# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'A K Powell'
_publ_contact_author_email       POWELL@AOC.UNI-KARLSRUHE.DE

_publ_section_title              
;
Inclusion of a well resolved T4(2)6(2) water tape in a
H-bonded, pi - stacked 3D framework with a seh topology
;
loop_
_publ_author_name
'A K Powell'
'Ghulam Abbas'
'Christopher E. Anson'
'George E Kostakis'

# Attachment 'tetrazole_watertape.cif'

data_26103
_database_code_depnum_ccdc_archive 'CCDC 693449'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H21 Ce N8 O8, C8 H4 N8, 12(H2 O)'
_chemical_formula_sum            'C16 H49 Ce N16 O20'
_chemical_formula_weight         925.83

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   11.2155(5)
_cell_length_b                   28.9919(13)
_cell_length_c                   11.9052(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.216(1)
_cell_angle_gamma                90.00
_cell_volume                     3608.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14506
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.03

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1900
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2005)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18231
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         25.68
_reflns_number_total             6787
_reflns_number_gt                6042
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_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.
One of the lattice water molecules was disordered and refined as two
isotropic half oxygen atoms, O(22A) and O(22B), and no attempt was made
to locate the hydrogens on this water.
Geometrical restraints were applied to the water hydrogen atoms, mainly to
the O-H distances.
;

