# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_TBABrDNPC4P
_database_code_depnum_ccdc_archive 'CCDC 1482084'
_audit_update_record             
;
2016-05-26 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Cis-Dinitrophenyl-Calix[4]pyrrole-Tetrabutylammonium bromide 
;
_chemical_name_common            Cis-DNP-Calix[4]pyrrole-TBABr
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H72 Br N9 O8'
_chemical_formula_weight         1055.12

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'
Br Br -0.2901 2.4595 '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   P21/n

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

_cell_length_a                   12.865(3)
_cell_length_b                   18.623(5)
_cell_length_c                   22.483(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.143(4)
_cell_angle_gamma                90.00
_cell_volume                     5387(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    12587
_cell_measurement_theta_min      1.4198
_cell_measurement_theta_max      27.5204

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2232
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8863
_exptl_absorpt_correction_T_max  0.9757
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35858
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9070
_reflns_number_gt                7595
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_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)+(0.0500P)²+27.2084P] 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_number_reflns         9070
_refine_ls_number_parameters     659
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.1197
_refine_ls_wR_factor_ref         0.2598
_refine_ls_wR_factor_gt          0.2515
_refine_ls_goodness_of_fit_ref   1.366
_refine_ls_restrained_S_all      1.366
_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
Br1 Br 0.95802(8) 0.75814(6) 0.13111(5) 0.0649(3) Uani 1 1 d . . .
C1 C 0.8714(4) 0.6645(3) 0.2950(2) 0.0123(10) Uani 1 1 d . . .
C2 C 0.7984(4) 0.6608(3) 0.3396(2) 0.0164(11) Uani 1 1 d . . .
H2 H 0.7928 0.6243 0.3689 0.020 Uiso 1 1 calc R . .
C3 C 0.7325(4) 0.7224(3) 0.3336(2) 0.0197(12) Uani 1 1 d . . .
H3 H 0.6750 0.7338 0.3583 0.024 Uiso 1 1 calc R . .
C4 C 0.7662(4) 0.7619(3) 0.2865(2) 0.0138(11) Uani 1 1 d . . .
C5 C 0.7203(4) 0.8275(3) 0.2564(2) 0.0143(11) Uani 1 1 d . . .
C6 C 0.6842(4) 0.8075(3) 0.1921(2) 0.0197(12) Uani 1 1 d . . .
H6A H 0.7449 0.7957 0.1678 0.030 Uiso 1 1 calc R . .
H6B H 0.6473 0.8483 0.1744 0.030 Uiso 1 1 calc R . .
H6C H 0.6376 0.7659 0.1938 0.030 Uiso 1 1 calc R . .
C7 C 0.6245(4) 0.8511(3) 0.2926(3) 0.0237(13) Uani 1 1 d . . .
H7A H 0.5744 0.8115 0.2942 0.036 Uiso 1 1 calc R . .
H7B H 0.5921 0.8928 0.2734 0.036 Uiso 1 1 calc R . .
H7C H 0.6461 0.8639 0.3330 0.036 Uiso 1 1 calc R . .
C8 C 0.7959(4) 0.8888(3) 0.2539(2) 0.0144(11) Uani 1 1 d . . .
C9 C 0.7952(5) 0.9537(3) 0.2832(3) 0.0228(13) Uani 1 1 d . . .
H9 H 0.7473 0.9678 0.3131 0.027 Uiso 1 1 calc R . .
C10 C 0.8788(5) 0.9963(3) 0.2610(3) 0.0225(12) Uani 1 1 d . . .
H10 H 0.8958 1.0439 0.2729 0.027 Uiso 1 1 calc R . .
C11 C 0.9290(4) 0.9567(3) 0.2200(2) 0.0133(10) Uani 1 1 d . . .
C12 C 1.0227(4) 0.9747(3) 0.1804(2) 0.0151(11) Uani 1 1 d . . .
C13 C 1.0411(5) 1.0557(3) 0.1805(2) 0.0199(12) Uani 1 1 d . . .
H13A H 0.9792 1.0802 0.1651 0.030 Uiso 1 1 calc R . .
H13B H 1.1009 1.0670 0.1553 0.030 Uiso 1 1 calc R . .
H13C H 1.0549 1.0719 0.2213 0.030 Uiso 1 1 calc R . .
C14 C 0.9968(4) 0.9520(3) 0.1156(2) 0.0139(11) Uani 1 1 d . . .
C15 C 0.8953(4) 0.9608(3) 0.0936(2) 0.0157(11) Uani 1 1 d . . .
H15 H 0.8428 0.9814 0.1179 0.019 Uiso 1 1 calc R . .
C16 C 0.8727(4) 0.9390(3) 0.0363(2) 0.0167(11) Uani 1 1 d . . .
C17 C 0.9443(5) 0.9094(3) -0.0010(2) 0.0193(12) Uani 1 1 d . . .
H17 H 0.9264 0.8940 -0.0400 0.023 Uiso 1 1 calc R . .
C18 C 1.0457(4) 0.9030(3) 0.0214(2) 0.0183(12) Uani 1 1 d . . .
C19 C 1.0727(4) 0.9238(3) 0.0787(2) 0.0163(11) Uani 1 1 d . . .
H19 H 1.1422 0.9187 0.0925 0.020 Uiso 1 1 calc R . .
C20 C 1.1192(4) 0.9360(3) 0.2022(2) 0.0152(11) Uani 1 1 d . . .
C21 C 1.2119(4) 0.9622(3) 0.2243(3) 0.0219(12) Uani 1 1 d . . .
H21 H 1.2285 1.0113 0.2307 0.026 Uiso 1 1 calc R . .
C22 C 1.2778(4) 0.9033(3) 0.2355(3) 0.0221(12) Uani 1 1 d . . .
H22 H 1.3463 0.9059 0.2513 0.026 Uiso 1 1 calc R . .
C23 C 1.2262(4) 0.8412(3) 0.2199(2) 0.0187(12) Uani 1 1 d . . .
C24 C 1.2622(4) 0.7643(3) 0.2173(3) 0.0193(12) Uani 1 1 d . . .
C25 C 1.3780(5) 0.7610(4) 0.2370(3) 0.0340(16) Uani 1 1 d . . .
H25A H 1.3834 0.7738 0.2792 0.051 Uiso 1 1 calc R . .
H25B H 1.4188 0.7948 0.2133 0.051 Uiso 1 1 calc R . .
H25C H 1.4046 0.7122 0.2311 0.051 Uiso 1 1 calc R . .
C26 C 1.2566(5) 0.7372(3) 0.1520(3) 0.0264(13) Uani 1 1 d . . .
H26A H 1.2848 0.6883 0.1498 0.040 Uiso 1 1 calc R . .
H26B H 1.2975 0.7690 0.1265 0.040 Uiso 1 1 calc R . .
H26C H 1.1841 0.7370 0.1386 0.040 Uiso 1 1 calc R . .
C27 C 1.2003(4) 0.7144(3) 0.2557(2) 0.0158(11) Uani 1 1 d . . .
C28 C 1.2267(5) 0.6770(3) 0.3071(3) 0.0216(12) Uani 1 1 d . . .
H28 H 1.2913 0.6798 0.3276 0.026 Uiso 1 1 calc R . .
C29 C 1.1415(4) 0.6344(3) 0.3235(2) 0.0190(12) Uani 1 1 d . . .
H29 H 1.1385 0.6034 0.3570 0.023 Uiso 1 1 calc R . .
C30 C 1.0627(4) 0.6452(3) 0.2827(2) 0.0135(10) Uani 1 1 d . . .
C31 C 0.9550(4) 0.6119(3) 0.2773(2) 0.0143(11) Uani 1 1 d . . .
C32 C 0.9488(5) 0.5447(3) 0.3178(2) 0.0208(12) Uani 1 1 d . . .
H32A H 1.0016 0.5099 0.3056 0.031 Uiso 1 1 calc R . .
H32B H 0.8796 0.5230 0.3142 0.031 Uiso 1 1 calc R . .
H32C H 0.9611 0.5588 0.3592 0.031 Uiso 1 1 calc R . .
C33 C 0.9385(4) 0.5863(3) 0.2130(2) 0.0119(10) Uani 1 1 d . . .
C34 C 0.8443(4) 0.5975(3) 0.1825(2) 0.0135(10) Uani 1 1 d . . .
H34 H 0.7887 0.6224 0.2010 0.016 Uiso 1 1 calc R . .
C35 C 0.8337(4) 0.5718(3) 0.1255(2) 0.0120(10) Uani 1 1 d . . .
C36 C 0.9091(4) 0.5341(3) 0.0955(2) 0.0176(11) Uani 1 1 d . . .
H36 H 0.8993 0.5171 0.0560 0.021 Uiso 1 1 calc R . .
C37 C 1.0014(4) 0.5226(3) 0.1273(2) 0.0152(11) Uani 1 1 d . . .
C38 C 1.0164(4) 0.5486(3) 0.1844(2) 0.0170(11) Uani 1 1 d . . .
H38 H 1.0807 0.5404 0.2042 0.020 Uiso 1 1 calc R . .
C39 C 0.4403(5) 0.6553(3) 0.9831(3) 0.0244(13) Uani 1 1 d . . .
H39A H 0.4558 0.6034 0.9796 0.029 Uiso 1 1 calc R . .
H39B H 0.4509 0.6689 1.0252 0.029 Uiso 1 1 calc R . .
C40 C 0.3267(5) 0.6665(4) 0.9678(3) 0.0355(16) Uani 1 1 d . . .
H40A H 0.3131 0.6494 0.9269 0.043 Uiso 1 1 calc R . .
H40B H 0.3101 0.7183 0.9696 0.043 Uiso 1 1 calc R . .
C41 C 0.2579(5) 0.6257(3) 1.0113(3) 0.0321(15) Uani 1 1 d . . .
H41A H 0.2782 0.6380 1.0526 0.039 Uiso 1 1 calc R . .
H41B H 0.2681 0.5734 1.0058 0.039 Uiso 1 1 calc R . .
C42 C 0.1438(6) 0.6443(4) 1.0016(3) 0.0403(17) Uani 1 1 d . . .
H42A H 0.1328 0.6954 1.0098 0.060 Uiso 1 1 calc R . .
H42B H 0.1007 0.6155 1.0285 0.060 Uiso 1 1 calc R . .
H42C H 0.1244 0.6339 0.9603 0.060 Uiso 1 1 calc R . .
C43 C 0.4913(5) 0.7754(3) 0.9459(3) 0.0229(12) Uani 1 1 d . . .
H43A H 0.4243 0.7818 0.9248 0.027 Uiso 1 1 calc R . .
H43B H 0.5450 0.8017 0.9231 0.027 Uiso 1 1 calc R . .
C44 C 0.4826(5) 0.8095(4) 1.0074(3) 0.0309(15) Uani 1 1 d . . .
H44A H 0.5487 0.8024 1.0293 0.037 Uiso 1 1 calc R . .
H44B H 0.4268 0.7852 1.0300 0.037 Uiso 1 1 calc R . .
C45 C 0.4586(5) 0.8898(3) 1.0037(3) 0.0259(13) Uani 1 1 d . . .
H45A H 0.5178 0.9148 0.9847 0.031 Uiso 1 1 calc R . .
H45B H 0.3965 0.8972 0.9784 0.031 Uiso 1 1 calc R . .
C46 C 0.4392(6) 0.9221(4) 1.0649(3) 0.0373(16) Uani 1 1 d . . .
H46A H 0.3798 0.8980 1.0834 0.056 Uiso 1 1 calc R . .
H46B H 0.4242 0.9734 1.0608 0.056 Uiso 1 1 calc R . .
H46C H 0.5011 0.9156 1.0898 0.056 Uiso 1 1 calc R . .
C47 C 0.6247(5) 0.6839(3) 0.9732(3) 0.0263(14) Uani 1 1 d . . .
H47A H 0.6393 0.6317 0.9730 0.032 Uiso 1 1 calc R . .
H47B H 0.6223 0.6996 1.0152 0.032 Uiso 1 1 calc R . .
C48 C 0.7146(5) 0.7225(3) 0.9427(3) 0.0309(15) Uani 1 1 d . . .
H48A H 0.7172 0.7082 0.9003 0.037 Uiso 1 1 calc R . .
H48B H 0.7032 0.7750 0.9445 0.037 Uiso 1 1 calc R . .
C49 C 0.8163(5) 0.7042(4) 0.9723(3) 0.0383(17) Uani 1 1 d . . .
H49A H 0.8196 0.6518 0.9793 0.046 Uiso 1 1 calc R . .
H49B H 0.8200 0.7286 1.0114 0.046 Uiso 1 1 calc R . .
C50 C 0.9091(6) 0.7270(5) 0.9345(5) 0.058(2) Uani 1 1 d . . .
H50A H 0.9099 0.6991 0.8976 0.088 Uiso 1 1 calc R . .
H50B H 0.9736 0.7184 0.9567 0.088 Uiso 1 1 calc R . .
H50C H 0.9034 0.7783 0.9250 0.088 Uiso 1 1 calc R . .
C51 C 0.5164(5) 0.6707(3) 0.8804(2) 0.0218(12) Uani 1 1 d . . .
H51A H 0.4427 0.6664 0.8681 0.026 Uiso 1 1 calc R . .
H51B H 0.5481 0.7088 0.8557 0.026 Uiso 1 1 calc R . .
C52 C 0.5707(5) 0.6000(4) 0.8659(3) 0.0284(14) Uani 1 1 d . . .
H52A H 0.5698 0.5945 0.8221 0.034 Uiso 1 1 calc R . .
H52B H 0.6444 0.6051 0.8779 0.034 Uiso 1 1 calc R . .
C53 C 0.5311(6) 0.5305(3) 0.8921(3) 0.0290(14) Uani 1 1 d . . .
H53A H 0.4549 0.5278 0.8862 0.035 Uiso 1 1 calc R . .
H53B H 0.5448 0.5305 0.9355 0.035 Uiso 1 1 calc R . .
C54 C 0.5814(6) 0.4648(4) 0.8645(3) 0.0334(15) Uani 1 1 d . . .
H54A H 0.5697 0.4651 0.8215 0.050 Uiso 1 1 calc R . .
H54B H 0.5507 0.4213 0.8817 0.050 Uiso 1 1 calc R . .
H54C H 0.6563 0.4654 0.8727 0.050 Uiso 1 1 calc R . .
N1 N 0.8523(3) 0.7263(2) 0.26335(19) 0.0118(9) Uani 1 1 d . . .
H1 H 0.8892 0.7413 0.2329 0.014 Uiso 1 1 calc R . .
N2 N 0.8798(3) 0.8907(2) 0.21576(18) 0.0106(9) Uani 1 1 d . . .
H2A H 0.8990 0.8554 0.1923 0.013 Uiso 1 1 calc R . .
N3 N 1.1290(3) 0.8618(2) 0.19959(19) 0.0144(9) Uani 1 1 d . . .
H3A H 1.0805 0.8321 0.1869 0.017 Uiso 1 1 calc R . .
N4 N 1.0988(3) 0.6944(2) 0.24231(19) 0.0133(9) Uani 1 1 d . . .
H4 H 1.0626 0.7110 0.2120 0.016 Uiso 1 1 calc R . .
N5 N 0.5186(4) 0.6962(3) 0.9456(2) 0.0241(11) Uani 1 1 d . . .
N6 N 1.0837(4) 0.4826(3) 0.0979(2) 0.0245(11) Uani 1 1 d . . .
N7 N 0.7316(4) 0.5824(3) 0.09539(19) 0.0178(10) Uani 1 1 d . . .
N8 N 0.7656(4) 0.9459(3) 0.0142(2) 0.0265(12) Uani 1 1 d . . .
N9 N 1.1242(4) 0.8687(3) -0.0166(2) 0.0288(12) Uani 1 1 d . . .
O1 O 1.0698(4) 0.4604(3) 0.04747(18) 0.0321(11) Uani 1 1 d . . .
O2 O 1.1642(4) 0.4713(4) 0.1253(2) 0.0576(17) Uani 1 1 d . . .
O3 O 0.6711(3) 0.6259(2) 0.11706(18) 0.0270(10) Uani 1 1 d . . .
O4 O 0.7137(3) 0.5474(2) 0.05056(19) 0.0292(10) Uani 1 1 d . . .
O5 O 0.7007(4) 0.9754(3) 0.0469(2) 0.0476(14) Uani 1 1 d . . .
O6 O 0.7449(4) 0.9225(3) -0.0355(2) 0.0379(12) Uani 1 1 d . . .
O7 O 1.2082(4) 0.8536(4) 0.0064(2) 0.0515(15) Uani 1 1 d . . .
O8 O 1.1015(4) 0.8570(3) -0.0680(2) 0.0403(12) Uani 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
C1 N1 1.375(7) . ?
C1 C2 1.379(7) . ?
C1 C31 1.509(7) . ?
C2 C3 1.432(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.360(8) . ?
C3 H3 0.9500 . ?
C4 N1 1.393(7) . ?
C4 C5 1.516(7) . ?
C5 C8 1.501(8) . ?
C5 C7 1.542(7) . ?
C5 C6 1.562(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.377(8) . ?
C8 N2 1.380(7) . ?
C9 C10 1.427(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.347(8) . ?
C10 H10 0.9500 . ?
C11 N2 1.385(7) . ?
C11 C12 1.537(7) . ?
C12 C20 1.516(8) . ?
C12 C13 1.526(7) . ?
C12 C14 1.553(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C19 1.386(8) . ?
C14 C15 1.404(8) . ?
C15 C16 1.381(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.363(8) . ?
C16 N8 1.470(7) . ?
C17 C18 1.403(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(8) . ?
C18 N9 1.470(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.380(8) . ?
C20 N3 1.389(7) . ?
C21 C22 1.409(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.378(8) . ?
C22 H22 0.9500 . ?
C23 N3 1.383(7) . ?
C23 C24 1.507(8) . ?
C24 C27 1.499(8) . ?
C24 C26 1.553(8) . ?
C24 C25 1.554(8) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 N4 1.390(7) . ?
C27 C28 1.392(8) . ?
C28 C29 1.403(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.379(7) . ?
C29 H29 0.9500 . ?
C30 N4 1.372(7) . ?
C30 C31 1.522(7) . ?
C31 C33 1.536(7) . ?
C31 C32 1.548(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C38 1.384(8) . ?
C33 C34 1.407(7) . ?
C34 C35 1.375(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.376(8) . ?
C35 N7 1.488(7) . ?
C36 C37 1.402(8) . ?
C36 H36 0.9500 . ?
C37 C38 1.386(8) . ?
C37 N6 1.454(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.514(9) . ?
C39 N5 1.520(8) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.523(9) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.524(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N5 1.517(8) . ?
C43 C44 1.527(9) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.529(9) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.524(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 N5 1.516(7) . ?
C47 C48 1.525(10) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.505(9) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.528(12) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.527(9) . ?
C51 N5 1.539(7) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.511(9) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.519(9) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
N1 H1 0.8800 . ?
N2 H2A 0.8800 . ?
N3 H3A 0.8800 . ?
N4 H4 0.8800 . ?
N6 O1 1.219(6) . ?
N6 O2 1.222(7) . ?
N7 O4 1.222(6) . ?
N7 O3 1.225(6) . ?
N8 O6 1.229(7) . ?
N8 O5 1.242(7) . ?
N9 O8 1.211(7) . ?
N9 O7 1.229(8) . ?

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 107.2(5) . . ?
N1 C1 C31 122.3(4) . . ?
C2 C1 C31 130.3(5) . . ?
C1 C2 C3 107.2(5) . . ?
C1 C2 H2 126.4 . . ?
C3 C2 H2 126.4 . . ?
C4 C3 C2 108.5(5) . . ?
C4 C3 H3 125.8 . . ?
C2 C3 H3 125.8 . . ?
C3 C4 N1 106.8(5) . . ?
C3 C4 C5 131.2(5) . . ?
N1 C4 C5 121.7(4) . . ?
C8 C5 C4 112.2(4) . . ?
C8 C5 C7 108.8(4) . . ?
C4 C5 C7 107.7(4) . . ?
C8 C5 C6 109.8(4) . . ?
C4 C5 C6 109.6(4) . . ?
C7 C5 C6 108.6(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N2 106.3(5) . . ?
C9 C8 C5 130.2(5) . . ?
N2 C8 C5 123.4(4) . . ?
C8 C9 C10 108.4(5) . . ?
C8 C9 H9 125.8 . . ?
C10 C9 H9 125.8 . . ?
C11 C10 C9 107.3(5) . . ?
C11 C10 H10 126.4 . . ?
C9 C10 H10 126.4 . . ?
C10 C11 N2 108.3(5) . . ?
C10 C11 C12 130.8(5) . . ?
N2 C11 C12 120.9(4) . . ?
C20 C12 C13 110.0(4) . . ?
C20 C12 C11 110.6(4) . . ?
C13 C12 C11 109.7(4) . . ?
C20 C12 C14 110.3(4) . . ?
C13 C12 C14 107.7(4) . . ?
C11 C12 C14 108.5(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 119.3(5) . . ?
C19 C14 C12 121.0(5) . . ?
C15 C14 C12 119.7(5) . . ?
C16 C15 C14 119.1(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C17 C16 C15 123.6(5) . . ?
C17 C16 N8 117.5(5) . . ?
C15 C16 N8 119.0(5) . . ?
C16 C17 C18 116.2(5) . . ?
C16 C17 H17 121.9 . . ?
C18 C17 H17 121.9 . . ?
C19 C18 C17 122.7(5) . . ?
C19 C18 N9 119.3(5) . . ?
C17 C18 N9 117.9(5) . . ?
C14 C19 C18 119.1(5) . . ?
C14 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C21 C20 N3 106.7(5) . . ?
C21 C20 C12 130.9(5) . . ?
N3 C20 C12 122.3(5) . . ?
C20 C21 C22 108.0(5) . . ?
C20 C21 H21 126.0 . . ?
C22 C21 H21 126.0 . . ?
C23 C22 C21 108.5(5) . . ?
C23 C22 H22 125.7 . . ?
C21 C22 H22 125.7 . . ?
C22 C23 N3 106.6(5) . . ?
C22 C23 C24 131.2(5) . . ?
N3 C23 C24 121.9(5) . . ?
C27 C24 C23 113.7(5) . . ?
C27 C24 C26 108.6(5) . . ?
C23 C24 C26 109.4(5) . . ?
C27 C24 C25 108.7(5) . . ?
C23 C24 C25 108.7(5) . . ?
C26 C24 C25 107.4(5) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N4 C27 C28 105.9(5) . . ?
N4 C27 C24 122.8(5) . . ?
C28 C27 C24 131.2(5) . . ?
C27 C28 C29 108.1(5) . . ?
C27 C28 H28 126.0 . . ?
C29 C28 H28 126.0 . . ?
C30 C29 C28 108.5(5) . . ?
C30 C29 H29 125.7 . . ?
C28 C29 H29 125.7 . . ?
N4 C30 C29 106.7(5) . . ?
N4 C30 C31 121.9(4) . . ?
C29 C30 C31 131.3(5) . . ?
C1 C31 C30 111.3(4) . . ?
C1 C31 C33 110.5(4) . . ?
C30 C31 C33 109.0(4) . . ?
C1 C31 C32 109.4(4) . . ?
C30 C31 C32 109.3(4) . . ?
C33 C31 C32 107.2(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C38 C33 C34 118.2(5) . . ?
C38 C33 C31 119.7(5) . . ?
C34 C33 C31 122.0(5) . . ?
C35 C34 C33 119.1(5) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C34 C35 C36 124.5(5) . . ?
C34 C35 N7 117.6(5) . . ?
C36 C35 N7 117.8(4) . . ?
C35 C36 C37 115.2(5) . . ?
C35 C36 H36 122.4 . . ?
C37 C36 H36 122.4 . . ?
C38 C37 C36 122.3(5) . . ?
C38 C37 N6 120.1(5) . . ?
C36 C37 N6 117.6(5) . . ?
C33 C38 C37 120.6(5) . . ?
C33 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C40 C39 N5 116.5(5) . . ?
C40 C39 H39A 108.2 . . ?
N5 C39 H39A 108.2 . . ?
C40 C39 H39B 108.2 . . ?
N5 C39 H39B 108.2 . . ?
H39A C39 H39B 107.3 . . ?
C39 C40 C41 110.4(5) . . ?
C39 C40 H40A 109.6 . . ?
C41 C40 H40A 109.6 . . ?
C39 C40 H40B 109.6 . . ?
C41 C40 H40B 109.6 . . ?
H40A C40 H40B 108.1 . . ?
C40 C41 C42 110.9(6) . . ?
C40 C41 H41A 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 108.0 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C43 C44 115.2(5) . . ?
N5 C43 H43A 108.5 . . ?
C44 C43 H43A 108.5 . . ?
N5 C43 H43B 108.5 . . ?
C44 C43 H43B 108.5 . . ?
H43A C43 H43B 107.5 . . ?
C43 C44 C45 111.8(5) . . ?
C43 C44 H44A 109.2 . . ?
C45 C44 H44A 109.2 . . ?
C43 C44 H44B 109.2 . . ?
C45 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
C46 C45 C44 111.7(5) . . ?
C46 C45 H45A 109.3 . . ?
C44 C45 H45A 109.3 . . ?
C46 C45 H45B 109.3 . . ?
C44 C45 H45B 109.3 . . ?
H45A C45 H45B 107.9 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N5 C47 C48 115.4(5) . . ?
N5 C47 H47A 108.4 . . ?
C48 C47 H47A 108.4 . . ?
N5 C47 H47B 108.4 . . ?
C48 C47 H47B 108.4 . . ?
H47A C47 H47B 107.5 . . ?
C49 C48 C47 110.7(5) . . ?
C49 C48 H48A 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 108.1 . . ?
C48 C49 C50 111.8(6) . . ?
C48 C49 H49A 109.3 . . ?
C50 C49 H49A 109.3 . . ?
C48 C49 H49B 109.3 . . ?
C50 C49 H49B 109.3 . . ?
H49A C49 H49B 107.9 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 N5 117.5(5) . . ?
C52 C51 H51A 107.9 . . ?
N5 C51 H51A 107.9 . . ?
C52 C51 H51B 107.9 . . ?
N5 C51 H51B 107.9 . . ?
H51A C51 H51B 107.2 . . ?
C53 C52 C51 120.0(5) . . ?
C53 C52 H52A 107.3 . . ?
C51 C52 H52A 107.3 . . ?
C53 C52 H52B 107.3 . . ?
C51 C52 H52B 107.3 . . ?
H52A C52 H52B 106.9 . . ?
C52 C53 C54 112.7(6) . . ?
C52 C53 H53A 109.0 . . ?
C54 C53 H53A 109.0 . . ?
C52 C53 H53B 109.0 . . ?
C54 C53 H53B 109.0 . . ?
H53A C53 H53B 107.8 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C1 N1 C4 110.2(4) . . ?
C1 N1 H1 124.9 . . ?
C4 N1 H1 124.9 . . ?
C8 N2 C11 109.8(4) . . ?
C8 N2 H2A 125.1 . . ?
C11 N2 H2A 125.1 . . ?
C23 N3 C20 110.1(4) . . ?
C23 N3 H3A 124.9 . . ?
C20 N3 H3A 124.9 . . ?
C30 N4 C27 110.8(4) . . ?
C30 N4 H4 124.6 . . ?
C27 N4 H4 124.6 . . ?
C47 N5 C43 110.6(5) . . ?
C47 N5 C39 107.1(4) . . ?
C43 N5 C39 109.4(5) . . ?
C47 N5 C51 111.0(5) . . ?
C43 N5 C51 107.5(4) . . ?
C39 N5 C51 111.3(5) . . ?
O1 N6 O2 122.2(5) . . ?
O1 N6 C37 119.4(5) . . ?
O2 N6 C37 118.4(5) . . ?
O4 N7 O3 124.1(5) . . ?
O4 N7 C35 118.0(5) . . ?
O3 N7 C35 117.9(4) . . ?
O6 N8 O5 123.5(5) . . ?
O6 N8 C16 118.5(5) . . ?
O5 N8 C16 118.0(5) . . ?
O8 N9 O7 124.7(5) . . ?
O8 N9 C18 117.9(5) . . ?
O7 N9 C18 117.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         0.930
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.137
####################################################################### 
# 
# 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_TBACl-DNPC4P
_database_code_depnum_ccdc_archive 'CCDC 1482085'
_audit_update_record             
;
2016-05-26 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Cis-Dintrophenyl-calix[4]pyrrole-tetrabutylammonium chloride 
;
_chemical_name_common            Cis-DNP-Calix[4]pyrrole-TBACl
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 N8 O8, C16 H36 N, Cl'
_chemical_formula_sum            'C54 H72 Cl N9 O8'
_chemical_formula_weight         1010.66

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'
Cl Cl 0.1484 0.1585 '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   P21/n

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

_cell_length_a                   13.0109(16)
_cell_length_b                   18.833(2)
_cell_length_c                   22.702(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.423(3)
_cell_angle_gamma                90.00
_cell_volume                     5562.6(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    21580
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      27.47

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2160
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9626
_exptl_absorpt_correction_T_max  0.9936
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku SCX-Mini with Mercury CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30899
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.48
_reflns_number_total             12550
_reflns_number_gt                7570
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXS-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)+(0.0500P)²+2.8930P] 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_number_reflns         12550
_refine_ls_number_parameters     659
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0666
_refine_ls_wR_factor_ref         0.1677
_refine_ls_wR_factor_gt          0.1447
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_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
C53 C 0.1879(2) 0.80725(16) 0.18947(13) 0.0529(7) Uani 1 1 d . . .
H53A H 0.2470 0.7915 0.1672 0.079 Uiso 1 1 calc R . .
H53B H 0.1571 0.8481 0.1702 0.079 Uiso 1 1 calc R . .
H53C H 0.1379 0.7691 0.1915 0.079 Uiso 1 1 calc R . .
C54 C 0.4515(2) 0.90761(14) -0.00234(12) 0.0465(7) Uani 1 1 d . . .
H54 H 0.4352 0.8929 -0.0409 0.056 Uiso 1 1 calc R . .
N9 N 0.01851(19) 0.69761(13) 0.94781(10) 0.0551(6) Uani 1 1 d . . .
C1 C 0.6207(2) 0.93434(13) 0.20135(11) 0.0382(6) Uani 1 1 d . . .
C2 C 0.7112(2) 0.95997(16) 0.22383(14) 0.0538(8) Uani 1 1 d . . .
H2 H 0.7270 1.0081 0.2303 0.065 Uiso 1 1 calc R . .
C3 C 0.7769(2) 0.90177(17) 0.23568(15) 0.0590(8) Uani 1 1 d . . .
H3 H 0.8436 0.9045 0.2516 0.071 Uiso 1 1 calc R . .
C4 C 0.72635(19) 0.84056(15) 0.21983(12) 0.0438(6) Uani 1 1 d . . .
C5 C 0.7623(2) 0.76369(16) 0.21801(13) 0.0495(7) Uani 1 1 d . . .
C6 C 0.7568(2) 0.73653(17) 0.15336(14) 0.0617(8) Uani 1 1 d . . .
H6A H 0.6866 0.7399 0.1390 0.093 Uiso 1 1 calc R . .
H6B H 0.7792 0.6874 0.1519 0.093 Uiso 1 1 calc R . .
H6C H 0.8012 0.7653 0.1289 0.093 Uiso 1 1 calc R . .
C7 C 0.8756(2) 0.7609(2) 0.23913(18) 0.0748(11) Uani 1 1 d . . .
H7A H 0.9176 0.7896 0.2132 0.112 Uiso 1 1 calc R . .
H7B H 0.8997 0.7122 0.2384 0.112 Uiso 1 1 calc R . .
H7C H 0.8805 0.7793 0.2790 0.112 Uiso 1 1 calc R . .
C8 C 0.69913(19) 0.71474(14) 0.25719(12) 0.0410(6) Uani 1 1 d . . .
C9 C 0.7251(2) 0.67786(15) 0.30718(13) 0.0508(7) Uani 1 1 d . . .
H9 H 0.7886 0.6803 0.3271 0.061 Uiso 1 1 calc R . .
C10 C 0.6401(2) 0.63538(15) 0.32370(12) 0.0467(7) Uani 1 1 d . . .
H10 H 0.6370 0.6050 0.3565 0.056 Uiso 1 1 calc R . .
C11 C 0.5627(2) 0.64685(12) 0.28292(10) 0.0354(6) Uani 1 1 d . . .
C12 C 0.4556(2) 0.61513(12) 0.27705(10) 0.0353(6) Uani 1 1 d . . .
C13 C 0.4483(3) 0.54882(14) 0.31760(12) 0.0511(7) Uani 1 1 d . . .
H13A H 0.5028 0.5158 0.3079 0.077 Uiso 1 1 calc R . .
H13B H 0.3821 0.5260 0.3117 0.077 Uiso 1 1 calc R . .
H13C H 0.4553 0.5633 0.3584 0.077 Uiso 1 1 calc R . .
C14 C 0.4387(2) 0.58867(12) 0.21293(10) 0.0337(5) Uani 1 1 d . . .
C15 C 0.3453(2) 0.59834(12) 0.18326(10) 0.0350(6) Uani 1 1 d . . .
H15 H 0.2911 0.6227 0.2015 0.042 Uiso 1 1 calc R . .
C16 C 0.3331(2) 0.57164(13) 0.12645(11) 0.0357(6) Uani 1 1 d . . .
C17 C 0.4086(2) 0.53526(13) 0.09728(11) 0.0415(6) Uani 1 1 d . . .
H17 H 0.3986 0.5175 0.0590 0.050 Uiso 1 1 calc R . .
C18 C 0.5004(2) 0.52621(14) 0.12765(11) 0.0425(6) Uani 1 1 d . . .
C19 C 0.5165(2) 0.55189(13) 0.18439(11) 0.0401(6) Uani 1 1 d . . .
H19 H 0.5800 0.5444 0.2035 0.048 Uiso 1 1 calc R . .
C20 C 0.37257(19) 0.66745(13) 0.29408(10) 0.0343(5) Uani 1 1 d . . .
C21 C 0.3001(2) 0.66532(15) 0.33777(11) 0.0441(7) Uani 1 1 d . . .
H21 H 0.2942 0.6301 0.3668 0.053 Uiso 1 1 calc R . .
C22 C 0.2363(2) 0.72542(16) 0.33131(12) 0.0481(7) Uani 1 1 d . . .
H22 H 0.1807 0.7372 0.3557 0.058 Uiso 1 1 calc R . .
C23 C 0.26859(19) 0.76368(13) 0.28374(11) 0.0370(6) Uani 1 1 d . . .
C24 C 0.22289(19) 0.82826(14) 0.25310(12) 0.0408(6) Uani 1 1 d . . .
C25 C 0.1274(2) 0.85224(17) 0.28784(15) 0.0618(9) Uani 1 1 d . . .
H25A H 0.0793 0.8131 0.2907 0.093 Uiso 1 1 calc R . .
H25B H 0.0948 0.8917 0.2676 0.093 Uiso 1 1 calc R . .
H25C H 0.1482 0.8670 0.3271 0.093 Uiso 1 1 calc R . .
C26 C 0.29775(19) 0.88998(13) 0.24985(11) 0.0368(6) Uani 1 1 d . . .
C27 C 0.2940(2) 0.95544(15) 0.27584(14) 0.0555(8) Uani 1 1 d . . .
H27 H 0.2446 0.9705 0.3032 0.067 Uiso 1 1 calc R . .
C28 C 0.3769(2) 0.99674(14) 0.25465(13) 0.0530(8) Uani 1 1 d . . .
H28 H 0.3918 1.0439 0.2652 0.064 Uiso 1 1 calc R . .
C29 C 0.4313(2) 0.95576(12) 0.21625(11) 0.0351(6) Uani 1 1 d . . .
C30 C 0.5247(2) 0.97177(12) 0.17881(11) 0.0366(6) Uani 1 1 d . . .
C31 C 0.5444(2) 1.05314(13) 0.17862(13) 0.0516(7) Uani 1 1 d . . .
H31A H 0.5609 1.0688 0.2183 0.077 Uiso 1 1 calc R . .
H31B H 0.4832 1.0776 0.1647 0.077 Uiso 1 1 calc R . .
H31C H 0.6014 1.0638 0.1528 0.077 Uiso 1 1 calc R . .
C32 C 0.5004(2) 0.94980(12) 0.11409(11) 0.0364(6) Uani 1 1 d . . .
C33 C 0.4014(2) 0.95868(13) 0.09156(11) 0.0391(6) Uani 1 1 d . . .
H33 H 0.3497 0.9788 0.1150 0.047 Uiso 1 1 calc R . .
C34 C 0.3795(2) 0.93736(14) 0.03387(12) 0.0433(6) Uani 1 1 d . . .
C35 C 0.5491(2) 0.90049(14) 0.02098(12) 0.0452(7) Uani 1 1 d . . .
C36 C 0.5756(2) 0.92096(14) 0.07782(11) 0.0418(6) Uani 1 1 d . . .
H36 H 0.6434 0.9154 0.0917 0.050 Uiso 1 1 calc R . .
C37 C 0.1236(3) 0.68453(18) 0.97555(14) 0.0628(9) Uani 1 1 d . . .
H37A H 0.1356 0.6332 0.9769 0.075 Uiso 1 1 calc R . .
H37B H 0.1222 0.7017 1.0163 0.075 Uiso 1 1 calc R . .
C38 C 0.2151(3) 0.71948(19) 0.94433(17) 0.0730(10) Uani 1 1 d . . .
H38A H 0.2178 0.7027 0.9035 0.088 Uiso 1 1 calc R . .
H38B H 0.2051 0.7711 0.9435 0.088 Uiso 1 1 calc R . .
C39 C 0.3150(3) 0.7027(2) 0.9748(2) 0.0963(13) Uani 1 1 d . . .
H39A H 0.3166 0.7262 1.0133 0.116 Uiso 1 1 calc R . .
H39B H 0.3193 0.6514 0.9815 0.116 Uiso 1 1 calc R . .
C40 C 0.4063(3) 0.7262(3) 0.9397(3) 0.132(2) Uani 1 1 d . . .
H40A H 0.4138 0.6957 0.9056 0.198 Uiso 1 1 calc R . .
H40B H 0.4677 0.7233 0.9641 0.198 Uiso 1 1 calc R . .
H40C H 0.3963 0.7748 0.9269 0.198 Uiso 1 1 calc R . .
C41 C -0.0056(3) 0.77724(16) 0.94879(14) 0.0588(8) Uani 1 1 d . . .
H41A H -0.0708 0.7850 0.9279 0.071 Uiso 1 1 calc R . .
H41B H 0.0481 0.8021 0.9268 0.071 Uiso 1 1 calc R . .
C42 C -0.0134(3) 0.81112(18) 1.01002(15) 0.0687(9) Uani 1 1 d . . .
H42A H -0.0678 0.7874 1.0322 0.082 Uiso 1 1 calc R . .
H42B H 0.0516 0.8042 1.0314 0.082 Uiso 1 1 calc R . .
C43 C -0.0366(3) 0.88962(17) 1.00627(16) 0.0681(9) Uani 1 1 d . . .
H43A H 0.0205 0.9138 0.9867 0.082 Uiso 1 1 calc R . .
H43B H -0.0986 0.8967 0.9822 0.082 Uiso 1 1 calc R . .
C44 C -0.0589(3) 0.65759(17) 0.98495(14) 0.0629(9) Uani 1 1 d . . .
H44A H -0.0497 0.6720 1.0261 0.075 Uiso 1 1 calc R . .
H44B H -0.0432 0.6068 0.9826 0.075 Uiso 1 1 calc R . .
C45 C -0.1715(3) 0.6682(2) 0.96806(16) 0.0767(11) Uani 1 1 d . . .
H45A H -0.1883 0.7189 0.9695 0.092 Uiso 1 1 calc R . .
H45B H -0.1830 0.6516 0.9276 0.092 Uiso 1 1 calc R . .
C46 C -0.2410(3) 0.62788(19) 1.00934(16) 0.0770(11) Uani 1 1 d . . .
H46A H -0.2232 0.6401 1.0501 0.092 Uiso 1 1 calc R . .
H46B H -0.2298 0.5768 1.0042 0.092 Uiso 1 1 calc R . .
C47 C -0.3529(3) 0.6446(2) 0.9983(2) 0.0966(13) Uani 1 1 d . . .
H47A H -0.3656 0.6943 1.0068 0.145 Uiso 1 1 calc R . .
H47B H -0.3951 0.6152 1.0235 0.145 Uiso 1 1 calc R . .
H47C H -0.3698 0.6350 0.9573 0.145 Uiso 1 1 calc R . .
C48 C 0.0159(3) 0.67408(18) 0.88307(13) 0.0654(9) Uani 1 1 d . . .
H48A H 0.0523 0.7099 0.8599 0.078 Uiso 1 1 calc R . .
H48B H -0.0559 0.6743 0.8698 0.078 Uiso 1 1 calc R . .
C50 C 0.0343(5) 0.5346(3) 0.8903(2) 0.130(2) Uani 1 1 d . . .
H50A H -0.0407 0.5313 0.8871 0.156 Uiso 1 1 calc R . .
H50B H 0.0515 0.5345 0.9324 0.156 Uiso 1 1 calc R . .
C51 C 0.0783(3) 0.4691(2) 0.86411(17) 0.0858(12) Uani 1 1 d . . .
H51A H 0.0678 0.4698 0.8218 0.129 Uiso 1 1 calc R . .
H51B H 0.0445 0.4279 0.8806 0.129 Uiso 1 1 calc R . .
H51C H 0.1513 0.4669 0.8728 0.129 Uiso 1 1 calc R . .
Cl1 Cl 0.46142(5) 0.75845(3) 0.13257(3) 0.03719(16) Uani 1 1 d . . .
N1 N 0.63019(16) 0.86095(11) 0.19983(9) 0.0391(5) Uani 1 1 d . . .
H1 H 0.5824 0.8319 0.1880 0.047 Uiso 1 1 calc R . .
N2 N 0.59914(15) 0.69570(11) 0.24287(9) 0.0370(5) Uani 1 1 d . . .
H2A H 0.5644 0.7122 0.2130 0.044 Uiso 1 1 calc R . .
N3 N 0.35379(15) 0.72865(10) 0.26183(8) 0.0334(5) Uani 1 1 d . . .
H3A H 0.3902 0.7430 0.2321 0.040 Uiso 1 1 calc R . .
N4 N 0.38266(15) 0.89042(10) 0.21419(8) 0.0339(5) Uani 1 1 d . . .
H4 H 0.4031 0.8545 0.1932 0.041 Uiso 1 1 calc R . .
N5 N 0.6281(2) 0.86691(15) -0.01608(13) 0.0650(7) Uani 1 1 d . . .
N6 N 0.2730(2) 0.94554(16) 0.01148(13) 0.0662(7) Uani 1 1 d . . .
N7 N 0.5844(2) 0.48679(15) 0.09846(11) 0.0632(7) Uani 1 1 d . . .
N8 N 0.2319(2) 0.58097(13) 0.09696(10) 0.0498(6) Uani 1 1 d . . .
O1 O 0.7112(2) 0.85207(19) 0.00670(14) 0.1090(11) Uani 1 1 d . . .
O2 O 0.6064(2) 0.85388(16) -0.06717(11) 0.0966(9) Uani 1 1 d . . .
O3 O 0.2531(2) 0.92221(16) -0.03813(11) 0.0929(9) Uani 1 1 d . . .
O4 O 0.2099(2) 0.97520(19) 0.04298(13) 0.1080(11) Uani 1 1 d . . .
O5 O 0.6643(2) 0.4791(2) 0.12507(13) 0.1329(15) Uani 1 1 d . . .
O6 O 0.5691(2) 0.46353(14) 0.04945(10) 0.0820(8) Uani 1 1 d . . .
O7 O 0.21372(17) 0.54544(12) 0.05258(10) 0.0683(6) Uani 1 1 d . . .
O8 O 0.17106(17) 0.62363(13) 0.11825(10) 0.0695(6) Uani 1 1 d . . .
C52 C -0.0526(4) 0.9225(2) 1.06586(18) 0.0924(13) Uani 1 1 d . . .
H52A H -0.1114 0.9006 1.0845 0.139 Uiso 1 1 calc R . .
H52B H -0.0648 0.9730 1.0614 0.139 Uiso 1 1 calc R . .
H52C H 0.0082 0.9150 1.0901 0.139 Uiso 1 1 calc R . .
C49 C 0.0630(5) 0.5992(2) 0.86789(17) 0.130(2) Uani 1 1 d . . .
H49A H 0.0567 0.5945 0.8250 0.156 Uiso 1 1 calc R . .
H49B H 0.1368 0.6033 0.8763 0.156 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
C53 C24 1.562(4) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C53 H53C 0.9700 . ?
C54 C34 1.370(4) . ?
C54 C35 1.379(4) . ?
C54 H54 0.9400 . ?
N9 C44 1.519(4) . ?
N9 C37 1.522(4) . ?
N9 C41 1.532(4) . ?
N9 C48 1.535(4) . ?
C1 C2 1.368(4) . ?
C1 N1 1.388(3) . ?
C1 C30 1.520(4) . ?
C2 C3 1.415(4) . ?
C2 H2 0.9400 . ?
C3 C4 1.374(4) . ?
C3 H3 0.9400 . ?
C4 N1 1.382(3) . ?
C4 C5 1.522(4) . ?
C5 C8 1.526(4) . ?
C5 C7 1.547(4) . ?
C5 C6 1.555(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 C9 1.371(4) . ?
C8 N2 1.386(3) . ?
C9 C10 1.419(4) . ?
C9 H9 0.9400 . ?
C10 C11 1.379(3) . ?
C10 H10 0.9400 . ?
C11 N2 1.380(3) . ?
C11 C12 1.522(4) . ?
C12 C20 1.514(3) . ?
C12 C14 1.553(3) . ?
C12 C13 1.555(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 C19 1.391(3) . ?
C14 C15 1.397(3) . ?
C15 C16 1.392(3) . ?
C15 H15 0.9400 . ?
C16 C17 1.372(4) . ?
C16 N8 1.483(3) . ?
C17 C18 1.386(4) . ?
C17 H17 0.9400 . ?
C18 C19 1.390(4) . ?
C18 N7 1.482(4) . ?
C19 H19 0.9400 . ?
C20 C21 1.374(3) . ?
C20 N3 1.386(3) . ?
C21 C22 1.411(4) . ?
C21 H21 0.9400 . ?
C22 C23 1.367(4) . ?
C22 H22 0.9400 . ?
C23 N3 1.386(3) . ?
C23 C24 1.520(4) . ?
C24 C26 1.519(4) . ?
C24 C25 1.544(4) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.368(4) . ?
C26 N4 1.374(3) . ?
C27 C28 1.417(4) . ?
C27 H27 0.9400 . ?
C28 C29 1.366(3) . ?
C28 H28 0.9400 . ?
C29 N4 1.384(3) . ?
C29 C30 1.518(3) . ?
C30 C31 1.554(3) . ?
C30 C32 1.556(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C32 C33 1.393(4) . ?
C32 C36 1.394(4) . ?
C33 C34 1.397(4) . ?
C33 H33 0.9400 . ?
C34 N6 1.480(4) . ?
C35 C36 1.388(4) . ?
C35 N5 1.475(4) . ?
C36 H36 0.9400 . ?
C37 C38 1.537(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C38 C39 1.502(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C39 C40 1.502(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 H40C 0.9700 . ?
C41 C42 1.533(5) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C42 C43 1.511(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C43 C52 1.503(5) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C44 C45 1.525(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C45 C46 1.511(5) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C46 C47 1.509(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 H47C 0.9700 . ?
C48 C49 1.577(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C50 C49 1.371(6) . ?
C50 C51 1.486(6) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C51 H51C 0.9700 . ?
N1 H1 0.8700 . ?
N2 H2A 0.8700 . ?
N3 H3A 0.8700 . ?
N4 H4 0.8700 . ?
N5 O2 1.217(4) . ?
N5 O1 1.227(4) . ?
N6 O4 1.228(4) . ?
N6 O3 1.235(3) . ?
N7 O5 1.207(3) . ?
N7 O6 1.211(3) . ?
N8 O8 1.229(3) . ?
N8 O7 1.231(3) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 H52C 0.9700 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?

