# Electronic Supplementary Material for CrystEngComm
# This journal is © The Royal Society of Chemistry 2008


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

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

_publ_section_title              
;
A new class of 3-D porous framework: [Ln(H2O)n]3+ ions act as
pillars between ?-stacked and H-bonded sheets of (m-BDTH) organic anions in
[Ln(H2O)n](m-BDTH)3?9(H2O) (Ln = Pr, n = 9; Ln = Gd, n = 8)
;
loop_
_publ_author_name
'A K Powell'
'Ghulam Abbas'
'Christopher Anson'
'George E Kostakis'

# Attachment 'B804676J_ccdc_680457_680458_cif.txt'

# Attachment 'kostakis.cif'
data_26025
_database_code_depnum_ccdc_archive 'CCDC 680457'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'H18 O9 Pr, 3(C8 H5 N8), 9(H2 O)'
_chemical_formula_sum            'C24 H51 N24 O18 Pr'
_chemical_formula_weight         1104.80

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'
Pr Pr -0.2180 2.8214 '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                   9.8788(6)
_cell_length_b                   19.6459(12)
_cell_length_c                   22.7918(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.545(1)
_cell_angle_gamma                90.00
_cell_volume                     4333.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2463
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      22.40

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2264
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_T_max  0.884
_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            20763
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         28.23
_reflns_number_total             9675
_reflns_number_gt                7241
_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.
;

