# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_Uc1_free
_database_code_depnum_ccdc_archive 'CCDC 1534255'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-06-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_Uc1_free            
;
PROBLEM: Short Inter D...A Contact  O3S    ..  O3S     ..       2.42 Ang.
RESPONSE: The crystal structure contains disordered p-nitrophenyl substituent and partially occupied solvent molecules such as disordered n-pentan, water, and methanol molecules. All of the oxygen-containing solvent molecules, except the water molecule located within macrocyclic cavity, were refinement without the hydrogen atoms. It is noteworthy that, the exact dimensions and cell volume should be probably doubled (i.e.: a = 8.214 \%A, b = 19.363 \%A, c = 23.930 \%A, ? = 109.07\%, ? = 97.28\%, ? = 93.34\%, V = 3547.71 \%A3) as compared to the data mentioned in the cif file. However, since the reflections proving this assumption were weak, the final structure was refinement as the average from two smaller elemental cells.
;
# Added during the CSD deposition process: Wednesday 22 February 2017 05:32 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '22-membered pentamide Unclosed Cryptand'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H33.25 N7 O13.10'
_chemical_formula_weight         701.49

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.2136(7)
_cell_length_b                   10.2940(9)
_cell_length_c                   22.413(2)
_cell_angle_alpha                85.572(7)
_cell_angle_beta                 88.689(9)
_cell_angle_gamma                69.865(5)
_cell_volume                     1773.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8543
_cell_measurement_theta_min      3
_cell_measurement_theta_max      29

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             734
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.6479
_diffrn_standards_number         '1 frame'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        2
_diffrn_reflns_number            33596
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         28.62
_reflns_number_total             8543
_reflns_number_gt                6232
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL-97

_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)+(0.1176P)²+0.0693P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8543
_refine_ls_number_parameters     599
_refine_ls_number_restraints     502
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1744
_refine_ls_wR_factor_gt          0.1631
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.083
_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
O4 O 0.41728(14) 0.58648(11) 0.18497(5) 0.0205(2) Uani 1 1 d . . .
O6 O 0.14966(14) 0.71277(12) 0.05299(5) 0.0235(3) Uani 1 1 d . . .
O11 O 0.34422(17) 1.14966(14) -0.00349(5) 0.0335(3) Uani 1 1 d . . .
O18 O 0.6615(2) 1.25845(13) 0.26855(6) 0.0392(3) Uani 1 1 d . . .
O23 O 1.0364(2) 0.89530(19) 0.31224(7) 0.0580(5) Uani 1 1 d . . .
O25 O 0.87932(14) 0.61666(12) 0.29371(5) 0.0246(3) Uani 1 1 d . . .
O30 O 0.51441(15) 0.73778(11) 0.33797(5) 0.0251(3) Uani 1 1 d . A .
N7 N 0.17474(16) 0.82556(13) 0.13335(6) 0.0195(3) Uani 1 1 d . . .
H7 H 0.2223 0.8193 0.1687 0.023 Uiso 1 1 calc R . .
N10 N 0.27494(18) 1.06395(14) 0.08547(6) 0.0229(3) Uani 1 1 d . . .
H10 H 0.3007 1.0444 0.1238 0.027 Uiso 1 1 calc R . .
N17 N 0.49749(17) 1.15364(13) 0.14293(6) 0.0212(3) Uani 1 1 d . . .
N19 N 0.5317(2) 1.09800(15) 0.26308(6) 0.0316(4) Uani 1 1 d . . .
H19 H 0.4933 1.0498 0.2397 0.038 Uiso 1 1 calc R . .
N22 N 0.7811(2) 0.86759(15) 0.33741(6) 0.0298(3) Uani 1 1 d . . .
H22 H 0.7228 0.8100 0.3388 0.036 Uiso 1 1 calc R . .
N29 N 0.59423(16) 0.54306(13) 0.28744(6) 0.0185(3) Uani 1 1 d . A .
H29 H 0.6031 0.4553 0.2879 0.022 Uiso 1 1 calc R . .
C1 C 0.7939(2) 0.64945(16) 0.23958(7) 0.0195(3) Uani 1 1 d . . .
C2 C 0.65027(19) 0.60663(15) 0.23630(6) 0.0173(3) Uani 1 1 d . . .
C3 C 0.55991(19) 0.62786(15) 0.18238(7) 0.0176(3) Uani 1 1 d . . .
C5 C 0.3399(2) 0.57768(16) 0.12996(7) 0.0212(3) Uani 1 1 d . . .
H5A H 0.2781 0.5106 0.1367 0.025 Uiso 1 1 calc R . .
H5B H 0.4335 0.5398 0.1008 0.025 Uiso 1 1 calc R . .
C6 C 0.21336(19) 0.71332(16) 0.10209(7) 0.0186(3) Uani 1 1 d . . .
C8 C 0.0540(2) 0.95824(16) 0.10897(8) 0.0241(3) Uani 1 1 d . . .
H8A H 0.0125 1.0206 0.1418 0.029 Uiso 1 1 calc R . .
H8B H -0.0477 0.9432 0.0920 0.029 Uiso 1 1 calc R . .
C9 C 0.1350(2) 1.02821(17) 0.06076(7) 0.0240(3) Uani 1 1 d . . .
H9A H 0.1807 0.9651 0.0285 0.029 Uiso 1 1 calc R . .
H9B H 0.0454 1.1134 0.0432 0.029 Uiso 1 1 calc R . .
C11 C 0.3648(2) 1.12602(16) 0.05075(7) 0.0217(3) Uani 1 1 d . . .
C12 C 0.4913(2) 1.17263(16) 0.08314(7) 0.0204(3) Uani 1 1 d . . .
C13 C 0.5906(2) 1.23832(17) 0.05006(7) 0.0239(3) Uani 1 1 d . . .
H13 H 0.5846 1.2478 0.0076 0.029 Uiso 1 1 calc R . .
C14 C 0.6980(2) 1.28940(17) 0.08035(8) 0.0262(4) Uani 1 1 d . . .
H14 H 0.7683 1.3334 0.0589 0.031 Uiso 1 1 calc R . .
C15 C 0.7014(2) 1.27543(16) 0.14246(8) 0.0250(3) Uani 1 1 d . . .
H15 H 0.7711 1.3120 0.1645 0.030 Uiso 1 1 calc R . .
C17 C 0.5998(2) 1.20622(15) 0.17157(7) 0.0225(3) Uani 1 1 d . . .
C18 C 0.5994(3) 1.18977(16) 0.23854(8) 0.0285(4) Uani 1 1 d . . .
C20 C 0.5197(3) 1.07569(18) 0.32778(8) 0.0349(4) Uani 1 1 d . . .
H20A H 0.4469 1.0175 0.3369 0.042 Uiso 1 1 calc R . .
H20B H 0.4617 1.1662 0.3447 0.042 Uiso 1 1 calc R . .
C21 C 0.6953(3) 1.00593(19) 0.35761(8) 0.0369(5) Uani 1 1 d . . .
H21A H 0.7691 1.0632 0.3482 0.044 Uiso 1 1 calc R . .
H21B H 0.6802 0.9991 0.4016 0.044 Uiso 1 1 calc R . .
C23 C 0.9424(3) 0.8238(2) 0.31703(8) 0.0353(4) Uani 1 1 d . . .
C24 C 1.0114(2) 0.6733(2) 0.30282(8) 0.0332(4) Uani 1 1 d . . .
H24A H 1.0834 0.6649 0.2663 0.040 Uiso 1 1 calc R . .
H24B H 1.0872 0.6181 0.3361 0.040 Uiso 1 1 calc R . .
C26 C 0.8420(2) 0.71732(18) 0.18995(7) 0.0249(3) Uani 1 1 d . . .
H26 H 0.9361 0.7504 0.1925 0.030 Uiso 1 1 calc R . .
C27 C 0.7515(2) 0.73622(18) 0.13673(7) 0.0245(3) Uani 1 1 d . . .
H27 H 0.7859 0.7813 0.1027 0.029 Uiso 1 1 calc R . .
C28 C 0.6121(2) 0.69114(16) 0.13179(7) 0.0208(3) Uani 1 1 d . . .
H28 H 0.5531 0.7030 0.0947 0.025 Uiso 1 1 calc R . .
C30 C 0.52796(19) 0.61482(16) 0.33507(7) 0.0191(3) Uani 1 1 d . . .