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
C24 C53 H53A 109.5 . . ?
C24 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C24 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C34 C54 C35 116.2(2) . . ?
C34 C54 H54 121.9 . . ?
C35 C54 H54 121.9 . . ?
C44 N9 C37 106.7(2) . . ?
C44 N9 C41 110.0(2) . . ?
C37 N9 C41 109.6(2) . . ?
C44 N9 C48 112.2(3) . . ?
C37 N9 C48 111.3(2) . . ?
C41 N9 C48 107.1(2) . . ?
C2 C1 N1 106.5(2) . . ?
C2 C1 C30 131.7(2) . . ?
N1 C1 C30 121.8(2) . . ?
C1 C2 C3 108.4(2) . . ?
C1 C2 H2 125.8 . . ?
C3 C2 H2 125.8 . . ?
C4 C3 C2 108.2(2) . . ?
C4 C3 H3 125.9 . . ?
C2 C3 H3 125.9 . . ?
C3 C4 N1 106.5(2) . . ?
C3 C4 C5 131.2(3) . . ?
N1 C4 C5 122.2(2) . . ?
C4 C5 C8 113.0(2) . . ?
C4 C5 C7 108.4(2) . . ?
C8 C5 C7 108.4(3) . . ?
C4 C5 C6 109.1(2) . . ?
C8 C5 C6 109.3(2) . . ?
C7 C5 C6 108.6(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N2 106.8(2) . . ?
C9 C8 C5 131.1(3) . . ?
N2 C8 C5 121.9(2) . . ?
C8 C9 C10 108.4(2) . . ?
C8 C9 H9 125.8 . . ?
C10 C9 H9 125.8 . . ?
C11 C10 C9 107.5(2) . . ?
C11 C10 H10 126.2 . . ?
C9 C10 H10 126.2 . . ?
N2 C11 C10 107.1(2) . . ?
N2 C11 C12 121.5(2) . . ?
C10 C11 C12 131.4(2) . . ?
C20 C12 C11 112.14(19) . . ?
C20 C12 C14 110.6(2) . . ?
C11 C12 C14 109.3(2) . . ?
C20 C12 C13 108.9(2) . . ?
C11 C12 C13 108.9(2) . . ?
C14 C12 C13 106.76(19) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 118.3(2) . . ?
C19 C14 C12 119.9(2) . . ?
C15 C14 C12 121.8(2) . . ?
C16 C15 C14 119.5(2) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C17 C16 C15 123.4(2) . . ?
C17 C16 N8 118.5(2) . . ?
C15 C16 N8 118.0(2) . . ?
C16 C17 C18 116.1(2) . . ?
C16 C17 H17 122.0 . . ?
C18 C17 H17 122.0 . . ?
C17 C18 C19 122.8(2) . . ?
C17 C18 N7 118.4(2) . . ?
C19 C18 N7 118.8(3) . . ?
C14 C19 C18 120.0(2) . . ?
C14 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 N3 106.6(2) . . ?
C21 C20 C12 131.3(2) . . ?
N3 C20 C12 122.0(2) . . ?
C20 C21 C22 107.9(2) . . ?
C20 C21 H21 126.0 . . ?
C22 C21 H21 126.0 . . ?
C23 C22 C21 108.7(2) . . ?
C23 C22 H22 125.6 . . ?
C21 C22 H22 125.6 . . ?
C22 C23 N3 106.5(2) . . ?
C22 C23 C24 131.4(2) . . ?
N3 C23 C24 121.9(2) . . ?
C26 C24 C23 112.7(2) . . ?
C26 C24 C25 108.6(2) . . ?
C23 C24 C25 108.3(2) . . ?
C26 C24 C53 109.4(2) . . ?
C23 C24 C53 109.3(2) . . ?
C25 C24 C53 108.5(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N4 106.3(2) . . ?
C27 C26 C24 130.1(2) . . ?
N4 C26 C24 123.5(2) . . ?
C26 C27 C28 108.6(2) . . ?
C26 C27 H27 125.7 . . ?
C28 C27 H27 125.7 . . ?
C29 C28 C27 107.8(2) . . ?
C29 C28 H28 126.1 . . ?
C27 C28 H28 126.1 . . ?
C28 C29 N4 106.6(2) . . ?
C28 C29 C30 131.7(2) . . ?
N4 C29 C30 121.7(2) . . ?
C1 C30 C29 112.2(2) . . ?
C1 C30 C31 108.8(2) . . ?
C29 C30 C31 109.3(2) . . ?
C1 C30 C32 110.8(2) . . ?
C29 C30 C32 108.6(2) . . ?
C31 C30 C32 107.0(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C36 118.8(2) . . ?
C33 C32 C30 119.7(2) . . ?
C36 C32 C30 121.5(2) . . ?
C32 C33 C34 119.4(2) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C54 C34 C33 123.0(3) . . ?
C54 C34 N6 118.6(3) . . ?
C33 C34 N6 118.4(3) . . ?
C54 C35 C36 123.5(3) . . ?
C54 C35 N5 117.8(3) . . ?
C36 C35 N5 118.7(3) . . ?
C35 C36 C32 119.1(3) . . ?
C35 C36 H36 120.4 . . ?
C32 C36 H36 120.4 . . ?
N9 C37 C38 115.9(2) . . ?
N9 C37 H37A 108.3 . . ?
C38 C37 H37A 108.3 . . ?
N9 C37 H37B 108.3 . . ?
C38 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C39 C38 C37 111.6(3) . . ?
C39 C38 H38A 109.3 . . ?
C37 C38 H38A 109.3 . . ?
C39 C38 H38B 109.3 . . ?
C37 C38 H38B 109.3 . . ?
H38A C38 H38B 108.0 . . ?
C40 C39 C38 112.3(4) . . ?
C40 C39 H39A 109.1 . . ?
C38 C39 H39A 109.1 . . ?
C40 C39 H39B 109.1 . . ?
C38 C39 H39B 109.1 . . ?
H39A C39 H39B 107.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N9 C41 C42 115.8(2) . . ?
N9 C41 H41A 108.3 . . ?
C42 C41 H41A 108.3 . . ?
N9 C41 H41B 108.3 . . ?
C42 C41 H41B 108.3 . . ?
H41A C41 H41B 107.4 . . ?
C43 C42 C41 111.8(3) . . ?
C43 C42 H42A 109.3 . . ?
C41 C42 H42A 109.3 . . ?
C43 C42 H42B 109.3 . . ?
C41 C42 H42B 109.3 . . ?
H42A C42 H42B 107.9 . . ?
C52 C43 C42 112.4(3) . . ?
C52 C43 H43A 109.1 . . ?
C42 C43 H43A 109.1 . . ?
C52 C43 H43B 109.1 . . ?
C42 C43 H43B 109.1 . . ?
H43A C43 H43B 107.9 . . ?
N9 C44 C45 115.8(2) . . ?
N9 C44 H44A 108.3 . . ?
C45 C44 H44A 108.3 . . ?
N9 C44 H44B 108.3 . . ?
C45 C44 H44B 108.3 . . ?
H44A C44 H44B 107.4 . . ?
C46 C45 C44 110.9(3) . . ?
C46 C45 H45A 109.5 . . ?
C44 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 108.1 . . ?
C45 C46 C47 111.9(3) . . ?
C45 C46 H46A 109.2 . . ?
C47 C46 H46A 109.2 . . ?
C45 C46 H46B 109.2 . . ?
C47 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N9 C48 C49 117.5(3) . . ?
N9 C48 H48A 107.9 . . ?
C49 C48 H48A 107.9 . . ?
N9 C48 H48B 107.9 . . ?
C49 C48 H48B 107.9 . . ?
H48A C48 H48B 107.2 . . ?
C49 C50 C51 118.7(5) . . ?
C49 C50 H50A 107.6 . . ?
C51 C50 H50A 107.6 . . ?
C49 C50 H50B 107.6 . . ?
C51 C50 H50B 107.6 . . ?
H50A C50 H50B 107.1 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C4 N1 C1 110.4(2) . . ?
C4 N1 H1 124.8 . . ?
C1 N1 H1 124.8 . . ?
C11 N2 C8 110.1(2) . . ?
C11 N2 H2A 124.9 . . ?
C8 N2 H2A 124.9 . . ?
C23 N3 C20 110.16(19) . . ?
C23 N3 H3A 124.9 . . ?
C20 N3 H3A 124.9 . . ?
C26 N4 C29 110.8(2) . . ?
C26 N4 H4 124.6 . . ?
C29 N4 H4 124.6 . . ?
O2 N5 O1 123.6(3) . . ?
O2 N5 C35 118.2(3) . . ?
O1 N5 C35 118.2(3) . . ?
O4 N6 O3 123.8(3) . . ?
O4 N6 C34 118.4(3) . . ?
O3 N6 C34 117.8(3) . . ?
O5 N7 O6 123.5(3) . . ?
O5 N7 C18 118.1(3) . . ?
O6 N7 C18 118.4(3) . . ?
O8 N8 O7 123.9(3) . . ?
O8 N8 C16 118.2(2) . . ?
O7 N8 C16 118.0(2) . . ?
C43 C52 H52A 109.5 . . ?
C43 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C43 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C49 C48 127.2(5) . . ?
C50 C49 H49A 105.5 . . ?
C48 C49 H49A 105.5 . . ?
C50 C49 H49B 105.5 . . ?
C48 C49 H49B 105.5 . . ?
H49A C49 H49B 106.1 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.052
####################################################################### 
# 
# 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_TBAI-DNPC4P
_database_code_depnum_ccdc_archive 'CCDC 1482086'
_audit_update_record             
;
2016-05-26 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Cis-dinitrophenyl-cali[4]pyrrole, terabutylammonium iodide
;
_chemical_name_common            Cis-DNP-Calix[4]pyrrole-TBAI
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H72 I N9 O8'
_chemical_formula_weight         1102.11

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'
I I -0.4742 1.8119 '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           Orthorhombic
_symmetry_space_group_name_H-M   Pca21

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

_cell_length_a                   21.335(12)
_cell_length_b                   15.168(8)
_cell_length_c                   37.948(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     12280(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    15495
_cell_measurement_theta_min      1.7189
_cell_measurement_theta_max      27.5165

_exptl_crystal_description       Block
_exptl_crystal_colour            Organge
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4608
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9187
_exptl_absorpt_correction_T_max  0.9663
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku SCX-Mini with Mercury CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32198
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.1258
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.34
_diffrn_reflns_theta_max         25.00
_reflns_number_total             16640
_reflns_number_gt                11575
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_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. 
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 1.137 0.249 0.278 405 144 ' '
2 0.363 0.249 0.778 405 143 ' '
3 0.637 0.751 0.278 405 145 ' '
4 0.863 0.751 0.778 405 144 ' '
_platon_squeeze_details          
;
The unit cell contain disordered diethylether molecules which have been 
treated as a diffuse contribution to the overall scattering without 
specific ation position by SQUEEZE/PLATON 
;

_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)+(0.1102P)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    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   0.73(3)
_refine_ls_number_reflns         16640
_refine_ls_number_parameters     1309
_refine_ls_number_restraints     133
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.2090
_refine_ls_wR_factor_gt          0.1835
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.005

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 0.3841(6) 0.0014(6) 0.3538(4) 0.041(3) Uani 1 1 d . . .
C2 C 0.3518(5) -0.0790(7) 0.3582(3) 0.054(3) Uani 1 1 d . . .
H2 H 0.3423 -0.1189 0.3400 0.064 Uiso 1 1 calc R . .
C3 C 0.3361(5) -0.0904(7) 0.3932(3) 0.053(3) Uani 1 1 d . . .
H3 H 0.3154 -0.1393 0.4031 0.063 Uiso 1 1 calc R . .
C4 C 0.3565(5) -0.0161(6) 0.4113(4) 0.041(2) Uani 1 1 d . . .
C5 C 0.3469(6) 0.0090(7) 0.4496(3) 0.041(3) Uani 1 1 d . . .
C6 C 0.3287(5) 0.1095(7) 0.4520(3) 0.056(3) Uani 1 1 d . . .
H6A H 0.3638 0.1453 0.4442 0.085 Uiso 1 1 calc R . .
H6B H 0.3184 0.1243 0.4761 0.085 Uiso 1 1 calc R . .
H6C H 0.2927 0.1208 0.4370 0.085 Uiso 1 1 calc R . .
C7 C 0.2899(4) -0.0410(7) 0.4650(3) 0.058(3) Uani 1 1 d . . .
H7A H 0.2983 -0.1039 0.4648 0.086 Uiso 1 1 calc R . .
H7B H 0.2531 -0.0288 0.4509 0.086 Uiso 1 1 calc R . .
H7C H 0.2826 -0.0217 0.4891 0.086 Uiso 1 1 calc R . .
C8 C 0.4071(6) -0.0089(7) 0.4724(4) 0.041(3) Uani 1 1 d . . .
C9 C 0.4120(5) -0.0527(8) 0.5034(3) 0.062(3) Uani 1 1 d . . .
H9 H 0.3799 -0.0809 0.5161 0.075 Uiso 1 1 calc R . .
C10 C 0.4754(5) -0.0469(8) 0.5125(3) 0.057(3) Uani 1 1 d . . .
H10 H 0.4937 -0.0720 0.5326 0.068 Uiso 1 1 calc R . .
C11 C 0.5053(6) -0.0008(7) 0.4883(3) 0.036(3) Uani 1 1 d . . .
C12 C 0.5750(4) 0.0288(7) 0.4863(2) 0.033(2) Uani 1 1 d . . .
C13 C 0.6116(6) -0.0129(7) 0.5190(3) 0.045(3) Uani 1 1 d . . .
H13A H 0.5925 0.0071 0.5408 0.068 Uiso 1 1 calc R . .
H13B H 0.6551 0.0056 0.5184 0.068 Uiso 1 1 calc R . .
H13C H 0.6094 -0.0767 0.5178 0.068 Uiso 1 1 calc R . .
C14 C 0.5818(4) 0.1269(6) 0.4891(2) 0.0350(19) Uani 1 1 d . . .
C15 C 0.6378(4) 0.1692(6) 0.4792(2) 0.0335(19) Uani 1 1 d . . .
H15 H 0.6722 0.1359 0.4713 0.040 Uiso 1 1 calc R . .
C16 C 0.6421(5) 0.2610(7) 0.4812(3) 0.044(2) Uani 1 1 d . . .
C17 C 0.5944(4) 0.3158(6) 0.4925(2) 0.039(2) Uani 1 1 d . . .
H17 H 0.5984 0.3774 0.4933 0.047 Uiso 1 1 calc R . .
C18 C 0.5387(5) 0.2714(6) 0.5027(3) 0.038(2) Uani 1 1 d . . .
C19 C 0.5304(4) 0.1817(6) 0.5013(3) 0.042(2) Uani 1 1 d . . .
H19 H 0.4921 0.1562 0.5081 0.051 Uiso 1 1 calc R . .
C20 C 0.6042(6) -0.0030(5) 0.4530(3) 0.030(3) Uani 1 1 d . . .
C21 C 0.6389(4) -0.0774(7) 0.4439(3) 0.049(2) Uani 1 1 d . . .
H21 H 0.6501 -0.1230 0.4595 0.058 Uiso 1 1 calc R . .
C22 C 0.6549(5) -0.0741(6) 0.4078(3) 0.050(2) Uani 1 1 d . . .
H22 H 0.6785 -0.1167 0.3956 0.060 Uiso 1 1 calc R . .
C23 C 0.6306(6) 0.0005(6) 0.3938(4) 0.045(3) Uani 1 1 d . . .
C24 C 0.6380(5) 0.0363(7) 0.3564(3) 0.048(2) Uani 1 1 d . . .
C25 C 0.6967(7) -0.0050(8) 0.3410(4) 0.072(5) Uani 1 1 d . . .
H25A H 0.6927 -0.0687 0.3414 0.108 Uiso 1 1 calc R . .
H25B H 0.7328 0.0124 0.3549 0.108 Uiso 1 1 calc R . .
H25C H 0.7022 0.0149 0.3169 0.108 Uiso 1 1 calc R . .
C26 C 0.5802(6) 0.0196(7) 0.3354(3) 0.039(2) Uani 1 1 d . . .
C27 C 0.5746(8) -0.0131(8) 0.3005(3) 0.061(4) Uani 1 1 d . . .
H27 H 0.6071 -0.0348 0.2863 0.073 Uiso 1 1 calc R . .
C28 C 0.5100(7) -0.0065(8) 0.2914(4) 0.055(3) Uani 1 1 d . . .
H28 H 0.4924 -0.0237 0.2698 0.066 Uiso 1 1 calc R . .
C29 C 0.4783(5) 0.0280(8) 0.3186(3) 0.044(2) Uani 1 1 d . . .
C30 C 0.4095(5) 0.0476(6) 0.3216(3) 0.045(2) Uani 1 1 d . . .
C31 C 0.3732(7) 0.0131(8) 0.2877(3) 0.049(3) Uani 1 1 d . . .
H31A H 0.3925 0.0372 0.2667 0.074 Uiso 1 1 calc R . .
H31B H 0.3297 0.0317 0.2889 0.074 Uiso 1 1 calc R . .
H31C H 0.3751 -0.0508 0.2869 0.074 Uiso 1 1 calc R . .
C32 C 0.3963(4) 0.1471(6) 0.3249(2) 0.037(2) Uani 1 1 d . . .
C33 C 0.4431(6) 0.2078(8) 0.3185(3) 0.052(3) Uani 1 1 d . . .
H33 H 0.4838 0.1895 0.3123 0.062 Uiso 1 1 calc R . .
C34 C 0.4283(6) 0.2974(7) 0.3215(3) 0.054(3) Uani 1 1 d . . .
C35 C 0.3701(6) 0.3284(7) 0.3323(2) 0.053(3) Uani 1 1 d . . .
H35 H 0.3625 0.3890 0.3353 0.063 Uiso 1 1 calc R . .
C36 C 0.3249(5) 0.2679(6) 0.3383(3) 0.042(2) Uani 1 1 d . . .
N1 N 0.3850(3) 0.0377(5) 0.3875(2) 0.0413(19) Uani 1 1 d . . .
H1 H 0.4018 0.0884 0.3927 0.050 Uiso 1 1 calc R . .
N2 N 0.4631(4) 0.0218(6) 0.4624(2) 0.0374(18) Uani 1 1 d . . .
H2A H 0.4713 0.0507 0.4432 0.045 Uiso 1 1 calc R . .
N3 N 0.5995(3) 0.0431(5) 0.42043(19) 0.0391(18) Uani 1 1 d . . .
H3A H 0.5793 0.0924 0.4178 0.047 Uiso 1 1 calc R . .
N4 N 0.5207(3) 0.0454(5) 0.34490(18) 0.0389(17) Uani 1 1 d . . .
H4 H 0.5111 0.0695 0.3650 0.047 Uiso 1 1 calc R . .
N5 N 0.2636(5) 0.2959(7) 0.3498(3) 0.060(3) Uani 1 1 d . . .
N6 N 0.4792(5) 0.3635(8) 0.3166(3) 0.065(3) Uani 1 1 d . . .
N7 N 0.4854(5) 0.3286(9) 0.5122(3) 0.068(3) Uani 1 1 d . . .
N8 N 0.7021(4) 0.3033(7) 0.4707(3) 0.057(2) Uani 1 1 d . . .
O1 O 0.2237(5) 0.2435(6) 0.3563(4) 0.091(4) Uani 1 1 d . . .
O2 O 0.2557(5) 0.3752(5) 0.3550(3) 0.079(3) Uani 1 1 d . . .
O3 O 0.4673(5) 0.4414(6) 0.3217(3) 0.074(2) Uani 1 1 d . . .
O4 O 0.5316(5) 0.3353(7) 0.3067(3) 0.098(4) Uani 1 1 d . . .
O5 O 0.4360(5) 0.2901(8) 0.5200(4) 0.119(5) Uani 1 1 d . . .
O6 O 0.4902(5) 0.4088(6) 0.5108(3) 0.077(3) Uani 1 1 d . . .
O7 O 0.7082(5) 0.3815(5) 0.4744(3) 0.084(3) Uani 1 1 d . . .
O8 O 0.7422(6) 0.2573(7) 0.4598(5) 0.120(6) Uani 1 1 d . . .
I1 I 0.48697(3) 0.23054(3) 0.409978(13) 0.04167(16) Uani 1 1 d . . .
C37 C 0.3370(4) 0.1786(6) 0.3348(2) 0.039(2) Uani 1 1 d . . .
H37 H 0.3046 0.1380 0.3392 0.047 Uiso 1 1 calc R . .
C38 C 0.6509(5) 0.1382(7) 0.3590(3) 0.062(3) Uani 1 1 d . . .
H38A H 0.6562 0.1622 0.3355 0.093 Uiso 1 1 calc R . .
H38B H 0.6888 0.1482 0.3726 0.093 Uiso 1 1 calc R . .
H38C H 0.6158 0.1669 0.3705 0.093 Uiso 1 1 calc R . .
C39 C 0.3324(5) 0.5210(8) 0.2307(3) 0.037(2) Uani 1 1 d . . .
C40 C 0.3272(5) 0.4820(8) 0.2621(3) 0.052(3) Uani 1 1 d . . .
H40 H 0.3608 0.4575 0.2748 0.063 Uiso 1 1 calc R . .
C41 C 0.2639(7) 0.4826(9) 0.2737(3) 0.056(3) Uani 1 1 d . . .
H41 H 0.2486 0.4608 0.2952 0.068 Uiso 1 1 calc R . .
C42 C 0.2296(5) 0.5213(7) 0.2473(3) 0.036(2) Uani 1 1 d . . .
C43 C 0.1604(4) 0.5413(6) 0.2433(2) 0.039(2) Uani 1 1 d . . .
C44 C 0.1264(7) 0.5029(8) 0.2753(4) 0.056(4) Uani 1 1 d . . .
H44A H 0.1381 0.4415 0.2781 0.084 Uiso 1 1 calc R . .
H44B H 0.0815 0.5072 0.2717 0.084 Uiso 1 1 calc R . .
H44C H 0.1381 0.5356 0.2962 0.084 Uiso 1 1 calc R . .
C45 C 0.1471(4) 0.6396(6) 0.2427(2) 0.040(2) Uani 1 1 d . . .
C46 C 0.0886(5) 0.6723(6) 0.2330(3) 0.044(2) Uani 1 1 d . . .
H46 H 0.0558 0.6340 0.2267 0.052 Uiso 1 1 calc R . .
C47 C 0.0800(6) 0.7646(7) 0.2329(3) 0.052(3) Uani 1 1 d . . .
C48 C 0.1240(5) 0.8251(7) 0.2405(3) 0.053(3) Uani 1 1 d . . .
H48 H 0.1155 0.8859 0.2397 0.063 Uiso 1 1 calc R . .
C49 C 0.1806(5) 0.7940(8) 0.2492(3) 0.051(3) Uani 1 1 d . . .
C50 C 0.1309(6) 0.4955(6) 0.2113(3) 0.034(3) Uani 1 1 d . . .
C51 C 0.1050(5) 0.4153(7) 0.2074(3) 0.045(2) Uani 1 1 d . . .
H51 H 0.0991 0.3727 0.2251 0.054 Uiso 1 1 calc R . .
C52 C 0.0883(4) 0.4074(6) 0.1715(3) 0.048(2) Uani 1 1 d . . .
H52 H 0.0687 0.3581 0.1613 0.058 Uiso 1 1 calc R . .
C53 C 0.1048(5) 0.4815(7) 0.1542(3) 0.038(2) Uani 1 1 d . . .
C54 C 0.0968(6) 0.5076(7) 0.1162(4) 0.048(3) Uani 1 1 d . . .
C55 C 0.0428(4) 0.4566(8) 0.0998(3) 0.058(3) Uani 1 1 d . . .
H55A H 0.0366 0.4761 0.0758 0.088 Uiso 1 1 calc R . .
H55B H 0.0049 0.4670 0.1133 0.088 Uiso 1 1 calc R . .
H55C H 0.0525 0.3941 0.1000 0.088 Uiso 1 1 calc R . .
C56 C 0.0814(5) 0.6105(6) 0.1135(3) 0.048(2) Uani 1 1 d . . .
H56A H 0.1183 0.6443 0.1200 0.072 Uiso 1 1 calc R . .
H56B H 0.0473 0.6248 0.1294 0.072 Uiso 1 1 calc R . .
H56C H 0.0695 0.6250 0.0896 0.072 Uiso 1 1 calc R . .
C57 C 0.1528(6) 0.4911(7) 0.0941(3) 0.036(3) Uani 1 1 d . . .
C58 C 0.1608(5) 0.4481(8) 0.0624(3) 0.064(3) Uani 1 1 d . . .
H58 H 0.1287 0.4201 0.0496 0.077 Uiso 1 1 calc R . .
C59 C 0.2261(5) 0.4523(9) 0.0516(3) 0.066(4) Uani 1 1 d . . .
H59 H 0.2433 0.4272 0.0311 0.080 Uiso 1 1 calc R . .
C60 C 0.2582(7) 0.4996(5) 0.0768(3) 0.037(3) Uani 1 1 d . . .
C61 C 0.3254(5) 0.5235(8) 0.0789(3) 0.041(2) Uani 1 1 d . . .
C62 C 0.3606(6) 0.4877(7) 0.0494(3) 0.048(3) Uani 1 1 d . . .
H62A H 0.3647 0.4244 0.0521 0.072 Uiso 1 1 calc R . .
H62B H 0.4020 0.5143 0.0487 0.072 Uiso 1 1 calc R . .
H62C H 0.3387 0.5005 0.0275 0.072 Uiso 1 1 calc R . .
C63 C 0.3313(4) 0.6302(5) 0.0760(2) 0.0301(17) Uani 1 1 d . . .
C64 C 0.2825(4) 0.6795(6) 0.0643(2) 0.035(2) Uani 1 1 d . . .
H64 H 0.2452 0.6522 0.0570 0.043 Uiso 1 1 calc R . .
C65 C 0.2882(5) 0.7729(5) 0.0631(3) 0.033(2) Uani 1 1 d . . .
C66 C 0.3404(5) 0.8138(6) 0.0733(2) 0.045(2) Uani 1 1 d . . .
H66 H 0.3430 0.8757 0.0735 0.054 Uiso 1 1 calc R . .
C67 C 0.3907(4) 0.7619(7) 0.0836(3) 0.038(2) Uani 1 1 d . . .
C68 C 0.3866(4) 0.6695(6) 0.0850(3) 0.043(2) Uani 1 1 d . . .
H68 H 0.4212 0.6354 0.0920 0.051 Uiso 1 1 calc R . .
C69 C 0.3561(7) 0.4956(7) 0.1146(4) 0.046(3) Uani 1 1 d . . .
C70 C 0.3903(5) 0.4205(7) 0.1197(3) 0.052(3) Uani 1 1 d . . .
H70 H 0.4002 0.3767 0.1031 0.062 Uiso 1 1 calc R . .
C71 C 0.4076(4) 0.4240(7) 0.1563(3) 0.050(2) Uani 1 1 d . . .
H71 H 0.4322 0.3816 0.1679 0.060 Uiso 1 1 calc R . .
C72 C 0.3831(6) 0.4977(6) 0.1717(3) 0.038(3) Uani 1 1 d . . .
C73 C 0.3898(4) 0.5369(8) 0.2074(3) 0.049(3) Uani 1 1 d . . .
C74 C 0.4007(5) 0.6362(7) 0.2067(3) 0.058(3) Uani 1 1 d . . .
H74A H 0.4366 0.6494 0.1920 0.087 Uiso 1 1 calc R . .
H74B H 0.4084 0.6573 0.2304 0.087 Uiso 1 1 calc R . .
H74C H 0.3638 0.6653 0.1972 0.087 Uiso 1 1 calc R . .
C75 C 0.4458(6) 0.4954(9) 0.2268(3) 0.060(4) Uani 1 1 d . . .
H75A H 0.4393 0.4323 0.2289 0.090 Uiso 1 1 calc R . .
H75B H 0.4494 0.5212 0.2501 0.090 Uiso 1 1 calc R . .
H75C H 0.4839 0.5065 0.2136 0.090 Uiso 1 1 calc R . .
C76 C 0.1926(5) 0.7066(7) 0.2513(2) 0.044(2) Uani 1 1 d . . .
H76 H 0.2327 0.6886 0.2586 0.053 Uiso 1 1 calc R . .
I2 I 0.23695(3) 0.72857(3) 0.157749(13) 0.04313(16) Uani 1 1 d . . .
N9 N 0.2725(4) 0.5422(5) 0.2206(2) 0.0417(18) Uani 1 1 d . . .
H9A H 0.2625 0.5653 0.2004 0.050 Uiso 1 1 calc R . .
N10 N 0.3507(3) 0.5420(5) 0.14500(19) 0.0356(17) Uani 1 1 d . . .
H10A H 0.3303 0.5913 0.1475 0.043 Uiso 1 1 calc R . .
N11 N 0.2138(4) 0.5221(6) 0.1022(2) 0.0402(19) Uani 1 1 d . . .
H11 H 0.2226 0.5522 0.1211 0.048 Uiso 1 1 calc R . .
N12 N 0.1352(4) 0.5355(5) 0.1790(2) 0.0383(17) Uani 1 1 d . . .
H12 H 0.1535 0.5856 0.1746 0.046 Uiso 1 1 calc R . .
N13 N 0.2329(4) 0.8258(7) 0.0547(3) 0.053(2) Uani 1 1 d . . .
N14 N 0.4498(4) 0.8034(6) 0.0942(3) 0.054(2) Uani 1 1 d . . .
N15 N 0.0150(6) 0.7944(8) 0.2225(3) 0.074(3) Uani 1 1 d . . .
N16 N 0.2305(6) 0.8567(7) 0.2552(3) 0.073(3) Uani 1 1 d . . .
O9 O 0.2787(5) 0.8267(6) 0.2657(4) 0.123(5) Uani 1 1 d . . .
O10 O 0.2223(5) 0.9329(6) 0.2485(3) 0.093(3) Uani 1 1 d . . .
O11 O -0.0292(6) 0.7391(7) 0.2220(4) 0.109(5) Uani 1 1 d . . .
O12 O 0.0078(5) 0.8735(6) 0.2169(3) 0.093(3) Uani 1 1 d . . .
O13 O 0.4935(6) 0.7614(6) 0.1049(5) 0.119(6) Uani 1 1 d . . .
O14 O 0.4517(4) 0.8844(6) 0.0931(3) 0.081(3) Uani 1 1 d . . .
O15 O 0.2370(4) 0.9035(5) 0.0553(3) 0.076(3) Uani 1 1 d . . .
O16 O 0.1860(6) 0.7868(7) 0.0442(4) 0.127(6) Uani 1 1 d . . .
N1A N 0.4020(5) 0.5487(6) 0.4289(2) 0.066(3) Uani 1 1 d D . .
C1A C 0.3768(6) 0.4548(7) 0.4291(4) 0.064(3) Uani 1 1 d D . .
H1A1 H 0.3820 0.4305 0.4054 0.077 Uiso 1 1 calc R . .
H1A2 H 0.4033 0.4198 0.4450 0.077 Uiso 1 1 calc R . .
C2A C 0.3098(5) 0.4414(8) 0.4400(4) 0.082(4) Uani 1 1 d D . .
H2A1 H 0.2823 0.4620 0.4210 0.099 Uiso 1 1 calc R . .
H2A2 H 0.3012 0.4773 0.4609 0.099 Uiso 1 1 calc R . .
C3A C 0.2938(6) 0.3419(9) 0.4485(5) 0.093(5) Uani 1 1 d D . .
H3A1 H 0.3095 0.3047 0.4293 0.112 Uiso 1 1 calc R . .
H3A2 H 0.3158 0.3246 0.4701 0.112 Uiso 1 1 calc R . .
C4A C 0.2273(6) 0.3256(11) 0.4530(5) 0.095(5) Uani 1 1 d D . .
H4A1 H 0.2119 0.3595 0.4729 0.143 Uiso 1 1 calc R . .
H4A2 H 0.2204 0.2633 0.4573 0.143 Uiso 1 1 calc R . .
H4A3 H 0.2051 0.3431 0.4318 0.143 Uiso 1 1 calc R . .
C5A C 0.3556(5) 0.6108(7) 0.4103(4) 0.083(4) Uani 1 1 d D . .
H5A1 H 0.3166 0.6119 0.4240 0.099 Uiso 1 1 calc R . .
H5A2 H 0.3731 0.6705 0.4107 0.099 Uiso 1 1 calc R . .
C6A C 0.3397(8) 0.5880(10) 0.3728(4) 0.106(6) Uani 1 1 d D . .
H6A1 H 0.3150 0.5336 0.3729 0.127 Uiso 1 1 calc R . .
H6A2 H 0.3788 0.5758 0.3602 0.127 Uiso 1 1 calc R . .
C7A C 0.3015(11) 0.6617(16) 0.3512(7) 0.164(9) Uani 1 1 d DU . .
H7A1 H 0.3198 0.7202 0.3551 0.196 Uiso 1 1 calc R . .
H7A2 H 0.3027 0.6488 0.3259 0.196 Uiso 1 1 calc R . .
C8A C 0.2396(14) 0.659(3) 0.3636(10) 0.282(17) Uani 1 1 d DU . .
H8A1 H 0.2395 0.6410 0.3881 0.424 Uiso 1 1 calc R . .
H8A2 H 0.2156 0.6174 0.3498 0.424 Uiso 1 1 calc R . .
H8A3 H 0.2210 0.7172 0.3616 0.424 Uiso 1 1 calc R . .
C9A C 0.4636(5) 0.5496(9) 0.4079(4) 0.087(4) Uani 1 1 d D . .
H9A1 H 0.4556 0.5248 0.3845 0.104 Uiso 1 1 calc R . .
H9A2 H 0.4768 0.6109 0.4047 0.104 Uiso 1 1 calc R . .
C10A C 0.5168(7) 0.4994(10) 0.4245(4) 0.084(5) Uani 1 1 d DU . .
H10B H 0.5083 0.4360 0.4261 0.100 Uiso 1 1 calc R . .
H10C H 0.5282 0.5225 0.4477 0.100 Uiso 1 1 calc R . .
C11A C 0.5701(13) 0.524(2) 0.3936(7) 0.225(14) Uani 1 1 d DU . .
H11A H 0.5554 0.5050 0.3703 0.271 Uiso 1 1 calc R . .
H11B H 0.5782 0.5871 0.3931 0.271 Uiso 1 1 calc R . .
C12A C 0.6258(15) 0.477(2) 0.4030(9) 0.298(18) Uani 1 1 d DU . .
H12A H 0.6231 0.4165 0.3944 0.448 Uiso 1 1 calc R . .
H12B H 0.6302 0.4761 0.4285 0.448 Uiso 1 1 calc R . .
H12C H 0.6619 0.5054 0.3926 0.448 Uiso 1 1 calc R . .
C13A C 0.4124(8) 0.5768(9) 0.4669(3) 0.090(5) Uani 1 1 d D . .
H13D H 0.3725 0.5732 0.4796 0.107 Uiso 1 1 calc R . .
H13E H 0.4417 0.5355 0.4781 0.107 Uiso 1 1 calc R . .
C14A C 0.4379(10) 0.6682(12) 0.4702(5) 0.148(8) Uani 1 1 d DU . .
H14A H 0.4093 0.7094 0.4585 0.178 Uiso 1 1 calc R . .
H14B H 0.4785 0.6713 0.4582 0.178 Uiso 1 1 calc R . .
C15A C 0.4468(9) 0.6979(15) 0.5110(5) 0.115(6) Uani 1 1 d DU . .
H15A H 0.4424 0.7619 0.5135 0.138 Uiso 1 1 calc R . .
H15B H 0.4162 0.6686 0.5262 0.138 Uiso 1 1 calc R . .
C16A C 0.5081(9) 0.6706(15) 0.5190(6) 0.145(8) Uani 1 1 d DU . .
H16A H 0.5261 0.6409 0.4987 0.217 Uiso 1 1 calc R . .
H16B H 0.5072 0.6305 0.5389 0.217 Uiso 1 1 calc R . .
H16C H 0.5334 0.7217 0.5248 0.217 Uiso 1 1 calc R . .
N2A N 0.1475(5) 0.0425(6) 0.1386(3) 0.064(3) Uani 1 1 d D . .
C1B C 0.1210(6) -0.0498(7) 0.1391(4) 0.082(4) Uani 1 1 d D . .
H1B1 H 0.1215 -0.0708 0.1635 0.099 Uiso 1 1 calc R . .
H1B2 H 0.1493 -0.0878 0.1256 0.099 Uiso 1 1 calc R . .
C2B C 0.0549(7) -0.0622(8) 0.1246(4) 0.089(4) Uani 1 1 d D . .
H2B1 H 0.0527 -0.0374 0.1008 0.107 Uiso 1 1 calc R . .
H2B2 H 0.0252 -0.0297 0.1395 0.107 Uiso 1 1 calc R . .
C3B C 0.0355(8) -0.1593(9) 0.1233(5) 0.111(6) Uani 1 1 d D . .
H3B1 H 0.0622 -0.1897 0.1062 0.134 Uiso 1 1 calc R . .
H3B2 H 0.0435 -0.1857 0.1465 0.134 Uiso 1 1 calc R . .
C4B C -0.0268(9) -0.1741(17) 0.1144(9) 0.211(15) Uani 1 1 d D . .
H4B1 H -0.0507 -0.1869 0.1355 0.317 Uiso 1 1 calc R . .
H4B2 H -0.0294 -0.2238 0.0984 0.317 Uiso 1 1 calc R . .
H4B3 H -0.0438 -0.1220 0.1031 0.317 Uiso 1 1 calc R . .
C5B C 0.2089(6) 0.0475(8) 0.1586(4) 0.084(4) Uani 1 1 d D . .
H5B1 H 0.2208 0.1095 0.1612 0.100 Uiso 1 1 calc R . .
H5B2 H 0.2027 0.0232 0.1823 0.100 Uiso 1 1 calc R . .
C6B C 0.2618(8) -0.0012(12) 0.1412(6) 0.133(9) Uani 1 1 d D . .
H6B1 H 0.2723 0.0299 0.1194 0.159 Uiso 1 1 calc R . .
H6B2 H 0.2465 -0.0598 0.1346 0.159 Uiso 1 1 calc R . .
C7B C 0.3242(8) -0.0133(13) 0.1632(5) 0.117(6) Uani 1 1 d DU . .
H7B1 H 0.3159 -0.0521 0.1833 0.141 Uiso 1 1 calc R . .
H7B2 H 0.3559 -0.0418 0.1484 0.141 Uiso 1 1 calc R . .
C8B C 0.3468(14) 0.0639(17) 0.1751(9) 0.234(13) Uani 1 1 d DU . .
H8B1 H 0.3787 0.0530 0.1927 0.352 Uiso 1 1 calc R . .
H8B2 H 0.3130 0.0980 0.1854 0.352 Uiso 1 1 calc R . .
H8B3 H 0.3649 0.0966 0.1556 0.352 Uiso 1 1 calc R . .
C9B C 0.1527(7) 0.0744(9) 0.1010(3) 0.088(4) Uani 1 1 d D . .
H9B1 H 0.1110 0.0701 0.0903 0.105 Uiso 1 1 calc R . .
H9B2 H 0.1798 0.0329 0.0883 0.105 Uiso 1 1 calc R . .
C10B C 0.1776(11) 0.1681(11) 0.0938(4) 0.145(9) Uani 1 1 d D . .
H10D H 0.2119 0.1795 0.1104 0.174 Uiso 1 1 calc R . .
H10E H 0.1440 0.2100 0.0993 0.174 Uiso 1 1 calc R . .
C11B C 0.2024(13) 0.189(2) 0.0550(6) 0.181(11) Uani 1 1 d DU . .
H11C H 0.1694 0.1725 0.0384 0.217 Uiso 1 1 calc R . .
H11D H 0.2078 0.2532 0.0532 0.217 Uiso 1 1 calc R . .
C12B C 0.2569(15) 0.150(2) 0.0440(10) 0.270(16) Uani 1 1 d DU . .
H12D H 0.2821 0.1347 0.0643 0.405 Uiso 1 1 calc R . .
H12E H 0.2801 0.1914 0.0293 0.405 Uiso 1 1 calc R . .
H12F H 0.2472 0.0978 0.0305 0.405 Uiso 1 1 calc R . .
C13B C 0.1033(7) 0.1086(8) 0.1571(3) 0.084(4) Uani 1 1 d D . .
H13F H 0.1231 0.1670 0.1564 0.101 Uiso 1 1 calc R . .
H13G H 0.0645 0.1122 0.1434 0.101 Uiso 1 1 calc R . .
C14B C 0.0862(8) 0.0880(10) 0.1953(4) 0.099(5) Uani 1 1 d D . .
H14C H 0.1232 0.0932 0.2105 0.119 Uiso 1 1 calc R . .
H14D H 0.0697 0.0280 0.1973 0.119 Uiso 1 1 calc R . .
C15B C 0.0350(8) 0.1572(12) 0.2063(5) 0.112(6) Uani 1 1 d DU . .
H15C H 0.0370 0.1673 0.2318 0.135 Uiso 1 1 calc R . .
H15D H 0.0429 0.2134 0.1944 0.135 Uiso 1 1 calc R . .
C16B C -0.0242(10) 0.1263(14) 0.1973(6) 0.149(8) Uani 1 1 d DU . .
H16D H -0.0222 0.0976 0.1745 0.223 Uiso 1 1 calc R . .
H16E H -0.0533 0.1754 0.1962 0.223 Uiso 1 1 calc R . .
H16F H -0.0383 0.0844 0.2149 0.223 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 1.392(16) . ?
C1 C2 1.412(15) . ?
C1 C30 1.512(17) . ?
C2 C3 1.383(16) . ?
C2 H2 0.9400 . ?
C3 C4 1.389(16) . ?
C3 H3 0.9400 . ?
C4 N1 1.358(14) . ?
C4 C5 1.519(19) . ?
C5 C7 1.549(14) . ?
C5 C8 1.570(17) . ?
C5 C6 1.575(16) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 N2 1.337(15) . ?
C8 C9 1.356(16) . ?
C9 C10 1.397(14) . ?
C9 H9 0.9400 . ?
C10 C11 1.318(15) . ?
C10 H10 0.9400 . ?
C11 N2 1.378(14) . ?
C11 C12 1.553(15) . ?
C12 C20 1.491(15) . ?
C12 C14 1.499(13) . ?
C12 C13 1.598(13) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 C15 1.406(12) . ?
C14 C19 1.453(13) . ?
C15 C16 1.397(13) . ?
C15 H15 0.9400 . ?
C16 C17 1.381(14) . ?
C16 N8 1.488(13) . ?
C17 C18 1.418(13) . ?
C17 H17 0.9400 . ?
C18 C19 1.374(14) . ?
C18 N7 1.475(14) . ?
C19 H19 0.9400 . ?
C20 C21 1.393(14) . ?
C20 N3 1.422(13) . ?
C21 C22 1.413(15) . ?
C21 H21 0.9400 . ?
C22 C23 1.355(15) . ?
C22 H22 0.9400 . ?
C23 N3 1.372(13) . ?
C23 C24 1.525(17) . ?
C24 C26 1.491(15) . ?
C24 C25 1.519(15) . ?
C24 C38 1.573(15) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 N4 1.377(14) . ?
C26 C27 1.417(16) . ?
C27 C28 1.42(2) . ?
C27 H27 0.9400 . ?
C28 C29 1.338(17) . ?
C28 H28 0.9400 . ?
C29 N4 1.373(12) . ?
C29 C30 1.502(14) . ?
C30 C32 1.540(13) . ?
C30 C31 1.590(14) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C32 C33 1.380(14) . ?
C32 C37 1.405(13) . ?
C33 C34 1.400(15) . ?
C33 H33 0.9400 . ?
C34 C35 1.390(17) . ?
C34 N6 1.489(14) . ?
C35 C36 1.350(14) . ?
C35 H35 0.9400 . ?
C36 C37 1.385(14) . ?
C36 N5 1.443(15) . ?
N1 H1 0.8700 . ?
N2 H2A 0.8700 . ?
N3 H3A 0.8700 . ?
N4 H4 0.8700 . ?
N5 O1 1.191(13) . ?
N5 O2 1.231(13) . ?
N6 O3 1.224(15) . ?
N6 O4 1.256(14) . ?
N7 O6 1.221(16) . ?
N7 O5 1.241(14) . ?
N8 O8 1.179(15) . ?
N8 O7 1.202(13) . ?
C37 H37 0.9400 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 C40 1.332(16) . ?
C39 N9 1.374(13) . ?
C39 C73 1.530(14) . ?
C40 C41 1.420(18) . ?
C40 H40 0.9400 . ?
C41 C42 1.372(16) . ?
C41 H41 0.9400 . ?
C42 N9 1.402(13) . ?
C42 C43 1.516(14) . ?
C43 C45 1.518(13) . ?
C43 C44 1.527(15) . ?
C43 C50 1.536(15) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 H44C 0.9700 . ?
C45 C46 1.393(14) . ?
C45 C76 1.442(13) . ?
C46 C47 1.412(13) . ?
C46 H46 0.9400 . ?
C47 C48 1.345(16) . ?
C47 N15 1.510(15) . ?
C48 C49 1.337(16) . ?
C48 H48 0.9400 . ?
C49 C76 1.353(15) . ?
C49 N16 1.446(15) . ?
C50 C51 1.344(14) . ?
C50 N12 1.371(14) . ?
C51 C52 1.412(15) . ?
C51 H51 0.9400 . ?
C52 C53 1.349(15) . ?
C52 H52 0.9400 . ?
C53 N12 1.405(13) . ?
C53 C54 1.51(2) . ?
C54 C57 1.481(19) . ?
C54 C55 1.519(15) . ?
C54 C56 1.599(14) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C55 H55C 0.9700 . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 H56C 0.9700 . ?
C57 C58 1.380(17) . ?
C57 N11 1.416(13) . ?
C58 C59 1.453(15) . ?
C58 H58 0.9400 . ?
C59 C60 1.376(16) . ?
C59 H59 0.9400 . ?
C60 N11 1.397(15) . ?
C60 C61 1.480(17) . ?
C61 C62 1.454(16) . ?
C61 C69 1.566(17) . ?
C61 C63 1.627(13) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C62 H62C 0.9700 . ?
C63 C64 1.357(12) . ?
C63 C68 1.364(12) . ?
C64 C65 1.423(13) . ?
C64 H64 0.9400 . ?
C65 C66 1.332(14) . ?
C65 N13 1.463(12) . ?
C66 C67 1.388(14) . ?
C66 H66 0.9400 . ?
C67 C68 1.406(14) . ?
C67 N14 1.466(12) . ?
C68 H68 0.9400 . ?
C69 N10 1.354(16) . ?
C69 C70 1.366(15) . ?
C70 C71 1.439(16) . ?
C70 H70 0.9400 . ?
C71 C72 1.366(14) . ?
C71 H71 0.9400 . ?
C72 N10 1.399(13) . ?
C72 C73 1.486(16) . ?
C73 C74 1.525(15) . ?
C73 C75 1.536(14) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C74 H74C 0.9700 . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C75 H75C 0.9700 . ?
C76 H76 0.9400 . ?
N9 H9A 0.8700 . ?
N10 H10A 0.8700 . ?
N11 H11 0.8700 . ?
N12 H12 0.8700 . ?
N13 O15 1.181(13) . ?
N13 O16 1.229(14) . ?
N14 O13 1.201(14) . ?
N14 O14 1.230(13) . ?
N15 O12 1.228(15) . ?
N15 O11 1.262(16) . ?
N16 O9 1.193(14) . ?
N16 O10 1.196(15) . ?
N1A C13A 1.521(11) . ?
N1A C1A 1.522(11) . ?
N1A C5A 1.538(11) . ?
N1A C9A 1.539(12) . ?
C1A C2A 1.502(13) . ?
C1A H1A1 0.9800 . ?
C1A H1A2 0.9800 . ?
C2A C3A 1.580(15) . ?
C2A H2A1 0.9800 . ?
C2A H2A2 0.9800 . ?
C3A C4A 1.452(15) . ?
C3A H3A1 0.9800 . ?
C3A H3A2 0.9800 . ?
C4A H4A1 0.9700 . ?
C4A H4A2 0.9700 . ?
C4A H4A3 0.9700 . ?
C5A C6A 1.501(15) . ?
C5A H5A1 0.9800 . ?
C5A H5A2 0.9800 . ?
C6A C7A 1.609(17) . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C7A C8A 1.40(2) . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C8A H8A3 0.9700 . ?
C9A C10A 1.504(14) . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C10A C11A 1.674(19) . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C11A C12A 1.43(2) . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
C12A H12C 0.9700 . ?
C13A C14A 1.494(15) . ?
C13A H13D 0.9800 . ?
C13A H13E 0.9800 . ?
C14A C15A 1.621(17) . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C15A C16A 1.405(17) . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C16A H16A 0.9700 . ?
C16A H16B 0.9700 . ?
C16A H16C 0.9700 . ?
N2A C1B 1.509(11) . ?
N2A C9B 1.513(12) . ?
N2A C5B 1.515(11) . ?
N2A C13B 1.544(11) . ?
C1B C2B 1.526(14) . ?
C1B H1B1 0.9800 . ?
C1B H1B2 0.9800 . ?
C2B C3B 1.530(15) . ?
C2B H2B1 0.9800 . ?
C2B H2B2 0.9800 . ?
C3B C4B 1.390(16) . ?
C3B H3B1 0.9800 . ?
C3B H3B2 0.9800 . ?
C4B H4B1 0.9700 . ?
C4B H4B2 0.9700 . ?
C4B H4B3 0.9700 . ?
C5B C6B 1.500(15) . ?
C5B H5B1 0.9800 . ?
C5B H5B2 0.9800 . ?
C6B C7B 1.584(17) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C7B C8B 1.343(18) . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C8B H8B3 0.9700 . ?
C9B C10B 1.542(14) . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C10B C11B 1.597(18) . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C11B C12B 1.368(19) . ?
C11B H11C 0.9800 . ?
C11B H11D 0.9800 . ?
C12B H12D 0.9700 . ?
C12B H12E 0.9700 . ?
C12B H12F 0.9700 . ?
C13B C14B 1.528(14) . ?
C13B H13F 0.9800 . ?
C13B H13G 0.9800 . ?
C14B C15B 1.573(16) . ?
C14B H14C 0.9800 . ?
C14B H14D 0.9800 . ?
C15B C16B 1.389(16) . ?
C15B H15C 0.9800 . ?
C15B H15D 0.9800 . ?
C16B H16D 0.9700 . ?
C16B H16E 0.9700 . ?
C16B H16F 0.9700 . ?

