# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

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

data_C6BPC@CB6
_audit_block_doi                 10.5517/cc14j2d4
_database_code_depnum_ccdc_archive 'CCDC 1058135'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C5CC04409J 2015
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2016-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        C6BPC-CB6
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H56 N26 O16'
_chemical_formula_weight         1325.25

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p-1

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

_cell_length_a                   12.0755(7)
_cell_length_b                   12.3189(6)
_cell_length_c                   12.3197(6)
_cell_angle_alpha                106.538(4)
_cell_angle_beta                 97.085(5)
_cell_angle_gamma                107.693(5)
_cell_volume                     1628.92(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             690
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11534
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.85
_diffrn_reflns_theta_max         67.08
_reflns_number_total             5822
_reflns_number_gt                4872
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0411P)²+2.3783P] 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         5822
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1263
_refine_ls_wR_factor_gt          0.1225
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.41547(15) 0.14049(15) 0.10027(14) 0.0231(4) Uani 1 1 d . . .
O2 O -0.28908(15) 0.11998(15) -0.15055(14) 0.0247(4) Uani 1 1 d . . .
O3 O 0.07101(15) 0.36158(16) 0.33908(15) 0.0248(4) Uani 1 1 d . . .
O4 O 0.06841(16) -0.07437(16) -0.38506(15) 0.0256(4) Uani 1 1 d . . .
O5 O -0.04754(15) 0.38686(15) 0.06676(15) 0.0248(4) Uani 1 1 d . . .
O6 O 0.30714(16) 0.17116(16) -0.15693(15) 0.0260(4) Uani 1 1 d . . .
O7 O 0.66455(17) 0.54730(16) 0.26399(16) 0.0304(4) Uani 1 1 d . . .
O8 O 0.64088(19) 0.49338(17) 0.42074(16) 0.0335(5) Uani 1 1 d . . .
N6 N 0.21827(18) 0.27890(18) 0.35722(17) 0.0195(4) Uani 1 1 d . . .
N1 N -0.27165(18) -0.02164(18) -0.30981(17) 0.0204(4) Uani 1 1 d . . .
N10 N 0.16059(18) 0.25067(18) -0.18861(17) 0.0197(4) Uani 1 1 d . . .
N13 N 0.78277(18) 0.18707(18) 0.18217(17) 0.0200(4) Uani 1 1 d . . .
N2 N -0.13649(18) 0.16475(18) -0.24574(17) 0.0206(4) Uani 1 1 d . . .
N11 N 0.00289(18) 0.08804(18) -0.34206(17) 0.0206(4) Uani 1 1 d . . .
N7 N 0.37089(18) 0.20928(18) 0.27928(17) 0.0208(4) Uani 1 1 d . . .
N12 N -0.13146(18) -0.09883(17) -0.40564(17) 0.0205(4) Uani 1 1 d . . .
N5 N 0.22988(18) 0.39764(18) 0.25041(17) 0.0210(4) Uani 1 1 d . . .
N3 N 0.02192(18) 0.33528(18) -0.10012(17) 0.0214(4) Uani 1 1 d . . .
N8 N 0.37035(18) 0.31467(18) 0.15995(17) 0.0208(4) Uani 1 1 d . . .
N4 N 0.15243(18) 0.41896(18) 0.06983(17) 0.0222(4) Uani 1 1 d . . .
N9 N 0.29388(18) 0.33663(19) -0.01943(17) 0.0229(4) Uani 1 1 d . . .
C1 C 0.0327(2) 0.3802(2) 0.0173(2) 0.0204(5) Uani 1 1 d . . .
C2 C 0.1632(2) 0.3479(2) 0.3177(2) 0.0205(5) Uani 1 1 d . . .
C3 C -0.2369(2) 0.0914(2) -0.2271(2) 0.0196(5) Uani 1 1 d . . .
C4 C 0.7133(2) 0.3792(2) 0.2763(2) 0.0189(5) Uani 1 1 d . . .
C5 C 0.3879(2) 0.2136(2) 0.1719(2) 0.0186(5) Uani 1 1 d . . .
C6 C -0.0122(2) -0.0333(2) -0.37706(19) 0.0200(5) Uani 1 1 d . . .
C7 C 0.1358(2) 0.3583(2) -0.1323(2) 0.0194(5) Uani 1 1 d . . .
H7 H 0.1461 0.4127 -0.1779 0.023 Uiso 1 1 calc R . .
C8 C 0.7343(2) 0.2340(2) 0.1122(2) 0.0226(5) Uani 1 1 d . . .
H8 H 0.7241 0.2009 0.0322 0.027 Uiso 1 1 calc R . .
C9 C 0.3409(2) 0.3105(2) 0.3443(2) 0.0194(5) Uani 1 1 d . . .
H9 H 0.3978 0.3567 0.4196 0.023 Uiso 1 1 calc R . .
C10 C 0.6697(2) 0.4825(2) 0.3253(2) 0.0220(5) Uani 1 1 d . . .
C11 C -0.2037(2) -0.0234(2) -0.3988(2) 0.0200(5) Uani 1 1 d . . .
H11 H -0.2545 -0.0417 -0.4750 0.024 Uiso 1 1 calc R . .
C12 C 0.6993(2) 0.3307(2) 0.1574(2) 0.0225(5) Uani 1 1 d . . .
H12 H 0.6663 0.3633 0.1081 0.027 Uiso 1 1 calc R . .
C13 C -0.1095(2) 0.1075(2) -0.3544(2) 0.0189(5) Uani 1 1 d . . .
H13 H -0.1169 0.1497 -0.4099 0.023 Uiso 1 1 calc R . .
C14 C 0.3468(2) 0.3870(2) 0.2643(2) 0.0205(5) Uani 1 1 d . . .
H14 H 0.4105 0.4666 0.3000 0.025 Uiso 1 1 calc R . .
C15 C 0.2583(2) 0.2449(2) -0.1252(2) 0.0202(5) Uani 1 1 d . . .
C16 C 0.8013(2) 0.2350(2) 0.2987(2) 0.0237(5) Uani 1 1 d . . .
H16 H 0.8380 0.2034 0.3465 0.028 Uiso 1 1 calc R . .
C17 C 0.2277(2) 0.4177(2) -0.0135(2) 0.0204(5) Uani 1 1 d . . .
H17 H 0.2800 0.4998 -0.0038 0.024 Uiso 1 1 calc R . .
C18 C 0.7663(2) 0.3303(2) 0.3469(2) 0.0234(5) Uani 1 1 d . . .
H18 H 0.7781 0.3624 0.4273 0.028 Uiso 1 1 calc R . .
C19 C 0.3981(2) 0.3573(2) 0.0654(2) 0.0225(5) Uani 1 1 d . . .
H19A H 0.4443 0.4435 0.0969 0.027 Uiso 1 1 calc R . .
H19B H 0.4474 0.3168 0.0271 0.027 Uiso 1 1 calc R . .
C20 C 0.1974(2) 0.4763(2) 0.1942(2) 0.0225(5) Uani 1 1 d . . .
H20A H 0.1370 0.5016 0.2279 0.027 Uiso 1 1 calc R . .
H20B H 0.2670 0.5484 0.2099 0.027 Uiso 1 1 calc R . .
C21 C -0.1803(2) -0.2303(2) -0.4457(2) 0.0221(5) Uani 1 1 d . . .
H21A H -0.2481 -0.2588 -0.5110 0.026 Uiso 1 1 calc R . .
H21B H -0.1203 -0.2612 -0.4734 0.026 Uiso 1 1 calc R . .
C22 C 0.1171(2) 0.1838(2) -0.3119(2) 0.0212(5) Uani 1 1 d . . .
H22A H 0.1111 0.2398 -0.3521 0.025 Uiso 1 1 calc R . .
H22B H 0.1750 0.1493 -0.3394 0.025 Uiso 1 1 calc R . .
C23 C -0.3836(2) -0.1159(2) -0.3226(2) 0.0198(5) Uani 1 1 d . . .
H23A H -0.4341 -0.0795 -0.2817 0.024 Uiso 1 1 calc R . .
H23B H -0.4237 -0.1527 -0.4044 0.024 Uiso 1 1 calc R . .
C24 C 0.8130(2) 0.0782(2) 0.1291(2) 0.0252(5) Uani 1 1 d . . .
H24A H 0.7470 0.0207 0.0652 0.030 Uiso 1 1 calc R . .
H24B H 0.8222 0.0399 0.1867 0.030 Uiso 1 1 calc R . .
C25 C -0.0886(2) 0.2949(2) -0.1845(2) 0.0217(5) Uani 1 1 d . . .
H25A H -0.0760 0.3359 -0.2408 0.026 Uiso 1 1 calc R . .
H25B H -0.1471 0.3179 -0.1453 0.026 Uiso 1 1 calc R . .
C26 C 0.9247(2) 0.1058(2) 0.0847(2) 0.0262(5) Uani 1 1 d . . .
H26A H 0.9923 0.1584 0.1491 0.031 Uiso 1 1 calc R . .
H26B H 0.9181 0.1479 0.0301 0.031 Uiso 1 1 calc R . .
C27 C 0.9454(2) -0.0102(2) 0.0251(2) 0.0265(6) Uani 1 1 d . . .
H27A H 0.9534 -0.0508 0.0809 0.032 Uiso 1 1 calc R . .
H27B H 0.8760 -0.0635 -0.0370 0.032 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C5 1.226(3) . ?
O2 C3 1.226(3) . ?
O3 C2 1.224(3) . ?
O4 C6 1.228(3) . ?
O5 C1 1.217(3) . ?
O6 C15 1.227(3) . ?
O7 C10 1.255(3) . ?
O8 C10 1.249(3) . ?
N6 C2 1.379(3) . ?
N6 C21 1.444(3) 2 ?
N6 C9 1.453(3) . ?
N1 C3 1.373(3) . ?
N1 C23 1.446(3) . ?
N1 C11 1.447(3) . ?
N10 C15 1.365(3) . ?
N10 C22 1.445(3) . ?
N10 C7 1.449(3) . ?
N13 C8 1.336(3) . ?
N13 C16 1.349(3) . ?
N13 C24 1.489(3) . ?
N2 C3 1.364(3) . ?
N2 C13 1.450(3) . ?
N2 C25 1.454(3) . ?
N11 C6 1.379(3) . ?
N11 C22 1.438(3) . ?
N11 C13 1.446(3) . ?
N7 C5 1.377(3) . ?
N7 C23 1.438(3) 2 ?
N7 C9 1.451(3) . ?
N12 C6 1.362(3) . ?
N12 C11 1.448(3) . ?
N12 C21 1.452(3) . ?
N5 C2 1.366(3) . ?
N5 C14 1.451(3) . ?
N5 C20 1.456(3) . ?
N3 C1 1.368(3) . ?
N3 C25 1.438(3) . ?
N3 C7 1.445(3) . ?
N8 C5 1.369(3) . ?
N8 C19 1.443(3) . ?
N8 C14 1.456(3) . ?
N4 C1 1.382(3) . ?
N4 C20 1.445(3) . ?
N4 C17 1.452(3) . ?
N9 C15 1.374(3) . ?
N9 C19 1.439(3) . ?
N9 C17 1.449(3) . ?
C4 C12 1.381(3) . ?
C4 C18 1.387(3) . ?
C4 C10 1.521(3) . ?
C7 C17 1.551(3) . ?
C8 C12 1.376(3) . ?
C9 C14 1.540(3) . ?
C11 C13 1.557(3) . ?
C16 C18 1.370(3) . ?
C21 N6 1.444(3) 2 ?
C23 N7 1.438(3) 2 ?
C24 C26 1.497(3) . ?
C26 C27 1.520(3) . ?
C27 C27 1.507(5) 2_755 ?

