# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Qi-Yu Zheng'
_publ_contact_author_email       ZHENGQY@ICCAS.AC.CN

_publ_section_title              
;
Molecular encapsulation of a discrete water of (H2O)32
cluster with S6 symmetry in an organic crystalline supermolecule
;
loop_
_publ_author_name
'Qi-Yu Zheng.'
'Zhi-Tang Huang.'
'Junliang Sun.'
'Wen-Zhi Xu.'

# Attachment 'WZXu_revised.cif'

data_Water32cluster
_database_code_depnum_ccdc_archive 'CCDC 696129'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90 H163 N27 O50'
_chemical_formula_weight         2423.47

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

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   19.5542(3)
_cell_length_b                   19.5542(3)
_cell_length_c                   19.5316(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6467.68(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    9213
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      25.0

_exptl_crystal_description       hexagon
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2584
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9740
_exptl_absorpt_correction_T_max  0.9799
_exptl_absorpt_process_details   crystalclear

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            64775
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0108
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3824
_reflns_number_gt                3753
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrystalClear
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'CrystalStructure 3.7.0'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0780P)^2^+6.1748P] where P=(Fo^2^+2Fc^2^)/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         3824
_refine_ls_number_parameters     299
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1521
_refine_ls_wR_factor_gt          0.1514
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 1.08139(12) 0.35279(12) 0.83289(10) 0.0365(5) Uani 1 1 d D . .
H1A H 1.0983(3) 0.3895(5) 0.8646(5) 0.044 Uiso 1 1 calc RD . .
H1B H 1.0573(4) 0.3028(7) 0.8446(2) 0.044 Uiso 1 1 calc RD . .
N2 N 1.06758(11) 0.31851(11) 0.71884(9) 0.0324(4) Uani 1 1 d D . .
H2A H 1.07517(15) 0.3322(2) 0.6766(6) 0.039 Uiso 1 1 calc RD . .
H2B H 1.0440(3) 0.2694(7) 0.72968(17) 0.039 Uiso 1 1 calc RD . .
N3 N 1.12874(11) 0.44873(12) 0.75122(10) 0.0346(5) Uani 1 1 d D . .
H3A H 1.13657(16) 0.4630(2) 0.7090(6) 0.042 Uiso 1 1 calc RD . .
H3B H 1.1446(3) 0.4838(5) 0.7830(4) 0.042 Uiso 1 1 calc RD . .
N4 N 1.03911(8) 0.07821(15) 0.7500 0.0363(7) Uani 1 2 d SD . .
H4A H 1.0916(10) 0.1044(15) 0.7484(14) 0.044 Uiso 1 1 d D . .
N5 N 0.29515(10) -0.29315(9) 0.61441(9) 0.0245(4) Uani 1 1 d D . .
H5A H 0.3214(4) -0.2420(7) 0.61523(9) 0.029 Uiso 1 1 calc RD . .
H5B H 0.2440(7) -0.3181(3) 0.61400(9) 0.029 Uiso 1 1 calc RD . .
C17 C 1.09229(12) 0.37296(13) 0.76728(11) 0.0285(5) Uani 1 1 d . . .
C18 C 1.0000 0.0000 0.7500 0.0296(11) Uani 1 6 d S . .
C19 C 0.3333 -0.3333 0.61378(17) 0.0195(7) Uani 1 3 d S . .
O1 O 0.95236(10) 0.15896(11) 0.76108(18) 0.0843(10) Uani 1 1 d . . .
C1 C 0.87909(10) 0.12091(10) 0.7500 0.0513(11) Uani 1 2 d S . .
C2 C 0.83494(8) 0.16506(8) 0.7500 0.0286(7) Uani 1 2 d S . .
C3 C 0.76175(12) 0.13385(12) 0.71778(11) 0.0275(5) Uani 1 1 d . . .
H3 H 0.7393(6) 0.0833(14) 0.6955(6) 0.033 Uiso 1 1 calc R . .
C4 C 0.72108(12) 0.17480(11) 0.71749(10) 0.0223(4) Uani 1 1 d . . .
H4 H 0.6701(13) 0.1522(6) 0.6942(6) 0.027 Uiso 1 1 calc R . .
C5 C 0.75190(8) 0.24810(8) 0.7500 0.0187(5) Uani 1 2 d S . .
C6 C 0.70810(7) 0.29190(7) 0.7500 0.0176(5) Uani 1 2 d S . .
C7 C 0.62567(8) 0.25134(15) 0.7500 0.0184(5) Uani 1 2 d S . .
H7 H 0.5966(5) 0.193(2) 0.7500 0.022 Uiso 1 2 calc SR . .
O2 O 0.39009(8) -0.12462(7) 0.62054(7) 0.0229(3) Uani 1 1 d . . .
O3 O 0.50053(8) -0.12621(8) 0.59651(8) 0.0268(3) Uani 1 1 d . . .