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 103.9(11) . . ?
N1 C1 C30 123.8(8) . . ?
C2 C1 C30 132.1(11) . . ?
C3 C2 C1 109.8(10) . . ?
C3 C2 H2 125.1 . . ?
C1 C2 H2 125.1 . . ?
C2 C3 C4 107.2(10) . . ?
C2 C3 H3 126.4 . . ?
C4 C3 H3 126.4 . . ?
N1 C4 C3 107.6(11) . . ?
N1 C4 C5 123.0(10) . . ?
C3 C4 C5 129.2(10) . . ?
C4 C5 C7 110.2(10) . . ?
C4 C5 C8 111.9(11) . . ?
C7 C5 C8 110.4(9) . . ?
C4 C5 C6 109.3(9) . . ?
C7 C5 C6 105.0(9) . . ?
C8 C5 C6 109.8(9) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 110.3(11) . . ?
N2 C8 C5 120.9(10) . . ?
C9 C8 C5 128.8(11) . . ?
C8 C9 C10 105.0(10) . . ?
C8 C9 H9 127.5 . . ?
C10 C9 H9 127.5 . . ?
C11 C10 C9 109.4(10) . . ?
C11 C10 H10 125.3 . . ?
C9 C10 H10 125.3 . . ?
C10 C11 N2 108.1(10) . . ?
C10 C11 C12 130.7(10) . . ?
N2 C11 C12 121.2(9) . . ?
C20 C12 C14 109.8(8) . . ?
C20 C12 C11 110.4(9) . . ?
C14 C12 C11 112.1(8) . . ?
C20 C12 C13 109.1(8) . . ?
C14 C12 C13 106.9(8) . . ?
C11 C12 C13 108.3(8) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 117.7(8) . . ?
C15 C14 C12 121.2(8) . . ?
C19 C14 C12 121.1(8) . . ?
C16 C15 C14 119.7(8) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C17 C16 C15 124.6(9) . . ?
C17 C16 N8 117.3(9) . . ?
C15 C16 N8 118.0(9) . . ?
C16 C17 C18 114.6(8) . . ?
C16 C17 H17 122.7 . . ?
C18 C17 H17 122.7 . . ?
C19 C18 C17 124.6(9) . . ?
C19 C18 N7 119.5(9) . . ?
C17 C18 N7 115.7(8) . . ?
C18 C19 C14 118.8(8) . . ?
C18 C19 H19 120.6 . . ?
C14 C19 H19 120.6 . . ?
C21 C20 N3 102.8(9) . . ?
C21 C20 C12 133.9(9) . . ?
N3 C20 C12 123.2(8) . . ?
C20 C21 C22 109.8(9) . . ?
C20 C21 H21 125.1 . . ?
C22 C21 H21 125.1 . . ?
C23 C22 C21 108.6(9) . . ?
C23 C22 H22 125.7 . . ?
C21 C22 H22 125.7 . . ?
C22 C23 N3 106.7(11) . . ?
C22 C23 C24 128.6(10) . . ?
N3 C23 C24 124.6(9) . . ?
C26 C24 C25 114.0(10) . . ?
C26 C24 C23 110.7(9) . . ?
C25 C24 C23 107.2(10) . . ?
C26 C24 C38 110.2(10) . . ?
C25 C24 C38 106.5(8) . . ?
C23 C24 C38 108.1(9) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N4 C26 C27 105.5(11) . . ?
N4 C26 C24 125.0(9) . . ?
C27 C26 C24 129.0(12) . . ?
C26 C27 C28 106.4(12) . . ?
C26 C27 H27 126.8 . . ?
C28 C27 H27 126.8 . . ?
C29 C28 C27 109.2(11) . . ?
C29 C28 H28 125.4 . . ?
C27 C28 H28 125.4 . . ?
C28 C29 N4 107.7(10) . . ?
C28 C29 C30 129.0(11) . . ?
N4 C29 C30 123.3(9) . . ?
C29 C30 C1 108.7(10) . . ?
C29 C30 C32 112.3(9) . . ?
C1 C30 C32 108.8(8) . . ?
C29 C30 C31 110.5(9) . . ?
C1 C30 C31 109.1(9) . . ?
C32 C30 C31 107.4(8) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C37 118.2(9) . . ?
C33 C32 C30 120.5(9) . . ?
C37 C32 C30 121.3(8) . . ?
C32 C33 C34 118.0(11) . . ?
C32 C33 H33 121.0 . . ?
C34 C33 H33 121.0 . . ?
C35 C34 C33 123.7(10) . . ?
C35 C34 N6 117.4(11) . . ?
C33 C34 N6 118.6(12) . . ?
C36 C35 C34 117.2(10) . . ?
C36 C35 H35 121.4 . . ?
C34 C35 H35 121.4 . . ?
C35 C36 C37 121.1(10) . . ?
C35 C36 N5 119.8(9) . . ?
C37 C36 N5 119.0(9) . . ?
C4 N1 C1 111.4(9) . . ?
C4 N1 H1 124.3 . . ?
C1 N1 H1 124.3 . . ?
C8 N2 C11 107.3(9) . . ?
C8 N2 H2A 126.4 . . ?
C11 N2 H2A 126.4 . . ?
C23 N3 C20 112.0(9) . . ?
C23 N3 H3A 124.0 . . ?
C20 N3 H3A 124.0 . . ?
C29 N4 C26 111.2(8) . . ?
C29 N4 H4 124.4 . . ?
C26 N4 H4 124.4 . . ?
O1 N5 O2 121.3(12) . . ?
O1 N5 C36 121.0(11) . . ?
O2 N5 C36 117.5(10) . . ?
O3 N6 O4 124.1(11) . . ?
O3 N6 C34 118.6(11) . . ?
O4 N6 C34 117.2(12) . . ?
O6 N7 O5 123.4(11) . . ?
O6 N7 C18 120.7(10) . . ?
O5 N7 C18 115.9(11) . . ?
O8 N8 O7 123.2(10) . . ?
O8 N8 C16 117.7(9) . . ?
O7 N8 C16 119.1(10) . . ?
C36 C37 C32 121.7(9) . . ?
C36 C37 H37 119.2 . . ?
C32 C37 H37 119.2 . . ?
C24 C38 H38A 109.5 . . ?
C24 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C24 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 N9 106.0(10) . . ?
C40 C39 C73 130.8(10) . . ?
N9 C39 C73 123.1(9) . . ?
C39 C40 C41 110.7(10) . . ?
C39 C40 H40 124.6 . . ?
C41 C40 H40 124.6 . . ?
C42 C41 C40 106.5(11) . . ?
C42 C41 H41 126.7 . . ?
C40 C41 H41 126.8 . . ?
C41 C42 N9 106.0(10) . . ?
C41 C42 C43 132.7(11) . . ?
N9 C42 C43 121.3(9) . . ?
C42 C43 C45 112.3(8) . . ?
C42 C43 C44 107.9(9) . . ?
C45 C43 C44 107.4(8) . . ?
C42 C43 C50 112.7(8) . . ?
C45 C43 C50 110.9(8) . . ?
C44 C43 C50 105.2(9) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C76 114.4(9) . . ?
C46 C45 C43 121.3(9) . . ?
C76 C45 C43 124.3(9) . . ?
C45 C46 C47 118.0(9) . . ?
C45 C46 H46 121.0 . . ?
C47 C46 H46 121.0 . . ?
C48 C47 C46 125.9(10) . . ?
C48 C47 N15 119.5(10) . . ?
C46 C47 N15 114.6(11) . . ?
C49 C48 C47 116.3(10) . . ?
C49 C48 H48 121.9 . . ?
C47 C48 H48 121.9 . . ?
C48 C49 C76 122.1(10) . . ?
C48 C49 N16 118.2(11) . . ?
C76 C49 N16 119.7(10) . . ?
C51 C50 N12 109.2(10) . . ?
C51 C50 C43 131.7(10) . . ?
N12 C50 C43 118.7(9) . . ?
C50 C51 C52 106.7(9) . . ?
C50 C51 H51 126.7 . . ?
C52 C51 H51 126.7 . . ?
C53 C52 C51 109.4(9) . . ?
C53 C52 H52 125.3 . . ?
C51 C52 H52 125.3 . . ?
C52 C53 N12 106.3(10) . . ?
C52 C53 C54 131.0(10) . . ?
N12 C53 C54 122.7(10) . . ?
C57 C54 C53 113.9(11) . . ?
C57 C54 C55 107.2(10) . . ?
C53 C54 C55 110.1(11) . . ?
C57 C54 C56 107.1(10) . . ?
C53 C54 C56 109.9(9) . . ?
C55 C54 C56 108.5(10) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C58 C57 N11 103.5(10) . . ?
C58 C57 C54 132.3(10) . . ?
N11 C57 C54 124.2(10) . . ?
C57 C58 C59 110.0(10) . . ?
C57 C58 H58 125.0 . . ?
C59 C58 H58 125.0 . . ?
C60 C59 C58 107.8(11) . . ?
C60 C59 H59 126.1 . . ?
C58 C59 H59 126.1 . . ?
C59 C60 N11 105.6(11) . . ?
C59 C60 C61 130.3(12) . . ?
N11 C60 C61 124.1(10) . . ?
C62 C61 C60 111.5(10) . . ?
C62 C61 C69 110.5(9) . . ?
C60 C61 C69 112.7(10) . . ?
C62 C61 C63 106.2(9) . . ?
C60 C61 C63 108.4(8) . . ?
C69 C61 C63 107.1(8) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C64 C63 C68 120.2(8) . . ?
C64 C63 C61 120.7(8) . . ?
C68 C63 C61 119.0(8) . . ?
C63 C64 C65 119.6(8) . . ?
C63 C64 H64 120.2 . . ?
C65 C64 H64 120.2 . . ?
C66 C65 C64 121.7(8) . . ?
C66 C65 N13 118.8(8) . . ?
C64 C65 N13 119.0(8) . . ?
C65 C66 C67 117.7(8) . . ?
C65 C66 H66 121.2 . . ?
C67 C66 H66 121.2 . . ?
C66 C67 C68 121.9(9) . . ?
C66 C67 N14 119.9(9) . . ?
C68 C67 N14 118.2(9) . . ?
C63 C68 C67 118.7(8) . . ?
C63 C68 H68 120.6 . . ?
C67 C68 H68 120.6 . . ?
N10 C69 C70 111.1(12) . . ?
N10 C69 C61 124.2(10) . . ?
C70 C69 C61 124.8(12) . . ?
C69 C70 C71 104.0(10) . . ?
C69 C70 H70 128.0 . . ?
C71 C70 H70 128.0 . . ?
C72 C71 C70 110.3(9) . . ?
C72 C71 H71 124.9 . . ?
C70 C71 H71 124.9 . . ?
C71 C72 N10 105.7(10) . . ?
C71 C72 C73 132.9(11) . . ?
N10 C72 C73 121.2(9) . . ?
C72 C73 C74 113.1(8) . . ?
C72 C73 C39 112.7(9) . . ?
C74 C73 C39 106.7(10) . . ?
C72 C73 C75 110.4(10) . . ?
C74 C73 C75 107.2(9) . . ?
C39 C73 C75 106.3(9) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C73 C75 H75A 109.5 . . ?
C73 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C73 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C49 C76 C45 123.3(10) . . ?
C49 C76 H76 118.3 . . ?
C45 C76 H76 118.3 . . ?
C39 N9 C42 110.6(8) . . ?
C39 N9 H9A 124.7 . . ?
C42 N9 H9A 124.7 . . ?
C69 N10 C72 109.0(9) . . ?
C69 N10 H10A 125.5 . . ?
C72 N10 H10A 125.5 . . ?
C60 N11 C57 113.1(9) . . ?
C60 N11 H11 123.5 . . ?
C57 N11 H11 123.5 . . ?
C50 N12 C53 108.0(9) . . ?
C50 N12 H12 126.0 . . ?
C53 N12 H12 126.0 . . ?
O15 N13 O16 123.3(10) . . ?
O15 N13 C65 118.8(10) . . ?
O16 N13 C65 117.6(10) . . ?
O13 N14 O14 121.1(10) . . ?
O13 N14 C67 122.2(9) . . ?
O14 N14 C67 116.6(9) . . ?
O12 N15 O11 123.5(12) . . ?
O12 N15 C47 116.9(12) . . ?
O11 N15 C47 119.4(11) . . ?
O9 N16 O10 124.5(12) . . ?
O9 N16 C49 115.9(11) . . ?
O10 N16 C49 119.6(12) . . ?
C13A N1A C1A 107.9(9) . . ?
C13A N1A C5A 111.0(10) . . ?
C1A N1A C5A 110.4(9) . . ?
C13A N1A C9A 111.3(12) . . ?
C1A N1A C9A 108.2(9) . . ?
C5A N1A C9A 107.9(9) . . ?
C2A C1A N1A 117.6(10) . . ?
C2A C1A H1A1 107.9 . . ?
N1A C1A H1A1 107.9 . . ?
C2A C1A H1A2 107.9 . . ?
N1A C1A H1A2 107.9 . . ?
H1A1 C1A H1A2 107.2 . . ?
C1A C2A C3A 113.0(10) . . ?
C1A C2A H2A1 109.0 . . ?
C3A C2A H2A1 109.0 . . ?
C1A C2A H2A2 109.0 . . ?
C3A C2A H2A2 109.0 . . ?
H2A1 C2A H2A2 107.8 . . ?
C4A C3A C2A 113.4(13) . . ?
C4A C3A H3A1 108.9 . . ?
C2A C3A H3A1 108.9 . . ?
C4A C3A H3A2 108.9 . . ?
C2A C3A H3A2 108.9 . . ?
H3A1 C3A H3A2 107.7 . . ?
C3A C4A H4A1 109.5 . . ?
C3A C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C3A C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
C6A C5A N1A 116.0(10) . . ?
C6A C5A H5A1 108.3 . . ?
N1A C5A H5A1 108.3 . . ?
C6A C5A H5A2 108.3 . . ?
N1A C5A H5A2 108.3 . . ?
H5A1 C5A H5A2 107.4 . . ?
C5A C6A C7A 116.0(14) . . ?
C5A C6A H6A1 108.3 . . ?
C7A C6A H6A1 108.3 . . ?
C5A C6A H6A2 108.3 . . ?
C7A C6A H6A2 108.3 . . ?
H6A1 C6A H6A2 107.4 . . ?
C8A C7A C6A 107(2) . . ?
C8A C7A H7A1 110.4 . . ?
C6A C7A H7A1 110.4 . . ?
C8A C7A H7A2 110.5 . . ?
C6A C7A H7A2 110.4 . . ?
H7A1 C7A H7A2 108.6 . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.4 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.4 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C10A C9A N1A 115.0(12) . . ?
C10A C9A H9A1 108.5 . . ?
N1A C9A H9A1 108.5 . . ?
C10A C9A H9A2 108.5 . . ?
N1A C9A H9A2 108.5 . . ?
H9A1 C9A H9A2 107.5 . . ?
C9A C10A C11A 96.2(14) . . ?
C9A C10A H10B 112.5 . . ?
C11A C10A H10B 112.5 . . ?
C9A C10A H10C 112.5 . . ?
C11A C10A H10C 112.5 . . ?
H10B C10A H10C 110.0 . . ?
C12A C11A C10A 106(2) . . ?
C12A C11A H11A 110.5 . . ?
C10A C11A H11A 110.4 . . ?
C12A C11A H11B 110.5 . . ?
C10A C11A H11B 110.5 . . ?
H11A C11A H11B 108.7 . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C11A C12A H12C 109.4 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C14A C13A N1A 113.2(12) . . ?
C14A C13A H13D 108.9 . . ?
N1A C13A H13D 108.9 . . ?
C14A C13A H13E 108.9 . . ?
N1A C13A H13E 108.9 . . ?
H13D C13A H13E 107.8 . . ?
C13A C14A C15A 112.4(15) . . ?
C13A C14A H14A 109.1 . . ?
C15A C14A H14A 109.1 . . ?
C13A C14A H14B 109.1 . . ?
C15A C14A H14B 109.1 . . ?
H14A C14A H14B 107.9 . . ?
C16A C15A C14A 103.5(18) . . ?
C16A C15A H15A 111.1 . . ?
C14A C15A H15A 111.1 . . ?
C16A C15A H15B 111.0 . . ?
C14A C15A H15B 111.1 . . ?
H15A C15A H15B 109.0 . . ?
C15A C16A H16A 109.4 . . ?
C15A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C15A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C1B N2A C9B 109.5(10) . . ?
C1B N2A C5B 111.4(9) . . ?
C9B N2A C5B 113.1(10) . . ?
C1B N2A C13B 111.6(9) . . ?
C9B N2A C13B 105.4(9) . . ?
C5B N2A C13B 105.6(10) . . ?
N2A C1B C2B 117.2(11) . . ?
N2A C1B H1B1 108.0 . . ?
C2B C1B H1B1 108.0 . . ?
N2A C1B H1B2 108.0 . . ?
C2B C1B H1B2 108.0 . . ?
H1B1 C1B H1B2 107.2 . . ?
C1B C2B C3B 112.3(12) . . ?
C1B C2B H2B1 109.1 . . ?
C3B C2B H2B1 109.1 . . ?
C1B C2B H2B2 109.1 . . ?
C3B C2B H2B2 109.1 . . ?
H2B1 C2B H2B2 107.9 . . ?
C4B C3B C2B 114.9(17) . . ?
C4B C3B H3B1 108.5 . . ?
C2B C3B H3B1 108.5 . . ?
C4B C3B H3B2 108.6 . . ?
C2B C3B H3B2 108.5 . . ?
H3B1 C3B H3B2 107.5 . . ?
C3B C4B H4B1 109.4 . . ?
C3B C4B H4B2 109.5 . . ?
H4B1 C4B H4B2 109.5 . . ?
C3B C4B H4B3 109.5 . . ?
H4B1 C4B H4B3 109.5 . . ?
H4B2 C4B H4B3 109.5 . . ?
C6B C5B N2A 113.9(12) . . ?
C6B C5B H5B1 108.8 . . ?
N2A C5B H5B1 108.8 . . ?
C6B C5B H5B2 108.8 . . ?
N2A C5B H5B2 108.8 . . ?
H5B1 C5B H5B2 107.7 . . ?
C5B C6B C7B 117.2(16) . . ?
C5B C6B H6B1 108.0 . . ?
C7B C6B H6B1 108.0 . . ?
C5B C6B H6B2 108.0 . . ?
C7B C6B H6B2 108.0 . . ?
H6B1 C6B H6B2 107.2 . . ?
C8B C7B C6B 112(2) . . ?
C8B C7B H7B1 109.2 . . ?
C6B C7B H7B1 109.2 . . ?
C8B C7B H7B2 109.2 . . ?
C6B C7B H7B2 109.2 . . ?
H7B1 C7B H7B2 107.9 . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.4 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
N2A C9B C10B 119.1(11) . . ?
N2A C9B H9B1 107.5 . . ?
C10B C9B H9B1 107.5 . . ?
N2A C9B H9B2 107.5 . . ?
C10B C9B H9B2 107.5 . . ?
H9B1 C9B H9B2 107.0 . . ?
C9B C10B C11B 117.5(17) . . ?
C9B C10B H10D 107.9 . . ?
C11B C10B H10D 107.9 . . ?
C9B C10B H10E 107.9 . . ?
C11B C10B H10E 107.9 . . ?
H10D C10B H10E 107.2 . . ?
C12B C11B C10B 119(3) . . ?
C12B C11B H11C 107.7 . . ?
C10B C11B H11C 107.6 . . ?
C12B C11B H11D 107.7 . . ?
C10B C11B H11D 107.7 . . ?
H11C C11B H11D 107.1 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.4 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C14B C13B N2A 116.3(10) . . ?
C14B C13B H13F 108.2 . . ?
N2A C13B H13F 108.2 . . ?
C14B C13B H13G 108.2 . . ?
N2A C13B H13G 108.2 . . ?
H13F C13B H13G 107.4 . . ?
C13B C14B C15B 106.4(13) . . ?
C13B C14B H14C 110.4 . . ?
C15B C14B H14C 110.4 . . ?
C13B C14B H14D 110.4 . . ?
C15B C14B H14D 110.4 . . ?
H14C C14B H14D 108.6 . . ?
C16B C15B C14B 109.9(16) . . ?
C16B C15B H15C 109.7 . . ?
C14B C15B H15C 109.7 . . ?
C16B C15B H15D 109.7 . . ?
C14B C15B H15D 109.7 . . ?
H15C C15B H15D 108.2 . . ?
C15B C16B H16D 109.4 . . ?
C15B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C15B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.118
####################################################################### 
# 
# 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_TBAF-CNPC4P
_database_code_depnum_ccdc_archive 'CCDC 1482087'
_audit_update_record             
;
2016-05-26 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Cis-Dintrophenyl-calix[4]pyrrole-Tetrabutylammonium fluoride/chloride 
;
_chemical_name_common            Cis-DNP-C4P-TBAF/Cl
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H72 Cl0.63 F0.37 N9 O8'
_chemical_formula_weight         1004.57

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'
Cl Cl 0.1484 0.1585 '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'
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   P21/n

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

_cell_length_a                   12.9168(7)
_cell_length_b                   18.9009(10)
_cell_length_c                   22.5896(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.650(3)
_cell_angle_gamma                90.00
_cell_volume                     5514.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    13016
_cell_measurement_theta_min      1.8031
_cell_measurement_theta_max      27.4816

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2148
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9801
_exptl_absorpt_correction_T_max  0.9911
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku SCX-Mini with Mercury CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37500
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         27.50
_reflns_number_total             12621
_reflns_number_gt                6659
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'

_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)+(0.0500P)²+1.3000P] 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_number_reflns         12621
_refine_ls_number_parameters     668
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1487
_refine_ls_R_factor_gt           0.0757
_refine_ls_wR_factor_ref         0.2084
_refine_ls_wR_factor_gt          0.1577
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_restrained_S_all      1.278
_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 0.7001(2) 0.71424(16) 0.25636(15) 0.0511(8) Uani 1 1 d . . .
C2 C 0.7270(3) 0.67635(18) 0.30620(16) 0.0637(10) Uani 1 1 d . . .
H2 H 0.7915 0.6781 0.3258 0.076 Uiso 1 1 calc R . .
C3 C 0.6415(3) 0.63414(17) 0.32324(15) 0.0564(9) Uani 1 1 d . . .
H3 H 0.6391 0.6031 0.3557 0.068 Uiso 1 1 calc R . .
C4 C 0.5631(2) 0.64722(15) 0.28329(13) 0.0453(7) Uani 1 1 d . . .
C5 C 0.4550(2) 0.61576(15) 0.27744(12) 0.0453(7) Uani 1 1 d . . .
C6 C 0.4471(3) 0.54986(16) 0.31824(14) 0.0622(10) Uani 1 1 d . . .
H6A H 0.4547 0.5644 0.3592 0.093 Uiso 1 1 calc R . .
H6B H 0.5014 0.5166 0.3085 0.093 Uiso 1 1 calc R . .
H6C H 0.3801 0.5275 0.3124 0.093 Uiso 1 1 calc R . .
C7 C 0.4369(2) 0.58961(14) 0.21322(13) 0.0435(7) Uani 1 1 d . . .
C8 C 0.5155(3) 0.55281(16) 0.18493(14) 0.0514(8) Uani 1 1 d . . .
H8 H 0.5797 0.5457 0.2040 0.062 Uiso 1 1 calc R . .
C9 C 0.4981(3) 0.52670(17) 0.12820(15) 0.0537(8) Uani 1 1 d . . .
C10 C 0.4062(3) 0.53558(16) 0.09764(14) 0.0533(8) Uani 1 1 d . . .
H10 H 0.3960 0.5179 0.0591 0.064 Uiso 1 1 calc R . .
C11 C 0.3304(3) 0.57194(15) 0.12699(14) 0.0475(8) Uani 1 1 d . . .
C12 C 0.3437(2) 0.59905(15) 0.18365(13) 0.0458(7) Uani 1 1 d . . .
H12 H 0.2895 0.6237 0.2019 0.055 Uiso 1 1 calc R . .
C13 C 0.3718(2) 0.66822(15) 0.29458(13) 0.0446(7) Uani 1 1 d . . .
C14 C 0.2986(3) 0.66605(18) 0.33765(14) 0.0563(9) Uani 1 1 d . . .
H14 H 0.2919 0.6307 0.3666 0.068 Uiso 1 1 calc R . .
C15 C 0.2347(3) 0.72606(19) 0.33106(15) 0.0598(9) Uani 1 1 d . . .
H15 H 0.1785 0.7378 0.3552 0.072 Uiso 1 1 calc R . .
C16 C 0.2685(2) 0.76449(16) 0.28340(14) 0.0464(7) Uani 1 1 d . . .
C17 C 0.2229(2) 0.82876(16) 0.25227(15) 0.0507(8) Uani 1 1 d . . .
C18 C 0.1269(3) 0.8528(2) 0.28640(18) 0.0724(11) Uani 1 1 d . . .
H18A H 0.0777 0.8142 0.2884 0.109 Uiso 1 1 calc R . .
H18B H 0.0951 0.8927 0.2662 0.109 Uiso 1 1 calc R . .
H18C H 0.1473 0.8668 0.3262 0.109 Uiso 1 1 calc R . .
C19 C 0.1886(3) 0.80747(19) 0.18859(16) 0.0650(10) Uani 1 1 d . . .
H19A H 0.2484 0.7919 0.1665 0.098 Uiso 1 1 calc R . .
H19B H 0.1574 0.8479 0.1689 0.098 Uiso 1 1 calc R . .
H19C H 0.1385 0.7693 0.1906 0.098 Uiso 1 1 calc R . .
C20 C 0.2982(2) 0.88999(15) 0.24929(14) 0.0460(7) Uani 1 1 d . . .
C21 C 0.2928(3) 0.95576(18) 0.27396(17) 0.0685(10) Uani 1 1 d . . .
H21 H 0.2421 0.9714 0.3005 0.082 Uiso 1 1 calc R . .
C22 C 0.3762(3) 0.99634(18) 0.25286(16) 0.0649(10) Uani 1 1 d . . .
H22 H 0.3903 1.0438 0.2625 0.078 Uiso 1 1 calc R . .
C23 C 0.4330(2) 0.95458(14) 0.21601(13) 0.0445(7) Uani 1 1 d . . .
C24 C 0.5264(2) 0.96995(15) 0.17846(14) 0.0475(8) Uani 1 1 d . . .
C25 C 0.5470(3) 1.05067(16) 0.17818(16) 0.0643(10) Uani 1 1 d . . .
H25A H 0.4860 1.0752 0.1634 0.096 Uiso 1 1 calc R . .
H25B H 0.6052 1.0609 0.1528 0.096 Uiso 1 1 calc R . .
H25C H 0.5626 1.0665 0.2182 0.096 Uiso 1 1 calc R . .
C26 C 0.5013(3) 0.94841(15) 0.11400(13) 0.0461(7) Uani 1 1 d . . .
C27 C 0.5759(3) 0.91852(16) 0.07732(14) 0.0524(8) Uani 1 1 d . . .
H27 H 0.6441 0.9119 0.0912 0.063 Uiso 1 1 calc R . .
C28 C 0.5481(3) 0.89875(17) 0.02016(15) 0.0572(9) Uani 1 1 d . . .
C29 C 0.4499(3) 0.90746(17) -0.00259(15) 0.0588(9) Uani 1 1 d . . .
H29 H 0.4326 0.8929 -0.0412 0.071 Uiso 1 1 calc R . .
C30 C 0.3778(3) 0.93834(16) 0.03344(15) 0.0543(8) Uani 1 1 d . . .
C31 C 0.4016(3) 0.95872(15) 0.09098(14) 0.0510(8) Uani 1 1 d . . .
H31 H 0.3505 0.9796 0.1146 0.061 Uiso 1 1 calc R . .
C32 C 0.6234(2) 0.93188(16) 0.20092(14) 0.0500(8) Uani 1 1 d . . .
C33 C 0.7155(3) 0.95718(18) 0.22243(16) 0.0650(10) Uani 1 1 d . . .
H33 H 0.7324 1.0050 0.2286 0.078 Uiso 1 1 calc R . .
C34 C 0.7806(3) 0.8987(2) 0.23376(18) 0.0707(11) Uani 1 1 d . . .
H34 H 0.8486 0.9010 0.2489 0.085 Uiso 1 1 calc R . .
C35 C 0.7282(2) 0.83812(18) 0.21916(15) 0.0550(8) Uani 1 1 d . . .
C36 C 0.7629(2) 0.76182(18) 0.21692(17) 0.0607(9) Uani 1 1 d . . .
C37 C 0.7549(3) 0.7344(2) 0.15222(18) 0.0784(12) Uani 1 1 d . . .
H37A H 0.6833 0.7366 0.1388 0.118 Uiso 1 1 calc R . .
H37B H 0.7791 0.6859 0.1506 0.118 Uiso 1 1 calc R . .
H37C H 0.7972 0.7637 0.1269 0.118 Uiso 1 1 calc R . .
C38 C 0.8776(3) 0.7580(2) 0.2364(2) 0.0925(14) Uani 1 1 d . . .
H38A H 0.9192 0.7857 0.2095 0.139 Uiso 1 1 calc R . .
H38B H 0.9005 0.7091 0.2359 0.139 Uiso 1 1 calc R . .
H38C H 0.8851 0.7768 0.2762 0.139 Uiso 1 1 calc R . .
N1 N 0.59924(19) 0.69562(12) 0.24323(11) 0.0478(6) Uani 1 1 d . . .
H1 H 0.5633 0.7123 0.2135 0.057 Uiso 1 1 calc R . .
N2 N 0.35342(18) 0.72914(12) 0.26200(11) 0.0434(6) Uani 1 1 d . . .
H2A H 0.3903 0.7431 0.2322 0.052 Uiso 1 1 calc R . .
N3 N 0.38412(19) 0.88974(12) 0.21451(10) 0.0431(6) Uani 1 1 d . . .
H3A H 0.4052 0.8535 0.1942 0.052 Uiso 1 1 calc R . .
N4 N 0.63161(19) 0.85927(13) 0.19950(11) 0.0487(6) Uani 1 1 d . . .
H4 H 0.5827 0.8307 0.1878 0.058 Uiso 1 1 calc R . .
N5 N 0.6265(3) 0.86463(19) -0.01708(17) 0.0818(10) Uani 1 1 d . . .
N6 N 0.2715(3) 0.94867(19) 0.01097(16) 0.0768(9) Uani 1 1 d . . .
N7 N 0.5823(3) 0.48772(19) 0.09885(16) 0.0807(10) Uani 1 1 d . . .
N8 N 0.2282(3) 0.58128(16) 0.09710(14) 0.0636(8) Uani 1 1 d . . .
O1 O 0.7103(3) 0.8496(2) 0.00536(17) 0.1267(14) Uani 1 1 d . . .
O2 O 0.6028(3) 0.8504(2) -0.06728(15) 0.1228(13) Uani 1 1 d . . .
O3 O 0.2499(2) 0.92575(19) -0.03847(14) 0.1086(11) Uani 1 1 d . . .
O4 O 0.2093(3) 0.9789(2) 0.04238(16) 0.1258(14) Uani 1 1 d . . .
O5 O 0.2105(2) 0.54602(15) 0.05259(12) 0.0851(9) Uani 1 1 d . . .
O6 O 0.1667(2) 0.62289(16) 0.11835(12) 0.0844(8) Uani 1 1 d . . .
O7 O 0.5688(3) 0.46521(17) 0.04992(13) 0.0999(10) Uani 1 1 d . . .
O8 O 0.6632(3) 0.4809(3) 0.12491(18) 0.170(2) Uani 1 1 d . . .
N9 N 0.0222(3) 0.69910(16) 0.94738(13) 0.0721(9) Uani 1 1 d . . .
C39 C -0.0029(3) 0.77821(19) 0.94906(17) 0.0730(11) Uani 1 1 d . . .
H39A H 0.0503 0.8035 0.9268 0.088 Uiso 1 1 calc R . .
H39B H -0.0691 0.7857 0.9284 0.088 Uiso 1 1 calc R . .
C40 C -0.0097(4) 0.8111(2) 1.00982(18) 0.0817(12) Uani 1 1 d . . .
H40A H -0.0634 0.7868 1.0324 0.098 Uiso 1 1 calc R . .
H40B H 0.0564 0.8048 1.0308 0.098 Uiso 1 1 calc R . .
C41 C -0.0350(3) 0.8890(2) 1.0064(2) 0.0819(12) Uani 1 1 d . . .
H41A H 0.0211 0.9137 0.9862 0.098 Uiso 1 1 calc R . .
H41B H -0.0985 0.8954 0.9828 0.098 Uiso 1 1 calc R . .
C42 C -0.0498(4) 0.9214(2) 1.0665(2) 0.1060(16) Uani 1 1 d . . .
H42A H -0.1084 0.8994 1.0856 0.159 Uiso 1 1 calc R . .
H42B H -0.0625 0.9718 1.0622 0.159 Uiso 1 1 calc R . .
H42C H 0.0121 0.9141 1.0905 0.159 Uiso 1 1 calc R . .
C43 C 0.1278(4) 0.6862(2) 0.97518(18) 0.0872(13) Uani 1 1 d . . .
H43A H 0.1407 0.6351 0.9755 0.105 Uiso 1 1 calc R . .
H43B H 0.1260 0.7020 1.0165 0.105 Uiso 1 1 calc R . .
C44 C 0.2187(4) 0.7223(3) 0.9451(2) 0.0968(15) Uani 1 1 d . . .
H44A H 0.2225 0.7070 0.9037 0.116 Uiso 1 1 calc R . .
H44B H 0.2092 0.7737 0.9458 0.116 Uiso 1 1 calc R . .
C45 C 0.3167(5) 0.7029(3) 0.9773(3) 0.129(2) Uani 1 1 d . . .
H45A H 0.3192 0.7267 1.0158 0.155 Uiso 1 1 calc R . .
H45B H 0.3188 0.6517 0.9840 0.155 Uiso 1 1 calc R . .
C46 C 0.4030(6) 0.7239(4) 0.9429(5) 0.215(5) Uani 1 1 d . . .
H46A H 0.4083 0.6933 0.9086 0.323 Uiso 1 1 calc R . .
H46B H 0.4657 0.7202 0.9667 0.323 Uiso 1 1 calc R . .
H46C H 0.3938 0.7724 0.9300 0.323 Uiso 1 1 calc R . .
C47 C 0.0197(4) 0.6761(2) 0.88282(17) 0.0865(13) Uani 1 1 d . . .
H47A H 0.0577 0.7114 0.8599 0.104 Uiso 1 1 calc R . .
H47B H -0.0525 0.6773 0.8690 0.104 Uiso 1 1 calc R . .
C48 C 0.0653(6) 0.6008(3) 0.8677(2) 0.154(3) Uani 1 1 d . . .
H48A H 0.0582 0.5963 0.8246 0.185 Uiso 1 1 calc R . .
H48B H 0.1398 0.6045 0.8759 0.185 Uiso 1 1 calc R . .
C49 C 0.0371(6) 0.5371(3) 0.8896(3) 0.150(3) Uani 1 1 d . . .
H49A H -0.0385 0.5338 0.8861 0.180 Uiso 1 1 calc R . .
H49B H 0.0541 0.5371 0.9319 0.180 Uiso 1 1 calc R . .
C50 C 0.0805(4) 0.4719(3) 0.8641(2) 0.1100(17) Uani 1 1 d . . .
H50A H 0.0730 0.4732 0.8213 0.165 Uiso 1 1 calc R . .
H50B H 0.0437 0.4312 0.8795 0.165 Uiso 1 1 calc R . .
H50C H 0.1532 0.4683 0.8747 0.165 Uiso 1 1 calc R . .
C51 C -0.0546(4) 0.6590(2) 0.98384(18) 0.0849(13) Uani 1 1 d . . .
H51A H -0.0454 0.6730 1.0253 0.102 Uiso 1 1 calc R . .
H51B H -0.0385 0.6084 0.9811 0.102 Uiso 1 1 calc R . .
C52 C -0.1683(4) 0.6694(3) 0.9666(2) 0.0977(15) Uani 1 1 d . . .
H52A H -0.1856 0.7198 0.9689 0.117 Uiso 1 1 calc R . .
H52B H -0.1794 0.6539 0.9257 0.117 Uiso 1 1 calc R . .
C53 C -0.2377(5) 0.6285(3) 1.0065(2) 0.1059(16) Uani 1 1 d . . .
H53A H -0.2213 0.6406 1.0477 0.127 Uiso 1 1 calc R . .
H53B H -0.2244 0.5778 1.0013 0.127 Uiso 1 1 calc R . .
C54 C -0.3498(5) 0.6429(3) 0.9945(3) 0.130(2) Uani 1 1 d . . .
H54A H -0.3633 0.6930 0.9994 0.195 Uiso 1 1 calc R . .
H54B H -0.3916 0.6162 1.0220 0.195 Uiso 1 1 calc R . .
H54C H -0.3672 0.6289 0.9543 0.195 Uiso 1 1 calc R . .
Cl1 Cl 0.46102(10) 0.75802(6) 0.13220(6) 0.0463(3) Uani 0.63 1 d P A 1
F1 F 0.4712(4) 0.7701(2) 0.1691(2) 0.0441(11) Uani 0.37 1 d P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.376(5) . ?
C1 N1 1.379(4) . ?
C1 C36 1.509(5) . ?
C2 C3 1.419(5) . ?
C2 H2 0.9400 . ?
C3 C4 1.371(4) . ?
C3 H3 0.9400 . ?
C4 N1 1.372(4) . ?
C4 C5 1.522(4) . ?
C5 C13 1.516(4) . ?
C5 C7 1.548(4) . ?
C5 C6 1.553(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 C12 1.382(4) . ?
C7 C8 1.392(4) . ?
C8 C9 1.389(4) . ?
C8 H8 0.9400 . ?
C9 C10 1.377(4) . ?
C9 N7 1.477(4) . ?
C10 C11 1.373(4) . ?
C10 H10 0.9400 . ?
C11 C12 1.387(4) . ?
C11 N8 1.487(4) . ?
C12 H12 0.9400 . ?
C13 C14 1.365(4) . ?
C13 N2 1.386(4) . ?
C14 C15 1.409(5) . ?
C14 H14 0.9400 . ?
C15 C16 1.374(4) . ?
C15 H15 0.9400 . ?
C16 N2 1.377(4) . ?
C16 C17 1.519(4) . ?
C17 C20 1.513(4) . ?
C17 C18 1.537(4) . ?
C17 C19 1.554(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 C21 1.365(4) . ?
C20 N3 1.367(4) . ?
C21 C22 1.410(5) . ?
C21 H21 0.9400 . ?
C22 C23 1.367(4) . ?
C22 H22 0.9400 . ?
C23 N3 1.379(3) . ?
C23 C24 1.511(4) . ?
C24 C32 1.527(4) . ?
C24 C26 1.543(4) . ?
C24 C25 1.549(4) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C31 1.397(4) . ?
C26 C27 1.397(4) . ?
C27 C28 1.388(4) . ?
C27 H27 0.9400 . ?
C28 C29 1.374(5) . ?
C28 N5 1.472(5) . ?
C29 C30 1.374(5) . ?
C29 H29 0.9400 . ?
C30 C31 1.387(4) . ?
C30 N6 1.472(5) . ?
C31 H31 0.9400 . ?
C32 C33 1.366(4) . ?
C32 N4 1.377(4) . ?
C33 C34 1.410(5) . ?
C33 H33 0.9400 . ?
C34 C35 1.368(4) . ?
C34 H34 0.9400 . ?
C35 N4 1.379(4) . ?
C35 C36 1.511(5) . ?
C36 C38 1.542(5) . ?
C36 C37 1.553(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
N1 H1 0.8700 . ?
N2 H2A 0.8700 . ?
N3 H3A 0.8700 . ?
N4 H4 0.8700 . ?
N5 O2 1.201(4) . ?
N5 O1 1.224(4) . ?
N6 O4 1.220(4) . ?
N6 O3 1.227(4) . ?
N7 O7 1.195(4) . ?
N7 O8 1.200(4) . ?
N8 O6 1.220(4) . ?
N8 O5 1.226(4) . ?
N9 C51 1.502(5) . ?
N9 C43 1.516(5) . ?
N9 C47 1.522(5) . ?
N9 C39 1.530(5) . ?
C39 C40 1.510(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C40 C41 1.510(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C41 C42 1.504(6) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 H42C 0.9700 . ?
C43 C44 1.524(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C44 C45 1.497(6) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C45 C46 1.422(9) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 H46C 0.9700 . ?
C47 C48 1.579(7) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C48 C49 1.354(7) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C49 C50 1.473(7) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C50 H50C 0.9700 . ?
C51 C52 1.527(6) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C52 C53 1.493(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C53 C54 1.495(7) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 H54C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 105.8(3) . . ?
C2 C1 C36 131.4(3) . . ?
N1 C1 C36 122.6(3) . . ?
C1 C2 C3 108.9(3) . . ?
C1 C2 H2 125.5 . . ?
C3 C2 H2 125.5 . . ?
C4 C3 C2 107.0(3) . . ?
C4 C3 H3 126.5 . . ?
C2 C3 H3 126.5 . . ?
C3 C4 N1 107.4(3) . . ?
C3 C4 C5 131.0(3) . . ?
N1 C4 C5 121.5(3) . . ?
C13 C5 C4 112.0(2) . . ?
C13 C5 C7 110.4(2) . . ?
C4 C5 C7 109.5(2) . . ?
C13 C5 C6 108.8(3) . . ?
C4 C5 C6 109.2(3) . . ?
C7 C5 C6 106.9(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 118.6(3) . . ?
C12 C7 C5 122.2(3) . . ?
C8 C7 C5 119.1(3) . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C10 C9 C8 123.3(3) . . ?
C10 C9 N7 118.1(3) . . ?
C8 C9 N7 118.6(3) . . ?
C11 C10 C9 115.7(3) . . ?
C11 C10 H10 122.1 . . ?
C9 C10 H10 122.1 . . ?
C10 C11 C12 123.3(3) . . ?
C10 C11 N8 118.3(3) . . ?
C12 C11 N8 118.3(3) . . ?
C7 C12 C11 119.7(3) . . ?
C7 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 N2 106.7(3) . . ?
C14 C13 C5 131.4(3) . . ?
N2 C13 C5 121.7(3) . . ?
C13 C14 C15 108.1(3) . . ?
C13 C14 H14 126.0 . . ?
C15 C14 H14 126.0 . . ?
C16 C15 C14 108.5(3) . . ?
C16 C15 H15 125.7 . . ?
C14 C15 H15 125.7 . . ?
C15 C16 N2 106.3(3) . . ?
C15 C16 C17 131.4(3) . . ?
N2 C16 C17 122.1(3) . . ?
C20 C17 C16 112.7(3) . . ?
C20 C17 C18 108.6(3) . . ?
C16 C17 C18 108.4(3) . . ?
C20 C17 C19 109.5(3) . . ?
C16 C17 C19 109.1(3) . . ?
C18 C17 C19 108.5(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N3 106.5(3) . . ?
C21 C20 C17 130.0(3) . . ?
N3 C20 C17 123.3(3) . . ?
C20 C21 C22 108.3(3) . . ?
C20 C21 H21 125.8 . . ?
C22 C21 H21 125.8 . . ?
C23 C22 C21 108.0(3) . . ?
C23 C22 H22 126.0 . . ?
C21 C22 H22 126.0 . . ?
C22 C23 N3 106.2(3) . . ?
C22 C23 C24 131.9(3) . . ?
N3 C23 C24 121.7(2) . . ?
C23 C24 C32 112.4(2) . . ?
C23 C24 C26 108.6(2) . . ?
C32 C24 C26 110.6(3) . . ?
C23 C24 C25 109.3(3) . . ?
C32 C24 C25 109.0(3) . . ?
C26 C24 C25 106.9(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C31 C26 C27 118.3(3) . . ?
C31 C26 C24 119.8(3) . . ?
C27 C26 C24 121.8(3) . . ?
C28 C27 C26 119.2(3) . . ?
C28 C27 H27 120.4 . . ?
C26 C27 H27 120.4 . . ?
C29 C28 C27 122.9(3) . . ?
C29 C28 N5 118.5(3) . . ?
C27 C28 N5 118.5(4) . . ?
C30 C29 C28 117.3(3) . . ?
C30 C29 H29 121.3 . . ?
C28 C29 H29 121.3 . . ?
C29 C30 C31 121.9(3) . . ?
C29 C30 N6 119.2(3) . . ?
C31 C30 N6 118.9(3) . . ?
C30 C31 C26 120.3(3) . . ?
C30 C31 H31 119.9 . . ?
C26 C31 H31 119.9 . . ?
C33 C32 N4 106.8(3) . . ?
C33 C32 C24 131.4(3) . . ?
N4 C32 C24 121.7(3) . . ?
C32 C33 C34 107.8(3) . . ?
C32 C33 H33 126.1 . . ?
C34 C33 H33 126.1 . . ?
C35 C34 C33 108.7(3) . . ?
C35 C34 H34 125.7 . . ?
C33 C34 H34 125.7 . . ?
C34 C35 N4 106.1(3) . . ?
C34 C35 C36 131.4(3) . . ?
N4 C35 C36 122.2(3) . . ?
C1 C36 C35 112.8(3) . . ?
C1 C36 C38 108.9(3) . . ?
C35 C36 C38 108.6(3) . . ?
C1 C36 C37 109.0(3) . . ?
C35 C36 C37 109.5(3) . . ?
C38 C36 C37 107.9(3) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C4 N1 C1 110.9(3) . . ?
C4 N1 H1 124.6 . . ?
C1 N1 H1 124.6 . . ?
C16 N2 C13 110.4(2) . . ?
C16 N2 H2A 124.8 . . ?
C13 N2 H2A 124.8 . . ?
C20 N3 C23 110.9(2) . . ?
C20 N3 H3A 124.5 . . ?
C23 N3 H3A 124.5 . . ?
C32 N4 C35 110.6(3) . . ?
C32 N4 H4 124.7 . . ?
C35 N4 H4 124.7 . . ?
O2 N5 O1 123.6(4) . . ?
O2 N5 C28 117.9(4) . . ?
O1 N5 C28 118.4(4) . . ?
O4 N6 O3 123.4(4) . . ?
O4 N6 C30 118.7(3) . . ?
O3 N6 C30 118.0(4) . . ?
O7 N7 O8 122.2(4) . . ?
O7 N7 C9 119.5(4) . . ?
O8 N7 C9 118.3(3) . . ?
O6 N8 O5 123.9(3) . . ?
O6 N8 C11 118.5(3) . . ?
O5 N8 C11 117.7(3) . . ?
C51 N9 C43 106.8(3) . . ?
C51 N9 C47 112.0(3) . . ?
C43 N9 C47 111.1(3) . . ?
C51 N9 C39 109.8(3) . . ?
C43 N9 C39 109.7(3) . . ?
C47 N9 C39 107.5(3) . . ?
C40 C39 N9 116.0(3) . . ?
C40 C39 H39A 108.3 . . ?
N9 C39 H39A 108.3 . . ?
C40 C39 H39B 108.3 . . ?
N9 C39 H39B 108.3 . . ?
H39A C39 H39B 107.4 . . ?
C41 C40 C39 111.7(3) . . ?
C41 C40 H40A 109.3 . . ?
C39 C40 H40A 109.3 . . ?
C41 C40 H40B 109.3 . . ?
C39 C40 H40B 109.3 . . ?
H40A C40 H40B 107.9 . . ?
C42 C41 C40 112.4(4) . . ?
C42 C41 H41A 109.1 . . ?
C40 C41 H41A 109.1 . . ?
C42 C41 H41B 109.1 . . ?
C40 C41 H41B 109.1 . . ?
H41A C41 H41B 107.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C43 C44 116.0(3) . . ?
N9 C43 H43A 108.3 . . ?
C44 C43 H43A 108.3 . . ?
N9 C43 H43B 108.3 . . ?
C44 C43 H43B 108.3 . . ?
H43A C43 H43B 107.4 . . ?
C45 C44 C43 109.0(4) . . ?
C45 C44 H44A 109.9 . . ?
C43 C44 H44A 109.9 . . ?
C45 C44 H44B 109.9 . . ?
C43 C44 H44B 109.9 . . ?
H44A C44 H44B 108.3 . . ?
C46 C45 C44 109.3(6) . . ?
C46 C45 H45A 109.8 . . ?
C44 C45 H45A 109.8 . . ?
C46 C45 H45B 109.8 . . ?
C44 C45 H45B 109.8 . . ?
H45A C45 H45B 108.3 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N9 C47 C48 117.5(3) . . ?
N9 C47 H47A 107.9 . . ?
C48 C47 H47A 107.9 . . ?
N9 C47 H47B 107.9 . . ?
C48 C47 H47B 107.9 . . ?
H47A C47 H47B 107.2 . . ?
C49 C48 C47 128.3(6) . . ?
C49 C48 H48A 105.2 . . ?
C47 C48 H48A 105.2 . . ?
C49 C48 H48B 105.2 . . ?
C47 C48 H48B 105.2 . . ?
H48A C48 H48B 105.9 . . ?
C48 C49 C50 119.8(6) . . ?
C48 C49 H49A 107.4 . . ?
C50 C49 H49A 107.4 . . ?
C48 C49 H49B 107.4 . . ?
C50 C49 H49B 107.4 . . ?
H49A C49 H49B 106.9 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N9 C51 C52 115.7(3) . . ?
N9 C51 H51A 108.3 . . ?
C52 C51 H51A 108.3 . . ?
N9 C51 H51B 108.3 . . ?
C52 C51 H51B 108.3 . . ?
H51A C51 H51B 107.4 . . ?
C53 C52 C51 111.2(4) . . ?
C53 C52 H52A 109.4 . . ?
C51 C52 H52A 109.4 . . ?
C53 C52 H52B 109.4 . . ?
C51 C52 H52B 109.4 . . ?
H52A C52 H52B 108.0 . . ?
C52 C53 C54 112.5(5) . . ?
C52 C53 H53A 109.1 . . ?
C54 C53 H53A 109.1 . . ?
C52 C53 H53B 109.1 . . ?
C54 C53 H53B 109.1 . . ?
H53A C53 H53B 107.8 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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_TBAHPO4-DNPC4P
_database_code_depnum_ccdc_archive 'CCDC 1482088'
_audit_update_record             
;
2016-05-26 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Cis-dinitrophenyl-calix[4]pyrrole-tetrabutylammonium 
dihydrogenphosphate 
;
_chemical_name_common            Cis-DNP-Calix[4]pyrrole-TBAH2PO4
_chemical_melting_point          ?
_chemical_formula_moiety         
;
2(C38H36N8O8),C16H34N,3(C16H36 N),4(H2O4P),2(CHCl)
;
_chemical_formula_sum            'C72 H116 Cl3 N10 O18 P2'
_chemical_formula_weight         1578.04

