 d . . .
H30 H 1.0664 1.1959 0.9283 0.066 Uiso 1 1 calc R . .
C31 C 1.0178(3) 1.13216(15) 0.97069(11) 0.0471(7) Uani 1 1 d . . .
H31 H 0.9543 1.1316 0.9614 0.057 Uiso 1 1 calc R . .
C32 C 1.0445(2) 1.09501(15) 1.00359(11) 0.0436(7) Uani 1 1 d . . .
H32 H 0.9985 1.0694 1.0168 0.052 Uiso 1 1 calc R . .
C33 C 1.0752(2) 0.86738(13) 0.96411(9) 0.0335(6) Uani 1 1 d . . .
H33 H 1.0438 0.8277 0.9626 0.040 Uiso 1 1 calc R . .
O1 O 1.06174(15) 0.79333(9) 1.03364(6) 0.0361(4) Uani 1 1 d . . .
H4 H 1.0627 0.7759 1.0560 0.043 Uiso 1 1 d R . .
C34 C 1.0744(2) 0.86111(14) 0.89248(9) 0.0377(6) Uani 1 1 d . . .
H34 H 1.0437 0.8198 0.8994 0.045 Uiso 1 1 calc R . .
C35 C 1.0045(2) 0.90231(14) 0.86814(9) 0.0383(6) Uani 1 1 d . . .
H35 H 1.0348 0.9438 0.8614 0.046 Uiso 1 1 calc R . .
C36 C 0.9760(3) 0.86857(17) 0.82812(10) 0.0484(8) Uani 1 1 d . . .
H36A H 0.9420 0.8289 0.8348 0.058 Uiso 1 1 calc R . .
H36B H 0.9329 0.8961 0.8122 0.058 Uiso 1 1 calc R . .
C37 C 1.0630(3) 0.85325(18) 0.80236(10) 0.0522(9) Uani 1 1 d . . .
H37A H 1.0924 0.8933 0.7930 0.063 Uiso 1 1 calc R . .
H37B H 1.0436 0.8290 0.7777 0.063 Uiso 1 1 calc R . .
C38 C 1.1358(3) 0.81467(18) 0.82657(10) 0.0521(9) Uani 1 1 d . . .
H38A H 1.1098 0.7722 0.8329 0.063 Uiso 1 1 calc R . .
H38B H 1.1934 0.8089 0.8098 0.063 Uiso 1 1 calc R . .
C39 C 1.1609(3) 0.84885(16) 0.86652(10) 0.0451(7) Uani 1 1 d . . .
H39A H 1.2062 0.8227 0.8823 0.054 Uiso 1 1 calc R . .
H39B H 1.1918 0.8897 0.8600 0.054 Uiso 1 1 calc R . .
N3 N 1.09966(19) 0.89390(12) 0.93058(8) 0.0373(5) Uani 1 1 d . . .
N4 N 0.92131(18) 0.91331(12) 0.89306(8) 0.0379(5) Uani 1 1 d . . .
C40 C 0.8983(2) 0.97014(14) 0.90234(9) 0.0378(6) Uani 1 1 d . . .
H40 H 0.9369 1.0041 0.8932 0.045 Uiso 1 1 calc R . .
C41 C 0.8143(2) 0.98428(14) 0.92657(9) 0.0356(6) Uani 1 1 d . . .
C42 C 0.7577(2) 0.93554(14) 0.94176(9) 0.0371(6) Uani 1 1 d . . .
C43 C 0.6746(2) 0.95033(14) 0.96433(9) 0.0378(6) Uani 1 1 d . . .
C44 C 0.6537(2) 1.01417(14) 0.97124(9) 0.0378(6) Uani 1 1 d . . .
H44 H 0.5997 1.0245 0.9872 0.045 Uiso 1 1 calc R . .
C45 C 0.7090(2) 1.06358(13) 0.95558(9) 0.0352(6) Uani 1 1 d . . .
C46 C 0.7881(2) 1.04757(14) 0.93353(9) 0.0368(6) Uani 1 1 d . . .
H46 H 0.8263 1.0805 0.9226 0.044 Uiso 1 1 calc R . .
C47 C 0.6835(2) 1.13349(13) 0.96625(10) 0.0357(6) Uani 1 1 d . . .
C48 C 0.7502(2) 1.18051(13) 0.94321(10) 0.0350(6) Uani 1 1 d . . .
C49 C 0.7513(2) 1.17904(14) 0.90017(10) 0.0399(6) Uani 1 1 d . . .
H49 H 0.7122 1.1497 0.8860 0.048 Uiso 1 1 calc R . .
C50 C 0.8086(2) 1.21985(15) 0.87795(11) 0.0437(7) Uani 1 1 d . . .
H50 H 0.8098 1.2174 0.8488 0.052 Uiso 1 1 calc R . .
C51 C 0.8636(2) 1.26391(15) 0.89795(11) 0.0442(7) Uani 1 1 d . . .
H51 H 0.9036 1.2914 0.8828 0.053 Uiso 1 1 calc R . .
C52 C 0.8602(2) 1.26780(14) 0.94016(11) 0.0422(7) Uani 1 1 d . . .
H52 H 0.8962 1.2992 0.9540 0.051 Uiso 1 1 calc R . .
C53 C 0.8044(2) 1.22593(14) 0.96281(11) 0.0399(6) Uani 1 1 d . . .
H53 H 0.8036 1.2286 0.9919 0.048 Uiso 1 1 calc R . .
C54 C 0.5838(2) 1.15288(15) 0.95180(10) 0.0385(6) Uani 1 1 d . . .
C55 C 0.5550(2) 1.21574(16) 0.95866(11) 0.0444(7) Uani 1 1 d . . .
H55 H 0.5953 1.2438 0.9733 0.053 Uiso 1 1 calc R . .
C56 C 0.4687(3) 1.23754(19) 0.94444(13) 0.0554(9) Uani 1 1 d . . .
H56 H 0.4500 1.2800 0.9499 0.067 Uiso 1 1 calc R . .
C57 C 0.4103(2) 1.1983(2) 0.92261(13) 0.0545(9) Uani 1 1 d . . .
H57 H 0.3523 1.2139 0.9120 0.065 Uiso 1 1 calc R . .
C58 C 0.4357(2) 1.1371(2) 0.91622(13) 0.0544(9) Uani 1 1 d . . .
H58 H 0.3940 1.1097 0.9018 0.065 Uiso 1 1 calc R . .
C59 C 0.5222(2) 1.11314(16) 0.93038(10) 0.0445(7) Uani 1 1 d . . .
H59 H 0.5387 1.0702 0.9254 0.053 Uiso 1 1 calc R . .
C60 C 0.6939(2) 1.13903(13) 1.01305(10) 0.0366(6) Uani 1 1 d . . .
C61 C 0.6200(3) 1.15474(15) 1.03969(11) 0.0462(7) Uani 1 1 d . . .
H61 H 0.5585 1.1611 1.0288 0.055 Uiso 1 1 calc R . .
C62 C 0.6344(3) 1.16119(18) 1.08138(12) 0.0550(9) Uani 1 1 d . . .
H62 H 0.5831 1.1719 1.0988 0.066 Uiso 1 1 calc R . .
C63 C 0.7237(3) 1.15209(16) 1.09816(11) 0.0533(9) Uani 1 1 d . . .
H63 H 0.7342 1.1579 1.1267 0.064 Uiso 1 1 calc R . .
C64 C 0.7970(3) 1.13430(16) 1.07234(11) 0.0502(8) Uani 1 1 d . . .
H64 H 0.8580 1.1268 1.0834 0.060 Uiso 1 1 calc R . .
C65 C 0.7819(2) 1.12751(15) 1.03108(11) 0.0440(7) Uani 1 1 d . . .
H65 H 0.8329 1.1145 1.0141 0.053 Uiso 1 1 calc R . .
C66 C 0.6143(2) 0.89852(14) 0.97762(9) 0.0375(6) Uani 1 1 d . . .
H66 H 0.6357 0.8564 0.9731 0.045 Uiso 1 1 calc R . .
O2 O 0.78081(16) 0.87389(9) 0.93668(7) 0.0413(5) Uani 1 1 d . . .
H3 H 0.8396 0.8768 0.9219 0.050 Uiso 1 1 d R . .
C67 C 0.4799(2) 0.84874(13) 1.00279(9) 0.0364(6) Uani 1 1 d . . .
H67 H 0.5182 0.8108 0.9950 0.044 Uiso 1 1 calc R . .
C68 C 0.4540(2) 0.84444(13) 1.04845(9) 0.0349(6) Uani 1 1 d . . .
H68 H 0.4188 0.8835 1.0568 0.042 Uiso 1 1 calc R . .
C69 C 0.3918(2) 0.78602(15) 1.05568(11) 0.0432(7) Uani 1 1 d . . .