_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)+(0.0416P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9675
_refine_ls_number_parameters     721
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1098
_refine_ls_wR_factor_gt          0.0996
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.07301(2) 0.186701(13) 0.244519(11) 0.01395(8) Uani 1 1 d . . .
O1 O 0.2848(4) 0.2373(2) 0.30807(15) 0.0252(9) Uani 1 1 d D . .
H11 H 0.291(6) 0.234(3) 0.342(2) 0.038 Uiso 1 1 d . . .
H12 H 0.312(6) 0.270(2) 0.291(2) 0.038 Uiso 1 1 d D . .
O2 O -0.0334(4) 0.17628(17) 0.13656(14) 0.0192(8) Uani 1 1 d D . .
H21 H -0.006(5) 0.145(2) 0.119(2) 0.029 Uiso 1 1 d D . .
H22 H -0.055(6) 0.202(3) 0.115(2) 0.029 Uiso 1 1 d . . .
O3 O -0.1082(3) 0.27941(19) 0.21931(15) 0.0209(8) Uani 1 1 d . . .
H31 H -0.122(5) 0.313(3) 0.243(2) 0.031 Uiso 1 1 d . . .
H32 H -0.161(6) 0.274(3) 0.192(2) 0.031 Uiso 1 1 d . . .
O4 O 0.2804(4) 0.15039(19) 0.20653(16) 0.0244(8) Uani 1 1 d . . .
H41 H 0.324(6) 0.125(3) 0.233(2) 0.037 Uiso 1 1 d . . .
H42 H 0.273(6) 0.128(3) 0.176(2) 0.037 Uiso 1 1 d . . .
O5 O 0.0513(4) 0.0580(2) 0.20611(17) 0.0299(9) Uani 1 1 d . . .
H51 H 0.062(6) 0.046(3) 0.176(3) 0.045 Uiso 1 1 d . . .
H52 H 0.084(6) 0.028(3) 0.227(3) 0.045 Uiso 1 1 d . . .
O6 O -0.1459(4) 0.13259(19) 0.25310(16) 0.0238(8) Uani 1 1 d . . .
H61 H -0.203(6) 0.154(3) 0.259(3) 0.036 Uiso 1 1 d . . .
H62 H -0.173(5) 0.091(3) 0.241(2) 0.036 Uiso 1 1 d . . .
O7 O 0.1636(4) 0.28335(18) 0.19352(16) 0.0213(8) Uani 1 1 d . . .
H71 H 0.227(6) 0.278(3) 0.177(2) 0.032 Uiso 1 1 d . . .
H72 H 0.124(6) 0.314(3) 0.177(2) 0.032 Uiso 1 1 d . . .
O8 O 0.1578(4) 0.10316(19) 0.32718(16) 0.0228(8) Uani 1 1 d . . .
H81 H 0.156(6) 0.064(3) 0.321(2) 0.034 Uiso 1 1 d . . .
H82 H 0.206(6) 0.105(3) 0.357(2) 0.034 Uiso 1 1 d . . .
O9 O 0.0098(4) 0.23359(18) 0.33797(15) 0.0208(8) Uani 1 1 d D . .
H91 H -0.032(6) 0.267(3) 0.335(2) 0.031 Uiso 1 1 d . . .
H92 H 0.054(5) 0.231(3) 0.3725(16) 0.031 Uiso 1 1 d D . .
C1 C 1.1323(5) 0.4160(2) 0.4905(2) 0.0165(10) Uani 1 1 d . . .
C2 C 0.9895(5) 0.4157(2) 0.4882(2) 0.0165(10) Uani 1 1 d . . .
H2A H 0.9271 0.4167 0.4506 0.020 Uiso 1 1 calc R . .
C3 C 0.9389(5) 0.4138(2) 0.5412(2) 0.0162(10) Uani 1 1 d . . .
C4 C 1.0332(5) 0.4117(2) 0.5959(2) 0.0198(10) Uani 1 1 d . . .
H4A H 0.9999 0.4109 0.6322 0.024 Uiso 1 1 calc R . .
C5 C 1.1735(5) 0.4109(2) 0.5979(2) 0.0233(11) Uani 1 1 d . . .
H5A H 1.2363 0.4079 0.6353 0.028 Uiso 1 1 calc R . .
C6 C 1.2221(5) 0.4143(2) 0.5455(2) 0.0192(10) Uani 1 1 d . . .
H6A H 1.3189 0.4155 0.5470 0.023 Uiso 1 1 calc R . .
C7 C 1.1857(5) 0.4205(2) 0.4348(2) 0.0184(10) Uani 1 1 d . . .
N1 N 1.3197(4) 0.4267(2) 0.43174(18) 0.0218(9) Uani 1 1 d . . .
H1 H 1.408(5) 0.424(2) 0.458(2) 0.026 Uiso 1 1 d . . .
N2 N 1.3286(4) 0.4316(2) 0.37412(19) 0.0285(10) Uani 1 1 d . . .
N3 N 1.2030(5) 0.4288(2) 0.34357(19) 0.0343(12) Uani 1 1 d . . .
N4 N 1.1116(4) 0.4214(2) 0.38027(18) 0.0267(10) Uani 1 1 d . . .
C8 C 0.7900(5) 0.4151(2) 0.5403(2) 0.0152(10) Uani 1 1 d . . .
N5 N 0.7361(4) 0.40765(19) 0.58911(17) 0.0186(9) Uani 1 1 d . . .
N6 N 0.5992(4) 0.41160(19) 0.56938(17) 0.0189(9) Uani 1 1 d . . .
N7 N 0.5720(4) 0.42147(19) 0.51098(17) 0.0184(9) Uani 1 1 d . . .
N8 N 0.6909(4) 0.42323(18) 0.49074(17) 0.0162(8) Uani 1 1 d . . .
C9 C 0.7142(5) 0.0819(2) 0.46615(19) 0.0131(9) Uani 1 1 d . . .
C10 C 0.8136(5) 0.0773(2) 0.5187(2) 0.0165(10) Uani 1 1 d . . .
H10A H 0.7864 0.0717 0.5561 0.020 Uiso 1 1 calc R . .
C11 C 0.9545(5) 0.0808(2) 0.5162(2) 0.0147(9) Uani 1 1 d . . .
C12 C 0.9924(5) 0.0891(2) 0.4613(2) 0.0167(10) Uani 1 1 d . . .
H12A H 1.0875 0.0923 0.4597 0.020 Uiso 1 1 calc R . .
C13 C 0.8944(5) 0.0930(2) 0.4089(2) 0.0174(10) Uani 1 1 d . . .
H13A H 0.9219 0.0982 0.3715 0.021 Uiso 1 1 calc R . .
C14 C 0.7559(5) 0.0892(2) 0.4114(2) 0.0182(10) Uani 1 1 d . . .
H14A H 0.6881 0.0916 0.3754 0.022 Uiso 1 1 calc R . .
C15 C 0.5655(5) 0.0814(2) 0.4675(2) 0.0160(10) Uani 1 1 d . . .
N9 N 0.4661(4) 0.0825(2) 0.41792(17) 0.0193(9) Uani 1 1 d . . .
N10 N 0.3467(4) 0.08345(19) 0.43738(18) 0.0199(9) Uani 1 1 d . . .
N11 N 0.3742(4) 0.08343(18) 0.49628(17) 0.0166(8) Uani 1 1 d . . .
N12 N 0.5121(4) 0.08208(18) 0.51656(16) 0.0158(8) Uani 1 1 d . . .
C16 C 1.0581(5) 0.0762(2) 0.5714(2) 0.0153(10) Uani 1 1 d . . .
N13 N 1.1951(4) 0.0795(2) 0.57475(17) 0.0169(9) Uani 1 1 d . . .
H13 H 1.243(5) 0.084(2) 0.551(2) 0.020 Uiso 1 1 d . . .
N14 N 1.2588(4) 0.0724(2) 0.63221(17) 0.0212(9) Uani 1 1 d . . .
N15 N 1.1620(4) 0.0660(2) 0.66275(17) 0.0221(9) Uani 1 1 d . . .
N16 N 1.0363(4) 0.06894(19) 0.62647(17) 0.0184(9) Uani 1 1 d . . .
C17 C 0.8086(4) 0.2467(2) 0.52742(19) 0.0125(9) Uani 1 1 d . . .
C18 C 0.6690(4) 0.2463(2) 0.53127(19) 0.0140(9) Uani 1 1 d . . .
H18A H 0.6431 0.2421 0.5691 0.017 Uiso 1 1 calc R . .
C19 C 0.5685(4) 0.2521(2) 0.47925(19) 0.0115(9) Uani 1 1 d . . .