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'
P P 0.1023 0.0942 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   18.5581(12)
_cell_length_b                   19.3272(12)
_cell_length_c                   23.1017(15)
_cell_angle_alpha                86.218(2)
_cell_angle_beta                 87.845(2)
_cell_angle_gamma                81.721(2)
_cell_volume                     8178.5(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    51459
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.535

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3372
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9549
_exptl_absorpt_correction_T_max  0.9890
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            68468
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.00
_reflns_number_total             27777
_reflns_number_gt                21124
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_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)+(0.1045P)²+13.4490P] 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_number_reflns         27777
_refine_ls_number_parameters     1923
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.2032
_refine_ls_wR_factor_gt          0.1846
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.005
_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
C23 C 0.01547(17) 0.88863(17) 0.09300(13) 0.0191(7) Uani 1 1 d . . .
C1 C 0.20463(17) 0.76001(16) 0.27285(14) 0.0196(7) Uani 1 1 d . . .
C2 C 0.24667(18) 0.78460(17) 0.31226(15) 0.0237(7) Uani 1 1 d . . .
H2 H 0.2984 0.7799 0.3114 0.028 Uiso 1 1 calc R . .
C3 C 0.19896(18) 0.81833(17) 0.35446(15) 0.0230(7) Uani 1 1 d . . .
H3 H 0.2131 0.8402 0.3870 0.028 Uiso 1 1 calc R . .
C4 C 0.12888(17) 0.81394(16) 0.34010(13) 0.0182(6) Uani 1 1 d . . .
C5 C 0.05781(18) 0.83798(17) 0.37228(14) 0.0215(7) Uani 1 1 d . . .
C6 C 0.0752(2) 0.8658(2) 0.42992(14) 0.0298(8) Uani 1 1 d . . .
H6A H 0.1050 0.8287 0.4529 0.045 Uiso 1 1 calc R . .
H6B H 0.0297 0.8808 0.4514 0.045 Uiso 1 1 calc R . .
H6C H 0.1020 0.9058 0.4223 0.045 Uiso 1 1 calc R . .
C7 C 0.01577(19) 0.77508(18) 0.38592(15) 0.0271(8) Uani 1 1 d . . .
H7A H 0.0040 0.7564 0.3495 0.041 Uiso 1 1 calc R . .
H7B H -0.0294 0.7905 0.4077 0.041 Uiso 1 1 calc R . .
H7C H 0.0460 0.7385 0.4091 0.041 Uiso 1 1 calc R . .
C8 C 0.00967(17) 0.89575(17) 0.33845(14) 0.0202(7) Uani 1 1 d . . .
C9 C -0.01461(19) 0.96350(18) 0.35126(15) 0.0258(7) Uani 1 1 d . . .
H9 H -0.0012 0.9860 0.3837 0.031 Uiso 1 1 calc R . .
C10 C -0.06319(18) 0.99433(17) 0.30778(15) 0.0236(7) Uani 1 1 d . . .
H10 H -0.0884 1.0408 0.3060 0.028 Uiso 1 1 calc R . .
C11 C -0.06704(17) 0.94470(17) 0.26874(14) 0.0209(7) Uani 1 1 d . . .
C12 C -0.10984(17) 0.94863(17) 0.21393(14) 0.0219(7) Uani 1 1 d . . .
C13 C -0.15956(18) 1.01980(17) 0.20892(16) 0.0272(8) Uani 1 1 d . . .
H13A H -0.1938 1.0234 0.2423 0.041 Uiso 1 1 calc R . .
H13B H -0.1867 1.0234 0.1730 0.041 Uiso 1 1 calc R . .
H13C H -0.1297 1.0578 0.2083 0.041 Uiso 1 1 calc R . .
C14 C -0.16154(17) 0.89264(16) 0.21663(15) 0.0217(7) Uani 1 1 d . . .
C15 C -0.18732(17) 0.87219(17) 0.16573(15) 0.0241(7) Uani 1 1 d . . .
H15 H -0.1692 0.8887 0.1292 0.029 Uiso 1 1 calc R . .
C16 C -0.23965(19) 0.82759(18) 0.16843(16) 0.0273(8) Uani 1 1 d . . .
C17 C -0.26828(18) 0.80122(18) 0.21996(16) 0.0275(8) Uani 1 1 d . . .
H17 H -0.3044 0.7709 0.2210 0.033 Uiso 1 1 calc R . .
C18 C -0.24092(18) 0.82191(18) 0.26997(15) 0.0264(8) Uani 1 1 d . . .
C19 C -0.18855(18) 0.86626(17) 0.26921(15) 0.0251(7) Uani 1 1 d . . .
H19 H -0.1710 0.8787 0.3047 0.030 Uiso 1 1 calc R . .
C20 C -0.06016(17) 0.94261(16) 0.16033(14) 0.0199(7) Uani 1 1 d . . .
C21 C -0.04322(18) 0.99301(17) 0.11966(15) 0.0240(7) Uani 1 1 d . . .
H21 H -0.0603 1.0418 0.1197 0.029 Uiso 1 1 calc R . .
C22 C 0.00460(18) 0.95921(17) 0.07727(14) 0.0236(7) Uani 1 1 d . . .
H22 H 0.0253 0.9814 0.0440 0.028 Uiso 1 1 calc R . .
C24 C 0.06019(18) 0.82800(17) 0.06366(13) 0.0203(7) Uani 1 1 d . . .
C25 C 0.01548(19) 0.76701(18) 0.06278(14) 0.0242(7) Uani 1 1 d . . .
H25A H 0.0437 0.7286 0.0425 0.036 Uiso 1 1 calc R . .
H25B H -0.0300 0.7830 0.0426 0.036 Uiso 1 1 calc R . .
H25C H 0.0043 0.7505 0.1027 0.036 Uiso 1 1 calc R . .
C26 C 0.0780(2) 0.85308(19) 0.00090(14) 0.0272(8) Uani 1 1 d . . .
H26A H 0.1048 0.8932 0.0012 0.041 Uiso 1 1 calc R . .
H26B H 0.0327 0.8671 -0.0199 0.041 Uiso 1 1 calc R . .
H26C H 0.1080 0.8150 -0.0186 0.041 Uiso 1 1 calc R . .
C27 C 0.13069(17) 0.80352(16) 0.09410(13) 0.0189(7) Uani 1 1 d . . .
C28 C 0.20124(18) 0.80894(19) 0.07649(15) 0.0271(8) Uani 1 1 d . . .
H28 H 0.2164 0.8304 0.0408 0.033 Uiso 1 1 calc R . .
C29 C 0.24753(19) 0.77683(19) 0.12097(15) 0.0285(8) Uani 1 1 d . . .
H29 H 0.2992 0.7731 0.1203 0.034 Uiso 1 1 calc R . .
C30 C 0.20507(17) 0.75227(16) 0.16491(14) 0.0201(7) Uani 1 1 d . . .
C31 C 0.22692(16) 0.71459(17) 0.22258(14) 0.0197(7) Uani 1 1 d . . .
C32 C 0.31077(17) 0.69518(18) 0.22135(16) 0.0248(7) Uani 1 1 d . . .
H32A H 0.3335 0.7380 0.2161 0.037 Uiso 1 1 calc R . .
H32B H 0.3259 0.6653 0.1891 0.037 Uiso 1 1 calc R . .
H32C H 0.3261 0.6699 0.2580 0.037 Uiso 1 1 calc R . .
C33 C 0.19552(16) 0.64496(16) 0.23313(14) 0.0192(7) Uani 1 1 d . . .
C34 C 0.17995(17) 0.60625(17) 0.18748(15) 0.0222(7) Uani 1 1 d . . .
H34 H 0.1856 0.6235 0.1484 0.027 Uiso 1 1 calc R . .
C35 C 0.15604(17) 0.54199(17) 0.20027(15) 0.0240(7) Uani 1 1 d . . .
C36 C 0.14699(17) 0.51384(18) 0.25616(16) 0.0260(8) Uani 1 1 d . . .
H36 H 0.1300 0.4700 0.2639 0.031 Uiso 1 1 calc R . .
C37 C 0.16405(17) 0.55302(17) 0.29989(15) 0.0236(7) Uani 1 1 d . . .
C38 C 0.18767(17) 0.61769(17) 0.28972(15) 0.0215(7) Uani 1 1 d . . .
H38 H 0.1984 0.6432 0.3213 0.026 Uiso 1 1 calc R . .
C39 C 0.27783(16) 0.24764(16) 0.23397(14) 0.0190(7) Uani 1 1 d . . .
C40 C 0.23104(18) 0.21601(17) 0.20322(15) 0.0244(7) Uani 1 1 d . . .
H40 H 0.1802 0.2173 0.2110 0.029 Uiso 1 1 calc R . .
C41 C 0.27148(18) 0.18116(18) 0.15793(15) 0.0245(7) Uani 1 1 d . . .
H41 H 0.2529 0.1545 0.1303 0.029 Uiso 1 1 calc R . .
C42 C 0.34267(17) 0.19281(17) 0.16112(14) 0.0206(7) Uani 1 1 d . . .
C43 C 0.40735(19) 0.17412(18) 0.12002(15) 0.0256(7) Uani 1 1 d . . .
C44 C 0.4467(2) 0.23885(19) 0.10727(15) 0.0305(8) Uani 1 1 d . . .
H44A H 0.4641 0.2531 0.1436 0.046 Uiso 1 1 calc R . .
H44B H 0.4127 0.2774 0.0897 0.046 Uiso 1 1 calc R . .
H44C H 0.4881 0.2272 0.0804 0.046 Uiso 1 1 calc R . .
C45 C 0.3795(2) 0.1533(2) 0.06269(16) 0.0354(9) Uani 1 1 d . . .
H45A H 0.4207 0.1435 0.0352 0.053 Uiso 1 1 calc R . .
H45B H 0.3445 0.1918 0.0464 0.053 Uiso 1 1 calc R . .
H45C H 0.3557 0.1114 0.0700 0.053 Uiso 1 1 calc R . .
C46 C 0.46019(18) 0.11395(19) 0.14533(15) 0.0271(8) Uani 1 1 d . . .
C47 C 0.4831(2) 0.0480(2) 0.12599(17) 0.0337(9) Uani 1 1 d . . .
H47 H 0.4678 0.0297 0.0921 0.040 Uiso 1 1 calc R . .
C48 C 0.53374(19) 0.01285(19) 0.16608(17) 0.0326(8) Uani 1 1 d . . .
H48 H 0.5586 -0.0334 0.1636 0.039 Uiso 1 1 calc R . .
C49 C 0.54100(18) 0.05660(18) 0.20906(16) 0.0267(8) Uani 1 1 d . . .
C50 C 0.58933(18) 0.04732(17) 0.26097(16) 0.0274(8) Uani 1 1 d . . .
C51 C 0.63650(19) -0.02531(19) 0.26006(19) 0.0345(9) Uani 1 1 d . . .
H51A H 0.6049 -0.0619 0.2631 0.052 Uiso 1 1 calc R . .
H51B H 0.6693 -0.0316 0.2928 0.052 Uiso 1 1 calc R . .
H51C H 0.6652 -0.0285 0.2236 0.052 Uiso 1 1 calc R . .
C52 C 0.64301(17) 0.10185(17) 0.25604(16) 0.0251(8) Uani 1 1 d . . .
C53 C 0.67052(17) 0.12313(17) 0.20190(16) 0.0266(8) Uani 1 1 d . . .
H53 H 0.6526 0.1083 0.1675 0.032 Uiso 1 1 calc R . .
C54 C 0.72439(18) 0.16615(18) 0.19878(16) 0.0276(8) Uani 1 1 d . . .
C55 C 0.75169(18) 0.19078(18) 0.24695(17) 0.0293(8) Uani 1 1 d . . .
H55 H 0.7886 0.2203 0.2439 0.035 Uiso 1 1 calc R . .
C56 C 0.72234(18) 0.17005(18) 0.29966(16) 0.0280(8) Uani 1 1 d . . .
C57 C 0.66864(18) 0.12633(18) 0.30525(17) 0.0293(8) Uani 1 1 d . . .
H57 H 0.6497 0.1134 0.3426 0.035 Uiso 1 1 calc R . .
C58 C 0.54686(17) 0.05133(17) 0.31825(16) 0.0262(8) Uani 1 1 d . . .
C59 C 0.54207(18) 0.00107(19) 0.36294(17) 0.0306(8) Uani 1 1 d . . .
H59 H 0.5623 -0.0469 0.3627 0.037 Uiso 1 1 calc R . .
C60 C 0.50166(19) 0.03393(18) 0.40907(16) 0.0299(8) Uani 1 1 d . . .
H60 H 0.4902 0.0118 0.4455 0.036 Uiso 1 1 calc R . .
C61 C 0.48167(17) 0.10352(18) 0.39219(15) 0.0251(7) Uani 1 1 d . . .
C62 C 0.44471(18) 0.16368(18) 0.42668(14) 0.0246(7) Uani 1 1 d . . .
C63 C 0.4326(2) 0.1358(2) 0.48979(15) 0.0323(8) Uani 1 1 d . . .
H63A H 0.4098 0.1743 0.5128 0.048 Uiso 1 1 calc R . .
H63B H 0.4796 0.1160 0.5062 0.048 Uiso 1 1 calc R . .
H63C H 0.4008 0.0994 0.4905 0.048 Uiso 1 1 calc R . .
C64 C 0.4957(2) 0.2202(2) 0.42690(16) 0.0309(8) Uani 1 1 d . . .
H64A H 0.5033 0.2392 0.3871 0.046 Uiso 1 1 calc R . .
H64B H 0.5426 0.1993 0.4429 0.046 Uiso 1 1 calc R . .
H64C H 0.4734 0.2580 0.4509 0.046 Uiso 1 1 calc R . .
C65 C 0.37142(18) 0.19692(17) 0.40349(14) 0.0215(7) Uani 1 1 d . . .
C66 C 0.30433(19) 0.20780(17) 0.43160(14) 0.0243(7) Uani 1 1 d . . .
H66 H 0.2935 0.1926 0.4705 0.029 Uiso 1 1 calc R . .
C67 C 0.25433(18) 0.24573(17) 0.39222(15) 0.0235(7) Uani 1 1 d . . .
H67 H 0.2041 0.2608 0.4002 0.028 Uiso 1 1 calc R . .
C68 C 0.29098(17) 0.25695(16) 0.34056(14) 0.0197(7) Uani 1 1 d . . .
C69 C 0.26318(16) 0.29438(17) 0.28422(14) 0.0200(7) Uani 1 1 d . . .
C70 C 0.17974(17) 0.31586(17) 0.29078(15) 0.0239(7) Uani 1 1 d . . .
H70A H 0.1610 0.3392 0.2543 0.036 Uiso 1 1 calc R . .
H70B H 0.1691 0.3480 0.3221 0.036 Uiso 1 1 calc R . .
H70C H 0.1564 0.2740 0.3001 0.036 Uiso 1 1 calc R . .
C71 C 0.29573(16) 0.36313(16) 0.27162(14) 0.0192(7) Uani 1 1 d . . .
C72 C 0.31240(17) 0.40071(17) 0.31753(14) 0.0220(7) Uani 1 1 d . . .
H72 H 0.3071 0.3827 0.3565 0.026 Uiso 1 1 calc R . .
C73 C 0.33688(17) 0.46473(17) 0.30568(15) 0.0227(7) Uani 1 1 d . . .
C74 C 0.34719(17) 0.49338(17) 0.25021(15) 0.0235(7) Uani 1 1 d . . .
H74 H 0.3650 0.5369 0.2430 0.028 Uiso 1 1 calc R . .
C75 C 0.33005(17) 0.45491(17) 0.20596(15) 0.0227(7) Uani 1 1 d . . .
C76 C 0.30394(17) 0.39151(17) 0.21512(15) 0.0213(7) Uani 1 1 d . . .
H76 H 0.2917 0.3674 0.1831 0.026 Uiso 1 1 calc R . .
C77 C 1.01850(18) 0.32795(17) 0.09960(14) 0.0234(7) Uani 1 1 d . . .
H77A H 1.0256 0.3516 0.0609 0.028 Uiso 1 1 calc R . .
H77B H 1.0535 0.3429 0.1259 0.028 Uiso 1 1 calc R . .
C78 C 1.03697(18) 0.24975(18) 0.09441(15) 0.0255(7) Uani 1 1 d . . .
H78A H 0.9999 0.2331 0.0711 0.031 Uiso 1 1 calc R . .
H78B H 1.0363 0.2255 0.1335 0.031 Uiso 1 1 calc R . .
C79 C 1.11207(19) 0.23199(19) 0.06555(15) 0.0281(8) Uani 1 1 d . . .
H79A H 1.1124 0.2562 0.0264 0.034 Uiso 1 1 calc R . .
H79B H 1.1488 0.2494 0.0887 0.034 Uiso 1 1 calc R . .
C80 C 1.1328(2) 0.1542(2) 0.06010(18) 0.0358(9) Uani 1 1 d . . .
H80A H 1.1321 0.1299 0.0987 0.054 Uiso 1 1 calc R . .
H80B H 1.1818 0.1450 0.0425 0.054 Uiso 1 1 calc R . .
H80C H 1.0980 0.1371 0.0356 0.054 Uiso 1 1 calc R . .
C81 C 0.93592(19) 0.42960(17) 0.13577(14) 0.0230(7) Uani 1 1 d . . .
H81A H 0.8869 0.4443 0.1529 0.028 Uiso 1 1 calc R . .
H81B H 0.9718 0.4336 0.1656 0.028 Uiso 1 1 calc R . .
C82 C 0.9484(2) 0.48015(17) 0.08463(14) 0.0258(7) Uani 1 1 d . . .
H82A H 0.9160 0.4742 0.0528 0.031 Uiso 1 1 calc R . .
H82B H 0.9995 0.4707 0.0701 0.031 Uiso 1 1 calc R . .
C83 C 0.9321(2) 0.55487(18) 0.10456(15) 0.0307(8) Uani 1 1 d . . .
H83A H 0.8809 0.5637 0.1191 0.037 Uiso 1 1 calc R . .
H83B H 0.9639 0.5598 0.1370 0.037 Uiso 1 1 calc R . .
C84 C 0.9441(2) 0.6089(2) 0.05577(17) 0.0374(9) Uani 1 1 d . . .
H84A H 0.9958 0.6036 0.0441 0.056 Uiso 1 1 calc R . .
H84B H 0.9290 0.6560 0.0691 0.056 Uiso 1 1 calc R . .
H84C H 0.9152 0.6020 0.0225 0.056 Uiso 1 1 calc R . .
C85 C 0.88773(19) 0.34352(18) 0.07565(14) 0.0255(7) Uani 1 1 d . . .
H85A H 0.9054 0.3632 0.0380 0.031 Uiso 1 1 calc R . .
H85B H 0.8882 0.2927 0.0721 0.031 Uiso 1 1 calc R . .
C86 C 0.8093(2) 0.3768(2) 0.08616(16) 0.0320(8) Uani 1 1 d . . .
H86A H 0.8065 0.4284 0.0827 0.038 Uiso 1 1 calc R . .
H86B H 0.7931 0.3630 0.1260 0.038 Uiso 1 1 calc R . .
C87 C 0.7590(3) 0.3538(3) 0.0426(2) 0.0550(13) Uani 1 1 d . . .
H87A H 0.7635 0.3021 0.0462 0.066 Uiso 1 1 calc R . .
H87B H 0.7082 0.3722 0.0539 0.066 Uiso 1 1 calc R . .
C88 C 0.7707(3) 0.3749(3) -0.0174(2) 0.0629(14) Uani 1 1 d . . .
H88A H 0.7690 0.4259 -0.0217 0.094 Uiso 1 1 calc R . .
H88B H 0.7326 0.3609 -0.0405 0.094 Uiso 1 1 calc R . .
H88C H 0.8185 0.3522 -0.0310 0.094 Uiso 1 1 calc R . .
C89 C 0.92305(18) 0.31058(18) 0.17683(14) 0.0217(7) Uani 1 1 d . . .
H89A H 0.9222 0.2617 0.1669 0.026 Uiso 1 1 calc R . .
H89B H 0.8733 0.3294 0.1905 0.026 Uiso 1 1 calc R . .
C90 C 0.97465(18) 0.30985(18) 0.22663(14) 0.0242(7) Uani 1 1 d . . .
H90A H 0.9686 0.3566 0.2428 0.029 Uiso 1 1 calc R . .
H90B H 1.0257 0.2988 0.2123 0.029 Uiso 1 1 calc R . .
C91 C 0.9580(2) 0.25476(19) 0.27377(15) 0.0308(8) Uani 1 1 d . . .
H91A H 0.9851 0.2605 0.3088 0.037 Uiso 1 1 calc R . .
H91B H 0.9053 0.2631 0.2842 0.037 Uiso 1 1 calc R . .
C92 C 0.9776(3) 0.1802(2) 0.2560(2) 0.0529(12) Uani 1 1 d . . .
H92A H 0.9471 0.1725 0.2239 0.079 Uiso 1 1 calc R . .
H92B H 0.9694 0.1476 0.2891 0.079 Uiso 1 1 calc R . .
H92C H 1.0290 0.1723 0.2434 0.079 Uiso 1 1 calc R . .
C93 C 0.5527(3) 0.5578(3) 0.1308(2) 0.0575(13) Uani 1 1 d . . .
H93A H 0.5962 0.5395 0.1537 0.069 Uiso 1 1 calc R . .
H93B H 0.5097 0.5583 0.1575 0.069 Uiso 1 1 calc R . .
C94 C 0.5461(3) 0.5082(3) 0.0858(2) 0.0654(15) Uani 1 1 d . . .
H94A H 0.5858 0.5107 0.0562 0.079 Uiso 1 1 calc R . .
H94B H 0.4992 0.5219 0.0662 0.079 Uiso 1 1 calc R . .
C95 C 0.5499(3) 0.4337(3) 0.1114(2) 0.0730(17) Uani 1 1 d . . .
H95A H 0.5983 0.4194 0.1284 0.088 Uiso 1 1 calc R . .
H95B H 0.5129 0.4326 0.1433 0.088 Uiso 1 1 calc R . .
C96 C 0.5381(4) 0.3825(4) 0.0700(3) 0.099(3) Uani 1 1 d . . .
H96A H 0.4872 0.3908 0.0584 0.148 Uiso 1 1 calc R . .
H96B H 0.5492 0.3351 0.0882 0.148 Uiso 1 1 calc R . .
H96C H 0.5701 0.3874 0.0357 0.148 Uiso 1 1 calc R . .
C97 C 0.6202(2) 0.6350(3) 0.0636(2) 0.0530(12) Uani 1 1 d . . .
H97A H 0.6055 0.6138 0.0288 0.064 Uiso 1 1 calc R . .
H97B H 0.6245 0.6846 0.0524 0.064 Uiso 1 1 calc R . .
C98 C 0.6944(2) 0.5982(3) 0.0802(2) 0.0513(11) Uani 1 1 d . . .
H98A H 0.7168 0.6274 0.1062 0.062 Uiso 1 1 calc R . .
H98B H 0.6893 0.5531 0.1017 0.062 Uiso 1 1 calc R . .
C99 C 0.7435(3) 0.5849(3) 0.0275(2) 0.0589(13) Uani 1 1 d . . .
H99A H 0.7919 0.5626 0.0407 0.071 Uiso 1 1 calc R . .
H99B H 0.7235 0.5509 0.0046 0.071 Uiso 1 1 calc R . .
C100 C 0.7538(3) 0.6473(3) -0.0118(2) 0.0642(14) Uani 1 1 d . . .
H10A H 0.7069 0.6679 -0.0281 0.096 Uiso 1 1 calc R . .
H10B H 0.7883 0.6330 -0.0434 0.096 Uiso 1 1 calc R . .
H10C H 0.7728 0.6821 0.0101 0.096 Uiso 1 1 calc R . .
C101 C 0.4878(3) 0.6641(3) 0.0816(2) 0.0649(15) Uani 1 1 d . . .
H10D H 0.4839 0.6396 0.0459 0.078 Uiso 1 1 calc R . .
H10E H 0.4472 0.6537 0.1083 0.078 Uiso 1 1 calc R . .
C102 C 0.4772(3) 0.7416(3) 0.0659(3) 0.0693(15) Uani 1 1 d . . .
H10F H 0.5220 0.7550 0.0464 0.083 Uiso 1 1 calc R . .
H10G H 0.4678 0.7676 0.1016 0.083 Uiso 1 1 calc R . .
C103 C 0.4135(3) 0.7610(3) 0.0259(2) 0.0695(16) Uani 1 1 d . . .
H10H H 0.4246 0.7368 -0.0105 0.083 Uiso 1 1 calc R . .
H10I H 0.3699 0.7441 0.0446 0.083 Uiso 1 1 calc R . .
C104 C 0.3967(4) 0.8376(4) 0.0116(3) 0.087(2) Uani 1 1 d . . .
H10J H 0.3867 0.8620 0.0475 0.130 Uiso 1 1 calc R . .
H10K H 0.3539 0.8471 -0.0128 0.130 Uiso 1 1 calc R . .
H10L H 0.4384 0.8541 -0.0094 0.130 Uiso 1 1 calc R . .
C105 C 0.5748(3) 0.6731(3) 0.1606(2) 0.0568(13) Uani 1 1 d . . .
H10M H 0.6210 0.6497 0.1774 0.068 Uiso 1 1 calc R . .
H10N H 0.5829 0.7207 0.1458 0.068 Uiso 1 1 calc R . .
C106 C 0.5183(3) 0.6803(3) 0.2081(2) 0.0663(15) Uani 1 1 d . . .
H10O H 0.5125 0.6332 0.2257 0.080 Uiso 1 1 calc R . .
H10P H 0.4711 0.7016 0.1918 0.080 Uiso 1 1 calc R . .
C107 C 0.5381(3) 0.7247(3) 0.2542(2) 0.0715(16) Uani 1 1 d . . .
H10Q H 0.5836 0.7008 0.2718 0.086 Uiso 1 1 calc R . .
H10R H 0.5493 0.7695 0.2350 0.086 Uiso 1 1 calc R . .
C108 C 0.4841(3) 0.7415(4) 0.3015(3) 0.092(2) Uani 1 1 d . . .
H10S H 0.4398 0.7684 0.2854 0.138 Uiso 1 1 calc R . .
H10T H 0.5043 0.7693 0.3292 0.138 Uiso 1 1 calc R . .
H10U H 0.4723 0.6980 0.3214 0.138 Uiso 1 1 calc R . .
C109 C 0.6825(2) 0.5221(2) 0.40180(18) 0.0429(10) Uani 1 1 d . . .
H10V H 0.7000 0.5606 0.3773 0.051 Uiso 1 1 calc R . .
H10W H 0.6682 0.4883 0.3755 0.051 Uiso 1 1 calc R . .
C110 C 0.6158(3) 0.5518(3) 0.4369(2) 0.0563(13) Uani 1 1 d . . .
H11A H 0.6303 0.5824 0.4658 0.068 Uiso 1 1 calc R . .
H11B H 0.5945 0.5131 0.4581 0.068 Uiso 1 1 calc R . .
C111 C 0.5590(3) 0.5938(3) 0.3978(3) 0.0734(18) Uani 1 1 d . . .
H11C H 0.5447 0.5632 0.3688 0.088 Uiso 1 1 calc R . .
H11D H 0.5804 0.6325 0.3767 0.088 Uiso 1 1 calc R . .
C112 C 0.4913(3) 0.6240(4) 0.4328(3) 0.095(2) Uani 1 1 d . . .
H11E H 0.4714 0.5859 0.4552 0.143 Uiso 1 1 calc R . .
H11F H 0.4546 0.6481 0.4063 0.143 Uiso 1 1 calc R . .
H11G H 0.5046 0.6573 0.4593 0.143 Uiso 1 1 calc R . .
C113 C 0.7710(2) 0.53548(19) 0.47849(15) 0.0302(8) Uani 1 1 d . . .
H11H H 0.7319 0.5477 0.5079 0.036 Uiso 1 1 calc R . .
H11I H 0.8137 0.5104 0.4993 0.036 Uiso 1 1 calc R . .
C114 C 0.7919(3) 0.6028(2) 0.45026(16) 0.0398(10) Uani 1 1 d . . .
H11J H 0.7481 0.6330 0.4353 0.048 Uiso 1 1 calc R . .
H11K H 0.8265 0.5923 0.4172 0.048 Uiso 1 1 calc R . .
C115 C 0.8271(3) 0.6402(2) 0.49500(17) 0.0449(11) Uani 1 1 d . . .
H11L H 0.7922 0.6495 0.5280 0.054 Uiso 1 1 calc R . .
H11M H 0.8704 0.6092 0.5099 0.054 Uiso 1 1 calc R . .
C116 C 0.8500(3) 0.7090(2) 0.4709(2) 0.0548(13) Uani 1 1 d . . .
H11N H 0.8813 0.7009 0.4362 0.082 Uiso 1 1 calc R . .
H11O H 0.8769 0.7284 0.5003 0.082 Uiso 1 1 calc R . .
H11P H 0.8066 0.7423 0.4607 0.082 Uiso 1 1 calc R . .
C117 C 0.8057(2) 0.4585(2) 0.39593(15) 0.0351(9) Uani 1 1 d . . .
H11Q H 0.7872 0.4253 0.3713 0.042 Uiso 1 1 calc R . .
H11R H 0.8177 0.4985 0.3702 0.042 Uiso 1 1 calc R . .
C118 C 0.8754(2) 0.4220(2) 0.42356(17) 0.0419(10) Uani 1 1 d . . .
H11S H 0.8975 0.4561 0.4448 0.050 Uiso 1 1 calc R . .
H11T H 0.8635 0.3843 0.4519 0.050 Uiso 1 1 calc R . .
C119 C 0.9288(3) 0.3914(3) 0.3790(2) 0.0564(13) Uani 1 1 d . . .
H11U H 0.9364 0.4284 0.3487 0.068 Uiso 1 1 calc R . .
H11V H 0.9078 0.3544 0.3604 0.068 Uiso 1 1 calc R . .
C120 C 1.0018(3) 0.3602(3) 0.4034(3) 0.0643(15) Uani 1 1 d . . .
H12A H 1.0244 0.3971 0.4198 0.096 Uiso 1 1 calc R . .
H12B H 1.0335 0.3396 0.3723 0.096 Uiso 1 1 calc R . .
H12C H 0.9947 0.3239 0.4338 0.096 Uiso 1 1 calc R . .
C121 C 0.7226(2) 0.42581(19) 0.47773(15) 0.0323(8) Uani 1 1 d . . .
H12D H 0.6845 0.4456 0.5056 0.039 Uiso 1 1 calc R . .
H12E H 0.7652 0.4043 0.5004 0.039 Uiso 1 1 calc R . .
C122 C 0.6938(2) 0.3684(2) 0.44736(18) 0.0385(9) Uani 1 1 d . . .
H12F H 0.6479 0.3880 0.4282 0.046 Uiso 1 1 calc R . .
H12G H 0.7296 0.3508 0.4170 0.046 Uiso 1 1 calc R . .
C123 C 0.6801(3) 0.3088(3) 0.4894(2) 0.0624(14) Uani 1 1 d . . .
H12H H 0.6506 0.3276 0.5230 0.075 Uiso 1 1 calc R . .
H12I H 0.6517 0.2776 0.4703 0.075 Uiso 1 1 calc R . .
C124 C 0.7497(5) 0.2670(3) 0.5108(4) 0.142(4) Uani 1 1 d . . .
H12J H 0.7845 0.2593 0.4781 0.213 Uiso 1 1 calc R . .
H12K H 0.7396 0.2218 0.5284 0.213 Uiso 1 1 calc R . .
H12L H 0.7703 0.2928 0.5398 0.213 Uiso 1 1 calc R . .
C125 C 0.2030(2) 1.09505(18) 0.35217(16) 0.0315(8) Uani 1 1 d . . .
H12M H 0.1982 1.1321 0.3203 0.038 Uiso 1 1 calc R . .
H12N H 0.2321 1.1108 0.3826 0.038 Uiso 1 1 calc R . .
C126 C 0.1270(2) 1.0884(2) 0.37779(17) 0.0352(9) Uani 1 1 d . . .
H12O H 0.0984 1.0695 0.3487 0.042 Uiso 1 1 calc R . .
H12P H 0.1314 1.0548 0.4122 0.042 Uiso 1 1 calc R . .
C127 C 0.0868(2) 1.1583(2) 0.39553(18) 0.0390(9) Uani 1 1 d . . .
C128 C 0.0111(3) 1.1503(2) 0.42021(19) 0.0475(11) Uani 1 1 d . . .
H12Q H -0.0183 1.1363 0.3898 0.071 Uiso 1 1 calc R . .
H12R H -0.0122 1.1951 0.4343 0.071 Uiso 1 1 calc R . .
H12S H 0.0150 1.1145 0.4524 0.071 Uiso 1 1 calc R . .
C129 C 0.2653(2) 0.97414(19) 0.37828(16) 0.0292(8) Uani 1 1 d . . .
H12T H 0.2202 0.9674 0.4010 0.035 Uiso 1 1 calc R . .
H12U H 0.2838 0.9292 0.3611 0.035 Uiso 1 1 calc R . .
C130 C 0.3212(2) 0.9896(2) 0.41996(17) 0.0335(9) Uani 1 1 d . . .
H13D H 0.2994 1.0278 0.4445 0.040 Uiso 1 1 calc R . .
H13E H 0.3632 1.0053 0.3978 0.040 Uiso 1 1 calc R . .
C131 C 0.3473(2) 0.9235(2) 0.45875(16) 0.0363(9) Uani 1 1 d . . .
H13F H 0.3772 0.9364 0.4898 0.044 Uiso 1 1 calc R . .
H13G H 0.3043 0.9054 0.4774 0.044 Uiso 1 1 calc R . .
C132 C 0.3918(2) 0.8656(2) 0.42579(18) 0.0413(10) Uani 1 1 d . . .
H13H H 0.3605 0.8478 0.3986 0.062 Uiso 1 1 calc R . .
H131 H 0.4115 0.8274 0.4533 0.062 Uiso 1 1 calc R . .
H13J H 0.4319 0.8842 0.4042 0.062 Uiso 1 1 calc R . .
C133 C 0.19702(18) 0.99572(17) 0.28978(14) 0.0229(7) Uani 1 1 d . . .
H13K H 0.2263 0.9539 0.2740 0.027 Uiso 1 1 calc R . .
H13L H 0.1569 0.9794 0.3140 0.027 Uiso 1 1 calc R . .
C134 C 0.16405(19) 1.04258(18) 0.23933(15) 0.0255(7) Uani 1 1 d . . .
H13M H 0.1400 1.0876 0.2536 0.031 Uiso 1 1 calc R . .
H13N H 0.2029 1.0526 0.2108 0.031 Uiso 1 1 calc R . .
C135 C 0.10876(19) 1.00663(19) 0.21041(15) 0.0278(8) Uani 1 1 d . . .
H13O H 0.0684 1.0001 0.2386 0.033 Uiso 1 1 calc R . .
H13P H 0.0881 1.0376 0.1775 0.033 Uiso 1 1 calc R . .
C136 C 0.1397(2) 0.9369(2) 0.18852(18) 0.0407(10) Uani 1 1 d . . .
H13Q H 0.1804 0.9427 0.1612 0.061 Uiso 1 1 calc R . .
H13R H 0.1019 0.9177 0.1688 0.061 Uiso 1 1 calc R . .
H13S H 0.1571 0.9048 0.2213 0.061 Uiso 1 1 calc R . .
C137 C 0.3121(2) 1.0488(2) 0.29528(17) 0.0332(9) Uani 1 1 d . . .
H13T H 0.2956 1.0819 0.2623 0.040 Uiso 1 1 calc R . .
H13U H 0.3393 1.0740 0.3211 0.040 Uiso 1 1 calc R . .
C138 C 0.3644(2) 0.9886(2) 0.27162(19) 0.0420(10) Uani 1 1 d . . .
H13V H 0.4145 1.0004 0.2726 0.050 Uiso 1 1 calc R . .
H13W H 0.3621 0.9465 0.2980 0.050 Uiso 1 1 calc R . .
C139 C 0.3511(2) 0.9702(3) 0.21054(19) 0.0488(11) Uani 1 1 d . . .
H13$ H 0.3622 1.0087 0.1828 0.059 Uiso 1 1 calc R . .
H13I H 0.2990 0.9655 0.2072 0.059 Uiso 1 1 calc R . .
C140 C 0.3982(3) 0.9013(3) 0.1943(2) 0.0613(13) Uani 1 1 d . . .
H14A H 0.4491 0.9028 0.2035 0.092 Uiso 1 1 calc R . .
H14B H 0.3948 0.8957 0.1527 0.092 Uiso 1 1 calc R . .
H14C H 0.3807 0.8617 0.2165 0.092 Uiso 1 1 calc R . .
C1A C 0.8188(2) 0.9717(2) 0.42509(17) 0.0400(10) Uani 1 1 d . . .
H1A H 0.8472 0.9655 0.3877 0.048 Uiso 1 1 calc R . .
C2A C 0.2690(3) 0.0262(4) 0.9900(2) 0.0750(16) Uani 1 1 d . . .
H2A H 0.2617 0.0783 0.9924 0.090 Uiso 1 1 calc R . .
Cl1 Cl 0.83801(7) 0.89559(7) 0.46940(5) 0.0591(3) Uani 1 1 d . . .
Cl2 Cl 0.72485(7) 0.98617(7) 0.41014(6) 0.0572(3) Uani 1 1 d . . .
Cl3 Cl 0.84514(7) 1.04288(7) 0.45815(6) 0.0652(4) Uani 1 1 d . . .
Cl4 Cl 0.28170(8) -0.01088(7) 1.06074(5) 0.0638(3) Uani 1 1 d . . .
Cl5 Cl 0.18913(8) 0.00373(7) 0.96282(6) 0.0647(4) Uani 1 1 d . . .
Cl6 Cl 0.34191(9) 0.00562(9) 0.94297(7) 0.0821(5) Uani 1 1 d . . .
N1 N 0.13279(14) 0.77830(13) 0.29011(11) 0.0175(5) Uani 1 1 d . . .
H1 H 0.0950 0.7686 0.2719 0.021 Uiso 1 1 calc R . .
N2 N -0.02236(14) 0.88516(14) 0.28790(11) 0.0197(6) Uani 1 1 d . . .
H2E H -0.0153 0.8457 0.2702 0.024 Uiso 1 1 calc R . .
N3 N -0.02416(14) 0.87936(14) 0.14393(11) 0.0192(6) Uani 1 1 d . . .
H3A H -0.0261 0.8388 0.1632 0.023 Uiso 1 1 calc R . .
N4 N 0.13375(14) 0.76817(13) 0.14793(11) 0.0184(6) Uani 1 1 d . . .
H4 H 0.0957 0.7573 0.1685 0.022 Uiso 1 1 calc R . .
N5 N 0.15654(17) 0.52568(17) 0.36059(14) 0.0344(7) Uani 1 1 d . . .
N6 N 0.13619(16) 0.50221(16) 0.15235(14) 0.0324(7) Uani 1 1 d . . .
N7 N -0.27118(18) 0.79798(18) 0.32612(14) 0.0375(8) Uani 1 1 d . . .
N8 N -0.26522(18) 0.80713(17) 0.11354(15) 0.0376(8) Uani 1 1 d . . .
N9 N 0.34585(14) 0.23242(14) 0.20788(12) 0.0206(6) Uani 1 1 d . . .
H9A H 0.3858 0.2462 0.2196 0.025 Uiso 1 1 calc R . .
N10 N 0.36266(14) 0.22748(14) 0.34809(11) 0.0200(6) Uani 1 1 d . . .
H101 H 0.3977 0.2281 0.3214 0.024 Uiso 1 1 calc R . .
N11 N 0.50929(14) 0.11331(14) 0.33667(12) 0.0238(6) Uani 1 1 d . . .
H11 H 0.5038 0.1534 0.3158 0.029 Uiso 1 1 calc R . .
N12 N 0.49560(14) 0.11820(14) 0.19580(13) 0.0237(6) Uani 1 1 d . . .
H12 H 0.4901 0.1551 0.2168 0.028 Uiso 1 1 calc R . .
N13 N 0.34166(18) 0.48247(17) 0.14584(14) 0.0362(8) Uani 1 1 d . . .
N14 N 0.35189(16) 0.50494(16) 0.35483(14) 0.0315(7) Uani 1 1 d . . .
N15 N 0.75538(17) 0.18493(17) 0.14161(15) 0.0362(8) Uani 1 1 d . . .
N16 N 0.74889(18) 0.19411(18) 0.35305(15) 0.0400(8) Uani 1 1 d . . .
N17 N 0.24504(15) 1.02901(15) 0.32876(12) 0.0259(6) Uani 1 1 d . . .
N18 N 0.94163(15) 0.35306(14) 0.12208(11) 0.0210(6) Uani 1 1 d . . .
N19 N 0.74515(18) 0.48538(16) 0.43848(12) 0.0317(7) Uani 1 1 d . . .
N20 N 0.55891(17) 0.63334(19) 0.10986(14) 0.0403(8) Uani 1 1 d . . .
O1 O 0.1673(2) 0.56282(19) 0.39921(13) 0.0646(10) Uani 1 1 d . . .
O2 O 0.14054(16) 0.46653(13) 0.36960(12) 0.0411(7) Uani 1 1 d . . .
O3 O 0.12396(15) 0.44214(14) 0.16358(13) 0.0422(7) Uani 1 1 d . . .
O4 O 0.13146(19) 0.53212(17) 0.10354(13) 0.0523(8) Uani 1 1 d . . .
O5 O -0.2436(2) 0.8120(2) 0.36976(14) 0.0636(10) Uani 1 1 d . . .
O6 O -0.3238(2) 0.7670(2) 0.32644(14) 0.0667(10) Uani 1 1 d . . .
O7 O -0.22851(18) 0.81504(18) 0.06922(13) 0.0520(8) Uani 1 1 d . . .
O8 O -0.32354(17) 0.78393(19) 0.11458(14) 0.0568(9) Uani 1 1 d . . .
O9 O 0.3287(3) 0.4474(2) 0.10648(14) 0.0815(14) Uani 1 1 d . . .
O10 O 0.36525(15) 0.53847(14) 0.13822(12) 0.0388(6) Uani 1 1 d . . .
O11 O 0.3470(3) 0.4778(2) 0.40382(14) 0.0816(14) Uani 1 1 d . . .
O12 O 0.36923(17) 0.56278(14) 0.34443(13) 0.0452(7) Uani 1 1 d . . .
O13 O 0.71400(17) 0.18573(18) 0.39823(13) 0.0532(8) Uani 1 1 d . . .
O14 O 0.80555(17) 0.22000(19) 0.34988(14) 0.0548(8) Uani 1 1 d . . .
O15 O 0.81480(14) 0.20620(15) 0.13978(12) 0.0406(7) Uani 1 1 d . . .
O16 O 0.72172(19) 0.1766(2) 0.09854(14) 0.0630(10) Uani 1 1 d . . .
O17 O 1.00537(11) 0.75949(11) 0.22733(9) 0.0193(5) Uani 1 1 d . . .
O18 O 0.90056(12) 0.71706(11) 0.18507(9) 0.0210(5) Uani 1 1 d . . .
O19 O 0.92643(12) 0.68483(12) 0.29084(9) 0.0216(5) Uani 1 1 d . . .
H19A H 0.9024 0.6514 0.2894 0.032 Uiso 1 1 calc R . .
O20 O 1.01330(12) 0.63343(11) 0.21370(10) 0.0242(5) Uani 1 1 d . . .
H20 H 0.9899 0.5995 0.2122 0.036 Uiso 1 1 calc R . .
O21 O 0.82908(12) 0.52391(13) 0.24262(12) 0.0322(6) Uani 1 1 d . . .
H21A H 0.8738 0.5272 0.2401 0.048 Uiso 1 1 calc R . .
O22 O 0.80402(15) 0.62973(15) 0.30289(10) 0.0363(6) Uani 1 1 d . . .
O23 O 0.79556(12) 0.64565(12) 0.19428(10) 0.0263(5) Uani 1 1 d . . .
H23 H 0.8395 0.6515 0.1907 0.040 Uiso 1 1 calc R . .
O24 O 0.70266(12) 0.58869(13) 0.25563(12) 0.0320(6) Uani 1 1 d . . .
O25 O 0.48164(11) 0.23971(11) 0.26448(10) 0.0207(5) Uani 1 1 d . . .
O26 O 0.56696(12) 0.31139(12) 0.31132(9) 0.0238(5) Uani 1 1 d . . .
H26 H 0.5916 0.3442 0.3038 0.036 Uiso 1 1 calc R . .
O27 O 0.47528(12) 0.36571(12) 0.23756(10) 0.0240(5) Uani 1 1 d . . .
H27 H 0.4992 0.3991 0.2299 0.036 Uiso 1 1 calc R . .
O28 O 0.58451(12) 0.28054(12) 0.20671(10) 0.0223(5) Uani 1 1 d . . .
O29 O 0.69245(13) 0.34932(13) 0.20011(11) 0.0315(6) Uani 1 1 d . . .
H29A H 0.6481 0.3445 0.2011 0.047 Uiso 1 1 calc R . .
O30 O 0.68922(14) 0.36575(15) 0.30681(11) 0.0373(6) Uani 1 1 d . . .
O31 O 0.66371(12) 0.47167(13) 0.23639(12) 0.0335(6) Uani 1 1 d . . .
H31 H 0.6188 0.4694 0.2382 0.050 Uiso 1 1 calc R . .
O32 O 0.78921(12) 0.40396(13) 0.24555(12) 0.0329(6) Uani 1 1 d . . .
O1A O 0.97494(13) 0.51148(12) 0.25721(11) 0.0283(5) Uani 1 1 d . . .
O2A O 0.51947(13) 0.48543(12) 0.26362(12) 0.0331(6) Uani 1 1 d . . .
P1 P 0.95996(4) 0.70007(4) 0.23205(3) 0.01597(17) Uani 1 1 d . . .
P2 P 0.78577(5) 0.59615(5) 0.24549(4) 0.02274(19) Uani 1 1 d . . .
P3 P 0.52876(4) 0.29802(4) 0.25782(3) 0.01732(18) Uani 1 1 d . . .
P4 P 0.70562(5) 0.39864(5) 0.24422(4) 0.0242(2) Uani 1 1 d . . .
C1F C 0.4853(6) 0.4159(6) 0.4244(5) 0.158(4) Uani 1 1 d U . .
H1F1 H 0.5213 0.3873 0.4492 0.236 Uiso 1 1 calc R . .
H1F2 H 0.4408 0.3939 0.4248 0.236 Uiso 1 1 calc R . .
H1F3 H 0.4738 0.4628 0.4390 0.236 Uiso 1 1 calc R . .
O1B O 0.5102(2) 0.42042(19) 0.37465(16) 0.0728(13) Uani 1 1 d U . .
H1B H 0.5252 0.3801 0.3637 0.109 Uiso 1 1 calc R . .
C1B C 0.9974(3) 0.5758(3) 0.4157(2) 0.0672(15) Uani 1 1 d U . .
H1B1 H 1.0174 0.6166 0.4279 0.101 Uiso 1 1 calc R . .
H1B2 H 1.0269 0.5328 0.4310 0.101 Uiso 1 1 calc R . .
H1B3 H 0.9471 0.5771 0.4306 0.101 Uiso 1 1 calc R . .
O2B O 0.9985(2) 0.57701(15) 0.35773(13) 0.0569(9) Uani 1 1 d U . .
H2B H 0.9675 0.6098 0.3448 0.085 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
C23 C22 1.377(4) . ?
C23 N3 1.379(4) . ?
C23 C24 1.518(5) . ?
C1 C2 1.371(5) . ?
C1 N1 1.380(4) . ?
C1 C31 1.511(5) . ?
C2 C3 1.419(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.370(5) . ?
C3 H3 0.9500 . ?
C4 N1 1.378(4) . ?
C4 C5 1.518(4) . ?
C5 C8 1.518(4) . ?
C5 C6 1.531(5) . ?
C5 C7 1.546(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.370(5) . ?
C8 N2 1.370(4) . ?
C9 C10 1.418(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.370(5) . ?
C10 H10 0.9500 . ?
C11 N2 1.376(4) . ?
C11 C12 1.512(5) . ?
C12 C20 1.516(4) . ?
C12 C14 1.543(5) . ?
C12 C13 1.542(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C19 1.390(5) . ?
C14 C15 1.388(5) . ?
C15 C16 1.385(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(5) . ?
C16 N8 1.468(5) . ?
C17 C18 1.384(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(5) . ?
C18 N7 1.467(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.369(5) . ?
C20 N3 1.375(4) . ?
C21 C22 1.423(5) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C24 C27 1.509(4) . ?
C24 C25 1.538(5) . ?
C24 C26 1.537(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 N4 1.378(4) . ?
C27 C28 1.373(5) . ?
C28 C29 1.417(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.364(5) . ?
C29 H29 0.9500 . ?
C30 N4 1.381(4) . ?
C30 C31 1.516(4) . ?
C31 C33 1.543(4) . ?
C31 C32 1.547(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C38 1.388(5) . ?
C33 C34 1.394(5) . ?
C34 C35 1.388(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.381(5) . ?
C35 N6 1.475(5) . ?
C36 C37 1.374(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.386(5) . ?
C37 N5 1.474(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.374(5) . ?
C39 N9 1.379(4) . ?
C39 C69 1.510(5) . ?
C40 C41 1.414(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.377(5) . ?
C41 H41 0.9500 . ?
C42 N9 1.372(4) . ?
C42 C43 1.519(5) . ?
C43 C46 1.510(5) . ?
C43 C45 1.538(5) . ?
C43 C44 1.543(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 N12 1.373(5) . ?
C46 C47 1.381(5) . ?
C47 C48 1.415(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.368(5) . ?
C48 H48 0.9500 . ?
C49 N12 1.380(4) . ?
C49 C50 1.510(5) . ?
C50 C58 1.515(5) . ?
C50 C52 1.547(5) . ?
C50 C51 1.545(5) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C57 1.385(5) . ?
C52 C53 1.392(5) . ?
C53 C54 1.386(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.380(5) . ?
C54 N15 1.465(5) . ?
C55 C56 1.374(5) . ?
C55 H55 0.9500 . ?
C56 C57 1.394(5) . ?
C56 N16 1.472(5) . ?
C57 H57 0.9500 . ?
C58 C59 1.379(5) . ?
C58 N11 1.381(4) . ?
C59 C60 1.412(6) . ?
C59 H59 0.9500 . ?
C60 C61 1.377(5) . ?
C60 H60 0.9500 . ?
C61 N11 1.375(4) . ?
C61 C62 1.519(5) . ?
C62 C65 1.519(4) . ?
C62 C63 1.540(5) . ?
C62 C64 1.545(5) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 C66 1.378(5) . ?
C65 N10 1.379(4) . ?
C66 C67 1.416(5) . ?
C66 H66 0.9500 . ?
C67 C68 1.372(5) . ?
C67 H67 0.9500 . ?
C68 N10 1.382(4) . ?
C68 C69 1.517(4) . ?
C69 C71 1.543(4) . ?
C69 C70 1.549(4) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 C72 1.392(5) . ?
C71 C76 1.394(5) . ?
C72 C73 1.386(5) . ?
C72 H72 0.9500 . ?
C73 C74 1.380(5) . ?
C73 N14 1.474(5) . ?
C74 C75 1.376(5) . ?
C74 H74 0.9500 . ?
C75 C76 1.382(5) . ?
C75 N13 1.474(4) . ?
C76 H76 0.9500 . ?
C77 C78 1.513(5) . ?
C77 N18 1.523(4) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C78 C79 1.525(5) . ?
C78 H78A 0.9900 . ?
C78 H78B 0.9900 . ?
C79 C80 1.510(5) . ?
C79 H79A 0.9900 . ?
C79 H79B 0.9900 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 C82 1.515(4) . ?
C81 N18 1.521(4) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 C83 1.530(5) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 C84 1.518(5) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 C86 1.521(5) . ?
C85 N18 1.531(4) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 C87 1.527(6) . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C87 C88 1.436(7) . ?
C87 H87A 0.9900 . ?
C87 H87B 0.9900 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C89 N18 1.518(4) . ?
C89 C90 1.522(4) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C90 C91 1.527(5) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C91 C92 1.515(6) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C93 C94 1.481(8) . ?
C93 N20 1.526(6) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C94 C95 1.512(7) . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
C95 C96 1.464(8) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
C97 C98 1.507(6) . ?
C97 N20 1.533(5) . ?
C97 H97A 0.9900 . ?
C97 H97B 0.9900 . ?
C98 C99 1.506(7) . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
C99 C100 1.492(7) . ?
C99 H99A 0.9900 . ?
C99 H99B 0.9900 . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
C101 C102 1.504(8) . ?
C101 N20 1.519(6) . ?
C101 H10D 0.9900 . ?
C101 H10E 0.9900 . ?
C102 C103 1.516(7) . ?
C102 H10F 0.9900 . ?
C102 H10G 0.9900 . ?
C103 C104 1.486(8) . ?
C103 H10H 0.9900 . ?
C103 H10I 0.9900 . ?
C104 H10J 0.9800 . ?
C104 H10K 0.9800 . ?
C104 H10L 0.9800 . ?
C105 C106 1.488(7) . ?
C105 N20 1.505(6) . ?
C105 H10M 0.9900 . ?
C105 H10N 0.9900 . ?
C106 C107 1.499(8) . ?
C106 H10O 0.9900 . ?
C106 H10P 0.9900 . ?
C107 C108 1.476(8) . ?
C107 H10Q 0.9900 . ?
C107 H10R 0.9900 . ?
C108 H10S 0.9800 . ?
C108 H10T 0.9800 . ?
C108 H10U 0.9800 . ?
C109 C110 1.517(7) . ?
C109 N19 1.526(5) . ?
C109 H10V 0.9900 . ?
C109 H10W 0.9900 . ?
C110 C111 1.520(6) . ?
C110 H11A 0.9900 . ?
C110 H11B 0.9900 . ?
C111 C112 1.532(9) . ?
C111 H11C 0.9900 . ?
C111 H11D 0.9900 . ?
C112 H11E 0.9800 . ?
C112 H11F 0.9800 . ?
C112 H11G 0.9800 . ?
C113 C114 1.511(5) . ?
C113 N19 1.519(5) . ?
C113 H11H 0.9900 . ?
C113 H11I 0.9900 . ?
C114 C115 1.518(6) . ?
C114 H11J 0.9900 . ?
C114 H11K 0.9900 . ?
C115 C116 1.519(6) . ?
C115 H11L 0.9900 . ?
C115 H11M 0.9900 . ?
C116 H11N 0.9800 . ?
C116 H11O 0.9800 . ?
C116 H11P 0.9800 . ?
C117 C118 1.522(6) . ?
C117 N19 1.522(5) . ?
C117 H11Q 0.9900 . ?
C117 H11R 0.9900 . ?
C118 C119 1.492(6) . ?
C118 H11S 0.9900 . ?
C118 H11T 0.9900 . ?
C119 C120 1.515(7) . ?
C119 H11U 0.9900 . ?
C119 H11V 0.9900 . ?
C120 H12A 0.9800 . ?
C120 H12B 0.9800 . ?
C120 H12C 0.9800 . ?
C121 N19 1.515(5) . ?
C121 C122 1.520(6) . ?
C121 H12D 0.9900 . ?
C121 H12E 0.9900 . ?
C122 C123 1.502(6) . ?
C122 H12F 0.9900 . ?
C122 H12G 0.9900 . ?
C123 C124 1.503(9) . ?
C123 H12H 0.9900 . ?
C123 H12I 0.9900 . ?
C124 H12J 0.9800 . ?
C124 H12K 0.9800 . ?
C124 H12L 0.9800 . ?
C125 N17 1.518(5) . ?
C125 C126 1.528(5) . ?
C125 H12M 0.9900 . ?
C125 H12N 0.9900 . ?
C126 C127 1.520(5) . ?
C126 H12O 0.9900 . ?
C126 H12P 0.9900 . ?
C127 C128 1.522(6) . ?
C128 H12Q 0.9800 . ?
C128 H12R 0.9800 . ?
C128 H12S 0.9800 . ?
C129 C130 1.515(5) . ?
C129 N17 1.527(4) . ?
C129 H12T 0.9900 . ?
C129 H12U 0.9900 . ?
C130 C131 1.541(5) . ?
C130 H13D 0.9900 . ?
C130 H13E 0.9900 . ?
C131 C132 1.521(6) . ?
C131 H13F 0.9900 . ?
C131 H13G 0.9900 . ?
C132 H13H 0.9800 . ?
C132 H131 0.9800 . ?
C132 H13J 0.9800 . ?
C133 C134 1.519(5) . ?
C133 N17 1.523(4) . ?
C133 H13K 0.9900 . ?
C133 H13L 0.9900 . ?
C134 C135 1.516(5) . ?
C134 H13M 0.9900 . ?
C134 H13N 0.9900 . ?
C135 C136 1.499(5) . ?
C135 H13O 0.9900 . ?
C135 H13P 0.9900 . ?
C136 H13Q 0.9800 . ?
C136 H13R 0.9800 . ?
C136 H13S 0.9800 . ?
C137 C138 1.521(6) . ?
C137 N17 1.522(5) . ?
C137 H13T 0.9900 . ?
C137 H13U 0.9900 . ?
C138 C139 1.516(6) . ?
C138 H13V 0.9900 . ?
C138 H13W 0.9900 . ?
C139 C140 1.543(7) . ?
C139 H13$ 0.9900 . ?
C139 H13I 0.9900 . ?
C140 H14A 0.9800 . ?
C140 H14B 0.9800 . ?
C140 H14C 0.9800 . ?
C1A Cl1 1.737(4) . ?
C1A Cl3 1.753(4) . ?
C1A Cl2 1.769(4) . ?
C1A H1A 1.0000 . ?
C2A Cl6 1.721(6) . ?
C2A Cl4 1.750(6) . ?
C2A Cl5 1.754(6) . ?
C2A H2A 1.0000 . ?
N1 H1 0.8800 . ?
N2 H2E 0.8800 . ?
N3 H3A 0.8800 . ?
N4 H4 0.8800 . ?
N5 O1 1.221(4) . ?
N5 O2 1.225(4) . ?
N6 O3 1.224(4) . ?
N6 O4 1.233(4) . ?
N7 O5 1.210(4) . ?
N7 O6 1.216(4) . ?
N8 O7 1.222(4) . ?
N8 O8 1.229(4) . ?
N9 H9A 0.8800 . ?
N10 H101 0.8800 . ?
N11 H11 0.8800 . ?
N12 H12 0.8800 . ?
N13 O9 1.220(5) . ?
N13 O10 1.225(4) . ?
N14 O12 1.214(4) . ?
N14 O11 1.222(5) . ?
N15 O15 1.230(4) . ?
N15 O16 1.226(4) . ?
N16 O13 1.222(4) . ?
N16 O14 1.226(4) . ?
O17 P1 1.515(2) . ?
O18 P1 1.562(2) . ?
O19 P1 1.502(2) . ?
O19 H19A 0.8400 . ?
O20 P1 1.578(2) . ?
O20 H20 0.8400 . ?
O21 P2 1.512(3) . ?
O21 H21A 0.8400 . ?
O22 P2 1.583(3) . ?
O23 P2 1.494(2) . ?
O23 H23 0.8400 . ?
O24 P2 1.577(2) . ?
O25 P3 1.520(2) . ?
O26 P3 1.503(2) . ?
O26 H26 0.8400 . ?
O27 P3 1.580(2) . ?
O27 H27 0.8400 . ?
O28 P3 1.562(2) . ?
O29 P4 1.490(3) . ?
O29 H29A 0.8400 . ?
O30 P4 1.578(3) . ?
O31 P4 1.513(3) . ?
O31 H31 0.8400 . ?
O32 P4 1.571(2) . ?
C1F O1B 1.225(11) . ?
C1F H1F1 0.9800 . ?
C1F H1F2 0.9800 . ?
C1F H1F3 0.9800 . ?
O1B H1B 0.8400 . ?
C1B O2B 1.337(6) . ?
C1B H1B1 0.9800 . ?
C1B H1B2 0.9800 . ?
C1B H1B3 0.9800 . ?
O2B H2B 0.8400 . ?