H69A H 0.4284 0.7473 1.0493 0.052 Uiso 1 1 calc R . .
H69B H 0.3735 0.7842 1.0850 0.052 Uiso 1 1 calc R . .
C70 C 0.3038(2) 0.78739(17) 1.02946(12) 0.0484(8) Uani 1 1 d . . .
H70A H 0.2669 0.7482 1.0341 0.058 Uiso 1 1 calc R . .
H70B H 0.2641 0.8239 1.0375 0.058 Uiso 1 1 calc R . .
C71 C 0.3289(3) 0.79272(17) 0.98452(12) 0.0506(8) Uani 1 1 d . . .
H71A H 0.2704 0.7961 0.9681 0.061 Uiso 1 1 calc R . .
H71B H 0.3628 0.7540 0.9757 0.061 Uiso 1 1 calc R . .
C72 C 0.3902(3) 0.85020(16) 0.97675(11) 0.0470(7) Uani 1 1 d . . .
H72A H 0.3540 0.8891 0.9832 0.056 Uiso 1 1 calc R . .
H72B H 0.4076 0.8517 0.9473 0.056 Uiso 1 1 calc R . .
N5 N 0.53516(19) 0.90615(11) 0.99487(8) 0.0387(5) Uani 1 1 d . . .
N6 N 0.53960(18) 0.83886(12) 1.07306(8) 0.0377(5) Uani 1 1 d . . .
C73 C 0.5413(2) 0.86467(14) 1.10828(9) 0.0365(6) Uani 1 1 d . . .
H73 H 0.4888 0.8893 1.1169 0.044 Uiso 1 1 calc R . .
C74 C 0.6214(2) 0.85756(13) 1.13593(9) 0.0357(6) Uani 1 1 d . . .
C75 C 0.7033(2) 0.82352(13) 1.12421(9) 0.0347(6) Uani 1 1 d . . .
C76 C 0.7781(2) 0.81724(14) 1.15194(9) 0.0359(6) Uani 1 1 d . . .
C77 C 0.7700(2) 0.84591(14) 1.19061(9) 0.0359(6) Uani 1 1 d . . .
H77 H 0.8218 0.8430 1.2090 0.043 Uiso 1 1 calc R . .
C78 C 0.6904(2) 0.87811(14) 1.20323(9) 0.0375(6) Uani 1 1 d . . .
C79 C 0.6165(2) 0.88408(14) 1.17540(9) 0.0375(6) Uani 1 1 d . . .
H79 H 0.5615 0.9067 1.1833 0.045 Uiso 1 1 calc R . .
C80 C 0.6768(2) 0.90971(15) 1.24602(9) 0.0396(7) Uani 1 1 d . . .
C81 C 0.5957(2) 0.87853(15) 1.27053(10) 0.0407(7) Uani 1 1 d . . .
C82 C 0.5530(3) 0.82301(17) 1.25871(11) 0.0489(8) Uani 1 1 d . . .
H82 H 0.5707 0.8034 1.2336 0.059 Uiso 1 1 calc R . .
C83 C 0.4829(3) 0.7948(2) 1.28346(12) 0.0597(10) Uani 1 1 d . . .
H83 H 0.4536 0.7566 1.2747 0.072 Uiso 1 1 calc R . .
C84 C 0.4570(3) 0.8216(2) 1.31956(13) 0.0608(10) Uani 1 1 d . . .
H84 H 0.4089 0.8027 1.3358 0.073 Uiso 1 1 calc R . .
C85 C 0.5009(3) 0.8769(2) 1.33287(12) 0.0590(10) Uani 1 1 d . . .
H85 H 0.4845 0.8952 1.3586 0.071 Uiso 1 1 calc R . .
C86 C 0.5689(3) 0.90521(19) 1.30825(11) 0.0509(8) Uani 1 1 d . . .
H86 H 0.5979 0.9434 1.3171 0.061 Uiso 1 1 calc R . .
C87 C 0.7644(2) 0.90126(15) 1.27423(9) 0.0400(7) Uani 1 1 d . . .
C88 C 0.7981(3) 0.84009(16) 1.28112(10) 0.0440(7) Uani 1 1 d . . .
H88 H 0.7659 0.8050 1.2694 0.053 Uiso 1 1 calc R . .
C89 C 0.8782(3) 0.8297(2) 1.30483(11) 0.0584(9) Uani 1 1 d . . .
H89 H 0.9033 0.7882 1.3075 0.070 Uiso 1 1 calc R . .
C90 C 0.9214(3) 0.8807(3) 1.32464(12) 0.0667(11) Uani 1 1 d . . .
H90 H 0.9756 0.8739 1.3412 0.080 Uiso 1 1 calc R . .
C91 C 0.8844(3) 0.9418(2) 1.32006(12) 0.0624(10) Uani 1 1 d . . .
H91 H 0.9128 0.9767 1.3339 0.075 Uiso 1 1 calc R . .
C92 C 0.8058(3) 0.95121(18) 1.29509(11) 0.0510(8) Uani 1 1 d . . .
H92 H 0.7802 0.9926 1.2923 0.061 Uiso 1 1 calc R . .
C93 C 0.6565(3) 0.97952(16) 1.23580(9) 0.0455(7) Uani 1 1 d . . .
C94 C 0.7302(3) 1.01651(17) 1.21892(11) 0.0532(9) Uani 1 1 d . . .
H94 H 0.7919 0.9991 1.2169 0.064 Uiso 1 1 calc R . .
C95 C 0.7139(4) 1.07667(18) 1.20554(13) 0.0683(12) Uani 1 1 d . . .
H95 H 0.7647 1.1013 1.1951 0.082 Uiso 1 1 calc R . .
C96 C 0.6232(5) 1.1026(2) 1.20707(13) 0.0758(15) Uani 1 1 d . . .
H96 H 0.6118 1.1444 1.1975 0.091 Uiso 1 1 calc R . .
C97 C 0.5515(4) 1.0670(2) 1.22252(12) 0.0661(12) Uani 1 1 d . . .
H97 H 0.4895 1.0840 1.2231 0.079 Uiso 1 1 calc R . .
C98 C 0.5671(3) 1.00622(19) 1.23746(10) 0.0544(9) Uani 1 1 d . . .
H98 H 0.5163 0.9828 1.2489 0.065 Uiso 1 1 calc R . .
C99 C 0.8553(2) 0.77423(14) 1.14277(9) 0.0365(6) Uani 1 1 d . . .
H99 H 0.8516 0.7493 1.1185 0.044 Uiso 1 1 calc R . .
O3 O 0.70938(15) 0.79660(10) 1.08683(6) 0.0385(4) Uani 1 1 d . . .
H5 H 0.6648 0.8118 1.0762 0.046 Uiso 1 1 d R . .
C1S C 0.7659(3) 0.96239(18) 1.06460(12) 0.0529(8) Uani 1 1 d . . .
H1S3 H 0.7128 0.9342 1.0631 0.063 Uiso 0.21(2) 1 d PR . .
H1S4 H 0.7544 0.9993 1.0482 0.063 Uiso 0.21(2) 1 d PR . .
H1S1 H 0.7280 0.9250 1.0615 0.063 Uiso 0.79(2) 1 d PR . .
H1S2 H 0.7349 0.9960 1.0500 0.063 Uiso 0.79(2) 1 d PR . .
Cl1 Cl 0.8748(2) 0.9478(4) 1.04118(15) 0.0735(13) Uani 0.79(2) 1 d P . .
Cl2 Cl 0.7705(6) 0.9831(2) 1.11745(16) 0.0602(10) Uani 0.79(2) 1 d P . .
Cl11 Cl 0.8724(7) 0.9227(12) 1.0528(8) 0.080(4) Uani 0.21(2) 1 d P . .
Cl12 Cl 0.7924(18) 0.9790(13) 1.1132(8) 0.075(5) Uani 0.21(2) 1 d P . .
C2S C 0.8705(3) 1.3012(2) 1.20086(17) 0.0716(12) Uani 1 1 d . . .
H2S1 H 0.9144 1.3131 1.2232 0.086 Uiso 1 1 calc R . .
H2S2 H 0.9086 1.2865 1.1772 0.086 Uiso 1 1 calc R . .
Cl3 Cl 0.79741(11) 1.23850(6) 1.21786(5) 0.0894(4) Uani 1 1 d . . .
Cl4 Cl 0.80528(11) 1.36719(8) 1.18636(5) 0.1009(5) Uani 1 1 d . . .
C4S C 1.3006(4) 0.8639(3) 1.20907(15) 0.0780(13) Uani 1 1 d . . .
H4S1 H 1.3322 0.8687 1.2360 0.094 Uiso 1 1 calc R . .
H4S2 H 1.2320 0.8592 1.2140 0.094 Uiso 1 1 calc R . .
Cl7 Cl 1.32159(10) 0.93204(7) 1.17859(5) 0.0879(4) Uani 1 1 d . . .