C20 C 0.6077(5) 0.2569(2) 0.4242(2) 0.0168(10) Uani 1 1 d . . .
H20A H 0.5389 0.2604 0.3886 0.020 Uiso 1 1 calc R . .
C21 C 0.7459(5) 0.2568(2) 0.4205(2) 0.0174(10) Uani 1 1 d . . .
H21A H 0.7717 0.2595 0.3826 0.021 Uiso 1 1 calc R . .
C22 C 0.8459(5) 0.2526(2) 0.4720(2) 0.0156(10) Uani 1 1 d . . .
H22A H 0.9408 0.2537 0.4697 0.019 Uiso 1 1 calc R . .
C23 C 0.9143(4) 0.2389(2) 0.58214(19) 0.0121(9) Uani 1 1 d . . .
N17 N 1.0523(4) 0.23930(19) 0.58497(16) 0.0135(8) Uani 1 1 d . . .
H17 H 1.100(5) 0.242(2) 0.561(2) 0.016 Uiso 1 1 d . . .
N18 N 1.1166(4) 0.23136(18) 0.64247(16) 0.0156(8) Uani 1 1 d . . .
N19 N 1.0188(4) 0.22528(19) 0.67307(17) 0.0177(8) Uani 1 1 d . . .
N20 N 0.8931(4) 0.22982(19) 0.63722(17) 0.0187(9) Uani 1 1 d . . .
C24 C 0.4195(4) 0.2497(2) 0.48086(19) 0.0125(9) Uani 1 1 d . . .
N21 N 0.3209(4) 0.24627(19) 0.43139(16) 0.0149(8) Uani 1 1 d . . .
N22 N 0.2015(4) 0.24259(19) 0.45064(16) 0.0168(8) Uani 1 1 d . . .
N23 N 0.2291(4) 0.24472(18) 0.50980(16) 0.0148(8) Uani 1 1 d . . .
N24 N 0.3660(4) 0.24940(18) 0.53040(16) 0.0136(8) Uani 1 1 d . . .
O11 O -0.1277(4) 0.35443(18) 0.32017(16) 0.0275(8) Uani 1 1 d D . .
H111 H -0.203(5) 0.367(3) 0.328(2) 0.041 Uiso 1 1 d D . .
H112 H -0.061(5) 0.386(2) 0.334(2) 0.041 Uiso 1 1 d D . .
O12 O -0.3618(4) 0.1978(2) 0.28290(16) 0.0331(9) Uani 1 1 d D . .
H121 H -0.411(6) 0.161(2) 0.283(3) 0.050 Uiso 1 1 d D . .
H122 H -0.404(6) 0.222(3) 0.255(2) 0.050 Uiso 1 1 d D . .
O13 O -0.2377(4) 0.00094(19) 0.22666(16) 0.0363(10) Uani 1 1 d D . .
H131 H -0.204(6) -0.018(3) 0.192(2) 0.054 Uiso 1 1 d D . .
H132 H -0.205(6) -0.025(3) 0.260(2) 0.054 Uiso 1 1 d D . .
O14 O 0.1638(4) -0.0376(2) 0.30301(16) 0.0286(9) Uani 1 1 d D . .
H141 H 0.244(4) -0.049(3) 0.311(2) 0.043 Uiso 1 1 d D . .
H142 H 0.105(5) -0.048(3) 0.322(2) 0.043 Uiso 1 1 d D . .
O15 O 0.4487(4) 0.34912(19) 0.27850(16) 0.0274(8) Uani 1 1 d D . .
H151 H 0.507(5) 0.340(3) 0.257(2) 0.041 Uiso 1 1 d D . .
H152 H 0.392(5) 0.376(3) 0.256(2) 0.041 Uiso 1 1 d D . .
O16 O 0.0834(4) 0.40893(19) 0.14306(16) 0.0251(8) Uani 1 1 d D . .
H161 H 0.061(6) 0.409(3) 0.1077(17) 0.038 Uiso 1 1 d D . .
H162 H 0.020(5) 0.426(3) 0.156(2) 0.038 Uiso 1 1 d D . .
O17 O -0.3399(4) 0.4196(2) 0.36161(16) 0.0289(9) Uani 1 1 d D . .
H171 H -0.417(5) 0.400(3) 0.347(2) 0.043 Uiso 1 1 d D . .
H172 H -0.331(6) 0.416(3) 0.4005(17) 0.043 Uiso 1 1 d D . .
O18 O 0.4661(4) 0.0923(2) 0.29516(17) 0.0385(10) Uani 1 1 d D . .
H181 H 0.465(6) 0.049(2) 0.280(3) 0.058 Uiso 1 1 d D . .
H182 H 0.452(6) 0.092(3) 0.331(2) 0.058 Uiso 1 1 d D . .
O19 O -0.0012(4) 0.4682(2) 0.24307(18) 0.0460(11) Uani 1 1 d D . .
H191 H -0.089(5) 0.472(3) 0.263(3) 0.069 Uiso 1 1 d D . .
H192 H 0.091(5) 0.455(3) 0.274(2) 0.069 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O6 2.453(3) . ?
Pr1 O2 2.483(3) . ?
Pr1 O4 2.483(3) . ?
Pr1 O7 2.485(3) . ?
Pr1 O1 2.500(4) . ?
Pr1 O9 2.511(3) . ?
Pr1 O8 2.513(3) . ?
Pr1 O3 2.538(3) . ?
Pr1 O5 2.670(4) . ?
O1 H11 0.77(5) . ?
O1 H12 0.81(3) . ?
O2 H21 0.81(3) . ?
O2 H22 0.72(5) . ?
O3 H31 0.87(5) . ?
O3 H32 0.73(5) . ?
O4 H41 0.83(6) . ?
O4 H42 0.80(5) . ?
O5 H51 0.75(6) . ?
O5 H52 0.79(6) . ?
O6 H61 0.74(6) . ?
O6 H62 0.89(5) . ?
O7 H71 0.80(5) . ?
O7 H72 0.76(5) . ?
O8 H81 0.79(5) . ?
O8 H82 0.75(5) . ?
O9 H91 0.77(5) . ?
O9 H92 0.82(3) . ?
C1 C6 1.382(6) . ?
C1 C2 1.401(6) . ?
C1 C7 1.471(6) . ?
C2 C3 1.397(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.399(6) . ?
C3 C8 1.467(6) . ?
C4 C5 1.378(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.377(6) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 N4 1.311(6) . ?
C7 N1 1.345(6) . ?
N1 N2 1.337(5) . ?
N1 H1 0.96(5) . ?
N2 N3 1.297(5) . ?
N3 N4 1.356(5) . ?
C8 N5 1.334(5) . ?
C8 N8 1.348(6) . ?
N5 N6 1.339(5) . ?
N6 N7 1.318(5) . ?
N7 N8 1.345(5) . ?
C9 C10 1.392(6) . ?
C9 C14 1.398(6) . ?
C9 C15 1.476(6) . ?
C10 C11 1.406(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.386(6) . ?
C11 C16 1.458(6) . ?
C12 C13 1.381(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.383(6) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 N12 1.329(5) . ?
C15 N9 1.340(6) . ?
N9 N10 1.341(5) . ?
N10 N11 1.315(5) . ?
N11 N12 1.349(5) . ?
C16 N16 1.322(5) . ?
C16 N13 1.342(5) . ?
N13 N14 1.342(5) . ?
N13 H13 0.78(5) . ?
N14 N15 1.297(5) . ?
N15 N16 1.348(5) . ?
C17 C22 1.389(6) . ?
C17 C18 1.399(6) . ?
C17 C23 1.466(6) . ?
C18 C19 1.390(6) . ?
C18 H18A 0.9500 . ?
C19 C20 1.390(6) . ?
C19 C24 1.480(6) . ?
C20 C21 1.384(6) . ?
C20 H20A 0.9500 . ?
C21 C22 1.378(6) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 N20 1.326(5) . ?
C23 N17 1.352(5) . ?
N17 N18 1.346(5) . ?
N17 H17 0.80(4) . ?
N18 N19 1.305(5) . ?
N19 N20 1.346(5) . ?
C24 N21 1.336(5) . ?
C24 N24 1.339(5) . ?
N21 N22 1.340(5) . ?
N22 N23 1.322(5) . ?
N23 N24 1.344(5) . ?
O11 H111 0.83(4) . ?