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 N6 C21 120.89(19) . 2 ?
C2 N6 C9 110.83(19) . . ?
C21 N6 C9 122.15(19) 2 . ?
C3 N1 C23 121.87(19) . . ?
C3 N1 C11 112.27(19) . . ?
C23 N1 C11 123.68(19) . . ?
C15 N10 C22 121.83(19) . . ?
C15 N10 C7 112.00(19) . . ?
C22 N10 C7 122.55(19) . . ?
C8 N13 C16 120.9(2) . . ?
C8 N13 C24 118.8(2) . . ?
C16 N13 C24 120.3(2) . . ?
C3 N2 C13 112.03(19) . . ?
C3 N2 C25 121.68(19) . . ?
C13 N2 C25 123.38(19) . . ?
C6 N11 C22 123.7(2) . . ?
C6 N11 C13 112.4(2) . . ?
C22 N11 C13 123.44(19) . . ?
C5 N7 C23 123.62(19) . 2 ?
C5 N7 C9 112.43(19) . . ?
C23 N7 C9 123.94(19) 2 . ?
C6 N12 C11 112.64(19) . . ?
C6 N12 C21 123.4(2) . . ?
C11 N12 C21 123.9(2) . . ?
C2 N5 C14 112.25(19) . . ?
C2 N5 C20 122.4(2) . . ?
C14 N5 C20 123.8(2) . . ?
C1 N3 C25 123.5(2) . . ?
C1 N3 C7 113.0(2) . . ?
C25 N3 C7 122.04(19) . . ?
C5 N8 C19 122.83(19) . . ?
C5 N8 C14 112.31(19) . . ?
C19 N8 C14 123.5(2) . . ?
C1 N4 C20 122.4(2) . . ?
C1 N4 C17 112.58(19) . . ?
C20 N4 C17 124.0(2) . . ?
C15 N9 C19 121.6(2) . . ?
C15 N9 C17 112.3(2) . . ?
C19 N9 C17 125.3(2) . . ?
O5 C1 N3 126.6(2) . . ?
O5 C1 N4 126.2(2) . . ?
N3 C1 N4 107.2(2) . . ?
O3 C2 N5 126.4(2) . . ?
O3 C2 N6 126.0(2) . . ?
N5 C2 N6 107.6(2) . . ?
O2 C3 N2 126.6(2) . . ?
O2 C3 N1 124.9(2) . . ?
N2 C3 N1 108.5(2) . . ?
C12 C4 C18 118.3(2) . . ?
C12 C4 C10 119.5(2) . . ?
C18 C4 C10 122.2(2) . . ?
O1 C5 N8 126.1(2) . . ?
O1 C5 N7 125.9(2) . . ?
N8 C5 N7 108.01(19) . . ?
O4 C6 N12 126.3(2) . . ?
O4 C6 N11 125.4(2) . . ?
N12 C6 N11 108.2(2) . . ?
N3 C7 N10 114.78(19) . . ?
N3 C7 C17 103.51(18) . . ?
N10 C7 C17 103.75(18) . . ?
N13 C8 C12 120.7(2) . . ?
N7 C9 N6 114.74(19) . . ?
N7 C9 C14 103.43(18) . . ?
N6 C9 C14 103.68(18) . . ?
O8 C10 O7 126.6(2) . . ?
O8 C10 C4 117.4(2) . . ?
O7 C10 C4 116.0(2) . . ?
N1 C11 N12 115.47(19) . . ?
N1 C11 C13 103.01(18) . . ?
N12 C11 C13 103.39(19) . . ?
C8 C12 C4 119.7(2) . . ?
N11 C13 N2 114.80(19) . . ?
N11 C13 C11 103.16(18) . . ?
N2 C13 C11 103.48(18) . . ?
N5 C14 N8 115.4(2) . . ?
N5 C14 C9 103.08(18) . . ?
N8 C14 C9 103.60(18) . . ?
O6 C15 N10 126.1(2) . . ?
O6 C15 N9 125.5(2) . . ?
N10 C15 N9 108.4(2) . . ?
N13 C16 C18 120.1(2) . . ?
N9 C17 N4 115.73(19) . . ?
N9 C17 C7 103.01(18) . . ?
N4 C17 C7 102.93(19) . . ?
C16 C18 C4 120.2(2) . . ?
N9 C19 N8 113.4(2) . . ?
N4 C20 N5 113.17(19) . . ?
N6 C21 N12 113.57(19) 2 . ?
N11 C22 N10 114.06(19) . . ?
N7 C23 N1 113.92(19) 2 . ?
N13 C24 C26 113.6(2) . . ?
N3 C25 N2 113.61(19) . . ?
C24 C26 C27 110.6(2) . . ?
C27 C27 C26 113.7(3) 2_755 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        67.08
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.057

# SQUEEZE RESULTS
# 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 -0.499 0.001 0.500 403 134 ' '
_platon_squeeze_details          ?

####################################################################### 
# 
# 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_C6BPCA@CB6-NO3
_audit_block_doi                 10.5517/cc14j2f5
_database_code_depnum_ccdc_archive 'CCDC 1058136'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C5CC04409J 2015
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2016-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        C6BPCA-CB6-NO3
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H104 N56 O44'
_chemical_formula_weight         2890.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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                   12.5869(4)
_cell_length_b                   16.1378(8)
_cell_length_c                   17.8631(7)
_cell_angle_alpha                87.780(4)
_cell_angle_beta                 89.749(3)
_cell_angle_gamma                67.888(4)
_cell_volume                     3358.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19476
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0822
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         67.08
_reflns_number_total             11508
_reflns_number_gt                6002
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11508
_refine_ls_number_parameters     874
_refine_ls_number_restraints     880
_refine_ls_R_factor_all          0.2878
_refine_ls_R_factor_gt           0.2422
_refine_ls_wR_factor_ref         0.6357
_refine_ls_wR_factor_gt          0.5971
_refine_ls_goodness_of_fit_ref   2.240
_refine_ls_restrained_S_all      2.191
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.006