O37A O 0.1221(10) 0.4635(9) 0.5612(3) 0.0550(17) Uani 0.354(5) 1 d PDU A 1
O37B O 0.2444(12) 0.2593(8) 0.5304(3) 0.0656(17) Uani 0.354(5) 1 d PDU A 1
N37A N 0.2161(11) 0.3848(8) 0.5270(3) 0.0446(16) Uani 0.354(5) 1 d PDU A 1
C31A C 0.4652(2) 0.54013(17) 0.38553(7) 0.0228(5) Uani 0.354(5) 1 d PDU A 1
C32A C 0.3282(19) 0.6396(8) 0.4223(6) 0.0166(16) Uani 0.354(5) 1 d PDU A 1
H32A H 0.2961 0.7372 0.4144 0.020 Uiso 0.354(5) 1 calc PR A 1
C33A C 0.2503(15) 0.5820(10) 0.4688(6) 0.0225(17) Uani 0.354(5) 1 d PDU A 1
H33A H 0.1627 0.6411 0.4925 0.027 Uiso 0.354(5) 1 calc PR A 1
C34A C 0.2977(12) 0.4484(10) 0.4792(3) 0.0304(19) Uani 0.354(5) 1 d PDU A 1
C35A C 0.4215(12) 0.3568(8) 0.4485(5) 0.0324(18) Uani 0.354(5) 1 d PDU A 1
H35A H 0.4546 0.2599 0.4587 0.039 Uiso 0.354(5) 1 calc PR A 1
C36A C 0.5043(15) 0.4118(17) 0.3983(7) 0.029(2) Uani 0.354(5) 1 d PDU A 1
H36A H 0.5891 0.3488 0.3751 0.035 Uiso 0.354(5) 1 calc PR A 1
O37C O 0.1688(6) 0.3911(5) 0.55585(19) 0.0534(10) Uani 0.646(5) 1 d PDU A 2
O37D O 0.3610(6) 0.1982(3) 0.53262(13) 0.0595(10) Uani 0.646(5) 1 d PDU A 2
N37B N 0.2896(5) 0.3240(4) 0.52551(15) 0.0401(8) Uani 0.646(5) 1 d PDU A 2
C31B C 0.4652(2) 0.54013(17) 0.38553(7) 0.0228(5) Uani 0.65 1 d PD A 2
C32B C 0.3352(13) 0.6051(5) 0.4196(4) 0.0261(13) Uani 0.646(5) 1 d PDU A 2
H32B H 0.2803 0.7024 0.4121 0.031 Uiso 0.646(5) 1 calc PR A 2
C33B C 0.2740(9) 0.5367(6) 0.4665(3) 0.0294(12) Uani 0.646(5) 1 d PDU A 2
H33B H 0.1800 0.5869 0.4905 0.035 Uiso 0.646(5) 1 calc PR A 2
C34B C 0.3499(6) 0.4002(5) 0.47685(16) 0.0212(9) Uani 0.646(5) 1 d PDU A 2
C35B C 0.4911(6) 0.3227(4) 0.44306(17) 0.0258(9) Uani 0.646(5) 1 d PDU A 2
H35B H 0.5441 0.2255 0.4518 0.031 Uiso 0.646(5) 1 calc PR A 2
C36B C 0.5513(8) 0.3905(8) 0.3969(4) 0.0249(11) Uani 0.646(5) 1 d PDU A 2
H36B H 0.6463 0.3411 0.3730 0.030 Uiso 0.646(5) 1 calc PR A 2
O1S O 0.30545(18) 0.91321(13) 0.23958(6) 0.0302(3) Uani 1 1 d D . .
H1SA H 0.402(3) 0.843(2) 0.2600(11) 0.064(8) Uiso 1 1 d D . .
H1SB H 0.210(3) 0.900(4) 0.2589(15) 0.097(11) Uiso 1 1 d D . .
C1R C -0.0060(7) 0.0710(6) 0.4885(2) 0.0616(13) Uani 0.50 1 d PDU . 1
H1R1 H 0.0138 0.1212 0.5219 0.074 Uiso 0.50 1 calc PR . 1
H1R2 H -0.1246 0.1212 0.4729 0.074 Uiso 0.50 1 calc PR . 1
C2R C 0.1214(14) 0.0721(12) 0.4401(4) 0.078(2) Uani 0.50 1 d PDU B 1
H2R1 H 0.1158 0.0094 0.4094 0.094 Uiso 0.50 1 calc PR B 1
H2R2 H 0.2401 0.0377 0.4570 0.094 Uiso 0.50 1 calc PR B 1
C3R C 0.0822(13) 0.2176(12) 0.4113(5) 0.073(3) Uani 0.25 1 d PDU B 1
H3R1 H 0.1651 0.2165 0.3791 0.110 Uiso 0.25 1 calc PR B 1
H3R2 H 0.0918 0.2788 0.4414 0.110 Uiso 0.25 1 calc PR B 1
H3R3 H -0.0358 0.2517 0.3948 0.110 Uiso 0.25 1 calc PR B 1
C4R C 0.078(2) 0.103(2) 0.4408(11) 0.078(7) Uiso 0.15 1 d PD C 2
O4R O 0.2353(17) -0.0060(14) 0.4457(6) 0.071(4) Uiso 0.15 1 d PD C 2
C5R C 0.078(2) 0.103(2) 0.4408(11) 0.078(7) Uiso 0.10 1 d PD D 3
O5R O -0.0864(19) 0.1830(18) 0.4558(9) 0.064(5) Uiso 0.10 1 d PD D 3
C4S C 0.1845(7) 0.3438(5) 0.2644(3) 0.0670(15) Uani 0.50 1 d P E 4
H4S1 H 0.1615 0.4409 0.2502 0.101 Uiso 0.50 1 calc PR E 4
H4S2 H 0.3048 0.2888 0.2555 0.101 Uiso 0.50 1 calc PR E 4
H4S3 H 0.1655 0.3375 0.3077 0.101 Uiso 0.50 1 calc PR E 4
O5S O 0.0762(4) 0.2943(4) 0.2364(3) 0.0671(13) Uani 0.50 1 d P E 4
O6S O 0.2785(7) 0.4027(5) 0.2824(3) 0.0796(16) Uani 0.40 1 d P F 5
O7S O 0.0389(6) 0.2636(5) 0.2846(4) 0.0702(18) Uani 0.35 1 d P G 6
O8S O 0.0972(7) 0.3508(6) 0.1802(4) 0.0771(18) Uani 0.35 1 d P H 7
O2S O 0.009(3) 0.4861(18) 0.0095(4) 0.0605(19) Uani 0.35 1 d P . .
O3S O 0.0278(6) 0.4528(5) 0.0513(3) 0.0607(13) Uani 0.40 1 d P . .
O4S O 0.0523(5) 0.3986(4) 0.1015(3) 0.0723(12) Uani 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 C3 1.3761(17) . ?
O4 C5 1.4229(18) . ?
O6 C6 1.2305(18) . ?
O11 C11 1.2252(19) . ?
O18 C18 1.245(2) . ?
O23 C23 1.234(2) . ?
O25 C1 1.3749(18) . ?
O25 C24 1.422(2) . ?
O30 C30 1.2387(18) . ?
N7 C6 1.337(2) . ?
N7 C8 1.458(2) . ?
N7 H7 0.8800 . ?
N10 C11 1.334(2) . ?
N10 C9 1.455(2) . ?
N10 H10 0.8800 . ?
N17 C12 1.339(2) . ?
N17 C17 1.343(2) . ?
N19 C18 1.331(2) . ?
N19 C20 1.457(2) . ?
N19 H19 0.8800 . ?
N22 C23 1.326(3) . ?
N22 C21 1.457(2) . ?
N22 H22 0.8800 . ?
N29 C30 1.342(2) . ?
N29 C2 1.4216(18) . ?
N29 H29 0.8800 . ?
C1 C26 1.390(2) . ?
C1 C2 1.400(2) . ?
C2 C3 1.396(2) . ?
C3 C28 1.396(2) . ?
C5 C6 1.522(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C8 C9 1.518(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 C12 1.506(2) . ?
C12 C13 1.395(2) . ?
C13 C14 1.385(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.388(2) . ?
C14 H14 0.9500 . ?
C15 C17 1.394(2) . ?
C15 H15 0.9500 . ?
C17 C18 1.497(2) . ?
C20 C21 1.517(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C23 C24 1.512(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C27 1.385(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.385(2) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C30 C31A 1.499(2) . ?
O37A N37A 1.216(6) . ?
O37B N37A 1.228(6) . ?
N37A C34A 1.479(7) . ?
C31A C36A 1.258(17) . ?
C31A C32A 1.514(12) . ?
C32A C33A 1.407(17) . ?
C32A H32A 0.9500 . ?
C33A C34A 1.297(10) . ?
C33A H33A 0.9500 . ?
C34A C35A 1.344(10) . ?
C35A C36A 1.476(18) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
O37C N37B 1.223(4) . ?
O37D N37B 1.223(4) . ?
N37B C34B 1.470(4) . ?
C32B C33B 1.400(11) . ?
C32B H32B 0.9500 . ?
C33B C34B 1.330(6) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.404(5) . ?
C35B C36B 1.381(9) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
O1S H1SA 0.962(17) . ?
O1S H1SB 0.933(18) . ?
C1R C1R 1.482(12) 2_556 ?
C1R C2R 1.492(8) . ?
C1R H1R1 0.9900 . ?
C1R H1R2 0.9900 . ?
C2R C3R 1.514(9) . ?
C2R H2R1 0.9900 . ?
C2R H2R2 0.9900 . ?
C3R H3R1 0.9800 . ?
C3R H3R2 0.9800 . ?
C3R H3R3 0.9800 . ?
C4R O4R 1.390(9) . ?
C4S O5S 1.352(7) . ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?
O8S O4S 1.807(10) . ?
O2S O2S 0.492(11) 2_565 ?
O2S O3S 0.969(10) . ?