O11 H112 0.91(4) . ?
O12 H121 0.87(4) . ?
O12 H122 0.85(4) . ?
O13 H131 0.99(4) . ?
O13 H132 0.91(4) . ?
O14 H141 0.81(4) . ?
O14 H142 0.81(4) . ?
O15 H151 0.85(4) . ?
O15 H152 0.86(4) . ?
O16 H161 0.79(4) . ?
O16 H162 0.82(4) . ?
O17 H171 0.85(4) . ?
O17 H172 0.88(4) . ?
O18 H181 0.92(4) . ?
O18 H182 0.86(4) . ?
O19 H191 1.05(4) . ?
O19 H192 1.07(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
O6 Pr1 O2 80.69(11) . . ?
O6 Pr1 O4 134.88(12) . . ?
O2 Pr1 O4 81.13(11) . . ?
O6 Pr1 O7 140.75(12) . . ?
O2 Pr1 O7 73.74(12) . . ?
O4 Pr1 O7 69.94(12) . . ?
O6 Pr1 O1 140.82(11) . . ?
O2 Pr1 O1 138.24(11) . . ?
O4 Pr1 O1 70.31(12) . . ?
O7 Pr1 O1 68.24(11) . . ?
O6 Pr1 O9 73.65(12) . . ?
O2 Pr1 O9 137.99(11) . . ?
O4 Pr1 O9 139.78(12) . . ?
O7 Pr1 O9 106.88(12) . . ?
O1 Pr1 O9 71.58(11) . . ?
O6 Pr1 O8 79.87(12) . . ?
O2 Pr1 O8 134.48(12) . . ?
O4 Pr1 O8 84.21(12) . . ?
O7 Pr1 O8 138.82(12) . . ?
O1 Pr1 O8 73.17(12) . . ?
O9 Pr1 O8 72.90(12) . . ?
O6 Pr1 O3 74.68(12) . . ?
O2 Pr1 O3 72.27(11) . . ?
O4 Pr1 O3 136.14(11) . . ?
O7 Pr1 O3 69.47(11) . . ?
O1 Pr1 O3 108.45(12) . . ?
O9 Pr1 O3 69.20(11) . . ?
O8 Pr1 O3 138.84(11) . . ?
O6 Pr1 O5 66.52(12) . . ?
O2 Pr1 O5 66.84(11) . . ?
O4 Pr1 O5 68.36(12) . . ?
O7 Pr1 O5 125.66(11) . . ?
O1 Pr1 O5 124.70(13) . . ?
O9 Pr1 O5 127.46(11) . . ?
O8 Pr1 O5 67.68(12) . . ?
O3 Pr1 O5 126.78(12) . . ?
Pr1 O1 H11 116(4) . . ?
Pr1 O1 H12 111(4) . . ?
H11 O1 H12 125(6) . . ?
Pr1 O2 H21 116(4) . . ?
Pr1 O2 H22 129(5) . . ?
H21 O2 H22 106(6) . . ?
Pr1 O3 H31 126(3) . . ?
Pr1 O3 H32 116(4) . . ?
H31 O3 H32 117(6) . . ?
Pr1 O4 H41 105(4) . . ?
Pr1 O4 H42 121(4) . . ?
H41 O4 H42 105(5) . . ?
Pr1 O5 H51 125(5) . . ?
Pr1 O5 H52 121(5) . . ?
H51 O5 H52 101(6) . . ?
Pr1 O6 H61 119(5) . . ?
Pr1 O6 H62 126(3) . . ?
H61 O6 H62 113(6) . . ?
Pr1 O7 H71 121(4) . . ?
Pr1 O7 H72 128(4) . . ?
H71 O7 H72 105(5) . . ?
Pr1 O8 H81 121(4) . . ?
Pr1 O8 H82 135(4) . . ?
H81 O8 H82 101(6) . . ?
Pr1 O9 H91 117(4) . . ?
Pr1 O9 H92 128(4) . . ?
H91 O9 H92 108(5) . . ?
C6 C1 C2 119.5(4) . . ?
C6 C1 C7 120.5(4) . . ?
C2 C1 C7 120.0(4) . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 118.7(4) . . ?
C2 C3 C8 121.2(4) . . ?
C4 C3 C8 120.0(4) . . ?
C5 C4 C3 121.1(4) . . ?
C5 C4 H4A 119.4 . . ?
C3 C4 H4A 119.4 . . ?
C6 C5 C4 119.5(5) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C1 121.1(4) . . ?
C5 C6 H6A 119.5 . . ?
C1 C6 H6A 119.5 . . ?
N4 C7 N1 108.5(4) . . ?
N4 C7 C1 126.2(4) . . ?
N1 C7 C1 125.2(4) . . ?
N2 N1 C7 108.5(4) . . ?
N2 N1 H1 113(3) . . ?
C7 N1 H1 138(3) . . ?
N3 N2 N1 106.3(4) . . ?
N2 N3 N4 110.9(4) . . ?
C7 N4 N3 105.8(4) . . ?
N5 C8 N8 111.5(4) . . ?
N5 C8 C3 123.5(4) . . ?
N8 C8 C3 124.9(4) . . ?
C8 N5 N6 105.0(4) . . ?
N7 N6 N5 109.6(3) . . ?
N6 N7 N8 109.5(4) . . ?
N7 N8 C8 104.3(4) . . ?
C10 C9 C14 119.5(4) . . ?
C10 C9 C15 121.1(4) . . ?
C14 C9 C15 119.4(4) . . ?
C9 C10 C11 119.7(4) . . ?
C9 C10 H10A 120.2 . . ?
C11 C10 H10A 120.2 . . ?
C12 C11 C10 119.4(4) . . ?
C12 C11 C16 121.1(4) . . ?
C10 C11 C16 119.4(4) . . ?
C13 C12 C11 121.3(4) . . ?
C13 C12 H12A 119.4 . . ?
C11 C12 H12A 119.4 . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 H13A 120.4 . . ?
C14 C13 H13A 120.4 . . ?
C13 C14 C9 120.9(4) . . ?
C13 C14 H14A 119.6 . . ?
C9 C14 H14A 119.6 . . ?
N12 C15 N9 111.2(4) . . ?
N12 C15 C9 125.6(4) . . ?
N9 C15 C9 123.2(4) . . ?
C15 N9 N10 105.4(4) . . ?
N11 N10 N9 108.8(4) . . ?
N10 N11 N12 109.7(3) . . ?
C15 N12 N11 104.8(4) . . ?
N16 C16 N13 107.8(4) . . ?
N16 C16 C11 127.3(4) . . ?
N13 C16 C11 124.9(4) . . ?
C16 N13 N14 108.7(4) . . ?
C16 N13 H13 135(4) . . ?
N14 N13 H13 116(4) . . ?
N15 N14 N13 106.4(4) . . ?
N14 N15 N16 110.7(4) . . ?
C16 N16 N15 106.3(4) . . ?
C22 C17 C18 120.1(4) . . ?
C22 C17 C23 120.6(4) . . ?
C18 C17 C23 119.3(4) . . ?
C19 C18 C17 119.4(4) . . ?
C19 C18 H18A 120.3 . . ?
C17 C18 H18A 120.3 . . ?
C20 C19 C18 119.7(4) . . ?
C20 C19 C24 118.9(4) . . ?
C18 C19 C24 121.4(4) . . ?
C21 C20 C19 120.8(4) . . ?
C21 C20 H20A 119.6 . . ?
C19 C20 H20A 119.6 . . ?
C22 C21 C20 119.7(4) . . ?
C22 C21 H21A 120.2 . . ?
C20 C21 H21A 120.2 . . ?
C21 C22 C17 120.3(4) . . ?
C21 C22 H22A 119.8 . . ?
C17 C22 H22A 119.8 . . ?
N20 C23 N17 107.8(4) . . ?
N20 C23 C17 126.8(4) . . ?
N17 C23 C17 125.5(4) . . ?
N18 N17 C23 108.7(3) . . ?
N18 N17 H17 117(3) . . ?
C23 N17 H17 134(3) . . ?
N19 N18 N17 106.0(3) . . ?
N18 N19 N20 111.2(3) . . ?
C23 N20 N19 106.4(3) . . ?
N21 C24 N24 111.6(4) . . ?
N21 C24 C19 122.8(4) . . ?
N24 C24 C19 125.7(4) . . ?
C24 N21 N22 105.5(3) . . ?
N23 N22 N21 108.5(4) . . ?
N22 N23 N24 110.3(3) . . ?
C24 N24 N23 104.2(3) . . ?
H111 O11 H112 110(5) . . ?
H121 O12 H122 107(6) . . ?
H131 O13 H132 109(5) . . ?
H141 O14 H142 125(6) . . ?
H151 O15 H152 102(5) . . ?
H161 O16 H162 108(6) . . ?
H171 O17 H172 105(5) . . ?
H181 O18 H182 111(6) . . ?
H191 O19 H192 113(5) . . ?