Cl8 Cl 1.34368(10) 0.79635(6) 1.18415(4) 0.0782(3) Uani 1 1 d . . .
C5S C 1.2667(6) 0.9906(3) 0.91588(15) 0.101(2) Uani 1 1 d D . .
H5S1 H 1.2311 0.9518 0.9231 0.121 Uiso 1 1 calc R . .
H5S2 H 1.2850 1.0124 0.9416 0.121 Uiso 1 1 calc R . .
Cl9 Cl 1.19910(12) 1.03888(7) 0.88680(7) 0.1141(6) Uani 1 1 d D . .
Cl10 Cl 1.37521(12) 0.96924(8) 0.88534(7) 0.1093(5) Uani 1 1 d D . .
C6S C 1.0088(4) 0.9188(2) 1.2099(2) 0.0842(15) Uani 1 1 d . . .
H6S1 H 0.9611 0.9281 1.2308 0.126 Uiso 1 1 calc R . .
H6S2 H 0.9815 0.9250 1.1825 0.126 Uiso 1 1 calc R . .
H6S3 H 1.0628 0.9473 1.2134 0.126 Uiso 1 1 calc R . .
O6S O 1.0385(2) 0.85620(15) 1.21389(9) 0.0647(7) Uani 1 1 d . . .
H6 H 1.0091 0.8246 1.1968 0.078 Uiso 1 1 d R . .


_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 N1 1.464(4) . ?
C1 C6 1.527(5) . ?
C1 C2 1.537(5) . ?
C2 N2 1.457(4) . ?
C2 C3 1.523(4) . ?
C3 C4 1.528(6) . ?
C4 C5 1.494(7) . ?
C5 C6 1.547(6) . ?
N1 C99 1.287(4) . ?
N2 C7 1.274(4) . ?
C7 C8 1.455(4) . ?
C8 C13 1.397(4) . ?
C8 C9 1.405(4) . ?
C9 O1 1.353(3) . ?
C9 C10 1.407(4) . ?
C10 C11 1.405(4) . ?
C10 C33 1.447(4) . ?
C11 C12 1.388(4) . ?
C12 C13 1.384(5) . ?
C12 C14 1.553(4) . ?
C14 C15 1.542(4) . ?
C14 C27 1.544(5) . ?
C14 C21 1.560(4) . ?
C15 C16 1.394(5) . ?
C15 C20 1.410(4) . ?
C16 C17 1.394(5) . ?
C17 C18 1.397(5) . ?
C18 C19 1.364(6) . ?
C19 C20 1.380(5) . ?
C21 C22 1.379(6) . ?
C21 C26 1.384(6) . ?
C22 C23 1.419(6) . ?
C23 C24 1.343(9) . ?
C24 C25 1.394(10) . ?
C25 C26 1.406(7) . ?
C27 C32 1.387(5) . ?
C27 C28 1.391(5) . ?
C28 C29 1.391(6) . ?
C29 C30 1.370(6) . ?
C30 C31 1.392(5) . ?
C31 C32 1.380(5) . ?
C33 N3 1.275(4) . ?
C34 N3 1.465(4) . ?
C34 C39 1.512(4) . ?
C34 C35 1.537(4) . ?
C35 N4 1.451(4) . ?
C35 C36 1.539(5) . ?
C36 C37 1.527(5) . ?
C37 C38 1.533(5) . ?
C38 C39 1.529(5) . ?
N4 C40 1.279(4) . ?
C40 C41 1.458(4) . ?
C41 C42 1.396(4) . ?
C41 C46 1.404(4) . ?
C42 O2 1.351(4) . ?
C42 C43 1.422(4) . ?
C43 C44 1.397(4) . ?
C43 C66 1.453(4) . ?
C44 C45 1.400(4) . ?
C45 C46 1.374(4) . ?
C45 C47 1.557(4) . ?
C47 C60 1.535(4) . ?
C47 C54 1.545(4) . ?
C47 C48 1.562(4) . ?
C48 C53 1.384(4) . ?
C48 C49 1.402(5) . ?
C49 C50 1.387(5) . ?
C50 C51 1.377(5) . ?
C51 C52 1.378(5) . ?
C52 C53 1.397(5) . ?
C54 C59 1.397(5) . ?
C54 C55 1.405(5) . ?
C55 C56 1.386(5) . ?
C56 C57 1.370(6) . ?
C57 C58 1.358(6) . ?
C58 C59 1.403(5) . ?
C60 C61 1.400(5) . ?
C60 C65 1.401(5) . ?
C61 C62 1.380(5) . ?
C62 C63 1.391(6) . ?
C63 C64 1.388(6) . ?
C64 C65 1.368(5) . ?
C66 N5 1.266(4) . ?
C67 N5 1.465(4) . ?
C67 C72 1.529(5) . ?
C67 C68 1.534(4) . ?
C68 N6 1.459(4) . ?
C68 C69 1.534(4) . ?
C69 C70 1.512(5) . ?
C70 C71 1.510(6) . ?
C71 C72 1.513(5) . ?
N6 C73 1.269(4) . ?
C73 C74 1.457(4) . ?
C74 C79 1.403(4) . ?
C74 C75 1.417(4) . ?
C75 O3 1.346(4) . ?
C75 C76 1.399(4) . ?
C76 C77 1.401(4) . ?
C76 C99 1.454(4) . ?
C77 C78 1.380(4) . ?
C78 C79 1.390(5) . ?
C78 C80 1.556(4) . ?
C80 C93 1.537(4) . ?
C80 C81 1.546(5) . ?
C80 C87 1.554(5) . ?
C81 C82 1.374(5) . ?
C81 C86 1.403(5) . ?
C82 C83 1.410(5) . ?
C83 C84 1.355(6) . ?
C84 C85 1.392(7) . ?
C85 C86 1.388(6) . ?
C87 C92 1.384(5) . ?
C87 C88 1.394(5) . ?
C88 C89 1.389(6) . ?
C89 C90 1.395(7) . ?
C90 C91 1.400(7) . ?
C91 C92 1.394(6) . ?
C93 C98 1.388(6) . ?
C93 C94 1.415(6) . ?
C94 C95 1.361(5) . ?
C95 C96 1.399(8) . ?
C96 C97 1.360(8) . ?
C97 C98 1.388(6) . ?
C1S Cl12 1.66(3) . ?
C1S Cl1 1.750(5) . ?
C1S Cl11 1.769(13) . ?
C1S Cl2 1.777(6) . ?
Cl1 Cl11 0.65(2) . ?
C2S Cl4 1.737(5) . ?
C2S Cl3 1.769(5) . ?
C4S Cl8 1.749(5) . ?
C4S Cl7 1.773(6) . ?
C5S Cl9 1.688(6) . ?
C5S Cl10 1.887(7) . ?
C6S O6S 1.392(6) . ?

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
N1 C1 C6 107.6(3) . . ?
N1 C1 C2 110.8(2) . . ?
C6 C1 C2 109.8(3) . . ?
N2 C2 C3 109.7(3) . . ?
N2 C2 C1 108.2(2) . . ?
C3 C2 C1 110.0(3) . . ?
C2 C3 C4 110.9(3) . . ?
C5 C4 C3 112.4(4) . . ?
C4 C5 C6 111.4(4) . . ?
C1 C6 C5 111.8(3) . . ?
C99 N1 C1 116.9(3) . . ?
C7 N2 C2 119.4(3) . . ?
N2 C7 C8 121.4(3) . . ?
C13 C8 C9 119.0(3) . . ?
C13 C8 C7 119.8(3) . . ?
C9 C8 C7 121.2(2) . . ?
O1 C9 C8 121.1(3) . . ?
O1 C9 C10 118.4(2) . . ?
C8 C9 C10 120.3(2) . . ?
C11 C10 C9 117.7(3) . . ?
C11 C10 C33 123.2(3) . . ?
C9 C10 C33 119.1(2) . . ?
C12 C11 C10 122.8(3) . . ?
C13 C12 C11 117.6(3) . . ?
C13 C12 C14 119.1(3) . . ?
C11 C12 C14 123.0(3) . . ?
C12 C13 C8 122.0(3) . . ?
C15 C14 C27 105.2(2) . . ?
C15 C14 C12 112.5(3) . . ?
C27 C14 C12 110.6(3) . . ?
C15 C14 C21 110.8(3) . . ?
C27 C14 C21 114.1(3) . . ?
C12 C14 C21 103.9(2) . . ?
C16 C15 C20 117.6(3) . . ?
C16 C15 C14 125.2(3) . . ?
C20 C15 C14 117.1(3) . . ?
C17 C16 C15 121.0(3) . . ?
C16 C17 C18 120.1(4) . . ?
C19 C18 C17 119.1(3) . . ?
C18 C19 C20 121.6(3) . . ?
C19 C20 C15 120.6(4) . . ?