_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)+(0.0287P)²+18.2612P] 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         6787
_refine_ls_number_parameters     594
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.070
_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
Ce1 Ce 0.30601(2) 0.431273(8) 0.53611(2) 0.00858(7) Uani 1 1 d . . .
O1 O 0.4228(3) 0.42006(11) 0.7569(3) 0.0176(7) Uani 1 1 d D . .
H11 H 0.504(3) 0.4247(18) 0.772(5) 0.026 Uiso 1 1 d D . .
H12 H 0.390(5) 0.4108(18) 0.805(4) 0.026 Uiso 1 1 d D . .
O2 O 0.1537(3) 0.43190(11) 0.6427(3) 0.0171(6) Uani 1 1 d D . .
H21 H 0.120(5) 0.4123(16) 0.674(5) 0.026 Uiso 1 1 d D . .
H22 H 0.143(5) 0.4585(14) 0.669(5) 0.026 Uiso 1 1 d D . .
O3 O 0.3178(3) 0.34965(11) 0.5910(3) 0.0157(7) Uani 1 1 d D . .
H31 H 0.360(5) 0.3391(17) 0.660(3) 0.024 Uiso 1 1 d D . .
H32 H 0.287(5) 0.3311(16) 0.534(4) 0.024 Uiso 1 1 d D . .
O4 O 0.5400(3) 0.43248(11) 0.5802(3) 0.0151(6) Uani 1 1 d D . .
H41 H 0.590(4) 0.4147(16) 0.563(5) 0.023 Uiso 1 1 d D . .
H42 H 0.573(5) 0.4592(13) 0.595(5) 0.023 Uiso 1 1 d D . .
O5 O 0.3776(3) 0.50680(11) 0.6444(3) 0.0185(7) Uani 1 1 d D . .
H51 H 0.344(5) 0.5337(14) 0.618(5) 0.028 Uiso 1 1 d D . .
H52 H 0.417(5) 0.5068(19) 0.722(3) 0.028 Uiso 1 1 d D . .
O6 O 0.3422(3) 0.48198(10) 0.3724(3) 0.0141(6) Uani 1 1 d D . .
H61 H 0.272(4) 0.4857(18) 0.311(4) 0.021 Uiso 1 1 d D . .
H62 H 0.391(4) 0.4667(16) 0.344(4) 0.021 Uiso 1 1 d D . .
O7 O 0.1383(3) 0.49382(11) 0.4518(3) 0.0173(7) Uani 1 1 d D . .
H71 H 0.063(4) 0.4875(18) 0.399(4) 0.026 Uiso 1 1 d D . .
H72 H 0.150(5) 0.5228(12) 0.465(5) 0.026 Uiso 1 1 d D . .
O8 O 0.1084(3) 0.39601(11) 0.3937(3) 0.0166(7) Uani 1 1 d D . .
H81 H 0.093(5) 0.3954(18) 0.320(3) 0.025 Uiso 1 1 d D . .
H82 H 0.039(4) 0.3955(18) 0.408(5) 0.025 Uiso 1 1 d D . .
C1 C 0.4940(4) 0.28984(14) 0.2359(4) 0.0113(8) Uani 1 1 d . . .
C2 C 0.4558(4) 0.24718(14) 0.2657(4) 0.0110(8) Uani 1 1 d . . .
H2A H 0.3991 0.2459 0.3086 0.013 Uiso 1 1 calc R . .
C3 C 0.5007(4) 0.20652(14) 0.2327(4) 0.0104(8) Uani 1 1 d . . .
C4 C 0.5862(4) 0.20823(14) 0.1719(4) 0.0133(9) Uani 1 1 d . . .
H4A H 0.6189 0.1806 0.1513 0.016 Uiso 1 1 calc R . .
C5 C 0.6230(4) 0.25071(15) 0.1419(4) 0.0173(9) Uani 1 1 d . . .
H5A H 0.6802 0.2520 0.0996 0.021 Uiso 1 1 calc R . .
C6 C 0.5775(4) 0.29119(15) 0.1728(4) 0.0140(9) Uani 1 1 d . . .
H6A H 0.6031 0.3200 0.1510 0.017 Uiso 1 1 calc R . .
C7 C 0.4507(4) 0.33341(14) 0.2727(4) 0.0107(8) Uani 1 1 d . . .
N1 N 0.4907(3) 0.37516(12) 0.2532(3) 0.0122(7) Uani 1 1 d . . .
N2 N 0.4346(3) 0.40490(12) 0.3040(3) 0.0127(7) Uani 1 1 d . . .
N3 N 0.3641(3) 0.38232(12) 0.3535(3) 0.0137(8) Uani 1 1 d . . .
N4 N 0.3720(3) 0.33668(12) 0.3346(3) 0.0120(7) Uani 1 1 d . . .
C8 C 0.4621(4) 0.16134(14) 0.2632(4) 0.0105(8) Uani 1 1 d . . .
N5 N 0.3747(3) 0.15332(12) 0.3124(3) 0.0119(7) Uani 1 1 d D . .
H5 H 0.326(4) 0.1713(15) 0.332(4) 0.014 Uiso 1 1 d D . .
N6 N 0.3658(4) 0.10785(12) 0.3269(3) 0.0149(8) Uani 1 1 d . . .
N7 N 0.4468(3) 0.08839(12) 0.2865(3) 0.0140(8) Uani 1 1 d . . .
N8 N 0.5085(3) 0.12081(12) 0.2460(3) 0.0124(7) Uani 1 1 d . . .
C9 C 0.2018(4) 0.20304(14) 0.0197(3) 0.0080(8) Uani 1 1 d U . .
C10 C 0.2439(4) 0.24600(14) -0.0043(4) 0.0116(8) Uani 1 1 d . . .
H10A H 0.3069 0.2476 -0.0402 0.014 Uiso 1 1 calc R . .
C11 C 0.1943(4) 0.28645(14) 0.0238(4) 0.0102(8) Uani 1 1 d . . .
C12 C 0.1011(4) 0.28402(15) 0.0761(4) 0.0138(9) Uani 1 1 d . . .
H12A H 0.0671 0.3116 0.0957 0.017 Uiso 1 1 calc R . .
C13 C 0.0586(4) 0.24174(16) 0.0996(4) 0.0175(9) Uani 1 1 d . . .
H13A H -0.0053 0.2404 0.1344 0.021 Uiso 1 1 calc R . .
C14 C 0.1086(4) 0.20103(15) 0.0724(4) 0.0137(9) Uani 1 1 d . . .
H14A H 0.0796 0.1720 0.0896 0.016 Uiso 1 1 calc R . .
C15 C 0.2548(4) 0.15963(13) -0.0080(4) 0.0095(8) Uani 1 1 d . . .
N9 N 0.2214(3) 0.11768(12) 0.0155(3) 0.0128(7) Uani 1 1 d . . .
N10 N 0.2941(3) 0.08853(12) -0.0209(3) 0.0141(8) Uani 1 1 d . . .
N11 N 0.3678(4) 0.11250(12) -0.0643(3) 0.0145(8) Uani 1 1 d . . .
N12 N 0.3448(3) 0.15765(12) -0.0571(3) 0.0121(7) Uani 1 1 d . . .
C16 C 0.2378(4) 0.33205(14) -0.0021(4) 0.0096(8) Uani 1 1 d . . .
N13 N 0.3154(3) 0.33887(12) -0.0636(3) 0.0124(7) Uani 1 1 d . . .
N14 N 0.3281(4) 0.38494(12) -0.0681(3) 0.0158(8) Uani 1 1 d . . .
N15 N 0.2605(4) 0.40470(12) -0.0108(3) 0.0144(8) Uani 1 1 d . . .
N16 N 0.2025(3) 0.37222(12) 0.0317(3) 0.0123(7) Uani 1 1 d . . .
O11 O 0.2156(3) 0.28619(10) 0.4137(3) 0.0147(6) Uani 1 1 d D . .
H111 H 0.258(5) 0.3017(16) 0.381(4) 0.022 Uiso 1 1 d D . .
H112 H 0.140(3) 0.2930(18) 0.375(4) 0.022 Uiso 1 1 d D . .
O12 O 0.2156(3) 0.19410(11) 0.4032(3) 0.0153(6) Uani 1 1 d D . .
H121 H 0.250(5) 0.1808(17) 0.469(4) 0.023 Uiso 1 1 d D . .
H122 H 0.224(5) 0.2233(12) 0.407(5) 0.023 Uiso 1 1 d D . .
O13 O 0.6691(3) 0.42726(12) 0.9112(3) 0.0266(8) Uani 1 1 d D . .
H131 H 0.731(5) 0.416(2) 0.891(5) 0.040 Uiso 1 1 d D . .
H132 H 0.699(6) 0.4527(15) 0.944(5) 0.040 Uiso 1 1 d D . .
O14 O 0.4432(3) 0.30236(11) 0.8008(3) 0.0144(6) Uani 1 1 d D . .
H141 H 0.521(3) 0.3085(18) 0.838(4) 0.022 Uiso 1 1 d D . .
H142 H 0.407(5) 0.3118(18) 0.847(4) 0.022 Uiso 1 1 d D . .
O15 O 0.9539(3) 0.29337(11) 0.3078(3) 0.0167(7) Uani 1 1 d D . .
H151 H 0.926(5) 0.3057(18) 0.358(4) 0.025 Uiso 1 1 d D . .
H152 H 0.942(5) 0.2653(12) 0.307(5) 0.025 Uiso 1 1 d D . .
O16 O 0.1273(3) 0.49647(11) 0.1711(3) 0.0203(7) Uani 1 1 d D . .
H161 H 0.087(5) 0.4708(14) 0.167(5) 0.031 Uiso 1 1 d D . .
H162 H 0.083(5) 0.5199(16) 0.186(5) 0.031 Uiso 1 1 d D . .
O17 O 0.0485(3) 0.40635(11) 0.1510(3) 0.0167(7) Uani 1 1 d D . .
H171 H -0.021(4) 0.3909(17) 0.127(5) 0.025 Uiso 1 1 d D . .
H172 H 0.091(5) 0.3938(18) 0.113(5) 0.025 Uiso 1 1 d D . .
O18 O 0.1745(4) 0.49592(13) 0.9558(4) 0.0375(10) Uani 1 1 d D . .
H181 H 0.206(6) 0.4681(15) 0.961(6) 0.056 Uiso 1 1 d D . .
H182 H 0.141(6) 0.501(2) 1.010(5) 0.056 Uiso 1 1 d D . .
O19 O 0.8357(3) 0.34989(11) 0.1166(3) 0.0189(7) Uani 1 1 d D . .
H191 H 0.874(5) 0.3311(17) 0.173(4) 0.028 Uiso 1 1 d D . .
H192 H 0.794(5) 0.3705(16) 0.139(5) 0.028 Uiso 1 1 d D . .
O20 O 0.8908(3) 0.48054(11) 0.2789(3) 0.0217(7) Uani 1 1 d D . .
H201 H 0.862(5) 0.485(2) 0.201(3) 0.033 Uiso 1 1 d D . .
H202 H 0.848(5) 0.4562(15) 0.281(5) 0.033 Uiso 1 1 d D . .
O21 O 0.6772(3) 0.41132(12) 0.1670(3) 0.0246(8) Uani 1 1 d D . .
H211 H 0.630(5) 0.3963(19) 0.196(5) 0.037 Uiso 1 1 d D . .
H212 H 0.627(5) 0.4263(19) 0.111(4) 0.037 Uiso 1 1 d D . .
O22A O 0.5473(8) 0.5152(3) 0.8826(7) 0.0300(17) Uiso 0.50 1 d P A 1
O22B O 0.5023(8) 0.5187(3) 0.9141(7) 0.0319(18) Uiso 0.50 1 d P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O3 2.446(3) . ?
Ce1 O2 2.470(3) . ?
Ce1 O8 2.472(3) . ?
Ce1 O4 2.483(3) . ?
Ce1 O1 2.498(3) . ?
Ce1 O5 2.521(3) . ?
Ce1 O7 2.543(3) . ?
Ce1 O6 2.588(3) . ?
Ce1 N3 2.862(4) . ?
O1 H11 0.87(3) . ?
O1 H12 0.83(3) . ?
O2 H21 0.84(3) . ?
O2 H22 0.86(3) . ?
O3 H31 0.84(3) . ?
O3 H32 0.83(3) . ?
O4 H41 0.84(3) . ?
O4 H42 0.85(3) . ?
O5 H51 0.87(3) . ?
O5 H52 0.86(3) . ?
O6 H61 0.87(3) . ?
O6 H62 0.86(3) . ?
O7 H71 0.87(3) . ?
O7 H72 0.86(3) . ?
O8 H81 0.84(3) . ?
O8 H82 0.86(3) . ?
C1 C2 1.396(6) . ?
C1 C6 1.398(6) . ?
C1 C7 1.476(6) . ?
C2 C3 1.393(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.396(6) . ?
C3 C8 1.466(6) . ?
C4 C5 1.386(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.381(6) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 N1 1.340(5) . ?
C7 N4 1.342(5) . ?
N1 N2 1.334(5) . ?
N2 N3 1.318(5) . ?
N3 N4 1.350(5) . ?
C8 N8 1.331(5) . ?
C8 N5 1.331(5) . ?
N5 N6 1.338(5) . ?
N5 H5 0.84(3) . ?
N6 N7 1.300(5) . ?
N7 N8 1.355(5) . ?
C9 C10 1.398(6) . ?
C9 C14 1.401(6) . ?
C9 C15 1.479(5) . ?
C10 C11 1.389(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.399(6) . ?
C11 C16 1.479(6) . ?
C12 C13 1.380(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.394(6) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 N9 1.332(5) . ?
C15 N12 1.338(5) . ?
N9 N10 1.350(5) . ?
N10 N11 1.320(5) . ?
N11 N12 1.343(5) . ?
C16 N16 1.338(5) . ?
C16 N13 1.340(5) . ?
N13 N14 1.346(5) . ?
N14 N15 1.319(5) . ?
N15 N16 1.343(5) . ?
O11 H111 0.84(3) . ?
O11 H112 0.83(3) . ?
O12 H121 0.83(3) . ?
O12 H122 0.85(3) . ?
O13 H131 0.87(4) . ?
O13 H132 0.85(4) . ?
O14 H141 0.84(3) . ?
O14 H142 0.83(3) . ?
O15 H151 0.85(3) . ?
O15 H152 0.82(3) . ?
O16 H161 0.86(3) . ?
O16 H162 0.89(3) . ?
O17 H171 0.85(3) . ?
O17 H172 0.85(3) . ?
O18 H181 0.87(4) . ?
O18 H182 0.87(4) . ?
O19 H191 0.85(3) . ?
O19 H192 0.86(3) . ?
O20 H201 0.87(3) . ?
O20 H202 0.86(3) . ?
O21 H211 0.85(4) . ?
O21 H212 0.82(3) . ?