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 N21 0.77(5) 2.01(5) 2.767(5) 168(6) .
O1 H12 O15 0.81(3) 2.12(4) 2.888(5) 157(5) .
O2 H21 N6 0.81(3) 2.01(3) 2.801(5) 164(5) 4_565
O2 H22 N24 0.72(5) 2.14(5) 2.830(5) 160(6) 4_565
O3 H31 O11 0.87(5) 1.96(5) 2.770(5) 154(5) .
O3 H32 N18 0.73(5) 2.27(5) 2.932(5) 151(6) 4_465
O4 H41 O18 0.83(6) 1.90(6) 2.695(5) 161(5) .
O4 H42 N5 0.80(5) 2.07(5) 2.861(5) 167(5) 4_565
O5 H51 N6 0.75(6) 2.66(6) 3.299(5) 144(6) 4_565
O5 H52 O14 0.79(6) 2.18(6) 2.943(5) 165(6) .
O6 H61 O12 0.74(6) 1.96(6) 2.689(5) 170(6) .
O6 H62 O13 0.89(5) 1.89(6) 2.767(5) 171(5) .
O7 H71 N20 0.80(5) 2.04(5) 2.832(5) 177(5) 4_565
O7 H72 O16 0.76(5) 2.04(5) 2.770(5) 160(6) .
O8 H81 O14 0.79(5) 2.04(5) 2.823(5) 176(6) .
O8 H82 N10 0.75(5) 2.11(5) 2.840(5) 166(6) .
O9 H91 O11 0.77(5) 1.96(5) 2.725(5) 174(6) .
O9 H92 N22 0.82(3) 2.07(4) 2.875(5) 165(5) .
N1 H1 N7 0.96(5) 1.81(5) 2.772(6) 177(4) 1_655
N13 H13 N11 0.78(5) 1.98(5) 2.757(5) 173(5) 1_655
N17 H17 N23 0.80(4) 1.89(4) 2.682(5) 174(5) 1_655
O11 H111 O17 0.83(4) 1.98(4) 2.778(5) 161(6) .
O11 H112 N4 0.91(4) 1.95(4) 2.811(5) 158(5) 1_455
O12 H121 O18 0.87(4) 1.87(4) 2.731(6) 168(6) 1_455
O12 H122 N19 0.85(4) 2.13(4) 2.960(5) 168(6) 4_465
O13 H131 O17 0.99(4) 1.84(4) 2.794(5) 161(5) 2_445
O13 H132 N15 0.91(4) 1.91(4) 2.808(5) 167(5) 3_656
O14 H141 O16 0.81(4) 1.99(4) 2.761(5) 159(6) 2_545
O14 H142 N16 0.81(4) 2.04(4) 2.853(5) 175(6) 3_656
O15 H151 N19 0.85(4) 2.32(5) 3.010(5) 138(5) 4_565
O15 H152 O14 0.86(4) 2.17(4) 2.968(6) 154(5) 2
O16 H161 N12 0.79(4) 2.04(4) 2.833(5) 174(6) 4_565
O16 H162 O19 0.82(4) 2.19(5) 2.831(5) 135(5) .
O17 H171 O15 0.85(4) 2.09(4) 2.878(5) 153(5) 1_455
O17 H172 N8 0.88(4) 2.03(4) 2.898(5) 171(5) 1_455
O18 H181 O19 0.92(4) 1.73(4) 2.634(6) 167(6) 2_545
O18 H182 N9 0.86(4) 1.96(4) 2.804(5) 166(6) .
O19 H191 O13 1.05(4) 1.87(5) 2.873(6) 158(5) 2_455
O19 H192 N3 1.07(4) 1.81(4) 2.840(6) 160(5) 1_455