C8 C 0.46239(11) -0.09040(11) 0.60447(10) 0.0196(4) Uani 1 1 d . . .
C9 C 0.50493(11) -0.00235(11) 0.59552(9) 0.0183(4) Uani 1 1 d . . .
C10 C 0.57873(11) 0.03730(11) 0.56386(10) 0.0188(4) Uani 1 1 d . . .
H10 H 0.6036(6) 0.0076(7) 0.5478(4) 0.023 Uiso 1 1 calc R . .
C11 C 0.61701(11) 0.11841(11) 0.55499(9) 0.0185(4) Uani 1 1 d . . .
H11 H 0.6694(13) 0.1455(7) 0.5320(6) 0.022 Uiso 1 1 calc R . .
C12 C 0.58335(10) 0.16294(11) 0.57783(9) 0.0167(4) Uani 1 1 d . . .
C13 C 0.50960(11) 0.12263(11) 0.61018(10) 0.0188(4) Uani 1 1 d . . .
H13 H 0.4858(6) 0.1515(7) 0.6268(4) 0.023 Uiso 1 1 calc R . .
C14 C 0.47080(11) 0.04132(11) 0.61839(10) 0.0198(4) Uani 1 1 d . . .
H14 H 0.4214(13) 0.0156(7) 0.6394(6) 0.024 Uiso 1 1 calc R . .
C15 C 0.62599(10) 0.25034(10) 0.57172(9) 0.0166(4) Uani 1 1 d . . .
C16 C 0.70824(11) 0.29300(11) 0.57129(9) 0.0170(4) Uani 1 1 d . . .
H16 H 0.7366(7) 0.2656(7) 0.57070(9) 0.020 Uiso 1 1 calc R . .
OW4 O 0.26677(9) -0.10411(9) 0.57713(8) 0.0280(4) Uani 1 1 d G . .
H24A H 0.3069 -0.1062 0.5847 0.046(6) Uiso 1 1 d G . .
H24B H 0.2371 -0.1459 0.5578 0.046(6) Uiso 1 1 d G . .
OW5 O 0.83579(10) 0.23992(9) 0.49146(9) 0.0339(4) Uani 1 1 d G . .
H25A H 0.8499 0.2849 0.4763 0.066(7) Uiso 1 1 d G . .
H25B H 0.8779 0.2406 0.5003 0.066(7) Uiso 1 1 d G . .
OW6 O 0.97567(11) 0.23803(11) 0.52086(9) 0.0419(4) Uani 1 1 d GD . .
H26A H 1.0167 0.2805 0.5322 0.090(10) Uiso 1 1 d G . .
H26B H 0.9858 0.2278 0.4813 0.090(10) Uiso 1 1 d G . .
OW7 O 1.17198(13) 0.20031(12) 0.60652(11) 0.0623(6) Uani 1 1 d G . .
H27A H 1.1264 0.1711 0.5918 0.093 Uiso 1 1 d GD . .
H27B H 1.1797 0.1721 0.6338 0.093 Uiso 1 1 d GD . .
OW8 O 1.00813(19) 0.14394(17) 0.60896(14) 0.0469(11) Uani 0.705(9) 1 d PRD A 1
H28A H 1.0094 0.1689 0.5739 0.047 Uiso 0.705(9) 1 d PRD A 1
H28B H 0.9607 0.1197 0.6205 0.047 Uiso 0.352(4) 1 d PR A 1
H28C H 1.0086(6) 0.1053(10) 0.592(2) 0.047 Uiso 0.352(4) 1 d PD A 1
OW8B O 0.1710(10) 0.0504(12) 0.6124(8) 0.131(6) Uiso 0.295(9) 1 d P A 2
OW9 O 1.0000 0.0000 0.5709(3) 0.0990(16) Uani 1 3 d SD . .
H29A H 1.026(2) 0.0503(8) 0.5779(17) 0.099 Uiso 0.50 1 d PD . .
H29B H 1.0000 0.0000 0.5282(6) 0.099 Uiso 0.50 3 d SPD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0434(11) 0.0399(11) 0.0293(10) 0.0055(8) 0.0032(8) 0.0231(9)
N2 0.0324(10) 0.0327(10) 0.0304(10) 0.0048(8) 0.0039(8) 0.0151(8)
N3 0.0357(11) 0.0346(10) 0.0292(10) 0.0005(8) -0.0015(8) 0.0144(9)
N4 0.0201(10) 0.0193(13) 0.069(2) 0.000 0.0007(11) 0.0097(7)
N5 0.0150(8) 0.0156(8) 0.0424(11) -0.0015(7) -0.0004(7) 0.0072(7)
C17 0.0227(10) 0.0399(12) 0.0276(11) 0.0026(9) 0.0000(8) 0.0192(10)
C18 0.0214(15) 0.0214(15) 0.046(3) 0.000 0.000 0.0107(8)
C19 0.0182(10) 0.0182(10) 0.0223(16) 0.000 0.000 0.0091(5)
O1 0.0197(9) 0.0238(9) 0.213(3) -0.0044(13) -0.0058(13) 0.0133(8)
C1 0.0215(12) 0.0215(12) 0.113(4) 0.0061(16) 0.0061(16) 0.0126(14)
C2 0.0218(11) 0.0218(11) 0.0451(18) 0.0064(11) 0.0064(11) 0.0132(12)
C3 0.0261(11) 0.0185(10) 0.0390(12) -0.0008(9) 0.0021(9) 0.0120(9)
C4 0.0208(10) 0.0203(10) 0.0260(10) -0.0013(8) -0.0023(8) 0.0104(8)
C5 0.0186(9) 0.0186(9) 0.0194(13) 0.0024(9) 0.0024(9) 0.0097(11)
C6 0.0190(10) 0.0190(10) 0.0157(12) -0.0013(8) -0.0013(8) 0.0101(11)
C7 0.0200(10) 0.0161(13) 0.0177(13) 0.000 -0.0022(9) 0.0081(7)
O2 0.0184(7) 0.0160(7) 0.0318(8) 0.0002(5) 0.0025(6) 0.0068(6)
O3 0.0205(7) 0.0165(7) 0.0451(9) 0.0006(6) 0.0013(6) 0.0105(6)
C8 0.0187(9) 0.0166(9) 0.0224(9) -0.0015(7) -0.0028(7) 0.0079(8)
C9 0.0179(9) 0.0158(9) 0.0204(9) -0.0018(7) -0.0030(7) 0.0079(8)
C10 0.0171(9) 0.0183(9) 0.0231(9) -0.0032(7) -0.0014(7) 0.0105(8)
C11 0.0155(9) 0.0178(9) 0.0209(9) -0.0001(7) 0.0015(7) 0.0074(8)
C12 0.0163(9) 0.0161(9) 0.0173(9) -0.0012(7) -0.0024(7) 0.0077(7)
C13 0.0180(9) 0.0166(9) 0.0240(10) -0.0019(7) -0.0004(7) 0.0103(8)
C14 0.0147(9) 0.0174(9) 0.0251(10) -0.0001(7) 0.0010(7) 0.0064(8)
C15 0.0169(9) 0.0162(9) 0.0164(9) -0.0008(7) -0.0001(7) 0.0081(7)