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
O3 Ce1 O2 81.38(11) . . ?
O3 Ce1 O8 74.43(11) . . ?
O2 Ce1 O8 74.96(11) . . ?
O3 Ce1 O4 90.37(11) . . ?
O2 Ce1 O4 139.98(10) . . ?
O8 Ce1 O4 140.11(10) . . ?
O3 Ce1 O1 68.63(10) . . ?
O2 Ce1 O1 69.92(11) . . ?
O8 Ce1 O1 131.79(11) . . ?
O4 Ce1 O1 70.60(10) . . ?
O3 Ce1 O5 136.66(11) . . ?
O2 Ce1 O5 83.24(11) . . ?
O8 Ce1 O5 138.66(11) . . ?
O4 Ce1 O5 76.27(10) . . ?
O1 Ce1 O5 68.04(11) . . ?
O3 Ce1 O7 139.12(11) . . ?
O2 Ce1 O7 69.34(11) . . ?
O8 Ce1 O7 70.90(11) . . ?
O4 Ce1 O7 130.36(10) . . ?
O1 Ce1 O7 122.63(11) . . ?
O5 Ce1 O7 68.64(11) . . ?
O3 Ce1 O6 137.98(10) . . ?
O2 Ce1 O6 135.16(10) . . ?
O8 Ce1 O6 93.68(10) . . ?
O4 Ce1 O6 73.11(10) . . ?
O1 Ce1 O6 134.53(10) . . ?
O5 Ce1 O6 77.53(10) . . ?
O7 Ce1 O6 65.98(10) . . ?
O3 Ce1 N3 73.63(10) . . ?
O2 Ce1 N3 141.63(11) . . ?
O8 Ce1 N3 70.60(11) . . ?
O4 Ce1 N3 69.76(10) . . ?
O1 Ce1 N3 123.93(11) . . ?
O5 Ce1 N3 134.54(11) . . ?
O7 Ce1 N3 113.14(10) . . ?
O6 Ce1 N3 64.44(10) . . ?
Ce1 O1 H11 108(4) . . ?
Ce1 O1 H12 125(4) . . ?
H11 O1 H12 127(5) . . ?
Ce1 O2 H21 137(4) . . ?
Ce1 O2 H22 114(4) . . ?
H21 O2 H22 107(5) . . ?
Ce1 O3 H31 125(4) . . ?
Ce1 O3 H32 116(4) . . ?
H31 O3 H32 118(5) . . ?
Ce1 O4 H41 133(4) . . ?
Ce1 O4 H42 114(4) . . ?
H41 O4 H42 109(5) . . ?
Ce1 O5 H51 125(4) . . ?
Ce1 O5 H52 119(4) . . ?
H51 O5 H52 112(5) . . ?
Ce1 O6 H61 111(3) . . ?
Ce1 O6 H62 107(3) . . ?
H61 O6 H62 104(5) . . ?
Ce1 O7 H71 121(4) . . ?
Ce1 O7 H72 126(4) . . ?
H71 O7 H72 113(5) . . ?
Ce1 O8 H81 121(4) . . ?
Ce1 O8 H82 122(4) . . ?
H81 O8 H82 111(5) . . ?
C2 C1 C6 119.2(4) . . ?
C2 C1 C7 121.3(4) . . ?
C6 C1 C7 119.5(4) . . ?
C3 C2 C1 120.2(4) . . ?
C3 C2 H2A 119.9 . . ?
C1 C2 H2A 119.9 . . ?
C2 C3 C4 120.1(4) . . ?
C2 C3 C8 121.1(4) . . ?
C4 C3 C8 118.7(4) . . ?
C5 C4 C3 119.3(4) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
C6 C5 C4 120.9(4) . . ?
C6 C5 H5A 119.5 . . ?
C4 C5 H5A 119.5 . . ?
C5 C6 C1 120.2(4) . . ?
C5 C6 H6A 119.9 . . ?
C1 C6 H6A 119.9 . . ?
N1 C7 N4 111.0(4) . . ?
N1 C7 C1 123.7(4) . . ?
N4 C7 C1 125.2(4) . . ?
N2 N1 C7 105.2(3) . . ?
N3 N2 N1 109.8(3) . . ?
N2 N3 N4 109.0(3) . . ?
N2 N3 Ce1 115.5(2) . . ?
N4 N3 Ce1 131.2(3) . . ?
C7 N4 N3 104.9(3) . . ?
N8 C8 N5 107.8(4) . . ?
N8 C8 C3 125.7(4) . . ?
N5 C8 C3 126.5(4) . . ?
C8 N5 N6 109.2(3) . . ?
C8 N5 H5 132(3) . . ?
N6 N5 H5 119(3) . . ?
N7 N6 N5 106.6(3) . . ?
N6 N7 N8 110.2(3) . . ?
C8 N8 N7 106.2(3) . . ?
C10 C9 C14 119.4(4) . . ?
C10 C9 C15 121.3(4) . . ?
C14 C9 C15 119.3(4) . . ?
C11 C10 C9 120.6(4) . . ?
C11 C10 H10A 119.7 . . ?
C9 C10 H10A 119.7 . . ?
C10 C11 C12 119.6(4) . . ?
C10 C11 C16 120.9(4) . . ?
C12 C11 C16 119.5(4) . . ?
C13 C12 C11 120.2(4) . . ?
C13 C12 H12A 119.9 . . ?
C11 C12 H12A 119.9 . . ?
C12 C13 C14 120.5(4) . . ?
C12 C13 H13A 119.8 . . ?
C14 C13 H13A 119.8 . . ?
C13 C14 C9 119.8(4) . . ?
C13 C14 H14A 120.1 . . ?
C9 C14 H14A 120.1 . . ?
N9 C15 N12 111.5(4) . . ?
N9 C15 C9 124.3(4) . . ?
N12 C15 C9 124.2(4) . . ?
C15 N9 N10 104.8(3) . . ?
N11 N10 N9 109.4(3) . . ?
N10 N11 N12 109.0(3) . . ?
C15 N12 N11 105.2(3) . . ?
N16 C16 N13 110.9(4) . . ?
N16 C16 C11 124.0(4) . . ?
N13 C16 C11 125.0(4) . . ?
C16 N13 N14 105.5(3) . . ?
N15 N14 N13 108.8(3) . . ?
N14 N15 N16 109.7(3) . . ?
C16 N16 N15 105.1(3) . . ?
H111 O11 H112 104(5) . . ?
H121 O12 H122 114(5) . . ?
H131 O13 H132 104(6) . . ?
H141 O14 H142 104(5) . . ?
H151 O15 H152 109(5) . . ?
H161 O16 H162 110(5) . . ?
H171 O17 H172 102(5) . . ?
H181 O18 H182 112(6) . . ?
H191 O19 H192 112(5) . . ?
H201 O20 H202 100(5) . . ?
H211 O21 H212 105(6) . . ?