O2S O3S 1.450(9) 2_565 ?
O3S O4S 1.205(7) . ?
O3S O2S 1.450(9) 2_565 ?

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
C3 O4 C5 117.80(12) . . ?
C1 O25 C24 117.70(13) . . ?
C6 N7 C8 120.16(13) . . ?
C6 N7 H7 119.9 . . ?
C8 N7 H7 119.9 . . ?
C11 N10 C9 120.79(14) . . ?
C11 N10 H10 119.6 . . ?
C9 N10 H10 119.6 . . ?
C12 N17 C17 117.25(14) . . ?
C18 N19 C20 121.38(15) . . ?
C18 N19 H19 119.3 . . ?
C20 N19 H19 119.3 . . ?
C23 N22 C21 123.55(16) . . ?
C23 N22 H22 118.2 . . ?
C21 N22 H22 118.2 . . ?
C30 N29 C2 120.99(12) . . ?
C30 N29 H29 119.5 . . ?
C2 N29 H29 119.5 . . ?
O25 C1 C26 125.08(14) . . ?
O25 C1 C2 114.91(13) . . ?
C26 C1 C2 120.00(14) . . ?
C3 C2 C1 119.63(13) . . ?
C3 C2 N29 119.61(13) . . ?
C1 C2 N29 120.75(13) . . ?
O4 C3 C2 114.58(13) . . ?
O4 C3 C28 124.91(13) . . ?
C2 C3 C28 120.47(14) . . ?
O4 C5 C6 115.76(12) . . ?
O4 C5 H5A 108.3 . . ?
C6 C5 H5A 108.3 . . ?
O4 C5 H5B 108.3 . . ?
C6 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
O6 C6 N7 123.90(14) . . ?
O6 C6 C5 118.35(13) . . ?
N7 C6 C5 117.73(13) . . ?
N7 C8 C9 112.69(13) . . ?
N7 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N7 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
N10 C9 C8 110.70(13) . . ?
N10 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
N10 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
O11 C11 N10 123.79(15) . . ?
O11 C11 C12 120.83(14) . . ?
N10 C11 C12 115.33(14) . . ?
N17 C12 C13 123.17(15) . . ?
N17 C12 C11 117.84(14) . . ?
C13 C12 C11 118.93(14) . . ?
C14 C13 C12 118.69(15) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C13 C14 C15 119.06(15) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C14 C15 C17 118.10(15) . . ?
C14 C15 H15 121.0 . . ?
C17 C15 H15 121.0 . . ?
N17 C17 C15 123.67(15) . . ?
N17 C17 C18 116.68(14) . . ?
C15 C17 C18 119.64(15) . . ?
O18 C18 N19 123.08(16) . . ?
O18 C18 C17 120.56(15) . . ?
N19 C18 C17 116.35(14) . . ?
N19 C20 C21 112.81(17) . . ?
N19 C20 H20A 109.0 . . ?
C21 C20 H20A 109.0 . . ?
N19 C20 H20B 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
N22 C21 C20 111.30(14) . . ?
N22 C21 H21A 109.4 . . ?
C20 C21 H21A 109.4 . . ?
N22 C21 H21B 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
O23 C23 N22 124.3(2) . . ?
O23 C23 C24 120.57(19) . . ?
N22 C23 C24 115.06(15) . . ?
O25 C24 C23 113.65(15) . . ?
O25 C24 H24A 108.8 . . ?
C23 C24 H24A 108.8 . . ?
O25 C24 H24B 108.8 . . ?
C23 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
C27 C26 C1 119.36(15) . . ?
C27 C26 H26 120.3 . . ?
C1 C26 H26 120.3 . . ?
C28 C27 C26 121.75(15) . . ?
C28 C27 H27 119.1 . . ?
C26 C27 H27 119.1 . . ?
C27 C28 C3 118.70(14) . . ?
C27 C28 H28 120.6 . . ?
C3 C28 H28 120.6 . . ?
O30 C30 N29 122.96(14) . . ?
O30 C30 C31A 120.21(14) . . ?
N29 C30 C31A 116.82(13) . . ?
O37A N37A O37B 123.8(7) . . ?
O37A N37A C34A 116.1(6) . . ?
O37B N37A C34A 120.1(7) . . ?
C36A C31A C30 129.4(6) . . ?
C36A C31A C32A 118.7(7) . . ?
C30 C31A C32A 111.8(4) . . ?
C33A C32A C31A 117.4(6) . . ?
C33A C32A H32A 121.3 . . ?
C31A C32A H32A 121.3 . . ?
C34A C33A C32A 120.2(8) . . ?
C34A C33A H33A 119.9 . . ?
C32A C33A H33A 119.9 . . ?
C33A C34A C35A 124.2(7) . . ?
C33A C34A N37A 121.4(8) . . ?
C35A C34A N37A 114.4(7) . . ?
C34A C35A C36A 117.8(7) . . ?
C34A C35A H35A 121.1 . . ?
C36A C35A H35A 121.1 . . ?
C31A C36A C35A 121.7(8) . . ?
C31A C36A H36A 119.2 . . ?
C35A C36A H36A 119.2 . . ?
O37C N37B O37D 124.3(3) . . ?
O37C N37B C34B 117.3(4) . . ?
O37D N37B C34B 118.4(3) . . ?
C33B C32B H32B 118.7 . . ?
C34B C33B C32B 118.8(5) . . ?
C34B C33B H33B 120.6 . . ?
C32B C33B H33B 120.6 . . ?
C33B C34B C35B 122.4(4) . . ?
C33B C34B N37B 120.7(5) . . ?
C35B C34B N37B 116.9(4) . . ?
C36B C35B C34B 118.7(4) . . ?
C36B C35B H35B 120.7 . . ?
C34B C35B H35B 120.7 . . ?
C35B C36B H36B 120.8 . . ?
H1SA O1S H1SB 103(3) . . ?
C1R C1R C2R 113.1(6) 2_556 . ?
C1R C1R H1R1 109.0 2_556 . ?
C2R C1R H1R1 109.0 . . ?
C1R C1R H1R2 109.0 2_556 . ?
C2R C1R H1R2 109.0 . . ?
H1R1 C1R H1R2 107.8 . . ?
C1R C2R C3R 110.3(9) . . ?
C1R C2R H2R1 109.6 . . ?
C3R C2R H2R1 109.6 . . ?
C1R C2R H2R2 109.6 . . ?
C3R C2R H2R2 109.6 . . ?
H2R1 C2R H2R2 108.1 . . ?
C2R C3R H3R1 109.5 . . ?
C2R C3R H3R2 109.5 . . ?
H3R1 C3R H3R2 109.5 . . ?
C2R C3R H3R3 109.5 . . ?
H3R1 C3R H3R3 109.5 . . ?
H3R2 C3R H3R3 109.5 . . ?
O2S O2S O3S 165(6) 2_565 . ?
O2S O2S O3S 10(4) 2_565 2_565 ?
O3S O2S O3S 175(2) . 2_565 ?
O2S O3S O4S 173.5(11) . . ?
O2S O3S O2S 5(2) . 2_565 ?
O4S O3S O2S 176.5(9) . 2_565 ?
O3S O4S O8S 167.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C24 O25 C1 C26 9.6(2) . . . . ?
C24 O25 C1 C2 -171.62(14) . . . . ?
O25 C1 C2 C3 -176.50(13) . . . . ?
C26 C1 C2 C3 2.4(2) . . . . ?
O25 C1 C2 N29 4.2(2) . . . . ?
C26 C1 C2 N29 -176.96(14) . . . . ?
C30 N29 C2 C3 -112.41(16) . . . . ?
C30 N29 C2 C1 66.93(19) . . . . ?
C5 O4 C3 C2 -167.24(12) . . . . ?
C5 O4 C3 C28 15.1(2) . . . . ?
C1 C2 C3 O4 -177.66(13) . . . . ?
N29 C2 C3 O4 1.7(2) . . . . ?
C1 C2 C3 C28 0.1(2) . . . . ?
N29 C2 C3 C28 179.48(13) . . . . ?
C3 O4 C5 C6 -82.90(16) . . . . ?
C8 N7 C6 O6 -1.6(2) . . . . ?
C8 N7 C6 C5 -179.86(13) . . . . ?
O4 C5 C6 O6 176.33(13) . . . . ?
O4 C5 C6 N7 -5.3(2) . . . . ?
C6 N7 C8 C9 -76.34(18) . . . . ?
C11 N10 C9 C8 179.71(14) . . . . ?
N7 C8 C9 N10 -64.13(17) . . . . ?
C9 N10 C11 O11 -4.3(2) . . . . ?
C9 N10 C11 C12 172.98(13) . . . . ?
C17 N17 C12 C13 2.8(2) . . . . ?
C17 N17 C12 C11 -174.44(13) . . . . ?
O11 C11 C12 N17 174.67(15) . . . . ?
N10 C11 C12 N17 -2.7(2) . . . . ?
O11 C11 C12 C13 -2.7(2) . . . . ?
N10 C11 C12 C13 179.93(14) . . . . ?
N17 C12 C13 C14 -1.5(2) . . . . ?
C11 C12 C13 C14 175.66(14) . . . . ?