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.0911(7) 0.7398(6) -0.3295(4) 0.130(4) Uani 1 1 d . . .
O2 O 0.2707(5) 0.3555(5) -0.3241(4) 0.092(2) Uani 1 1 d . . .
O3 O 0.0336(6) 0.7775(5) -0.4992(4) 0.105(3) Uani 1 1 d . . .
O4 O -0.0613(6) 0.7376(6) -0.6763(4) 0.125(4) Uani 1 1 d . . .
O5 O 0.3095(5) 0.3526(6) -0.6574(4) 0.105(3) Uani 1 1 d . . .
O6 O 0.4064(6) 0.3994(6) -0.4816(4) 0.106(3) Uani 1 1 d . . .
N68 N 0.3484(7) 0.5371(8) -0.5467(4) 0.122(5) Uani 1 1 d . . .
O8 O -0.0616(7) 1.1719(7) 0.2138(4) 0.133(4) Uani 1 1 d . . .
N66 N 0.0212(5) 0.6083(6) -0.7442(4) 0.087(3) Uani 1 1 d . . .
O10 O 0.1216(6) 0.7711(7) 0.1887(4) 0.130(4) Uani 1 1 d . . .
O11 O 0.3680(8) 0.9871(7) -0.0619(4) 0.135(4) Uani 1 1 d . . .
N69 N 0.3408(5) 0.5353(7) -0.4228(4) 0.094(3) Uani 1 1 d . . .
O7 O -0.1512(7) 0.7984(8) 0.0978(4) 0.144(5) Uani 1 1 d . . .
N70 N 0.1989(6) 0.6857(6) -0.5522(4) 0.087(3) Uani 1 1 d . . .
N64 N 0.1597(6) 0.4584(7) -0.7267(4) 0.090(3) Uani 1 1 d . . .
N75 N -0.0218(6) 0.6081(7) -0.2572(5) 0.097(3) Uani 1 1 d . . .
O12 O 0.3284(7) 0.8069(6) -0.1188(4) 0.115(3) Uani 1 1 d . . .
N67 N 0.1315(6) 0.6510(7) -0.6696(4) 0.094(3) Uani 1 1 d . . .
N53 N 0.1807(7) 1.1919(9) 0.0320(4) 0.137(6) Uani 1 1 d . . .
N56 N 0.2936(7) 0.7627(7) 0.1279(4) 0.097(3) Uani 1 1 d . . .
N73 N 0.1190(7) 0.4549(8) -0.2583(5) 0.111(4) Uani 1 1 d . . .
N51 N 0.0982(9) 1.1792(9) 0.1545(5) 0.137(6) Uani 1 1 d . . .
N72 N 0.2406(9) 0.5005(11) -0.3138(5) 0.150(7) Uani 1 1 d . . .
N59 N 0.0749(7) 0.7302(8) -0.1111(4) 0.118(4) Uani 1 1 d . . .
N57 N 0.1735(7) 0.7025(7) 0.0758(4) 0.101(3) Uani 1 1 d . . .
O9 O 0.1729(7) 0.9546(8) 0.2493(4) 0.152(5) Uani 1 1 d . . .
N61 N 0.3703(6) 0.7743(6) 0.0067(4) 0.081(2) Uani 1 1 d . . .
N65 N 0.2816(7) 0.5074(8) -0.6641(5) 0.112(4) Uani 1 1 d . . .
O60 O -0.5948(7) 1.0078(10) -0.3774(7) 0.176(6) Uani 1 1 d . . .
H60A H -0.6327 1.0223 -0.3392 0.264 Uiso 1 1 calc R . .
N60 N 0.2468(8) 0.7189(8) -0.0459(4) 0.109(4) Uani 1 1 d . . .
N54 N 0.2537(6) 1.0347(9) 0.1741(4) 0.112(4) Uani 1 1 d . . .
C37 C 0.3054(7) 0.6263(9) -0.4433(5) 0.096(2) Uani 1 1 d U . .
H37 H 0.3588 0.6499 -0.4212 0.116 Uiso 1 1 calc R . .
N62 N 0.3990(6) 0.8949(7) 0.0490(4) 0.092(3) Uani 1 1 d . . .
N48 N 0.4763(15) 0.4779(10) 0.1739(9) 0.129(4) Uiso 1 1 d . . .
C21 C -0.4868(11) 0.9910(11) -0.3620(8) 0.131(3) Uani 1 1 d U . .
N55 N 0.3224(7) 0.8858(8) 0.1696(5) 0.115(4) Uani 1 1 d . . .
N63 N 0.3411(7) 1.0498(7) 0.0532(5) 0.109(4) Uani 1 1 d . . .
N74 N 0.0979(9) 0.6532(8) -0.3141(5) 0.127(5) Uani 1 1 d . . .
N58 N -0.0074(8) 0.7300(7) 0.0132(4) 0.116(4) Uani 1 1 d . . .
N71 N 0.1905(7) 0.6871(8) -0.4306(5) 0.122(5) Uani 1 1 d . . .
C29 C 0.0299(10) 1.0281(11) -0.0266(6) 0.126(4) Uani 1 1 d U . .
H29A H -0.0187 1.0912 -0.0294 0.151 Uiso 1 1 calc R . .
H29B H 0.1038 1.0217 -0.0058 0.151 Uiso 1 1 calc R . .
C33 C 0.2262(10) 0.4351(11) -0.3045(7) 0.106(3) Uani 1 1 d U . .
C49 C 0.1236(9) 1.2369(9) 0.0977(6) 0.108(3) Uani 1 1 d U . .
H49 H 0.1624 1.2730 0.1191 0.129 Uiso 1 1 calc R . .
C38 C 0.3675(7) 0.4821(8) -0.4851(5) 0.089(3) Uani 1 1 d U . .
C45 C 0.2622(8) 0.4341(10) -0.6806(5) 0.097(3) Uani 1 1 d U . .
C42 C 0.0211(8) 0.6704(9) -0.6963(5) 0.106(3) Uani 1 1 d U . .
C41 C 0.3773(7) 0.5015(8) -0.6222(5) 0.093(2) Uani 1 1 d U . .
H41 H 0.4519 0.4775 -0.6400 0.112 Uiso 1 1 calc R . .
C30 C -0.0120(9) 0.6773(9) -0.3055(6) 0.107(3) Uani 1 1 d U . .
O59 O -0.4485(8) 1.0264(10) -0.3181(7) 0.185(7) Uani 1 1 d . . .
C39 C 0.3168(7) 0.6298(8) -0.5310(5) 0.095(2) Uani 1 1 d U . .
H39 H 0.3730 0.6547 -0.5483 0.114 Uiso 1 1 calc R . .
C31 C 0.0893(8) 0.5424(9) -0.2307(5) 0.107(3) Uani 1 1 d U . .
H31 H 0.0975 0.5412 -0.1761 0.129 Uiso 1 1 calc R . .
C44 C 0.1363(8) 0.5434(9) -0.7561(5) 0.103(3) Uani 1 1 d U . .
H44 H 0.1557 0.5420 -0.8093 0.124 Uiso 1 1 calc R . .
C46 C 0.1310(7) 0.3930(8) -0.7651(5) 0.101(3) Uani 1 1 d U . .
H46A H 0.1294 0.4059 -0.8187 0.122 Uiso 1 1 calc R . .
H46B H 0.1898 0.3342 -0.7549 0.122 Uiso 1 1 calc R . .
C56 C 0.3379(8) 0.7960(9) 0.1873(5) 0.099(2) Uani 1 1 d U . .
H56 H 0.3719 0.7639 0.2309 0.119 Uiso 1 1 calc R . .
C60 C 0.2722(8) 0.6773(9) 0.0289(5) 0.097(2) Uani 1 1 d U . .
H60 H 0.3082 0.6121 0.0266 0.116 Uiso 1 1 calc R . .
C35 C 0.3489(8) 0.4945(9) -0.3474(5) 0.102(3) Uani 1 1 d U . .
H35A H 0.3983 0.4318 -0.3491 0.122 Uiso 1 1 calc R . .
H35B H 0.3857 0.5227 -0.3148 0.122 Uiso 1 1 calc R . .
C59 C 0.3525(8) 0.7141(8) 0.0639(5) 0.098(2) Uani 1 1 d U . .
H59 H 0.4251 0.6661 0.0789 0.118 Uiso 1 1 calc R . .
C19 C -0.1172(10) 0.6172(10) -0.4794(6) 0.120(3) Uani 1 1 d U . .
H19A H -0.0796 0.6308 -0.4370 0.144 Uiso 1 1 calc R . .
H19B H -0.1732 0.5939 -0.4603 0.144 Uiso 1 1 calc R . .
C53 C 0.3531(8) 1.0108(9) 0.1314(5) 0.101(2) Uani 1 1 d U . .
H53 H 0.4081 1.0290 0.1580 0.121 Uiso 1 1 calc R . .
C43 C 0.2111(8) 0.5791(9) -0.7111(5) 0.102(2) Uani 1 1 d U . .
H43 H 0.2576 0.6013 -0.7444 0.122 Uiso 1 1 calc R . .
C54 C 0.4038(8) 0.9158(8) 0.1247(5) 0.102(2) Uani 1 1 d U . .
H54 H 0.4820 0.8904 0.1452 0.122 Uiso 1 1 calc R . .
C40 C 0.1653(8) 0.7135(9) -0.6301(5) 0.104(2) Uani 1 1 d U . .
H40A H 0.1019 0.7711 -0.6314 0.124 Uiso 1 1 calc R . .
H40B H 0.2290 0.7211 -0.6560 0.124 Uiso 1 1 calc R . .
C57 C 0.4460(9) 0.8100(9) 0.0145(5) 0.101(2) Uani 1 1 d U . .
H57 H 0.5218 0.7837 -0.0005 0.121 Uiso 1 1 calc R . .
C32 C 0.1726(8) 0.5776(9) -0.2712(5) 0.103(2) Uani 1 1 d U . .
H32 H 0.2199 0.5942 -0.2359 0.123 Uiso 1 1 calc R . .
C36 C 0.1328(8) 0.7277(9) -0.4959(6) 0.105(3) Uani 1 1 d U . .
C63 C 0.1970(8) 0.6926(9) -0.1074(5) 0.102(3) Uani 1 1 d U . .
H63A H 0.2218 0.6279 -0.1049 0.123 Uiso 1 1 calc R . .
H63B H 0.2265 0.7092 -0.1534 0.123 Uiso 1 1 calc R . .
C58 C 0.1867(8) 0.7485(8) 0.1361(5) 0.098(3) Uani 1 1 d U . .
C47 C -0.0836(8) 0.6077(9) -0.7746(5) 0.107(3) Uani 1 1 d U . .
H47 H -0.1240 0.6467 -0.8135 0.128 Uiso 1 1 calc R . .
C52 C 0.2481(9) 0.9613(10) 0.2033(6) 0.104(3) Uani 1 1 d U . .
C48 C -0.0136(9) 1.2070(9) 0.1658(6) 0.106(3) Uani 1 1 d U . .
C50 C 0.1878(9) 1.1254(9) 0.2054(5) 0.106(3) Uani 1 1 d U . .
H50A H 0.1547 1.1176 0.2531 0.128 Uiso 1 1 calc R . .