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
O1 H11 O13 0.87(3) 1.99(4) 2.716(5) 139(5) .
O1 H12 N14 0.83(3) 2.02(4) 2.847(5) 174(6) 1_556
O2 H21 N8 0.84(3) 2.00(4) 2.819(5) 165(5) 4_566
O2 H22 O20 0.86(3) 1.95(3) 2.811(5) 176(5) 3_666
O3 H31 O14 0.84(3) 1.92(4) 2.748(4) 167(5) .
O3 H32 O11 0.83(3) 1.89(3) 2.721(4) 176(5) .
O4 H41 N9 0.84(3) 1.99(4) 2.826(5) 170(5) 4_666
O4 H42 O6 0.85(3) 1.92(3) 2.771(4) 176(5) 3_666
O5 H51 N10 0.87(3) 2.23(4) 3.072(5) 162(5) 2
O5 H52 O22A 0.86(3) 1.96(4) 2.795(8) 163(5) .
O5 H52 O22B 0.86(3) 2.17(4) 3.022(9) 170(5) .
O6 H61 O16 0.87(3) 1.88(3) 2.747(5) 175(5) .
O6 H62 N2 0.86(3) 1.96(4) 2.709(5) 145(5) .
O7 H71 O20 0.87(3) 1.96(3) 2.821(5) 174(5) 1_455
O7 H72 N10 0.86(3) 2.04(4) 2.888(5) 170(5) 2
O8 H81 O17 0.84(3) 1.91(4) 2.735(5) 169(5) .
O8 H82 N11 0.86(3) 2.07(4) 2.927(5) 174(5) 4_566
N5 H5 O12 0.84(3) 1.86(4) 2.674(5) 161(5) .
O11 H111 N4 0.84(3) 1.87(4) 2.703(5) 170(5) .
O11 H112 O15 0.83(3) 1.95(4) 2.751(5) 163(5) 1_455
O12 H121 O19 0.83(3) 1.89(3) 2.724(5) 177(5) 4_566
O12 H122 O11 0.85(3) 1.83(3) 2.673(4) 171(5) .
O13 H131 N6 0.87(4) 2.05(4) 2.918(5) 174(6) 4_666
O13 H132 O18 0.85(4) 2.10(4) 2.921(6) 162(6) 3_667
O14 H141 O12 0.84(3) 2.03(4) 2.852(5) 163(5) 4_666
O14 H142 N13 0.83(3) 1.90(3) 2.731(5) 173(5) 1_556
O15 H151 N12 0.85(3) 1.91(4) 2.743(5) 168(5) 4_666
O15 H152 O14 0.82(3) 1.96(4) 2.778(4) 170(5) 4_665
O16 H161 O17 0.86(3) 1.91(4) 2.741(5) 160(5) .
O16 H162 N7 0.89(3) 2.06(4) 2.890(5) 154(5) 2
O17 H171 O19 0.85(3) 1.97(4) 2.799(5) 164(5) 1_455
O17 H172 N16 0.85(3) 1.94(4) 2.785(5) 173(5) .
O18 H181 N15 0.87(4) 1.93(4) 2.794(5) 171(7) 1_556
O18 H182 O16 0.87(4) 1.98(4) 2.798(5) 156(7) 1_556
O19 H191 O15 0.85(3) 1.88(4) 2.728(5) 174(6) .
O19 H192 O21 0.86(3) 1.89(4) 2.732(5) 170(5) .
O20 H201 O18 0.87(3) 1.84(4) 2.707(6) 169(6) 3_666
O20 H202 O21 0.86(3) 2.31(4) 3.038(5) 143(5) .
O21 H211 N1 0.85(4) 2.01(4) 2.842(5) 165(6) .
O21 H212 O22A 0.82(3) 2.61(5) 3.185(9) 128(5) 3_666
O21 H212 O22B 0.82(3) 2.10(5) 2.775(9) 139(6) 3_666

