# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011


data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Wittenberg, James'
'Costales, Matthew'
'Zavalij, Peter'
'Isaacs, Lyle'

_publ_contact_author_name        'Isaacs, Lyle'
_publ_contact_author_email       LIsaacs@umd.edu

_publ_section_title              
;
A Clipped [3]Rotaxane Derived From Bis-nor-seco-Cucurbit[10]uril
;

# Attachment '- 1946.cif'

data_1946
_database_code_depnum_ccdc_archive 'CCDC 828943'
#TrackingRef '- 1946.cif'

# start Validation Reply Form
_vrf_PLAT772_1946                
;
PROBLEM: Suspect O-H Bond in CIF: O9W -- H102 .. 1.33 Ang.
RESPONSE: O9W and H102 atoms belong two two disordered water molecules
superiposed/located near each other
;
_vrf_PLAT417_1946                
;
PROBLEM: Short Inter D-H..H-D H12W .. H82W .. 2.09 Ang.
RESPONSE: Some water molecules are disorderd and some show slightly higher
adp's probably due to slight disorder of orientation. This may slightly
affect the accuracy in the refined H atoms position.
;
_vrf_PLAT731_1946                
;
PROBLEM: Bond Calc 0.83(6), Rep 0.826(13) ......
RESPONSE: Reported value of s.u. is more accurate as it is calculated
taking into account correlation matrix.
;
_vrf_PLAT735_1946                
;
PROBLEM: D-H Calc 0.83(6), Rep 0.820(13) ......
RESPONSE: Reported value of s.u. is more accurate as it is calculated
taking into account correlation matrix.
;
# end Validation Reply Form

_audit_creation_method           'SHELXL-97 & ZCIF'
_chemical_name_systematic        
;
CB10+ bis-p-xylenediammonium diiodide octadecahydrate
;
_chemical_name_common            'CB10+ xylenediammonium diiodide hydrate'
_chemical_formula_moiety         'C68 H72 N44 O22, 2(C8 H14 N2), 18(H2 O), 4(I)'
_chemical_formula_sum            'C84 H136 I4 N48 O40'
_chemical_formula_weight         2966.01

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   13.690(2)
_cell_length_b                   13.972(2)
_cell_length_c                   30.064(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.1108(19)
_cell_angle_gamma                90.00
_cell_volume                     5742.3(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    15779
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      28.2

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3016
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
Disorder-Order phase transition observed during the experiment:

At first crystal structure was indexed in a monoclinic system, sp.gr. P21/n,
a=14.901(9), b=14.231(8), c=29.591(18) , \b = 96.712(9)\0, V=6232(11)\%A^3^.
The structure determination revealed the same structure as reported one.
However all the water molecules except one and one of two iodine ions were
disordered as well as one ammonium group in the guest molecule. Analyses of
the frames showed that crystal was changing during the data collection.
Therefore after experiment was finished a new data collection was undertaken.
It revealed that even so symmetry is unchanged but cell dimensions are
noticeable different a=13.690(2), b=13.972(2), c=30.064(4) \%A, \b=93.1108(19)
\0, V=5742.3(15) \%A^3^. The crystal structure determination showed the same
composition and type of structure including guest-host system. However guest
molecule, both iodine ions, and most of the water molecules are fully ordered.

Thus the title compound undergoes disorder to order phase transition at 250 K
which takes about 10 hours for completion.
;

_diffrn_ambient_temperature      250(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  'three-circle diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_decay_%        0
_diffrn_reflns_number            40898
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         27.50
_reflns_number_total             13130
_reflns_number_gt                10224
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_cell_refinement       Apex2
_computing_data_reduction        Apex2
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97