C12 C13 C14 C15 -0.9(2) . . . . ?
C13 C14 C15 C17 2.0(2) . . . . ?
C12 N17 C17 C15 -1.6(2) . . . . ?
C12 N17 C17 C18 177.35(14) . . . . ?
C14 C15 C17 N17 -0.7(2) . . . . ?
C14 C15 C17 C18 -179.67(14) . . . . ?
C20 N19 C18 O18 2.5(3) . . . . ?
C20 N19 C18 C17 -178.29(16) . . . . ?
N17 C17 C18 O18 -165.43(16) . . . . ?
C15 C17 C18 O18 13.6(3) . . . . ?
N17 C17 C18 N19 15.3(2) . . . . ?
C15 C17 C18 N19 -165.68(16) . . . . ?
C18 N19 C20 C21 -69.2(2) . . . . ?
C23 N22 C21 C20 128.92(18) . . . . ?
N19 C20 C21 N22 -62.84(19) . . . . ?
C21 N22 C23 O23 -0.9(3) . . . . ?
C21 N22 C23 C24 175.53(15) . . . . ?
C1 O25 C24 C23 77.83(18) . . . . ?
O23 C23 C24 O25 -162.96(17) . . . . ?
N22 C23 C24 O25 20.5(2) . . . . ?
O25 C1 C26 C27 175.81(15) . . . . ?
C2 C1 C26 C27 -3.0(2) . . . . ?
C1 C26 C27 C28 1.0(3) . . . . ?
C26 C27 C28 C3 1.5(2) . . . . ?
O4 C3 C28 C27 175.53(14) . . . . ?
C2 C3 C28 C27 -2.0(2) . . . . ?
C2 N29 C30 O30 -1.3(2) . . . . ?
C2 N29 C30 C31A 177.29(13) . . . . ?
O30 C30 C31A C36A -160.2(10) . . . . ?
N29 C30 C31A C36A 21.2(10) . . . . ?
O30 C30 C31A C32A 23.6(7) . . . . ?
N29 C30 C31A C32A -155.0(7) . . . . ?
C36A C31A C32A C33A -0.7(17) . . . . ?
C30 C31A C32A C33A 175.9(10) . . . . ?
C31A C32A C33A C34A 0.8(19) . . . . ?
C32A C33A C34A C35A 1(2) . . . . ?
C32A C33A C34A N37A -179.0(11) . . . . ?
O37A N37A C34A C33A -10.5(14) . . . . ?
O37B N37A C34A C33A 169.3(11) . . . . ?
O37A N37A C34A C35A 169.8(8) . . . . ?
O37B N37A C34A C35A -10.5(12) . . . . ?
C33A C34A C35A C36A -2.3(17) . . . . ?
N37A C34A C35A C36A 177.5(9) . . . . ?
C30 C31A C36A C35A -176.7(7) . . . . ?
C32A C31A C36A C35A -0.7(18) . . . . ?
C34A C35A C36A C31A 2.2(18) . . . . ?
C32B C33B C34B C35B 1.1(10) . . . . ?
C32B C33B C34B N37B -179.8(6) . . . . ?
O37C N37B C34B C33B -0.5(7) . . . . ?
O37D N37B C34B C33B 178.6(5) . . . . ?
O37C N37B C34B C35B 178.7(4) . . . . ?
O37D N37B C34B C35B -2.3(6) . . . . ?
C33B C34B C35B C36B -1.0(8) . . . . ?
N37B C34B C35B C36B 179.8(5) . . . . ?
C1R C1R C2R C3R 170.2(7) 2_556 . . . ?
O2S O2S O3S O4S 149(14) 2_565 . . . ?
O3S O2S O3S O4S 149(14) 2_565 . . . ?
O3S O2S O3S O2S 0.0(2) 2_565 . . 2_565 ?
O2S O3S O4S O8S 166(10) . . . . ?
O2S O3S O4S O8S -147(16) 2_565 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O1S 0.88 2.16 2.9582(18) 150.6 .
N19 H19 O1S 0.88 2.42 3.159(2) 142.0 .
N22 H22 O30 0.88 2.09 2.9321(18) 160.3 .
N29 H29 O18 0.88 2.00 2.8521(17) 164.2 1_545
O1S H1SA O30 0.962(17) 2.05(2) 2.9144(18) 149(2) .
O1S H1SB O23 0.933(18) 1.85(2) 2.764(2) 166(3) 1_455

_diffrn_measured_fraction_theta_max 0.939
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.498
_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_Uc1_TBA_Cl
_database_code_depnum_ccdc_archive 'CCDC 1534256'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-06-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT355_Uc1_TBA_Cl          
;
PROBLEM: Long    O-H (X0.82,N0.98A)  O38    -   H38A   ..       1.14 Ang.
RESPONSE: This long distance is likely associated with the incomplete hydrogen bond saturation of the water molecule which is engaged in just two, albeit strong, hydrogen bonds with the oxygen carbonyl atoms of the adjacent macrocyclic molecules. From this reason, the water molecule is probably dislocated between these macrocycles.
;
# Added during the CSD deposition process: Wednesday 22 February 2017 05:43 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H65 Cl N8 O10'
_chemical_formula_weight         901.49

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   9.9445(6)
_cell_length_b                   15.7022(8)
_cell_length_c                   30.3358(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.244(5)
_cell_angle_gamma                90.00
_cell_volume                     4688.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11406
_cell_measurement_theta_min      3
_cell_measurement_theta_max      29

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.6479
_diffrn_standards_number         '1 frame'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        2
_diffrn_reflns_number            54618
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         28.66
_reflns_number_total             11406
_reflns_number_gt                7415
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL-97

_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)+(0.0446P)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    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00097(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11406
_refine_ls_number_parameters     838
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0780
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.916
_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
Cl1 Cl 0.32621(3) 0.483893(19) 0.073170(10) 0.02060(8) Uani 1 1 d . . .
O4 O 0.43301(8) 0.26183(5) 0.18850(3) 0.01854(19) Uani 1 1 d . . .
O6 O 0.70657(8) 0.15766(5) 0.14739(3) 0.0252(2) Uani 1 1 d . . .
O11 O 0.76082(9) 0.31891(5) 0.01563(3) 0.0250(2) Uani 1 1 d . . .
O18 O 0.70248(9) 0.73876(5) 0.09089(3) 0.0289(2) Uani 1 1 d . . .
O23 O 0.26066(8) 0.73217(5) 0.20202(3) 0.0210(2) Uani 1 1 d . . .
O25 O 0.18796(8) 0.51486(5) 0.17329(3) 0.01826(19) Uani 1 1 d . . .
O30 O 0.12722(8) 0.25918(5) 0.17875(3) 0.0208(2) Uani 1 1 d . . .
O37A O -0.06938(12) 0.18807(8) -0.05721(3) 0.0498(3) Uani 1 1 d . . .
O37B O -0.1443(9) 0.0794(5) -0.0195(4) 0.059(2) Uani 0.25 1 d P . .
O37C O -0.1979(3) 0.10933(17) -0.02234(11) 0.0473(7) Uani 0.75 1 d P . .
O38 O 0.94195(10) 0.14313(6) 0.21127(3) 0.0305(2) Uani 1 1 d . . .
N7 N 0.52948(11) 0.23518(7) 0.11297(3) 0.0186(2) Uani 1 1 d . . .
N10 N 0.57432(11) 0.36630(7) 0.04298(4) 0.0190(2) Uani 1 1 d . . .
N17 N 0.68648(10) 0.52276(6) 0.05617(3) 0.0173(2) Uani 1 1 d . . .
N19 N 0.52265(10) 0.64951(7) 0.07575(3) 0.0191(2) Uani 1 1 d . . .
N22 N 0.32114(10) 0.65540(7) 0.14485(4) 0.0193(2) Uani 1 1 d . . .
N29 N 0.23845(10) 0.35871(6) 0.14382(3) 0.0156(2) Uani 1 1 d . . .
N37 N -0.09935(14) 0.15745(9) -0.02267(4) 0.0426(3) Uani 1 1 d . . .
N39 N 0.04556(9) 0.10894(6) -0.18396(3) 0.0152(2) Uani 1 1 d . . .
C1 C 0.28921(12) 0.47095(7) 0.19939(4) 0.0170(3) Uani 1 1 d . . .
C2 C 0.31370(11) 0.38959(7) 0.18396(4) 0.0150(2) Uani 1 1 d . . .
C3 C 0.41601(12) 0.34010(7) 0.20729(4) 0.0162(3) Uani 1 1 d . . .
C5 C 0.56436(13) 0.22395(9) 0.19375(4) 0.0207(3) Uani 1 1 d . . .
C6 C 0.60541(12) 0.20257(7) 0.14879(4) 0.0185(3) Uani 1 1 d . . .
C8 C 0.55368(15) 0.21674(8) 0.06769(4) 0.0225(3) Uani 1 1 d . . .
C9 C 0.50151(14) 0.28652(8) 0.03491(4) 0.0207(3) Uani 1 1 d . . .
C11 C 0.69985(12) 0.37576(8) 0.03246(4) 0.0193(3) Uani 1 1 d . . .