C22 C21 C26 118.1(4) . . ?
C22 C21 C14 122.4(3) . . ?
C26 C21 C14 119.3(4) . . ?
C21 C22 C23 120.3(5) . . ?
C24 C23 C22 121.3(6) . . ?
C23 C24 C25 119.3(4) . . ?
C24 C25 C26 119.7(5) . . ?
C21 C26 C25 121.2(5) . . ?
C32 C27 C28 117.5(3) . . ?
C32 C27 C14 118.6(3) . . ?
C28 C27 C14 123.8(3) . . ?
C29 C28 C27 120.7(4) . . ?
C30 C29 C28 121.0(3) . . ?
C29 C30 C31 118.8(4) . . ?
C32 C31 C30 120.0(4) . . ?
C31 C32 C27 121.9(3) . . ?
N3 C33 C10 123.9(3) . . ?
N3 C34 C39 110.8(3) . . ?
N3 C34 C35 109.1(2) . . ?
C39 C34 C35 109.3(2) . . ?
N4 C35 C34 109.0(2) . . ?
N4 C35 C36 109.5(3) . . ?
C34 C35 C36 110.1(2) . . ?
C37 C36 C35 110.5(3) . . ?
C36 C37 C38 112.0(3) . . ?
C39 C38 C37 110.1(3) . . ?
C34 C39 C38 111.6(3) . . ?
C33 N3 C34 116.8(2) . . ?
C40 N4 C35 119.3(3) . . ?
N4 C40 C41 121.9(3) . . ?
C42 C41 C46 119.4(3) . . ?
C42 C41 C40 120.7(3) . . ?
C46 C41 C40 119.9(3) . . ?
O2 C42 C41 121.7(3) . . ?
O2 C42 C43 118.4(3) . . ?
C41 C42 C43 119.9(3) . . ?
C44 C43 C42 118.1(3) . . ?
C44 C43 C66 123.5(3) . . ?
C42 C43 C66 118.4(3) . . ?
C43 C44 C45 122.7(3) . . ?
C46 C45 C44 117.7(3) . . ?
C46 C45 C47 122.6(3) . . ?
C44 C45 C47 119.6(3) . . ?
C45 C46 C41 122.3(3) . . ?
C60 C47 C54 111.7(2) . . ?
C60 C47 C45 105.7(2) . . ?
C54 C47 C45 113.3(2) . . ?
C60 C47 C48 111.7(2) . . ?
C54 C47 C48 103.9(2) . . ?
C45 C47 C48 110.7(2) . . ?
C53 C48 C49 118.0(3) . . ?
C53 C48 C47 123.7(3) . . ?
C49 C48 C47 118.2(3) . . ?
C50 C49 C48 120.9(3) . . ?
C51 C50 C49 120.3(3) . . ?
C50 C51 C52 119.5(3) . . ?
C51 C52 C53 120.6(3) . . ?
C48 C53 C52 120.6(3) . . ?
C59 C54 C55 117.6(3) . . ?
C59 C54 C47 124.4(3) . . ?
C55 C54 C47 117.9(3) . . ?
C56 C55 C54 121.1(3) . . ?
C57 C56 C55 120.5(4) . . ?
C58 C57 C56 119.6(3) . . ?
C57 C58 C59 121.6(3) . . ?
C54 C59 C58 119.6(3) . . ?
C61 C60 C65 116.7(3) . . ?
C61 C60 C47 124.2(3) . . ?
C65 C60 C47 119.2(3) . . ?
C62 C61 C60 121.4(4) . . ?
C61 C62 C63 120.5(4) . . ?
C64 C63 C62 118.7(3) . . ?
C65 C64 C63 120.4(4) . . ?
C64 C65 C60 122.1(3) . . ?
N5 C66 C43 123.9(3) . . ?
N5 C67 C72 109.3(3) . . ?
N5 C67 C68 110.3(2) . . ?
C72 C67 C68 109.8(3) . . ?
N6 C68 C69 109.2(2) . . ?
N6 C68 C67 109.8(2) . . ?
C69 C68 C67 109.5(2) . . ?
C70 C69 C68 111.9(3) . . ?
C71 C70 C69 110.8(3) . . ?
C70 C71 C72 110.9(3) . . ?
C71 C72 C67 111.7(3) . . ?
C66 N5 C67 116.5(2) . . ?
C73 N6 C68 118.5(3) . . ?
N6 C73 C74 121.9(3) . . ?
C79 C74 C75 119.2(3) . . ?
C79 C74 C73 119.1(3) . . ?
C75 C74 C73 121.6(3) . . ?
O3 C75 C76 119.7(3) . . ?
O3 C75 C74 120.7(3) . . ?
C76 C75 C74 119.7(3) . . ?
C75 C76 C77 118.5(3) . . ?
C75 C76 C99 119.9(3) . . ?
C77 C76 C99 121.1(3) . . ?
C78 C77 C76 123.2(3) . . ?
C77 C78 C79 117.8(3) . . ?
C77 C78 C80 125.3(3) . . ?
C79 C78 C80 116.9(3) . . ?
C78 C79 C74 121.6(3) . . ?
C93 C80 C81 112.3(3) . . ?
C93 C80 C87 112.8(3) . . ?
C81 C80 C87 103.9(2) . . ?
C93 C80 C78 103.9(2) . . ?
C81 C80 C78 111.8(3) . . ?
C87 C80 C78 112.4(3) . . ?
C82 C81 C86 117.9(3) . . ?
C82 C81 C80 123.1(3) . . ?
C86 C81 C80 118.9(3) . . ?
C81 C82 C83 120.7(3) . . ?
C84 C83 C82 120.6(4) . . ?
C83 C84 C85 119.9(4) . . ?
C86 C85 C84 119.4(3) . . ?
C85 C86 C81 121.4(4) . . ?
C92 C87 C88 118.7(3) . . ?
C92 C87 C80 122.8(3) . . ?
C88 C87 C80 118.4(3) . . ?
C89 C88 C87 121.0(4) . . ?
C88 C89 C90 119.6(4) . . ?
C89 C90 C91 119.8(4) . . ?
C92 C91 C90 119.5(4) . . ?
C87 C92 C91 121.1(4) . . ?
C98 C93 C94 117.7(3) . . ?
C98 C93 C80 123.5(3) . . ?
C94 C93 C80 118.3(3) . . ?
C95 C94 C93 120.9(4) . . ?
C94 C95 C96 120.6(5) . . ?
C97 C96 C95 119.0(4) . . ?
C96 C97 C98 121.3(5) . . ?
C93 C98 C97 120.4(4) . . ?
N1 C99 C76 123.3(3) . . ?
Cl12 C1S Cl11 96.4(15) . . ?
Cl1 C1S Cl2 115.6(4) . . ?
Cl4 C2S Cl3 111.8(3) . . ?
Cl8 C4S Cl7 110.0(3) . . ?
Cl9 C5S Cl10 108.1(3) . . ?

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
_platon_squeeze_void_content
1 0.233 0.082 0.242 160 50 ' '
2 0.267 0.918 0.742 160 52 ' '
3 0.733 0.418 0.758 160 51 ' '
4 0.767 0.582 0.258 160 53 ' '
_platon_squeeze_details          
;
One molecule of dichloro methane was squeezed
;

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        66.60
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.058
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3fMeCN
_database_code_depnum_ccdc_archive 'CCDC 1422965'
_audit_update_record             
;
2015-10-29 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C99 H90 N6 O3, 0.75(C2 H3 N)'
_chemical_formula_sum            'C100.50 H92.25 N6.75 O3'
_chemical_formula_weight         1442.56
_chemical_absolute_configuration rm

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   15.1450(4)
_cell_length_b                   21.4200(4)
_cell_length_c                   25.2160(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8180.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9511
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      66.61

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3066
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6658
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57004
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.71
_diffrn_reflns_theta_max         66.61
_reflns_number_total             13961
_reflns_number_gt                10601
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0713P)²+2.3639P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00079(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_number_reflns         13961
_refine_ls_number_parameters     1005
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0542
_refine_ls_wR_factor_ref         0.1450
_refine_ls_wR_factor_gt          0.1304
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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 0.82878(17) 0.70442(9) 0.47212(9) 0.0458(6) Uani 1 1 d . . .
H1 H 0.8276 0.7116 0.4394 0.055 Uiso 1 1 calc R . .
O2 O 0.45171(16) 0.69495(10) 0.40847(10) 0.0456(6) Uani 1 1 d . . .
H2 H 0.3984 0.6945 0.4177 0.055 Uiso 1 1 calc R . .
O3 O 0.52436(15) 0.67209(9) 0.59536(10) 0.0462(6) Uani 1 1 d . . .
H3 H 0.5728 0.6805 0.6099 0.055 Uiso 1 1 calc R . .
N1 N 0.83669(18) 0.65265(11) 0.62432(11) 0.0405(6) Uani 1 1 d . . .