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
C22 C23 N3 106.9(3) . . ?
C22 C23 C24 130.7(3) . . ?
N3 C23 C24 122.4(3) . . ?
C2 C1 N1 107.2(3) . . ?
C2 C1 C31 130.0(3) . . ?
N1 C1 C31 122.5(3) . . ?
C1 C2 C3 107.6(3) . . ?
C1 C2 H2 126.2 . . ?
C3 C2 H2 126.2 . . ?
C4 C3 C2 108.1(3) . . ?
C4 C3 H3 125.9 . . ?
C2 C3 H3 125.9 . . ?
C3 C4 N1 107.0(3) . . ?
C3 C4 C5 129.6(3) . . ?
N1 C4 C5 123.3(3) . . ?
C8 C5 C4 112.7(3) . . ?
C8 C5 C6 108.3(3) . . ?
C4 C5 C6 108.7(3) . . ?
C8 C5 C7 109.3(3) . . ?
C4 C5 C7 109.7(3) . . ?
C6 C5 C7 108.1(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N2 106.6(3) . . ?
C9 C8 C5 130.5(3) . . ?
N2 C8 C5 122.8(3) . . ?
C8 C9 C10 108.4(3) . . ?
C8 C9 H9 125.8 . . ?
C10 C9 H9 125.8 . . ?
C11 C10 C9 107.3(3) . . ?
C11 C10 H10 126.3 . . ?
C9 C10 H10 126.3 . . ?
C10 C11 N2 107.1(3) . . ?
C10 C11 C12 130.3(3) . . ?
N2 C11 C12 122.6(3) . . ?
C11 C12 C20 111.7(3) . . ?
C11 C12 C14 111.3(3) . . ?
C20 C12 C14 110.7(3) . . ?
C11 C12 C13 108.7(3) . . ?
C20 C12 C13 108.5(3) . . ?
C14 C12 C13 105.6(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 118.3(3) . . ?
C19 C14 C12 121.6(3) . . ?
C15 C14 C12 119.9(3) . . ?
C16 C15 C14 119.7(3) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C17 C16 C15 123.3(3) . . ?
C17 C16 N8 118.7(3) . . ?
C15 C16 N8 117.9(3) . . ?
C16 C17 C18 115.6(3) . . ?
C16 C17 H17 122.2 . . ?
C18 C17 H17 122.2 . . ?
C17 C18 C19 122.9(3) . . ?
C17 C18 N7 118.3(3) . . ?
C19 C18 N7 118.8(3) . . ?
C18 C19 C14 120.1(3) . . ?
C18 C19 H19 120.0 . . ?
C14 C19 H19 120.0 . . ?
C21 C20 N3 107.4(3) . . ?
C21 C20 C12 130.3(3) . . ?
N3 C20 C12 122.2(3) . . ?
C20 C21 C22 107.7(3) . . ?
C20 C21 H21 126.2 . . ?
C22 C21 H21 126.2 . . ?
C23 C22 C21 107.8(3) . . ?
C23 C22 H22 126.1 . . ?
C21 C22 H22 126.1 . . ?
C27 C24 C23 111.6(3) . . ?
C27 C24 C25 109.8(3) . . ?
C23 C24 C25 109.5(3) . . ?
C27 C24 C26 108.6(3) . . ?
C23 C24 C26 108.2(3) . . ?
C25 C24 C26 109.1(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N4 C27 C28 106.7(3) . . ?
N4 C27 C24 123.0(3) . . ?
C28 C27 C24 130.3(3) . . ?
C27 C28 C29 107.9(3) . . ?
C27 C28 H28 126.0 . . ?
C29 C28 H28 126.0 . . ?
C30 C29 C28 108.1(3) . . ?
C30 C29 H29 125.9 . . ?
C28 C29 H29 125.9 . . ?
C29 C30 N4 106.9(3) . . ?
C29 C30 C31 129.6(3) . . ?
N4 C30 C31 123.4(3) . . ?
C1 C31 C30 111.9(3) . . ?
C1 C31 C33 109.2(3) . . ?
C30 C31 C33 112.5(3) . . ?
C1 C31 C32 108.7(3) . . ?
C30 C31 C32 108.1(3) . . ?
C33 C31 C32 106.2(2) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C38 C33 C34 119.1(3) . . ?
C38 C33 C31 118.8(3) . . ?
C34 C33 C31 122.0(3) . . ?
C35 C34 C33 118.8(3) . . ?
C35 C34 H34 120.6 . . ?
C33 C34 H34 120.6 . . ?
C36 C35 C34 123.4(3) . . ?
C36 C35 N6 117.4(3) . . ?
C34 C35 N6 119.1(3) . . ?
C37 C36 C35 116.0(3) . . ?
C37 C36 H36 122.0 . . ?
C35 C36 H36 122.0 . . ?
C36 C37 C38 123.0(3) . . ?
C36 C37 N5 118.9(3) . . ?
C38 C37 N5 118.1(3) . . ?
C37 C38 C33 119.6(3) . . ?
C37 C38 H38 120.2 . . ?
C33 C38 H38 120.2 . . ?
C40 C39 N9 106.5(3) . . ?
C40 C39 C69 130.6(3) . . ?
N9 C39 C69 122.8(3) . . ?
C39 C40 C41 108.3(3) . . ?
C39 C40 H40 125.9 . . ?
C41 C40 H40 125.9 . . ?
C42 C41 C40 107.6(3) . . ?
C42 C41 H41 126.2 . . ?
C40 C41 H41 126.2 . . ?
N9 C42 C41 107.0(3) . . ?
N9 C42 C43 122.8(3) . . ?
C41 C42 C43 130.0(3) . . ?
C46 C43 C42 111.5(3) . . ?
C46 C43 C45 109.0(3) . . ?
C42 C43 C45 108.9(3) . . ?
C46 C43 C44 109.6(3) . . ?
C42 C43 C44 109.2(3) . . ?
C45 C43 C44 108.6(3) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N12 C46 C47 107.0(3) . . ?
N12 C46 C43 122.2(3) . . ?
C47 C46 C43 130.9(3) . . ?
C46 C47 C48 107.3(3) . . ?
C46 C47 H47 126.4 . . ?
C48 C47 H47 126.4 . . ?
C49 C48 C47 108.7(3) . . ?
C49 C48 H48 125.7 . . ?
C47 C48 H48 125.7 . . ?
C48 C49 N12 106.5(3) . . ?
C48 C49 C50 131.2(3) . . ?
N12 C49 C50 122.2(3) . . ?
C49 C50 C58 113.0(3) . . ?
C49 C50 C52 110.1(3) . . ?
C58 C50 C52 110.4(3) . . ?
C49 C50 C51 108.4(3) . . ?
C58 C50 C51 108.3(3) . . ?
C52 C50 C51 106.3(3) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C57 C52 C53 118.8(3) . . ?
C57 C52 C50 120.8(3) . . ?
C53 C52 C50 120.1(3) . . ?
C54 C53 C52 119.3(3) . . ?
C54 C53 H53 120.4 . . ?
C52 C53 H53 120.4 . . ?
C55 C54 C53 123.3(3) . . ?
C55 C54 N15 118.2(3) . . ?
C53 C54 N15 118.5(3) . . ?
C56 C55 C54 116.0(3) . . ?
C56 C55 H55 122.0 . . ?
C54 C55 H55 122.0 . . ?
C55 C56 C57 123.0(4) . . ?
C55 C56 N16 119.1(3) . . ?
C57 C56 N16 117.9(3) . . ?
C52 C57 C56 119.6(3) . . ?
C52 C57 H57 120.2 . . ?
C56 C57 H57 120.2 . . ?
C59 C58 N11 106.9(3) . . ?
C59 C58 C50 130.4(3) . . ?
N11 C58 C50 122.4(3) . . ?
C58 C59 C60 107.6(3) . . ?
C58 C59 H59 126.2 . . ?
C60 C59 H59 126.2 . . ?
C61 C60 C59 108.3(3) . . ?
C61 C60 H60 125.8 . . ?
C59 C60 H60 125.8 . . ?
N11 C61 C60 106.7(3) . . ?
N11 C61 C62 122.6(3) . . ?
C60 C61 C62 130.3(3) . . ?
C65 C62 C61 113.7(3) . . ?
C65 C62 C63 108.1(3) . . ?
C61 C62 C63 108.6(3) . . ?
C65 C62 C64 109.2(3) . . ?
C61 C62 C64 109.0(3) . . ?
C63 C62 C64 108.2(3) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C66 C65 N10 106.9(3) . . ?
C66 C65 C62 129.7(3) . . ?
N10 C65 C62 123.3(3) . . ?
C65 C66 C67 107.8(3) . . ?
C65 C66 H66 126.1 . . ?
C67 C66 H66 126.1 . . ?
C68 C67 C66 108.1(3) . . ?
C68 C67 H67 125.9 . . ?
C66 C67 H67 125.9 . . ?
C67 C68 N10 106.9(3) . . ?
C67 C68 C69 129.7(3) . . ?
N10 C68 C69 123.4(3) . . ?
C39 C69 C68 111.6(3) . . ?
C39 C69 C71 111.1(3) . . ?
C68 C69 C71 111.0(3) . . ?
C39 C69 C70 108.1(3) . . ?
C68 C69 C70 108.7(3) . . ?
C71 C69 C70 106.1(2) . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C72 C71 C76 118.7(3) . . ?
C72 C71 C69 119.7(3) . . ?
C76 C71 C69 121.4(3) . . ?
C73 C72 C71 119.2(3) . . ?
C73 C72 H72 120.4 . . ?
C71 C72 H72 120.4 . . ?
C74 C73 C72 123.5(3) . . ?
C74 C73 N14 118.1(3) . . ?
C72 C73 N14 118.5(3) . . ?
C75 C74 C73 115.8(3) . . ?
C75 C74 H74 122.1 . . ?
C73 C74 H74 122.1 . . ?
C74 C75 C76 123.3(3) . . ?
C74 C75 N13 117.9(3) . . ?
C76 C75 N13 118.8(3) . . ?
C75 C76 C71 119.5(3) . . ?
C75 C76 H76 120.2 . . ?
C71 C76 H76 120.2 . . ?
C78 C77 N18 115.5(3) . . ?
C78 C77 H77A 108.4 . . ?
N18 C77 H77A 108.4 . . ?
C78 C77 H77B 108.4 . . ?
N18 C77 H77B 108.4 . . ?
H77A C77 H77B 107.5 . . ?
C77 C78 C79 110.6(3) . . ?
C77 C78 H78A 109.5 . . ?
C79 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
C79 C78 H78B 109.5 . . ?
H78A C78 H78B 108.1 . . ?
C80 C79 C78 112.2(3) . . ?
C80 C79 H79A 109.2 . . ?
C78 C79 H79A 109.2 . . ?
C80 C79 H79B 109.2 . . ?
C78 C79 H79B 109.2 . . ?
H79A C79 H79B 107.9 . . ?
C79 C80 H80A 109.5 . . ?
C79 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C79 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C82 C81 N18 115.5(3) . . ?
C82 C81 H81A 108.4 . . ?
N18 C81 H81A 108.4 . . ?
C82 C81 H81B 108.4 . . ?
N18 C81 H81B 108.4 . . ?
H81A C81 H81B 107.5 . . ?
C81 C82 C83 108.5(3) . . ?
C81 C82 H82A 110.0 . . ?
C83 C82 H82A 110.0 . . ?
C81 C82 H82B 110.0 . . ?
C83 C82 H82B 110.0 . . ?
H82A C82 H82B 108.4 . . ?
C84 C83 C82 111.8(3) . . ?
C84 C83 H83A 109.2 . . ?
C82 C83 H83A 109.2 . . ?
C84 C83 H83B 109.2 . . ?
C82 C83 H83B 109.2 . . ?
H83A C83 H83B 107.9 . . ?
C83 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C83 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C86 C85 N18 116.1(3) . . ?
C86 C85 H85A 108.3 . . ?
N18 C85 H85A 108.3 . . ?
C86 C85 H85B 108.3 . . ?
N18 C85 H85B 108.3 . . ?
H85A C85 H85B 107.4 . . ?
C85 C86 C87 111.0(3) . . ?
C85 C86 H86A 109.4 . . ?
C87 C86 H86A 109.4 . . ?
C85 C86 H86B 109.4 . . ?
C87 C86 H86B 109.4 . . ?
H86A C86 H86B 108.0 . . ?
C88 C87 C86 117.1(4) . . ?
C88 C87 H87A 108.0 . . ?
C86 C87 H87A 108.0 . . ?
C88 C87 H87B 108.0 . . ?
C86 C87 H87B 108.0 . . ?
H87A C87 H87B 107.3 . . ?
C87 C88 H88A 109.5 . . ?
C87 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
N18 C89 C90 115.4(3) . . ?
N18 C89 H89A 108.4 . . ?
C90 C89 H89A 108.4 . . ?
N18 C89 H89B 108.4 . . ?
C90 C89 H89B 108.4 . . ?
H89A C89 H89B 107.5 . . ?
C89 C90 C91 109.3(3) . . ?
C89 C90 H90A 109.8 . . ?
C91 C90 H90A 109.8 . . ?
C89 C90 H90B 109.8 . . ?
C91 C90 H90B 109.8 . . ?
H90A C90 H90B 108.3 . . ?
C92 C91 C90 113.6(3) . . ?
C92 C91 H91A 108.8 . . ?
C90 C91 H91A 108.8 . . ?
C92 C91 H91B 108.8 . . ?
C90 C91 H91B 108.8 . . ?
H91A C91 H91B 107.7 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C94 C93 N20 116.9(4) . . ?
C94 C93 H93A 108.1 . . ?
N20 C93 H93A 108.1 . . ?
C94 C93 H93B 108.1 . . ?
N20 C93 H93B 108.1 . . ?
H93A C93 H93B 107.3 . . ?
C93 C94 C95 111.8(4) . . ?
C93 C94 H94A 109.3 . . ?
C95 C94 H94A 109.3 . . ?
C93 C94 H94B 109.3 . . ?
C95 C94 H94B 109.3 . . ?
H94A C94 H94B 107.9 . . ?
C96 C95 C94 114.7(5) . . ?
C96 C95 H95A 108.6 . . ?
C94 C95 H95A 108.6 . . ?
C96 C95 H95B 108.6 . . ?
C94 C95 H95B 108.6 . . ?
H95A C95 H95B 107.6 . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
C98 C97 N20 116.7(4) . . ?
C98 C97 H97A 108.1 . . ?
N20 C97 H97A 108.1 . . ?
C98 C97 H97B 108.1 . . ?
N20 C97 H97B 108.1 . . ?
H97A C97 H97B 107.3 . . ?
C99 C98 C97 111.3(4) . . ?
C99 C98 H98A 109.4 . . ?
C97 C98 H98A 109.4 . . ?
C99 C98 H98B 109.4 . . ?
C97 C98 H98B 109.4 . . ?
H98A C98 H98B 108.0 . . ?
C100 C99 C98 116.4(4) . . ?
C100 C99 H99A 108.2 . . ?
C98 C99 H99A 108.2 . . ?
C100 C99 H99B 108.2 . . ?
C98 C99 H99B 108.2 . . ?
H99A C99 H99B 107.3 . . ?
C99 C100 H10A 109.5 . . ?
C99 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
C99 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C102 C101 N20 116.9(4) . . ?
C102 C101 H10D 108.1 . . ?
N20 C101 H10D 108.1 . . ?
C102 C101 H10E 108.1 . . ?
N20 C101 H10E 108.1 . . ?
H10D C101 H10E 107.3 . . ?
C101 C102 C103 110.2(5) . . ?
C101 C102 H10F 109.6 . . ?
C103 C102 H10F 109.6 . . ?
C101 C102 H10G 109.6 . . ?
C103 C102 H10G 109.6 . . ?
H10F C102 H10G 108.1 . . ?
C104 C103 C102 113.2(6) . . ?
C104 C103 H10H 108.9 . . ?
C102 C103 H10H 108.9 . . ?
C104 C103 H10I 108.9 . . ?
C102 C103 H10I 108.9 . . ?
H10H C103 H10I 107.8 . . ?
C103 C104 H10J 109.5 . . ?
C103 C104 H10K 109.5 . . ?
H10J C104 H10K 109.5 . . ?
C103 C104 H10L 109.5 . . ?
H10J C104 H10L 109.5 . . ?
H10K C104 H10L 109.5 . . ?
C106 C105 N20 116.7(4) . . ?
C106 C105 H10M 108.1 . . ?
N20 C105 H10M 108.1 . . ?
C106 C105 H10N 108.1 . . ?
N20 C105 H10N 108.1 . . ?
H10M C105 H10N 107.3 . . ?
C105 C106 C107 111.7(5) . . ?
C105 C106 H10O 109.3 . . ?
C107 C106 H10O 109.3 . . ?
C105 C106 H10P 109.3 . . ?
C107 C106 H10P 109.3 . . ?
H10O C106 H10P 107.9 . . ?
C108 C107 C106 117.7(6) . . ?
C108 C107 H10Q 107.9 . . ?
C106 C107 H10Q 107.9 . . ?
C108 C107 H10R 107.9 . . ?
C106 C107 H10R 107.9 . . ?
H10Q C107 H10R 107.2 . . ?
C107 C108 H10S 109.5 . . ?
C107 C108 H10T 109.5 . . ?
H10S C108 H10T 109.5 . . ?
C107 C108 H10U 109.5 . . ?
H10S C108 H10U 109.5 . . ?
H10T C108 H10U 109.5 . . ?
C110 C109 N19 114.2(3) . . ?
C110 C109 H10V 108.7 . . ?
N19 C109 H10V 108.7 . . ?
C110 C109 H10W 108.7 . . ?
N19 C109 H10W 108.7 . . ?
H10V C109 H10W 107.6 . . ?
C109 C110 C111 111.0(4) . . ?
C109 C110 H11A 109.4 . . ?
C111 C110 H11A 109.4 . . ?
C109 C110 H11B 109.4 . . ?
C111 C110 H11B 109.4 . . ?
H11A C110 H11B 108.0 . . ?
C110 C111 C112 111.5(5) . . ?
C110 C111 H11C 109.3 . . ?
C112 C111 H11C 109.3 . . ?
C110 C111 H11D 109.3 . . ?
C112 C111 H11D 109.3 . . ?
H11C C111 H11D 108.0 . . ?
C111 C112 H11E 109.5 . . ?
C111 C112 H11F 109.5 . . ?
H11E C112 H11F 109.5 . . ?
C111 C112 H11G 109.5 . . ?
H11E C112 H11G 109.5 . . ?
H11F C112 H11G 109.5 . . ?
C114 C113 N19 116.6(3) . . ?
C114 C113 H11H 108.2 . . ?
N19 C113 H11H 108.2 . . ?
C114 C113 H11I 108.2 . . ?
N19 C113 H11I 108.2 . . ?
H11H C113 H11I 107.3 . . ?
C113 C114 C115 108.8(3) . . ?
C113 C114 H11J 109.9 . . ?
C115 C114 H11J 109.9 . . ?
C113 C114 H11K 109.9 . . ?
C115 C114 H11K 109.9 . . ?
H11J C114 H11K 108.3 . . ?
C116 C115 C114 113.0(4) . . ?
C116 C115 H11L 109.0 . . ?
C114 C115 H11L 109.0 . . ?
C116 C115 H11M 109.0 . . ?
C114 C115 H11M 109.0 . . ?
H11L C115 H11M 107.8 . . ?
C115 C116 H11N 109.5 . . ?
C115 C116 H11O 109.5 . . ?
H11N C116 H11O 109.5 . . ?
C115 C116 H11P 109.5 . . ?
H11N C116 H11P 109.5 . . ?
H11O C116 H11P 109.5 . . ?
C118 C117 N19 115.1(3) . . ?
C118 C117 H11Q 108.5 . . ?
N19 C117 H11Q 108.5 . . ?
C118 C117 H11R 108.5 . . ?
N19 C117 H11R 108.5 . . ?
H11Q C117 H11R 107.5 . . ?
C119 C118 C117 111.4(4) . . ?
C119 C118 H11S 109.4 . . ?
C117 C118 H11S 109.4 . . ?
C119 C118 H11T 109.4 . . ?
C117 C118 H11T 109.4 . . ?
H11S C118 H11T 108.0 . . ?
C118 C119 C120 113.7(4) . . ?
C118 C119 H11U 108.8 . . ?
C120 C119 H11U 108.8 . . ?
C118 C119 H11V 108.8 . . ?
C120 C119 H11V 108.8 . . ?
H11U C119 H11V 107.7 . . ?
C119 C120 H12A 109.5 . . ?
C119 C120 H12B 109.5 . . ?
H12A C120 H12B 109.5 . . ?
C119 C120 H12C 109.5 . . ?
H12A C120 H12C 109.5 . . ?
H12B C120 H12C 109.5 . . ?
N19 C121 C122 115.7(3) . . ?
N19 C121 H12D 108.3 . . ?
C122 C121 H12D 108.3 . . ?
N19 C121 H12E 108.3 . . ?
C122 C121 H12E 108.3 . . ?
H12D C121 H12E 107.4 . . ?
C123 C122 C121 111.4(3) . . ?
C123 C122 H12F 109.4 . . ?
C121 C122 H12F 109.4 . . ?
C123 C122 H12G 109.4 . . ?
C121 C122 H12G 109.4 . . ?
H12F C122 H12G 108.0 . . ?
C124 C123 C122 112.1(5) . . ?
C124 C123 H12H 109.2 . . ?
C122 C123 H12H 109.2 . . ?
C124 C123 H12I 109.2 . . ?
C122 C123 H12I 109.2 . . ?
H12H C123 H12I 107.9 . . ?
C123 C124 H12J 109.5 . . ?
C123 C124 H12K 109.5 . . ?
H12J C124 H12K 109.5 . . ?
C123 C124 H12L 109.5 . . ?
H12J C124 H12L 109.5 . . ?
H12K C124 H12L 109.5 . . ?
N17 C125 C126 115.8(3) . . ?
N17 C125 H12M 108.3 . . ?
C126 C125 H12M 108.3 . . ?
N17 C125 H12N 108.3 . . ?
C126 C125 H12N 108.3 . . ?
H12M C125 H12N 107.4 . . ?
C127 C126 C125 112.0(3) . . ?
C127 C126 H12O 109.2 . . ?
C125 C126 H12O 109.2 . . ?
C127 C126 H12P 109.2 . . ?
C125 C126 H12P 109.2 . . ?
H12O C126 H12P 107.9 . . ?
C128 C127 C126 110.9(3) . . ?
C127 C128 H12Q 109.5 . . ?
C127 C128 H12R 109.5 . . ?
H12Q C128 H12R 109.5 . . ?
C127 C128 H12S 109.5 . . ?
H12Q C128 H12S 109.5 . . ?
H12R C128 H12S 109.5 . . ?
C130 C129 N17 116.8(3) . . ?
C130 C129 H12T 108.1 . . ?
N17 C129 H12T 108.1 . . ?
C130 C129 H12U 108.1 . . ?
N17 C129 H12U 108.1 . . ?
H12T C129 H12U 107.3 . . ?
C129 C130 C131 110.1(3) . . ?
C129 C130 H13D 109.6 . . ?
C131 C130 H13D 109.6 . . ?
C129 C130 H13E 109.6 . . ?
C131 C130 H13E 109.6 . . ?
H13D C130 H13E 108.2 . . ?
C132 C131 C130 113.4(3) . . ?
C132 C131 H13F 108.9 . . ?
C130 C131 H13F 108.9 . . ?
C132 C131 H13G 108.9 . . ?
C130 C131 H13G 108.9 . . ?
H13F C131 H13G 107.7 . . ?
C131 C132 H13H 109.5 . . ?
C131 C132 H131 109.5 . . ?
H13H C132 H131 109.5 . . ?
C131 C132 H13J 109.5 . . ?
H13H C132 H13J 109.5 . . ?
H131 C132 H13J 109.5 . . ?
C134 C133 N17 115.8(3) . . ?
C134 C133 H13K 108.3 . . ?
N17 C133 H13K 108.3 . . ?
C134 C133 H13L 108.3 . . ?
N17 C133 H13L 108.3 . . ?
H13K C133 H13L 107.4 . . ?
C135 C134 C133 109.8(3) . . ?
C135 C134 H13M 109.7 . . ?
C133 C134 H13M 109.7 . . ?
C135 C134 H13N 109.7 . . ?
C133 C134 H13N 109.7 . . ?
H13M C134 H13N 108.2 . . ?
C136 C135 C134 113.7(3) . . ?
C136 C135 H13O 108.8 . . ?
C134 C135 H13O 108.8 . . ?
C136 C135 H13P 108.8 . . ?
C134 C135 H13P 108.8 . . ?
H13O C135 H13P 107.7 . . ?
C135 C136 H13Q 109.5 . . ?
C135 C136 H13R 109.5 . . ?
H13Q C136 H13R 109.5 . . ?
C135 C136 H13S 109.5 . . ?
H13Q C136 H13S 109.5 . . ?
H13R C136 H13S 109.5 . . ?
C138 C137 N17 116.2(3) . . ?
C138 C137 H13T 108.2 . . ?
N17 C137 H13T 108.2 . . ?
C138 C137 H13U 108.2 . . ?
N17 C137 H13U 108.2 . . ?
H13T C137 H13U 107.4 . . ?
C139 C138 C137 116.1(3) . . ?
C139 C138 H13V 108.3 . . ?
C137 C138 H13V 108.3 . . ?
C139 C138 H13W 108.3 . . ?
C137 C138 H13W 108.3 . . ?
H13V C138 H13W 107.4 . . ?
C138 C139 C140 112.1(4) . . ?
C138 C139 H13$ 109.2 . . ?
C140 C139 H13$ 109.2 . . ?
C138 C139 H13I 109.2 . . ?
C140 C139 H13I 109.2 . . ?
H13$ C139 H13I 107.9 . . ?
C139 C140 H14A 109.5 . . ?
C139 C140 H14B 109.5 . . ?
H14A C140 H14B 109.5 . . ?
C139 C140 H14C 109.5 . . ?
H14A C140 H14C 109.5 . . ?
H14B C140 H14C 109.5 . . ?
Cl1 C1A Cl3 110.2(2) . . ?
Cl1 C1A Cl2 109.4(2) . . ?
Cl3 C1A Cl2 111.4(2) . . ?
Cl1 C1A H1A 108.6 . . ?
Cl3 C1A H1A 108.6 . . ?
Cl2 C1A H1A 108.6 . . ?
Cl6 C2A Cl4 114.4(3) . . ?
Cl6 C2A Cl5 110.8(3) . . ?
Cl4 C2A Cl5 109.8(3) . . ?
Cl6 C2A H2A 107.2 . . ?
Cl4 C2A H2A 107.2 . . ?
Cl5 C2A H2A 107.2 . . ?
C4 N1 C1 110.0(3) . . ?
C4 N1 H1 125.0 . . ?
C1 N1 H1 125.0 . . ?
C8 N2 C11 110.6(3) . . ?
C8 N2 H2E 124.7 . . ?
C11 N2 H2E 124.7 . . ?
C20 N3 C23 110.2(3) . . ?
C20 N3 H3A 124.9 . . ?
C23 N3 H3A 124.9 . . ?
C27 N4 C30 110.3(3) . . ?
C27 N4 H4 124.8 . . ?
C30 N4 H4 124.8 . . ?
O1 N5 O2 123.4(3) . . ?
O1 N5 C37 118.4(3) . . ?
O2 N5 C37 118.2(3) . . ?
O3 N6 O4 124.0(3) . . ?
O3 N6 C35 118.2(3) . . ?
O4 N6 C35 117.8(3) . . ?
O5 N7 O6 123.5(3) . . ?
O5 N7 C18 118.1(3) . . ?
O6 N7 C18 118.4(3) . . ?
O7 N8 O8 123.4(3) . . ?
O7 N8 C16 118.8(3) . . ?
O8 N8 C16 117.8(3) . . ?
C42 N9 C39 110.6(3) . . ?
C42 N9 H9A 124.7 . . ?
C39 N9 H9A 124.7 . . ?
C65 N10 C68 110.2(3) . . ?
C65 N10 H101 124.9 . . ?
C68 N10 H101 124.9 . . ?
C61 N11 C58 110.4(3) . . ?
C61 N11 H11 124.8 . . ?
C58 N11 H11 124.8 . . ?
C46 N12 C49 110.6(3) . . ?
C46 N12 H12 124.7 . . ?
C49 N12 H12 124.7 . . ?
O9 N13 O10 123.7(3) . . ?
O9 N13 C75 118.1(3) . . ?
O10 N13 C75 118.2(3) . . ?
O12 N14 O11 123.6(3) . . ?
O12 N14 C73 118.3(3) . . ?
O11 N14 C73 118.1(3) . . ?
O15 N15 O16 124.0(3) . . ?
O15 N15 C54 117.7(3) . . ?
O16 N15 C54 118.2(3) . . ?
O13 N16 O14 123.7(4) . . ?
O13 N16 C56 118.1(3) . . ?
O14 N16 C56 118.2(3) . . ?
C125 N17 C133 110.1(3) . . ?
C125 N17 C137 108.1(3) . . ?
C133 N17 C137 110.9(3) . . ?
C125 N17 C129 110.4(3) . . ?
C133 N17 C129 105.4(2) . . ?
C137 N17 C129 111.9(3) . . ?
C89 N18 C81 108.7(2) . . ?
C89 N18 C77 111.1(2) . . ?
C81 N18 C77 109.3(2) . . ?
C89 N18 C85 108.1(2) . . ?
C81 N18 C85 110.9(2) . . ?
C77 N18 C85 108.7(2) . . ?
C121 N19 C113 105.8(3) . . ?
C121 N19 C117 110.9(3) . . ?
C113 N19 C117 110.9(3) . . ?
C121 N19 C109 112.0(3) . . ?
C113 N19 C109 111.1(3) . . ?
C117 N19 C109 106.3(3) . . ?
C105 N20 C101 112.4(4) . . ?
C105 N20 C93 109.1(3) . . ?
C101 N20 C93 107.7(3) . . ?
C105 N20 C97 109.7(3) . . ?
C101 N20 C97 107.8(3) . . ?
C93 N20 C97 110.1(4) . . ?
P1 O19 H19A 109.5 . . ?
P1 O20 H20 109.5 . . ?
P2 O21 H21A 109.5 . . ?
P2 O23 H23 109.5 . . ?
P3 O26 H26 109.5 . . ?
P3 O27 H27 109.5 . . ?
P4 O29 H29A 109.5 . . ?
P4 O31 H31 109.5 . . ?
O19 P1 O17 116.04(13) . . ?
O19 P1 O18 111.19(12) . . ?
O17 P1 O18 106.96(12) . . ?
O19 P1 O20 109.36(13) . . ?
O17 P1 O20 105.32(12) . . ?
O18 P1 O20 107.53(13) . . ?
O23 P2 O21 115.40(14) . . ?
O23 P2 O24 110.24(14) . . ?
O21 P2 O24 108.86(14) . . ?
O23 P2 O22 109.66(14) . . ?
O21 P2 O22 109.55(16) . . ?
O24 P2 O22 102.32(14) . . ?
O26 P3 O25 115.81(13) . . ?
O26 P3 O28 110.99(13) . . ?
O25 P3 O28 107.20(13) . . ?
O26 P3 O27 109.87(13) . . ?
O25 P3 O27 105.08(12) . . ?
O28 P3 O27 107.42(13) . . ?
O29 P4 O31 115.36(15) . . ?
O29 P4 O32 109.81(14) . . ?
O31 P4 O32 108.97(13) . . ?
O29 P4 O30 109.34(15) . . ?
O31 P4 O30 109.85(16) . . ?
O32 P4 O30 102.75(14) . . ?
O1B C1F H1F1 109.5 . . ?
O1B C1F H1F2 109.5 . . ?
H1F1 C1F H1F2 109.5 . . ?
O1B C1F H1F3 109.5 . . ?
H1F1 C1F H1F3 109.5 . . ?
H1F2 C1F H1F3 109.5 . . ?
C1F O1B H1B 109.5 . . ?
O2B C1B H1B1 109.5 . . ?
O2B C1B H1B2 109.5 . . ?
H1B1 C1B H1B2 109.5 . . ?
O2B C1B H1B3 109.5 . . ?
H1B1 C1B H1B3 109.5 . . ?
H1B2 C1B H1B3 109.5 . . ?
C1B O2B H2B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         1.293
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.079
####################################################################### 
# 
# 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_TBAHCO3-DNPC4P
_database_code_depnum_ccdc_archive 'CCDC 1482089'
_audit_update_record             
;
2016-05-26 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Cis-dinitrophenyl-calix[4]pyrrole-tetraethylammonium hydrogencarbonate 
;
_chemical_name_common            DNP-Calix[4]pyrrole-TEAHCO3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H60 Cl6 N10 O14'
_chemical_formula_weight         1333.86