H50B H 0.2398 1.1557 0.2142 0.128 Uiso 1 1 calc R . .
C18 C -0.1777(10) 0.7021(10) -0.5269(6) 0.121(3) Uani 1 1 d U . .
H18A H -0.1208 0.7227 -0.5485 0.145 Uiso 1 1 calc R . .
H18B H -0.2182 0.6885 -0.5678 0.145 Uiso 1 1 calc R . .
N1 N -0.2580(5) 0.7728(5) -0.4850(3) 0.103(4) Uani 1 1 d G . .
C13 C -0.2218(4) 0.8361(5) -0.4549(4) 0.126(3) Uani 1 1 d GU . .
H13 H -0.1467 0.8320 -0.4617 0.151 Uiso 1 1 calc R . .
C14 C -0.2978(6) 0.9053(5) -0.4146(5) 0.129(3) Uani 1 1 d GU . .
H14 H -0.2736 0.9476 -0.3944 0.155 Uiso 1 1 calc R . .
C15 C -0.4100(5) 0.9113(5) -0.4044(4) 0.129(3) Uani 1 1 d GU . .
C16 C -0.4461(4) 0.8481(6) -0.4346(5) 0.131(3) Uani 1 1 d GU . .
H16 H -0.5212 0.8521 -0.4278 0.157 Uiso 1 1 calc R . .
C17 C -0.3702(5) 0.7789(5) -0.4749(4) 0.128(3) Uani 1 1 d GU . .
H17 H -0.3944 0.7366 -0.4950 0.154 Uiso 1 1 calc R . .
C20 C -0.0303(10) 0.5479(10) -0.5244(6) 0.126(4) Uani 1 1 d U . .
H20A H 0.0285 0.5697 -0.5406 0.151 Uiso 1 1 calc R . .
H20B H -0.0671 0.5377 -0.5688 0.151 Uiso 1 1 calc R . .
C51 C 0.3095(9) 1.1409(10) 0.0296(6) 0.112(3) Uani 1 1 d U . .
H51A H 0.3358 1.1442 -0.0211 0.134 Uiso 1 1 calc R . .
H51B H 0.3471 1.1689 0.0617 0.134 Uiso 1 1 calc R . .
C65 C -0.0016(9) 0.7035(10) -0.0634(5) 0.110(3) Uani 1 1 d U . .
H65 H 0.0138 0.6395 -0.0663 0.132 Uiso 1 1 calc R . .
O13 O 0.2662(11) 0.8534(9) -0.4652(8) 0.172(5) Uani 1 1 d U . .
C64 C -0.1098(9) 0.7848(10) 0.0340(6) 0.114(4) Uani 1 1 d U . .
C34 C 0.1441(9) 0.7161(10) -0.3551(6) 0.110(3) Uani 1 1 d U . .
H34A H 0.0832 0.7748 -0.3605 0.132 Uiso 1 1 calc R . .
H34B H 0.2045 0.7220 -0.3248 0.132 Uiso 1 1 calc R . .
C27 C 0.1094(11) 1.0433(11) -0.1532(7) 0.132(3) Uani 1 1 d U . .
H27A H 0.0637 1.1070 -0.1549 0.159 Uiso 1 1 calc R . .
H27B H 0.1834 1.0335 -0.1306 0.159 Uiso 1 1 calc R . .
C55 C 0.3714(9) 0.9850(9) 0.0029(6) 0.107(3) Uani 1 1 d U . .
C61 C 0.3170(9) 0.7667(9) -0.0573(5) 0.094(3) Uani 1 1 d U . .
C62 C 0.0839(10) 0.6844(9) 0.0698(5) 0.107(3) Uani 1 1 d U . .
H62 H 0.0753 0.6409 0.1022 0.129 Uiso 1 1 calc R . .
O19 O 0.4667(14) 0.5610(11) 0.2014(10) 0.184(5) Uiso 1 1 d . . .
C28 C 0.0449(10) 0.9892(11) -0.1053(6) 0.124(3) Uani 1 1 d U . .
H28A H -0.0290 0.9985 -0.1277 0.149 Uiso 1 1 calc R . .
H28B H 0.0908 0.9255 -0.1027 0.149 Uiso 1 1 calc R . .
N47 N 0.1702(17) 0.4316(16) 0.0001(13) 0.166(6) Uiso 1 1 d . . .
O16 O 0.124(2) 0.4700(16) 0.0579(16) 0.254(9) Uiso 1 1 d . . .
O15 O 0.1918(18) 0.4781(15) -0.0369(13) 0.221(8) Uiso 1 1 d . . .
O20 O 0.3791(18) 0.4766(13) 0.1616(12) 0.216(7) Uiso 1 1 d . . .
O18 O 0.555(3) 0.472(2) 0.156(2) 0.329(15) Uiso 1 1 d . . .
O17 O 0.198(4) 0.355(4) -0.026(3) 0.45(2) Uiso 1 1 d . . .
O14 O 0.1355(12) 0.9875(10) -0.5090(6) 0.164(5) Uani 1 1 d U . .
C66 C 0.1773(13) 0.9388(14) -0.4647(7) 0.140(3) Uani 1 1 d DU . .
N2 N 0.1242(7) 1.0079(6) -0.2300(3) 0.138(6) Uani 1 1 d G . .
C22 C 0.2133(7) 0.9285(6) -0.2466(3) 0.136(3) Uani 1 1 d GU . .
H22 H 0.2606 0.8930 -0.2084 0.163 Uiso 1 1 calc R . .
C23 C 0.2316(7) 0.9022(6) -0.3203(4) 0.137(3) Uani 1 1 d GU . .
H23 H 0.2912 0.8491 -0.3314 0.165 Uiso 1 1 calc R . .
C24 C 0.1609(8) 0.9554(7) -0.3773(3) 0.139(3) Uani 1 1 d GDU . .
C25 C 0.0718(7) 1.0348(7) -0.3607(3) 0.139(3) Uani 1 1 d GU . .
H25 H 0.0245 1.0703 -0.3989 0.167 Uiso 1 1 calc R . .
C26 C 0.0535(7) 1.0611(6) -0.2870(4) 0.134(3) Uani 1 1 d GU . .
H26 H -0.0061 1.1142 -0.2759 0.161 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C30 1.186(12) . ?
O2 C33 1.256(16) . ?
O3 C36 1.204(10) . ?
O4 C42 1.250(11) . ?
O5 C45 1.274(15) . ?
O6 C38 1.236(15) . ?
N68 C38 1.349(15) . ?
N68 C39 1.436(18) . ?
N68 C41 1.477(12) . ?
O8 C48 1.278(18) . ?
N66 C42 1.342(17) . ?
N66 C47 1.432(15) . ?
N66 C44 1.453(9) . ?
O10 C58 1.217(11) . ?
O11 C55 1.158(12) . ?
N69 C38 1.393(13) . ?
N69 C37 1.399(17) . ?
N69 C35 1.463(14) . ?
O7 C64 1.243(13) . ?
N70 C36 1.336(11) . ?
N70 C40 1.459(11) . ?
N70 C39 1.460(9) . ?
N64 C44 1.373(16) . ?
N64 C46 1.437(17) . ?
N64 C45 1.448(12) . ?
N75 C30 1.426(18) . ?
N75 C46 1.436(15) 2_564 ?
N75 C31 1.468(9) . ?
O12 C61 1.288(15) . ?
N67 C42 1.386(13) . ?
N67 C40 1.441(18) . ?
N67 C43 1.444(12) . ?
N53 C64 1.432(12) 2_575 ?
N53 C49 1.444(13) . ?
N53 C51 1.518(11) . ?
N56 C56 1.415(15) . ?
N56 C59 1.447(12) . ?
N56 C58 1.454(17) . ?
N73 C47 1.363(19) 2_564 ?
N73 C31 1.424(18) . ?
N73 C33 1.513(17) . ?
N51 C48 1.324(16) . ?
N51 C50 1.437(11) . ?
N51 C49 1.47(2) . ?
N72 C33 1.14(2) . ?
N72 C35 1.457(18) . ?
N72 C32 1.458(15) . ?
N59 C48 1.386(13) 2_575 ?
N59 C63 1.425(12) . ?
N59 C65 1.454(19) . ?
N57 C62 1.272(18) . ?
N57 C58 1.376(15) . ?
N57 C60 1.432(12) . ?
O9 C52 1.283(18) . ?
N61 C57 1.296(17) . ?
N61 C61 1.360(13) . ?
N61 C59 1.458(15) . ?
N65 C45 1.339(19) . ?
N65 C41 1.391(14) . ?
N65 C43 1.411(12) . ?
O60 C21 1.309(18) . ?
N60 C61 1.385(19) . ?
N60 C63 1.422(15) . ?
N60 C60 1.453(12) . ?
N54 C52 1.302(19) . ?
N54 C53 1.395(13) . ?
N54 C50 1.513(15) . ?
C37 N71 1.433(10) . ?
C37 C39 1.572(13) . ?
N62 C54 1.413(13) . ?
N62 C57 1.434(16) . ?
N62 C55 1.563(17) . ?
N48 O18 1.01(3) . ?
N48 O20 1.25(2) . ?
N48 O19 1.41(2) . ?
C21 O59 1.19(2) . ?
C21 C15 1.516(14) . ?
N55 C52 1.384(13) . ?
N55 C56 1.409(18) . ?
N55 C54 1.506(19) . ?
N63 C55 1.347(15) . ?
N63 C51 1.417(18) . ?
N63 C53 1.495(14) . ?
N74 C30 1.298(16) . ?
N74 C32 1.424(12) . ?
N74 C34 1.51(2) . ?
N58 C64 1.321(12) . ?
N58 C65 1.443(13) . ?
N58 C62 1.484(11) . ?
N71 C36 1.382(12) . ?
N71 C34 1.488(12) . ?
C29 C28 1.544(15) . ?
C29 C29 1.65(3) 2_575 ?
C49 C65 1.584(12) 2_575 ?
C31 C32 1.53(2) . ?
C44 C43 1.521(19) . ?
C46 N75 1.436(15) 2_564 ?
C60 C59 1.500(19) . ?
C19 C20 1.494(14) . ?
C19 C18 1.520(17) . ?
C53 C54 1.431(18) . ?
C47 N73 1.363(19) 2_564 ?
C48 N59 1.386(13) 2_575 ?
C18 N1 1.441(11) . ?
N1 C13 1.3900 . ?
N1 C17 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C20 C20 1.66(3) 2_564 ?
C65 C49 1.584(12) 2_575 ?
O13 C66 1.41(2) . ?
C64 N53 1.432(12) 2_575 ?
C27 N2 1.490(13) . ?
C27 C28 1.62(3) . ?
O19 O18 1.68(4) . ?
N47 O15 1.09(2) . ?
N47 O16 1.25(3) . ?
N47 O17 1.25(5) . ?
O14 C66 1.078(19) . ?
C66 C24 1.594(13) . ?
N2 C22 1.3900 . ?
N2 C26 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?