N2 N 0.29978(18) 0.64446(11) 0.43162(11) 0.0389(6) Uani 1 1 d . . .
N3 N 0.83861(18) 0.68401(12) 0.37376(11) 0.0423(7) Uani 1 1 d . . .
N4 N 0.28659(19) 0.60829(11) 0.54070(11) 0.0410(7) Uani 1 1 d . . .
N5 N 0.65778(19) 0.65675(12) 0.66019(11) 0.0432(7) Uani 1 1 d . . .
C6 C 0.8451(2) 0.64299(14) 0.48041(14) 0.0395(8) Uani 1 1 d . . .
N6 N 0.67474(19) 0.68684(12) 0.31650(12) 0.0446(7) Uani 1 1 d . . .
C2 C 0.8500(2) 0.62132(14) 0.53176(13) 0.0386(8) Uani 1 1 d . . .
C3 C 0.4271(2) 0.58603(14) 0.58209(14) 0.0422(8) Uani 1 1 d . . .
C4 C 0.8543(2) 0.60242(14) 0.43670(14) 0.0392(8) Uani 1 1 d . . .
C5 C 0.8316(2) 0.66497(14) 0.57535(14) 0.0390(8) Uani 1 1 d . . .
H5 H 0.8144 0.7061 0.5659 0.047 Uiso 1 1 calc R . .
C102 C 0.4708(2) 0.64154(14) 0.38159(13) 0.0392(8) Uani 1 1 d . . .
C7 C 0.4413(2) 0.41597(14) 0.63415(14) 0.0415(8) Uani 1 1 d . . .
C8 C 0.5434(2) 0.50963(15) 0.63804(14) 0.0454(8) Uani 1 1 d . . .
H8 H 0.5831 0.4839 0.6574 0.055 Uiso 1 1 calc R . .
C9 C 0.4331(2) 0.53586(14) 0.35498(14) 0.0405(8) Uani 1 1 d . . .
H9 H 0.3922 0.5022 0.3550 0.049 Uiso 1 1 calc R . .
C10 C 0.5638(2) 0.57253(15) 0.63134(14) 0.0424(8) Uani 1 1 d . . .
C11 C 0.8069(2) 0.70198(14) 0.66021(13) 0.0408(8) Uani 1 1 d . . .
H11 H 0.7854 0.7384 0.6390 0.049 Uiso 1 1 calc R . .
C12 C 0.4977(2) 0.41023(14) 0.32821(14) 0.0406(8) Uani 1 1 d . . .
C13 C 0.0736(2) 0.69940(15) 0.52132(15) 0.0462(9) Uani 1 1 d . . .
H13A H 0.0161 0.6958 0.5397 0.055 Uiso 1 1 calc R . .
H13B H 0.0955 0.7426 0.5262 0.055 Uiso 1 1 calc R . .
C14 C 0.5489(2) 0.63646(14) 0.35406(14) 0.0406(8) Uani 1 1 d . . .
C15 C 0.2271(2) 0.65524(14) 0.51774(13) 0.0389(8) Uani 1 1 d . . .
H15 H 0.2540 0.6976 0.5222 0.047 Uiso 1 1 calc R . .
C16 C 0.3620(2) 0.62688(14) 0.55629(13) 0.0418(8) Uani 1 1 d . . .
H16 H 0.3771 0.6695 0.5510 0.050 Uiso 1 1 calc R . .
C17 C 0.8312(2) 0.70969(15) 0.32029(13) 0.0412(8) Uani 1 1 d . . .
H17 H 0.8395 0.6758 0.2935 0.049 Uiso 1 1 calc R . .
C18 C 0.4262(2) 0.42096(14) 0.69444(14) 0.0428(8) Uani 1 1 d . . .
C19 C 0.5108(2) 0.36531(14) 0.62041(14) 0.0419(8) Uani 1 1 d . . .
C20 C 0.4986(2) 0.40884(15) 0.38296(14) 0.0432(8) Uani 1 1 d . . .
H20 H 0.5171 0.4448 0.4020 0.052 Uiso 1 1 calc R . .
C21 C 1.0037(2) 0.44539(14) 0.47943(14) 0.0421(8) Uani 1 1 d . . .
C22 C 0.8703(2) 0.55793(14) 0.54044(14) 0.0404(8) Uani 1 1 d . . .
H22 H 0.8760 0.5430 0.5757 0.048 Uiso 1 1 calc R . .
C23 C 0.9102(2) 0.42625(14) 0.56420(14) 0.0434(8) Uani 1 1 d . . .
C24 C 0.4111(2) 0.59138(14) 0.38153(14) 0.0400(8) Uani 1 1 d . . .
C25 C 0.5341(2) 0.46813(14) 0.29744(13) 0.0405(8) Uani 1 1 d . . .
C26 C 0.6819(2) 0.50095(15) 0.25659(14) 0.0444(8) Uani 1 1 d . . .
H26 H 0.6499 0.5258 0.2320 0.053 Uiso 1 1 calc R . .
C27 C 0.8461(2) 0.40198(14) 0.47890(14) 0.0418(8) Uani 1 1 d . . .
C28 C 0.8488(2) 0.62501(14) 0.38275(14) 0.0403(8) Uani 1 1 d . . .
H28 H 0.8527 0.5965 0.3540 0.048 Uiso 1 1 calc R . .
C29 C 0.1392(2) 0.65364(14) 0.54594(14) 0.0429(8) Uani 1 1 d . . .
H29A H 0.1479 0.6643 0.5838 0.051 Uiso 1 1 calc R . .
H29B H 0.1146 0.6109 0.5441 0.051 Uiso 1 1 calc R . .
C30 C 0.2142(2) 0.64219(14) 0.45873(13) 0.0385(8) Uani 1 1 d . . .
H30 H 0.1892 0.5993 0.4546 0.046 Uiso 1 1 calc R . .
C31 C 0.5129(2) 0.52898(14) 0.32870(13) 0.0389(8) Uani 1 1 d . . .
C32 C 0.5693(2) 0.57984(14) 0.32893(14) 0.0408(8) Uani 1 1 d . . .
H32 H 0.6244 0.5762 0.3112 0.049 Uiso 1 1 calc R . .
C33 C 0.6133(2) 0.68833(15) 0.35061(14) 0.0427(8) Uani 1 1 d . . .
H33 H 0.6085 0.7229 0.3741 0.051 Uiso 1 1 calc R . .
C34 C 0.9117(2) 0.44742(14) 0.50560(14) 0.0400(8) Uani 1 1 d . . .
C35 C 0.8737(2) 0.53926(14) 0.44730(14) 0.0405(8) Uani 1 1 d . . .
H35 H 0.8812 0.5113 0.4184 0.049 Uiso 1 1 calc R . .
C36 C 0.5197(2) 0.43822(15) 0.19930(14) 0.0455(8) Uani 1 1 d . . .
H36 H 0.5751 0.4177 0.2019 0.055 Uiso 1 1 calc R . .
C37 C 1.0738(2) 0.47635(15) 0.50438(15) 0.0465(9) Uani 1 1 d . . .
H37 H 1.0643 0.4961 0.5376 0.056 Uiso 1 1 calc R . .
C38 C 0.2170(2) 0.34859(15) 0.54428(17) 0.0513(10) Uani 1 1 d . . .
H38 H 0.1687 0.3333 0.5241 0.062 Uiso 1 1 calc R . .
C39 C 1.0185(3) 0.42075(14) 0.42937(15) 0.0479(9) Uani 1 1 d . . .
H39 H 0.9713 0.4015 0.4108 0.057 Uiso 1 1 calc R . .
C40 C 0.5053(2) 0.61061(14) 0.60266(15) 0.0430(8) Uani 1 1 d . . .
C41 C 0.1498(2) 0.68869(14) 0.43437(14) 0.0416(8) Uani 1 1 d . . .
H41A H 0.1747 0.7313 0.4368 0.050 Uiso 1 1 calc R . .
H41B H 0.1410 0.6787 0.3964 0.050 Uiso 1 1 calc R . .
C42 C 0.0614(2) 0.68653(15) 0.46305(14) 0.0452(8) Uani 1 1 d . . .
H42A H 0.0210 0.7180 0.4476 0.054 Uiso 1 1 calc R . .
H42B H 0.0342 0.6449 0.4583 0.054 Uiso 1 1 calc R . .
C43 C 0.4104(2) 0.52232(14) 0.58993(14) 0.0435(8) Uani 1 1 d . . .
H43 H 0.3576 0.5052 0.5757 0.052 Uiso 1 1 calc R . .
C44 C 0.8823(2) 0.51682(15) 0.49846(14) 0.0401(8) Uani 1 1 d . . .
C45 C 0.8310(3) 0.42892(15) 0.59252(14) 0.0469(9) Uani 1 1 d . . .
H45 H 0.7814 0.4486 0.5766 0.056 Uiso 1 1 calc R . .