C16 0.0176(9) 0.0169(9) 0.0182(9) -0.0002(7) 0.0001(7) 0.0099(8)
OW4 0.0232(8) 0.0278(8) 0.0331(8) -0.0048(6) -0.0021(6) 0.0129(6)
OW5 0.0300(8) 0.0260(8) 0.0443(10) -0.0008(7) -0.0024(7) 0.0131(7)
OW6 0.0378(10) 0.0429(10) 0.0425(10) -0.0045(8) -0.0090(7) 0.0184(8)
OW7 0.0647(14) 0.0452(11) 0.0552(12) 0.0052(9) -0.0023(10) 0.0112(10)
OW8 0.052(2) 0.0564(19) 0.0458(16) 0.0143(12) 0.0060(12) 0.0375(16)
OW9 0.106(3) 0.106(3) 0.084(3) 0.000 0.000 0.0532(13)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C17 1.326(3) . ?
N1 H1A 0.8772 . ?
N1 H1B 0.8772 . ?
N2 C17 1.322(3) . ?
N2 H2A 0.8577 . ?
N2 H2B 0.8577 . ?
N3 C17 1.321(3) . ?
N3 H3A 0.8599 . ?
N3 H3B 0.8599 . ?
N4 C18 1.324(3) . ?
N4 H4A 0.890(17) . ?
N5 C19 1.3273(16) . ?
N5 H5A 0.8659 . ?
N5 H5B 0.8659 . ?
C18 N4 1.324(3) 2_645 ?
C18 N4 1.324(3) 3_765 ?
C19 N5 1.3273(16) 3_655 ?
C19 N5 1.3273(16) 2_545 ?
O1 C1 1.260(2) . ?
C1 O1 1.260(2) 10_667 ?
C1 C2 1.495(4) . ?
C2 C3 1.394(3) 10_667 ?
C2 C3 1.394(3) . ?
C3 C4 1.382(3) . ?
C3 H3 0.9625 . ?
C4 C5 1.399(2) . ?
C4 H4 0.9777 . ?
C5 C4 1.399(2) 10_667 ?
C5 C6 1.483(3) . ?
C6 C7 1.3960(18) 2_655 ?
C6 C7 1.3960(18) . ?
C7 C6 1.3960(18) 3_665 ?
C7 H7 0.9855 . ?
O2 C8 1.264(2) . ?
O3 C8 1.262(2) . ?
C8 C9 1.501(3) . ?
C9 C10 1.395(3) . ?
C9 C14 1.394(3) . ?
C10 C11 1.385(3) . ?
C10 H10 0.9779 . ?
C11 C12 1.401(3) . ?
C11 H11 0.9943 . ?
C12 C13 1.401(3) . ?
C12 C15 1.485(2) . ?
C13 C14 1.387(3) . ?
C13 H13 0.9494 . ?
C14 H14 0.9325 . ?
C15 C16 1.393(3) . ?
C15 C16 1.400(3) 3_665 ?
C16 C15 1.400(3) 2_655 ?
C16 H16 0.9432 . ?
OW4 H24A 0.8196 . ?
OW4 H24B 0.8196 . ?
OW5 H25A 0.8338 . ?
OW5 H25B 0.8338 . ?
OW6 H26A 0.8464 . ?
OW6 H26B 0.8464 . ?
OW7 H27A 0.8339 . ?
OW7 H27B 0.8339 . ?
OW8 H28A 0.8339 . ?
OW8 H28B 0.8338 . ?
OW8 H28C 0.826(10) . ?
OW9 H29A 0.863(10) . ?
OW9 H29B 0.833(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 N1 H1A 120.0 . . ?
C17 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C17 N2 H2A 120.0 . . ?
C17 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C17 N3 H3A 120.0 . . ?
C17 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C18 N4 H4A 119.9(18) . . ?
C19 N5 H5A 120.0 . . ?
C19 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
N3 C17 N2 120.6(2) . . ?
N3 C17 N1 118.6(2) . . ?
N2 C17 N1 120.8(2) . . ?
N4 C18 N4 120.0 . 2_645 ?
N4 C18 N4 120.000(1) . 3_765 ?
N4 C18 N4 120.0 2_645 3_765 ?
N5 C19 N5 119.991(6) . 3_655 ?
N5 C19 N5 119.991(6) . 2_545 ?
N5 C19 N5 119.991(6) 3_655 2_545 ?
O1 C1 O1 123.5(3) . 10_667 ?
O1 C1 C2 118.26(15) . . ?
O1 C1 C2 118.26(15) 10_667 . ?
C3 C2 C3 118.7(3) 10_667 . ?
C3 C2 C1 120.66(13) 10_667 . ?
C3 C2 C1 120.66(13) . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.92(19) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C4 118.1(2) . 10_667 ?
C4 C5 C6 120.95(12) . . ?
C4 C5 C6 120.95(12) 10_667 . ?
C7 C6 C7 118.9(3) 2_655 . ?
C7 C6 C5 120.53(13) 2_655 . ?
C7 C6 C5 120.53(13) . . ?
C6 C7 C6 121.1(3) 3_665 . ?
C6 C7 H7 119.5 3_665 . ?
C6 C7 H7 119.5 . . ?
O3 C8 O2 123.47(17) . . ?
O3 C8 C9 118.65(16) . . ?
O2 C8 C9 117.88(16) . . ?
C10 C9 C14 118.71(17) . . ?
C10 C9 C8 120.99(16) . . ?
C14 C9 C8 120.29(17) . . ?
C11 C10 C9 120.55(17) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 121.26(17) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C13 117.72(17) . . ?
C11 C12 C15 121.45(16) . . ?
C13 C12 C15 120.75(16) . . ?
C14 C13 C12 121.08(17) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C9 120.67(17) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
C16 C15 C16 118.69(18) . 3_665 ?
C16 C15 C12 120.36(16) . . ?
C16 C15 C12 120.79(16) 3_665 . ?
C15 C16 C15 121.30(18) . 2_655 ?
C15 C16 H16 119.3 . . ?
C15 C16 H16 119.3 2_655 . ?
H24A OW4 H24B 104.6 . . ?
H25A OW5 H25B 104.6 . . ?
H26A OW6 H26B 104.6 . . ?
H27A OW7 H27B 104.6 . . ?
H28A OW8 H28B 104.6 . . ?
H28A OW8 H28C 101.8 . . ?
H28B OW8 H28C 95.9 . . ?
H29A OW9 H29B 99(2) . . ?