_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     
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+24.22P], P=(max(Fo^2^,0)+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         13130
_refine_ls_number_parameters     862
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.0994
_refine_ls_wR_factor_gt          0.0953
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.260
_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
I1 I 0.72477(3) 0.20990(3) 0.662308(12) 0.04164(10) Uani 1 1 d . . .
I2 I 0.01597(3) 0.11708(3) 0.602585(13) 0.04668(11) Uani 1 1 d . . .
N1 N 0.1915(3) 0.6188(4) 0.66704(15) 0.0463(12) Uani 1 1 d . . .
H1A H 0.2353 0.5845 0.6838 0.069 Uiso 1 1 calc R . .
H1B H 0.1319 0.5922 0.6684 0.069 Uiso 1 1 calc R . .
H1C H 0.1899 0.6792 0.6774 0.069 Uiso 1 1 calc R . .
C1 C 0.2198(4) 0.6197(4) 0.62090(17) 0.0391(12) Uani 1 1 d . . .
H1D H 0.1771 0.6646 0.6040 0.047 Uiso 1 1 calc R . .
H1E H 0.2081 0.5559 0.6082 0.047 Uiso 1 1 calc R . .
C2 C 0.3247(3) 0.6470(4) 0.61432(15) 0.0289(10) Uani 1 1 d . . .
C3 C 0.3836(4) 0.6969(4) 0.64505(16) 0.0343(11) Uani 1 1 d . . .
H3 H 0.3593 0.7133 0.6727 0.041 Uiso 1 1 calc R . .
C4 C 0.4773(4) 0.7230(4) 0.63564(16) 0.0349(11) Uani 1 1 d . . .
H4 H 0.5158 0.7576 0.6569 0.042 Uiso 1 1 calc R . .
C5 C 0.5162(4) 0.6992(4) 0.59543(15) 0.0312(10) Uani 1 1 d . . .
C6 C 0.4582(4) 0.6462(4) 0.56519(16) 0.0346(11) Uani 1 1 d . . .
H6 H 0.4834 0.6270 0.5381 0.042 Uiso 1 1 calc R . .
C7 C 0.3641(4) 0.6215(4) 0.57444(15) 0.0334(11) Uani 1 1 d . . .
H7 H 0.3256 0.5866 0.5533 0.040 Uiso 1 1 calc R . .
C8 C 0.6181(4) 0.7306(4) 0.58543(17) 0.0386(12) Uani 1 1 d . . .
H8A H 0.6450 0.7704 0.6100 0.046 Uiso 1 1 calc R . .
H8B H 0.6600 0.6741 0.5833 0.046 Uiso 1 1 calc R . .
N8 N 0.6190(3) 0.7850(4) 0.54368(16) 0.0473(12) Uani 1 1 d . . .
H8C H 0.6063 0.7454 0.5205 0.071 Uiso 1 1 calc R . .
H8D H 0.6782 0.8119 0.5413 0.071 Uiso 1 1 calc R . .
H8E H 0.5730 0.8311 0.5436 0.071 Uiso 1 1 calc R . .
N10 N 0.1985(3) 0.6062(3) 0.48275(12) 0.0254(8) Uani 1 1 d . . .
C11 C 0.2522(3) 0.6603(3) 0.45073(14) 0.0248(9) Uani 1 1 d . . .
H11 H 0.2312 0.6430 0.4197 0.030 Uiso 1 1 calc R . .
N12 N 0.3581(3) 0.6585(3) 0.45748(12) 0.0257(8) Uani 1 1 d . . .
C13 C 0.1398(3) 0.6666(4) 0.50594(14) 0.0255(10) Uani 1 1 d . . .
O13 O 0.0774(2) 0.6391(3) 0.53082(11) 0.0322(8) Uani 1 1 d . . .
C14 C 0.3979(3) 0.7471(3) 0.46655(14) 0.0255(9) Uani 1 1 d . . .
O14 O 0.4854(2) 0.7646(3) 0.46833(11) 0.0320(8) Uani 1 1 d . . .
N15 N 0.1630(3) 0.7585(3) 0.49688(12) 0.0275(8) Uani 1 1 d . . .
C16 C 0.2287(3) 0.7657(3) 0.46072(14) 0.0251(9) Uani 1 1 d . . .
H16 H 0.1968 0.7979 0.4344 0.030 Uiso 1 1 calc R . .
N17 N 0.3233(3) 0.8075(3) 0.47269(13) 0.0267(8) Uani 1 1 d . . .
C18 C 0.1138(3) 0.8404(4) 0.51505(15) 0.0283(10) Uani 1 1 d . . .
H18A H 0.0960 0.8849 0.4907 0.034 Uiso 1 1 calc R . .
H18B H 0.0531 0.8186 0.5276 0.034 Uiso 1 1 calc R . .
C19 C 0.3409(4) 0.9078(3) 0.47852(15) 0.0281(10) Uani 1 1 d . . .
H19A H 0.2957 0.9431 0.4581 0.034 Uiso 1 1 calc R . .
H19B H 0.4075 0.9220 0.4702 0.034 Uiso 1 1 calc R . .
N20 N 0.1714(3) 0.8910(3) 0.54904(12) 0.0282(8) Uani 1 1 d . . .
C21 C 0.2366(3) 0.9698(3) 0.54018(14) 0.0257(9) Uani 1 1 d . . .
H21 H 0.2036 1.0192 0.5211 0.031 Uiso 1 1 calc R . .
N22 N 0.3295(3) 0.9422(3) 0.52353(12) 0.0277(8) Uani 1 1 d . . .
C23 C 0.1579(3) 0.8804(4) 0.59352(15) 0.0278(10) Uani 1 1 d . . .
O23 O 0.1023(3) 0.8233(3) 0.60976(11) 0.0374(8) Uani 1 1 d . . .
C24 C 0.4066(3) 0.9606(3) 0.55306(15) 0.0272(10) Uani 1 1 d . . .
O24 O 0.4929(2) 0.9442(3) 0.54735(11) 0.0351(8) Uani 1 1 d . . .
N25 N 0.2167(3) 0.9449(3) 0.61615(12) 0.0261(8) Uani 1 1 d . . .
C26 C 0.2658(3) 1.0092(3) 0.58744(15) 0.0256(9) Uani 1 1 d . . .
H26 H 0.2437 1.0761 0.5910 0.031 Uiso 1 1 calc R . .
N27 N 0.3715(3) 1.0020(3) 0.59025(13) 0.0291(9) Uani 1 1 d . . .
C28 C 0.2070(3) 0.9644(4) 0.66281(14) 0.0280(10) Uani 1 1 d . . .
H28A H 0.1469 0.9343 0.6722 0.034 Uiso 1 1 calc R . .
H28B H 0.2004 1.0337 0.6669 0.034 Uiso 1 1 calc R . .
C29 C 0.4340(4) 1.0435(4) 0.62573(16) 0.0314(11) Uani 1 1 d . . .
H29A H 0.4989 1.0546 0.6144 0.038 Uiso 1 1 calc R . .
H29B H 0.4072 1.1059 0.6336 0.038 Uiso 1 1 calc R . .
N30 N 0.2886(3) 0.9305(3) 0.69112(13) 0.0271(8) Uani 1 1 d . . .
C31 C 0.3764(3) 0.9867(3) 0.70086(15) 0.0262(9) Uani 1 1 d . . .
H31 H 0.3610 1.0526 0.7104 0.031 Uiso 1 1 calc R . .
N32 N 0.4452(3) 0.9859(3) 0.66578(12) 0.0280(8) Uani 1 1 d . . .
C33 C 0.2804(3) 0.8552(3) 0.71935(14) 0.0251(9) Uani 1 1 d . . .
O33 O 0.2115(2) 0.7990(2) 0.71938(11) 0.0301(7) Uani 1 1 d . . .
C34 C 0.5296(3) 0.9375(4) 0.67767(16) 0.0299(10) Uani 1 1 d . . .
O34 O 0.6012(2) 0.9301(3) 0.65546(12) 0.0387(9) Uani 1 1 d . . .
N35 N 0.3616(3) 0.8539(3) 0.74796(12) 0.0275(8) Uani 1 1 d . . .
C36 C 0.4304(3) 0.9285(3) 0.73889(15) 0.0261(9) Uani 1 1 d . . .
H36 H 0.4452 0.9688 0.7655 0.031 Uiso 1 1 calc R . .
N37 N 0.5193(3) 0.8974(3) 0.71889(13) 0.0286(9) Uani 1 1 d . . .
C38 C 0.3742(3) 0.7841(4) 0.78357(14) 0.0276(10) Uani 1 1 d . . .
H38A H 0.4075 0.8150 0.8095 0.033 Uiso 1 1 calc R . .
H38B H 0.3095 0.7637 0.7923 0.033 Uiso 1 1 calc R . .
C39 C 0.5985(3) 0.8479(4) 0.74292(16) 0.0304(10) Uani 1 1 d . . .
H39A H 0.6036 0.8715 0.7737 0.036 Uiso 1 1 calc R . .
H39B H 0.6599 0.8631 0.7292 0.036 Uiso 1 1 calc R . .
N40 N 0.4290(3) 0.7011(3) 0.77192(12) 0.0263(8) Uani 1 1 d . . .
C41 C 0.5346(3) 0.6935(3) 0.77695(14) 0.0251(9) Uani 1 1 d . . .
H41 H 0.5593 0.7103 0.8075 0.030 Uiso 1 1 calc R . .
N42 N 0.5865(3) 0.7449(3) 0.74363(12) 0.0269(8) Uani 1 1 d . . .
C43 C 0.3864(3) 0.6179(4) 0.75795(14) 0.0250(9) Uani 1 1 d . . .
O43 O 0.2981(2) 0.6037(3) 0.75144(11) 0.0318(8) Uani 1 1 d . . .
C44 C 0.6427(3) 0.6849(3) 0.71944(15) 0.0258(10) Uani 1 1 d . . .
O44 O 0.7014(2) 0.7107(3) 0.69247(11) 0.0358(8) Uani 1 1 d . . .
N45 N 0.4578(3) 0.5513(3) 0.75317(12) 0.0269(8) Uani 1 1 d . . .
C46 C 0.5544(3) 0.5872(3) 0.76610(14) 0.0251(9) Uani 1 1 d . . .
H46 H 0.5835 0.5527 0.7924 0.030 Uiso 1 1 calc R . .
N47 N 0.6223(3) 0.5930(3) 0.73077(12) 0.0268(8) Uani 1 1 d . . .
C48 C 0.4355(4) 0.4545(3) 0.74026(14) 0.0277(10) Uani 1 1 d . . .
H48A H 0.3673 0.4408 0.7462 0.033 Uiso 1 1 calc R . .
H48B H 0.4770 0.4110 0.7585 0.033 Uiso 1 1 calc R . .
C49 C 0.6709(3) 0.5115(3) 0.71203(15) 0.0258(10) Uani 1 1 d . . .
H49A H 0.7347 0.5322 0.7024 0.031 Uiso 1 1 calc R . .
H49B H 0.6825 0.4635 0.7355 0.031 Uiso 1 1 calc R . .
N50 N 0.4501(3) 0.4359(3) 0.69354(12) 0.0247(8) Uani 1 1 d . . .
C51 C 0.5408(3) 0.3973(3) 0.67902(14) 0.0233(9) Uani 1 1 d . . .
H51 H 0.5635 0.3425 0.6978 0.028 Uiso 1 1 calc R . .
N52 N 0.6175(3) 0.4672(3) 0.67481(12) 0.0256(8) Uani 1 1 d . . .
C53 C 0.3731(3) 0.4152(3) 0.66424(15) 0.0253(9) Uani 1 1 d . . .
O53 O 0.2865(2) 0.4247(3) 0.67171(11) 0.0341(8) Uani 1 1 d . . .
C54 C 0.6390(3) 0.4810(3) 0.63124(15) 0.0250(9) Uani 1 1 d . . .
O54 O 0.7053(2) 0.5305(3) 0.61822(11) 0.0330(8) Uani 1 1 d . . .
N55 N 0.4085(3) 0.3824(3) 0.62479(12) 0.0248(8) Uani 1 1 d . . .
C56 C 0.5138(3) 0.3654(3) 0.63053(14) 0.0236(9) Uani 1 1 d . . .
H56 H 0.5301 0.2973 0.6258 0.028 Uiso 1 1 calc R . .
N57 N 0.5741(3) 0.4284(3) 0.60505(12) 0.0248(8) Uani 1 1 d . . .
C58 C 0.3471(3) 0.3186(3) 0.59618(15) 0.0271(10) Uani 1 1 d . . .
H58A H 0.3889 0.2866 0.5753 0.033 Uiso 1 1 calc R . .
H58B H 0.3199 0.2690 0.6149 0.033 Uiso 1 1 calc R . .
C59 C 0.5790(3) 0.4272(3) 0.55762(14) 0.0262(10) Uani 1 1 d . . .
H59A H 0.6076 0.4873 0.5477 0.031 Uiso 1 1 calc R . .
H59B H 0.5127 0.4221 0.5437 0.031 Uiso 1 1 calc R . .
N60 N 0.2681(3) 0.3640(3) 0.57116(13) 0.0330(10) Uani 1 1 d . . .
C61 C 0.1675(3) 0.3657(4) 0.58460(18) 0.0360(12) Uani 1 1 d . . .
H61A H 0.1626 0.3991 0.6130 0.043 Uiso 1 1 calc R . .
H61B H 0.1417 0.3006 0.5874 0.043 Uiso 1 1 calc R . .
C62 C 0.2781(3) 0.4086(3) 0.53123(15) 0.0266(10) Uani 1 1 d . . .
O62 O 0.3527(2) 0.4114(3) 0.51028(11) 0.0326(8) Uani 1 1 d . . .
N63 N 0.1910(3) 0.4508(3) 0.51877(13) 0.0299(9) Uani 1 1 d . . .
C64 C 0.1132(3) 0.4197(4) 0.54688(16) 0.0355(12) Uani 1 1 d . . .
H64A H 0.0667 0.3778 0.5304 0.043 Uiso 1 1 calc R . .
H64B H 0.0778 0.4747 0.5583 0.043 Uiso 1 1 calc R . .
C65 C 0.1746(3) 0.5042(3) 0.47805(15) 0.0275(10) Uani 1 1 d . . .
H65A H 0.1058 0.4979 0.4678 0.033 Uiso 1 1 calc R . .
H65B H 0.2144 0.4764 0.4552 0.033 Uiso 1 1 calc R . .
O1W O 0.1001(4) 0.7209(3) 0.79381(15) 0.0560(11) Uani 1 1 d D . .
H11W H 0.137(4) 0.739(6) 0.7746(17) 0.084 Uiso 1 1 d D . .
H12W H 0.050(3) 0.707(6) 0.7795(19) 0.084 Uiso 1 1 d D . .
O2W O 0.8008(3) 0.8726(4) 0.54485(17) 0.0584(12) Uani 1 1 d D . .
H21W H 0.827(5) 0.906(4) 0.565(2) 0.088 Uiso 1 1 d D . .
H22W H 0.8312(19) 0.8225(16) 0.543(3) 0.088 Uiso 1 1 d D . .
O3W O 1.0103(3) 0.5268(4) 0.65595(17) 0.0541(11) Uani 1 1 d D . .
H31W H 0.985(5) 0.478(3) 0.645(2) 0.081 Uiso 1 1 d D . .
H32W H 0.967(4) 0.568(3) 0.653(3) 0.081 Uiso 1 1 d D . .
O4W O 0.8967(3) 0.7034(4) 0.55994(19) 0.0651(13) Uani 1 1 d D . .
H41W H 0.951(3) 0.690(6) 0.551(3) 0.098 Uiso 1 1 d D . .
H42W H 0.886(6) 0.665(5) 0.580(2) 0.098 Uiso 1 1 d D . .
O5W O 0.0636(4) 0.6505(3) 0.37447(19) 0.0616(12) Uani 1 1 d D . .
H51W H 0.116(3) 0.659(5) 0.363(3) 0.092 Uiso 1 1 d D . .
H52W H 0.046(5) 0.704(2) 0.382(3) 0.092 Uiso 1 1 d D . .
O6W O 0.9445(4) 0.8552(4) 0.66655(17) 0.0729(15) Uani 1 1 d D . .
H61W H 0.990(4) 0.847(7) 0.650(2) 0.109 Uiso 1 1 d D . .
H62W H 0.896(4) 0.866(4) 0.650(3) 0.109 Uiso 0.654(19) 1 d PD A 1
H63W H 0.941(16) 0.805(9) 0.681(7) 0.109 Uiso 0.346(19) 1 d PD A 2
O7W O 0.7911(4) 0.9708(4) 0.6274(2) 0.0756(15) Uani 1 1 d D . .
H71W H 0.744(5) 0.958(6) 0.642(3) 0.113 Uiso 1 1 d D . .
H72W H 0.801(6) 1.0281(18) 0.631(3) 0.113 Uiso 1 1 d D . .
O8W O 0.5691(5) 0.1255(5) 0.7453(2) 0.0874(18) Uani 1 1 d D . .
H81W H 0.612(6) 0.134(7) 0.727(3) 0.131 Uiso 1 1 d D . .
H82W H 0.574(4) 0.174(3) 0.761(2) 0.131 Uiso 1 1 d D . .
O9W O 0.8792(7) 0.6787(9) 0.6599(5) 0.061(3) Uani 0.654(19) 1 d PDU A 1
H91W H 0.902(7) 0.725(3) 0.6738(15) 0.091 Uiso 0.654(19) 1 d PD A 1
H92W H 0.823(3) 0.672(8) 0.667(4) 0.091 Uiso 0.654(19) 1 d PD A 1
O10W O 0.8666(15) 0.6524(16) 0.6407(9) 0.061(3) Uani 0.346(19) 1 d PD A 2
H101 H 0.840(7) 0.705(3) 0.643(3) 0.091 Uiso 0.346(19) 1 d PD A 2
H102 H 0.822(3) 0.613(4) 0.640(8) 0.091 Uiso 0.346(19) 1 d PD A 2