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.059
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.109

data_26116
_database_code_depnum_ccdc_archive 'CCDC 702192'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H21 N8 Nd O8, C8 H4 N8, 12(H2 O)'
_chemical_formula_sum            'C16 H49 N16 Nd O20'
_chemical_formula_weight         929.95

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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   11.2104(17)
_cell_length_b                   28.980(4)
_cell_length_c                   11.9110(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.184(2)
_cell_angle_gamma                90.00
_cell_volume                     3608.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14506
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.04

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1908
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2005)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24695
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         28.13
_reflns_number_total             8155
_reflns_number_gt                6949
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_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.
One of the lattice water molecules was disordered and refined as two
isotropic half oxygen atoms, O(22A) and O(22B), and no attempt was made
to locate the hydrogens on this water.
Geometrical restraints were applied to the water hydrogen atoms, mainly to
the O-H distances.
;

_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)+(0.0535P)²+8.7998P] 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         8155
_refine_ls_number_parameters     594
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1205
_refine_ls_wR_factor_gt          0.1152
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.130
_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
Nd1 Nd 0.305899(19) 0.431373(7) 0.53604(2) 0.00957(8) Uani 1 1 d . . .
O1 O 0.4225(3) 0.42002(11) 0.7562(3) 0.0164(6) Uani 1 1 d D . .
H11 H 0.503(3) 0.4232(19) 0.797(5) 0.025 Uiso 1 1 d D . .
H12 H 0.391(5) 0.4106(19) 0.808(4) 0.025 Uiso 1 1 d D . .
O2 O 0.1545(3) 0.43185(10) 0.6420(3) 0.0146(6) Uani 1 1 d D . .
H21 H 0.115(5) 0.4129(16) 0.668(5) 0.022 Uiso 1 1 d D . .
H22 H 0.142(5) 0.4590(13) 0.666(5) 0.022 Uiso 1 1 d D . .
O3 O 0.3172(3) 0.35024(10) 0.5898(3) 0.0144(6) Uani 1 1 d D . .
H31 H 0.359(5) 0.3371(17) 0.657(4) 0.022 Uiso 1 1 d D . .
H32 H 0.291(5) 0.3321(17) 0.535(4) 0.022 Uiso 1 1 d D . .
O4 O 0.5385(3) 0.43253(10) 0.5793(3) 0.0136(6) Uani 1 1 d D . .
H41 H 0.589(5) 0.4141(16) 0.562(5) 0.020 Uiso 1 1 d D . .
H42 H 0.579(5) 0.4589(14) 0.598(5) 0.020 Uiso 1 1 d D . .
O5 O 0.3775(3) 0.50626(11) 0.6435(3) 0.0173(7) Uani 1 1 d D . .
H51 H 0.353(5) 0.5331(13) 0.622(5) 0.026 Uiso 1 1 d D . .
H52 H 0.419(5) 0.507(2) 0.719(3) 0.026 Uiso 1 1 d D . .
O6 O 0.3423(3) 0.48192(10) 0.3741(3) 0.0137(6) Uani 1 1 d D . .
H61 H 0.279(4) 0.4894(18) 0.313(4) 0.021 Uiso 1 1 d D . .
H62 H 0.377(5) 0.4649(17) 0.337(5) 0.021 Uiso 1 1 d D . .
O7 O 0.1391(3) 0.49342(11) 0.4528(3) 0.0149(6) Uani 1 1 d D . .
H71 H 0.065(4) 0.4909(18) 0.395(4) 0.022 Uiso 1 1 d D . .
H72 H 0.151(5) 0.5216(12) 0.469(5) 0.022 Uiso 1 1 d D . .
O8 O 0.1109(3) 0.39590(11) 0.3947(3) 0.0152(6) Uani 1 1 d D . .
H81 H 0.097(5) 0.4001(19) 0.320(3) 0.023 Uiso 1 1 d D . .
H82 H 0.037(4) 0.3985(18) 0.402(5) 0.023 Uiso 1 1 d D . .
C1 C 0.4933(4) 0.29011(14) 0.2354(4) 0.0097(8) Uani 1 1 d . . .
C2 C 0.4560(4) 0.24743(14) 0.2654(4) 0.0105(8) Uani 1 1 d . . .
H2A H 0.3994 0.2461 0.3085 0.013 Uiso 1 1 calc R . .
C3 C 0.5010(4) 0.20690(14) 0.2328(4) 0.0095(8) Uani 1 1 d . . .
C4 C 0.5858(4) 0.20856(15) 0.1707(4) 0.0129(8) Uani 1 1 d . . .
H4A H 0.6176 0.1808 0.1494 0.015 Uiso 1 1 calc R . .
C5 C 0.6228(4) 0.25087(15) 0.1404(4) 0.0158(9) Uani 1 1 d . . .
H5A H 0.6798 0.2522 0.0977 0.019 Uiso 1 1 calc R . .
C6 C 0.5770(4) 0.29139(15) 0.1722(4) 0.0140(8) Uani 1 1 d . . .
H6A H 0.6027 0.3203 0.1509 0.017 Uiso 1 1 calc R . .
C7 C 0.4507(4) 0.33349(14) 0.2728(4) 0.0094(8) Uani 1 1 d . . .
N1 N 0.4901(3) 0.37551(12) 0.2526(3) 0.0118(7) Uani 1 1 d . . .
N2 N 0.4344(3) 0.40525(12) 0.3044(3) 0.0122(7) Uani 1 1 d . . .
N3 N 0.3639(3) 0.38237(12) 0.3542(3) 0.0126(7) Uani 1 1 d . . .
N4 N 0.3720(3) 0.33699(12) 0.3347(3) 0.0110(7) Uani 1 1 d . . .
C8 C 0.4630(4) 0.16148(14) 0.2629(4) 0.0103(8) Uani 1 1 d . . .
N5 N 0.3750(3) 0.15343(12) 0.3123(3) 0.0125(7) Uani 1 1 d D . .
H5 H 0.326(4) 0.1699(16) 0.334(5) 0.015 Uiso 1 1 d D . .
N6 N 0.3666(3) 0.10769(12) 0.3264(3) 0.0144(7) Uani 1 1 d . . .
N7 N 0.4473(3) 0.08838(12) 0.2855(3) 0.0145(7) Uani 1 1 d . . .
N8 N 0.5092(3) 0.12091(12) 0.2448(3) 0.0113(7) Uani 1 1 d . . .
C9 C 0.2012(4) 0.20286(14) 0.0189(3) 0.0081(7) Uani 1 1 d U . .
C10 C 0.2436(4) 0.24592(14) -0.0048(4) 0.0102(8) Uani 1 1 d . . .
H10A H 0.3069 0.2474 -0.0404 0.012 Uiso 1 1 calc R . .
C11 C 0.1942(4) 0.28670(14) 0.0232(4) 0.0092(8) Uani 1 1 d . . .
C12 C 0.1009(4) 0.28423(15) 0.0757(4) 0.0134(8) Uani 1 1 d . . .