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
O1 C1 C2 C3 -20.4(2) . . . 10_667 ?
O1 C1 C2 C3 159.6(2) 10_667 . . 10_667 ?
O1 C1 C2 C3 159.6(2) . . . . ?
O1 C1 C2 C3 -20.4(2) 10_667 . . . ?
C3 C2 C3 C4 0.30(14) 10_667 . . . ?
C1 C2 C3 C4 -179.70(14) . . . . ?
C2 C3 C4 C5 -0.6(3) . . . . ?
C3 C4 C5 C4 0.30(14) . . . 10_667 ?
C3 C4 C5 C6 -179.70(14) . . . . ?
C4 C5 C6 C7 -148.05(9) . . . 2_655 ?
C4 C5 C6 C7 31.95(9) 10_667 . . 2_655 ?
C4 C5 C6 C7 31.95(9) . . . . ?
C4 C5 C6 C7 -148.05(9) 10_667 . . . ?
C7 C6 C7 C6 0.0 2_655 . . 3_665 ?
C5 C6 C7 C6 180.0 . . . 3_665 ?
O3 C8 C9 C10 14.9(3) . . . . ?
O2 C8 C9 C10 -166.01(17) . . . . ?
O3 C8 C9 C14 -165.62(18) . . . . ?
O2 C8 C9 C14 13.5(3) . . . . ?
C14 C9 C10 C11 -0.4(3) . . . . ?
C8 C9 C10 C11 179.09(17) . . . . ?
C9 C10 C11 C12 0.5(3) . . . . ?
C10 C11 C12 C13 0.2(3) . . . . ?
C10 C11 C12 C15 176.74(17) . . . . ?
C11 C12 C13 C14 -0.9(3) . . . . ?
C15 C12 C13 C14 -177.53(17) . . . . ?
C12 C13 C14 C9 1.0(3) . . . . ?
C10 C9 C14 C13 -0.3(3) . . . . ?
C8 C9 C14 C13 -179.85(17) . . . . ?
C11 C12 C15 C16 -27.4(3) . . . . ?
C13 C12 C15 C16 149.11(18) . . . . ?
C11 C12 C15 C16 157.29(17) . . . 3_665 ?
C13 C12 C15 C16 -26.2(3) . . . 3_665 ?
C16 C15 C16 C15 1.2(4) 3_665 . . 2_655 ?
C12 C15 C16 C15 -174.25(12) . . . 2_655 ?