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.224(6)
_cell_length_b                   13.636(8)
_cell_length_c                   22.374(13)
_cell_angle_alpha                101.011(8)
_cell_angle_beta                 98.751(9)
_cell_angle_gamma                91.381(11)
_cell_volume                     3317(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    7745
_cell_measurement_theta_min      0.9392
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9649
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41120
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11463
_reflns_number_gt                9316
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_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)+(0.0800P)²+4.6819P] 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_number_reflns         11463
_refine_ls_number_parameters     842
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.1123
_refine_ls_wR_factor_ref         0.2644
_refine_ls_wR_factor_gt          0.2536
_refine_ls_goodness_of_fit_ref   1.354
_refine_ls_restrained_S_all      1.365
_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 0.8230(4) 0.8420(3) 0.6152(2) 0.0303(9) Uani 1 1 d . . .
C2 C 0.8903(4) 0.9088(3) 0.5945(2) 0.0325(10) Uani 1 1 d . . .
H2 H 0.9353 0.8939 0.5615 0.039 Uiso 1 1 calc R . .
C3 C 0.8811(4) 1.0054(3) 0.6311(2) 0.0311(10) Uani 1 1 d . . .
H3 H 0.9195 1.0660 0.6270 0.037 Uiso 1 1 calc R . .
C4 C 0.8079(4) 0.9954(3) 0.6729(2) 0.0271(9) Uani 1 1 d . . .
C5 C 0.7748(4) 1.0714(3) 0.7268(2) 0.0298(9) Uani 1 1 d . . .
C6 C 0.8177(4) 1.0353(3) 0.7882(2) 0.0363(10) Uani 1 1 d . . .
H6A H 0.8009 1.0855 0.8231 0.054 Uiso 1 1 calc R . .
H6B H 0.9046 1.0259 0.7925 0.054 Uiso 1 1 calc R . .
H6C H 0.7745 0.9717 0.7877 0.054 Uiso 1 1 calc R . .
C7 C 0.8411(4) 1.1723(3) 0.7299(2) 0.0372(11) Uani 1 1 d . . .
H7A H 0.8174 1.1953 0.6911 0.056 Uiso 1 1 calc R . .
H7B H 0.9285 1.1646 0.7365 0.056 Uiso 1 1 calc R . .
H7C H 0.8200 1.2215 0.7642 0.056 Uiso 1 1 calc R . .
C8 C 0.6404(4) 1.0862(3) 0.72047(19) 0.0272(9) Uani 1 1 d . . .
C9 C 0.5753(4) 1.1690(3) 0.7133(2) 0.0369(11) Uani 1 1 d . . .
H9 H 0.6077 1.2319 0.7092 0.044 Uiso 1 1 calc R . .
C10 C 0.4518(4) 1.1438(3) 0.7130(2) 0.0393(11) Uani 1 1 d . . .
H10 H 0.3871 1.1870 0.7091 0.047 Uiso 1 1 calc R . .
C11 C 0.4428(4) 1.0458(3) 0.7195(2) 0.0333(10) Uani 1 1 d . . .
C12 C 0.3326(4) 0.9788(3) 0.7215(2) 0.0373(11) Uani 1 1 d . . .
C13 C 0.2240(4) 1.0457(4) 0.7321(3) 0.0538(15) Uani 1 1 d . . .
H13A H 0.2025 1.0783 0.6968 0.081 Uiso 1 1 calc R . .
H13B H 0.2465 1.0968 0.7697 0.081 Uiso 1 1 calc R . .
H13C H 0.1546 1.0041 0.7364 0.081 Uiso 1 1 calc R . .
C14 C 0.3557(4) 0.9218(3) 0.7740(2) 0.0359(11) Uani 1 1 d . . .
C15 C 0.4365(4) 0.9598(3) 0.8282(2) 0.0400(11) Uani 1 1 d . . .
H15 H 0.4786 1.0229 0.8332 0.048 Uiso 1 1 calc R . .
C16 C 0.4543(5) 0.9047(4) 0.8744(3) 0.0463(12) Uani 1 1 d . . .
C17 C 0.3980(5) 0.8106(4) 0.8701(3) 0.0466(12) Uani 1 1 d . . .
H17 H 0.4132 0.7732 0.9019 0.056 Uiso 1 1 calc R . .
C18 C 0.3192(5) 0.7759(4) 0.8167(3) 0.0464(13) Uani 1 1 d . . .
C19 C 0.2955(4) 0.8292(4) 0.7699(3) 0.0418(12) Uani 1 1 d . . .
H19 H 0.2376 0.8026 0.7345 0.050 Uiso 1 1 calc R . .
C20 C 0.2990(4) 0.9044(3) 0.6612(2) 0.0348(10) Uani 1 1 d . . .
C21 C 0.2011(4) 0.8976(3) 0.6154(2) 0.0409(12) Uani 1 1 d . . .
H21 H 0.1399 0.9443 0.6133 0.049 Uiso 1 1 calc R . .
C22 C 0.2075(4) 0.8082(3) 0.5717(2) 0.0370(11) Uani 1 1 d . . .
H22 H 0.1520 0.7850 0.5348 0.044 Uiso 1 1 calc R . .
C23 C 0.3085(4) 0.7610(3) 0.5923(2) 0.0306(9) Uani 1 1 d . . .
C24 C 0.3537(4) 0.6581(3) 0.5682(2) 0.0316(10) Uani 1 1 d . . .
C25 C 0.3628(4) 0.5959(3) 0.6194(2) 0.0366(10) Uani 1 1 d . . .
H25A H 0.3899 0.5295 0.6038 0.055 Uiso 1 1 calc R . .
H25B H 0.2834 0.5891 0.6318 0.055 Uiso 1 1 calc R . .
H25C H 0.4208 0.6298 0.6550 0.055 Uiso 1 1 calc R . .
C26 C 0.2629(4) 0.6047(4) 0.5128(2) 0.0408(11) Uani 1 1 d . . .
H26A H 0.2571 0.6436 0.4800 0.061 Uiso 1 1 calc R . .
H26B H 0.1836 0.5982 0.5253 0.061 Uiso 1 1 calc R . .
H26C H 0.2899 0.5380 0.4976 0.061 Uiso 1 1 calc R . .
C27 C 0.4762(4) 0.6676(3) 0.5481(2) 0.0292(9) Uani 1 1 d . . .
C28 C 0.5116(4) 0.6407(3) 0.4913(2) 0.0335(10) Uani 1 1 d . . .
H28 H 0.4601 0.6144 0.4536 0.040 Uiso 1 1 calc R . .
C29 C 0.6386(4) 0.6594(3) 0.4990(2) 0.0326(10) Uani 1 1 d . . .
H29 H 0.6873 0.6474 0.4674 0.039 Uiso 1 1 calc R . .
C30 C 0.6785(4) 0.6984(3) 0.5610(2) 0.0292(9) Uani 1 1 d . . .
C31 C 0.8048(4) 0.7285(3) 0.5964(2) 0.0313(10) Uani 1 1 d . . .
C32 C 0.8979(4) 0.6889(3) 0.5545(2) 0.0382(11) Uani 1 1 d . . .
H32A H 0.8864 0.6160 0.5420 0.057 Uiso 1 1 calc R . .
H32B H 0.9797 0.7067 0.5771 0.057 Uiso 1 1 calc R . .
H32C H 0.8865 0.7190 0.5177 0.057 Uiso 1 1 calc R . .
C33 C 0.8260(4) 0.6804(3) 0.6538(2) 0.0305(9) Uani 1 1 d . . .
C34 C 0.9029(4) 0.7280(3) 0.7074(2) 0.0329(10) Uani 1 1 d . . .
H34 H 0.9440 0.7903 0.7087 0.039 Uiso 1 1 calc R . .
C35 C 0.9181(4) 0.6830(3) 0.7584(2) 0.0374(11) Uani 1 1 d . . .
C36 C 0.8640(4) 0.5909(3) 0.7595(2) 0.0390(11) Uani 1 1 d . . .
H36 H 0.8747 0.5617 0.7951 0.047 Uiso 1 1 calc R . .
C37 C 0.7930(4) 0.5449(3) 0.7045(2) 0.0358(10) Uani 1 1 d . . .
C38 C 0.7726(4) 0.5868(3) 0.6528(2) 0.0332(10) Uani 1 1 d . . .
H38 H 0.7223 0.5519 0.6166 0.040 Uiso 1 1 calc R . .
N1 N 0.7710(3) 0.8955(2) 0.66298(17) 0.0283(8) Uani 1 1 d . . .
H1 H 0.7220 0.8696 0.6837 0.034 Uiso 1 1 calc R . .
N2 N 0.5784(3) 0.7037(2) 0.59048(17) 0.0274(8) Uani 1 1 d . . .
H2A H 0.5795 0.7266 0.6301 0.033 Uiso 1 1 calc R . .
N3 N 0.3645(3) 0.8214(2) 0.64638(17) 0.0291(8) Uani 1 1 d . . .
H3A H 0.4324 0.8088 0.6683 0.035 Uiso 1 1 calc R . .
N4 N 0.5577(3) 1.0107(2) 0.72360(16) 0.0274(8) Uani 1 1 d . . .
H4 H 0.5757 0.9496 0.7276 0.033 Uiso 1 1 calc R . .
N5 N 0.5424(5) 0.9452(4) 0.9301(2) 0.0620(13) Uani 1 1 d . . .
N6 N 0.2600(5) 0.6730(4) 0.8054(3) 0.0575(13) Uani 1 1 d . . .
N7 N 0.9929(4) 0.7360(3) 0.8160(2) 0.0498(11) Uani 1 1 d . . .
N8 N 0.7338(4) 0.4459(3) 0.7027(2) 0.0466(10) Uani 1 1 d . . .
O1 O 0.1977(4) 0.6402(3) 0.7559(2) 0.0637(11) Uani 1 1 d . . .
O2 O 0.2822(5) 0.6268(4) 0.8474(3) 0.0843(15) Uani 1 1 d . . .
O3 O 0.5487(5) 0.9004(4) 0.9735(2) 0.0840(15) Uani 1 1 d . . .
O4 O 0.6040(4) 1.0202(3) 0.9303(2) 0.0709(12) Uani 1 1 d . . .
O5 O 0.6716(5) 0.4042(3) 0.6546(2) 0.0773(14) Uani 1 1 d . . .
O6 O 0.7496(4) 0.4109(3) 0.74950(18) 0.0543(10) Uani 1 1 d . . .
O7 O 1.0091(5) 0.6958(3) 0.8597(2) 0.0778(14) Uani 1 1 d . . .
O8 O 1.0369(3) 0.8207(3) 0.81613(18) 0.0520(9) Uani 1 1 d . . .
C39 C 0.6224(4) 0.7694(3) 0.7673(2) 0.0313(10) Uani 1 1 d . . .
O9 O 0.5976(2) 0.8021(2) 0.71779(14) 0.0301(7) Uani 1 1 d . . .
O10 O 0.5634(3) 0.6832(2) 0.76820(15) 0.0386(8) Uani 1 1 d . . .
H10A H 0.5847 0.6666 0.8024 0.058 Uiso 1 1 calc R . .
O11 O 0.6966(3) 0.8111(2) 0.81350(15) 0.0428(8) Uani 1 1 d . . .
C40 C 0.6621(6) 0.6829(4) 0.9247(3) 0.0588(15) Uani 1 1 d . . .
O12 O 0.5898(4) 0.6456(3) 0.8772(2) 0.0731(13) Uani 1 1 d . . .
O13 O 0.7408(4) 0.7574(3) 0.9216(2) 0.0728(13) Uani 1 1 d . . .
H13 H 0.7281 0.7711 0.8862 0.109 Uiso 1 1 calc R . .
O14 O 0.6711(5) 0.6530(4) 0.9750(2) 0.0778(13) Uani 1 1 d . . .
N9 N 0.4429(6) 0.6495(4) 0.1053(3) 0.0803(18) Uani 1 1 d . . .
C41 C 0.3198(6) 0.6565(5) 0.1255(3) 0.0647(16) Uani 1 1 d . . .
H41A H 0.3314 0.6800 0.1708 0.078 Uiso 1 1 calc R . .
H41B H 0.2756 0.7076 0.1064 0.078 Uiso 1 1 calc R . .
C42 C 0.2421(7) 0.5594(6) 0.1091(3) 0.081(2) Uani 1 1 d . . .
H42A H 0.2371 0.5314 0.0650 0.122 Uiso 1 1 calc R . .
H42B H 0.1609 0.5726 0.1185 0.122 Uiso 1 1 calc R . .
H42C H 0.2782 0.5116 0.1332 0.122 Uiso 1 1 calc R . .
C43 C 0.5200(7) 0.5739(5) 0.1340(4) 0.083(2) Uani 1 1 d . . .
H43A H 0.4794 0.5066 0.1185 0.099 Uiso 1 1 calc R . .
H43B H 0.5984 0.5730 0.1188 0.099 Uiso 1 1 calc R . .
C44 C 0.5448(7) 0.5911(5) 0.2027(4) 0.086(2) Uani 1 1 d . . .
H44A H 0.5868 0.6568 0.2189 0.129 Uiso 1 1 calc R . .
H44B H 0.5955 0.5390 0.2156 0.129 Uiso 1 1 calc R . .
H44C H 0.4684 0.5889 0.2186 0.129 Uiso 1 1 calc R . .
C45 C 0.4988(8) 0.7544(5) 0.1244(3) 0.081(2) Uani 1 1 d . . .
H45A H 0.4983 0.7776 0.1691 0.098 Uiso 1 1 calc R . .
H45B H 0.4483 0.7987 0.1022 0.098 Uiso 1 1 calc R . .
C46 C 0.6283(9) 0.7649(6) 0.1119(4) 0.104(3) Uani 1 1 d . . .
H46A H 0.6793 0.7216 0.1340 0.156 Uiso 1 1 calc R . .
H46B H 0.6590 0.8346 0.1263 0.156 Uiso 1 1 calc R . .
H46C H 0.6294 0.7451 0.0676 0.156 Uiso 1 1 calc R . .
C47 C 0.4274(12) 0.6137(7) 0.0353(4) 0.124(4) Uani 1 1 d . . .
H47A H 0.5085 0.6085 0.0232 0.149 Uiso 1 1 calc R . .
H47B H 0.3877 0.5456 0.0249 0.149 Uiso 1 1 calc R . .
C48 C 0.3589(14) 0.6753(8) -0.0010(4) 0.150(6) Uani 1 1 d . . .
H48A H 0.2746 0.6729 0.0056 0.225 Uiso 1 1 calc R . .
H48B H 0.3627 0.6506 -0.0448 0.225 Uiso 1 1 calc R . .
H48C H 0.3926 0.7445 0.0113 0.225 Uiso 1 1 calc R . .
C1E C 0.8721(5) 0.5882(5) 0.3235(3) 0.0564(14) Uani 1 1 d . . .
H1E H 0.8223 0.5250 0.3046 0.068 Uiso 1 1 calc R . .
Cl1 Cl 0.7744(2) 0.67591(19) 0.35383(10) 0.1044(8) Uani 1 1 d . . .
Cl2 Cl 0.9330(2) 0.62720(15) 0.26476(11) 0.0951(7) Uani 1 1 d . . .
Cl3 Cl 0.9756(3) 0.5622(3) 0.38320(12) 0.1438(13) Uani 1 1 d . . .
C2E C 0.8980(9) 0.6393(7) 0.0598(4) 0.104(3) Uani 1 1 d . . .
H2E H 0.8214 0.6665 0.0421 0.125 Uiso 1 1 calc R . .
Cl4 Cl 0.9839(3) 0.6198(3) 0.00266(13) 0.1397(11) Uani 1 1 d . . .
Cl5 Cl 0.8546(2) 0.53364(17) 0.08889(10) 0.0944(6) Uani 1 1 d . . .
Cl6 Cl 0.9666(2) 0.73314(19) 0.12316(10) 0.1054(8) Uani 1 1 d . . .
N10 N 0.5000 1.0000 0.5000 0.0336(12) Uani 1 2 d SD . .
C1A C 0.5968(7) 0.9257(6) 0.5138(4) 0.036(2) Uani 0.50 1 d PD . 1
C1B C 0.5688(8) 0.9868(6) 0.4423(4) 0.036(2) Uani 0.50 1 d PD . 2
C2A C 0.6686(5) 0.9061(5) 0.4539(3) 0.0681(18) Uani 1 1 d D . .
C3A C 0.4127(8) 0.9608(6) 0.4416(4) 0.036(2) Uani 0.50 1 d PD . 1
C3B C 0.4445(8) 0.8993(6) 0.5051(4) 0.038(2) Uani 0.50 1 d PD . 2
C4A C 0.3530(5) 0.8530(4) 0.4428(3) 0.0517(14) Uani 1 1 d D . .
N10A N 0.0000 1.0000 0.0000 0.075(2) Uani 1 2 d SD . .
C1C C 0.1048(11) 0.9810(10) 0.0457(6) 0.068(3) Uani 0.50 1 d PD . 1
C2C C -0.0199(12) 1.1167(9) 0.0307(7) 0.074(4) Uani 0.50 1 d PD . 1
C1D C -0.0244(11) 0.9975(11) 0.0636(5) 0.067(3) Uani 0.50 1 d PD . 2
C2D C 0.1221(11) 1.0485(12) -0.0020(8) 0.087(5) Uani 0.50 1 d PD . 2
C3C C -0.1569(8) 0.9535(7) 0.0647(4) 0.100(3) Uani 1 1 d D . .
C4C C 0.1351(9) 0.8636(11) 0.0188(7) 0.167(6) Uani 1 1 d 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
C1 C2 1.361(6) . ?
C1 N1 1.388(6) . ?
C1 C31 1.525(6) . ?
C2 C3 1.427(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.359(6) . ?
C3 H3 0.9500 . ?
C4 N1 1.381(5) . ?
C4 C5 1.531(6) . ?
C5 C8 1.516(6) . ?
C5 C7 1.533(6) . ?
C5 C6 1.559(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N4 1.388(5) . ?
C8 C9 1.381(6) . ?
C9 C10 1.418(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.375(6) . ?
C10 H10 0.9500 . ?
C11 N4 1.383(5) . ?
C11 C12 1.531(6) . ?
C12 C20 1.515(6) . ?
C12 C14 1.523(7) . ?
C12 C13 1.560(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.401(7) . ?
C14 C19 1.398(7) . ?
C15 C16 1.384(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.397(7) . ?
C16 N5 1.472(7) . ?
C17 C18 1.369(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(8) . ?
C18 N6 1.498(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.373(7) . ?
C20 N3 1.379(5) . ?
C21 C22 1.421(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(6) . ?
C22 H22 0.9500 . ?
C23 N3 1.378(5) . ?
C23 C24 1.532(6) . ?
C24 C27 1.520(6) . ?
C24 C26 1.530(6) . ?
C24 C25 1.542(7) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.375(6) . ?
C27 N2 1.386(5) . ?
C28 C29 1.421(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(6) . ?
C29 H29 0.9500 . ?
C30 N2 1.383(5) . ?
C30 C31 1.521(6) . ?
C31 C33 1.540(6) . ?
C31 C32 1.547(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C38 1.391(6) . ?
C33 C34 1.402(6) . ?
C34 C35 1.385(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.388(7) . ?
C35 N7 1.475(6) . ?
C36 C37 1.388(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.376(7) . ?
C37 N8 1.481(6) . ?
C38 H38 0.9500 . ?
N1 H1 0.8800 . ?
N2 H2A 0.8800 . ?
N3 H3A 0.8800 . ?
N4 H4 0.8800 . ?
N5 O4 1.219(7) . ?
N5 O3 1.237(7) . ?
N6 O1 1.215(7) . ?
N6 O2 1.226(7) . ?
N7 O7 1.203(6) . ?
N7 O8 1.243(6) . ?
N8 O6 1.222(5) . ?
N8 O5 1.220(6) . ?
C39 O11 1.256(5) . ?
C39 O9 1.266(5) . ?
C39 O10 1.341(5) . ?
O10 H10A 0.8400 . ?
C40 O12 1.248(7) . ?
C40 O14 1.260(7) . ?
C40 O13 1.348(7) . ?
O13 H13 0.8400 . ?
N9 C45 1.504(8) . ?
N9 C41 1.517(9) . ?
N9 C47 1.530(10) . ?
N9 C43 1.533(10) . ?
C41 C42 1.520(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.491(11) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.529(12) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.435(16) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C1E Cl2 1.731(6) . ?
C1E Cl3 1.729(6) . ?
C1E Cl1 1.753(6) . ?
C1E H1E 1.0000 . ?
C2E Cl4 1.700(10) . ?
C2E Cl5 1.777(9) . ?
C2E Cl6 1.781(8) . ?
C2E H2E 1.0000 . ?
N10 C3A 1.508(8) 2_676 ?
N10 C3A 1.508(8) . ?
N10 C3B 1.526(8) 2_676 ?
N10 C3B 1.526(8) . ?
N10 C1A 1.540(7) . ?
N10 C1A 1.540(7) 2_676 ?
N10 C1B 1.587(8) . ?
N10 C1B 1.587(8) 2_676 ?
C1A C2A 1.648(10) . ?
C1A C3A 1.690(12) 2_676 ?
C1B C2A 1.617(9) . ?
C1B C3B 1.786(12) 2_676 ?
C3A C4A 1.607(9) . ?
C3A C1A 1.690(12) 2_676 ?
C3B C4A 1.610(9) . ?
C3B C1B 1.786(12) 2_676 ?
N10A C1D 1.496(10) . ?
N10A C1D 1.496(10) 2_575 ?
N10A C1C 1.498(10) 2_575 ?
N10A C1C 1.498(10) . ?
N10A C2D 1.519(11) 2_575 ?
N10A C2D 1.519(11) . ?
N10A C2C 1.642(11) . ?
N10A C2C 1.642(11) 2_575 ?
C1C C4C 1.662(16) . ?
C1C C2C 2.043(17) 2_575 ?
C2C C4C 1.633(17) 2_575 ?
C2C C1C 2.043(17) 2_575 ?
C1D C3C 1.596(13) . ?
C1D C2D 1.635(18) 2_575 ?
C2D C3C 1.506(18) 2_575 ?
C2D C1D 1.635(18) 2_575 ?
C3C C2D 1.506(18) 2_575 ?
C4C C2C 1.633(17) 2_575 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 107.2(4) . . ?
C2 C1 C31 131.2(4) . . ?
N1 C1 C31 121.6(4) . . ?
C1 C2 C3 107.7(4) . . ?
C1 C2 H2 126.1 . . ?
C3 C2 H2 126.1 . . ?
C4 C3 C2 108.1(4) . . ?
C4 C3 H3 126.0 . . ?
C2 C3 H3 126.0 . . ?
C3 C4 N1 107.3(4) . . ?
C3 C4 C5 130.9(4) . . ?
N1 C4 C5 121.6(4) . . ?
C8 C5 C4 112.5(3) . . ?
C8 C5 C7 108.7(3) . . ?
C4 C5 C7 109.0(4) . . ?
C8 C5 C6 109.3(4) . . ?
C4 C5 C6 109.1(3) . . ?
C7 C5 C6 108.2(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 C9 106.7(4) . . ?
N4 C8 C5 122.0(3) . . ?
C9 C8 C5 131.3(4) . . ?
C8 C9 C10 108.3(4) . . ?
C8 C9 H9 125.9 . . ?
C10 C9 H9 125.9 . . ?
C11 C10 C9 107.7(4) . . ?
C11 C10 H10 126.2 . . ?
C9 C10 H10 126.2 . . ?
C10 C11 N4 107.5(4) . . ?
C10 C11 C12 130.8(4) . . ?
N4 C11 C12 121.6(4) . . ?
C20 C12 C11 110.7(4) . . ?
C20 C12 C14 108.9(4) . . ?
C11 C12 C14 111.5(4) . . ?
C20 C12 C13 108.8(4) . . ?
C11 C12 C13 108.8(4) . . ?
C14 C12 C13 108.1(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 117.5(5) . . ?
C15 C14 C12 121.8(4) . . ?
C19 C14 C12 120.7(4) . . ?
C16 C15 C14 119.4(4) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 123.7(5) . . ?
C15 C16 N5 118.2(5) . . ?
C17 C16 N5 118.0(5) . . ?
C18 C17 C16 115.3(5) . . ?
C18 C17 H17 122.3 . . ?
C16 C17 H17 122.3 . . ?
C19 C18 C17 123.2(5) . . ?
C19 C18 N6 116.9(5) . . ?
C17 C18 N6 119.8(5) . . ?
C18 C19 C14 120.7(5) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
C21 C20 N3 107.2(4) . . ?
C21 C20 C12 130.7(4) . . ?
N3 C20 C12 121.9(4) . . ?
C20 C21 C22 107.8(4) . . ?
C20 C21 H21 126.1 . . ?
C22 C21 H21 126.1 . . ?
C23 C22 C21 107.8(4) . . ?
C23 C22 H22 126.1 . . ?
C21 C22 H22 126.1 . . ?
N3 C23 C22 106.9(4) . . ?
N3 C23 C24 121.7(4) . . ?
C22 C23 C24 131.1(4) . . ?
C27 C24 C26 108.9(4) . . ?
C27 C24 C23 111.2(3) . . ?
C26 C24 C23 108.8(4) . . ?
C27 C24 C25 109.7(4) . . ?
C26 C24 C25 109.1(4) . . ?
C23 C24 C25 109.2(4) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 N2 107.5(4) . . ?
C28 C27 C24 131.1(4) . . ?
N2 C27 C24 121.4(4) . . ?
C27 C28 C29 108.0(4) . . ?
C27 C28 H28 126.0 . . ?
C29 C28 H28 126.0 . . ?
C30 C29 C28 107.5(4) . . ?
C30 C29 H29 126.2 . . ?
C28 C29 H29 126.2 . . ?
N2 C30 C29 107.3(4) . . ?
N2 C30 C31 121.6(4) . . ?
C29 C30 C31 131.1(4) . . ?
C30 C31 C1 110.8(3) . . ?
C30 C31 C33 109.9(3) . . ?
C1 C31 C33 110.3(4) . . ?
C30 C31 C32 108.7(4) . . ?
C1 C31 C32 109.1(3) . . ?
C33 C31 C32 108.0(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C38 C33 C34 118.4(4) . . ?
C38 C33 C31 120.7(4) . . ?
C34 C33 C31 120.9(4) . . ?
C35 C34 C33 119.1(4) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C36 C35 C34 123.9(4) . . ?
C36 C35 N7 116.9(5) . . ?
C34 C35 N7 119.2(4) . . ?
C35 C36 C37 114.7(5) . . ?
C35 C36 H36 122.6 . . ?
C37 C36 H36 122.6 . . ?
C38 C37 C36 123.9(4) . . ?
C38 C37 N8 118.9(4) . . ?
C36 C37 N8 117.2(4) . . ?
C37 C38 C33 119.8(4) . . ?
C37 C38 H38 120.1 . . ?
C33 C38 H38 120.1 . . ?
C4 N1 C1 109.7(4) . . ?
C4 N1 H1 125.2 . . ?
C1 N1 H1 125.2 . . ?
C27 N2 C30 109.7(4) . . ?
C27 N2 H2A 125.2 . . ?
C30 N2 H2A 125.2 . . ?
C20 N3 C23 110.3(3) . . ?
C20 N3 H3A 124.9 . . ?
C23 N3 H3A 124.9 . . ?
C8 N4 C11 109.9(3) . . ?
C8 N4 H4 125.1 . . ?
C11 N4 H4 125.1 . . ?
O4 N5 O3 124.4(5) . . ?
O4 N5 C16 118.1(5) . . ?
O3 N5 C16 117.4(5) . . ?
O1 N6 O2 124.9(5) . . ?
O1 N6 C18 119.0(5) . . ?
O2 N6 C18 116.0(5) . . ?
O7 N7 O8 123.7(5) . . ?
O7 N7 C35 119.2(5) . . ?
O8 N7 C35 117.2(4) . . ?
O6 N8 O5 123.8(4) . . ?
O6 N8 C37 118.2(4) . . ?
O5 N8 C37 118.0(4) . . ?
O11 C39 O9 125.0(4) . . ?
O11 C39 O10 119.7(4) . . ?
O9 C39 O10 115.3(4) . . ?
C39 O10 H10A 109.5 . . ?
O12 C40 O14 124.7(6) . . ?
O12 C40 O13 118.3(5) . . ?
O14 C40 O13 116.9(6) . . ?
C40 O13 H13 109.5 . . ?
C45 N9 C41 104.6(5) . . ?
C45 N9 C47 111.3(6) . . ?
C41 N9 C47 109.5(7) . . ?
C45 N9 C43 112.4(6) . . ?
C41 N9 C43 112.5(5) . . ?
C47 N9 C43 106.6(7) . . ?
C42 C41 N9 115.0(5) . . ?
C42 C41 H41A 108.5 . . ?
N9 C41 H41A 108.5 . . ?
C42 C41 H41B 108.5 . . ?
N9 C41 H41B 108.5 . . ?
H41A C41 H41B 107.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 N9 116.8(5) . . ?
C44 C43 H43A 108.1 . . ?
N9 C43 H43A 108.1 . . ?
C44 C43 H43B 108.1 . . ?
N9 C43 H43B 108.1 . . ?
H43A C43 H43B 107.3 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N9 C45 C46 114.1(6) . . ?
N9 C45 H45A 108.7 . . ?
C46 C45 H45A 108.7 . . ?
N9 C45 H45B 108.7 . . ?
C46 C45 H45B 108.7 . . ?
H45A C45 H45B 107.6 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 N9 116.0(8) . . ?
C48 C47 H47A 108.3 . . ?
N9 C47 H47A 108.3 . . ?
C48 C47 H47B 108.3 . . ?
N9 C47 H47B 108.3 . . ?
H47A C47 H47B 107.4 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Cl2 C1E Cl3 115.5(4) . . ?
Cl2 C1E Cl1 110.7(3) . . ?
Cl3 C1E Cl1 109.0(3) . . ?
Cl2 C1E H1E 107.1 . . ?
Cl3 C1E H1E 107.1 . . ?
Cl1 C1E H1E 107.1 . . ?
Cl4 C2E Cl5 117.6(6) . . ?
Cl4 C2E Cl6 111.5(5) . . ?
Cl5 C2E Cl6 108.3(4) . . ?
Cl4 C2E H2E 106.3 . . ?
Cl5 C2E H2E 106.3 . . ?
Cl6 C2E H2E 106.3 . . ?
C3A N10 C3A 179.999(3) 2_676 . ?
C3A N10 C3B 71.8(5) 2_676 2_676 ?
C3A N10 C3B 108.2(5) . 2_676 ?
C3A N10 C3B 108.2(5) 2_676 . ?
C3A N10 C3B 71.8(5) . . ?
C3B N10 C3B 180.0(7) 2_676 . ?
C3A N10 C1A 67.3(5) 2_676 . ?
C3A N10 C1A 112.7(5) . . ?
C3B N10 C1A 112.1(5) 2_676 . ?
C3B N10 C1A 67.9(5) . . ?
C3A N10 C1A 112.7(5) 2_676 2_676 ?
C3A N10 C1A 67.3(5) . 2_676 ?
C3B N10 C1A 67.9(5) 2_676 2_676 ?
C3B N10 C1A 112.1(5) . 2_676 ?
C1A N10 C1A 179.999(4) . 2_676 ?
C3A N10 C1B 110.0(5) 2_676 . ?
C3A N10 C1B 70.0(5) . . ?
C3B N10 C1B 70.0(5) 2_676 . ?
C3B N10 C1B 110.0(5) . . ?
C1A N10 C1B 76.1(5) . . ?
C1A N10 C1B 103.9(5) 2_676 . ?
C3A N10 C1B 70.0(5) 2_676 2_676 ?
C3A N10 C1B 110.0(5) . 2_676 ?
C3B N10 C1B 110.0(5) 2_676 2_676 ?
C3B N10 C1B 70.0(5) . 2_676 ?
C1A N10 C1B 103.8(5) . 2_676 ?
C1A N10 C1B 76.1(5) 2_676 2_676 ?
C1B N10 C1B 179.998(3) . 2_676 ?
N10 C1A C2A 106.0(5) . . ?
N10 C1A C3A 55.4(4) . 2_676 ?
C2A C1A C3A 124.2(6) . 2_676 ?
N10 C1B C2A 105.3(5) . . ?
N10 C1B C3B 53.4(4) . 2_676 ?
C2A C1B C3B 124.6(6) . 2_676 ?
C1B C2A C1A 72.4(5) . . ?
N10 C3A C4A 111.0(5) . . ?
N10 C3A C1A 57.2(4) . 2_676 ?
C4A C3A C1A 131.0(7) . 2_676 ?
N10 C3B C4A 109.9(5) . . ?
N10 C3B C1B 56.6(4) . 2_676 ?
C4A C3B C1B 126.8(7) . 2_676 ?
C3B C4A C3A 67.2(5) . . ?
C1D N10A C1D 179.998(2) . 2_575 ?
C1D N10A C1C 116.6(7) . 2_575 ?
C1D N10A C1C 63.4(7) 2_575 2_575 ?
C1D N10A C1C 63.4(7) . . ?
C1D N10A C1C 116.6(7) 2_575 . ?
C1C N10A C1C 179.999(3) 2_575 . ?
C1D N10A C2D 65.7(8) . 2_575 ?
C1D N10A C2D 114.3(8) 2_575 2_575 ?
C1C N10A C2D 62.6(8) 2_575 2_575 ?
C1C N10A C2D 117.4(8) . 2_575 ?
C1D N10A C2D 114.3(8) . . ?
C1D N10A C2D 65.7(8) 2_575 . ?
C1C N10A C2D 117.4(8) 2_575 . ?
C1C N10A C2D 62.6(8) . . ?
C2D N10A C2D 180.0(11) 2_575 . ?
C1D N10A C2C 74.8(8) . . ?
C1D N10A C2C 105.2(8) 2_575 . ?
C1C N10A C2C 81.0(7) 2_575 . ?
C1C N10A C2C 99.0(7) . . ?
C2D N10A C2C 100.4(8) 2_575 . ?
C2D N10A C2C 79.6(8) . . ?
C1D N10A C2C 105.2(8) . 2_575 ?
C1D N10A C2C 74.8(8) 2_575 2_575 ?
C1C N10A C2C 99.0(7) 2_575 2_575 ?
C1C N10A C2C 81.0(7) . 2_575 ?
C2D N10A C2C 79.6(8) 2_575 2_575 ?
C2D N10A C2C 100.4(8) . 2_575 ?
C2C N10A C2C 180.0(10) . 2_575 ?
N10A C1C C4C 103.6(8) . . ?
N10A C1C C2C 52.6(5) . 2_575 ?
C4C C1C C2C 51.0(6) . 2_575 ?
C4C C2C N10A 98.7(8) 2_575 . ?
C4C C2C C1C 52.3(7) 2_575 2_575 ?
N10A C2C C1C 46.4(4) . 2_575 ?
N10A C1D C3C 113.3(8) . . ?
N10A C1D C2D 57.8(6) . 2_575 ?
C3C C1D C2D 55.6(7) . 2_575 ?
C3C C2D N10A 117.2(10) 2_575 . ?
C3C C2D C1D 60.9(8) 2_575 2_575 ?
N10A C2D C1D 56.5(5) . 2_575 ?
C2D C3C C1D 63.5(7) 2_575 . ?
C2C C4C C1C 76.7(7) 2_575 . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.341
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.095
####################################################################### 
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# 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_TBAHSO4-DNPC4P
_database_code_depnum_ccdc_archive 'CCDC 1482090'
_audit_update_record             
;
2016-05-26 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Cis-dinitrophenyl-calix[4]pyrrole-tetrabutylammonium chloride 
;
_chemical_name_common            Cis-DNP-Calix[4]pyrrole-TBAHSO4
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 N8 O8, 2(C16 H36 N), 2(H O4S)'
_chemical_formula_sum            'C70 H110 N10 O16 S2'
_chemical_formula_weight         1411.80

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   14.239(3)
_cell_length_b                   21.245(4)
_cell_length_c                   24.510(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.19(3)
_cell_angle_gamma                90.00
_cell_volume                     7409(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    38090
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.52