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
C38 N68 C39 114.2(8) . . ?
C38 N68 C41 121.4(10) . . ?
C39 N68 C41 123.6(10) . . ?
C42 N66 C47 121.2(7) . . ?
C42 N66 C44 111.7(9) . . ?
C47 N66 C44 127.0(10) . . ?
C38 N69 C37 111.7(9) . . ?
C38 N69 C35 120.4(11) . . ?
C37 N69 C35 127.8(9) . . ?
C36 N70 C40 121.1(7) . . ?
C36 N70 C39 115.0(8) . . ?
C40 N70 C39 121.7(7) . . ?
C44 N64 C46 122.6(8) . . ?
C44 N64 C45 107.4(11) . . ?
C46 N64 C45 122.1(9) . . ?
C30 N75 C46 122.1(7) . 2_564 ?
C30 N75 C31 113.4(10) . . ?
C46 N75 C31 124.4(11) 2_564 . ?
C42 N67 C40 123.6(9) . . ?
C42 N67 C43 109.3(9) . . ?
C40 N67 C43 122.9(9) . . ?
C64 N53 C49 113.7(7) 2_575 . ?
C64 N53 C51 122.6(8) 2_575 . ?
C49 N53 C51 122.5(9) . . ?
C56 N56 C59 129.1(9) . . ?
C56 N56 C58 120.7(8) . . ?
C59 N56 C58 107.7(10) . . ?
C47 N73 C31 122.8(9) 2_564 . ?
C47 N73 C33 125.4(10) 2_564 . ?
C31 N73 C33 107.5(13) . . ?
C48 N51 C50 126.8(11) . . ?
C48 N51 C49 110.6(9) . . ?
C50 N51 C49 118.8(13) . . ?
C33 N72 C35 116.9(12) . . ?
C33 N72 C32 118.8(15) . . ?
C35 N72 C32 121.2(17) . . ?
C48 N59 C63 123.2(11) 2_575 . ?
C48 N59 C65 110.9(9) 2_575 . ?
C63 N59 C65 125.6(9) . . ?
C62 N57 C58 119.9(9) . . ?
C62 N57 C60 128.9(10) . . ?
C58 N57 C60 111.2(10) . . ?
C57 N61 C61 128.3(11) . . ?
C57 N61 C59 122.2(8) . . ?
C61 N61 C59 107.8(10) . . ?
C45 N65 C41 121.2(9) . . ?
C45 N65 C43 108.1(10) . . ?
C41 N65 C43 128.5(14) . . ?
C61 N60 C63 121.0(10) . . ?
C61 N60 C60 106.9(10) . . ?
C63 N60 C60 128.2(14) . . ?
C52 N54 C53 107.5(10) . . ?
C52 N54 C50 122.3(10) . . ?
C53 N54 C50 126.9(14) . . ?
N69 C37 N71 121.2(11) . . ?
N69 C37 C39 105.2(9) . . ?
N71 C37 C39 103.7(6) . . ?
C54 N62 C57 129.6(9) . . ?
C54 N62 C55 105.5(10) . . ?
C57 N62 C55 121.8(8) . . ?
O18 N48 O20 151(3) . . ?
O18 N48 O19 86(2) . . ?
O20 N48 O19 110.6(16) . . ?
O59 C21 O60 128.0(12) . . ?
O59 C21 C15 121.4(11) . . ?
O60 C21 C15 110.4(14) . . ?
C52 N55 C56 127.2(12) . . ?
C52 N55 C54 105.9(13) . . ?
C56 N55 C54 125.3(7) . . ?
C55 N63 C51 120.8(10) . . ?
C55 N63 C53 110.9(11) . . ?
C51 N63 C53 128.2(10) . . ?
C30 N74 C32 118.6(13) . . ?
C30 N74 C34 119.4(10) . . ?
C32 N74 C34 120.6(11) . . ?
C64 N58 C65 114.6(8) . . ?
C64 N58 C62 120.5(8) . . ?
C65 N58 C62 123.3(7) . . ?
C36 N71 C37 112.9(7) . . ?
C36 N71 C34 122.5(7) . . ?
C37 N71 C34 123.8(7) . . ?
C28 C29 C29 107.4(17) . 2_575 ?
N72 C33 O2 138.1(15) . . ?
N72 C33 N73 107.7(12) . . ?
O2 C33 N73 114.1(16) . . ?
N53 C49 N51 114.9(13) . . ?
N53 C49 C65 100.7(8) . 2_575 ?
N51 C49 C65 103.7(10) . 2_575 ?
O6 C38 N68 128.1(9) . . ?
O6 C38 N69 124.2(9) . . ?
N68 C38 N69 107.7(11) . . ?
O5 C45 N65 131.8(10) . . ?
O5 C45 N64 117.6(14) . . ?
N65 C45 N64 110.2(10) . . ?
O4 C42 N66 128.7(11) . . ?
O4 C42 N67 121.5(12) . . ?
N66 C42 N67 109.8(8) . . ?
N65 C41 N68 113.1(7) . . ?
O1 C30 N74 132.2(16) . . ?
O1 C30 N75 124.3(13) . . ?
N74 C30 N75 103.5(9) . . ?
N68 C39 N70 113.9(10) . . ?
N68 C39 C37 100.9(9) . . ?
N70 C39 C37 100.1(6) . . ?
N73 C31 N75 115.1(10) . . ?
N73 C31 C32 103.4(9) . . ?
N75 C31 C32 101.2(10) . . ?
N64 C44 N66 116.2(10) . . ?
N64 C44 C43 105.0(7) . . ?
N66 C44 C43 103.1(9) . . ?
N75 C46 N64 112.1(8) 2_564 . ?
N55 C56 N56 109.0(8) . . ?
N57 C60 N60 112.8(7) . . ?
N57 C60 C59 105.8(9) . . ?
N60 C60 C59 106.0(12) . . ?
N72 C35 N69 115.8(7) . . ?
N56 C59 N61 111.1(10) . . ?
N56 C59 C60 106.4(9) . . ?
N61 C59 C60 105.4(7) . . ?
C20 C19 C18 110.8(9) . . ?
N54 C53 C54 110.9(13) . . ?
N54 C53 N63 117.1(7) . . ?
C54 C53 N63 105.7(8) . . ?
N65 C43 N67 112.5(8) . . ?
N65 C43 C44 106.6(13) . . ?
N67 C43 C44 104.9(8) . . ?
N62 C54 C53 109.5(9) . . ?
N62 C54 N55 109.1(11) . . ?
C53 C54 N55 101.4(8) . . ?
N67 C40 N70 113.7(12) . . ?
N61 C57 N62 112.0(8) . . ?
N74 C32 N72 115.8(8) . . ?
N74 C32 C31 103.0(9) . . ?
N72 C32 C31 101.5(13) . . ?
O3 C36 N70 127.5(9) . . ?
O3 C36 N71 124.5(9) . . ?
N70 C36 N71 106.4(7) . . ?
N60 C63 N59 115.2(8) . . ?
O10 C58 N57 125.8(13) . . ?
O10 C58 N56 125.6(12) . . ?
N57 C58 N56 108.6(8) . . ?
N73 C47 N66 114.2(8) 2_564 . ?
O9 C52 N54 127.0(11) . . ?
O9 C52 N55 119.8(16) . . ?
N54 C52 N55 112.4(12) . . ?
O8 C48 N51 125.0(10) . . ?
O8 C48 N59 122.8(10) . 2_575 ?
N51 C48 N59 111.4(12) . 2_575 ?
N51 C50 N54 110.8(9) . . ?
N1 C18 C19 112.9(9) . . ?
C13 N1 C17 120.0 . . ?
C13 N1 C18 118.9(9) . . ?
C17 N1 C18 121.1(9) . . ?
C14 C13 N1 120.0 . . ?
C13 C14 C15 120.0 . . ?
C14 C15 C16 120.0 . . ?
C14 C15 C21 115.8(9) . . ?
C16 C15 C21 124.2(9) . . ?
C17 C16 C15 120.0 . . ?
C16 C17 N1 120.0 . . ?
C19 C20 C20 111.7(12) . 2_564 ?
N63 C51 N53 112.1(12) . . ?
N58 C65 N59 115.2(14) . . ?
N58 C65 C49 104.1(7) . 2_575 ?
N59 C65 C49 102.0(9) . 2_575 ?
O7 C64 N58 129.5(9) . . ?
O7 C64 N53 121.8(9) . 2_575 ?
N58 C64 N53 106.4(8) . 2_575 ?
N71 C34 N74 114.3(12) . . ?
N2 C27 C28 106.4(14) . . ?
O11 C55 N63 132.4(14) . . ?
O11 C55 N62 120.8(12) . . ?
N63 C55 N62 106.2(9) . . ?
O12 C61 N61 120.4(15) . . ?
O12 C61 N60 126.6(11) . . ?
N61 C61 N60 112.8(10) . . ?
N57 C62 N58 122.6(13) . . ?
N48 O19 O18 36.8(12) . . ?
C29 C28 C27 104.9(14) . . ?
O15 N47 O16 110(3) . . ?
O15 N47 O17 113(3) . . ?
O16 N47 O17 137(4) . . ?
N48 O18 O19 57(2) . . ?
O14 C66 O13 132.2(14) . . ?
O14 C66 C24 125.3(15) . . ?
O13 C66 C24 102.0(12) . . ?
C22 N2 C26 120.0 . . ?
C22 N2 C27 121.6(6) . . ?
C26 N2 C27 118.1(6) . . ?
C23 C22 N2 120.0 . . ?
C22 C23 C24 120.0 . . ?
C23 C24 C25 120.0 . . ?
C23 C24 C66 125.9(7) . . ?
C25 C24 C66 113.9(7) . . ?
C24 C25 C26 120.0 . . ?
C25 C26 N2 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        67.08
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         0.787
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.159