C12 C 0.76627(12) 0.46009(8) 0.04457(4) 0.0187(3) Uani 1 1 d . . .
C13 C 0.90546(13) 0.46956(9) 0.04528(4) 0.0248(3) Uani 1 1 d . . .
C14 C 0.96609(14) 0.54554(9) 0.05976(4) 0.0266(3) Uani 1 1 d . . .
C15 C 0.88570(13) 0.61040(8) 0.07195(4) 0.0231(3) Uani 1 1 d . . .
C16 C 0.74612(12) 0.59702(8) 0.06896(4) 0.0184(3) Uani 1 1 d . . .
C18 C 0.65523(12) 0.66777(8) 0.07977(4) 0.0197(3) Uani 1 1 d . . .
C20 C 0.42280(14) 0.71438(8) 0.08196(4) 0.0204(3) Uani 1 1 d . . .
C21 C 0.40068(14) 0.72540(8) 0.12997(4) 0.0216(3) Uani 1 1 d . . .
C23 C 0.25293(12) 0.66664(7) 0.17921(4) 0.0170(3) Uani 1 1 d . . .
C24 C 0.15495(13) 0.59744(8) 0.18827(5) 0.0204(3) Uani 1 1 d . . .
C26 C 0.36374(13) 0.50148(8) 0.23834(4) 0.0210(3) Uani 1 1 d . . .
C27 C 0.46244(13) 0.44969(8) 0.26156(4) 0.0229(3) Uani 1 1 d . . .
C28 C 0.49000(13) 0.36892(8) 0.24678(4) 0.0201(3) Uani 1 1 d . . .
C30 C 0.15149(11) 0.29238(7) 0.14397(4) 0.0156(3) Uani 1 1 d . . .
C31 C 0.08876(11) 0.25862(7) 0.09942(4) 0.0156(3) Uani 1 1 d . . .
C32 C 0.13194(13) 0.28337(8) 0.05967(4) 0.0195(3) Uani 1 1 d . . .
C33 C 0.07357(14) 0.24823(8) 0.01959(5) 0.0249(3) Uani 1 1 d . . .
C34 C -0.02872(13) 0.18932(8) 0.02001(4) 0.0240(3) Uani 1 1 d . . .
C35 C -0.07307(13) 0.16251(8) 0.05880(4) 0.0217(3) Uani 1 1 d . . .
C36 C -0.01373(12) 0.19771(8) 0.09857(4) 0.0185(3) Uani 1 1 d . . .
C40 C 0.16324(13) 0.05819(8) -0.15912(4) 0.0203(3) Uani 1 1 d . . .
C41 C 0.19237(14) 0.07385(9) -0.10944(5) 0.0254(3) Uani 1 1 d . . .
C42 C 0.33695(17) 0.04728(11) -0.09107(6) 0.0411(4) Uani 1 1 d . . .
C43 C 0.3700(2) 0.06211(13) -0.04141(7) 0.0609(6) Uani 1 1 d . . .
C44 C 0.07924(13) 0.20393(7) -0.18420(5) 0.0164(3) Uani 1 1 d . . .
C45 C 0.20032(13) 0.22981(8) -0.20626(5) 0.0182(3) Uani 1 1 d . . .
C46 C 0.21297(13) 0.32680(8) -0.20506(5) 0.0198(3) Uani 1 1 d . . .
C47 C 0.32595(15) 0.35986(9) -0.22935(5) 0.0257(3) Uani 1 1 d . . .
C48 C 0.01960(13) 0.07378(8) -0.23111(4) 0.0170(3) Uani 1 1 d . . .
C49 C -0.09713(13) 0.11315(8) -0.26184(4) 0.0188(3) Uani 1 1 d . . .
C50 C -0.11407(14) 0.06685(8) -0.30660(4) 0.0227(3) Uani 1 1 d . . .
C51 C -0.23215(18) 0.09975(11) -0.33916(5) 0.0370(4) Uani 1 1 d . . .
C52 C -0.08008(12) 0.10148(8) -0.16107(4) 0.0165(3) Uani 1 1 d . . .
C53 C -0.13818(13) 0.01295(8) -0.15807(5) 0.0208(3) Uani 1 1 d . . .
C54 C -0.25951(13) 0.01790(8) -0.13246(5) 0.0220(3) Uani 1 1 d . . .
C55 C -0.32640(16) -0.06796(9) -0.12798(6) 0.0315(3) Uani 1 1 d . . .
H5A H 0.6334(14) 0.2613(8) 0.2100(4) 0.025(4) Uiso 1 1 d . . .
H5B H 0.5657(12) 0.1719(8) 0.2109(4) 0.023(3) Uiso 1 1 d . . .
H7 H 0.4599(14) 0.2614(8) 0.1167(4) 0.020(4) Uiso 1 1 d . . .
H8A H 0.5068(12) 0.1619(8) 0.0572(4) 0.023(3) Uiso 1 1 d . . .
H8B H 0.6532(14) 0.2082(8) 0.0692(4) 0.027(4) Uiso 1 1 d . . .
H9A H 0.4059(13) 0.3007(8) 0.0358(4) 0.019(3) Uiso 1 1 d . . .
H9B H 0.5125(12) 0.2669(8) 0.0054(4) 0.019(3) Uiso 1 1 d . . .
H10 H 0.5346(14) 0.4083(9) 0.0517(5) 0.031(4) Uiso 1 1 d . . .
H13 H 0.9563(13) 0.4238(8) 0.0369(4) 0.025(4) Uiso 1 1 d . . .
H14 H 1.0627(15) 0.5508(9) 0.0619(5) 0.037(4) Uiso 1 1 d . . .
H15 H 0.9242(13) 0.6656(8) 0.0829(4) 0.025(4) Uiso 1 1 d . . .
H19 H 0.4951(14) 0.5962(9) 0.0690(5) 0.034(4) Uiso 1 1 d . . .
H20A H 0.4580(12) 0.7706(8) 0.0726(4) 0.018(3) Uiso 1 1 d . . .
H20B H 0.3366(13) 0.6991(8) 0.0635(4) 0.022(3) Uiso 1 1 d . . .
H21A H 0.4893(14) 0.7304(8) 0.1497(4) 0.027(4) Uiso 1 1 d . . .
H21B H 0.3493(12) 0.7803(8) 0.1326(4) 0.020(3) Uiso 1 1 d . . .
H22 H 0.3098(13) 0.6087(9) 0.1299(5) 0.026(4) Uiso 1 1 d . . .
H24A H 0.0654(14) 0.6108(8) 0.1712(4) 0.026(4) Uiso 1 1 d . . .
H24B H 0.1447(12) 0.5984(8) 0.2189(5) 0.020(3) Uiso 1 1 d . . .
H26 H 0.3476(12) 0.5576(8) 0.2494(4) 0.024(3) Uiso 1 1 d . . .
H27 H 0.5122(13) 0.4701(8) 0.2886(4) 0.023(3) Uiso 1 1 d . . .
H28 H 0.5536(13) 0.3347(8) 0.2621(4) 0.025(4) Uiso 1 1 d . . .
H29 H 0.2443(13) 0.3905(9) 0.1186(5) 0.031(4) Uiso 1 1 d . . .
H32 H 0.2006(13) 0.3263(8) 0.0588(4) 0.019(3) Uiso 1 1 d . . .
H33 H 0.0999(13) 0.2645(8) -0.0088(5) 0.028(4) Uiso 1 1 d . . .
H35 H -0.1432(14) 0.1222(8) 0.0579(4) 0.029(4) Uiso 1 1 d . . .
H36 H -0.0436(12) 0.1813(8) 0.1255(4) 0.018(3) Uiso 1 1 d . . .
H38A H 0.842(3) 0.1553(17) 0.1888(10) 0.147(10) Uiso 1 1 d . . .
H38B H 1.011(2) 0.1848(13) 0.1994(7) 0.090(7) Uiso 1 1 d . . .
H40A H 0.1419(12) -0.0016(8) -0.1657(4) 0.020(3) Uiso 1 1 d . . .
H40B H 0.2425(13) 0.0729(8) -0.1740(4) 0.021(3) Uiso 1 1 d . . .
H41A H 0.1824(13) 0.1330(9) -0.1026(4) 0.024(3) Uiso 1 1 d . . .
H41B H 0.1249(14) 0.0426(9) -0.0941(4) 0.030(4) Uiso 1 1 d . . .
H42A H 0.3490(15) -0.0124(10) -0.0988(5) 0.039(4) Uiso 1 1 d . . .
H42B H 0.3987(15) 0.0803(10) -0.1069(5) 0.044(5) Uiso 1 1 d . . .
H43A H 0.465(2) 0.0492(12) -0.0311(6) 0.073(6) Uiso 1 1 d . . .
H43B H 0.3521(17) 0.1247(12) -0.0340(6) 0.065(6) Uiso 1 1 d . . .
H43C H 0.3108(18) 0.0287(12) -0.0239(6) 0.068(6) Uiso 1 1 d . . .
H44A H -0.0001(13) 0.2292(7) -0.1990(4) 0.016(3) Uiso 1 1 d . . .