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
I1 0.03265(17) 0.0553(2) 0.03698(18) 0.00599(17) 0.00216(13) 0.01311(16)
I2 0.04043(19) 0.0574(3) 0.0417(2) 0.00031(18) -0.00229(15) 0.01304(18)
N1 0.037(2) 0.065(3) 0.037(2) -0.008(2) 0.0055(19) -0.011(2)
C1 0.036(3) 0.052(3) 0.029(3) 0.002(2) -0.005(2) -0.003(2)
C2 0.033(2) 0.028(3) 0.025(2) 0.0021(19) -0.0038(19) 0.000(2)
C3 0.040(3) 0.038(3) 0.025(2) -0.008(2) 0.002(2) -0.002(2)
C4 0.039(3) 0.037(3) 0.028(2) -0.008(2) -0.004(2) -0.005(2)
C5 0.035(2) 0.033(3) 0.025(2) 0.003(2) -0.0007(19) 0.000(2)
C6 0.043(3) 0.039(3) 0.022(2) -0.003(2) 0.002(2) 0.000(2)
C7 0.043(3) 0.034(3) 0.023(2) -0.003(2) -0.007(2) -0.004(2)
C8 0.032(3) 0.051(4) 0.032(3) 0.007(2) -0.004(2) 0.001(2)
N8 0.032(2) 0.061(3) 0.048(3) 0.018(3) -0.005(2) -0.007(2)
N10 0.0228(18) 0.031(2) 0.0228(18) -0.0009(16) 0.0024(14) 0.0036(16)
C11 0.023(2) 0.035(3) 0.0164(19) -0.0028(18) 0.0001(16) 0.0027(19)
N12 0.0211(18) 0.034(2) 0.0221(18) -0.0050(16) 0.0034(14) 0.0018(16)
C13 0.022(2) 0.036(3) 0.018(2) -0.0036(19) -0.0015(16) 0.0001(19)
O13 0.0268(16) 0.041(2) 0.0296(17) -0.0021(15) 0.0086(14) 0.0003(15)
C14 0.027(2) 0.032(3) 0.017(2) 0.0004(18) 0.0030(17) 0.0003(19)
O14 0.0224(16) 0.039(2) 0.0349(18) -0.0046(15) 0.0037(13) 0.0000(14)
N15 0.0262(19) 0.032(2) 0.0248(19) -0.0047(16) 0.0072(15) 0.0025(16)
C16 0.025(2) 0.034(3) 0.017(2) 0.0003(18) 0.0022(16) 0.0042(19)
N17 0.0237(18) 0.029(2) 0.0277(19) -0.0028(16) 0.0049(15) 0.0011(16)
C18 0.024(2) 0.035(3) 0.027(2) -0.006(2) 0.0041(18) 0.0055(19)
C19 0.033(2) 0.028(3) 0.024(2) 0.0024(19) 0.0087(18) 0.002(2)
N20 0.031(2) 0.031(2) 0.0229(19) -0.0022(17) 0.0063(15) -0.0034(17)
C21 0.031(2) 0.025(2) 0.022(2) 0.0010(18) 0.0032(18) 0.0040(19)
N22 0.029(2) 0.032(2) 0.0224(19) -0.0029(16) 0.0051(15) 0.0020(17)
C23 0.030(2) 0.028(3) 0.026(2) -0.0005(19) 0.0066(18) 0.005(2)
O23 0.044(2) 0.038(2) 0.0317(18) -0.0039(16) 0.0131(16) -0.0106(17)
C24 0.033(2) 0.023(2) 0.026(2) 0.0042(19) 0.0071(18) -0.0019(19)
O24 0.0281(17) 0.043(2) 0.0344(19) 0.0035(16) 0.0060(14) -0.0016(15)
N25 0.0297(19) 0.028(2) 0.0207(18) -0.0023(16) 0.0058(15) 0.0002(16)
C26 0.031(2) 0.022(2) 0.024(2) -0.0007(18) 0.0017(18) 0.0037(18)
N27 0.030(2) 0.036(2) 0.0223(19) -0.0026(17) 0.0034(15) -0.0025(17)
C28 0.028(2) 0.034(3) 0.023(2) -0.002(2) 0.0037(18) 0.007(2)
C29 0.036(3) 0.030(3) 0.028(2) 0.003(2) 0.000(2) -0.008(2)
N30 0.0257(19) 0.030(2) 0.0258(19) 0.0025(17) 0.0008(15) 0.0023(16)
C31 0.032(2) 0.023(2) 0.024(2) -0.0040(18) 0.0028(18) 0.0007(19)
N32 0.029(2) 0.032(2) 0.0235(19) 0.0000(16) 0.0024(15) -0.0005(17)
C33 0.027(2) 0.026(2) 0.023(2) -0.0033(18) 0.0066(17) 0.0079(19)
O33 0.0260(16) 0.0335(19) 0.0309(17) 0.0006(15) 0.0032(13) -0.0010(14)
C34 0.032(2) 0.026(3) 0.032(2) -0.005(2) 0.003(2) -0.004(2)
O34 0.0315(18) 0.044(2) 0.042(2) 0.0034(17) 0.0134(16) -0.0010(16)
N35 0.0273(19) 0.033(2) 0.0222(18) 0.0015(16) 0.0030(15) 0.0011(17)
C36 0.030(2) 0.026(2) 0.022(2) -0.0056(18) 0.0009(18) 0.0012(19)
N37 0.0285(19) 0.029(2) 0.028(2) -0.0001(17) 0.0039(16) 0.0018(17)
C38 0.029(2) 0.035(3) 0.020(2) 0.0007(19) 0.0057(17) 0.006(2)
C39 0.026(2) 0.034(3) 0.031(2) -0.006(2) -0.0001(19) -0.006(2)
N40 0.0242(18) 0.030(2) 0.0249(19) -0.0025(16) 0.0012(15) 0.0041(16)
C41 0.025(2) 0.032(3) 0.019(2) -0.0028(18) 0.0017(16) 0.0024(19)
N42 0.0260(19) 0.032(2) 0.0234(19) -0.0012(16) 0.0028(15) 0.0030(16)
C43 0.028(2) 0.031(3) 0.0164(19) 0.0037(18) 0.0050(16) -0.0013(19)
O43 0.0249(16) 0.040(2) 0.0304(17) 0.0001(15) 0.0041(13) -0.0028(15)
C44 0.022(2) 0.032(3) 0.023(2) -0.0040(19) -0.0013(17) 0.0000(18)
O44 0.0313(17) 0.042(2) 0.0355(18) -0.0008(16) 0.0127(15) -0.0023(16)
N45 0.0257(19) 0.029(2) 0.0263(19) -0.0028(16) 0.0064(15) -0.0015(16)
C46 0.025(2) 0.032(3) 0.018(2) 0.0006(18) 0.0007(17) 0.0028(19)
N47 0.0239(18) 0.033(2) 0.0243(19) -0.0073(16) 0.0049(15) 0.0002(16)
C48 0.035(2) 0.029(3) 0.020(2) 0.0029(19) 0.0082(18) 0.000(2)
C49 0.020(2) 0.031(3) 0.026(2) -0.0019(19) -0.0012(17) 0.0034(18)
N50 0.0253(18) 0.028(2) 0.0217(18) -0.0013(16) 0.0056(15) 0.0003(16)
C51 0.025(2) 0.022(2) 0.023(2) 0.0009(17) 0.0031(17) 0.0019(18)
N52 0.0255(18) 0.029(2) 0.0226(18) -0.0024(16) 0.0047(15) -0.0042(16)
C53 0.029(2) 0.023(2) 0.025(2) 0.0050(18) 0.0055(18) 0.0027(18)
O53 0.0246(16) 0.047(2) 0.0318(18) 0.0007(16) 0.0075(14) 0.0052(15)
C54 0.024(2) 0.026(2) 0.026(2) -0.0018(19) 0.0067(17) 0.0043(18)
O54 0.0327(18) 0.035(2) 0.0320(18) -0.0042(15) 0.0108(14) -0.0081(15)
N55 0.0242(18) 0.028(2) 0.0222(18) 0.0017(16) 0.0061(14) 0.0034(16)
C56 0.024(2) 0.023(2) 0.024(2) 0.0009(18) 0.0040(17) 0.0018(17)
N57 0.0275(19) 0.027(2) 0.0205(18) -0.0022(15) 0.0081(15) -0.0031(16)
C58 0.026(2) 0.028(3) 0.027(2) 0.0012(19) 0.0023(18) 0.0012(19)
C59 0.024(2) 0.034(3) 0.021(2) 0.0002(19) 0.0042(17) 0.0035(19)
N60 0.0221(19) 0.048(3) 0.029(2) 0.0085(19) 0.0027(16) 0.0019(18)
C61 0.023(2) 0.045(3) 0.040(3) 0.008(2) 0.006(2) -0.001(2)
C62 0.024(2) 0.031(3) 0.025(2) -0.0025(19) -0.0001(17) -0.0024(19)
O62 0.0241(16) 0.048(2) 0.0262(16) 0.0032(15) 0.0057(13) 0.0030(15)
N63 0.0216(18) 0.039(2) 0.029(2) 0.0060(18) 0.0015(15) 0.0016(17)
C64 0.023(2) 0.052(3) 0.032(3) 0.003(2) 0.0007(19) -0.002(2)
C65 0.024(2) 0.034(3) 0.024(2) -0.0019(19) -0.0019(17) 0.0002(19)
O1W 0.064(3) 0.043(3) 0.063(3) 0.005(2) 0.021(2) 0.002(2)
O2W 0.046(2) 0.063(3) 0.066(3) 0.013(2) -0.002(2) -0.004(2)
O3W 0.039(2) 0.054(3) 0.068(3) -0.004(2) -0.002(2) -0.001(2)
O4W 0.046(3) 0.060(3) 0.091(4) -0.011(3) 0.018(2) 0.005(2)
O5W 0.052(3) 0.052(3) 0.080(4) 0.006(3) -0.007(2) -0.002(2)
O6W 0.063(3) 0.096(4) 0.061(3) -0.011(3) 0.011(2) 0.001(3)
O7W 0.061(3) 0.057(3) 0.110(5) -0.018(3) 0.015(3) -0.007(3)
O8W 0.083(4) 0.111(5) 0.070(4) 0.006(3) 0.018(3) -0.014(4)
O9W 0.038(3) 0.056(6) 0.089(7) -0.007(4) 0.017(5) 0.003(3)
O10W 0.038(3) 0.056(6) 0.089(7) -0.007(4) 0.017(5) 0.003(3)