# SQUEEZE RESULTS
# 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 0.067 0.071 0.357 7 1 ' '
2 0.500 -0.500 1.000 458 205 ' '
3 0.933 0.929 0.643 7 1 ' '
_platon_squeeze_details          ?

# start Validation Reply Form
_vrf_RFACG01_C6BPCA@CB6-NO3      
;
PROBLEM: The value of the R factor is > 0.20
RESPONSE: We made several attempts to obtain better quality data for
this structure, but the R factor is still high due to poor crystal quality and weak diffraction of macromolecular structure. However, this structure was included for comparison with the other similar compound. We are confident the structural
characterization is valid.
;
_vrf_RFACR01_C6BPCA@CB6-NO3      
;
PROBLEM: The value of the weighted R factor is > 0.45
RESPONSE: See RFACG01_ALERT_3_A, from above.
;
_vrf_PLAT082_C6BPCA@CB6-NO3      
;
PROBLEM: High R1 Value .................................. 0.24 Report
RESPONSE: See RFACG01_ALERT_3_A, from above.
;
_vrf_PLAT084_C6BPCA@CB6-NO3      
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.64 Report
RESPONSE: See RFACG01_ALERT_3_A, from above.
;



####################################################################### 
# 
# 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_1
_audit_block_doi                 10.5517/cc14j2g6
_database_code_depnum_ccdc_archive 'CCDC 1058137'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C5CC04409J 2015
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2016-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        u1
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H56 N26 O22 S U'
_chemical_formula_weight         1691.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   15.4905(4)
_cell_length_b                   15.7934(5)
_cell_length_c                   16.7184(6)
_cell_angle_alpha                68.423(3)
_cell_angle_beta                 89.602(3)
_cell_angle_gamma                83.048(3)
_cell_volume                     3772.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1692
_exptl_absorpt_coefficient_mu    7.054
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27126
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         67.08
_reflns_number_total             13434
_reflns_number_gt                12397
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0602P)²+2.9708P] 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         13434
_refine_ls_number_parameters     937
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.1004
_refine_ls_wR_factor_gt          0.0985
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
U1 U 0.588971(8) 0.072197(9) 0.603096(9) 0.03173(6) Uani 1 1 d . . .
O3 O 0.4774(2) 0.1212(2) 0.4956(2) 0.0420(8) Uani 1 1 d . . .
O2 O 0.6582(2) 0.1366(2) 0.5267(3) 0.0478(8) Uani 1 1 d . . .
O21 O 0.3361(2) 0.6124(2) 0.1854(2) 0.0415(8) Uani 1 1 d . . .
O15 O 0.9802(2) 0.4278(2) 0.2504(2) 0.0480(8) Uani 1 1 d . . .
O17 O 0.7061(2) 0.6451(3) 0.3993(2) 0.0468(8) Uani 1 1 d . . .
O20 O 0.7759(2) 0.4874(3) 0.1180(2) 0.0530(10) Uani 1 1 d . . .
O18 O 0.8823(2) 0.4126(2) 0.7735(2) 0.0399(7) Uani 1 1 d . . .
O19 O 0.7338(2) 0.4489(2) 0.6022(2) 0.0428(8) Uani 1 1 d . . .
N2 N 0.8876(2) 0.5614(3) 0.2212(2) 0.0357(8) Uani 1 1 d . . .
O23 O 0.4493(2) 0.3730(2) 0.2921(2) 0.0470(8) Uani 1 1 d . . .
O6 O 0.5597(5) 0.3251(4) 0.5400(3) 0.108(2) Uani 1 1 d . . .
O22 O 0.6627(2) 0.3238(3) 0.2493(2) 0.0458(8) Uani 1 1 d . . .
O14 O 1.1498(2) 0.1989(2) 0.6234(2) 0.0453(8) Uani 1 1 d . . .
O25 O 0.5606(2) 0.2135(3) -0.0501(2) 0.0492(8) Uani 1 1 d . . .
N8 N 0.2622(2) 0.5159(3) 0.1428(2) 0.0342(8) Uani 1 1 d . . .
N9 N 0.8043(2) 0.3035(3) 0.6290(2) 0.0345(8) Uani 1 1 d . . .
N10 N 0.3294(3) 0.3601(3) 0.2188(3) 0.0410(9) Uani 1 1 d . . .
O16 O 0.9929(2) 0.2308(3) 0.4496(2) 0.0480(8) Uani 1 1 d . . .
N12 N 0.9077(2) 0.2792(3) 0.7462(2) 0.0353(8) Uani 1 1 d . . .
N13 N 0.4566(2) 0.4102(3) 0.7836(2) 0.0352(8) Uani 1 1 d . . .
N14 N 0.7925(3) 0.3762(3) 0.0587(2) 0.0424(9) Uani 1 1 d . . .
N15 N 0.8444(2) 0.4316(3) 0.3081(2) 0.0338(8) Uani 1 1 d . . .
N16 N 0.7519(2) 0.3874(3) 0.4968(2) 0.0359(8) Uani 1 1 d . . .
N17 N 0.8511(2) 0.2956(3) 0.4376(2) 0.0351(8) Uani 1 1 d . . .
O24 O 0.3388(3) 0.2882(3) -0.0174(2) 0.0552(9) Uani 1 1 d . . .
N19 N 0.9112(2) 0.2199(3) 0.5676(3) 0.0386(9) Uani 1 1 d . . .
N20 N 0.2851(3) 0.3250(3) 0.0955(3) 0.0413(9) Uani 1 1 d . . .
N21 N 1.0149(2) 0.1975(3) 0.6833(2) 0.0364(8) Uani 1 1 d . . .
N22 N 0.5925(3) 0.2202(3) 0.2150(3) 0.0400(9) Uani 1 1 d . . .
N23 N 1.0161(2) 0.3239(3) 0.8016(3) 0.0365(8) Uani 1 1 d . . .
N24 N 0.2469(3) 0.6652(3) 0.0628(2) 0.0386(9) Uani 1 1 d . . .
N25 N 0.7778(3) 0.6477(3) 0.2774(3) 0.0378(8) Uani 1 1 d . . .
N26 N 0.4040(3) 0.2258(3) 0.1184(3) 0.0430(9) Uani 1 1 d . . .
N27 N 0.2011(2) 0.3279(2) 0.4213(2) 0.0321(8) Uani 1 1 d . . .
N29 N 0.6767(3) 0.2155(3) 0.0347(3) 0.0415(9) Uani 1 1 d . . .
N33 N 1.1228(2) 0.2396(3) 0.7412(3) 0.0393(9) Uani 1 1 d . . .
C3 C 0.3331(3) 0.1872(3) 0.4537(3) 0.0292(9) Uani 1 1 d . . .
C4 C 0.3490(3) 0.2703(3) 0.4566(3) 0.0293(8) Uani 1 1 d . . .
H4 H 0.4047 0.2789 0.4697 0.035 Uiso 1 1 calc R . .
N30 N 0.4431(3) 0.2522(3) 0.2482(3) 0.0404(9) Uani 1 1 d . . .
N31 N 0.7183(3) 0.2562(3) 0.1555(3) 0.0429(9) Uani 1 1 d . . .
N28 N 0.5527(3) 0.1754(3) 0.0965(3) 0.0440(9) Uani 1 1 d . . .
N32 N 0.7321(2) 0.5183(3) 0.3619(2) 0.0365(8) Uani 1 1 d . . .
C10 C 0.4067(3) 0.1104(3) 0.4706(3) 0.0314(9) Uani 1 1 d . . .
C11 C 0.5293(3) 0.2071(3) 0.2806(3) 0.0418(11) Uani 1 1 d . . .
H11A H 0.5485 0.2299 0.3230 0.050 Uiso 1 1 calc R . .
H11B H 0.5266 0.1418 0.3094 0.050 Uiso 1 1 calc R . .
N34 N 0.2073(3) 0.4785(3) 0.0267(3) 0.0419(9) Uani 1 1 d . . .
C13 C 0.1288(3) 0.4052(3) 0.4019(3) 0.0390(11) Uani 1 1 d . . .
H13A H 0.0832 0.3957 0.3677 0.047 Uiso 1 1 calc R . .
H13B H 0.1505 0.4623 0.3680 0.047 Uiso 1 1 calc R . .
C14 C 0.8421(3) 0.3329(3) 0.3448(3) 0.0374(10) Uani 1 1 d . . .
H14A H 0.7873 0.3194 0.3274 0.045 Uiso 1 1 calc R . .
H14B H 0.8887 0.3029 0.3218 0.045 Uiso 1 1 calc R . .
C15 C 0.4286(3) 0.4590(4) 0.8431(3) 0.0412(11) Uani 1 1 d . . .
H15A H 0.3782 0.4339 0.8731 0.049 Uiso 1 1 calc R . .
H15B H 0.4111 0.5234 0.8092 0.049 Uiso 1 1 calc R . .
C16 C 1.0537(3) 0.2369(3) 0.7999(3) 0.0353(9) Uani 1 1 d . . .
H16 H 1.0712 0.1931 0.8580 0.042 Uiso 1 1 calc R . .
C18 C 0.6119(3) 0.1587(3) 0.1688(3) 0.0435(11) Uani 1 1 d . . .
H18 H 0.6182 0.0942 0.2079 0.052 Uiso 1 1 calc R . .
C19 C 0.0909(3) 0.4132(3) 0.4825(3) 0.0354(10) Uani 1 1 d . . .
H19A H 0.1366 0.4207 0.5178 0.042 Uiso 1 1 calc R . .
H19B H 0.0669 0.3573 0.5154 0.042 Uiso 1 1 calc R . .
C20 C 0.9109(3) 0.4692(3) 0.2591(3) 0.0346(9) Uani 1 1 d . . .
C21 C 0.7964(3) 0.5874(3) 0.2306(3) 0.0323(9) Uani 1 1 d . . .
H21 H 0.7644 0.6118 0.1747 0.039 Uiso 1 1 calc R . .
C22 C 0.2502(3) 0.1767(3) 0.4334(4) 0.0469(12) Uani 1 1 d . . .
H22 H 0.2389 0.1219 0.4294 0.056 Uiso 1 1 calc R . .
C23 C 0.8203(3) 0.2410(3) 0.5845(3) 0.0321(9) Uani 1 1 d . . .
H23 H 0.7929 0.1852 0.6122 0.039 Uiso 1 1 calc R . .
C24 C 0.9299(3) 0.3464(3) 0.7731(3) 0.0316(9) Uani 1 1 d . . .
C25 C 0.1840(3) 0.6289(3) 0.0236(3) 0.0385(10) Uani 1 1 d . . .
H25 H 0.1251 0.6608 0.0207 0.046 Uiso 1 1 calc R . .
C26 C 0.9734(3) 0.1560(3) 0.6326(3) 0.0400(10) Uani 1 1 d . . .
H26A H 0.9438 0.1067 0.6706 0.048 Uiso 1 1 calc R . .
H26B H 1.0178 0.1293 0.6046 0.048 Uiso 1 1 calc R . .
C27 C 0.4650(3) 0.1550(4) 0.1042(4) 0.0461(12) Uani 1 1 d . . .
H27A H 0.4629 0.0972 0.1519 0.055 Uiso 1 1 calc R . .
H27B H 0.4467 0.1474 0.0522 0.055 Uiso 1 1 calc R . .