H44B H 0.0933(11) 0.2217(7) -0.1540(4) 0.009(3) Uiso 1 1 d . . .
H45A H 0.2844(14) 0.2059(8) -0.1906(4) 0.024(3) Uiso 1 1 d . . .
H45B H 0.1875(13) 0.2114(8) -0.2368(5) 0.024(4) Uiso 1 1 d . . .
H46A H 0.1257(14) 0.3521(8) -0.2192(4) 0.025(4) Uiso 1 1 d . . .
H46B H 0.2301(12) 0.3471(8) -0.1740(5) 0.021(3) Uiso 1 1 d . . .
H47A H 0.3061(14) 0.3442(9) -0.2609(5) 0.037(4) Uiso 1 1 d . . .
H47B H 0.3349(14) 0.4208(10) -0.2276(5) 0.035(4) Uiso 1 1 d . . .
H47C H 0.4129(15) 0.3356(9) -0.2155(5) 0.035(4) Uiso 1 1 d . . .
H48A H 0.1041(13) 0.0815(8) -0.2435(4) 0.018(3) Uiso 1 1 d . . .
H48B H 0.0034(11) 0.0140(8) -0.2280(4) 0.010(3) Uiso 1 1 d . . .
H49A H -0.1841(13) 0.1073(8) -0.2491(4) 0.023(3) Uiso 1 1 d . . .
H49B H -0.0819(13) 0.1730(9) -0.2658(4) 0.024(3) Uiso 1 1 d . . .
H50A H -0.0312(14) 0.0719(8) -0.3201(4) 0.028(4) Uiso 1 1 d . . .
H50B H -0.1271(13) 0.0047(9) -0.3015(4) 0.025(3) Uiso 1 1 d . . .
H51A H -0.2185(15) 0.1587(11) -0.3470(5) 0.044(5) Uiso 1 1 d . . .
H51B H -0.3195(17) 0.0956(10) -0.3269(5) 0.049(5) Uiso 1 1 d . . .
H51C H -0.2431(16) 0.0662(11) -0.3678(6) 0.061(5) Uiso 1 1 d . . .
H52A H -0.1475(12) 0.1403(7) -0.1770(4) 0.014(3) Uiso 1 1 d . . .
H52B H -0.0546(12) 0.1257(7) -0.1301(4) 0.017(3) Uiso 1 1 d . . .
H53A H -0.0711(14) -0.0275(9) -0.1431(4) 0.031(4) Uiso 1 1 d . . .
H53B H -0.1675(13) -0.0110(8) -0.1868(5) 0.025(4) Uiso 1 1 d . . .
H54A H -0.3296(13) 0.0597(8) -0.1485(4) 0.028(4) Uiso 1 1 d . . .
H54B H -0.2289(13) 0.0437(8) -0.1034(5) 0.028(4) Uiso 1 1 d . . .
H55A H -0.4085(16) -0.0617(9) -0.1122(5) 0.043(4) Uiso 1 1 d . . .
H55B H -0.2645(17) -0.1074(11) -0.1095(6) 0.054(5) Uiso 1 1 d . . .
H55C H -0.3499(17) -0.0933(11) -0.1580(6) 0.063(6) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 C3 1.3753(14) . ?
O4 C5 1.4233(14) . ?
O6 C6 1.2342(14) . ?
O11 C11 1.2303(14) . ?
O18 C18 1.2376(14) . ?
O23 C23 1.2362(14) . ?
O25 C1 1.3737(14) . ?
O25 C24 1.4277(14) . ?
O30 C30 1.2315(14) . ?
O37A N37 1.2278(15) . ?
O37B O37C 0.707(7) . ?
O37B N37 1.313(9) . ?
O37C N37 1.238(3) . ?
O38 H38A 1.14(3) . ?
O38 H38B 1.05(2) . ?
N7 C6 1.3333(16) . ?
N7 C8 1.4573(16) . ?
N7 H7 0.826(13) . ?
N10 C11 1.3404(15) . ?
N10 C9 1.4501(15) . ?
N10 H10 0.831(14) . ?
N17 C16 1.3402(15) . ?
N17 C12 1.3423(15) . ?
N19 C18 1.3376(15) . ?
N19 C20 1.4536(15) . ?
N19 H19 0.895(14) . ?
N22 C23 1.3342(15) . ?
N22 C21 1.4629(16) . ?
N22 H22 0.861(14) . ?
N29 C30 1.3540(15) . ?
N29 C2 1.4199(15) . ?
N29 H29 0.923(14) . ?
N37 C34 1.4695(17) . ?
N39 C52 1.5183(15) . ?
N39 C48 1.5203(15) . ?
N39 C40 1.5229(15) . ?
N39 C44 1.5291(14) . ?
C1 C26 1.3873(17) . ?
C1 C2 1.3940(16) . ?
C2 C3 1.3905(16) . ?
C3 C28 1.3887(17) . ?
C5 C6 1.5164(18) . ?
C5 H5A 0.979(14) . ?
C5 H5B 0.968(13) . ?
C8 C9 1.5199(18) . ?
C8 H8A 1.009(13) . ?
C8 H8B 0.993(14) . ?
C9 H9A 0.981(13) . ?
C9 H9B 0.969(13) . ?
C11 C12 1.5017(17) . ?
C12 C13 1.3892(17) . ?
C13 C14 1.3799(19) . ?
C13 H13 0.934(13) . ?
C14 C15 1.3776(19) . ?
C14 H14 0.957(14) . ?
C15 C16 1.3938(17) . ?
C15 H15 0.986(13) . ?
C16 C18 1.4979(17) . ?
C20 C21 1.5135(18) . ?
C20 H20A 1.005(12) . ?
C20 H20B 0.984(13) . ?
C21 H21A 0.995(13) . ?
C21 H21B 1.012(12) . ?
C23 C24 1.5108(17) . ?
C24 H24A 0.986(13) . ?
C24 H24B 0.949(13) . ?
C26 C27 1.3865(18) . ?
C26 H26 0.964(13) . ?
C27 C28 1.3857(18) . ?
C27 H27 0.951(13) . ?
C28 H28 0.907(13) . ?
C30 C31 1.5017(17) . ?
C31 C32 1.3920(17) . ?
C31 C36 1.3953(17) . ?
C32 C33 1.3846(18) . ?
C32 H32 0.963(13) . ?
C33 C34 1.3764(18) . ?
C33 H33 0.970(14) . ?
C34 C35 1.3803(18) . ?
C35 C36 1.3801(18) . ?
C35 H35 0.939(14) . ?
C36 H36 0.943(13) . ?
C40 C41 1.5137(19) . ?
C40 H40A 0.977(13) . ?
C40 H40B 0.989(12) . ?
C41 C42 1.524(2) . ?
C41 H41A 0.960(13) . ?
C41 H41B 0.999(14) . ?
C42 C43 1.513(3) . ?
C42 H42A 0.979(15) . ?
C42 H42B 0.980(16) . ?
C43 H43A 0.977(19) . ?
C43 H43B 1.029(18) . ?
C43 H43C 0.996(19) . ?
C44 C45 1.5146(17) . ?
C44 H44A 0.939(13) . ?
C44 H44B 0.949(12) . ?
C45 C46 1.5281(17) . ?
C45 H45A 0.976(13) . ?
C45 H45B 0.961(13) . ?
C46 C47 1.5206(18) . ?
C46 H46A 0.994(13) . ?
C46 H46B 0.987(13) . ?
C47 H47A 0.980(15) . ?
C47 H47B 0.962(15) . ?
C47 H47C 0.983(15) . ?
C48 C49 1.5127(17) . ?
C48 H48A 0.976(12) . ?
C48 H48B 0.959(12) . ?
C49 C50 1.5281(17) . ?
C49 H49A 1.000(13) . ?
C49 H49B 0.963(13) . ?
C50 C51 1.513(2) . ?
C50 H50A 0.974(13) . ?
C50 H50B 0.999(13) . ?
C51 H51A 0.969(16) . ?
C51 H51B 0.995(17) . ?
C51 H51C 1.010(18) . ?
C52 C53 1.5131(17) . ?
C52 H52A 0.981(12) . ?
C52 H52B 1.011(13) . ?
C53 C54 1.5280(17) . ?
C53 H53A 0.983(14) . ?
C53 H53B 0.956(13) . ?
C54 C55 1.5181(18) . ?
C54 H54A 1.027(13) . ?
C54 H54B 0.978(14) . ?
C55 H55A 1.009(16) . ?
C55 H55B 0.988(17) . ?
C55 H55C 0.990(19) . ?

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
C3 O4 C5 119.50(9) . . ?
C1 O25 C24 117.10(9) . . ?
O37C O37B N37 68.2(9) . . ?
O37B O37C N37 79.8(10) . . ?
H38A O38 H38B 104.3(17) . . ?
C6 N7 C8 122.77(11) . . ?
C6 N7 H7 117.9(9) . . ?
C8 N7 H7 118.8(9) . . ?
C11 N10 C9 121.01(11) . . ?
C11 N10 H10 119.3(10) . . ?
C9 N10 H10 119.3(10) . . ?
C16 N17 C12 117.39(10) . . ?
C18 N19 C20 121.38(10) . . ?