H12A H 0.0667 0.3118 0.0952 0.016 Uiso 1 1 calc R . .
C13 C 0.0581(4) 0.24174(15) 0.0992(4) 0.0152(9) Uani 1 1 d . . .
H13A H -0.0058 0.2404 0.1340 0.018 Uiso 1 1 calc R . .
C14 C 0.1080(4) 0.20099(14) 0.0723(4) 0.0112(8) Uani 1 1 d . . .
H14A H 0.0792 0.1720 0.0899 0.013 Uiso 1 1 calc R . .
C15 C 0.2545(4) 0.15950(14) -0.0077(4) 0.0097(8) Uani 1 1 d . . .
N9 N 0.2217(3) 0.11762(12) 0.0159(3) 0.0120(7) Uani 1 1 d . . .
N10 N 0.2934(3) 0.08835(12) -0.0218(3) 0.0141(7) Uani 1 1 d . . .
N11 N 0.3676(3) 0.11241(12) -0.0652(3) 0.0141(7) Uani 1 1 d . . .
N12 N 0.3456(3) 0.15748(12) -0.0572(3) 0.0113(7) Uani 1 1 d . . .
C16 C 0.2380(4) 0.33207(14) -0.0026(4) 0.0096(8) Uani 1 1 d . . .
N13 N 0.3149(3) 0.33883(12) -0.0648(3) 0.0117(7) Uani 1 1 d . . .
N14 N 0.3276(3) 0.38492(12) -0.0692(3) 0.0132(7) Uani 1 1 d . . .
N15 N 0.2604(3) 0.40499(12) -0.0111(4) 0.0143(7) Uani 1 1 d . . .
N16 N 0.2025(3) 0.37228(12) 0.0312(3) 0.0118(7) Uani 1 1 d . . .
O11 O 0.2151(3) 0.28614(11) 0.4136(3) 0.0150(6) Uani 1 1 d D . .
H111 H 0.262(5) 0.3015(17) 0.386(5) 0.022 Uiso 1 1 d D . .
H112 H 0.138(4) 0.2918(19) 0.376(5) 0.022 Uiso 1 1 d D . .
O12 O 0.2158(3) 0.19391(11) 0.4031(3) 0.0147(6) Uani 1 1 d D . .
H121 H 0.249(5) 0.1818(18) 0.470(4) 0.022 Uiso 1 1 d D . .
H122 H 0.223(5) 0.2228(12) 0.414(5) 0.022 Uiso 1 1 d D . .
O13 O 0.6691(3) 0.42724(12) 0.9106(4) 0.0253(8) Uani 1 1 d D . .
H131 H 0.734(5) 0.417(2) 0.891(6) 0.038 Uiso 1 1 d D . .
H132 H 0.691(6) 0.4534(15) 0.941(6) 0.038 Uiso 1 1 d D . .
O14 O 0.4426(3) 0.30230(11) 0.7995(3) 0.0141(6) Uani 1 1 d D . .
H141 H 0.515(4) 0.3080(19) 0.839(5) 0.021 Uiso 1 1 d D . .
H142 H 0.401(5) 0.3117(18) 0.840(5) 0.021 Uiso 1 1 d D . .
O15 O 0.9536(3) 0.29337(11) 0.3074(3) 0.0148(6) Uani 1 1 d D . .
H151 H 0.922(5) 0.3048(18) 0.354(4) 0.022 Uiso 1 1 d D . .
H152 H 0.936(5) 0.2652(12) 0.301(5) 0.022 Uiso 1 1 d D . .
O16 O 0.1286(3) 0.49655(11) 0.1727(3) 0.0193(7) Uani 1 1 d D . .
H161 H 0.096(5) 0.4690(14) 0.171(5) 0.029 Uiso 1 1 d D . .
H162 H 0.088(5) 0.5185(16) 0.188(5) 0.029 Uiso 1 1 d D . .
O17 O 0.0494(3) 0.40641(11) 0.1520(3) 0.0152(6) Uani 1 1 d D . .
H171 H -0.019(4) 0.3917(17) 0.122(5) 0.023 Uiso 1 1 d D . .
H172 H 0.088(5) 0.3932(18) 0.111(5) 0.023 Uiso 1 1 d D . .
O18 O 0.1735(4) 0.49613(13) 0.9549(4) 0.0341(9) Uani 1 1 d D . .
H181 H 0.207(6) 0.4689(16) 0.956(6) 0.051 Uiso 1 1 d D . .
H182 H 0.148(7) 0.499(2) 1.017(5) 0.051 Uiso 1 1 d D . .
O19 O 0.8358(3) 0.35006(12) 0.1164(3) 0.0171(6) Uani 1 1 d D . .
H191 H 0.869(5) 0.3302(17) 0.174(4) 0.026 Uiso 1 1 d D . .
H192 H 0.795(5) 0.3703(16) 0.140(5) 0.026 Uiso 1 1 d D . .
O20 O 0.8915(3) 0.48069(12) 0.2800(3) 0.0205(7) Uani 1 1 d D . .
H201 H 0.862(6) 0.484(2) 0.203(3) 0.031 Uiso 1 1 d D . .
H202 H 0.854(5) 0.4559(15) 0.288(5) 0.031 Uiso 1 1 d D . .
O21 O 0.6766(3) 0.41149(12) 0.1671(4) 0.0241(8) Uani 1 1 d D . .
H211 H 0.623(5) 0.3944(19) 0.182(6) 0.036 Uiso 1 1 d D . .
H212 H 0.642(6) 0.425(2) 0.099(4) 0.036 Uiso 1 1 d D . .
O22A O 0.5484(7) 0.5150(3) 0.8809(7) 0.0271(16) Uiso 0.50 1 d P A 1
O22B O 0.5034(7) 0.5180(3) 0.9129(7) 0.0271(16) Uiso 0.50 1 d P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O3 2.428(3) . ?
Nd1 O8 2.452(3) . ?
Nd1 O2 2.454(3) . ?
Nd1 O4 2.468(3) . ?
Nd1 O1 2.493(3) . ?
Nd1 O5 2.500(3) . ?
Nd1 O7 2.524(3) . ?
Nd1 O6 2.569(3) . ?
Nd1 N3 2.854(4) . ?
O1 H11 0.86(3) . ?
O1 H12 0.86(3) . ?
O2 H21 0.83(3) . ?
O2 H22 0.86(3) . ?
O3 H31 0.86(3) . ?
O3 H32 0.80(3) . ?
O4 H41 0.86(3) . ?
O4 H42 0.87(3) . ?
O5 H51 0.84(3) . ?
O5 H52 0.85(3) . ?
O6 H61 0.84(3) . ?
O6 H62 0.84(3) . ?
O7 H71 0.87(3) . ?
O7 H72 0.84(3) . ?
O8 H81 0.85(3) . ?
O8 H82 0.87(3) . ?
C1 C2 1.393(6) . ?
C1 C6 1.400(6) . ?
C1 C7 1.470(5) . ?
C2 C3 1.388(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.401(5) . ?
C3 C8 1.467(6) . ?
C4 C5 1.383(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.388(6) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 N4 1.343(5) . ?
C7 N1 1.346(5) . ?
N1 N2 1.339(5) . ?
N2 N3 1.325(5) . ?
N3 N4 1.344(5) . ?
C8 N8 1.334(5) . ?
C8 N5 1.340(5) . ?
N5 N6 1.344(5) . ?
N5 H5 0.84(3) . ?
N6 N7 1.299(5) . ?
N7 N8 1.359(5) . ?
C9 C10 1.400(5) . ?
C9 C14 1.407(5) . ?
C9 C15 1.474(5) . ?
C10 C11 1.396(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.401(5) . ?
C11 C16 1.474(6) . ?
C12 C13 1.386(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.393(6) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 N9 1.327(5) . ?
C15 N12 1.352(5) . ?
N9 N10 1.352(5) . ?
N10 N11 1.326(5) . ?
N11 N12 1.339(5) . ?
C16 N16 1.339(5) . ?
C16 N13 1.339(5) . ?
N13 N14 1.346(5) . ?
N14 N15 1.327(5) . ?
N15 N16 1.345(5) . ?
O11 H111 0.84(3) . ?
O11 H112 0.83(3) . ?
O12 H121 0.83(3) . ?
O12 H122 0.85(3) . ?
O13 H131 0.89(4) . ?
O13 H132 0.84(4) . ?
O14 H141 0.79(3) . ?
O14 H142 0.83(3) . ?
O15 H151 0.83(3) . ?
O15 H152 0.84(3) . ?
O16 H161 0.88(3) . ?
O16 H162 0.84(3) . ?
O17 H171 0.83(3) . ?
O17 H172 0.85(3) . ?
O18 H181 0.87(4) . ?
O18 H182 0.88(4) . ?
O19 H191 0.87(3) . ?
O19 H192 0.85(3) . ?
O20 H201 0.86(4) . ?
O20 H202 0.86(3) . ?
O21 H211 0.84(4) . ?
O21 H212 0.85(4) . ?