_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 C1 1.460(6) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
C1 C2 1.509(7) . ?
C1 H1D 0.9800 . ?
C1 H1E 0.9800 . ?
C2 C3 1.381(7) . ?
C2 C7 1.387(7) . ?
C3 C4 1.378(7) . ?
C3 H3 0.9400 . ?
C4 C5 1.387(7) . ?
C4 H4 0.9400 . ?
C5 C6 1.388(7) . ?
C5 C8 1.508(7) . ?
C6 C7 1.377(7) . ?
C6 H6 0.9400 . ?
C7 H7 0.9400 . ?
C8 N8 1.468(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
N8 H8C 0.9000 . ?
N8 H8D 0.9000 . ?
N8 H8E 0.9000 . ?
N10 C13 1.380(6) . ?
N10 C11 1.455(6) . ?
N10 C65 1.467(6) . ?
C11 N12 1.453(5) . ?
C11 C16 1.541(7) . ?
C11 H11 0.9900 . ?
N12 C14 1.373(6) . ?
N12 C59 1.558(6) 3_666 ?
C13 O13 1.228(5) . ?
C13 N15 1.354(6) . ?
C14 O14 1.222(5) . ?
C14 N17 1.345(6) . ?
N15 C18 1.449(6) . ?
N15 C16 1.451(5) . ?
C16 N17 1.448(6) . ?
C16 H16 0.9900 . ?
N17 C19 1.431(6) . ?
C18 N20 1.442(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 N22 1.452(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
N20 C23 1.368(6) . ?
N20 C21 1.451(6) . ?
C21 N22 1.444(6) . ?
C21 C26 1.556(6) . ?
C21 H21 0.9900 . ?
N22 C24 1.366(6) . ?
C23 O23 1.223(6) . ?
C23 N25 1.364(6) . ?
C24 O24 1.225(6) . ?
C24 N27 1.369(6) . ?
N25 C26 1.439(6) . ?
N25 C28 1.442(5) . ?
C26 N27 1.449(6) . ?
C26 H26 0.9900 . ?
N27 C29 1.452(6) . ?
C28 N30 1.447(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C29 N32 1.450(6) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
N30 C33 1.361(6) . ?
N30 C31 1.452(6) . ?
C31 N32 1.452(6) . ?
C31 C36 1.557(6) . ?
C31 H31 0.9900 . ?
N32 C34 1.369(6) . ?
C33 O33 1.227(6) . ?
C33 N35 1.369(6) . ?
C34 O34 1.219(6) . ?
C34 N37 1.374(6) . ?
N35 C36 1.441(6) . ?
N35 C38 1.451(6) . ?
C36 N37 1.453(6) . ?
C36 H36 0.9900 . ?
N37 C39 1.446(6) . ?
C38 N40 1.435(6) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C39 N42 1.448(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
N40 C43 1.358(6) . ?
N40 C41 1.448(5) . ?
C41 N42 1.450(6) . ?
C41 C46 1.548(7) . ?
C41 H41 0.9900 . ?
N42 C44 1.373(6) . ?
C43 O43 1.229(5) . ?
C43 N45 1.363(6) . ?
C44 O44 1.227(5) . ?
C44 N47 1.362(6) . ?
N45 C48 1.435(6) . ?
N45 C46 1.449(6) . ?
C46 N47 1.450(5) . ?
C46 H46 0.9900 . ?
N47 C49 1.448(6) . ?
C48 N50 1.453(5) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C49 N52 1.443(6) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
N50 C53 1.368(6) . ?
N50 C51 1.442(5) . ?
C51 N52 1.445(6) . ?
C51 C56 1.550(6) . ?
C51 H51 0.9900 . ?
N52 C54 1.371(5) . ?
C53 O53 1.225(5) . ?
C53 N55 1.383(6) . ?
C54 O54 1.222(5) . ?
C54 N57 1.369(6) . ?
N55 C56 1.462(5) . ?
N55 C58 1.471(6) . ?
C56 N57 1.453(5) . ?
C56 H56 0.9900 . ?
N57 C59 1.431(5) . ?
C58 N60 1.432(6) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C59 N12 1.558(6) 3_666 ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
N60 C62 1.366(6) . ?
N60 C61 1.456(6) . ?
C61 C64 1.522(7) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C62 O62 1.228(5) . ?
C62 N63 1.365(6) . ?
N63 C65 1.441(6) . ?
N63 C64 1.461(6) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
O1W H11W 0.826(13) . ?
O1W H12W 0.819(13) . ?
O2W H21W 0.820(13) . ?
O2W H22W 0.818(13) . ?
O3W H31W 0.822(13) . ?
O3W H32W 0.825(13) . ?
O4W H41W 0.821(13) . ?
O4W H42W 0.818(13) . ?
O5W H51W 0.820(13) . ?
O5W H52W 0.820(13) . ?
O6W H61W 0.825(13) . ?
O6W H62W 0.825(13) . ?
O6W H63W 0.823(13) . ?
O7W H71W 0.821(13) . ?
O7W H72W 0.818(13) . ?
O8W H81W 0.827(13) . ?
O8W H82W 0.830(13) . ?
O9W H91W 0.821(13) . ?
O9W H92W 0.820(13) . ?
O9W H101 0.81(8) . ?
O9W H102 1.33(11) . ?
O10W H92W 1.06(7) . ?
O10W H101 0.821(13) . ?
O10W H102 0.821(13) . ?