_diffrn_measured_fraction_theta_max 0.905
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.137

##################################################################

data_26015
_database_code_depnum_ccdc_archive 'CCDC 680458'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'H16 O8 Gd, 3(C8 H5 N8), 0.5(H5 O2), 7(H2 O), 0.5(H3 O2)'
_chemical_formula_sum            'C24 H49 Gd N24 O17'
_chemical_formula_weight         1103.12

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.9142(3)
_cell_length_b                   13.6521(5)
_cell_length_c                   16.9555(6)
_cell_angle_alpha                78.682(1)
_cell_angle_beta                 76.376(1)
_cell_angle_gamma                77.859(1)
_cell_volume                     2154.31(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10086
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.08

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.31
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1122
_exptl_absorpt_coefficient_mu    1.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_T_max  0.642
_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            12535
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         28.08
_reflns_number_total             9214
_reflns_number_gt                8664
_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.
Geometrical restraints were applied to O-H distances.
O13 and its inversion-related counterpart at -x, -y+2, -z form a (H3O2)⁻
anion; the disordered H⁺ between them, H132, could be refined.
Similarly, O15 and its counterpart at -x+1, -y+2, -z form a (H5O2)⁺
cation; again the intervening H-atom H153 could be refined.
;

_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)+(0.0463P)²+2.7181P] 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         9214
_refine_ls_number_parameters     691
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0802
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.011
_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
Gd1 Gd 0.046560(13) 0.259804(10) 0.768506(8) 0.01488(5) Uani 1 1 d D . .
O1 O 0.1976(2) 0.10112(16) 0.74962(14) 0.0205(4) Uani 1 1 d D . .
H11 H 0.223(4) 0.057(3) 0.786(2) 0.031 Uiso 1 1 d D . .
H12 H 0.180(4) 0.067(3) 0.719(2) 0.031 Uiso 1 1 d D . .
O2 O -0.1057(2) 0.14576(17) 0.77433(14) 0.0227(4) Uani 1 1 d D . .
H21 H -0.187(3) 0.157(3) 0.794(2) 0.034 Uiso 1 1 d D . .
H22 H -0.081(4) 0.106(3) 0.741(2) 0.034 Uiso 1 1 d D . .
O3 O 0.0760(2) 0.24877(17) 0.62604(13) 0.0202(4) Uani 1 1 d D . .
H31 H 0.014(4) 0.242(3) 0.603(2) 0.030 Uiso 1 1 d D . .
H32 H 0.153(3) 0.233(3) 0.597(2) 0.030 Uiso 1 1 d D . .
O4 O -0.1079(2) 0.25002(18) 0.90022(13) 0.0235(4) Uani 1 1 d D . .
H41 H -0.112(4) 0.293(3) 0.934(2) 0.035 Uiso 1 1 d D . .
H42 H -0.123(4) 0.187(2) 0.928(2) 0.035 Uiso 1 1 d D . .
O5 O 0.2675(2) 0.31703(18) 0.70180(14) 0.0246(5) Uani 1 1 d D . .
H51 H 0.260(4) 0.381(2) 0.685(3) 0.037 Uiso 1 1 d D . .
H52 H 0.325(4) 0.296(3) 0.660(2) 0.037 Uiso 1 1 d D . .
O6 O 0.2015(2) 0.2287(2) 0.86499(15) 0.0319(5) Uani 1 1 d D . .
H61 H 0.172(4) 0.168(2) 0.898(2) 0.048 Uiso 1 1 d D . .
H62 H 0.173(5) 0.267(3) 0.909(2) 0.048 Uiso 1 1 d D . .
O7 O -0.1540(2) 0.36900(18) 0.72469(15) 0.0260(5) Uani 1 1 d D . .
H71 H -0.198(4) 0.354(3) 0.695(2) 0.039 Uiso 1 1 d D . .
H72 H -0.213(4) 0.397(3) 0.760(2) 0.039 Uiso 1 1 d D . .
O8 O 0.0288(3) 0.42889(17) 0.79991(14) 0.0267(5) Uani 1 1 d D . .
H81 H -0.018(4) 0.463(2) 0.837(2) 0.040 Uiso 1 1 d D . .
H82 H 0.115(3) 0.416(3) 0.821(2) 0.040 Uiso 1 1 d D . .
C1 C 0.4648(3) 0.4212(2) 0.09094(16) 0.0150(5) Uani 1 1 d . . .
C2 C 0.3226(3) 0.4309(2) 0.08794(16) 0.0155(5) Uani 1 1 d . . .
H2A H 0.2550 0.4829 0.1118 0.019 Uiso 1 1 calc R . .
C3 C 0.2805(3) 0.3640(2) 0.04982(16) 0.0152(5) Uani 1 1 d . . .
C4 C 0.3811(3) 0.2886(2) 0.01433(17) 0.0181(5) Uani 1 1 d . . .
H4A H 0.3527 0.2426 -0.0113 0.022 Uiso 1 1 calc R . .
C5 C 0.5229(3) 0.2802(2) 0.01612(18) 0.0204(6) Uani 1 1 d . . .
H5A H 0.5908 0.2295 -0.0092 0.024 Uiso 1 1 calc R . .
C6 C 0.5650(3) 0.3457(2) 0.05485(18) 0.0186(6) Uani 1 1 d . . .
H6A H 0.6615 0.3394 0.0568 0.022 Uiso 1 1 calc R . .
C7 C 0.5063(3) 0.4921(2) 0.13132(17) 0.0173(5) Uani 1 1 d . . .
N1 N 0.4187(3) 0.5624(2) 0.17119(17) 0.0241(5) Uani 1 1 d . . .
N2 N 0.5019(3) 0.6140(2) 0.19454(18) 0.0283(6) Uani 1 1 d D . .
N3 N 0.6344(3) 0.5768(2) 0.17204(18) 0.0258(6) Uani 1 1 d . . .
N4 N 0.6384(3) 0.50039(19) 0.13229(15) 0.0184(5) Uani 1 1 d . . .
H4 H 0.720(4) 0.468(3) 0.111(2) 0.022 Uiso 1 1 d . . .
C8 C 0.1310(3) 0.3719(2) 0.04780(16) 0.0138(5) Uani 1 1 d . . .
N5 N 0.0224(2) 0.42813(18) 0.09145(14) 0.0155(4) Uani 1 1 d . . .
N6 N -0.0918(2) 0.41034(18) 0.07047(15) 0.0168(5) Uani 1 1 d . . .
N7 N -0.0539(2) 0.34645(18) 0.01691(15) 0.0173(5) Uani 1 1 d . . .
N8 N 0.0869(2) 0.32067(17) 0.00163(14) 0.0164(5) Uani 1 1 d . . .
C9 C 0.2075(3) 0.0352(2) 0.38375(17) 0.0154(5) Uani 1 1 d . . .
C10 C 0.2487(3) 0.0919(2) 0.43132(16) 0.0152(5) Uani 1 1 d . . .
H10A H 0.1796 0.1316 0.4667 0.018 Uiso 1 1 calc R . .
C11 C 0.3917(3) 0.0899(2) 0.42678(16) 0.0151(5) Uani 1 1 d . . .
C12 C 0.4937(3) 0.0304(2) 0.37560(17) 0.0175(5) Uani 1 1 d . . .
H12A H 0.5910 0.0293 0.3724 0.021 Uiso 1 1 calc R . .
C13 C 0.4521(3) -0.0271(2) 0.32953(18) 0.0199(6) Uani 1 1 d . . .
H13A H 0.5211 -0.0683 0.2952 0.024 Uiso 1 1 calc R . .
C14 C 0.3103(3) -0.0245(2) 0.33342(18) 0.0189(6) Uani 1 1 d . . .
H14A H 0.2828 -0.0639 0.3015 0.023 Uiso 1 1 calc R . .
C15 C 0.0579(3) 0.0397(2) 0.38328(16) 0.0151(5) Uani 1 1 d . . .
N9 N 0.0156(2) -0.01421(18) 0.33854(15) 0.0174(5) Uani 1 1 d . . .
N10 N -0.1253(2) 0.01209(18) 0.35196(15) 0.0175(5) Uani 1 1 d . . .
N11 N -0.1650(2) 0.07904(18) 0.40261(14) 0.0166(5) Uani 1 1 d . . .
N12 N -0.0518(2) 0.09866(18) 0.42363(14) 0.0162(5) Uani 1 1 d . . .
C16 C 0.4341(3) 0.1519(2) 0.47493(17) 0.0157(5) Uani 1 1 d . . .
N13 N 0.3489(2) 0.20626(19) 0.52963(15) 0.0189(5) Uani 1 1 d . . .
N14 N 0.4337(3) 0.2506(2) 0.55887(16) 0.0216(5) Uani 1 1 d . . .
N15 N 0.5648(3) 0.22542(19) 0.52438(16) 0.0208(5) Uani 1 1 d . . .
N16 N 0.5666(3) 0.16373(19) 0.47154(15) 0.0168(5) Uani 1 1 d . . .
H16 H 0.638(4) 0.142(3) 0.449(2) 0.020 Uiso 1 1 d . . .
C17 C 0.3668(3) 0.2905(2) 0.28348(17) 0.0173(5) Uani 1 1 d . . .
C18 C 0.3256(3) 0.2321(2) 0.23733(17) 0.0159(5) Uani 1 1 d . . .
H18A H 0.3948 0.1902 0.2037 0.019 Uiso 1 1 calc R . .
C19 C 0.1830(3) 0.2354(2) 0.24063(17) 0.0168(5) Uani 1 1 d . . .
C20 C 0.0813(3) 0.2966(2) 0.29009(19) 0.0227(6) Uani 1 1 d . . .
H20A H -0.0159 0.2989 0.2922 0.027 Uiso 1 1 calc R . .
C21 C 0.1226(3) 0.3538(3) 0.3360(2) 0.0286(7) Uani 1 1 d . . .
H21A H 0.0534 0.3951 0.3702 0.034 Uiso 1 1 calc R . .
C22 C 0.2639(3) 0.3515(2) 0.3325(2) 0.0242(6) Uani 1 1 d . . .
H22A H 0.2911 0.3919 0.3638 0.029 Uiso 1 1 calc R . .
C23 C 0.5156(3) 0.2914(2) 0.28066(17) 0.0166(5) Uani 1 1 d . . .
N17 N 0.5572(3) 0.35258(19) 0.31968(15) 0.0197(5) Uani 1 1 d . . .
N18 N 0.6985(3) 0.33243(19) 0.30114(16) 0.0214(5) Uani 1 1 d . . .
N19 N 0.7391(3) 0.26207(19) 0.25318(16) 0.0205(5) Uani 1 1 d . . .
N20 N 0.6261(2) 0.23378(19) 0.23908(15) 0.0184(5) Uani 1 1 d . . .
C24 C 0.1397(3) 0.1752(2) 0.19101(17) 0.0170(5) Uani 1 1 d . . .
N21 N 0.2250(3) 0.11192(18) 0.14323(15) 0.0192(5) Uani 1 1 d . . .
N22 N 0.1398(3) 0.07496(19) 0.10846(17) 0.0227(5) Uani 1 1 d . . .
N23 N 0.0091(3) 0.11266(19) 0.13299(16) 0.0227(5) Uani 1 1 d . . .
N24 N 0.0073(3) 0.17586(19) 0.18502(16) 0.0190(5) Uani 1 1 d . . .
H24 H -0.070(4) 0.207(3) 0.209(2) 0.023 Uiso 1 1 d . . .