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
O3 Nd1 O8 73.96(11) . . ?
O3 Nd1 O2 81.36(10) . . ?
O8 Nd1 O2 75.22(11) . . ?
O3 Nd1 O4 90.43(10) . . ?
O8 Nd1 O4 139.61(10) . . ?
O2 Nd1 O4 140.08(11) . . ?
O3 Nd1 O1 68.73(11) . . ?
O8 Nd1 O1 131.72(11) . . ?
O2 Nd1 O1 69.94(11) . . ?
O4 Nd1 O1 70.67(10) . . ?
O3 Nd1 O5 136.80(11) . . ?
O8 Nd1 O5 139.24(11) . . ?
O2 Nd1 O5 83.43(10) . . ?
O4 Nd1 O5 76.21(10) . . ?
O1 Nd1 O5 68.08(11) . . ?
O3 Nd1 O7 138.94(10) . . ?
O8 Nd1 O7 71.28(10) . . ?
O2 Nd1 O7 69.28(10) . . ?
O4 Nd1 O7 130.46(10) . . ?
O1 Nd1 O7 122.65(11) . . ?
O5 Nd1 O7 68.78(11) . . ?
O3 Nd1 O6 137.96(10) . . ?
O8 Nd1 O6 93.89(10) . . ?
O2 Nd1 O6 135.24(10) . . ?
O4 Nd1 O6 72.95(10) . . ?
O1 Nd1 O6 134.39(10) . . ?
O5 Nd1 O6 77.34(11) . . ?
O7 Nd1 O6 66.12(10) . . ?
O3 Nd1 N3 73.37(11) . . ?
O8 Nd1 N3 70.21(10) . . ?
O2 Nd1 N3 141.50(10) . . ?
O4 Nd1 N3 69.66(10) . . ?
O1 Nd1 N3 123.75(11) . . ?
O5 Nd1 N3 134.54(10) . . ?
O7 Nd1 N3 113.33(11) . . ?
O6 Nd1 N3 64.70(10) . . ?
Nd1 O1 H11 128(4) . . ?
Nd1 O1 H12 127(4) . . ?
H11 O1 H12 104(5) . . ?
Nd1 O2 H21 138(4) . . ?
Nd1 O2 H22 113(4) . . ?
H21 O2 H22 108(5) . . ?
Nd1 O3 H31 129(4) . . ?
Nd1 O3 H32 117(4) . . ?
H31 O3 H32 112(5) . . ?
Nd1 O4 H41 133(4) . . ?
Nd1 O4 H42 118(4) . . ?
H41 O4 H42 106(5) . . ?
Nd1 O5 H51 130(4) . . ?
Nd1 O5 H52 120(4) . . ?
H51 O5 H52 108(5) . . ?
Nd1 O6 H61 119(4) . . ?
Nd1 O6 H62 107(4) . . ?
H61 O6 H62 96(5) . . ?
Nd1 O7 H71 128(4) . . ?
Nd1 O7 H72 125(4) . . ?
H71 O7 H72 107(5) . . ?
Nd1 O8 H81 116(4) . . ?
Nd1 O8 H82 123(4) . . ?
H81 O8 H82 106(5) . . ?
C2 C1 C6 118.9(4) . . ?
C2 C1 C7 121.4(4) . . ?
C6 C1 C7 119.6(4) . . ?
C3 C2 C1 120.4(4) . . ?
C3 C2 H2A 119.8 . . ?
C1 C2 H2A 119.8 . . ?
C2 C3 C4 120.2(4) . . ?
C2 C3 C8 121.6(4) . . ?
C4 C3 C8 118.1(4) . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 H5A 119.9 . . ?
C5 C6 C1 120.7(4) . . ?
C5 C6 H6A 119.7 . . ?
C1 C6 H6A 119.7 . . ?
N4 C7 N1 110.7(3) . . ?
N4 C7 C1 125.5(4) . . ?
N1 C7 C1 123.8(4) . . ?
N2 N1 C7 105.2(3) . . ?
N3 N2 N1 109.7(3) . . ?
N2 N3 N4 108.9(3) . . ?
N2 N3 Nd1 115.3(3) . . ?
N4 N3 Nd1 131.8(3) . . ?
C7 N4 N3 105.5(3) . . ?
N8 C8 N5 108.0(3) . . ?
N8 C8 C3 126.0(4) . . ?
N5 C8 C3 126.0(4) . . ?
C8 N5 N6 108.8(3) . . ?
C8 N5 H5 135(4) . . ?
N6 N5 H5 116(4) . . ?
N7 N6 N5 106.7(3) . . ?
N6 N7 N8 110.5(3) . . ?
C8 N8 N7 106.0(3) . . ?
C10 C9 C14 119.2(4) . . ?
C10 C9 C15 121.5(4) . . ?
C14 C9 C15 119.3(4) . . ?
C11 C10 C9 120.9(4) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C10 C11 C12 119.2(4) . . ?
C10 C11 C16 121.0(4) . . ?
C12 C11 C16 119.8(4) . . ?
C13 C12 C11 120.2(4) . . ?
C13 C12 H12A 119.9 . . ?
C11 C12 H12A 119.9 . . ?
C12 C13 C14 120.7(4) . . ?
C12 C13 H13A 119.7 . . ?
C14 C13 H13A 119.7 . . ?
C13 C14 C9 119.8(4) . . ?
C13 C14 H14A 120.1 . . ?
C9 C14 H14A 120.1 . . ?
N9 C15 N12 111.3(3) . . ?
N9 C15 C9 124.7(4) . . ?
N12 C15 C9 124.0(4) . . ?
C15 N9 N10 105.1(3) . . ?
N11 N10 N9 109.4(3) . . ?
N10 N11 N12 109.1(3) . . ?
N11 N12 C15 105.1(3) . . ?
N16 C16 N13 111.0(4) . . ?
N16 C16 C11 123.8(4) . . ?
N13 C16 C11 125.1(4) . . ?
C16 N13 N14 105.4(3) . . ?
N15 N14 N13 109.1(3) . . ?
N14 N15 N16 109.1(3) . . ?
C16 N16 N15 105.4(3) . . ?
H111 O11 H112 111(5) . . ?
H121 O12 H122 107(5) . . ?
H131 O13 H132 106(6) . . ?
H141 O14 H142 105(6) . . ?
H151 O15 H152 108(6) . . ?
H161 O16 H162 116(6) . . ?
H171 O17 H172 96(5) . . ?
H181 O18 H182 109(6) . . ?
H191 O19 H192 109(5) . . ?
H201 O20 H202 101(6) . . ?
H211 O21 H212 110(6) . . ?