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
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
N1 C1 C2 115.5(4) . . ?
N1 C1 H1D 108.4 . . ?
C2 C1 H1D 108.4 . . ?
N1 C1 H1E 108.4 . . ?
C2 C1 H1E 108.4 . . ?
H1D C1 H1E 107.5 . . ?
C3 C2 C7 117.9(5) . . ?
C3 C2 C1 124.3(4) . . ?
C7 C2 C1 117.7(4) . . ?
C4 C3 C2 120.8(5) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 121.4(5) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C6 117.8(5) . . ?
C4 C5 C8 120.4(5) . . ?
C6 C5 C8 121.8(4) . . ?
C7 C6 C5 120.6(5) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 121.4(5) . . ?
C6 C7 H7 119.3 . . ?
C2 C7 H7 119.3 . . ?
N8 C8 C5 111.8(4) . . ?
N8 C8 H8A 109.2 . . ?
C5 C8 H8A 109.2 . . ?
N8 C8 H8B 109.2 . . ?
C5 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C8 N8 H8C 109.5 . . ?
C8 N8 H8D 109.5 . . ?
H8C N8 H8D 109.5 . . ?
C8 N8 H8E 109.5 . . ?
H8C N8 H8E 109.5 . . ?
H8D N8 H8E 109.5 . . ?
C13 N10 C11 110.2(4) . . ?
C13 N10 C65 120.7(4) . . ?
C11 N10 C65 124.0(4) . . ?
N12 C11 N10 115.8(4) . . ?
N12 C11 C16 101.9(4) . . ?
N10 C11 C16 104.4(3) . . ?
N12 C11 H11 111.3 . . ?
N10 C11 H11 111.3 . . ?
C16 C11 H11 111.3 . . ?
C14 N12 C11 113.2(4) . . ?
C14 N12 C59 122.1(4) . 3_666 ?
C11 N12 C59 122.4(4) . 3_666 ?
O13 C13 N15 126.7(4) . . ?
O13 C13 N10 124.0(5) . . ?
N15 C13 N10 109.2(4) . . ?
O14 C14 N17 128.2(5) . . ?
O14 C14 N12 124.6(4) . . ?
N17 C14 N12 107.3(4) . . ?
C13 N15 C18 123.6(4) . . ?
C13 N15 C16 112.2(4) . . ?
C18 N15 C16 123.2(4) . . ?
N17 C16 N15 115.1(4) . . ?
N17 C16 C11 103.9(3) . . ?
N15 C16 C11 103.0(4) . . ?
N17 C16 H16 111.5 . . ?
N15 C16 H16 111.5 . . ?
C11 C16 H16 111.5 . . ?
C14 N17 C19 120.5(4) . . ?
C14 N17 C16 112.9(4) . . ?
C19 N17 C16 124.5(4) . . ?
N20 C18 N15 114.0(4) . . ?
N20 C18 H18A 108.7 . . ?
N15 C18 H18A 108.7 . . ?
N20 C18 H18B 108.7 . . ?
N15 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
N17 C19 N22 114.4(4) . . ?
N17 C19 H19A 108.7 . . ?
N22 C19 H19A 108.7 . . ?
N17 C19 H19B 108.7 . . ?
N22 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C23 N20 C18 122.8(4) . . ?
C23 N20 C21 112.2(4) . . ?
C18 N20 C21 124.1(4) . . ?
N22 C21 N20 115.0(4) . . ?
N22 C21 C26 102.9(4) . . ?
N20 C21 C26 103.3(3) . . ?
N22 C21 H21 111.6 . . ?
N20 C21 H21 111.6 . . ?
C26 C21 H21 111.6 . . ?
C24 N22 C21 112.8(4) . . ?
C24 N22 C19 123.4(4) . . ?
C21 N22 C19 123.5(4) . . ?
O23 C23 N25 126.5(4) . . ?
O23 C23 N20 125.5(5) . . ?
N25 C23 N20 108.0(4) . . ?
O24 C24 N22 126.2(4) . . ?
O24 C24 N27 125.2(4) . . ?
N22 C24 N27 108.5(4) . . ?
C23 N25 C26 113.3(4) . . ?
C23 N25 C28 121.8(4) . . ?
C26 N25 C28 122.4(4) . . ?
N25 C26 N27 114.8(4) . . ?
N25 C26 C21 102.8(4) . . ?
N27 C26 C21 103.6(3) . . ?
N25 C26 H26 111.7 . . ?
N27 C26 H26 111.7 . . ?
C21 C26 H26 111.7 . . ?
C24 N27 C26 112.0(4) . . ?
C24 N27 C29 123.4(4) . . ?
C26 N27 C29 124.2(4) . . ?
N25 C28 N30 113.6(4) . . ?
N25 C28 H28A 108.8 . . ?
N30 C28 H28A 108.8 . . ?
N25 C28 H28B 108.8 . . ?
N30 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
N32 C29 N27 114.8(4) . . ?
N32 C29 H29A 108.6 . . ?
N27 C29 H29A 108.6 . . ?
N32 C29 H29B 108.6 . . ?
N27 C29 H29B 108.6 . . ?
H29A C29 H29B 107.5 . . ?
C33 N30 C28 122.1(4) . . ?
C33 N30 C31 112.9(4) . . ?
C28 N30 C31 123.1(4) . . ?
N30 C31 N32 114.3(4) . . ?
N30 C31 C36 102.8(4) . . ?
N32 C31 C36 103.2(4) . . ?
N30 C31 H31 111.9 . . ?
N32 C31 H31 111.9 . . ?
C36 C31 H31 111.9 . . ?
C34 N32 C29 122.7(4) . . ?
C34 N32 C31 112.7(4) . . ?
C29 N32 C31 123.7(4) . . ?
O33 C33 N30 125.8(4) . . ?
O33 C33 N35 126.1(4) . . ?
N30 C33 N35 108.0(4) . . ?
O34 C34 N32 126.2(5) . . ?
O34 C34 N37 125.8(5) . . ?
N32 C34 N37 108.1(4) . . ?
C33 N35 C36 112.9(4) . . ?
C33 N35 C38 122.1(4) . . ?
C36 N35 C38 125.0(4) . . ?
N35 C36 N37 115.6(4) . . ?
N35 C36 C31 103.2(4) . . ?
N37 C36 C31 103.1(4) . . ?
N35 C36 H36 111.4 . . ?
N37 C36 H36 111.4 . . ?
C31 C36 H36 111.4 . . ?
C34 N37 C39 122.3(4) . . ?
C34 N37 C36 112.4(4) . . ?
C39 N37 C36 124.0(4) . . ?
N40 C38 N35 113.9(4) . . ?
N40 C38 H38A 108.8 . . ?
N35 C38 H38A 108.8 . . ?
N40 C38 H38B 108.8 . . ?
N35 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
N37 C39 N42 113.6(4) . . ?
N37 C39 H39A 108.8 . . ?
N42 C39 H39A 108.8 . . ?
N37 C39 H39B 108.8 . . ?
N42 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
C43 N40 C38 123.1(4) . . ?
C43 N40 C41 112.3(4) . . ?
C38 N40 C41 124.5(4) . . ?
N40 C41 N42 114.5(4) . . ?
N40 C41 C46 103.6(4) . . ?
N42 C41 C46 103.4(3) . . ?
N40 C41 H41 111.6 . . ?
N42 C41 H41 111.6 . . ?
C46 C41 H41 111.6 . . ?
C44 N42 C39 122.1(4) . . ?
C44 N42 C41 111.9(4) . . ?
C39 N42 C41 124.2(4) . . ?
O43 C43 N40 126.1(4) . . ?
O43 C43 N45 125.3(5) . . ?
N40 C43 N45 108.6(4) . . ?
O44 C44 N47 126.3(4) . . ?
O44 C44 N42 125.3(5) . . ?
N47 C44 N42 108.4(4) . . ?
C43 N45 C48 121.9(4) . . ?
C43 N45 C46 112.7(4) . . ?
C48 N45 C46 125.2(4) . . ?
N45 C46 N47 115.8(4) . . ?
N45 C46 C41 102.7(3) . . ?
N47 C46 C41 103.2(4) . . ?
N45 C46 H46 111.5 . . ?
N47 C46 H46 111.5 . . ?
C41 C46 H46 111.5 . . ?
C44 N47 C49 122.6(4) . . ?
C44 N47 C46 112.6(4) . . ?
C49 N47 C46 124.5(4) . . ?
N45 C48 N50 113.1(4) . . ?
N45 C48 H48A 109.0 . . ?
N50 C48 H48A 109.0 . . ?
N45 C48 H48B 109.0 . . ?
N50 C48 H48B 109.0 . . ?
H48A C48 H48B 107.8 . . ?
N52 C49 N47 114.5(4) . . ?
N52 C49 H49A 108.6 . . ?
N47 C49 H49A 108.6 . . ?
N52 C49 H49B 108.6 . . ?
N47 C49 H49B 108.6 . . ?
H49A C49 H49B 107.6 . . ?
C53 N50 C51 111.8(4) . . ?
C53 N50 C48 121.2(4) . . ?
C51 N50 C48 121.7(4) . . ?
N50 C51 N52 114.5(4) . . ?
N50 C51 C56 103.1(3) . . ?
N52 C51 C56 104.4(3) . . ?
N50 C51 H51 111.4 . . ?
N52 C51 H51 111.4 . . ?
C56 C51 H51 111.4 . . ?
C54 N52 C49 123.7(4) . . ?
C54 N52 C51 111.9(4) . . ?
C49 N52 C51 124.2(4) . . ?
O53 C53 N50 125.4(4) . . ?
O53 C53 N55 125.5(4) . . ?
N50 C53 N55 109.1(4) . . ?
O54 C54 N57 126.1(4) . . ?
O54 C54 N52 125.9(4) . . ?
N57 C54 N52 107.9(4) . . ?
C53 N55 C56 110.0(4) . . ?
C53 N55 C58 119.1(4) . . ?
C56 N55 C58 119.9(4) . . ?
N57 C56 N55 115.1(4) . . ?
N57 C56 C51 102.1(3) . . ?
N55 C56 C51 104.3(3) . . ?
N57 C56 H56 111.6 . . ?
N55 C56 H56 111.6 . . ?
C51 C56 H56 111.6 . . ?
C54 N57 C59 121.0(4) . . ?
C54 N57 C56 113.0(4) . . ?
C59 N57 C56 125.3(4) . . ?
N60 C58 N55 115.5(4) . . ?
N60 C58 H58A 108.4 . . ?
N55 C58 H58A 108.4 . . ?
N60 C58 H58B 108.4 . . ?
N55 C58 H58B 108.4 . . ?
H58A C58 H58B 107.5 . . ?
N57 C59 N12 110.8(4) . 3_666 ?
N57 C59 H59A 109.5 . . ?
N12 C59 H59A 109.5 3_666 . ?
N57 C59 H59B 109.5 . . ?
N12 C59 H59B 109.5 3_666 . ?
H59A C59 H59B 108.1 . . ?
C62 N60 C58 123.7(4) . . ?
C62 N60 C61 112.2(4) . . ?
C58 N60 C61 124.1(4) . . ?
N60 C61 C64 103.4(4) . . ?
N60 C61 H61A 111.1 . . ?
C64 C61 H61A 111.1 . . ?
N60 C61 H61B 111.1 . . ?
C64 C61 H61B 111.1 . . ?
H61A C61 H61B 109.0 . . ?
O62 C62 N63 125.7(4) . . ?
O62 C62 N60 126.2(4) . . ?
N63 C62 N60 108.1(4) . . ?
C62 N63 C65 123.4(4) . . ?
C62 N63 C64 111.5(4) . . ?
C65 N63 C64 124.1(4) . . ?
N63 C64 C61 103.7(4) . . ?
N63 C64 H64A 111.0 . . ?
C61 C64 H64A 111.0 . . ?
N63 C64 H64B 111.0 . . ?
C61 C64 H64B 111.0 . . ?
H64A C64 H64B 109.0 . . ?
N63 C65 N10 113.4(4) . . ?
N63 C65 H65A 108.9 . . ?
N10 C65 H65A 108.9 . . ?
N63 C65 H65B 108.9 . . ?
N10 C65 H65B 108.9 . . ?
H65A C65 H65B 107.7 . . ?
H11W O1W H12W 104(3) . . ?
H21W O2W H22W 110(3) . . ?
H31W O3W H32W 104(3) . . ?
H41W O4W H42W 106(3) . . ?
H51W O5W H52W 106(3) . . ?
H61W O6W H62W 106(3) . . ?
H61W O6W H63W 105(3) . . ?
H62W O6W H63W 114(10) . . ?
H71W O7W H72W 106(3) . . ?
H81W O8W H82W 102(3) . . ?
H91W O9W H92W 107(3) . . ?
H91W O9W H101 101(7) . . ?
H92W O9W H101 69(10) . . ?
H91W O9W H102 166(8) . . ?
H92W O9W H102 60(9) . . ?
H101 O9W H102 71(8) . . ?
H92W O10W H101 57(8) . . ?
H92W O10W H102 75(10) . . ?
H101 O10W H102 106(3) . . ?