C28 C 0.3004(3) 0.2932(3) 0.1876(3) 0.0400(11) Uani 1 1 d . . .
H28 H 0.2505 0.2664 0.2187 0.048 Uiso 1 1 calc R . .
C29 C 0.1903(3) 0.5269(3) 0.0839(3) 0.0354(10) Uani 1 1 d . . .
H29 H 0.1363 0.5128 0.1141 0.043 Uiso 1 1 calc R . .
C30 C 0.5039(3) 0.3245(3) 0.6713(3) 0.0352(10) Uani 1 1 d . . .
C31 C 0.2812(3) 0.3398(3) 0.4398(3) 0.0322(9) Uani 1 1 d . . .
H31 H 0.2914 0.3961 0.4412 0.039 Uiso 1 1 calc R . .
C32 C 0.7792(3) 0.2984(3) 0.4933(3) 0.0316(9) Uani 1 1 d . . .
H32 H 0.7300 0.2715 0.4801 0.038 Uiso 1 1 calc R . .
C33 C 0.7850(3) 0.4648(4) 0.0561(3) 0.0410(11) Uani 1 1 d . . .
C34 C 0.9254(3) 0.2480(3) 0.4815(3) 0.0342(9) Uani 1 1 d . . .
C35 C 0.5303(4) 0.2800(4) 0.6070(4) 0.0494(13) Uani 1 1 d . . .
C36 C 0.7605(3) 0.3869(3) 0.5783(3) 0.0316(9) Uani 1 1 d . . .
C37 C 0.3812(3) 0.2211(3) 0.2044(3) 0.0404(11) Uani 1 1 d . . .
H37 H 0.3677 0.1597 0.2402 0.049 Uiso 1 1 calc R . .
C38 C 0.2870(3) 0.6001(3) 0.1353(3) 0.0335(9) Uani 1 1 d . . .
C39 C 0.4656(3) 0.2789(3) 0.7472(3) 0.0417(11) Uani 1 1 d . . .
H39 H 0.4555 0.2184 0.7606 0.050 Uiso 1 1 calc R . .
C40 C 0.5934(3) 0.2031(3) 0.0196(3) 0.0408(11) Uani 1 1 d . . .
C41 C 0.4421(3) 0.3227(3) 0.8032(3) 0.0425(11) Uani 1 1 d . . .
H41 H 0.4162 0.2919 0.8543 0.051 Uiso 1 1 calc R . .
C42 C 0.9782(3) 0.2054(3) 0.7605(3) 0.0348(9) Uani 1 1 d . . .
H42 H 0.9622 0.1467 0.7999 0.042 Uiso 1 1 calc R . .
C43 C 1.1008(3) 0.2110(3) 0.6763(3) 0.0359(10) Uani 1 1 d . . .
C44 C 0.8191(3) 0.2767(3) 0.7205(3) 0.0363(10) Uani 1 1 d . . .
H44A H 0.8045 0.2149 0.7489 0.044 Uiso 1 1 calc R . .
H44B H 0.7801 0.3171 0.7403 0.044 Uiso 1 1 calc R . .
C45 C 0.7364(3) 0.6077(3) 0.3521(3) 0.0353(10) Uani 1 1 d . . .
C46 C 0.6901(3) 0.4555(4) 0.4328(3) 0.0414(11) Uani 1 1 d . . .
H46A H 0.6522 0.4240 0.4105 0.050 Uiso 1 1 calc R . .
H46B H 0.6540 0.4903 0.4607 0.050 Uiso 1 1 calc R . .
C47 C 0.4661(3) 0.5023(4) 0.9667(3) 0.0405(11) Uani 1 1 d . . .
H47A H 0.4477 0.5661 0.9315 0.049 Uiso 1 1 calc R . .
H47B H 0.4157 0.4764 0.9960 0.049 Uiso 1 1 calc R . .
C48 C 0.7654(3) 0.4965(3) 0.2901(3) 0.0332(9) Uani 1 1 d . . .
H48 H 0.7201 0.4784 0.2613 0.040 Uiso 1 1 calc R . .
C49 C 0.3427(3) 0.2808(3) 0.0575(3) 0.0403(11) Uani 1 1 d . . .
C50 C 0.2050(3) 0.3811(4) 0.0517(4) 0.0462(12) Uani 1 1 d . . .
H50A H 0.1937 0.3680 0.0007 0.055 Uiso 1 1 calc R . .
H50B H 0.1570 0.3637 0.0894 0.055 Uiso 1 1 calc R . .
C51 C 0.0199(3) 0.4946(3) 0.4607(3) 0.0383(10) Uani 1 1 d . . .
H51A H 0.0443 0.5501 0.4275 0.046 Uiso 1 1 calc R . .
H51B H -0.0254 0.4868 0.4252 0.046 Uiso 1 1 calc R . .
C52 C 0.4114(3) 0.3340(3) 0.2555(3) 0.0370(10) Uani 1 1 d . . .
C53 C 0.2738(3) 0.4388(3) 0.2235(3) 0.0407(11) Uani 1 1 d . . .
H53A H 0.2173 0.4205 0.2425 0.049 Uiso 1 1 calc R . .
H53B H 0.2987 0.4577 0.2663 0.049 Uiso 1 1 calc R . .
C54 C 1.0583(3) 0.3784(3) 0.8378(3) 0.0377(10) Uani 1 1 d . . .
H54A H 1.0937 0.3378 0.8879 0.045 Uiso 1 1 calc R . .
H54B H 1.0142 0.4151 0.8570 0.045 Uiso 1 1 calc R . .
C55 C 0.1843(3) 0.2476(4) 0.4190(4) 0.0480(13) Uani 1 1 d . . .
H55 H 0.1277 0.2399 0.4075 0.058 Uiso 1 1 calc R . .
C56 C 0.4946(3) 0.4546(4) 0.7113(3) 0.0446(12) Uani 1 1 d . . .
H56 H 0.5056 0.5145 0.6997 0.054 Uiso 1 1 calc R . .
C57 C 0.4984(3) 0.4514(3) 0.9088(3) 0.0362(10) Uani 1 1 d . . .
H57A H 0.5490 0.4768 0.8794 0.043 Uiso 1 1 calc R . .
H57B H 0.5159 0.3872 0.9435 0.043 Uiso 1 1 calc R . .
C58 C 0.6986(3) 0.1858(3) 0.1256(3) 0.0407(11) Uani 1 1 d . . .
H58 H 0.7446 0.1333 0.1439 0.049 Uiso 1 1 calc R . .
C59 C 0.5178(3) 0.4138(4) 0.6540(3) 0.0428(11) Uani 1 1 d . . .
H59 H 0.5430 0.4464 0.6031 0.051 Uiso 1 1 calc R . .
C60 C 1.2100(3) 0.2564(3) 0.7558(3) 0.0412(11) Uani 1 1 d . . .
H60A H 1.2240 0.2311 0.8172 0.049 Uiso 1 1 calc R . .
H60B H 1.2507 0.2241 0.7291 0.049 Uiso 1 1 calc R . .
C61 C 0.6580(3) 0.2729(3) 0.2106(3) 0.0380(10) Uani 1 1 d . . .
C62 C 0.2612(3) 0.7593(3) 0.0328(3) 0.0427(11) Uani 1 1 d . . .
H62A H 0.2815 0.7726 0.0811 0.051 Uiso 1 1 calc R . .
H62B H 0.2060 0.7974 0.0115 0.051 Uiso 1 1 calc R . .
C65 C 0.7972(3) 0.2985(4) 0.1382(3) 0.0463(12) Uani 1 1 d . . .
H65A H 0.8102 0.3178 0.1850 0.056 Uiso 1 1 calc R . .
H65B H 0.8447 0.2532 0.1366 0.056 Uiso 1 1 calc R . .
O5 O 0.5182(3) 0.1959(2) 0.6300(3) 0.0518(9) Uani 1 1 d . . .
O7 O 0.6714(3) 0.0860(3) 0.7208(3) 0.0758(13) Uani 1 1 d . . .
S1 S 0.73519(11) -0.00076(12) 0.74548(11) 0.0722(5) Uani 1 1 d . . .
O8 O 0.7130(3) -0.0376(3) 0.6788(3) 0.0601(10) Uani 1 1 d . . .
O9 O 0.8228(3) 0.0220(4) 0.7396(4) 0.0993(19) Uani 1 1 d . . .
O10 O 0.7198(5) -0.0637(5) 0.8301(4) 0.119(2) Uani 1 1 d . . .
O1 O 0.5194(2) 0.0051(2) 0.6777(3) 0.0536(9) Uani 1 1 d . . .
O4 O 0.3898(2) 0.0415(2) 0.4583(3) 0.0598(11) 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
U1 O2 1.763(4) . ?
U1 O1 1.767(3) . ?
U1 O5 2.311(3) . ?
U1 O3 2.348(3) . ?
U1 O4 2.365(3) 2_656 ?
U1 O8 2.432(4) . ?
U1 O7 2.444(4) . ?
U1 S1 3.0903(15) . ?
O3 C10 1.228(5) . ?
O21 C38 1.218(5) . ?
O15 C20 1.225(5) . ?
O17 C45 1.210(5) . ?
O20 C33 1.216(5) . ?
O18 C24 1.206(5) . ?
O19 C36 1.216(5) . ?
N2 C20 1.360(6) . ?
N2 C54 1.440(6) 2_766 ?
N2 C21 1.446(5) . ?
O23 C52 1.211(6) . ?
O6 C35 1.206(7) . ?
O22 C61 1.210(6) . ?
O14 C43 1.214(5) . ?
O25 C40 1.221(6) . ?
N8 C38 1.389(6) . ?
N8 C53 1.441(6) . ?
N8 C29 1.443(6) . ?
N9 C36 1.373(6) . ?
N9 C23 1.437(5) . ?
N9 C44 1.441(6) . ?
N10 C52 1.363(6) . ?
N10 C53 1.451(6) . ?
N10 C28 1.454(6) . ?
O16 C34 1.218(5) . ?
N12 C24 1.374(6) . ?
N12 C42 1.448(5) . ?
N12 C44 1.450(6) . ?
N13 C56 1.328(6) . ?
N13 C41 1.345(6) . ?
N13 C15 1.500(5) . ?
N14 C33 1.374(7) . ?
N14 C65 1.435(7) . ?
N14 C25 1.449(5) 2_665 ?
N15 C20 1.366(6) . ?
N15 C48 1.454(5) . ?
N15 C14 1.455(6) . ?
N16 C36 1.367(6) . ?
N16 C32 1.439(6) . ?
N16 C46 1.462(6) . ?
N17 C34 1.352(6) . ?
N17 C14 1.444(6) . ?
N17 C32 1.453(5) . ?
O24 C49 1.215(6) . ?
N19 C34 1.366(6) . ?
N19 C26 1.448(6) . ?
N19 C23 1.457(5) . ?
N20 C49 1.363(6) . ?
N20 C28 1.444(6) . ?
N20 C50 1.460(7) . ?
N21 C43 1.370(6) . ?
N21 C26 1.443(6) . ?
N21 C42 1.447(6) . ?
N22 C61 1.373(6) . ?
N22 C11 1.439(6) . ?
N22 C18 1.453(6) . ?
N23 C24 1.381(6) . ?
N23 C54 1.435(6) . ?
N23 C16 1.436(6) . ?
N24 C38 1.361(6) . ?
N24 C62 1.428(6) . ?
N24 C25 1.460(6) . ?
N25 C45 1.370(6) . ?
N25 C21 1.443(5) . ?
N25 C60 1.444(6) 2_766 ?
N26 C49 1.362(7) . ?
N26 C37 1.456(6) . ?
N26 C27 1.460(6) . ?
N27 C31 1.332(6) . ?
N27 C55 1.339(6) . ?
N27 C13 1.494(5) . ?
N29 C40 1.367(6) . ?
N29 C58 1.445(6) . ?
N29 C62 1.452(6) 2_665 ?
N33 C43 1.379(6) . ?
N33 C16 1.441(6) . ?
N33 C60 1.448(6) . ?
C3 C22 1.375(6) . ?
C3 C4 1.381(6) . ?
C3 C10 1.507(5) . ?
C4 C31 1.373(6) . ?
N30 C52 1.374(6) . ?
N30 C11 1.442(6) . ?
N30 C37 1.443(6) . ?
N31 C61 1.378(6) . ?
N31 C65 1.439(6) . ?
N31 C58 1.440(6) . ?
N28 C40 1.371(6) . ?
N28 C27 1.427(6) . ?
N28 C18 1.448(7) . ?
N32 C45 1.370(6) . ?
N32 C48 1.442(5) . ?
N32 C46 1.447(6) . ?
C10 O4 1.236(5) . ?
N34 C33 1.357(7) 2_665 ?
N34 C29 1.434(5) . ?
N34 C50 1.443(7) . ?
C13 C19 1.508(6) . ?
C15 C57 1.509(6) . ?
C16 C42 1.563(6) . ?
C18 C58 1.552(7) . ?
C19 C51 1.520(5) . ?
C21 C48 1.546(6) . ?
C22 C55 1.372(7) . ?
C23 C32 1.553(6) . ?
C25 N14 1.449(5) 2_665 ?
C25 C29 1.545(7) . ?
C28 C37 1.539(7) . ?
C30 C59 1.375(7) . ?
C30 C39 1.379(7) . ?
C30 C35 1.516(6) . ?
C33 N34 1.357(7) 2_665 ?
C35 O5 1.277(6) . ?
C39 C41 1.378(6) . ?
C47 C47 1.511(8) 2_667 ?
C47 C57 1.519(6) . ?
C51 C51 1.504(8) 2_566 ?
C54 N2 1.440(6) 2_766 ?
C56 C59 1.362(6) . ?
C60 N25 1.444(6) 2_766 ?
C62 N29 1.452(6) 2_665 ?
O7 S1 1.512(5) . ?
S1 O10 1.437(6) . ?
S1 O9 1.439(5) . ?
S1 O8 1.492(5) . ?
O4 U1 2.365(3) 2_656 ?