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3040
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9747
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50642
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12438
_reflns_number_gt                8915
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_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)+(0.0522P)²+5.8533P] 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_number_reflns         12438
_refine_ls_number_parameters     897
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1292
_refine_ls_wR_factor_gt          0.1155
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
C70 C 0.86016(19) 0.97237(13) 0.12405(11) 0.0299(6) Uani 1 1 d . . .
H70 H 0.8999 0.9880 0.0969 0.036 Uiso 1 1 calc R . .
S1 S 0.30296(5) 0.70438(3) 0.16366(3) 0.02622(17) Uani 1 1 d . . .
O8 O 0.32182(14) 0.74404(9) 0.11029(7) 0.0351(5) Uani 1 1 d . . .
H8 H 0.3364 0.7811 0.1191 0.053 Uiso 1 1 calc R . .
O6 O 0.27891(14) 0.64289(9) 0.14355(8) 0.0354(5) Uani 1 1 d . . .
O7 O 0.22976(14) 0.73598(9) 0.19163(8) 0.0368(5) Uani 1 1 d . . .
O5 O 0.39262(13) 0.70612(9) 0.19567(7) 0.0306(5) Uani 1 1 d . . .
S2 S 0.48729(5) 0.85434(3) 0.18460(3) 0.02302(16) Uani 1 1 d . . .
O4 O 0.47626(13) 0.91915(8) 0.19958(7) 0.0297(4) Uani 1 1 d . . .
O2 O 0.44037(12) 0.81566(8) 0.23011(7) 0.0267(4) Uani 1 1 d . . .
H2C H 0.4449 0.7771 0.2233 0.040 Uiso 1 1 calc R . .
O3 O 0.43991(12) 0.83741(8) 0.13283(7) 0.0265(4) Uani 1 1 d . . .
N6 N 0.44487(17) 0.81817(11) 0.37330(8) 0.0266(5) Uani 1 1 d . . .
O1 O 0.58684(12) 0.83502(8) 0.18518(7) 0.0245(4) Uani 1 1 d . . .
N3 N 0.69858(15) 0.80348(10) 0.08457(8) 0.0250(5) Uani 1 1 d . . .
H3 H 0.6706 0.8126 0.1150 0.030 Uiso 1 1 calc R . .
N2 N 0.74441(15) 0.92521(9) 0.16548(8) 0.0221(5) Uani 1 1 d . . .
H2 H 0.6931 0.9034 0.1709 0.027 Uiso 1 1 calc R . .
O15 O 0.36913(14) 0.81080(9) 0.39498(8) 0.0334(5) Uani 1 1 d . . .
O16 O 0.48939(14) 0.86756(9) 0.37497(8) 0.0327(5) Uani 1 1 d . . .
C19 C 0.74022(18) 0.84698(12) 0.05171(10) 0.0244(6) Uani 1 1 d . . .
O14 O 0.32679(16) 0.61206(10) 0.29784(9) 0.0431(5) Uani 1 1 d . . .
O13 O 0.44448(14) 0.57130(9) 0.25711(8) 0.0368(5) Uani 1 1 d . . .
N4 N 0.68411(15) 0.70740(10) 0.19316(8) 0.0243(5) Uani 1 1 d . . .
H4 H 0.6373 0.7344 0.1943 0.029 Uiso 1 1 calc R . .
C28 C 0.80408(19) 0.64749(12) 0.21923(11) 0.0283(6) Uani 1 1 d . . .
H28 H 0.8516 0.6268 0.2408 0.034 Uiso 1 1 calc R . .
N1 N 0.74127(15) 0.83104(9) 0.27392(8) 0.0222(5) Uani 1 1 d . . .
H1 H 0.6941 0.8318 0.2497 0.027 Uiso 1 1 calc R . .
C34 C 0.48541(19) 0.76421(12) 0.34491(10) 0.0228(6) Uani 1 1 d . . .
O10 O 0.31731(16) 0.89027(10) -0.00360(10) 0.0535(6) Uani 1 1 d . . .
C33 C 0.57915(19) 0.76650(12) 0.33294(10) 0.0230(6) Uani 1 1 d . . .
H33 H 0.6160 0.8021 0.3433 0.028 Uiso 1 1 calc R . .
N5 N 0.40859(18) 0.61252(11) 0.28439(9) 0.0295(5) Uani 1 1 d . . .
C4 C 0.79580(18) 0.88233(12) 0.28892(10) 0.0227(6) Uani 1 1 d . . .
C9 C 0.87353(19) 0.98089(12) 0.18130(11) 0.0285(6) Uani 1 1 d . . .
H9 H 0.9241 1.0029 0.1991 0.034 Uiso 1 1 calc R . .
C13 C 0.62590(18) 0.93439(12) 0.06121(10) 0.0249(6) Uani 1 1 d . . .
C10 C 0.77994(19) 0.93768(12) 0.11477(11) 0.0251(6) Uani 1 1 d . . .
O12 O 0.52154(16) 1.07898(10) 0.15228(10) 0.0516(6) Uani 1 1 d . . .
C15 C 0.49743(19) 0.99716(13) 0.09058(11) 0.0282(6) Uani 1 1 d . . .
C37 C 0.56169(19) 0.66595(12) 0.28978(10) 0.0244(6) Uani 1 1 d . . .
H37 H 0.5868 0.6316 0.2702 0.029 Uiso 1 1 calc R . .
C32 C 0.61986(18) 0.71663(12) 0.30566(10) 0.0225(6) Uani 1 1 d . . .
N7 N 0.4632(2) 1.04820(12) 0.12557(11) 0.0396(6) Uani 1 1 d . . .
C11 C 0.73113(18) 0.91702(12) 0.06185(10) 0.0251(6) Uani 1 1 d . . .
C14 C 0.59263(19) 0.98432(13) 0.09196(11) 0.0273(6) Uani 1 1 d . . .
H14 H 0.6350 1.0093 0.1136 0.033 Uiso 1 1 calc R . .
C5 C 0.77724(18) 0.94771(12) 0.26605(10) 0.0246(6) Uani 1 1 d . . .
C22 C 0.70660(19) 0.74385(13) 0.06353(10) 0.0259(6) Uani 1 1 d . . .
O11 O 0.37832(16) 1.05704(11) 0.12633(10) 0.0558(6) Uani 1 1 d . . .
C2 C 0.84594(19) 0.79612(13) 0.33574(11) 0.0276(6) Uani 1 1 d . . .
H2A H 0.8812 0.7696 0.3601 0.033 Uiso 1 1 calc R . .
C36 C 0.46861(19) 0.66596(12) 0.30250(10) 0.0243(6) Uani 1 1 d . . .
C1 C 0.77152(18) 0.77838(12) 0.30244(10) 0.0236(6) Uani 1 1 d . . .
C3 C 0.86109(19) 0.86160(13) 0.32727(10) 0.0272(6) Uani 1 1 d . . .
H3A H 0.9083 0.8866 0.3451 0.033 Uiso 1 1 calc R . .
N8 N 0.4009(2) 0.87779(12) -0.00557(11) 0.0397(6) Uani 1 1 d . . .
C29 C 0.74012(19) 0.68902(12) 0.23754(10) 0.0244(6) Uani 1 1 d . . .
C26 C 0.71248(19) 0.67706(12) 0.14653(11) 0.0249(6) Uani 1 1 d . . .
C30 C 0.72510(18) 0.71435(12) 0.29445(10) 0.0244(6) Uani 1 1 d . . .
C35 C 0.42705(19) 0.71433(12) 0.33084(10) 0.0252(6) Uani 1 1 d . . .
H35 H 0.3628 0.7133 0.3400 0.030 Uiso 1 1 calc R . .
C18 C 0.56169(19) 0.90019(13) 0.02850(11) 0.0280(6) Uani 1 1 d . . .
H18 H 0.5827 0.8665 0.0066 0.034 Uiso 1 1 calc R . .
C17 C 0.4675(2) 0.91568(13) 0.02829(11) 0.0285(6) Uani 1 1 d . . .
C23 C 0.6636(2) 0.68794(12) 0.09123(11) 0.0283(6) Uani 1 1 d . . .
C20 C 0.77574(19) 0.81407(14) 0.00891(11) 0.0305(7) Uani 1 1 d . . .
H20 H 0.8083 0.8315 -0.0206 0.037 Uiso 1 1 calc R . .
C6 C 0.67338(19) 0.96528(13) 0.27329(12) 0.0309(7) Uani 1 1 d . . .
H6A H 0.6329 0.9360 0.2523 0.046 Uiso 1 1 calc R . .
H6B H 0.6621 1.0083 0.2602 0.046 Uiso 1 1 calc R . .
H6C H 0.6591 0.9627 0.3120 0.046 Uiso 1 1 calc R . .
C8 C 0.80107(18) 0.95201(12) 0.20637(11) 0.0237(6) Uani 1 1 d . . .
C7 C 0.8396(2) 0.99487(13) 0.29846(12) 0.0321(7) Uani 1 1 d . . .
H7A H 0.8247 0.9932 0.3371 0.048 Uiso 1 1 calc R . .
H7B H 0.8279 1.0375 0.2844 0.048 Uiso 1 1 calc R . .
H7C H 0.9058 0.9840 0.2944 0.048 Uiso 1 1 calc R . .
C27 C 0.7873(2) 0.64044(12) 0.16231(11) 0.0301(7) Uani 1 1 d . . .
H27 H 0.8223 0.6145 0.1390 0.036 Uiso 1 1 calc R . .
C16 C 0.4323(2) 0.96340(13) 0.05940(11) 0.0305(7) Uani 1 1 d . . .
H16 H 0.3670 0.9726 0.0594 0.037 Uiso 1 1 calc R . .
O9 O 0.43171(17) 0.83606(13) -0.03382(11) 0.0689(8) Uani 1 1 d . . .
C12 C 0.7741(2) 0.95288(14) 0.01393(11) 0.0310(7) Uani 1 1 d . . .
H12A H 0.8414 0.9434 0.0130 0.047 Uiso 1 1 calc R . .
H12B H 0.7654 0.9982 0.0190 0.047 Uiso 1 1 calc R . .
H12C H 0.7428 0.9397 -0.0205 0.047 Uiso 1 1 calc R . .
C21 C 0.75529(19) 0.74953(14) 0.01661(11) 0.0297(7) Uani 1 1 d . . .
H21 H 0.7723 0.7160 -0.0067 0.036 Uiso 1 1 calc R . .
C25 C 0.6759(2) 0.62926(14) 0.05580(12) 0.0395(8) Uani 1 1 d . . .
H25A H 0.6432 0.6354 0.0203 0.059 Uiso 1 1 calc R . .
H25B H 0.6494 0.5926 0.0740 0.059 Uiso 1 1 calc R . .
H25C H 0.7429 0.6222 0.0505 0.059 Uiso 1 1 calc R . .
C31 C 0.7710(2) 0.66794(13) 0.33667(11) 0.0316(7) Uani 1 1 d . . .
H31A H 0.7417 0.6264 0.3324 0.047 Uiso 1 1 calc R . .
H31B H 0.7618 0.6836 0.3737 0.047 Uiso 1 1 calc R . .
H31C H 0.8384 0.6646 0.3305 0.047 Uiso 1 1 calc R . .
C24 C 0.55776(19) 0.69917(14) 0.09722(12) 0.0335(7) Uani 1 1 d . . .
H24A H 0.5484 0.7380 0.1178 0.050 Uiso 1 1 calc R . .
H24B H 0.5306 0.6637 0.1167 0.050 Uiso 1 1 calc R . .
H24C H 0.5269 0.7029 0.0609 0.050 Uiso 1 1 calc R . .
N10 N 0.08190(15) 0.70385(10) 0.02720(8) 0.0242(5) Uani 1 1 d . . .
C53 C 0.06282(19) 0.75784(12) -0.01236(10) 0.0261(6) Uani 1 1 d . . .
H53A H 0.0613 0.7407 -0.0499 0.031 Uiso 1 1 calc R . .
H53B H -0.0005 0.7748 -0.0058 0.031 Uiso 1 1 calc R . .
C55 C 0.1013(2) 0.86357(13) -0.04961(11) 0.0301(7) Uani 1 1 d . . .
H55A H 0.1540 0.8934 -0.0535 0.036 Uiso 1 1 calc R . .
H55B H 0.0875 0.8444 -0.0858 0.036 Uiso 1 1 calc R . .
C65 C 0.17914(19) 0.67634(13) 0.02077(10) 0.0279(6) Uani 1 1 d . . .
H65A H 0.1860 0.6393 0.0452 0.034 Uiso 1 1 calc R . .
H65B H 0.2260 0.7080 0.0335 0.034 Uiso 1 1 calc R . .
C61 C 0.07865(19) 0.72635(13) 0.08618(10) 0.0266(6) Uani 1 1 d . . .
H61A H 0.0922 0.6900 0.1105 0.032 Uiso 1 1 calc R . .
H61B H 0.1296 0.7575 0.0927 0.032 Uiso 1 1 calc R . .
C62 C -0.01289(19) 0.75578(13) 0.10243(10) 0.0276(6) Uani 1 1 d . . .
H62A H -0.0659 0.7272 0.0928 0.033 Uiso 1 1 calc R . .
H62B H -0.0232 0.7959 0.0826 0.033 Uiso 1 1 calc R . .
C67 C 0.2936(2) 0.61793(14) -0.03486(12) 0.0368(7) Uani 1 1 d . . .
H67A H 0.2862 0.5814 -0.0103 0.044 Uiso 1 1 calc R . .
H67B H 0.3045 0.6014 -0.0719 0.044 Uiso 1 1 calc R . .
C63 C -0.00856(19) 0.76784(13) 0.16376(10) 0.0274(6) Uani 1 1 d . . .
H63A H -0.0050 0.7270 0.1832 0.033 Uiso 1 1 calc R . .
H63B H 0.0493 0.7918 0.1735 0.033 Uiso 1 1 calc R . .
C57 C 0.00562(19) 0.65542(12) 0.01464(11) 0.0274(6) Uani 1 1 d . . .
H57A H -0.0560 0.6770 0.0153 0.033 Uiso 1 1 calc R . .
H57B H 0.0132 0.6400 -0.0230 0.033 Uiso 1 1 calc R . .
C64 C -0.0926(2) 0.80407(13) 0.18250(11) 0.0305(7) Uani 1 1 d . . .
H64A H -0.0944 0.8455 0.1650 0.046 Uiso 1 1 calc R . .
H64B H -0.0877 0.8093 0.2222 0.046 Uiso 1 1 calc R . .
H64C H -0.1502 0.7809 0.1725 0.046 Uiso 1 1 calc R . .
C66 C 0.2029(2) 0.65607(14) -0.03666(11) 0.0317(7) Uani 1 1 d . . .
H66A H 0.2104 0.6937 -0.0599 0.038 Uiso 1 1 calc R . .
H66B H 0.1510 0.6303 -0.0528 0.038 Uiso 1 1 calc R . .
C58 C 0.0026(2) 0.59896(13) 0.05218(12) 0.0349(7) Uani 1 1 d . . .
H58A H -0.0077 0.6129 0.0900 0.042 Uiso 1 1 calc R . .
H58B H 0.0632 0.5761 0.0519 0.042 Uiso 1 1 calc R . .
C59 C -0.0770(2) 0.55575(14) 0.03264(14) 0.0418(8) Uani 1 1 d . . .
H59A H -0.1346 0.5812 0.0262 0.050 Uiso 1 1 calc R . .
H59B H -0.0606 0.5367 -0.0026 0.050 Uiso 1 1 calc R . .
C54 C 0.1320(2) 0.81183(13) -0.00954(11) 0.0316(7) Uani 1 1 d . . .
H54A H 0.1952 0.7964 -0.0185 0.038 Uiso 1 1 calc R . .
H54B H 0.1358 0.8291 0.0280 0.038 Uiso 1 1 calc R . .
C68 C 0.3791(2) 0.65575(17) -0.01528(13) 0.0454(8) Uani 1 1 d . . .
H68A H 0.3824 0.6948 -0.0364 0.068 Uiso 1 1 calc R . .
H68B H 0.4362 0.6309 -0.0203 0.068 Uiso 1 1 calc R . .
H68C H 0.3740 0.6659 0.0235 0.068 Uiso 1 1 calc R . .
C56 C 0.0169(3) 0.89933(16) -0.03283(19) 0.0698(13) Uani 1 1 d . . .
H56A H -0.0359 0.8702 -0.0291 0.105 Uiso 1 1 calc R . .
H56B H 0.0003 0.9310 -0.0606 0.105 Uiso 1 1 calc R . .
H56C H 0.0308 0.9202 0.0022 0.105 Uiso 1 1 calc R . .
C60 C -0.0975(3) 0.50388(15) 0.07229(15) 0.0574(10) Uani 1 1 d . . .
H60A H -0.0428 0.4760 0.0763 0.086 Uiso 1 1 calc R . .
H60B H -0.1520 0.4797 0.0585 0.086 Uiso 1 1 calc R . .
H60C H -0.1111 0.5222 0.1078 0.086 Uiso 1 1 calc R . .
N9 N 0.30014(15) 0.41112(10) 0.21262(8) 0.0246(5) Uani 1 1 d . . .
C49 C 0.19951(19) 0.43432(12) 0.20561(11) 0.0260(6) Uani 1 1 d . . .
H49A H 0.1598 0.4090 0.2296 0.031 Uiso 1 1 calc R . .
H49B H 0.1775 0.4263 0.1674 0.031 Uiso 1 1 calc R . .
C50 C 0.1841(2) 0.50367(13) 0.21825(12) 0.0309(7) Uani 1 1 d . . .
H50A H 0.1917 0.5108 0.2581 0.037 Uiso 1 1 calc R . .
H50B H 0.2314 0.5295 0.1999 0.037 Uiso 1 1 calc R . .
C42 C 0.29923(19) 0.34043(12) 0.20041(11) 0.0265(6) Uani 1 1 d . . .
H42A H 0.2606 0.3194 0.2277 0.032 Uiso 1 1 calc R . .
H42B H 0.2676 0.3339 0.1642 0.032 Uiso 1 1 calc R . .
C38 C 0.33894(19) 0.42399(13) 0.27042(10) 0.0263(6) Uani 1 1 d . . .
H38A H 0.4025 0.4053 0.2744 0.032 Uiso 1 1 calc R . .
H38B H 0.3457 0.4701 0.2752 0.032 Uiso 1 1 calc R . .
C41 C 0.3510(2) 0.47762(15) 0.38467(12) 0.0411(8) Uani 1 1 d . . .
H41A H 0.4007 0.4926 0.3613 0.062 Uiso 1 1 calc R . .
H41B H 0.3721 0.4815 0.4231 0.062 Uiso 1 1 calc R . .
H41C H 0.2943 0.5030 0.3781 0.062 Uiso 1 1 calc R . .
C40 C 0.3294(2) 0.40921(14) 0.37173(11) 0.0346(7) Uani 1 1 d . . .
H40A H 0.2893 0.3921 0.4003 0.041 Uiso 1 1 calc R . .
H40B H 0.3890 0.3851 0.3732 0.041 Uiso 1 1 calc R . .
C51 C 0.0860(2) 0.52309(13) 0.19849(12) 0.0354(7) Uani 1 1 d . . .
H51A H 0.0393 0.4958 0.2158 0.042 Uiso 1 1 calc R . .
H51B H 0.0795 0.5168 0.1585 0.042 Uiso 1 1 calc R . .
C39 C 0.2799(2) 0.39877(13) 0.31584(11) 0.0312(7) Uani 1 1 d . . .
H39A H 0.2686 0.3532 0.3102 0.037 Uiso 1 1 calc R . .
H39B H 0.2182 0.4203 0.3148 0.037 Uiso 1 1 calc R . .
C44 C 0.3841(2) 0.23864(14) 0.18539(12) 0.0396(8) Uani 1 1 d . . .
H44A H 0.4439 0.2170 0.1953 0.048 Uiso 1 1 calc R . .
H44B H 0.3345 0.2197 0.2073 0.048 Uiso 1 1 calc R . .
C43 C 0.3937(2) 0.30804(13) 0.20044(12) 0.0363(7) Uani 1 1 d . . .
H43A H 0.4247 0.3118 0.2371 0.044 Uiso 1 1 calc R . .
H43B H 0.4340 0.3292 0.1740 0.044 Uiso 1 1 calc R . .
C47 C 0.3371(2) 0.43989(15) 0.11356(11) 0.0414(8) Uani 1 1 d . . .
H47A H 0.3345 0.3948 0.1034 0.050 Uiso 1 1 calc R . .
H47B H 0.2738 0.4580 0.1065 0.050 Uiso 1 1 calc R . .
C46 C 0.3634(2) 0.44562(13) 0.17409(11) 0.0303(7) Uani 1 1 d . . .
H46A H 0.4283 0.4297 0.1802 0.036 Uiso 1 1 calc R . .
H46B H 0.3638 0.4908 0.1839 0.036 Uiso 1 1 calc R . .
C52 C 0.0652(2) 0.59169(14) 0.21181(13) 0.0416(8) Uani 1 1 d . . .
H52A H 0.0650 0.5971 0.2515 0.062 Uiso 1 1 calc R . .
H52B H 0.0035 0.6033 0.1957 0.062 Uiso 1 1 calc R . .
H52C H 0.1136 0.6187 0.1967 0.062 Uiso 1 1 calc R . .
C45 C 0.3601(3) 0.22714(17) 0.12554(14) 0.0562(10) Uani 1 1 d . . .
H45A H 0.2990 0.2461 0.1159 0.084 Uiso 1 1 calc R . .
H45B H 0.3574 0.1817 0.1186 0.084 Uiso 1 1 calc R . .
H45C H 0.4085 0.2462 0.1034 0.084 Uiso 1 1 calc R . .
C48 C 0.4466(4) 0.5275(3) 0.08978(19) 0.118(2) Uani 1 1 d . . .
H48A H 0.3996 0.5612 0.0882 0.177 Uiso 1 1 calc R . .
H48B H 0.4942 0.5357 0.0628 0.177 Uiso 1 1 calc R . .
H48C H 0.4768 0.5261 0.1264 0.177 Uiso 1 1 calc R . .
C69 C 0.4051(4) 0.4726(2) 0.07883(15) 0.0973(18) Uani 1 1 d . . .
H69A H 0.4566 0.4422 0.0735 0.117 Uiso 1 1 calc R . .
H69B H 0.3725 0.4778 0.0427 0.117 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
C70 C10 1.371(4) . ?
C70 C9 1.420(4) . ?
C70 H70 0.9500 . ?
S1 O6 1.4332(19) . ?
S1 O7 1.436(2) . ?
S1 O5 1.4731(19) . ?
S1 O8 1.5875(19) . ?
O8 H8 0.8400 . ?
S2 O4 1.4351(19) . ?
S2 O3 1.4592(18) . ?
S2 O1 1.4753(19) . ?
S2 O2 1.5567(18) . ?
O2 H2C 0.8400 . ?
N6 O16 1.226(3) . ?
N6 O15 1.230(3) . ?
N6 C34 1.471(3) . ?
N3 C22 1.374(3) . ?
N3 C19 1.375(3) . ?
N3 H3 0.8800 . ?
N2 C8 1.385(3) . ?
N2 C10 1.385(3) . ?
N2 H2 0.8800 . ?
C19 C20 1.373(4) . ?
C19 C11 1.515(4) . ?
O14 N5 1.223(3) . ?
O13 N5 1.225(3) . ?
N4 C29 1.380(3) . ?
N4 C26 1.386(3) . ?
N4 H4 0.8800 . ?
C28 C29 1.357(4) . ?
C28 C27 1.414(4) . ?
C28 H28 0.9500 . ?
N1 C4 1.380(3) . ?
N1 C1 1.379(3) . ?
N1 H1 0.8800 . ?
C34 C33 1.379(4) . ?
C34 C35 1.382(4) . ?
O10 N8 1.222(3) . ?
C33 C32 1.391(4) . ?
C33 H33 0.9500 . ?
N5 C36 1.479(3) . ?
C4 C3 1.369(4) . ?
C4 C5 1.517(4) . ?
C9 C8 1.367(4) . ?
C9 H9 0.9500 . ?
C13 C14 1.394(4) . ?
C13 C18 1.397(4) . ?
C13 C11 1.543(4) . ?
C10 C11 1.513(4) . ?
O12 N7 1.227(3) . ?
C15 C16 1.380(4) . ?
C15 C14 1.382(4) . ?
C15 N7 1.477(4) . ?
C37 C36 1.373(4) . ?
C37 C32 1.404(4) . ?
C37 H37 0.9500 . ?
C32 C30 1.535(4) . ?
N7 O11 1.224(3) . ?
C11 C12 1.546(4) . ?
C14 H14 0.9500 . ?
C5 C8 1.517(4) . ?
C5 C7 1.539(4) . ?
C5 C6 1.542(4) . ?
C22 C21 1.371(4) . ?
C22 C23 1.510(4) . ?
C2 C1 1.366(4) . ?
C2 C3 1.424(4) . ?
C2 H2A 0.9500 . ?
C36 C35 1.386(4) . ?
C1 C30 1.522(4) . ?
C3 H3A 0.9500 . ?
N8 O9 1.217(3) . ?
N8 C17 1.475(4) . ?
C29 C30 1.518(4) . ?
C26 C27 1.363(4) . ?
C26 C23 1.518(4) . ?
C30 C31 1.555(3) . ?
C35 H35 0.9500 . ?
C18 C17 1.381(4) . ?
C18 H18 0.9500 . ?
C17 C16 1.375(4) . ?
C23 C25 1.533(4) . ?
C23 C24 1.538(4) . ?
C20 C21 1.416(4) . ?
C20 H20 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C27 H27 0.9500 . ?
C16 H16 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 H21 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N10 C65 1.517(3) . ?
N10 C57 1.519(3) . ?
N10 C53 1.520(3) . ?
N10 C61 1.525(3) . ?
C53 C54 1.512(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C55 C56 1.493(4) . ?
C55 C54 1.527(4) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C65 C66 1.523(4) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C61 C62 1.513(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.524(4) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C67 C68 1.521(4) . ?
C67 C66 1.524(4) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C63 C64 1.509(4) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C57 C58 1.513(4) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C58 C59 1.521(4) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.505(4) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
N9 C46 1.519(3) . ?
N9 C49 1.519(3) . ?
N9 C38 1.526(3) . ?
N9 C42 1.531(3) . ?
C49 C50 1.523(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.518(4) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C42 C43 1.511(4) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C38 C39 1.518(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C41 C40 1.517(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C40 C39 1.533(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C51 C52 1.525(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C44 C45 1.513(4) . ?
C44 C43 1.525(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C47 C69 1.485(5) . ?
C47 C46 1.521(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C48 C69 1.332(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?

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
C10 C70 C9 108.2(2) . . ?
C10 C70 H70 125.9 . . ?
C9 C70 H70 125.9 . . ?
O6 S1 O7 114.97(12) . . ?
O6 S1 O5 113.38(11) . . ?
O7 S1 O5 111.36(11) . . ?
O6 S1 O8 104.25(11) . . ?
O7 S1 O8 107.10(12) . . ?
O5 S1 O8 104.77(11) . . ?
S1 O8 H8 109.5 . . ?
O4 S2 O3 114.05(11) . . ?
O4 S2 O1 112.27(11) . . ?
O3 S2 O1 110.60(11) . . ?
O4 S2 O2 105.60(11) . . ?
O3 S2 O2 107.23(10) . . ?
O1 S2 O2 106.56(10) . . ?
S2 O2 H2C 109.5 . . ?
O16 N6 O15 123.7(2) . . ?
O16 N6 C34 118.1(2) . . ?
O15 N6 C34 118.1(2) . . ?
C22 N3 C19 110.9(2) . . ?
C22 N3 H3 124.6 . . ?
C19 N3 H3 124.6 . . ?
C8 N2 C10 110.4(2) . . ?
C8 N2 H2 124.8 . . ?
C10 N2 H2 124.8 . . ?
C20 C19 N3 106.6(2) . . ?
C20 C19 C11 131.4(2) . . ?
N3 C19 C11 121.5(2) . . ?
C29 N4 C26 109.9(2) . . ?
C29 N4 H4 125.0 . . ?
C26 N4 H4 125.0 . . ?
C29 C28 C27 107.7(2) . . ?
C29 C28 H28 126.1 . . ?
C27 C28 H28 126.1 . . ?
C4 N1 C1 110.1(2) . . ?
C4 N1 H1 124.9 . . ?
C1 N1 H1 124.9 . . ?
C33 C34 C35 123.5(2) . . ?
C33 C34 N6 118.3(2) . . ?
C35 C34 N6 118.2(2) . . ?
C34 C33 C32 120.0(2) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
O14 N5 O13 124.3(2) . . ?
O14 N5 C36 118.1(2) . . ?
O13 N5 C36 117.7(2) . . ?
C3 C4 N1 106.8(2) . . ?
C3 C4 C5 130.7(2) . . ?
N1 C4 C5 122.4(2) . . ?
C8 C9 C70 108.2(2) . . ?
C8 C9 H9 125.9 . . ?
C70 C9 H9 125.9 . . ?
C14 C13 C18 118.5(2) . . ?
C14 C13 C11 121.8(2) . . ?
C18 C13 C11 119.7(2) . . ?
C70 C10 N2 106.5(2) . . ?
C70 C10 C11 130.6(2) . . ?
N2 C10 C11 122.8(2) . . ?
C16 C15 C14 123.3(3) . . ?
C16 C15 N7 118.2(3) . . ?
C14 C15 N7 118.4(3) . . ?
C36 C37 C32 120.1(2) . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
C33 C32 C37 117.7(2) . . ?
C33 C32 C30 122.5(2) . . ?
C37 C32 C30 119.7(2) . . ?
O11 N7 O12 124.0(3) . . ?
O11 N7 C15 118.0(3) . . ?
O12 N7 C15 118.0(3) . . ?
C10 C11 C19 112.7(2) . . ?
C10 C11 C13 110.7(2) . . ?
C19 C11 C13 108.8(2) . . ?
C10 C11 C12 109.0(2) . . ?
C19 C11 C12 108.7(2) . . ?
C13 C11 C12 106.7(2) . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C4 C5 C8 111.7(2) . . ?
C4 C5 C7 108.4(2) . . ?
C8 C5 C7 108.2(2) . . ?
C4 C5 C6 109.5(2) . . ?
C8 C5 C6 110.3(2) . . ?
C7 C5 C6 108.6(2) . . ?
C21 C22 N3 106.6(2) . . ?
C21 C22 C23 132.3(2) . . ?
N3 C22 C23 121.0(2) . . ?
C1 C2 C3 107.5(2) . . ?
C1 C2 H2A 126.2 . . ?
C3 C2 H2A 126.2 . . ?
C37 C36 C35 123.3(2) . . ?
C37 C36 N5 118.9(2) . . ?
C35 C36 N5 117.8(2) . . ?
C2 C1 N1 107.4(2) . . ?
C2 C1 C30 130.3(2) . . ?
N1 C1 C30 122.3(2) . . ?
C4 C3 C2 108.1(2) . . ?
C4 C3 H3A 125.9 . . ?
C2 C3 H3A 125.9 . . ?
O9 N8 O10 123.6(3) . . ?
O9 N8 C17 118.6(3) . . ?
O10 N8 C17 117.8(3) . . ?
C28 C29 N4 107.3(2) . . ?
C28 C29 C30 130.9(2) . . ?
N4 C29 C30 121.8(2) . . ?
C27 C26 N4 106.3(2) . . ?
C27 C26 C23 131.8(2) . . ?
N4 C26 C23 121.8(2) . . ?
C29 C30 C1 111.1(2) . . ?
C29 C30 C32 110.4(2) . . ?
C1 C30 C32 111.8(2) . . ?
C29 C30 C31 108.4(2) . . ?
C1 C30 C31 108.2(2) . . ?
C32 C30 C31 106.8(2) . . ?
C34 C35 C36 115.4(3) . . ?
C34 C35 H35 122.3 . . ?
C36 C35 H35 122.3 . . ?
C17 C18 C13 119.5(3) . . ?
C17 C18 H18 120.2 . . ?
C13 C18 H18 120.2 . . ?
C16 C17 C18 123.3(3) . . ?
C16 C17 N8 118.3(3) . . ?
C18 C17 N8 118.4(3) . . ?
C22 C23 C26 109.9(2) . . ?
C22 C23 C25 109.1(2) . . ?
C26 C23 C25 108.9(2) . . ?
C22 C23 C24 109.7(2) . . ?
C26 C23 C24 110.9(2) . . ?
C25 C23 C24 108.3(2) . . ?
C19 C20 C21 107.9(2) . . ?
C19 C20 H20 126.0 . . ?
C21 C20 H20 126.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C9 C8 N2 106.7(2) . . ?
C9 C8 C5 131.4(2) . . ?
N2 C8 C5 121.8(2) . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C26 C27 C28 108.7(2) . . ?
C26 C27 H27 125.7 . . ?
C28 C27 H27 125.7 . . ?
C17 C16 C15 116.0(3) . . ?
C17 C16 H16 122.0 . . ?
C15 C16 H16 122.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C22 C21 C20 108.1(2) . . ?
C22 C21 H21 126.0 . . ?
C20 C21 H21 126.0 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C65 N10 C57 111.5(2) . . ?
C65 N10 C53 111.5(2) . . ?
C57 N10 C53 105.85(19) . . ?
C65 N10 C61 106.27(19) . . ?
C57 N10 C61 110.9(2) . . ?
C53 N10 C61 110.92(19) . . ?
C54 C53 N10 116.3(2) . . ?
C54 C53 H53A 108.2 . . ?
N10 C53 H53A 108.2 . . ?
C54 C53 H53B 108.2 . . ?
N10 C53 H53B 108.2 . . ?
H53A C53 H53B 107.4 . . ?
C56 C55 C54 113.8(3) . . ?
C56 C55 H55A 108.8 . . ?
C54 C55 H55A 108.8 . . ?
C56 C55 H55B 108.8 . . ?
C54 C55 H55B 108.8 . . ?
H55A C55 H55B 107.7 . . ?
N10 C65 C66 116.2(2) . . ?
N10 C65 H65A 108.2 . . ?
C66 C65 H65A 108.2 . . ?
N10 C65 H65B 108.2 . . ?
C66 C65 H65B 108.2 . . ?
H65A C65 H65B 107.4 . . ?
C62 C61 N10 115.9(2) . . ?
C62 C61 H61A 108.3 . . ?
N10 C61 H61A 108.3 . . ?
C62 C61 H61B 108.3 . . ?
N10 C61 H61B 108.3 . . ?
H61A C61 H61B 107.4 . . ?
C61 C62 C63 109.1(2) . . ?
C61 C62 H62A 109.9 . . ?
C63 C62 H62A 109.9 . . ?
C61 C62 H62B 109.9 . . ?
C63 C62 H62B 109.9 . . ?
H62A C62 H62B 108.3 . . ?
C68 C67 C66 113.3(3) . . ?
C68 C67 H67A 108.9 . . ?
C66 C67 H67A 108.9 . . ?
C68 C67 H67B 108.9 . . ?
C66 C67 H67B 108.9 . . ?
H67A C67 H67B 107.7 . . ?
C64 C63 C62 112.6(2) . . ?
C64 C63 H63A 109.1 . . ?
C62 C63 H63A 109.1 . . ?
C64 C63 H63B 109.1 . . ?
C62 C63 H63B 109.1 . . ?
H63A C63 H63B 107.8 . . ?
C58 C57 N10 116.8(2) . . ?
C58 C57 H57A 108.1 . . ?
N10 C57 H57A 108.1 . . ?
C58 C57 H57B 108.1 . . ?
N10 C57 H57B 108.1 . . ?
H57A C57 H57B 107.3 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C65 C66 C67 110.0(2) . . ?
C65 C66 H66A 109.7 . . ?
C67 C66 H66A 109.7 . . ?
C65 C66 H66B 109.7 . . ?
C67 C66 H66B 109.7 . . ?
H66A C66 H66B 108.2 . . ?
C57 C58 C59 109.0(2) . . ?
C57 C58 H58A 109.9 . . ?
C59 C58 H58A 109.9 . . ?
C57 C58 H58B 109.9 . . ?
C59 C58 H58B 109.9 . . ?
H58A C58 H58B 108.3 . . ?
C60 C59 C58 113.5(3) . . ?
C60 C59 H59A 108.9 . . ?
C58 C59 H59A 108.9 . . ?
C60 C59 H59B 108.9 . . ?
C58 C59 H59B 108.9 . . ?
H59A C59 H59B 107.7 . . ?
C53 C54 C55 110.3(2) . . ?
C53 C54 H54A 109.6 . . ?
C55 C54 H54A 109.6 . . ?
C53 C54 H54B 109.6 . . ?
C55 C54 H54B 109.6 . . ?
H54A C54 H54B 108.1 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C46 N9 C49 110.7(2) . . ?
C46 N9 C38 106.77(19) . . ?
C49 N9 C38 110.7(2) . . ?
C46 N9 C42 110.6(2) . . ?
C49 N9 C42 107.17(19) . . ?
C38 N9 C42 110.94(19) . . ?
N9 C49 C50 115.7(2) . . ?
N9 C49 H49A 108.4 . . ?
C50 C49 H49A 108.4 . . ?
N9 C49 H49B 108.4 . . ?
C50 C49 H49B 108.4 . . ?
H49A C49 H49B 107.4 . . ?
C51 C50 C49 109.6(2) . . ?
C51 C50 H50A 109.7 . . ?
C49 C50 H50A 109.7 . . ?
C51 C50 H50B 109.7 . . ?
C49 C50 H50B 109.7 . . ?
H50A C50 H50B 108.2 . . ?
C43 C42 N9 116.5(2) . . ?
C43 C42 H42A 108.2 . . ?
N9 C42 H42A 108.2 . . ?
C43 C42 H42B 108.2 . . ?
N9 C42 H42B 108.2 . . ?
H42A C42 H42B 107.3 . . ?
C39 C38 N9 115.3(2) . . ?
C39 C38 H38A 108.5 . . ?
N9 C38 H38A 108.5 . . ?
C39 C38 H38B 108.5 . . ?
N9 C38 H38B 108.5 . . ?
H38A C38 H38B 107.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C41 C40 C39 114.1(2) . . ?
C41 C40 H40A 108.7 . . ?
C39 C40 H40A 108.7 . . ?
C41 C40 H40B 108.7 . . ?
C39 C40 H40B 108.7 . . ?
H40A C40 H40B 107.6 . . ?
C50 C51 C52 112.1(2) . . ?
C50 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
C50 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C38 C39 C40 110.8(2) . . ?
C38 C39 H39A 109.5 . . ?
C40 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C40 C39 H39B 109.5 . . ?
H39A C39 H39B 108.1 . . ?
C45 C44 C43 113.9(3) . . ?
C45 C44 H44A 108.8 . . ?
C43 C44 H44A 108.8 . . ?
C45 C44 H44B 108.8 . . ?
C43 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?
C42 C43 C44 111.6(2) . . ?
C42 C43 H43A 109.3 . . ?
C44 C43 H43A 109.3 . . ?
C42 C43 H43B 109.3 . . ?
C44 C43 H43B 109.3 . . ?
H43A C43 H43B 108.0 . . ?
C69 C47 C46 112.3(3) . . ?
C69 C47 H47A 109.1 . . ?
C46 C47 H47A 109.1 . . ?
C69 C47 H47B 109.1 . . ?
C46 C47 H47B 109.1 . . ?
H47A C47 H47B 107.9 . . ?
N9 C46 C47 116.0(2) . . ?
N9 C46 H46A 108.3 . . ?
C47 C46 H46A 108.3 . . ?
N9 C46 H46B 108.3 . . ?
C47 C46 H46B 108.3 . . ?
H46A C46 H46B 107.4 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C69 C48 H48A 109.5 . . ?
C69 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C69 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C48 C69 C47 126.1(4) . . ?
C48 C69 H69A 105.8 . . ?
C47 C69 H69A 105.8 . . ?
C48 C69 H69B 105.8 . . ?
C47 C69 H69B 105.8 . . ?
H69A C69 H69B 106.2 . . ?

_diffrn_measured_fraction_theta_max 0.953
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.953
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.050
####################################################################### 
# 
# 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_TBANO3-DNPC4P
_database_code_depnum_ccdc_archive 'CCDC 1482091'
_audit_update_record             
;
2016-05-26 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Cis-Dinitrophenyl-calix[4]pyrrole-tetrabutylammonium nitrate 
;
_chemical_name_common            Cis-DNP-Calix[4]pyrrole-TBANO3
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 N8 O8, C16 H36 N, N O3'
_chemical_formula_sum            'C54 H72 N10 O11'
_chemical_formula_weight         1037.22

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   P21/n

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

_cell_length_a                   12.8705(12)
_cell_length_b                   18.6776(18)
_cell_length_c                   23.141(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.418(2)
_cell_angle_gamma                90.00
_cell_volume                     5562.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    9110
_cell_measurement_theta_min      1.8047
_cell_measurement_theta_max      27.4971