C46 C 0.2117(2) 0.35218(15) 0.59828(17) 0.0509(10) Uani 1 1 d . . .
H46 H 0.1592 0.3390 0.6156 0.061 Uiso 1 1 calc R . .
C47 C 0.3584(2) 0.39427(14) 0.60381(15) 0.0435(8) Uani 1 1 d . . .
C48 C 0.4670(2) 0.48319(14) 0.61736(14) 0.0423(8) Uani 1 1 d . . .
C49 C 0.6404(2) 0.59793(15) 0.65866(14) 0.0438(8) Uani 1 1 d . . .
H49 H 0.6793 0.5699 0.6762 0.053 Uiso 1 1 calc R . .
C50 C 0.3254(2) 0.59505(14) 0.40827(13) 0.0392(7) Uani 1 1 d . . .
H50 H 0.2879 0.5595 0.4082 0.047 Uiso 1 1 calc R . .
C51 C 0.6860(2) 0.42356(16) 0.32405(14) 0.0454(8) Uani 1 1 d . . .
H51 H 0.6570 0.3952 0.3472 0.054 Uiso 1 1 calc R . .
C52 C 0.6352(2) 0.46210(14) 0.29176(14) 0.0420(8) Uani 1 1 d . . .
C53 C 0.9810(2) 0.39708(15) 0.58932(16) 0.0499(9) Uani 1 1 d . . .
H53 H 1.0360 0.3936 0.5714 0.060 Uiso 1 1 calc R . .
C54 C 0.2818(2) 0.37481(15) 0.62837(16) 0.0487(9) Uani 1 1 d . . .
H54 H 0.2769 0.3768 0.6659 0.058 Uiso 1 1 calc R . .
C55 C 0.2941(3) 0.36759(15) 0.51950(17) 0.0501(9) Uani 1 1 d . . .
H55 H 0.2991 0.3649 0.4820 0.060 Uiso 1 1 calc R . .
C56 C 0.7383(2) 0.73787(15) 0.31491(15) 0.0443(8) Uani 1 1 d . . .
H56 H 0.7270 0.7669 0.3452 0.053 Uiso 1 1 calc R . .
C57 C 0.4704(2) 0.35693(15) 0.30186(15) 0.0464(8) Uani 1 1 d . . .
H57 H 0.4682 0.3569 0.2642 0.056 Uiso 1 1 calc R . .
C58 C 0.3628(2) 0.39016(14) 0.54877(15) 0.0463(9) Uani 1 1 d . . .
H58 H 0.4149 0.4034 0.5311 0.056 Uiso 1 1 calc R . .
C59 C 0.4880(2) 0.47192(14) 0.24282(14) 0.0434(8) Uani 1 1 d . . .
C60 C 0.7602(2) 0.41862(15) 0.46847(14) 0.0435(8) Uani 1 1 d . . .
H60 H 0.7422 0.4606 0.4740 0.052 Uiso 1 1 calc R . .
C61 C 1.1699(3) 0.45187(15) 0.43143(17) 0.0526(10) Uani 1 1 d . . .
H61 H 1.2266 0.4533 0.4153 0.063 Uiso 1 1 calc R . .
C62 C 1.1568(2) 0.47852(15) 0.48129(16) 0.0495(9) Uani 1 1 d . . .
H62 H 1.2044 0.4981 0.4993 0.059 Uiso 1 1 calc R . .
C63 C 0.8706(2) 0.33989(15) 0.47088(15) 0.0486(9) Uani 1 1 d . . .
H63 H 0.9288 0.3269 0.4797 0.058 Uiso 1 1 calc R . .
C64 C 0.8206(2) 0.46625(17) 0.29085(16) 0.0515(9) Uani 1 1 d . . .
H64 H 0.8832 0.4688 0.2915 0.062 Uiso 1 1 calc R . .
C65 C 0.4901(2) 0.30308(14) 0.63225(14) 0.0459(8) Uani 1 1 d . . .
H65 H 0.4365 0.2940 0.6502 0.055 Uiso 1 1 calc R . .
C66 C 0.8223(3) 0.40422(16) 0.64231(15) 0.0511(9) Uani 1 1 d . . .
H66 H 0.7671 0.4064 0.6601 0.061 Uiso 1 1 calc R . .
C67 C 0.6989(3) 0.37510(16) 0.44993(15) 0.0502(9) Uani 1 1 d . . .
H67 H 0.6392 0.3870 0.4442 0.060 Uiso 1 1 calc R . .
C68 C 0.7716(3) 0.50381(16) 0.25700(15) 0.0493(9) Uani 1 1 d . . .
H68 H 0.8011 0.5319 0.2338 0.059 Uiso 1 1 calc R . .
C69 C 0.4730(2) 0.35567(16) 0.41093(15) 0.0494(9) Uani 1 1 d . . .
H69 H 0.4735 0.3559 0.4486 0.059 Uiso 1 1 calc R . .
C70 C 0.5457(3) 0.25472(16) 0.61854(15) 0.0505(9) Uani 1 1 d . . .
H70 H 0.5307 0.2131 0.6278 0.061 Uiso 1 1 calc R . .
C71 C 0.8940(3) 0.37606(15) 0.66678(16) 0.0517(9) Uani 1 1 d . . .
H71 H 0.8886 0.3592 0.7015 0.062 Uiso 1 1 calc R . .
C72 C 0.4459(3) 0.30323(16) 0.32971(16) 0.0528(10) Uani 1 1 d . . .
H72 H 0.4286 0.2669 0.3108 0.063 Uiso 1 1 calc R . .
C73 C 0.6226(3) 0.26659(16) 0.59160(16) 0.0532(9) Uani 1 1 d . . .
H73 H 0.6606 0.2332 0.5820 0.064 Uiso 1 1 calc R . .
C74 C 0.7314(2) 0.67668(15) 0.69389(14) 0.0443(8) Uani 1 1 d . . .
H74 H 0.7531 0.6400 0.7147 0.053 Uiso 1 1 calc R . .
C75 C 1.1014(2) 0.42380(15) 0.40607(17) 0.0514(9) Uani 1 1 d . . .
H75 H 1.1104 0.4060 0.3720 0.062 Uiso 1 1 calc R . .
C76 C 0.5876(2) 0.37609(16) 0.59272(15) 0.0493(9) Uani 1 1 d . . .
H76 H 0.6023 0.4177 0.5831 0.059 Uiso 1 1 calc R . .
C77 C 0.4725(2) 0.43405(16) 0.15268(15) 0.0469(9) Uani 1 1 d . . .
H77 H 0.4943 0.4090 0.1245 0.056 Uiso 1 1 calc R . .
C78 C 0.9723(3) 0.37296(17) 0.64017(17) 0.0549(10) Uani 1 1 d . . .
H78 H 1.0218 0.3540 0.6567 0.066 Uiso 1 1 calc R . .
C79 C 0.7765(3) 0.42519(17) 0.32357(16) 0.0516(9) Uani 1 1 d . . .
H79 H 0.8090 0.3979 0.3459 0.062 Uiso 1 1 calc R . .
C80 C 0.4467(3) 0.30265(17) 0.38396(16) 0.0523(9) Uani 1 1 d . . .
H80 H 0.4295 0.2663 0.4028 0.063 Uiso 1 1 calc R . .
C81 C 0.4701(2) 0.38534(15) 0.73280(15) 0.0474(9) Uani 1 1 d . . .
H81 H 0.5110 0.3544 0.7217 0.057 Uiso 1 1 calc R . .
C82 C 0.3647(3) 0.50272(17) 0.18789(15) 0.0519(9) Uani 1 1 d . . .
H82 H 0.3122 0.5264 0.1836 0.062 Uiso 1 1 calc R . .
C83 C 0.9018(2) 0.75967(16) 0.31308(16) 0.0509(9) Uani 1 1 d . . .
H83A H 0.8977 0.7901 0.3425 0.061 Uiso 1 1 calc R . .
H83B H 0.9608 0.7399 0.3147 0.061 Uiso 1 1 calc R . .
C84 C 0.7259(3) 0.31448(16) 0.44003(15) 0.0528(9) Uani 1 1 d . . .
H84 H 0.6852 0.2850 0.4261 0.063 Uiso 1 1 calc R . .
C85 C 0.7297(3) 0.77321(17) 0.26314(16) 0.0540(9) Uani 1 1 d . . .
H85A H 0.6710 0.7935 0.2618 0.065 Uiso 1 1 calc R . .
H85B H 0.7332 0.7432 0.2333 0.065 Uiso 1 1 calc R . .
C86 C 0.6446(3) 0.32759(16) 0.57841(15) 0.0523(9) Uani 1 1 d . . .
H86 H 0.6978 0.3363 0.5599 0.063 Uiso 1 1 calc R . .