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
O2 U1 O1 178.00(16) . . ?
O2 U1 O5 95.36(15) . . ?
O1 U1 O5 86.31(16) . . ?
O2 U1 O3 88.87(15) . . ?
O1 U1 O3 90.32(16) . . ?
O5 U1 O3 80.10(13) . . ?
O2 U1 O4 88.70(16) . 2_656 ?
O1 U1 O4 89.33(17) . 2_656 ?
O5 U1 O4 157.23(14) . 2_656 ?
O3 U1 O4 77.58(12) . 2_656 ?
O2 U1 O8 90.36(16) . . ?
O1 U1 O8 89.41(16) . . ?
O5 U1 O8 130.09(14) . . ?
O3 U1 O8 149.69(13) . . ?
O4 U1 O8 72.11(14) 2_656 . ?
O2 U1 O7 91.34(17) . . ?
O1 U1 O7 90.20(18) . . ?
O5 U1 O7 73.28(16) . . ?
O3 U1 O7 153.29(15) . . ?
O4 U1 O7 129.13(15) 2_656 . ?
O8 U1 O7 57.02(16) . . ?
O2 U1 S1 92.37(13) . . ?
O1 U1 S1 88.37(14) . . ?
O5 U1 S1 101.85(11) . . ?
O3 U1 S1 177.57(8) . . ?
O4 U1 S1 100.35(10) 2_656 . ?
O8 U1 S1 28.27(11) . . ?
O7 U1 S1 28.81(12) . . ?
C10 O3 U1 148.6(3) . . ?
C20 N2 C54 122.8(4) . 2_766 ?
C20 N2 C21 112.0(4) . . ?
C54 N2 C21 123.7(4) 2_766 . ?
C38 N8 C53 120.9(4) . . ?
C38 N8 C29 111.5(4) . . ?
C53 N8 C29 120.6(4) . . ?
C36 N9 C23 112.9(4) . . ?
C36 N9 C44 122.9(4) . . ?
C23 N9 C44 123.4(4) . . ?
C52 N10 C53 122.4(4) . . ?
C52 N10 C28 112.6(4) . . ?
C53 N10 C28 124.3(4) . . ?
C24 N12 C42 112.4(4) . . ?
C24 N12 C44 122.3(4) . . ?
C42 N12 C44 124.5(4) . . ?
C56 N13 C41 120.7(4) . . ?
C56 N13 C15 119.4(4) . . ?
C41 N13 C15 119.9(4) . . ?
C33 N14 C65 122.3(4) . . ?
C33 N14 C25 111.7(4) . 2_665 ?
C65 N14 C25 124.3(4) . 2_665 ?
C20 N15 C48 111.7(4) . . ?
C20 N15 C14 122.0(4) . . ?
C48 N15 C14 121.8(4) . . ?
C36 N16 C32 112.0(4) . . ?
C36 N16 C46 121.4(4) . . ?
C32 N16 C46 121.8(4) . . ?
C34 N17 C14 123.4(4) . . ?
C34 N17 C32 113.1(4) . . ?
C14 N17 C32 123.4(4) . . ?
C34 N19 C26 122.7(4) . . ?
C34 N19 C23 112.1(4) . . ?
C26 N19 C23 123.2(4) . . ?
C49 N20 C28 112.7(4) . . ?
C49 N20 C50 122.8(4) . . ?
C28 N20 C50 122.9(4) . . ?
C43 N21 C26 122.6(4) . . ?
C43 N21 C42 112.8(4) . . ?
C26 N21 C42 122.6(4) . . ?
C61 N22 C11 121.1(4) . . ?
C61 N22 C18 112.2(4) . . ?
C11 N22 C18 123.5(4) . . ?
C24 N23 C54 121.8(4) . . ?
C24 N23 C16 112.8(4) . . ?
C54 N23 C16 124.9(4) . . ?
C38 N24 C62 123.2(4) . . ?
C38 N24 C25 112.2(4) . . ?
C62 N24 C25 124.5(4) . . ?
C45 N25 C21 112.5(4) . . ?
C45 N25 C60 122.9(4) . 2_766 ?
C21 N25 C60 124.0(4) . 2_766 ?
C49 N26 C37 112.0(4) . . ?
C49 N26 C27 122.3(4) . . ?
C37 N26 C27 122.0(4) . . ?
C31 N27 C55 121.0(4) . . ?
C31 N27 C13 119.9(4) . . ?
C55 N27 C13 119.2(4) . . ?
C40 N29 C58 112.2(4) . . ?
C40 N29 C62 122.6(4) . 2_665 ?
C58 N29 C62 124.5(4) . 2_665 ?
C43 N33 C16 112.5(4) . . ?
C43 N33 C60 122.9(4) . . ?
C16 N33 C60 123.9(4) . . ?
C22 C3 C4 119.2(4) . . ?
C22 C3 C10 120.9(4) . . ?
C4 C3 C10 119.9(4) . . ?
C31 C4 C3 118.9(4) . . ?
C52 N30 C11 121.4(4) . . ?
C52 N30 C37 112.0(4) . . ?
C11 N30 C37 126.5(4) . . ?
C61 N31 C65 122.3(4) . . ?
C61 N31 C58 113.1(4) . . ?
C65 N31 C58 124.3(4) . . ?
C40 N28 C27 123.3(4) . . ?
C40 N28 C18 112.1(4) . . ?
C27 N28 C18 124.2(4) . . ?
C45 N32 C48 113.0(4) . . ?
C45 N32 C46 123.0(4) . . ?
C48 N32 C46 123.7(4) . . ?
O3 C10 O4 126.0(4) . . ?
O3 C10 C3 117.6(4) . . ?
O4 C10 C3 116.4(4) . . ?
N22 C11 N30 113.8(4) . . ?
C33 N34 C29 112.9(4) 2_665 . ?
C33 N34 C50 123.0(4) 2_665 . ?
C29 N34 C50 123.6(4) . . ?
N27 C13 C19 112.2(4) . . ?
N17 C14 N15 112.9(3) . . ?
N13 C15 C57 113.7(4) . . ?
N23 C16 N33 116.0(4) . . ?
N23 C16 C42 103.3(3) . . ?
N33 C16 C42 103.5(3) . . ?
N28 C18 N22 114.8(4) . . ?
N28 C18 C58 103.3(4) . . ?
N22 C18 C58 103.6(4) . . ?
C13 C19 C51 110.9(4) . . ?
O15 C20 N2 125.2(4) . . ?
O15 C20 N15 126.3(5) . . ?
N2 C20 N15 108.4(4) . . ?
N25 C21 N2 115.8(4) . . ?
N25 C21 C48 103.6(3) . . ?
N2 C21 C48 103.5(3) . . ?
C55 C22 C3 119.6(4) . . ?
N9 C23 N19 115.3(4) . . ?
N9 C23 C32 102.7(3) . . ?
N19 C23 C32 103.0(3) . . ?
O18 C24 N12 126.4(4) . . ?
O18 C24 N23 125.7(4) . . ?
N12 C24 N23 108.0(4) . . ?
N14 C25 N24 115.0(4) 2_665 . ?
N14 C25 C29 103.1(4) 2_665 . ?
N24 C25 C29 103.3(4) . . ?
N21 C26 N19 113.5(4) . . ?
N28 C27 N26 113.5(4) . . ?
N20 C28 N10 115.0(4) . . ?
N20 C28 C37 103.3(4) . . ?
N10 C28 C37 102.9(4) . . ?
N34 C29 N8 114.2(4) . . ?
N34 C29 C25 103.5(4) . . ?
N8 C29 C25 103.6(4) . . ?
C59 C30 C39 118.1(4) . . ?
C59 C30 C35 119.5(5) . . ?
C39 C30 C35 122.4(4) . . ?
N27 C31 C4 121.0(4) . . ?
N16 C32 N17 114.7(4) . . ?
N16 C32 C23 103.8(3) . . ?
N17 C32 C23 102.8(3) . . ?
O20 C33 N34 126.3(5) . 2_665 ?
O20 C33 N14 125.4(5) . . ?
N34 C33 N14 108.2(4) 2_665 . ?
O16 C34 N17 125.6(4) . . ?
O16 C34 N19 125.8(4) . . ?
N17 C34 N19 108.5(4) . . ?
O6 C35 O5 125.8(5) . . ?
O6 C35 C30 119.0(5) . . ?
O5 C35 C30 115.2(5) . . ?
O19 C36 N16 126.4(4) . . ?
O19 C36 N9 125.7(4) . . ?
N16 C36 N9 107.9(4) . . ?
N30 C37 N26 115.2(4) . . ?
N30 C37 C28 104.1(4) . . ?
N26 C37 C28 103.3(4) . . ?
O21 C38 N24 126.6(4) . . ?
O21 C38 N8 125.4(4) . . ?
N24 C38 N8 108.0(4) . . ?
C41 C39 C30 120.2(4) . . ?
O25 C40 N29 126.1(5) . . ?
O25 C40 N28 125.3(5) . . ?
N29 C40 N28 108.5(4) . . ?
N13 C41 C39 119.8(5) . . ?
N21 C42 N12 115.3(4) . . ?
N21 C42 C16 102.9(4) . . ?
N12 C42 C16 103.4(3) . . ?
O14 C43 N21 126.6(4) . . ?
O14 C43 N33 125.6(4) . . ?
N21 C43 N33 107.8(4) . . ?
N9 C44 N12 114.3(4) . . ?
O17 C45 N25 126.3(5) . . ?
O17 C45 N32 126.0(5) . . ?
N25 C45 N32 107.6(4) . . ?
N32 C46 N16 112.9(4) . . ?
C47 C47 C57 113.3(5) 2_667 . ?
N32 C48 N15 115.8(4) . . ?
N32 C48 C21 103.0(3) . . ?
N15 C48 C21 103.0(3) . . ?
O24 C49 N26 126.3(5) . . ?
O24 C49 N20 125.6(5) . . ?
N26 C49 N20 108.1(4) . . ?
N34 C50 N20 113.8(4) . . ?
C51 C51 C19 112.9(5) 2_566 . ?
O23 C52 N10 126.7(4) . . ?
O23 C52 N30 125.0(5) . . ?
N10 C52 N30 108.2(4) . . ?
N8 C53 N10 113.6(4) . . ?
N23 C54 N2 113.7(4) . 2_766 ?
N27 C55 C22 120.2(4) . . ?
N13 C56 C59 121.1(5) . . ?
C15 C57 C47 111.1(4) . . ?
N31 C58 N29 115.9(4) . . ?
N31 C58 C18 103.1(4) . . ?
N29 C58 C18 103.5(4) . . ?
C56 C59 C30 120.1(5) . . ?
N25 C60 N33 114.0(4) 2_766 . ?
O22 C61 N22 126.3(4) . . ?
O22 C61 N31 126.1(4) . . ?
N22 C61 N31 107.7(4) . . ?
N24 C62 N29 114.5(4) . 2_665 ?
N14 C65 N31 113.5(4) . . ?
C35 O5 U1 133.5(3) . . ?
S1 O7 U1 100.1(2) . . ?
O10 S1 O9 111.5(4) . . ?
O10 S1 O8 110.6(3) . . ?
O9 S1 O8 112.2(4) . . ?
O10 S1 O7 110.9(4) . . ?
O9 S1 O7 109.7(3) . . ?
O8 S1 O7 101.5(2) . . ?
O10 S1 U1 120.9(3) . . ?
O9 S1 U1 127.6(2) . . ?
O8 S1 U1 50.54(15) . . ?
O7 S1 U1 51.13(16) . . ?
S1 O8 U1 101.2(2) . . ?
C10 O4 U1 154.5(4) . 2_656 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        67.08
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.709
_refine_diff_density_min         -2.694
_refine_diff_density_rms         0.105

# SQUEEZE RESULTS
# 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 -0.003 0.000 0.001 1066 202 ' '
_platon_squeeze_details          ?