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
O1 H11 O13 0.86(3) 1.87(4) 2.719(5) 169(6) .
O1 H12 N14 0.86(3) 1.98(4) 2.845(5) 176(6) 1_556
O2 H21 N8 0.83(3) 2.00(4) 2.816(5) 168(6) 4_566
O2 H22 O20 0.86(3) 1.95(4) 2.810(5) 178(5) 3_666
O3 H31 O14 0.86(3) 1.90(4) 2.758(5) 174(5) .
O3 H32 O11 0.80(3) 1.93(4) 2.726(5) 174(6) .
O4 H41 N9 0.86(3) 1.98(4) 2.833(5) 169(5) 4_666
O4 H42 O6 0.87(3) 1.90(3) 2.776(4) 175(5) 3_666
O5 H51 N10 0.84(3) 2.29(4) 3.070(5) 155(5) 2
O5 H52 O22A 0.85(3) 1.96(4) 2.795(8) 166(6) .
O5 H52 O22B 0.85(3) 2.18(4) 3.021(9) 170(6) .
O6 H61 O16 0.84(3) 1.91(4) 2.743(5) 171(5) .
O6 H62 N2 0.84(3) 1.93(4) 2.704(5) 151(5) .
O7 H71 O20 0.87(3) 1.95(4) 2.820(5) 172(5) 1_455
O7 H72 N10 0.84(3) 2.06(4) 2.892(5) 172(5) 2
O8 H81 O17 0.85(3) 1.89(4) 2.735(5) 174(6) .
O8 H82 N11 0.87(3) 2.10(4) 2.944(5) 165(5) 4_566
N5 H5 O12 0.84(3) 1.85(4) 2.669(5) 166(5) .
O11 H111 N4 0.84(3) 1.87(4) 2.710(5) 176(6) .
O11 H112 O15 0.83(3) 1.93(4) 2.748(4) 167(6) 1_455
O12 H121 O19 0.83(3) 1.90(4) 2.724(5) 174(6) 4_566
O12 H122 O11 0.85(3) 1.84(4) 2.676(4) 170(6) .
O13 H131 N6 0.89(4) 2.04(4) 2.922(5) 173(6) 4_666
O13 H132 O18 0.84(4) 2.15(4) 2.927(6) 154(6) 3_667
O14 H141 O12 0.79(3) 2.10(4) 2.862(4) 160(6) 4_666
O14 H142 N13 0.83(3) 1.91(4) 2.730(5) 174(6) 1_556
O15 H151 N12 0.83(3) 1.92(4) 2.740(5) 168(6) 4_666
O15 H152 O14 0.84(3) 1.96(4) 2.776(4) 165(5) 4_665
O16 H161 O17 0.88(3) 1.88(4) 2.742(5) 168(6) .
O16 H162 N7 0.84(3) 2.11(4) 2.892(5) 155(6) 2
O17 H171 O19 0.83(3) 2.01(4) 2.801(4) 159(6) 1_455
O17 H172 N16 0.85(3) 1.95(4) 2.790(5) 168(5) .
O18 H181 N15 0.87(4) 1.94(4) 2.793(5) 165(7) 1_556
O18 H182 O16 0.88(4) 1.95(4) 2.815(5) 167(7) 1_556
O19 H191 O15 0.87(3) 1.86(4) 2.729(5) 173(6) .
O19 H192 O21 0.85(3) 1.90(4) 2.738(5) 169(6) .
O20 H201 O18 0.86(4) 1.87(4) 2.709(6) 165(6) 3_666
O20 H202 O21 0.86(3) 2.37(5) 3.048(5) 137(5) .
O21 H211 N1 0.84(4) 2.04(4) 2.834(5) 158(6) .
O21 H212 O22A 0.85(4) 2.83(7) 3.192(8) 107(5) 3_666
O21 H212 O22B 0.85(4) 2.29(6) 2.787(8) 117(5) 3_666

_diffrn_measured_fraction_theta_max 0.924
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.236
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.160