C18 N19 H19 119.1(9) . . ?
C20 N19 H19 119.5(9) . . ?
C23 N22 C21 119.98(10) . . ?
C23 N22 H22 118.7(9) . . ?
C21 N22 H22 120.9(9) . . ?
C30 N29 C2 121.21(10) . . ?
C30 N29 H29 122.3(9) . . ?
C2 N29 H29 116.0(9) . . ?
O37A N37 O37C 122.33(19) . . ?
O37A N37 O37B 123.7(5) . . ?
O37C N37 O37B 32.0(3) . . ?
O37A N37 C34 118.34(12) . . ?
O37C N37 C34 118.66(19) . . ?
O37B N37 C34 112.2(5) . . ?
C52 N39 C48 111.24(9) . . ?
C52 N39 C40 110.97(9) . . ?
C48 N39 C40 106.87(9) . . ?
C52 N39 C44 105.82(9) . . ?
C48 N39 C44 110.94(9) . . ?
C40 N39 C44 111.07(9) . . ?
O25 C1 C26 125.12(11) . . ?
O25 C1 C2 114.55(10) . . ?
C26 C1 C2 120.33(11) . . ?
C3 C2 C1 119.44(11) . . ?
C3 C2 N29 120.19(10) . . ?
C1 C2 N29 120.33(10) . . ?
O4 C3 C28 124.56(11) . . ?
O4 C3 C2 114.39(10) . . ?
C28 C3 C2 121.04(11) . . ?
O4 C5 C6 110.67(10) . . ?
O4 C5 H5A 111.8(7) . . ?
C6 C5 H5A 108.9(8) . . ?
O4 C5 H5B 110.8(7) . . ?
C6 C5 H5B 108.2(8) . . ?
H5A C5 H5B 106.3(11) . . ?
O6 C6 N7 124.09(12) . . ?
O6 C6 C5 118.90(11) . . ?
N7 C6 C5 117.00(11) . . ?
N7 C8 C9 112.73(11) . . ?
N7 C8 H8A 109.6(7) . . ?
C9 C8 H8A 108.1(7) . . ?
N7 C8 H8B 106.3(8) . . ?
C9 C8 H8B 111.8(8) . . ?
H8A C8 H8B 108.1(10) . . ?
N10 C9 C8 113.39(11) . . ?
N10 C9 H9A 105.2(7) . . ?
C8 C9 H9A 112.8(7) . . ?
N10 C9 H9B 108.1(7) . . ?
C8 C9 H9B 107.6(7) . . ?
H9A C9 H9B 109.6(10) . . ?
O11 C11 N10 123.33(11) . . ?
O11 C11 C12 121.04(11) . . ?
N10 C11 C12 115.56(11) . . ?
N17 C12 C13 122.87(12) . . ?
N17 C12 C11 117.05(10) . . ?
C13 C12 C11 120.03(11) . . ?
C14 C13 C12 119.10(13) . . ?
C14 C13 H13 121.5(8) . . ?
C12 C13 H13 119.4(8) . . ?
C15 C14 C13 118.73(12) . . ?
C15 C14 H14 122.2(9) . . ?
C13 C14 H14 119.0(9) . . ?
C14 C15 C16 118.81(12) . . ?
C14 C15 H15 121.9(7) . . ?
C16 C15 H15 119.3(7) . . ?
N17 C16 C15 123.04(11) . . ?
N17 C16 C18 116.92(10) . . ?
C15 C16 C18 120.03(11) . . ?
O18 C18 N19 123.27(12) . . ?
O18 C18 C16 120.68(11) . . ?
N19 C18 C16 116.03(10) . . ?
N19 C20 C21 113.65(11) . . ?
N19 C20 H20A 107.9(7) . . ?
C21 C20 H20A 106.0(7) . . ?
N19 C20 H20B 108.1(7) . . ?
C21 C20 H20B 109.9(7) . . ?
H20A C20 H20B 111.3(10) . . ?
N22 C21 C20 111.76(10) . . ?
N22 C21 H21A 110.2(7) . . ?
C20 C21 H21A 110.4(8) . . ?
N22 C21 H21B 108.3(7) . . ?
C20 C21 H21B 108.5(7) . . ?
H21A C21 H21B 107.4(10) . . ?
O23 C23 N22 123.33(11) . . ?
O23 C23 C24 119.13(11) . . ?
N22 C23 C24 117.41(10) . . ?
O25 C24 C23 114.31(10) . . ?
O25 C24 H24A 104.9(7) . . ?
C23 C24 H24A 108.0(8) . . ?
O25 C24 H24B 112.8(8) . . ?
C23 C24 H24B 109.3(8) . . ?
H24A C24 H24B 107.1(11) . . ?
C27 C26 C1 118.88(12) . . ?
C27 C26 H26 120.0(8) . . ?
C1 C26 H26 121.1(8) . . ?
C28 C27 C26 122.06(12) . . ?
C28 C27 H27 119.1(8) . . ?
C26 C27 H27 118.9(8) . . ?
C27 C28 C3 118.20(12) . . ?
C27 C28 H28 122.2(8) . . ?
C3 C28 H28 119.6(9) . . ?
O30 C30 N29 122.16(11) . . ?
O30 C30 C31 120.96(10) . . ?
N29 C30 C31 116.85(10) . . ?
C32 C31 C36 119.38(11) . . ?
C32 C31 C30 122.76(11) . . ?
C36 C31 C30 117.82(11) . . ?
C33 C32 C31 120.46(12) . . ?
C33 C32 H32 117.8(7) . . ?
C31 C32 H32 121.8(7) . . ?
C34 C33 C32 118.48(12) . . ?
C34 C33 H33 118.6(8) . . ?
C32 C33 H33 122.9(8) . . ?
C33 C34 C35 122.67(12) . . ?
C33 C34 N37 118.77(12) . . ?
C35 C34 N37 118.45(12) . . ?
C36 C35 C34 118.31(12) . . ?
C36 C35 H35 121.1(8) . . ?
C34 C35 H35 120.6(8) . . ?
C35 C36 C31 120.69(12) . . ?
C35 C36 H36 119.9(8) . . ?
C31 C36 H36 119.4(8) . . ?
C41 C40 N39 115.55(10) . . ?
C41 C40 H40A 111.4(7) . . ?
N39 C40 H40A 105.8(7) . . ?
C41 C40 H40B 111.3(7) . . ?
N39 C40 H40B 105.0(7) . . ?
H40A C40 H40B 107.2(10) . . ?
C40 C41 C42 110.83(12) . . ?
C40 C41 H41A 111.2(8) . . ?
C42 C41 H41A 107.9(8) . . ?
C40 C41 H41B 109.8(8) . . ?
C42 C41 H41B 110.9(8) . . ?
H41A C41 H41B 106.1(11) . . ?
C43 C42 C41 112.38(16) . . ?
C43 C42 H42A 111.8(9) . . ?
C41 C42 H42A 108.4(9) . . ?
C43 C42 H42B 110.1(9) . . ?
C41 C42 H42B 107.5(9) . . ?
H42A C42 H42B 106.4(13) . . ?
C42 C43 H43A 110.4(12) . . ?
C42 C43 H43B 110.1(10) . . ?
H43A C43 H43B 108.6(15) . . ?
C42 C43 H43C 112.9(10) . . ?
H43A C43 H43C 110.0(15) . . ?
H43B C43 H43C 104.6(15) . . ?
C45 C44 N39 116.90(10) . . ?
C45 C44 H44A 110.0(7) . . ?
N39 C44 H44A 104.2(7) . . ?
C45 C44 H44B 109.4(7) . . ?
N39 C44 H44B 106.5(7) . . ?
H44A C44 H44B 109.7(10) . . ?
C44 C45 C46 108.95(10) . . ?
C44 C45 H45A 111.2(7) . . ?
C46 C45 H45A 108.1(7) . . ?
C44 C45 H45B 109.9(8) . . ?
C46 C45 H45B 108.8(8) . . ?
H45A C45 H45B 109.9(11) . . ?
C47 C46 C45 113.13(11) . . ?
C47 C46 H46A 108.4(7) . . ?
C45 C46 H46A 108.9(7) . . ?
C47 C46 H46B 108.3(7) . . ?
C45 C46 H46B 110.4(7) . . ?
H46A C46 H46B 107.6(10) . . ?
C46 C47 H47A 109.2(8) . . ?
C46 C47 H47B 112.4(8) . . ?
H47A C47 H47B 107.9(11) . . ?
C46 C47 H47C 109.0(8) . . ?
H47A C47 H47C 111.3(12) . . ?
H47B C47 H47C 107.0(11) . . ?
C49 C48 N39 116.31(10) . . ?
C49 C48 H48A 109.8(7) . . ?
N39 C48 H48A 106.1(7) . . ?
C49 C48 H48B 109.6(7) . . ?
N39 C48 H48B 105.8(7) . . ?
H48A C48 H48B 109.0(10) . . ?
C48 C49 C50 109.29(10) . . ?
C48 C49 H49A 110.7(7) . . ?
C50 C49 H49A 107.9(7) . . ?
C48 C49 H49B 110.8(8) . . ?
C50 C49 H49B 110.6(8) . . ?