C87 C 0.8116(3) 0.29682(16) 0.45030(16) 0.0543(10) Uani 1 1 d . . .
H87 H 0.8303 0.2553 0.4433 0.065 Uiso 1 1 calc R . .
C88 C 0.8821(3) 0.72307(16) 0.69634(15) 0.0500(9) Uani 1 1 d . . .
H88A H 0.9313 0.7396 0.6746 0.060 Uiso 1 1 calc R . .
H88B H 0.9045 0.6869 0.7168 0.060 Uiso 1 1 calc R . .
C89 C 0.3543(3) 0.47513(17) 0.76684(16) 0.0556(10) Uani 1 1 d . . .
H89 H 0.3144 0.5065 0.7785 0.067 Uiso 1 1 calc R . .
C90 C 0.3679(3) 0.46712(16) 0.71350(16) 0.0498(9) Uani 1 1 d . . .
H90 H 0.3376 0.4931 0.6890 0.060 Uiso 1 1 calc R . .
C91 C 0.4102(2) 0.50566(16) 0.23509(15) 0.0482(9) Uani 1 1 d . . .
H91 H 0.3882 0.5311 0.2629 0.058 Uiso 1 1 calc R . .
C92 C 0.3972(3) 0.43876(18) 0.80396(17) 0.0595(10) Uani 1 1 d . . .
H92 H 0.3868 0.4444 0.8408 0.071 Uiso 1 1 calc R . .
C93 C 0.4556(3) 0.39393(17) 0.78598(16) 0.0533(10) Uani 1 1 d . . .
H93 H 0.4863 0.3687 0.8109 0.064 Uiso 1 1 calc R . .
C94 C 0.8920(3) 0.79389(18) 0.26065(16) 0.0603(10) Uani 1 1 d . . .
H94A H 0.9374 0.8270 0.2581 0.072 Uiso 1 1 calc R . .
H94B H 0.9014 0.7643 0.2310 0.072 Uiso 1 1 calc R . .
C95 C 0.3942(3) 0.46572(17) 0.14652(16) 0.0513(9) Uani 1 1 d . . .
H95 H 0.3612 0.4623 0.1146 0.062 Uiso 1 1 calc R . .
C96 C 0.8499(3) 0.77389(16) 0.73465(16) 0.0599(11) Uani 1 1 d . . .
H96A H 0.8990 0.7867 0.7582 0.072 Uiso 1 1 calc R . .
H96B H 0.8305 0.8109 0.7143 0.072 Uiso 1 1 calc R . .
C97 C 0.6988(3) 0.72692(17) 0.73235(16) 0.0572(10) Uani 1 1 d . . .
H97A H 0.6742 0.7625 0.7120 0.069 Uiso 1 1 calc R . .
H97B H 0.6511 0.7096 0.7548 0.069 Uiso 1 1 calc R . .
C98 C 0.7744(3) 0.74981(18) 0.76750(17) 0.0671(12) Uani 1 1 d . . .
H98A H 0.7527 0.7835 0.7910 0.081 Uiso 1 1 calc R . .
H98B H 0.7953 0.7150 0.7901 0.081 Uiso 1 1 calc R . .
C99 C 0.8008(3) 0.82274(18) 0.25617(17) 0.0639(11) Uani 1 1 d . . .
H99A H 0.7943 0.8428 0.2210 0.077 Uiso 1 1 calc R . .
H99B H 0.7937 0.8554 0.2836 0.077 Uiso 1 1 calc R . .
N100 N 0.5624(5) 0.4988(3) 0.4887(3) 0.100(2) Uani 0.75 1 d P . .
C101 C 0.6165(5) 0.6150(3) 0.4878(3) 0.089(2) Uani 0.75 1 d P . .
H10A H 0.6604 0.6206 0.4597 0.133 Uiso 0.75 1 calc PR . .
H10B H 0.6429 0.6255 0.5222 0.133 Uiso 0.75 1 calc PR . .
H10C H 0.5659 0.6424 0.4812 0.133 Uiso 0.75 1 calc PR . .
C1 C 0.5871(5) 0.5502(4) 0.4885(3) 0.0823(19) Uani 0.75 1 d P . .


_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 C6 1.355(4) . ?
O2 C102 1.361(4) . ?
O3 C40 1.361(4) . ?
N1 C5 1.265(4) . ?
N1 C11 1.463(4) . ?
N2 C50 1.272(4) . ?
N2 C30 1.467(4) . ?
N3 C28 1.293(4) . ?
N3 C17 1.461(4) . ?
N4 C16 1.272(4) . ?
N4 C15 1.469(4) . ?
N5 C49 1.288(4) . ?
N5 C74 1.466(4) . ?
C6 C2 1.378(5) . ?
C6 C4 1.410(5) . ?
N6 C33 1.268(4) . ?
N6 C56 1.457(4) . ?
C2 C22 1.409(4) . ?
C2 C5 1.470(5) . ?
C3 C40 1.396(5) . ?
C3 C43 1.402(4) . ?
C3 C16 1.470(5) . ?
C4 C35 1.410(4) . ?
C4 C28 1.446(5) . ?
C102 C14 1.376(5) . ?
C102 C24 1.404(4) . ?
C7 C18 1.541(5) . ?
C7 C47 1.541(5) . ?
C7 C48 1.551(4) . ?
C7 C19 1.551(5) . ?
C8 C48 1.390(5) . ?
C8 C10 1.393(5) . ?
C9 C31 1.387(5) . ?
C9 C24 1.405(4) . ?
C10 C40 1.405(5) . ?
C10 C49 1.455(5) . ?
C11 C74 1.524(5) . ?
C11 C88 1.527(5) . ?
C12 C20 1.381(5) . ?
C12 C57 1.384(5) . ?
C12 C25 1.563(5) . ?
C13 C42 1.506(5) . ?
C13 C29 1.527(5) . ?
C14 C32 1.403(5) . ?
C14 C33 1.481(5) . ?
C15 C29 1.511(5) . ?
C15 C30 1.527(5) . ?
C17 C83 1.524(5) . ?
C17 C56 1.537(5) . ?
C18 C81 1.400(5) . ?
C18 C90 1.410(5) . ?
C19 C76 1.376(5) . ?
C19 C65 1.401(5) . ?
C20 C69 1.395(5) . ?
C21 C39 1.386(5) . ?
C21 C37 1.401(5) . ?
C21 C34 1.543(5) . ?
C22 C44 1.389(5) . ?
C23 C53 1.393(5) . ?
C23 C45 1.397(5) . ?
C23 C34 1.546(5) . ?
C24 C50 1.464(5) . ?
C25 C52 1.543(5) . ?
C25 C59 1.546(5) . ?
C25 C31 1.557(4) . ?
C26 C68 1.360(5) . ?
C26 C52 1.406(5) . ?
C27 C60 1.373(5) . ?
C27 C63 1.396(5) . ?
C27 C34 1.545(5) . ?
C30 C41 1.523(4) . ?
C31 C32 1.384(4) . ?
C34 C44 1.562(4) . ?
C35 C44 1.383(5) . ?
C36 C77 1.379(5) . ?
C36 C59 1.398(5) . ?
C37 C62 1.386(5) . ?
C38 C46 1.366(5) . ?
C38 C55 1.385(5) . ?
C39 C75 1.387(5) . ?
C41 C42 1.523(5) . ?
C43 C48 1.384(5) . ?
C45 C66 1.369(5) . ?
C46 C54 1.392(5) . ?
C47 C54 1.380(5) . ?
C47 C58 1.392(5) . ?
C51 C79 1.372(5) . ?
C51 C52 1.391(5) . ?
C53 C78 1.389(5) . ?
C55 C58 1.364(5) . ?
C56 C85 1.514(5) . ?
C57 C72 1.398(5) . ?
C59 C91 1.397(5) . ?
C60 C67 1.397(5) . ?
C61 C75 1.359(5) . ?
C61 C62 1.395(5) . ?
C63 C87 1.385(5) . ?
C64 C79 1.378(5) . ?
C64 C68 1.388(5) . ?
C65 C70 1.379(5) . ?
C66 C71 1.387(5) . ?
C67 C84 1.384(5) . ?
C69 C80 1.382(5) . ?
C70 C73 1.372(6) . ?
C71 C78 1.365(6) . ?
C72 C80 1.368(5) . ?
C73 C86 1.389(5) . ?
C74 C97 1.531(5) . ?
C76 C86 1.398(5) . ?
C77 C95 1.374(5) . ?
C81 C93 1.371(5) . ?
C82 C91 1.377(5) . ?
C82 C95 1.385(5) . ?
C83 C94 1.519(5) . ?
C84 C87 1.377(6) . ?
C85 C99 1.522(5) . ?
C88 C96 1.535(5) . ?
C89 C90 1.372(5) . ?
C89 C92 1.380(5) . ?
C92 C93 1.383(5) . ?
C94 C99 1.518(6) . ?