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
N1 H1A O3 0.88 2.08 2.895(3) 154.1 10_667
N1 H1B OW7 0.88 2.03 2.876(3) 162.4 11_757
N2 H2A OW4 0.86 2.06 2.913(2) 174.8 2_655
N2 H2B O1 0.86 2.09 2.909(3) 158.6 .
N3 H3A O2 0.86 2.07 2.879(2) 155.8 2_655
N3 H3B O3 0.86 2.42 3.144(2) 141.7 10_667
N4 H4A O1 0.890(17) 1.957(17) 2.845(2) 176(3) 11_757
N5 H5A O2 0.87 2.00 2.864(2) 174.9 .
N5 H5B O3 0.87 2.03 2.884(2) 170.7 2_545
OW4 H24A O2 0.82 1.96 2.768(2) 167.4 .
OW4 H24B OW5 0.82 1.93 2.746(2) 175.7 7_656
OW5 H25A O3 0.83 2.10 2.892(2) 158.1 8_666
OW5 H25B OW6 0.83 1.98 2.813(2) 177.9 .
OW6 H26A OW4 0.85 1.95 2.782(2) 168.4 2_655
OW6 H26B OW7 0.85 1.98 2.786(3) 159.8 9_546
OW7 H27A OW8 0.83 2.12 2.820(4) 140.8 .
OW7 H27B O1 0.83 2.17 2.889(4) 145.1 11_757
OW8 H28A OW6 0.83 2.06 2.814(3) 150.8 .
OW8 H28C OW9 0.826(10) 2.025(12) 2.838(3) 168(4) .
OW9 H29A OW8 0.863(10) 2.11(3) 2.838(3) 141(4) .
OW9 H29B OW9 0.833(10) 1.934(15) 2.768(11) 180.000(1) 7_756

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.054

# Highest peak 0.58 at 0.0553 0.0704 0.5623 [ 0.59 A from H29A ]
# Deepest hole -0.72 at 0.0215 0.0277 0.4357 [ 0.51 A from OW9 ]