H49A C49 H49B 107.4(11) . . ?
C51 C50 C49 113.20(11) . . ?
C51 C50 H50A 108.8(8) . . ?
C49 C50 H50A 110.0(8) . . ?
C51 C50 H50B 109.2(7) . . ?
C49 C50 H50B 109.2(7) . . ?
H50A C50 H50B 106.3(11) . . ?
C50 C51 H51A 111.3(9) . . ?
C50 C51 H51B 111.8(9) . . ?
H51A C51 H51B 108.3(13) . . ?
C50 C51 H51C 111.3(10) . . ?
H51A C51 H51C 106.8(13) . . ?
H51B C51 H51C 107.2(13) . . ?
C53 C52 N39 116.40(10) . . ?
C53 C52 H52A 111.1(7) . . ?
N39 C52 H52A 106.0(7) . . ?
C53 C52 H52B 109.6(7) . . ?
N39 C52 H52B 106.4(7) . . ?
H52A C52 H52B 106.7(10) . . ?
C52 C53 C54 108.67(10) . . ?
C52 C53 H53A 112.4(8) . . ?
C54 C53 H53A 109.4(8) . . ?
C52 C53 H53B 112.1(8) . . ?
C54 C53 H53B 108.9(8) . . ?
H53A C53 H53B 105.3(11) . . ?
C55 C54 C53 112.85(11) . . ?
C55 C54 H54A 109.5(7) . . ?
C53 C54 H54A 108.9(7) . . ?
C55 C54 H54B 111.8(8) . . ?
C53 C54 H54B 108.2(8) . . ?
H54A C54 H54B 105.3(10) . . ?
C54 C55 H55A 110.5(8) . . ?
C54 C55 H55B 111.2(9) . . ?
H55A C55 H55B 105.7(13) . . ?
C54 C55 H55C 108.9(10) . . ?
H55A C55 H55C 112.1(13) . . ?
H55B C55 H55C 108.4(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O37B O37C N37 O37A 103.1(11) . . . . ?
O37B O37C N37 C34 -86.5(11) . . . . ?
O37C O37B N37 O37A -98.4(10) . . . . ?
O37C O37B N37 C34 108.9(9) . . . . ?
C24 O25 C1 C26 -1.75(16) . . . . ?
C24 O25 C1 C2 177.83(10) . . . . ?
O25 C1 C2 C3 178.66(10) . . . . ?
C26 C1 C2 C3 -1.73(17) . . . . ?
O25 C1 C2 N29 1.10(15) . . . . ?
C26 C1 C2 N29 -179.30(10) . . . . ?
C30 N29 C2 C3 68.50(14) . . . . ?
C30 N29 C2 C1 -113.95(12) . . . . ?
C5 O4 C3 C28 -32.58(16) . . . . ?
C5 O4 C3 C2 149.08(10) . . . . ?
C1 C2 C3 O4 -178.66(10) . . . . ?
N29 C2 C3 O4 -1.09(15) . . . . ?
C1 C2 C3 C28 2.94(17) . . . . ?
N29 C2 C3 C28 -179.49(11) . . . . ?
C3 O4 C5 C6 -124.53(11) . . . . ?
C8 N7 C6 O6 3.80(18) . . . . ?
C8 N7 C6 C5 -177.18(11) . . . . ?
O4 C5 C6 O6 -168.91(10) . . . . ?
O4 C5 C6 N7 12.02(15) . . . . ?
C6 N7 C8 C9 -154.68(11) . . . . ?
C11 N10 C9 C8 74.44(15) . . . . ?
N7 C8 C9 N10 66.46(15) . . . . ?
C9 N10 C11 O11 -0.01(19) . . . . ?
C9 N10 C11 C12 -177.17(10) . . . . ?
C16 N17 C12 C13 -0.16(17) . . . . ?
C16 N17 C12 C11 177.06(10) . . . . ?
O11 C11 C12 N17 169.84(11) . . . . ?
N10 C11 C12 N17 -12.93(16) . . . . ?
O11 C11 C12 C13 -12.86(18) . . . . ?
N10 C11 C12 C13 164.38(12) . . . . ?
N17 C12 C13 C14 2.04(19) . . . . ?
C11 C12 C13 C14 -175.10(11) . . . . ?
C12 C13 C14 C15 -1.69(19) . . . . ?
C13 C14 C15 C16 -0.37(19) . . . . ?
C12 N17 C16 C15 -2.07(17) . . . . ?
C12 N17 C16 C18 177.22(10) . . . . ?
C14 C15 C16 N17 2.36(19) . . . . ?
C14 C15 C16 C18 -176.91(11) . . . . ?
C20 N19 C18 O18 3.44(18) . . . . ?
C20 N19 C18 C16 -175.26(10) . . . . ?
N17 C16 C18 O18 -178.44(11) . . . . ?
C15 C16 C18 O18 0.87(18) . . . . ?
N17 C16 C18 N19 0.30(16) . . . . ?
C15 C16 C18 N19 179.61(11) . . . . ?
C18 N19 C20 C21 -86.79(14) . . . . ?
C23 N22 C21 C20 -157.22(11) . . . . ?
N19 C20 C21 N22 -74.63(14) . . . . ?
C21 N22 C23 O23 -5.65(18) . . . . ?
C21 N22 C23 C24 170.26(11) . . . . ?
C1 O25 C24 C23 78.61(13) . . . . ?
O23 C23 C24 O25 -157.41(11) . . . . ?
N22 C23 C24 O25 26.50(16) . . . . ?
O25 C1 C26 C27 179.45(11) . . . . ?
C2 C1 C26 C27 -0.10(17) . . . . ?
C1 C26 C27 C28 0.81(19) . . . . ?
C26 C27 C28 C3 0.35(19) . . . . ?
O4 C3 C28 C27 179.53(11) . . . . ?
C2 C3 C28 C27 -2.24(18) . . . . ?
C2 N29 C30 O30 4.50(17) . . . . ?
C2 N29 C30 C31 -173.44(10) . . . . ?
O30 C30 C31 C32 -167.75(11) . . . . ?
N29 C30 C31 C32 10.22(16) . . . . ?
O30 C30 C31 C36 9.95(16) . . . . ?
N29 C30 C31 C36 -172.08(10) . . . . ?
C36 C31 C32 C33 0.25(18) . . . . ?
C30 C31 C32 C33 177.91(11) . . . . ?
C31 C32 C33 C34 0.76(19) . . . . ?
C32 C33 C34 C35 -1.6(2) . . . . ?
C32 C33 C34 N37 174.64(12) . . . . ?
O37A N37 C34 C33 -3.9(2) . . . . ?
O37C N37 C34 C33 -174.72(17) . . . . ?
O37B N37 C34 C33 150.4(4) . . . . ?
O37A N37 C34 C35 172.47(13) . . . . ?
O37C N37 C34 C35 1.6(2) . . . . ?
O37B N37 C34 C35 -33.2(5) . . . . ?
C33 C34 C35 C36 1.3(2) . . . . ?
N37 C34 C35 C36 -174.93(12) . . . . ?
C34 C35 C36 C31 -0.21(18) . . . . ?
C32 C31 C36 C35 -0.53(18) . . . . ?
C30 C31 C36 C35 -178.31(11) . . . . ?
C52 N39 C40 C41 -49.73(14) . . . . ?
C48 N39 C40 C41 -171.17(11) . . . . ?
C44 N39 C40 C41 67.69(13) . . . . ?
N39 C40 C41 C42 -159.27(11) . . . . ?
C40 C41 C42 C43 179.93(13) . . . . ?
C52 N39 C44 C45 -178.76(11) . . . . ?
C48 N39 C44 C45 -57.98(14) . . . . ?
C40 N39 C44 C45 60.73(14) . . . . ?
N39 C44 C45 C46 177.29(11) . . . . ?
C44 C45 C46 C47 -175.96(12) . . . . ?
C52 N39 C48 C49 56.89(13) . . . . ?
C40 N39 C48 C49 178.16(10) . . . . ?
C44 N39 C48 C49 -60.62(13) . . . . ?
N39 C48 C49 C50 -176.54(10) . . . . ?
C48 C49 C50 C51 177.91(13) . . . . ?
C48 N39 C52 C53 57.16(14) . . . . ?
C40 N39 C52 C53 -61.69(14) . . . . ?
C44 N39 C52 C53 177.74(11) . . . . ?
N39 C52 C53 C54 177.65(11) . . . . ?
C52 C53 C54 C55 179.40(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O4 0.826(13) 2.233(13) 2.6412(14) 110.7(11) .
N10 H10 Cl1 0.831(14) 2.552(15) 3.3143(11) 153.0(12) .
N19 H19 Cl1 0.895(14) 2.451(14) 3.2468(11) 148.3(12) .
N22 H22 Cl1 0.861(14) 2.629(14) 3.4663(11) 164.5(12) .
N29 H29 Cl1 0.923(14) 2.244(15) 3.1235(11) 159.2(12) .
O38 H38A O6 1.14(3) 1.71(3) 2.8259(13) 167(2) .
O38 H38B O30 1.05(2) 1.82(2) 2.8652(13) 178.6(18) 1_655

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        28.50
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.041