O11 O 0.6907(2) 1.05998(18) 0.14586(15) 0.0236(5) Uani 1 1 d D . .
H111 H 0.675(4) 1.109(2) 0.173(2) 0.035 Uiso 1 1 d D . .
H112 H 0.727(5) 1.070(4) 0.109(3) 0.035 Uiso 1 1 d . . .
O12 O 0.1949(3) 0.51584(18) 0.66144(16) 0.0312(5) Uani 1 1 d D . .
H121 H 0.212(5) 0.527(3) 0.6027(19) 0.047 Uiso 1 1 d D . .
H122 H 0.231(5) 0.572(3) 0.672(2) 0.047 Uiso 1 1 d D . .
O13 O 0.1301(3) 0.93499(18) 0.00976(14) 0.0279(5) Uani 1 1 d D . .
H131 H 0.157(5) 0.964(3) 0.038(3) 0.042 Uiso 1 1 d D . .
H132 H 0.053(9) 0.971(7) -0.004(6) 0.042 Uiso 0.50 1 d P . .
O14 O 0.1069(2) 0.75462(19) 0.46983(16) 0.0300(5) Uani 1 1 d D . .
H141 H 0.099(5) 0.794(3) 0.510(2) 0.045 Uiso 1 1 d D . .
H142 H 0.135(5) 0.789(3) 0.4238(19) 0.045 Uiso 1 1 d D . .
O15 O 0.4877(3) 1.0003(2) 0.08476(17) 0.0336(6) Uani 1 1 d D . .
H151 H 0.407(3) 1.040(3) 0.103(3) 0.050 Uiso 1 1 d D . .
H152 H 0.563(3) 0.994(4) 0.100(3) 0.050 Uiso 1 1 d D . .
H153 H 0.498(11) 1.015(8) 0.029(6) 0.050 Uiso 0.50 1 d P . .
O16 O 0.3915(3) 0.8293(2) 0.18645(19) 0.0428(7) Uani 1 1 d D . .
O17 O 0.4302(3) 0.4998(2) 0.43410(18) 0.0439(7) Uani 1 1 d . . .
O18 O 0.3307(3) 0.6895(2) 0.35192(16) 0.0404(6) Uani 1 1 d . . .
O19 O 0.1302(3) 0.5392(2) 0.50604(18) 0.0472(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O2 2.360(2) . ?
Gd1 O4 2.389(2) . ?
Gd1 O1 2.392(2) . ?
Gd1 O3 2.395(2) . ?
Gd1 O7 2.396(2) . ?
Gd1 O6 2.419(2) . ?
Gd1 O5 2.427(2) . ?
Gd1 O8 2.431(2) . ?
O1 H11 0.82(3) . ?
O1 H12 0.84(3) . ?
O2 H21 0.79(3) . ?
O2 H22 0.82(3) . ?
O3 H31 0.83(3) . ?
O3 H32 0.82(3) . ?
O4 H41 0.88(3) . ?
O4 H42 0.92(3) . ?
O5 H51 0.85(3) . ?
O5 H52 0.85(3) . ?
O6 H61 0.96(3) . ?
O6 H62 0.95(3) . ?
O7 H71 0.82(3) . ?
O7 H72 0.83(3) . ?
O8 H81 0.84(3) . ?
O8 H82 0.97(3) . ?
C1 C6 1.398(4) . ?
C1 C2 1.400(4) . ?
C1 C7 1.461(4) . ?
C2 C3 1.395(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.395(4) . ?
C3 C8 1.472(4) . ?
C4 C5 1.393(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.387(4) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 N1 1.326(4) . ?
C7 N4 1.342(4) . ?
N1 N2 1.357(4) . ?
N2 N3 1.299(4) . ?
N3 N4 1.337(3) . ?
N4 H4 0.87(4) . ?
C8 N5 1.340(3) . ?
C8 N8 1.341(3) . ?
N5 N6 1.344(3) . ?
N6 N7 1.319(3) . ?
N7 N8 1.341(3) . ?
C9 C14 1.395(4) . ?
C9 C10 1.396(4) . ?
C9 C15 1.474(4) . ?
C10 C11 1.397(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.398(4) . ?
C11 C16 1.463(4) . ?
C12 C13 1.387(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.385(4) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 N9 1.338(4) . ?
C15 N12 1.340(3) . ?
N9 N10 1.343(3) . ?
N10 N11 1.313(3) . ?
N11 N12 1.346(3) . ?
C16 N13 1.327(3) . ?
C16 N16 1.343(4) . ?
N13 N14 1.360(3) . ?
N14 N15 1.297(3) . ?
N15 N16 1.340(3) . ?
N16 H16 0.75(4) . ?
C17 C22 1.393(4) . ?
C17 C18 1.395(4) . ?
C17 C23 1.468(4) . ?
C18 C19 1.394(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.393(4) . ?
C19 C24 1.469(4) . ?
C20 C21 1.382(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.382(4) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 N17 1.340(4) . ?
C23 N20 1.345(4) . ?
N17 N18 1.342(3) . ?
N18 N19 1.318(4) . ?
N19 N20 1.343(3) . ?
C24 N21 1.327(4) . ?
C24 N24 1.338(4) . ?
N21 N22 1.358(3) . ?
N22 N23 1.292(4) . ?
N23 N24 1.345(3) . ?
N24 H24 0.85(4) . ?
O11 H111 0.85(2) . ?
O11 H112 0.64(4) . ?
O12 H121 0.96(3) . ?
O12 H122 0.97(3) . ?
O13 H131 0.80(3) . ?
O13 H132 0.88(8) . ?
O14 H141 0.92(3) . ?
O14 H142 0.84(3) . ?
O15 H151 0.89(3) . ?
O15 H152 0.83(3) . ?
O15 H153 0.92(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Gd1 O4 71.71(7) . . ?
O2 Gd1 O1 74.76(7) . . ?
O4 Gd1 O1 111.57(8) . . ?
O2 Gd1 O3 78.68(8) . . ?
O4 Gd1 O3 146.27(7) . . ?
O1 Gd1 O3 74.62(7) . . ?
O2 Gd1 O7 77.14(8) . . ?
O4 Gd1 O7 83.41(8) . . ?
O1 Gd1 O7 141.47(8) . . ?
O3 Gd1 O7 74.43(8) . . ?
O2 Gd1 O6 120.73(9) . . ?
O4 Gd1 O6 75.57(8) . . ?
O1 Gd1 O6 73.38(8) . . ?
O3 Gd1 O6 135.37(7) . . ?
O7 Gd1 O6 144.82(8) . . ?
O2 Gd1 O5 146.64(7) . . ?
O4 Gd1 O5 138.83(7) . . ?
O1 Gd1 O5 79.44(8) . . ?
O3 Gd1 O5 74.33(7) . . ?
O7 Gd1 O5 113.17(8) . . ?
O6 Gd1 O5 69.90(9) . . ?
O2 Gd1 O8 137.98(8) . . ?
O4 Gd1 O8 78.84(8) . . ?
O1 Gd1 O8 145.61(8) . . ?
O3 Gd1 O8 115.55(8) . . ?
O7 Gd1 O8 70.18(8) . . ?
O6 Gd1 O8 78.19(8) . . ?
O5 Gd1 O8 72.83(8) . . ?
Gd1 O1 H11 126(3) . . ?
Gd1 O1 H12 118(3) . . ?
H11 O1 H12 102(4) . . ?
Gd1 O2 H21 122(3) . . ?
Gd1 O2 H22 117(3) . . ?
H21 O2 H22 117(4) . . ?
Gd1 O3 H31 126(3) . . ?
Gd1 O3 H32 122(3) . . ?
H31 O3 H32 109(4) . . ?
Gd1 O4 H41 121(3) . . ?
Gd1 O4 H42 118(3) . . ?
H41 O4 H42 112(4) . . ?
Gd1 O5 H51 114(3) . . ?
Gd1 O5 H52 127(3) . . ?
H51 O5 H52 99(4) . . ?
Gd1 O6 H61 98(2) . . ?
Gd1 O6 H62 117(3) . . ?
H61 O6 H62 95(3) . . ?
Gd1 O7 H71 123(3) . . ?
Gd1 O7 H72 117(3) . . ?
H71 O7 H72 107(4) . . ?
Gd1 O8 H81 137(3) . . ?
Gd1 O8 H82 96.9(18) . . ?
H81 O8 H82 94(3) . . ?
C6 C1 C2 120.3(3) . . ?
C6 C1 C7 120.8(2) . . ?
C2 C1 C7 118.8(2) . . ?
C3 C2 C1 119.8(2) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C4 C3 C2 119.5(2) . . ?
C4 C3 C8 120.1(2) . . ?
C2 C3 C8 120.4(2) . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
C6 C5 C4 120.1(3) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C1 119.6(3) . . ?
C5 C6 H6A 120.2 . . ?
C1 C6 H6A 120.2 . . ?
N1 C7 N4 108.0(2) . . ?
N1 C7 C1 125.4(3) . . ?
N4 C7 C1 126.5(3) . . ?
C7 N1 N2 105.5(2) . . ?
N3 N2 N1 111.2(2) . . ?
N2 N3 N4 106.0(2) . . ?
N3 N4 C7 109.2(2) . . ?
N3 N4 H4 119(2) . . ?
C7 N4 H4 132(2) . . ?
N5 C8 N8 111.4(2) . . ?
N5 C8 C3 125.7(2) . . ?
N8 C8 C3 122.9(2) . . ?
C8 N5 N6 104.3(2) . . ?
N7 N6 N5 110.2(2) . . ?
N6 N7 N8 108.8(2) . . ?
C8 N8 N7 105.3(2) . . ?
C14 C9 C10 119.4(2) . . ?
C14 C9 C15 119.1(2) . . ?
C10 C9 C15 121.5(2) . . ?
C9 C10 C11 119.9(2) . . ?
C9 C10 H10A 120.1 . . ?
C11 C10 H10A 120.1 . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 C16 119.6(2) . . ?
C12 C11 C16 120.2(2) . . ?
C13 C12 C11 119.6(3) . . ?
C13 C12 H12A 120.2 . . ?
C11 C12 H12A 120.2 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C13 C14 C9 120.7(3) . . ?
C13 C14 H14A 119.7 . . ?
C9 C14 H14A 119.7 . . ?
N9 C15 N12 111.3(2) . . ?
N9 C15 C9 122.7(2) . . ?
N12 C15 C9 126.0(2) . . ?
C15 N9 N10 105.3(2) . . ?
N11 N10 N9 108.9(2) . . ?
N10 N11 N12 110.0(2) . . ?
C15 N12 N11 104.5(2) . . ?
N13 C16 N16 107.9(2) . . ?
N13 C16 C11 126.2(2) . . ?
N16 C16 C11 125.9(2) . . ?
C16 N13 N14 105.7(2) . . ?
N15 N14 N13 111.0(2) . . ?
N14 N15 N16 106.2(2) . . ?
N15 N16 C16 109.1(2) . . ?
N15 N16 H16 117(3) . . ?
C16 N16 H16 134(3) . . ?
C22 C17 C18 119.2(3) . . ?
C22 C17 C23 118.8(3) . . ?
C18 C17 C23 122.0(3) . . ?
C19 C18 C17 120.0(3) . . ?
C19 C18 H18A 120.0 . . ?
C17 C18 H18A 120.0 . . ?
C20 C19 C18 120.1(3) . . ?
C20 C19 C24 119.9(3) . . ?
C18 C19 C24 119.9(2) . . ?
C21 C20 C19 119.7(3) . . ?
C21 C20 H20A 120.2 . . ?
C19 C20 H20A 120.2 . . ?
C20 C21 C22 120.4(3) . . ?
C20 C21 H21A 119.8 . . ?
C22 C21 H21A 119.8 . . ?
C21 C22 C17 120.5(3) . . ?
C21 C22 H22A 119.7 . . ?
C17 C22 H22A 119.7 . . ?
N17 C23 N20 111.6(2) . . ?
N17 C23 C17 122.8(3) . . ?
N20 C23 C17 125.5(3) . . ?
C23 N17 N18 104.9(2) . . ?
N19 N18 N17 109.2(2) . . ?
N18 N19 N20 110.1(2) . . ?
N19 N20 C23 104.2(2) . . ?
N21 C24 N24 108.0(2) . . ?
N21 C24 C19 126.1(2) . . ?
N24 C24 C19 125.9(3) . . ?
C24 N21 N22 105.7(2) . . ?
N23 N22 N21 111.1(2) . . ?
N22 N23 N24 106.2(2) . . ?
C24 N24 N23 109.0(2) . . ?
C24 N24 H24 131(3) . . ?
N23 N24 H24 120(3) . . ?
H111 O11 H112 112(5) . . ?
H121 O12 H122 102(3) . . ?
H131 O13 H132 109(7) . . ?
H141 O14 H142 108(3) . . ?
H151 O15 H152 126(4) . . ?
H151 O15 H153 104(7) . . ?
H152 O15 H153 113(7) . . ?