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2216
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9896
_exptl_absorpt_correction_T_max  0.9930
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku SCX-Mini with Mercury CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32722
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.49
_reflns_number_total             12637
_reflns_number_gt                5995
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_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)+(0.0500P)²+0.9814P] 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_number_reflns         12637
_refine_ls_number_parameters     686
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1714
_refine_ls_wR_factor_gt          0.1394
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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 0.43118(19) 0.04075(12) 0.21376(10) 0.0410(6) Uani 1 1 d . . .
C2 C 0.3813(2) -0.00165(15) 0.25279(13) 0.0628(8) Uani 1 1 d . . .
H2 H 0.3987 -0.0492 0.2621 0.075 Uiso 1 1 calc R . .
C3 C 0.2987(2) 0.03822(15) 0.27682(14) 0.0658(8) Uani 1 1 d . . .
H3 H 0.2524 0.0219 0.3052 0.079 Uiso 1 1 calc R . .
C4 C 0.29754(19) 0.10424(13) 0.25187(11) 0.0436(6) Uani 1 1 d . . .
C5 C 0.22080(18) 0.16479(14) 0.25855(11) 0.0485(7) Uani 1 1 d . . .
C6 C 0.1780(2) 0.18598(16) 0.19803(12) 0.0618(8) Uani 1 1 d . . .
H6A H 0.2344 0.2037 0.1744 0.093 Uiso 1 1 calc R . .
H6B H 0.1258 0.2231 0.2022 0.093 Uiso 1 1 calc R . .
H6C H 0.1470 0.1444 0.1796 0.093 Uiso 1 1 calc R . .
C7 C 0.1286(2) 0.13889(17) 0.29524(13) 0.0679(9) Uani 1 1 d . . .
H7A H 0.0982 0.0966 0.2776 0.102 Uiso 1 1 calc R . .
H7B H 0.0767 0.1764 0.2973 0.102 Uiso 1 1 calc R . .
H7C H 0.1529 0.1273 0.3339 0.102 Uiso 1 1 calc R . .
C8 C 0.26717(19) 0.23003(14) 0.28742(11) 0.0448(6) Uani 1 1 d . . .
C9 C 0.2361(2) 0.26946(16) 0.33393(12) 0.0584(8) Uani 1 1 d . . .
H9 H 0.1817 0.2575 0.3590 0.070 Uiso 1 1 calc R . .
C10 C 0.2991(2) 0.33109(15) 0.33809(11) 0.0525(7) Uani 1 1 d . . .
H10 H 0.2937 0.3674 0.3660 0.063 Uiso 1 1 calc R . .
C11 C 0.36973(19) 0.32858(13) 0.29415(10) 0.0415(6) Uani 1 1 d . . .
C12 C 0.4517(2) 0.38170(12) 0.27579(10) 0.0434(6) Uani 1 1 d . . .
C13 C 0.4433(2) 0.44933(14) 0.31419(12) 0.0610(8) Uani 1 1 d . . .
H13A H 0.4531 0.4361 0.3544 0.092 Uiso 1 1 calc R . .
H13B H 0.3753 0.4708 0.3091 0.092 Uiso 1 1 calc R . .
H13C H 0.4964 0.4835 0.3032 0.092 Uiso 1 1 calc R . .
C14 C 0.4334(2) 0.40596(12) 0.21246(10) 0.0414(6) Uani 1 1 d . . .
C15 C 0.3398(2) 0.39399(13) 0.18344(10) 0.0445(6) Uani 1 1 d . . .
H15 H 0.2855 0.3691 0.2015 0.053 Uiso 1 1 calc R . .
C16 C 0.3278(2) 0.41926(13) 0.12754(11) 0.0451(6) Uani 1 1 d . . .
C17 C 0.4032(2) 0.45579(14) 0.09820(11) 0.0522(7) Uani 1 1 d . . .
H17 H 0.3931 0.4721 0.0601 0.063 Uiso 1 1 calc R . .
C18 C 0.4949(2) 0.46716(14) 0.12807(11) 0.0504(7) Uani 1 1 d . . .
C19 C 0.5115(2) 0.44334(13) 0.18374(11) 0.0484(7) Uani 1 1 d . . .
H19 H 0.5754 0.4522 0.2024 0.058 Uiso 1 1 calc R . .
C20 C 0.56091(19) 0.35133(13) 0.28100(10) 0.0418(6) Uani 1 1 d . . .
C21 C 0.6399(2) 0.36433(14) 0.31946(11) 0.0509(7) Uani 1 1 d . . .
H21 H 0.6376 0.3953 0.3515 0.061 Uiso 1 1 calc R . .
C22 C 0.7255(2) 0.32259(15) 0.30213(12) 0.0567(8) Uani 1 1 d . . .
H22 H 0.7904 0.3211 0.3210 0.068 Uiso 1 1 calc R . .
C23 C 0.69968(19) 0.28480(14) 0.25386(11) 0.0461(7) Uani 1 1 d . . .
C24 C 0.76207(19) 0.23658(15) 0.21480(13) 0.0550(7) Uani 1 1 d . . .
C25 C 0.8776(2) 0.23995(18) 0.23341(16) 0.0823(10) Uani 1 1 d . . .
H25A H 0.8848 0.2231 0.2729 0.123 Uiso 1 1 calc R . .
H25B H 0.9020 0.2890 0.2310 0.123 Uiso 1 1 calc R . .
H25C H 0.9186 0.2099 0.2080 0.123 Uiso 1 1 calc R . .
C26 C 0.7539(2) 0.26378(16) 0.15168(13) 0.0698(9) Uani 1 1 d . . .
H26A H 0.7964 0.2339 0.1269 0.105 Uiso 1 1 calc R . .
H26B H 0.7782 0.3129 0.1498 0.105 Uiso 1 1 calc R . .
H26C H 0.6821 0.2616 0.1388 0.105 Uiso 1 1 calc R . .
C27 C 0.72737(18) 0.15885(14) 0.21729(11) 0.0488(7) Uani 1 1 d . . .
C28 C 0.7784(2) 0.09770(16) 0.23140(13) 0.0658(9) Uani 1 1 d . . .
H28 H 0.8462 0.0950 0.2466 0.079 Uiso 1 1 calc R . .
C29 C 0.7130(2) 0.03875(15) 0.21964(13) 0.0610(8) Uani 1 1 d . . .
H29 H 0.7299 -0.0097 0.2253 0.073 Uiso 1 1 calc R . .
C30 C 0.62122(19) 0.06440(13) 0.19857(10) 0.0447(6) Uani 1 1 d . . .
C31 C 0.5247(2) 0.02714(12) 0.17607(11) 0.0440(6) Uani 1 1 d . . .
C32 C 0.5458(2) -0.05460(13) 0.17352(12) 0.0597(8) Uani 1 1 d . . .
H32A H 0.6042 -0.0638 0.1483 0.090 Uiso 1 1 calc R . .
H32B H 0.4847 -0.0790 0.1586 0.090 Uiso 1 1 calc R . .
H32C H 0.5617 -0.0722 0.2120 0.090 Uiso 1 1 calc R . .
C33 C 0.5010(2) 0.05141(13) 0.11340(10) 0.0426(6) Uani 1 1 d . . .
C34 C 0.4017(2) 0.04136(13) 0.08997(11) 0.0479(7) Uani 1 1 d . . .
H34 H 0.3493 0.0201 0.1122 0.057 Uiso 1 1 calc R . .
C35 C 0.3812(2) 0.06284(14) 0.03399(12) 0.0520(7) Uani 1 1 d . . .
C36 C 0.4542(2) 0.09416(14) -0.00055(12) 0.0558(7) Uani 1 1 d . . .
H36 H 0.4386 0.1091 -0.0384 0.067 Uiso 1 1 calc R . .
N1 N 0.37924(15) 0.10526(10) 0.21409(8) 0.0413(5) Uani 1 1 d . . .
H1 H 0.3961 0.1420 0.1930 0.050 Uiso 1 1 calc R . .
N2 N 0.35026(15) 0.26644(10) 0.26402(8) 0.0417(5) Uani 1 1 d . . .
H2A H 0.3855 0.2520 0.2343 0.050 Uiso 1 1 calc R . .
N3 N 0.59813(15) 0.30247(10) 0.24143(9) 0.0441(5) Uani 1 1 d . . .
H3A H 0.5623 0.2852 0.2126 0.053 Uiso 1 1 calc R . .
N4 N 0.63049(15) 0.13824(11) 0.19823(9) 0.0447(5) Uani 1 1 d . . .
H4 H 0.5816 0.1676 0.1874 0.054 Uiso 1 1 calc R . .
N5 N 0.5790(2) 0.50657(15) 0.09908(12) 0.0750(8) Uani 1 1 d . . .
N6 N 0.2264(2) 0.40828(14) 0.09854(11) 0.0612(7) Uani 1 1 d . . .
N7 N 0.2752(2) 0.05278(17) 0.01024(13) 0.0777(8) Uani 1 1 d . . .
N8 N 0.6323(2) 0.13694(16) -0.01221(13) 0.0767(8) Uani 1 1 d . . .
O1 O 0.6584(2) 0.51720(19) 0.12552(13) 0.1380(13) Uani 1 1 d . . .
O2 O 0.5647(2) 0.52692(13) 0.05013(10) 0.0945(8) Uani 1 1 d . . .
O3 O 0.20816(17) 0.44283(12) 0.05461(9) 0.0822(7) Uani 1 1 d . . .
O4 O 0.16532(17) 0.36608(14) 0.11977(10) 0.0854(7) Uani 1 1 d . . .
O5 O 0.25618(19) 0.07648(15) -0.03783(11) 0.1060(9) Uani 1 1 d . . .
O6 O 0.2125(2) 0.02077(18) 0.03996(13) 0.1243(11) Uani 1 1 d . . .
O7 O 0.7129(2) 0.15535(16) 0.01148(12) 0.1085(9) Uani 1 1 d . . .
O8 O 0.6139(2) 0.14717(15) -0.06279(11) 0.1073(9) Uani 1 1 d . . .
N9 N 0.43909(18) 0.24620(11) 0.10770(10) 0.0469(5) Uani 1 1 d . . .
O9 O 0.46321(13) 0.23159(9) 0.15749(7) 0.0474(4) Uani 1 1 d . . .
O10 O 0.4980(2) 0.27816(17) 0.07623(11) 0.1180(10) Uani 1 1 d . . .
O11 O 0.35313(18) 0.22910(16) 0.08812(10) 0.1083(9) Uani 1 1 d . . .
N10 N 0.03200(19) 0.30458(13) 0.94218(10) 0.0678(7) Uani 1 1 d . . .
C37 C 0.5520(2) 0.10263(15) 0.02320(12) 0.0525(7) Uani 1 1 d . . .
C38 C 0.5770(2) 0.08172(13) 0.07885(11) 0.0491(7) Uani 1 1 d . . .
H38 H 0.6449 0.0879 0.0932 0.059 Uiso 1 1 calc R . .
C39 C 0.0053(2) 0.22431(17) 0.94462(14) 0.0741(9) Uani 1 1 d . . .
H39A H -0.0617 0.2170 0.9250 0.089 Uiso 1 1 calc R . .
H39B H 0.0579 0.1979 0.9228 0.089 Uiso 1 1 calc R . .
C40 C -0.0011(3) 0.19234(18) 1.00464(15) 0.0865(11) Uani 1 1 d . . .
H40A H -0.0535 0.2183 1.0269 0.104 Uiso 1 1 calc R . .
H40B H 0.0660 0.1981 1.0244 0.104 Uiso 1 1 calc R . .
C41 C -0.0293(3) 0.11346(18) 1.00274(17) 0.0871(11) Uani 1 1 d . . .
H41A H 0.0259 0.0871 0.9830 0.104 Uiso 1 1 calc R . .
H41B H -0.0935 0.1075 0.9802 0.104 Uiso 1 1 calc R . .
C42 C -0.0445(3) 0.0817(2) 1.06266(19) 0.1128(14) Uani 1 1 d . . .
H42A H 0.0187 0.0876 1.0852 0.169 Uiso 1 1 calc R . .
H42B H -0.0607 0.0312 1.0592 0.169 Uiso 1 1 calc R . .
H42C H -0.1013 0.1061 1.0817 0.169 Uiso 1 1 calc R . .
C43 C -0.0428(3) 0.34594(18) 0.97981(13) 0.0770(10) Uani 1 1 d . . .
H43A H -0.0249 0.3969 0.9776 0.092 Uiso 1 1 calc R . .
H43B H -0.0324 0.3308 1.0200 0.092 Uiso 1 1 calc R . .
C44 C -0.1571(3) 0.3377(2) 0.96475(16) 0.0907(11) Uani 1 1 d . . .
H44A H -0.1692 0.3556 0.9255 0.109 Uiso 1 1 calc R . .
H44B H -0.1751 0.2867 0.9652 0.109 Uiso 1 1 calc R . .
C45 C -0.2265(3) 0.3769(2) 1.00547(15) 0.0911(11) Uani 1 1 d . . .
H45A H -0.2106 0.4281 1.0039 0.109 Uiso 1 1 calc R . .
H45B H -0.2127 0.3603 1.0450 0.109 Uiso 1 1 calc R . .
C46 C -0.3390(3) 0.3658(2) 0.99127(19) 0.1097(13) Uani 1 1 d . . .
H46A H -0.3542 0.3859 0.9535 0.165 Uiso 1 1 calc R . .
H46B H -0.3813 0.3894 1.0201 0.165 Uiso 1 1 calc R . .
H46C H -0.3544 0.3149 0.9910 0.165 Uiso 1 1 calc R . .
C47 C 0.0250(3) 0.32735(19) 0.87904(13) 0.0772(10) Uani 1 1 d . . .
H47A H -0.0486 0.3282 0.8679 0.093 Uiso 1 1 calc R . .
H47B H 0.0586 0.2903 0.8557 0.093 Uiso 1 1 calc R . .
C48 C 0.0742(4) 0.4024(2) 0.86209(16) 0.1085(14) Uani 1 1 d . . .
H48A H 0.1482 0.3998 0.8721 0.130 Uiso 1 1 calc R . .
H48B H 0.0700 0.4060 0.8199 0.130 Uiso 1 1 calc R . .
C49 C 0.0369(4) 0.4689(3) 0.88447(19) 0.1298(16) Uani 1 1 d . . .
H49A H 0.0509 0.4703 0.9261 0.156 Uiso 1 1 calc R . .
H49B H -0.0386 0.4708 0.8790 0.156 Uiso 1 1 calc R . .
C50 C 0.0839(3) 0.5340(2) 0.85735(17) 0.1032(13) Uani 1 1 d . . .
H50A H 0.1584 0.5338 0.8639 0.155 Uiso 1 1 calc R . .
H50B H 0.0541 0.5767 0.8745 0.155 Uiso 1 1 calc R . .
H50C H 0.0696 0.5338 0.8161 0.155 Uiso 1 1 calc R . .
C51 C 0.1409(3) 0.31662(18) 0.96620(14) 0.0802(10) Uani 1 1 d . . .
H51A H 0.1544 0.3683 0.9670 0.096 Uiso 1 1 calc R . .
H51B H 0.1429 0.2995 1.0062 0.096 Uiso 1 1 calc R . .
C52 C 0.2280(3) 0.2806(2) 0.93329(17) 0.0914(12) Uani 1 1 d . . .
H52A H 0.2236 0.2287 0.9387 0.110 Uiso 1 1 calc R . .
H52B H 0.2198 0.2907 0.8919 0.110 Uiso 1 1 calc R . .
C53 C 0.3308(3) 0.3058(2) 0.95299(17) 0.1020(13) Uani 1 1 d . . .
H53A H 0.3412 0.2909 0.9932 0.122 Uiso 1 1 calc R . .
H53B H 0.3312 0.3583 0.9521 0.122 Uiso 1 1 calc R . .
C54 C 0.4197(3) 0.2791(3) 0.9181(2) 0.1262(16) Uani 1 1 d . . .
H54A H 0.4136 0.2277 0.9131 0.189 Uiso 1 1 calc R . .
H54B H 0.4845 0.2900 0.9379 0.189 Uiso 1 1 calc R . .
H54C H 0.4189 0.3021 0.8805 0.189 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 C2 1.365(3) . ?
C1 N1 1.378(3) . ?
C1 C31 1.513(3) . ?
C2 C3 1.415(4) . ?
C2 H2 0.9400 . ?
C3 C4 1.362(4) . ?
C3 H3 0.9400 . ?
C4 N1 1.372(3) . ?
C4 C5 1.510(3) . ?
C5 C8 1.510(4) . ?
C5 C7 1.542(3) . ?
C5 C6 1.553(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 C9 1.366(3) . ?
C8 N2 1.381(3) . ?
C9 C10 1.411(4) . ?
C9 H9 0.9400 . ?
C10 C11 1.369(3) . ?
C10 H10 0.9400 . ?
C11 N2 1.376(3) . ?
C11 C12 1.511(3) . ?
C12 C20 1.520(3) . ?
C12 C13 1.549(3) . ?
C12 C14 1.550(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 C15 1.393(3) . ?
C14 C19 1.397(3) . ?
C15 C16 1.384(3) . ?
C15 H15 0.9400 . ?
C16 C17 1.370(4) . ?
C16 N6 1.477(3) . ?
C17 C18 1.380(4) . ?
C17 H17 0.9400 . ?
C18 C19 1.378(3) . ?
C18 N5 1.474(4) . ?
C19 H19 0.9400 . ?
C20 C21 1.368(3) . ?
C20 N3 1.381(3) . ?
C21 C22 1.410(4) . ?
C21 H21 0.9400 . ?
C22 C23 1.360(3) . ?
C22 H22 0.9400 . ?
C23 N3 1.376(3) . ?
C23 C24 1.511(4) . ?
C24 C27 1.520(4) . ?
C24 C25 1.547(3) . ?
C24 C26 1.549(4) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C27 C28 1.356(3) . ?
C27 N4 1.375(3) . ?
C28 C29 1.411(4) . ?
C28 H28 0.9400 . ?
C29 C30 1.362(3) . ?
C29 H29 0.9400 . ?
C30 N4 1.384(3) . ?
C30 C31 1.512(3) . ?
C31 C33 1.548(3) . ?
C31 C32 1.552(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C33 C38 1.389(3) . ?
C33 C34 1.397(3) . ?
C34 C35 1.380(3) . ?
C34 H34 0.9400 . ?
C35 C36 1.370(4) . ?
C35 N7 1.478(4) . ?
C36 C37 1.378(4) . ?
C36 H36 0.9400 . ?
N1 H1 0.8700 . ?
N2 H2A 0.8700 . ?
N3 H3A 0.8700 . ?
N4 H4 0.8700 . ?
N5 O1 1.204(3) . ?
N5 O2 1.207(3) . ?
N6 O4 1.219(3) . ?
N6 O3 1.226(3) . ?
N7 O6 1.221(3) . ?
N7 O5 1.221(3) . ?
N8 O8 1.208(3) . ?
N8 O7 1.219(3) . ?
N8 C37 1.471(4) . ?
N9 O10 1.212(3) . ?
N9 O9 1.222(2) . ?
N9 O11 1.235(3) . ?
N10 C43 1.515(4) . ?
N10 C51 1.521(3) . ?
N10 C47 1.524(4) . ?
N10 C39 1.539(4) . ?
C37 C38 1.381(3) . ?
C38 H38 0.9400 . ?
C39 C40 1.515(4) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C40 C41 1.518(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C41 C42 1.522(5) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 H42C 0.9700 . ?
C43 C44 1.517(4) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C44 C45 1.494(4) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C45 C46 1.497(5) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 H46C 0.9700 . ?
C47 C48 1.590(5) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C48 C49 1.430(5) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C49 C50 1.498(5) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C50 H50C 0.9700 . ?
C51 C52 1.517(4) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C52 C53 1.473(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C53 C54 1.493(5) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 H54C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 105.8(2) . . ?
C2 C1 C31 131.6(2) . . ?
N1 C1 C31 122.6(2) . . ?
C1 C2 C3 108.2(2) . . ?
C1 C2 H2 125.9 . . ?
C3 C2 H2 125.9 . . ?
C4 C3 C2 108.4(3) . . ?
C4 C3 H3 125.8 . . ?
C2 C3 H3 125.8 . . ?
C3 C4 N1 106.1(2) . . ?
C3 C4 C5 129.8(3) . . ?
N1 C4 C5 124.0(2) . . ?
C4 C5 C8 113.1(2) . . ?
C4 C5 C7 109.1(2) . . ?
C8 C5 C7 108.2(2) . . ?
C4 C5 C6 109.1(2) . . ?
C8 C5 C6 109.3(2) . . ?
C7 C5 C6 107.9(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N2 106.0(2) . . ?
C9 C8 C5 131.8(2) . . ?
N2 C8 C5 121.9(2) . . ?
C8 C9 C10 108.8(2) . . ?
C8 C9 H9 125.6 . . ?
C10 C9 H9 125.6 . . ?
C11 C10 C9 107.8(2) . . ?
C11 C10 H10 126.1 . . ?
C9 C10 H10 126.1 . . ?
C10 C11 N2 106.6(2) . . ?
C10 C11 C12 130.9(2) . . ?
N2 C11 C12 122.4(2) . . ?
C11 C12 C20 112.32(19) . . ?
C11 C12 C13 108.8(2) . . ?
C20 C12 C13 109.1(2) . . ?
C11 C12 C14 110.86(19) . . ?
C20 C12 C14 108.6(2) . . ?
C13 C12 C14 107.06(19) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 118.3(2) . . ?
C15 C14 C12 122.3(2) . . ?
C19 C14 C12 119.4(2) . . ?
C16 C15 C14 119.0(2) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C17 C16 C15 123.9(2) . . ?
C17 C16 N6 118.1(2) . . ?
C15 C16 N6 118.0(3) . . ?
C16 C17 C18 115.8(2) . . ?
C16 C17 H17 122.1 . . ?
C18 C17 H17 122.1 . . ?
C19 C18 C17 123.0(3) . . ?
C19 C18 N5 118.5(2) . . ?
C17 C18 N5 118.5(2) . . ?
C18 C19 C14 119.9(2) . . ?
C18 C19 H19 120.0 . . ?
C14 C19 H19 120.0 . . ?
C21 C20 N3 106.8(2) . . ?
C21 C20 C12 131.9(2) . . ?
N3 C20 C12 121.3(2) . . ?
C20 C21 C22 107.2(2) . . ?
C20 C21 H21 126.4 . . ?
C22 C21 H21 126.4 . . ?
C23 C22 C21 109.5(2) . . ?
C23 C22 H22 125.2 . . ?
C21 C22 H22 125.2 . . ?
C22 C23 N3 105.8(2) . . ?
C22 C23 C24 132.3(2) . . ?
N3 C23 C24 121.7(2) . . ?
C23 C24 C27 112.9(2) . . ?
C23 C24 C25 108.9(2) . . ?
C27 C24 C25 108.1(2) . . ?
C23 C24 C26 109.6(2) . . ?
C27 C24 C26 109.3(2) . . ?
C25 C24 C26 107.9(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 N4 106.1(2) . . ?
C28 C27 C24 132.2(2) . . ?
N4 C27 C24 121.4(2) . . ?
C27 C28 C29 108.9(2) . . ?
C27 C28 H28 125.6 . . ?
C29 C28 H28 125.6 . . ?
C30 C29 C28 108.0(2) . . ?
C30 C29 H29 126.0 . . ?
C28 C29 H29 126.0 . . ?
C29 C30 N4 106.1(2) . . ?
C29 C30 C31 132.0(2) . . ?
N4 C30 C31 121.8(2) . . ?
C30 C31 C1 112.3(2) . . ?
C30 C31 C33 110.1(2) . . ?
C1 C31 C33 109.75(19) . . ?
C30 C31 C32 108.8(2) . . ?
C1 C31 C32 109.1(2) . . ?
C33 C31 C32 106.6(2) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C38 C33 C34 118.5(2) . . ?
C38 C33 C31 121.6(2) . . ?
C34 C33 C31 119.9(2) . . ?
C35 C34 C33 119.6(3) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C36 C35 C34 123.0(3) . . ?
C36 C35 N7 118.2(3) . . ?
C34 C35 N7 118.8(3) . . ?
C35 C36 C37 116.4(2) . . ?
C35 C36 H36 121.8 . . ?
C37 C36 H36 121.8 . . ?
C4 N1 C1 111.4(2) . . ?
C4 N1 H1 124.3 . . ?
C1 N1 H1 124.3 . . ?
C11 N2 C8 110.8(2) . . ?
C11 N2 H2A 124.6 . . ?
C8 N2 H2A 124.6 . . ?
C23 N3 C20 110.7(2) . . ?
C23 N3 H3A 124.7 . . ?
C20 N3 H3A 124.7 . . ?
C27 N4 C30 110.8(2) . . ?
C27 N4 H4 124.6 . . ?
C30 N4 H4 124.6 . . ?
O1 N5 O2 123.2(3) . . ?
O1 N5 C18 118.3(3) . . ?
O2 N5 C18 118.5(3) . . ?
O4 N6 O3 123.6(3) . . ?
O4 N6 C16 118.5(2) . . ?
O3 N6 C16 117.9(3) . . ?
O6 N7 O5 124.2(3) . . ?
O6 N7 C35 117.7(3) . . ?
O5 N7 C35 118.1(3) . . ?
O8 N8 O7 123.4(3) . . ?
O8 N8 C37 118.4(3) . . ?
O7 N8 C37 118.1(3) . . ?
O10 N9 O9 121.4(2) . . ?
O10 N9 O11 118.0(3) . . ?
O9 N9 O11 120.6(2) . . ?
C43 N10 C51 107.6(2) . . ?
C43 N10 C47 112.0(2) . . ?
C51 N10 C47 110.9(2) . . ?
C43 N10 C39 109.4(2) . . ?
C51 N10 C39 109.7(2) . . ?
C47 N10 C39 107.2(2) . . ?
C36 C37 C38 123.0(3) . . ?
C36 C37 N8 118.1(3) . . ?
C38 C37 N8 118.8(3) . . ?
C37 C38 C33 119.4(2) . . ?
C37 C38 H38 120.3 . . ?
C33 C38 H38 120.3 . . ?
C40 C39 N10 115.5(2) . . ?
C40 C39 H39A 108.4 . . ?
N10 C39 H39A 108.4 . . ?
C40 C39 H39B 108.4 . . ?
N10 C39 H39B 108.4 . . ?
H39A C39 H39B 107.5 . . ?
C39 C40 C41 111.8(3) . . ?
C39 C40 H40A 109.3 . . ?
C41 C40 H40A 109.3 . . ?
C39 C40 H40B 109.3 . . ?
C41 C40 H40B 109.3 . . ?
H40A C40 H40B 107.9 . . ?
C40 C41 C42 112.6(3) . . ?
C40 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
C40 C41 H41B 109.1 . . ?
C42 C41 H41B 109.1 . . ?
H41A C41 H41B 107.8 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N10 C43 C44 115.8(2) . . ?
N10 C43 H43A 108.3 . . ?
C44 C43 H43A 108.3 . . ?
N10 C43 H43B 108.3 . . ?
C44 C43 H43B 108.3 . . ?
H43A C43 H43B 107.4 . . ?
C45 C44 C43 112.9(3) . . ?
C45 C44 H44A 109.0 . . ?
C43 C44 H44A 109.0 . . ?
C45 C44 H44B 109.0 . . ?
C43 C44 H44B 109.0 . . ?
H44A C44 H44B 107.8 . . ?
C44 C45 C46 112.1(3) . . ?
C44 C45 H45A 109.2 . . ?
C46 C45 H45A 109.2 . . ?
C44 C45 H45B 109.2 . . ?
C46 C45 H45B 109.2 . . ?
H45A C45 H45B 107.9 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N10 C47 C48 117.5(2) . . ?
N10 C47 H47A 107.9 . . ?
C48 C47 H47A 107.9 . . ?
N10 C47 H47B 107.9 . . ?
C48 C47 H47B 107.9 . . ?
H47A C47 H47B 107.2 . . ?
C49 C48 C47 122.8(4) . . ?
C49 C48 H48A 106.6 . . ?
C47 C48 H48A 106.6 . . ?
C49 C48 H48B 106.6 . . ?
C47 C48 H48B 106.6 . . ?
H48A C48 H48B 106.6 . . ?
C48 C49 C50 114.6(4) . . ?
C48 C49 H49A 108.6 . . ?
C50 C49 H49A 108.6 . . ?
C48 C49 H49B 108.6 . . ?
C50 C49 H49B 108.6 . . ?
H49A C49 H49B 107.6 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 N10 115.7(2) . . ?
C52 C51 H51A 108.4 . . ?
N10 C51 H51A 108.4 . . ?
C52 C51 H51B 108.4 . . ?
N10 C51 H51B 108.4 . . ?
H51A C51 H51B 107.4 . . ?
C53 C52 C51 111.6(3) . . ?
C53 C52 H52A 109.3 . . ?
C51 C52 H52A 109.3 . . ?
C53 C52 H52B 109.3 . . ?
C51 C52 H52B 109.3 . . ?
H52A C52 H52B 108.0 . . ?
C52 C53 C54 114.6(3) . . ?
C52 C53 H53A 108.6 . . ?
C54 C53 H53A 108.6 . . ?
C52 C53 H53B 108.6 . . ?
C54 C53 H53B 108.6 . . ?
H53A C53 H53B 107.6 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.041
####################################################################### 
# 
# 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_TBAOAc-DNPC4P
_database_code_depnum_ccdc_archive 'CCDC 1482092'
_audit_update_record             
;
2016-05-26 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Cis-Dinitrophenyl-calix[4]pyrrole-etrabutylammonium acetate
;
_chemical_name_common            Cis-DNP-Calix[4]pyrrole-TBAOAc
_chemical_melting_point          'C38 H36 N8 O8, C16 H36 N, C2 H3 O2'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H75 N9 O10'
_chemical_formula_weight         1034.25

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   P21/n

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

_cell_length_a                   12.773(4)
_cell_length_b                   19.067(6)
_cell_length_c                   23.221(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.690(4)
_cell_angle_gamma                90.00
_cell_volume                     5653(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    9527
_cell_measurement_theta_min      1.7976
_cell_measurement_theta_max      27.4778

_exptl_crystal_description       Parism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2216
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9833
_exptl_absorpt_correction_T_max  0.9941
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku SCX-Mini with Mercury CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31728
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9943
_reflns_number_gt                6834
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_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)+(0.0300P)²+3.5409P] 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_number_reflns         9943
_refine_ls_number_parameters     687
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0636
_refine_ls_wR_factor_ref         0.1492
_refine_ls_wR_factor_gt          0.1269
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_restrained_S_all      1.196
_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 0.7371(2) 0.33084(15) 0.21467(12) 0.0446(7) Uani 1 1 d . . .
C2 C 0.7916(2) 0.39062(17) 0.22956(14) 0.0590(8) Uani 1 1 d . . .
H2 H 0.8604 0.3922 0.2450 0.071 Uiso 1 1 calc R . .
C3 C 0.7267(2) 0.44939(16) 0.21766(13) 0.0542(8) Uani 1 1 d . . .
H3 H 0.7450 0.4967 0.2234 0.065 Uiso 1 1 calc R . .
C4 C 0.6322(2) 0.42512(14) 0.19618(11) 0.0421(6) Uani 1 1 d . . .
C5 C 0.5363(2) 0.46362(13) 0.17271(11) 0.0404(6) Uani 1 1 d . . .
C6 C 0.5104(2) 0.44134(13) 0.11007(11) 0.0394(6) Uani 1 1 d . . .
C7 C 0.5865(2) 0.41246(14) 0.07508(12) 0.0437(7) Uani 1 1 d . . .
H7 H 0.6547 0.4045 0.0899 0.052 Uiso 1 1 calc R . .
C8 C 0.5603(2) 0.39571(14) 0.01832(12) 0.0467(7) Uani 1 1 d . . .
C9 C 0.4620(2) 0.40608(15) -0.00635(12) 0.0493(7) Uani 1 1 d . . .
H9 H 0.4460 0.3943 -0.0449 0.059 Uiso 1 1 calc R . .
C10 C 0.3884(2) 0.43481(14) 0.02917(12) 0.0454(7) Uani 1 1 d . . .
C11 C 0.4104(2) 0.45229(14) 0.08606(12) 0.0434(6) Uani 1 1 d . . .
H11 H 0.3577 0.4716 0.1086 0.052 Uiso 1 1 calc R . .
C12 C 0.5617(3) 0.54326(14) 0.17087(13) 0.0554(8) Uani 1 1 d . . .
H12A H 0.5794 0.5597 0.2095 0.083 Uiso 1 1 calc R . .
H12B H 0.5011 0.5687 0.1558 0.083 Uiso 1 1 calc R . .
H12C H 0.6205 0.5511 0.1462 0.083 Uiso 1 1 calc R . .
C13 C 0.4408(2) 0.45301(13) 0.20905(11) 0.0392(6) Uani 1 1 d . . .
C14 C 0.3874(2) 0.49865(15) 0.24279(13) 0.0551(8) Uani 1 1 d . . .
H14 H 0.4039 0.5461 0.2493 0.066 Uiso 1 1 calc R . .
C15 C 0.3026(2) 0.46144(15) 0.26608(14) 0.0568(8) Uani 1 1 d . . .
H15 H 0.2532 0.4800 0.2912 0.068 Uiso 1 1 calc R . .
C16 C 0.3046(2) 0.39389(14) 0.24597(11) 0.0416(6) Uani 1 1 d . . .
C17 C 0.2274(2) 0.33456(15) 0.25342(12) 0.0447(7) Uani 1 1 d . . .
C18 C 0.1364(2) 0.36130(18) 0.28982(14) 0.0644(9) Uani 1 1 d . . .
H18A H 0.1632 0.3750 0.3277 0.097 Uiso 1 1 calc R . .
H18B H 0.0850 0.3243 0.2937 0.097 Uiso 1 1 calc R . .
H18C H 0.1037 0.4014 0.2709 0.097 Uiso 1 1 calc R . .
C19 C 0.1819(2) 0.31220(17) 0.19366(13) 0.0569(8) Uani 1 1 d . . .
H19A H 0.1464 0.3518 0.1755 0.085 Uiso 1 1 calc R . .
H19B H 0.1325 0.2741 0.1984 0.085 Uiso 1 1 calc R . .
H19C H 0.2383 0.2967 0.1696 0.085 Uiso 1 1 calc R . .
C20 C 0.2759(2) 0.27090(14) 0.28351(12) 0.0437(7) Uani 1 1 d . . .
C21 C 0.2473(2) 0.23500(17) 0.33161(13) 0.0579(8) Uani 1 1 d . . .
H21 H 0.1954 0.2488 0.3571 0.069 Uiso 1 1 calc R . .
C22 C 0.3091(2) 0.17354(17) 0.33647(13) 0.0552(8) Uani 1 1 d . . .
H22 H 0.3053 0.1395 0.3656 0.066 Uiso 1 1 calc R . .
C23 C 0.3752(2) 0.17230(14) 0.29141(11) 0.0418(6) Uani 1 1 d . . .
C24 C 0.4540(2) 0.11747(13) 0.27319(11) 0.0407(6) Uani 1 1 d . . .
C25 C 0.4290(2) 0.09149(13) 0.21140(11) 0.0420(6) Uani 1 1 d . . .
C26 C 0.3329(2) 0.10390(14) 0.18303(12) 0.0454(7) Uani 1 1 d . . .
H26 H 0.2813 0.1305 0.2010 0.054 Uiso 1 1 calc R . .
C27 C 0.3139(2) 0.07674(15) 0.12815(12) 0.0496(7) Uani 1 1 d . . .
C28 C 0.3861(3) 0.03707(15) 0.09950(13) 0.0556(8) Uani 1 1 d . . .
H28 H 0.3722 0.0192 0.0623 0.067 Uiso 1 1 calc R . .
C29 C 0.4800(3) 0.02522(15) 0.12874(13) 0.0531(8) Uani 1 1 d . . .
C30 C 0.5034(2) 0.05128(14) 0.18303(12) 0.0487(7) Uani 1 1 d . . .
H30 H 0.5689 0.0421 0.2009 0.058 Uiso 1 1 calc R . .
C31 C 0.4450(3) 0.05283(15) 0.31337(13) 0.0564(8) Uani 1 1 d . . .
H31A H 0.4590 0.0670 0.3530 0.085 Uiso 1 1 calc R . .
H31B H 0.4955 0.0175 0.3025 0.085 Uiso 1 1 calc R . .
H31C H 0.3748 0.0335 0.3097 0.085 Uiso 1 1 calc R . .
C32 C 0.5657(2) 0.14469(13) 0.27726(11) 0.0402(6) Uani 1 1 d . . .
C33 C 0.6475(2) 0.12854(14) 0.31425(12) 0.0457(7) Uani 1 1 d . . .
H33 H 0.6457 0.0969 0.3452 0.055 Uiso 1 1 calc R . .
C34 C 0.7355(2) 0.16806(15) 0.29745(13) 0.0506(7) Uani 1 1 d . . .
H34 H 0.8022 0.1674 0.3156 0.061 Uiso 1 1 calc R . .
C35 C 0.7064(2) 0.20752(14) 0.25005(12) 0.0439(7) Uani 1 1 d . . .
C36 C 0.7711(2) 0.25461(15) 0.21229(13) 0.0494(7) Uani 1 1 d . . .
C37 C 0.8871(2) 0.24958(19) 0.23227(16) 0.0717(10) Uani 1 1 d . . .
H37A H 0.9291 0.2793 0.2082 0.108 Uiso 1 1 calc R . .
H37B H 0.9106 0.2014 0.2292 0.108 Uiso 1 1 calc R . .
H37C H 0.8945 0.2649 0.2720 0.108 Uiso 1 1 calc R . .
C38 C 0.7615(3) 0.22860(18) 0.14933(14) 0.0656(9) Uani 1 1 d . . .
H38A H 0.6892 0.2323 0.1357 0.098 Uiso 1 1 calc R . .
H38B H 0.7839 0.1801 0.1475 0.098 Uiso 1 1 calc R . .
H38C H 0.8054 0.2571 0.1253 0.098 Uiso 1 1 calc R . .
C39 C 0.5019(3) 0.20284(17) 0.06935(13) 0.0623(9) Uani 1 1 d . . .
H39A H 0.4601 0.1782 0.0403 0.093 Uiso 1 1 calc R . .
H39B H 0.5388 0.1691 0.0938 0.093 Uiso 1 1 calc R . .
H39C H 0.5522 0.2327 0.0507 0.093 Uiso 1 1 calc R . .
C40 C 0.4309(2) 0.24743(15) 0.10575(12) 0.0457(7) Uani 1 1 d . . .
N1 N 0.63936(17) 0.35275(11) 0.19497(9) 0.0420(5) Uani 1 1 d . . .
H1 H 0.5892 0.3248 0.1834 0.050 Uiso 1 1 calc R . .
N2 N 0.38972(16) 0.38922(11) 0.21124(9) 0.0386(5) Uani 1 1 d . . .
H2A H 0.4087 0.3515 0.1932 0.046 Uiso 1 1 calc R . .
N3 N 0.35565(16) 0.23259(11) 0.25964(9) 0.0399(5) Uani 1 1 d . . .
H3A H 0.3889 0.2447 0.2290 0.048 Uiso 1 1 calc R . .
N4 N 0.60213(16) 0.19302(11) 0.23820(9) 0.0419(5) Uani 1 1 d . . .
H4 H 0.5647 0.2116 0.2102 0.050 Uiso 1 1 calc R . .
N5 N 0.6411(2) 0.36410(15) -0.01751(13) 0.0635(7) Uani 1 1 d . . .
N6 N 0.2818(2) 0.44696(15) 0.00493(12) 0.0629(7) Uani 1 1 d . . .
N7 N 0.2114(2) 0.09030(15) 0.09924(13) 0.0656(8) Uani 1 1 d . . .
N8 N 0.5607(3) -0.01671(16) 0.09939(14) 0.0780(9) Uani 1 1 d . . .
O1 O 0.7164(2) 0.33607(16) 0.00694(12) 0.0927(9) Uani 1 1 d . . .
O2 O 0.6277(2) 0.36664(16) -0.06974(11) 0.0921(9) Uani 1 1 d . . .
O3 O 0.2604(2) 0.42655(15) -0.04385(11) 0.0864(8) Uani 1 1 d . . .
O4 O 0.2196(2) 0.47763(18) 0.03466(12) 0.1070(11) Uani 1 1 d . . .
O5 O 0.6445(3) -0.0249(2) 0.12391(16) 0.1466(17) Uani 1 1 d . . .
O6 O 0.5392(3) -0.04109(16) 0.05236(12) 0.1030(10) Uani 1 1 d . . .
O7 O 0.1930(2) 0.06215(14) 0.05246(11) 0.0900(8) Uani 1 1 d . . .
O8 O 0.1496(2) 0.12898(16) 0.12284(12) 0.0892(8) Uani 1 1 d . . .
N9 N 0.0679(2) 0.21397(15) 0.94486(12) 0.0688(8) Uani 1 1 d . . .
C1A C 0.0008(3) 0.16683(18) 0.98093(15) 0.0680(9) Uani 1 1 d . . .
H1A1 H 0.0126 0.1792 1.0216 0.082 Uiso 1 1 calc R . .
H1A2 H 0.0242 0.1183 0.9760 0.082 Uiso 1 1 calc R . .
C2A C -0.1156(3) 0.17019(19) 0.96707(16) 0.0717(10) Uani 1 1 d . . .
H2A1 H -0.1415 0.2175 0.9750 0.086 Uiso 1 1 calc R . .
H2A2 H -0.1284 0.1603 0.9261 0.086 Uiso 1 1 calc R . .
C3A C -0.1743(3) 0.1171(2) 1.00305(18) 0.0906(13) Uani 1 1 d . . .
H3A1 H -0.1610 0.1270 1.0440 0.109 Uiso 1 1 calc R . .
H3A2 H -0.1480 0.0699 0.9951 0.109 Uiso 1 1 calc R . .
C4A C -0.2899(4) 0.1193(3) 0.9902(2) 0.1229(19) Uani 1 1 d . . .
H4A1 H -0.3160 0.1662 0.9972 0.184 Uiso 1 1 calc R . .
H4A2 H -0.3250 0.0863 1.0149 0.184 Uiso 1 1 calc R . .
H4A3 H -0.3036 0.1068 0.9502 0.184 Uiso 1 1 calc R . .
C5A C 0.0617(3) 0.1925(2) 0.88159(17) 0.0876(13) Uani 1 1 d . . .
H5A1 H 0.1011 0.2269 0.8595 0.105 Uiso 1 1 calc R . .
H5A2 H -0.0117 0.1954 0.8682 0.105 Uiso 1 1 calc R . .
C6A C 0.1042(4) 0.1167(3) 0.8668(2) 0.1157(17) Uani 1 1 d . . .
H6A1 H 0.1339 0.1183 0.8284 0.139 Uiso 1 1 calc R . .
H6A2 H 0.1615 0.1055 0.8943 0.139 Uiso 1 1 calc R . .
C7A C 0.0311(4) 0.0622(4) 0.8677(2) 0.143(2) Uani 1 1 d . . .
H7A1 H -0.0256 0.0717 0.8395 0.171 Uiso 1 1 calc R . .
H7A2 H 0.0008 0.0596 0.9059 0.171 Uiso 1 1 calc R . .
C8A C 0.0852(4) -0.0104(2) 0.85310(19) 0.1061(15) Uani 1 1 d . . .
H8A1 H 0.1109 -0.0089 0.8142 0.159 Uiso 1 1 calc R . .
H8A2 H 0.0345 -0.0480 0.8560 0.159 Uiso 1 1 calc R . .
H8A3 H 0.1433 -0.0188 0.8801 0.159 Uiso 1 1 calc R . .
C9A C 0.0301(3) 0.28987(17) 0.94820(15) 0.0654(9) Uani 1 1 d . . .
H9A1 H 0.0781 0.3194 0.9267 0.078 Uiso 1 1 calc R . .
H9A2 H -0.0389 0.2929 0.9288 0.078 Uiso 1 1 calc R . .
C10A C 0.0218(3) 0.31987(19) 1.00835(16) 0.0772(10) Uani 1 1 d . . .
H10A H 0.0917 0.3219 1.0268 0.093 Uiso 1 1 calc R . .
H10B H -0.0216 0.2889 1.0314 0.093 Uiso 1 1 calc R . .
C11A C -0.0259(3) 0.39294(19) 1.00705(17) 0.0788(11) Uani 1 1 d . . .
H11A H 0.0209 0.4247 0.9868 0.095 Uiso 1 1 calc R . .
H11B H -0.0928 0.3914 0.9854 0.095 Uiso 1 1 calc R . .
C12A C -0.0440(4) 0.4218(2) 1.06699(19) 0.1042(14) Uani 1 1 d . . .
H12D H -0.0872 0.3894 1.0880 0.156 Uiso 1 1 calc R . .
H12E H -0.0791 0.4668 1.0638 0.156 Uiso 1 1 calc R . .
H12F H 0.0228 0.4277 1.0874 0.156 Uiso 1 1 calc R . .
C13A C 0.1794(3) 0.2079(2) 0.97054(19) 0.0908(13) Uani 1 1 d . . .
H13A H 0.1794 0.2265 1.0099 0.109 Uiso 1 1 calc R . .
H13B H 0.1971 0.1579 0.9734 0.109 Uiso 1 1 calc R . .
C14A C 0.2660(3) 0.2445(3) 0.9385(3) 0.138(2) Uani 1 1 d . . .
H14A H 0.2341 0.2651 0.9035 0.165 Uiso 1 1 calc R . .
H14B H 0.2912 0.2834 0.9627 0.165 Uiso 1 1 calc R . .
C15A C 0.3484(4) 0.2086(3) 0.9231(3) 0.140(2) Uani 1 1 d . . .
H15A H 0.3226 0.1764 0.8929 0.168 Uiso 1 1 calc R . .
H15B H 0.3675 0.1792 0.9563 0.168 Uiso 1 1 calc R . .
C16A C 0.4478(3) 0.2362(2) 0.90231(16) 0.0858(12) Uani 1 1 d . . .
H16A H 0.4350 0.2799 0.8819 0.129 Uiso 1 1 calc R . .
H16B H 0.4784 0.2025 0.8765 0.129 Uiso 1 1 calc R . .
H16C H 0.4956 0.2445 0.9348 0.129 Uiso 1 1 calc R . .
O9 O 0.46778(13) 0.26413(9) 0.15630(7) 0.0394(4) Uani 1 1 d . . .
O10 O 0.3458(2) 0.26593(18) 0.08655(10) 0.1012(10) Uani 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
C1 C2 1.374(4) . ?
C1 N1 1.382(3) . ?
C1 C36 1.518(4) . ?
C2 C3 1.417(4) . ?
C2 H2 0.9400 . ?
C3 C4 1.373(4) . ?
C3 H3 0.9400 . ?
C4 N1 1.383(3) . ?
C4 C5 1.516(4) . ?
C5 C13 1.516(4) . ?
C5 C6 1.542(4) . ?
C5 C12 1.554(4) . ?
C6 C7 1.399(4) . ?
C6 C11 1.394(4) . ?
C7 C8 1.388(4) . ?
C7 H7 0.9400 . ?
C8 C9 1.379(4) . ?
C8 N5 1.474(4) . ?
C9 C10 1.382(4) . ?
C9 H9 0.9400 . ?
C10 C11 1.383(4) . ?
C10 N6 1.476(4) . ?
C11 H11 0.9400 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 C14 1.367(4) . ?
C13 N2 1.382(3) . ?
C14 C15 1.415(4) . ?
C14 H14 0.9400 . ?
C15 C16 1.370(4) . ?
C15 H15 0.9400 . ?
C16 N2 1.376(3) . ?
C16 C17 1.514(4) . ?
C17 C20 1.523(4) . ?
C17 C18 1.544(4) . ?
C17 C19 1.549(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 C21 1.369(4) . ?
C20 N3 1.383(3) . ?
C21 C22 1.415(4) . ?
C21 H21 0.9400 . ?
C22 C23 1.364(4) . ?
C22 H22 0.9400 . ?
C23 N3 1.385(3) . ?
C23 C24 1.520(4) . ?
C24 C32 1.520(4) . ?
C24 C25 1.542(4) . ?
C24 C31 1.552(4) . ?
C25 C30 1.400(4) . ?
C25 C26 1.396(4) . ?
C26 C27 1.390(4) . ?
C26 H26 0.9400 . ?
C27 C28 1.379(4) . ?
C27 N7 1.476(4) . ?
C28 C29 1.379(4) . ?
C28 H28 0.9400 . ?
C29 C30 1.379(4) . ?
C29 N8 1.486(4) . ?
C30 H30 0.9400 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C32 C33 1.368(4) . ?
C32 N4 1.383(3) . ?
C33 C34 1.417(4) . ?
C33 H33 0.9400 . ?
C34 C35 1.375(4) . ?
C34 H34 0.9400 . ?
C35 N4 1.380(3) . ?
C35 C36 1.517(4) . ?
C36 C38 1.545(4) . ?
C36 C37 1.543(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 C40 1.518(4) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C40 O10 1.215(3) . ?
C40 O9 1.292(3) . ?
N1 H1 0.8700 . ?
N2 H2A 0.8700 . ?
N3 H3A 0.8700 . ?
N4 H4 0.8700 . ?
N5 O2 1.221(3) . ?
N5 O1 1.225(4) . ?
N6 O4 1.217(3) . ?
N6 O3 1.221(3) . ?
N7 O8 1.222(4) . ?
N7 O7 1.228(3) . ?
N8 O6 1.211(4) . ?
N8 O5 1.208(4) . ?
N9 C1A 1.512(4) . ?
N9 C9A 1.528(4) . ?
N9 C5A 1.525(5) . ?
N9 C13A 1.532(4) . ?
C1A C2A 1.513(5) . ?
C1A H1A1 0.9800 . ?
C1A H1A2 0.9800 . ?
C2A C3A 1.524(5) . ?
C2A H2A1 0.9800 . ?
C2A H2A2 0.9800 . ?
C3A C4A 1.499(6) . ?
C3A H3A1 0.9800 . ?
C3A H3A2 0.9800 . ?
C4A H4A1 0.9700 . ?
C4A H4A2 0.9700 . ?
C4A H4A3 0.9700 . ?
C5A C6A 1.585(6) . ?
C5A H5A1 0.9800 . ?
C5A H5A2 0.9800 . ?
C6A C7A 1.398(6) . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C7A C8A 1.590(7) . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C8A H8A3 0.9700 . ?
C9A C10A 1.516(5) . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C10A C11A 1.520(5) . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C11A C12A 1.521(5) . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C12A H12D 0.9700 . ?
C12A H12E 0.9700 . ?
C12A H12F 0.9700 . ?
C13A C14A 1.521(5) . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C14A C15A 1.314(5) . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C15A C16A 1.469(5) . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C16A H16A 0.9700 . ?
C16A H16B 0.9700 . ?
C16A H16C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 106.2(3) . . ?
C2 C1 C36 131.3(3) . . ?
N1 C1 C36 122.2(2) . . ?
C1 C2 C3 108.5(3) . . ?
C1 C2 H2 125.7 . . ?
C3 C2 H2 125.7 . . ?
C4 C3 C2 107.9(3) . . ?
C4 C3 H3 126.0 . . ?
C2 C3 H3 126.0 . . ?
C3 C4 N1 106.6(2) . . ?
C3 C4 C5 131.3(3) . . ?
N1 C4 C5 122.0(2) . . ?
C4 C5 C13 112.9(2) . . ?
C4 C5 C6 110.8(2) . . ?
C13 C5 C6 109.5(2) . . ?
C4 C5 C12 108.4(2) . . ?
C13 C5 C12 108.5(2) . . ?
C6 C5 C12 106.4(2) . . ?
C7 C6 C11 118.1(2) . . ?
C7 C6 C5 121.5(2) . . ?
C11 C6 C5 120.3(2) . . ?
C8 C7 C6 119.3(3) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C9 C8 C7 123.6(3) . . ?
C9 C8 N5 118.0(3) . . ?
C7 C8 N5 118.5(3) . . ?
C10 C9 C8 115.9(3) . . ?
C10 C9 H9 122.1 . . ?
C8 C9 H9 122.1 . . ?
C9 C10 C11 122.9(3) . . ?
C9 C10 N6 118.1(3) . . ?
C11 C10 N6 119.0(3) . . ?
C10 C11 C6 120.3(3) . . ?
C10 C11 H11 119.9 . . ?
C6 C11 H11 119.9 . . ?
C5 C12 H12A 109.5 . . ?
C5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N2 107.1(2) . . ?
C14 C13 C5 131.1(2) . . ?
N2 C13 C5 121.8(2) . . ?
C13 C14 C15 107.5(3) . . ?
C13 C14 H14 126.3 . . ?
C15 C14 H14 126.3 . . ?
C16 C15 C14 108.6(3) . . ?
C16 C15 H15 125.7 . . ?
C14 C15 H15 125.7 . . ?
C15 C16 N2 106.4(2) . . ?
C15 C16 C17 130.2(2) . . ?
N2 C16 C17 123.2(2) . . ?
C16 C17 C20 113.0(2) . . ?
C16 C17 C18 108.6(2) . . ?
C20 C17 C18 108.3(2) . . ?
C16 C17 C19 109.4(2) . . ?
C20 C17 C19 109.2(2) . . ?
C18 C17 C19 108.2(2) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N3 106.3(2) . . ?
C21 C20 C17 131.2(2) . . ?
N3 C20 C17 122.1(2) . . ?
C20 C21 C22 108.5(3) . . ?
C20 C21 H21 125.7 . . ?
C22 C21 H21 125.7 . . ?
C23 C22 C21 108.0(3) . . ?
C23 C22 H22 126.0 . . ?
C21 C22 H22 126.0 . . ?
C22 C23 N3 106.8(2) . . ?
C22 C23 C24 131.0(2) . . ?
N3 C23 C24 122.2(2) . . ?
C23 C24 C32 112.1(2) . . ?
C23 C24 C25 111.1(2) . . ?
C32 C24 C25 109.6(2) . . ?
C23 C24 C31 108.5(2) . . ?
C32 C24 C31 108.6(2) . . ?
C25 C24 C31 106.7(2) . . ?
C30 C25 C26 118.0(3) . . ?
C30 C25 C24 119.3(2) . . ?
C26 C25 C24 122.6(3) . . ?
C27 C26 C25 119.8(3) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C28 C27 C26 123.0(3) . . ?
C28 C27 N7 118.3(3) . . ?
C26 C27 N7 118.7(3) . . ?
C27 C28 C29 115.9(3) . . ?
C27 C28 H28 122.1 . . ?
C29 C28 H28 122.1 . . ?
C30 C29 C28 123.6(3) . . ?
C30 C29 N8 118.6(3) . . ?
C28 C29 N8 117.8(3) . . ?
C29 C30 C25 119.7(3) . . ?
C29 C30 H30 120.1 . . ?
C25 C30 H30 120.1 . . ?
C24 C31 H31A 109.5 . . ?
C24 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C24 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 N4 107.3(2) . . ?
C33 C32 C24 131.4(2) . . ?
N4 C32 C24 121.3(2) . . ?
C32 C33 C34 107.7(3) . . ?
C32 C33 H33 126.1 . . ?
C34 C33 H33 126.1 . . ?
C35 C34 C33 108.3(3) . . ?
C35 C34 H34 125.9 . . ?
C33 C34 H34 125.9 . . ?
C34 C35 N4 106.6(2) . . ?
C34 C35 C36 130.4(3) . . ?
N4 C35 C36 122.8(2) . . ?
C1 C36 C35 112.6(2) . . ?
C1 C36 C38 109.1(2) . . ?
C35 C36 C38 109.1(2) . . ?
C1 C36 C37 108.7(2) . . ?
C35 C36 C37 108.9(2) . . ?
C38 C36 C37 108.3(2) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 H39A 109.5 . . ?
C40 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C40 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O10 C40 O9 124.1(3) . . ?
O10 C40 C39 120.1(3) . . ?
O9 C40 C39 115.9(3) . . ?
C1 N1 C4 110.8(2) . . ?
C1 N1 H1 124.6 . . ?
C4 N1 H1 124.6 . . ?
C16 N2 C13 110.3(2) . . ?
C16 N2 H2A 124.8 . . ?
C13 N2 H2A 124.8 . . ?
C20 N3 C23 110.4(2) . . ?
C20 N3 H3A 124.8 . . ?
C23 N3 H3A 124.8 . . ?
C32 N4 C35 110.1(2) . . ?
C32 N4 H4 125.0 . . ?
C35 N4 H4 125.0 . . ?
O2 N5 O1 124.3(3) . . ?
O2 N5 C8 117.7(3) . . ?
O1 N5 C8 118.1(3) . . ?
O4 N6 O3 123.2(3) . . ?
O4 N6 C10 118.0(3) . . ?
O3 N6 C10 118.8(3) . . ?
O8 N7 O7 123.4(3) . . ?
O8 N7 C27 118.6(3) . . ?
O7 N7 C27 118.1(3) . . ?
O6 N8 O5 123.3(3) . . ?
O6 N8 C29 118.6(3) . . ?
O5 N8 C29 118.1(3) . . ?
C1A N9 C9A 110.4(2) . . ?
C1A N9 C5A 111.1(3) . . ?
C9A N9 C5A 107.2(2) . . ?
C1A N9 C13A 106.0(2) . . ?
C9A N9 C13A 110.1(3) . . ?
C5A N9 C13A 112.1(3) . . ?
N9 C1A C2A 115.3(3) . . ?
N9 C1A H1A1 108.5 . . ?
C2A C1A H1A1 108.5 . . ?
N9 C1A H1A2 108.5 . . ?
C2A C1A H1A2 108.5 . . ?
H1A1 C1A H1A2 107.5 . . ?
C3A C2A C1A 110.6(3) . . ?
C3A C2A H2A1 109.5 . . ?
C1A C2A H2A1 109.5 . . ?
C3A C2A H2A2 109.5 . . ?
C1A C2A H2A2 109.5 . . ?
H2A1 C2A H2A2 108.1 . . ?
C2A C3A C4A 111.7(4) . . ?
C2A C3A H3A1 109.3 . . ?
C4A C3A H3A1 109.3 . . ?
C2A C3A H3A2 109.3 . . ?
C4A C3A H3A2 109.3 . . ?
H3A1 C3A H3A2 107.9 . . ?
C3A C4A H4A1 109.5 . . ?
C3A C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C3A C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
N9 C5A C6A 116.4(3) . . ?
N9 C5A H5A1 108.2 . . ?
C6A C5A H5A1 108.2 . . ?
N9 C5A H5A2 108.2 . . ?
C6A C5A H5A2 108.2 . . ?
H5A1 C5A H5A2 107.4 . . ?
C7A C6A C5A 116.2(5) . . ?
C7A C6A H6A1 108.2 . . ?
C5A C6A H6A1 108.2 . . ?
C7A C6A H6A2 108.2 . . ?
C5A C6A H6A2 108.2 . . ?
H6A1 C6A H6A2 107.4 . . ?
C6A C7A C8A 110.5(5) . . ?
C6A C7A H7A1 109.6 . . ?
C8A C7A H7A1 109.6 . . ?
C6A C7A H7A2 109.6 . . ?
C8A C7A H7A2 109.6 . . ?
H7A1 C7A H7A2 108.1 . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C10A C9A N9 115.8(3) . . ?
C10A C9A H9A1 108.3 . . ?
N9 C9A H9A1 108.3 . . ?
C10A C9A H9A2 108.3 . . ?
N9 C9A H9A2 108.3 . . ?
H9A1 C9A H9A2 107.4 . . ?
C9A C10A C11A 111.5(3) . . ?
C9A C10A H10A 109.3 . . ?
C11A C10A H10A 109.3 . . ?
C9A C10A H10B 109.3 . . ?
C11A C10A H10B 109.3 . . ?
H10A C10A H10B 108.0 . . ?
C12A C11A C10A 112.6(3) . . ?
C12A C11A H11A 109.1 . . ?
C10A C11A H11A 109.1 . . ?
C12A C11A H11B 109.1 . . ?
C10A C11A H11B 109.1 . . ?
H11A C11A H11B 107.8 . . ?
C11A C12A H12D 109.5 . . ?
C11A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C11A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C14A C13A N9 117.1(3) . . ?
C14A C13A H13A 108.0 . . ?
N9 C13A H13A 108.0 . . ?
C14A C13A H13B 108.0 . . ?
N9 C13A H13B 108.0 . . ?
H13A C13A H13B 107.3 . . ?
C15A C14A C13A 119.7(4) . . ?
C15A C14A H14A 107.4 . . ?
C13A C14A H14A 107.4 . . ?
C15A C14A H14B 107.4 . . ?
C13A C14A H14B 107.4 . . ?
H14A C14A H14B 106.9 . . ?
C14A C15A C16A 127.6(5) . . ?
C14A C15A H15A 105.4 . . ?
C16A C15A H15A 105.4 . . ?
C14A C15A H15B 105.4 . . ?
C16A C15A H15B 105.4 . . ?
H15A C15A H15B 106.0 . . ?
C15A C16A H16A 109.5 . . ?
C15A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C15A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.046