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
N1 C1 C2 C3 -20.4(8) . . . . ?
N1 C1 C2 C7 160.7(5) . . . . ?
C7 C2 C3 C4 1.9(8) . . . . ?
C1 C2 C3 C4 -176.9(5) . . . . ?
C2 C3 C4 C5 -0.7(8) . . . . ?
C3 C4 C5 C6 -1.4(8) . . . . ?
C3 C4 C5 C8 178.5(5) . . . . ?
C4 C5 C6 C7 2.4(8) . . . . ?
C8 C5 C6 C7 -177.5(5) . . . . ?
C5 C6 C7 C2 -1.2(8) . . . . ?
C3 C2 C7 C6 -1.0(8) . . . . ?
C1 C2 C7 C6 178.0(5) . . . . ?
C4 C5 C8 N8 -124.6(5) . . . . ?
C6 C5 C8 N8 55.3(7) . . . . ?
C13 N10 C11 N12 117.7(4) . . . . ?
C65 N10 C11 N12 -87.6(5) . . . . ?
C13 N10 C11 C16 6.5(5) . . . . ?
C65 N10 C11 C16 161.2(4) . . . . ?
N10 C11 N12 C14 -116.9(4) . . . . ?
C16 C11 N12 C14 -4.3(5) . . . . ?
N10 C11 N12 C59 80.0(5) . . . 3_666 ?
C16 C11 N12 C59 -167.4(4) . . . 3_666 ?
C11 N10 C13 O13 170.2(4) . . . . ?
C65 N10 C13 O13 14.6(7) . . . . ?
C11 N10 C13 N15 -10.2(5) . . . . ?
C65 N10 C13 N15 -165.8(4) . . . . ?
C11 N12 C14 O14 -171.2(4) . . . . ?
C59 N12 C14 O14 -8.0(7) 3_666 . . . ?
C11 N12 C14 N17 8.7(5) . . . . ?
C59 N12 C14 N17 171.9(4) 3_666 . . . ?
O13 C13 N15 C18 -1.7(7) . . . . ?
N10 C13 N15 C18 178.6(4) . . . . ?
O13 C13 N15 C16 -170.6(4) . . . . ?
N10 C13 N15 C16 9.7(5) . . . . ?
C13 N15 C16 N17 -117.6(4) . . . . ?
C18 N15 C16 N17 73.5(5) . . . . ?
C13 N15 C16 C11 -5.3(5) . . . . ?
C18 N15 C16 C11 -174.2(4) . . . . ?
N12 C11 C16 N17 -1.4(4) . . . . ?
N10 C11 C16 N17 119.5(4) . . . . ?
N12 C11 C16 N15 -121.7(4) . . . . ?
N10 C11 C16 N15 -0.8(4) . . . . ?
O14 C14 N17 C19 5.9(7) . . . . ?
N12 C14 N17 C19 -174.0(4) . . . . ?
O14 C14 N17 C16 170.2(4) . . . . ?
N12 C14 N17 C16 -9.7(5) . . . . ?
N15 C16 N17 C14 118.7(4) . . . . ?
C11 C16 N17 C14 6.9(5) . . . . ?
N15 C16 N17 C19 -77.8(5) . . . . ?
C11 C16 N17 C19 170.4(4) . . . . ?
C13 N15 C18 N20 107.0(5) . . . . ?
C16 N15 C18 N20 -85.3(5) . . . . ?
C14 N17 C19 N22 -108.3(5) . . . . ?
C16 N17 C19 N22 89.3(5) . . . . ?
N15 C18 N20 C23 -101.5(5) . . . . ?
N15 C18 N20 C21 89.9(5) . . . . ?
C23 N20 C21 N22 112.3(4) . . . . ?
C18 N20 C21 N22 -78.0(5) . . . . ?
C23 N20 C21 C26 0.9(5) . . . . ?
C18 N20 C21 C26 170.6(4) . . . . ?
N20 C21 N22 C24 -112.5(4) . . . . ?
C26 C21 N22 C24 -0.9(5) . . . . ?
N20 C21 N22 C19 73.4(5) . . . . ?
C26 C21 N22 C19 -175.0(4) . . . . ?
N17 C19 N22 C24 101.8(5) . . . . ?
N17 C19 N22 C21 -84.8(5) . . . . ?
C18 N20 C23 O23 5.6(8) . . . . ?
C21 N20 C23 O23 175.5(5) . . . . ?
C18 N20 C23 N25 -173.9(4) . . . . ?
C21 N20 C23 N25 -4.1(5) . . . . ?
C21 N22 C24 O24 180.0(5) . . . . ?
C19 N22 C24 O24 -6.0(8) . . . . ?
C21 N22 C24 N27 -0.9(5) . . . . ?
C19 N22 C24 N27 173.2(4) . . . . ?
O23 C23 N25 C26 -173.7(5) . . . . ?
N20 C23 N25 C26 5.9(5) . . . . ?
O23 C23 N25 C28 -11.1(7) . . . . ?
N20 C23 N25 C28 168.5(4) . . . . ?
C23 N25 C26 N27 -116.9(4) . . . . ?
C28 N25 C26 N27 80.7(5) . . . . ?
C23 N25 C26 C21 -5.1(5) . . . . ?
C28 N25 C26 C21 -167.6(4) . . . . ?
N22 C21 C26 N25 -117.6(4) . . . . ?
N20 C21 C26 N25 2.4(4) . . . . ?
N22 C21 C26 N27 2.2(5) . . . . ?
N20 C21 C26 N27 122.3(4) . . . . ?
O24 C24 N27 C26 -178.3(5) . . . . ?
N22 C24 N27 C26 2.5(5) . . . . ?
O24 C24 N27 C29 8.3(8) . . . . ?
N22 C24 N27 C29 -170.8(4) . . . . ?
N25 C26 N27 C24 108.3(4) . . . . ?
C21 C26 N27 C24 -3.0(5) . . . . ?
N25 C26 N27 C29 -78.4(6) . . . . ?
C21 C26 N27 C29 170.3(4) . . . . ?
C23 N25 C28 N30 111.2(5) . . . . ?
C26 N25 C28 N30 -87.9(5) . . . . ?
C24 N27 C29 N32 -104.2(5) . . . . ?
C26 N27 C29 N32 83.2(6) . . . . ?
N25 C28 N30 C33 -109.7(5) . . . . ?
N25 C28 N30 C31 87.1(5) . . . . ?
C33 N30 C31 N32 115.8(4) . . . . ?
C28 N30 C31 N32 -79.6(5) . . . . ?
C33 N30 C31 C36 4.8(5) . . . . ?
C28 N30 C31 C36 169.4(4) . . . . ?
N27 C29 N32 C34 107.0(5) . . . . ?
N27 C29 N32 C31 -84.2(6) . . . . ?
N30 C31 N32 C34 -111.2(5) . . . . ?
C36 C31 N32 C34 -0.4(5) . . . . ?
N30 C31 N32 C29 79.0(6) . . . . ?
C36 C31 N32 C29 -170.2(4) . . . . ?
C28 N30 C33 O33 12.3(7) . . . . ?
C31 N30 C33 O33 177.1(4) . . . . ?
C28 N30 C33 N35 -167.0(4) . . . . ?
C31 N30 C33 N35 -2.2(5) . . . . ?
C29 N32 C34 O34 -6.1(8) . . . . ?
C31 N32 C34 O34 -176.0(5) . . . . ?
C29 N32 C34 N37 174.7(4) . . . . ?
C31 N32 C34 N37 4.8(5) . . . . ?
O33 C33 N35 C36 179.0(4) . . . . ?
N30 C33 N35 C36 -1.7(5) . . . . ?
O33 C33 N35 C38 -1.6(7) . . . . ?
N30 C33 N35 C38 177.7(4) . . . . ?
C33 N35 C36 N37 -107.3(4) . . . . ?
C38 N35 C36 N37 73.3(5) . . . . ?
C33 N35 C36 C31 4.5(5) . . . . ?
C38 N35 C36 C31 -174.9(4) . . . . ?
N30 C31 C36 N35 -5.3(4) . . . . ?
N32 C31 C36 N35 -124.4(4) . . . . ?
N30 C31 C36 N37 115.4(4) . . . . ?
N32 C31 C36 N37 -3.8(4) . . . . ?
O34 C34 N37 C39 6.0(8) . . . . ?
N32 C34 N37 C39 -174.7(4) . . . . ?
O34 C34 N37 C36 173.3(5) . . . . ?
N32 C34 N37 C36 -7.5(5) . . . . ?
N35 C36 N37 C34 118.8(4) . . . . ?
C31 C36 N37 C34 7.0(5) . . . . ?
N35 C36 N37 C39 -74.3(6) . . . . ?
C31 C36 N37 C39 173.9(4) . . . . ?
C33 N35 C38 N40 94.4(5) . . . . ?
C36 N35 C38 N40 -86.2(5) . . . . ?
C34 N37 C39 N42 -106.6(5) . . . . ?
C36 N37 C39 N42 87.7(5) . . . . ?
N35 C38 N40 C43 -97.1(5) . . . . ?
N35 C38 N40 C41 88.0(5) . . . . ?
C43 N40 C41 N42 108.8(4) . . . . ?
C38 N40 C41 N42 -75.8(5) . . . . ?
C43 N40 C41 C46 -3.0(5) . . . . ?
C38 N40 C41 C46 172.4(4) . . . . ?
N37 C39 N42 C44 108.1(5) . . . . ?
N37 C39 N42 C41 -88.1(5) . . . . ?
N40 C41 N42 C44 -119.8(4) . . . . ?
C46 C41 N42 C44 -7.9(5) . . . . ?
N40 C41 N42 C39 75.0(5) . . . . ?
C46 C41 N42 C39 -173.1(4) . . . . ?
C38 N40 C43 O43 3.7(7) . . . . ?
C41 N40 C43 O43 179.1(4) . . . . ?
C38 N40 C43 N45 -175.0(4) . . . . ?
C41 N40 C43 N45 0.4(5) . . . . ?
C39 N42 C44 O44 -6.5(7) . . . . ?
C41 N42 C44 O44 -172.1(4) . . . . ?
C39 N42 C44 N47 173.2(4) . . . . ?
C41 N42 C44 N47 7.6(5) . . . . ?
O43 C43 N45 C48 -1.0(7) . . . . ?
N40 C43 N45 C48 177.7(4) . . . . ?
O43 C43 N45 C46 -176.0(4) . . . . ?
N40 C43 N45 C46 2.7(5) . . . . ?
C43 N45 C46 N47 -115.9(4) . . . . ?
C48 N45 C46 N47 69.2(6) . . . . ?
C43 N45 C46 C41 -4.3(5) . . . . ?
C48 N45 C46 C41 -179.2(4) . . . . ?
N40 C41 C46 N45 4.1(4) . . . . ?
N42 C41 C46 N45 -115.6(4) . . . . ?
N40 C41 C46 N47 124.8(4) . . . . ?
N42 C41 C46 N47 5.1(4) . . . . ?
O44 C44 N47 C49 1.2(7) . . . . ?
N42 C44 N47 C49 -178.5(4) . . . . ?
O44 C44 N47 C46 175.8(4) . . . . ?
N42 C44 N47 C46 -3.9(5) . . . . ?
N45 C46 N47 C44 110.4(4) . . . . ?
C41 C46 N47 C44 -0.9(5) . . . . ?
N45 C46 N47 C49 -75.1(5) . . . . ?
C41 C46 N47 C49 173.5(4) . . . . ?
C43 N45 C48 N50 101.4(5) . . . . ?
C46 N45 C48 N50 -84.2(5) . . . . ?
C44 N47 C49 N52 -96.7(5) . . . . ?
C46 N47 C49 N52 89.3(5) . . . . ?
N45 C48 N50 C53 -113.6(5) . . . . ?
N45 C48 N50 C51 94.0(5) . . . . ?
C53 N50 C51 N52 123.9(4) . . . . ?
C48 N50 C51 N52 -81.4(5) . . . . ?
C53 N50 C51 C56 11.1(5) . . . . ?
C48 N50 C51 C56 165.8(4) . . . . ?
N47 C49 N52 C54 102.0(5) . . . . ?
N47 C49 N52 C51 -83.3(5) . . . . ?
N50 C51 N52 C54 -111.8(4) . . . . ?
C56 C51 N52 C54 0.2(5) . . . . ?
N50 C51 N52 C49 72.9(5) . . . . ?
C56 C51 N52 C49 -175.1(4) . . . . ?
C51 N50 C53 O53 166.9(5) . . . . ?
C48 N50 C53 O53 12.1(7) . . . . ?
C51 N50 C53 N55 -13.5(5) . . . . ?
C48 N50 C53 N55 -168.3(4) . . . . ?
C49 N52 C54 O54 1.0(7) . . . . ?
C51 N52 C54 O54 -174.3(4) . . . . ?
C49 N52 C54 N57 180.0(4) . . . . ?
C51 N52 C54 N57 4.7(5) . . . . ?
O53 C53 N55 C56 -170.6(5) . . . . ?
N50 C53 N55 C56 9.8(5) . . . . ?
O53 C53 N55 C58 -26.5(7) . . . . ?
N50 C53 N55 C58 153.9(4) . . . . ?
C53 N55 C56 N57 -113.7(4) . . . . ?
C58 N55 C56 N57 102.5(5) . . . . ?
C53 N55 C56 C51 -2.7(5) . . . . ?
C58 N55 C56 C51 -146.5(4) . . . . ?
N50 C51 C56 N57 115.4(4) . . . . ?
N52 C51 C56 N57 -4.6(4) . . . . ?
N50 C51 C56 N55 -4.8(4) . . . . ?
N52 C51 C56 N55 -124.8(4) . . . . ?
O54 C54 N57 C59 -0.1(7) . . . . ?
N52 C54 N57 C59 -179.1(4) . . . . ?
O54 C54 N57 C56 170.8(4) . . . . ?
N52 C54 N57 C56 -8.1(5) . . . . ?
N55 C56 N57 C54 120.2(4) . . . . ?
C51 C56 N57 C54 7.9(5) . . . . ?
N55 C56 N57 C59 -69.3(6) . . . . ?
C51 C56 N57 C59 178.4(4) . . . . ?
C53 N55 C58 N60 75.7(5) . . . . ?
C56 N55 C58 N60 -143.8(4) . . . . ?
C54 N57 C59 N12 93.3(5) . . . 3_666 ?
C56 N57 C59 N12 -76.5(5) . . . 3_666 ?
N55 C58 N60 C62 83.7(6) . . . . ?
N55 C58 N60 C61 -98.2(6) . . . . ?
C62 N60 C61 C64 -0.4(6) . . . . ?
C58 N60 C61 C64 -178.8(5) . . . . ?
C58 N60 C62 O62 4.5(8) . . . . ?
C61 N60 C62 O62 -173.9(5) . . . . ?
C58 N60 C62 N63 -174.8(4) . . . . ?
C61 N60 C62 N63 6.9(6) . . . . ?
O62 C62 N63 C65 1.0(8) . . . . ?
N60 C62 N63 C65 -179.7(4) . . . . ?
O62 C62 N63 C64 169.9(5) . . . . ?
N60 C62 N63 C64 -10.8(6) . . . . ?
C62 N63 C64 C61 10.2(6) . . . . ?
C65 N63 C64 C61 179.0(5) . . . . ?
N60 C61 C64 N63 -5.6(6) . . . . ?
C62 N63 C65 N10 -89.1(5) . . . . ?
C64 N63 C65 N10 103.4(5) . . . . ?
C13 N10 C65 N63 -71.7(5) . . . . ?
C11 N10 C65 N63 136.1(4) . . . . ?