C96 C98 1.503(6) . ?
C97 C98 1.529(6) . ?
N100 C1 1.163(9) . ?
C101 C1 1.457(10) . ?

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
C5 N1 C11 115.8(3) . . ?
C50 N2 C30 117.3(3) . . ?
C28 N3 C17 122.6(3) . . ?
C16 N4 C15 117.3(3) . . ?
C49 N5 C74 117.3(3) . . ?
O1 C6 C2 118.8(3) . . ?
O1 C6 C4 119.7(3) . . ?
C2 C6 C4 121.4(3) . . ?
C33 N6 C56 119.0(3) . . ?
C6 C2 C22 118.8(3) . . ?
C6 C2 C5 118.6(3) . . ?
C22 C2 C5 122.6(3) . . ?
C40 C3 C43 117.9(3) . . ?
C40 C3 C16 120.6(3) . . ?
C43 C3 C16 121.4(3) . . ?
C6 C4 C35 117.6(3) . . ?
C6 C4 C28 121.6(3) . . ?
C35 C4 C28 120.7(3) . . ?
N1 C5 C2 125.9(3) . . ?
O2 C102 C14 120.0(3) . . ?
O2 C102 C24 120.5(3) . . ?
C14 C102 C24 119.5(3) . . ?
C18 C7 C47 113.0(3) . . ?
C18 C7 C48 104.0(3) . . ?
C47 C7 C48 110.4(3) . . ?
C18 C7 C19 111.7(3) . . ?
C47 C7 C19 103.3(3) . . ?
C48 C7 C19 114.7(3) . . ?
C48 C8 C10 122.2(3) . . ?
C31 C9 C24 121.6(3) . . ?
C8 C10 C40 119.0(3) . . ?
C8 C10 C49 118.8(3) . . ?
C40 C10 C49 122.0(3) . . ?
N1 C11 C74 108.6(3) . . ?
N1 C11 C88 110.6(3) . . ?
C74 C11 C88 109.4(3) . . ?
C20 C12 C57 117.7(3) . . ?
C20 C12 C25 120.7(3) . . ?
C57 C12 C25 121.4(3) . . ?
C42 C13 C29 111.1(3) . . ?
C102 C14 C32 119.1(3) . . ?
C102 C14 C33 122.4(3) . . ?
C32 C14 C33 118.5(3) . . ?
N4 C15 C29 109.9(3) . . ?
N4 C15 C30 109.7(3) . . ?
C29 C15 C30 110.0(3) . . ?
N4 C16 C3 123.6(3) . . ?
N3 C17 C83 108.7(3) . . ?
N3 C17 C56 107.5(3) . . ?
C83 C17 C56 110.8(3) . . ?
C81 C18 C90 116.4(3) . . ?
C81 C18 C7 125.0(3) . . ?
C90 C18 C7 118.5(3) . . ?
C76 C19 C65 117.2(3) . . ?
C76 C19 C7 124.7(3) . . ?
C65 C19 C7 117.8(3) . . ?
C12 C20 C69 121.4(3) . . ?
C39 C21 C37 117.8(3) . . ?
C39 C21 C34 123.1(3) . . ?
C37 C21 C34 118.6(3) . . ?
C44 C22 C2 121.4(3) . . ?
C53 C23 C45 116.5(3) . . ?
C53 C23 C34 123.7(3) . . ?
C45 C23 C34 119.3(3) . . ?
C102 C24 C9 119.7(3) . . ?
C102 C24 C50 121.9(3) . . ?
C9 C24 C50 118.3(3) . . ?
C52 C25 C59 111.7(3) . . ?
C52 C25 C31 108.8(3) . . ?
C59 C25 C31 108.3(3) . . ?
C52 C25 C12 109.2(3) . . ?
C59 C25 C12 108.9(3) . . ?
C31 C25 C12 109.9(3) . . ?
C68 C26 C52 121.6(4) . . ?
C60 C27 C63 118.1(3) . . ?
C60 C27 C34 121.9(3) . . ?
C63 C27 C34 119.5(3) . . ?
N3 C28 C4 119.9(3) . . ?
C15 C29 C13 111.6(3) . . ?
N2 C30 C41 110.9(3) . . ?
N2 C30 C15 109.5(3) . . ?
C41 C30 C15 110.8(3) . . ?
C32 C31 C9 116.9(3) . . ?
C32 C31 C25 122.3(3) . . ?
C9 C31 C25 120.7(3) . . ?
C31 C32 C14 123.1(3) . . ?
N6 C33 C14 120.3(3) . . ?
C21 C34 C27 112.1(3) . . ?
C21 C34 C23 114.4(3) . . ?
C27 C34 C23 102.9(3) . . ?
C21 C34 C44 103.6(3) . . ?
C27 C34 C44 111.5(3) . . ?
C23 C34 C44 112.7(3) . . ?
C44 C35 C4 122.0(3) . . ?
C77 C36 C59 121.6(3) . . ?
C62 C37 C21 120.9(4) . . ?
C46 C38 C55 118.9(4) . . ?
C21 C39 C75 120.9(4) . . ?
O3 C40 C3 119.6(3) . . ?
O3 C40 C10 119.9(3) . . ?
C3 C40 C10 120.5(3) . . ?
C42 C41 C30 110.6(3) . . ?
C13 C42 C41 110.4(3) . . ?
C48 C43 C3 123.2(3) . . ?
C35 C44 C22 118.6(3) . . ?
C35 C44 C34 117.7(3) . . ?
C22 C44 C34 123.5(3) . . ?
C66 C45 C23 122.4(3) . . ?
C38 C46 C54 121.2(4) . . ?
C54 C47 C58 117.9(3) . . ?
C54 C47 C7 123.6(3) . . ?
C58 C47 C7 118.4(3) . . ?
C43 C48 C8 117.2(3) . . ?
C43 C48 C7 122.9(3) . . ?
C8 C48 C7 119.0(3) . . ?
N5 C49 C10 122.9(3) . . ?
N2 C50 C24 121.9(3) . . ?
C79 C51 C52 122.1(4) . . ?
C51 C52 C26 116.3(3) . . ?
C51 C52 C25 122.9(3) . . ?
C26 C52 C25 120.5(3) . . ?
C78 C53 C23 120.9(4) . . ?
C47 C54 C46 120.1(4) . . ?
C58 C55 C38 120.2(4) . . ?
N6 C56 C85 110.0(3) . . ?
N6 C56 C17 107.9(3) . . ?
C85 C56 C17 110.5(3) . . ?
C12 C57 C72 121.1(3) . . ?
C55 C58 C47 121.7(4) . . ?
C91 C59 C36 116.6(3) . . ?
C91 C59 C25 122.2(3) . . ?
C36 C59 C25 121.1(3) . . ?
C27 C60 C67 121.4(3) . . ?
C75 C61 C62 119.7(4) . . ?
C37 C62 C61 119.6(4) . . ?
C87 C63 C27 121.2(3) . . ?
C79 C64 C68 118.6(3) . . ?
C70 C65 C19 121.6(3) . . ?
C45 C66 C71 120.0(4) . . ?
C84 C67 C60 119.3(4) . . ?
C26 C68 C64 120.8(4) . . ?
C80 C69 C20 120.1(3) . . ?
C73 C70 C65 120.2(3) . . ?
C78 C71 C66 118.9(4) . . ?
C80 C72 C57 120.5(3) . . ?
C70 C73 C86 119.8(3) . . ?
N5 C74 C11 110.6(3) . . ?
N5 C74 C97 109.1(3) . . ?
C11 C74 C97 110.2(3) . . ?
C61 C75 C39 120.8(4) . . ?
C19 C76 C86 121.9(3) . . ?
C95 C77 C36 120.8(3) . . ?
C71 C78 C53 121.2(4) . . ?
C51 C79 C64 120.4(4) . . ?
C72 C80 C69 119.2(3) . . ?
C93 C81 C18 121.8(3) . . ?
C91 C82 C95 121.0(4) . . ?
C94 C83 C17 112.0(3) . . ?
C87 C84 C67 120.2(3) . . ?
C56 C85 C99 112.8(3) . . ?
C73 C86 C76 119.3(4) . . ?
C84 C87 C63 119.7(3) . . ?
C11 C88 C96 110.4(3) . . ?
C90 C89 C92 121.6(4) . . ?
C89 C90 C18 121.1(3) . . ?
C82 C91 C59 121.3(3) . . ?
C89 C92 C93 118.1(4) . . ?
C81 C93 C92 121.1(4) . . ?
C99 C94 C83 110.5(3) . . ?
C77 C95 C82 118.4(4) . . ?
C98 C96 C88 110.2(3) . . ?
C98 C97 C74 110.5(3) . . ?
C96 C98 C97 111.1(4) . . ?
C94 C99 C85 110.6(3) . . ?
N100 C1 C101 179.0(9) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        66.61
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.051