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 O43 0.90 2.18 2.865(6) 132 .
N1 H1A O53 0.90 2.37 3.008(7) 128 .
N1 H1B O3W 0.90 1.92 2.797(6) 166 1_455
N1 H1C O33 0.90 2.11 2.973(6) 161 .
N8 H8C O14 0.90 2.23 2.847(6) 125 .
N8 H8D O2W 0.90 1.88 2.772(6) 172 .
N8 H8E O24 0.90 1.93 2.821(6) 170 .
O1W H11W O33 0.826(13) 2.164(19) 2.982(5) 171(7) .
O1W H12W O8W 0.819(13) 2.09(3) 2.869(9) 160(8) 2_556
O2W H21W O7W 0.820(13) 2.17(5) 2.846(8) 139(7) .
O2W H22W O4W 0.818(13) 1.95(3) 2.731(7) 161(8) .
O3W H31W O5W 0.822(13) 1.995(17) 2.810(7) 171(7) 3_666
O3W H32W O10W 0.825(13) 1.84(3) 2.66(2) 174(7) .
O3W H32W O9W 0.825(13) 1.98(2) 2.786(11) 165(7) .
O4W H41W O13 0.821(13) 1.999(18) 2.816(5) 173(8) 1_655
O4W H42W O10W 0.818(13) 1.88(6) 2.58(3) 144(9) .
O4W H42W O9W 0.818(13) 2.42(7) 3.047(15) 134(8) .
O5W H51W I1 0.820(13) 2.98(4) 3.711(5) 150(6) 3_666
O5W H52W I2 0.820(13) 2.689(17) 3.506(5) 174(8) 3_566
O6W H61W O23 0.825(13) 2.036(14) 2.861(6) 178(10) 1_655
O6W H62W O7W 0.825(13) 2.13(4) 2.851(9) 145(7) .
O6W H63W O10W 0.823(13) 2.6(3) 3.11(3) 119(24) .
O7W H71W O34 0.821(13) 2.05(4) 2.835(6) 159(10) .
O7W H72W I1 0.818(13) 2.92(5) 3.632(5) 146(7) 1_565
O8W H81W I1 0.827(13) 2.77(3) 3.568(6) 163(10) .
O8W H82W O9W 0.830(13) 2.43(5) 2.993(15) 126(5) 2_646
O9W H91W O6W 0.821(13) 1.93(3) 2.627(14) 143(4) .
O9W H92W O44 0.820(13) 1.94(5) 2.709(10) 156(11) .
O10W H101 O44 0.821(13) 2.49(8) 2.93(2) 115(6) .
O10W H102 O54 0.821(13) 2.05(7) 2.84(2) 162(22) .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.092

_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0533562
_diffrn_orient_matrix_UB_12      -0.0489077
_diffrn_orient_matrix_UB_13      -0.0004118
_diffrn_orient_matrix_UB_21      -0.0374951
_diffrn_orient_matrix_UB_22      0.0372221
_diffrn_orient_matrix_UB_23      -0.0236646
_diffrn_orient_matrix_UB_31      0.0331509
_diffrn_orient_matrix_UB_32      -0.0366711
_diffrn_orient_matrix_UB_33      -0.0234413
_symmetry_space_group_name_Hall  '-P 2yn'
_exptl_crystal_id                'Isaacs/Wittenberg JW-3-138 @250K'
_diffrn_measurement_frame_width-CCD -0.30
_diffrn_measurement_details      610,610,310
_diffrn_measurement_total_frames-CCD 1330
_diffrn_measurement_frame_time-CCD 20
_diffrn_measurement_total_time-CCD 10
_diffrn_source_voltage           50.00
_diffrn_source_current           30.00
_diffrn_detector_distance-CCD    6.000
_diffrn_measurement_frame_size-CCD 512
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker Smart Apex II'

#_______________________________________________________________________________
#
_publ_section_references         
;
Bruker (2005). Apex2. Bruker AXS Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473.

Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.

Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany.

Spek, A. L. (1990). Acta Cryst., A46, C-34.
;