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 O11 0.82(3) 1.95(3) 2.752(3) 168(4) 2_666
O1 H12 N10 0.84(3) 1.99(3) 2.821(3) 176(4) 2_556
O2 H21 O16 0.79(3) 1.95(3) 2.717(3) 163(4) 2_566
O2 H22 N9 0.82(3) 1.93(3) 2.749(3) 178(4) 2_556
O3 H31 O14 0.83(3) 1.90(3) 2.718(3) 167(4) 2_566
O3 H32 N13 0.82(3) 2.00(3) 2.821(3) 174(4) .
O4 H41 N7 0.88(3) 1.95(3) 2.784(3) 156(4) 1_556
O4 H42 O13 0.92(3) 1.79(3) 2.706(3) 171(4) 2_566
O5 H51 O12 0.85(3) 1.82(3) 2.652(3) 165(4) .
O5 H52 N14 0.85(3) 1.95(3) 2.786(3) 172(4) .
O6 H62 N8 0.95(3) 1.81(3) 2.745(3) 166(4) 1_556
O7 H71 O18 0.82(3) 1.93(3) 2.732(3) 167(4) 2_566
O7 H72 N1 0.83(3) 2.12(3) 2.883(3) 154(4) 2_566
O8 H81 N5 0.84(3) 2.08(3) 2.831(3) 148(4) 2_566
O8 H82 N3 0.97(3) 2.54(3) 3.465(4) 159(3) 2_666
N4 H4 N6 0.87(4) 1.89(4) 2.751(3) 172(3) 1_655
N16 H16 N11 0.75(4) 2.00(4) 2.749(3) 172(4) 1_655
N24 H24 N19 0.85(4) 1.91(4) 2.750(4) 169(4) 1_455
O11 H111 N20 0.85(2) 2.13(3) 2.982(3) 177(4) 1_565
O11 H112 O13 0.64(4) 2.18(5) 2.810(3) 165(5) 2_675
O12 H121 O19 0.96(3) 1.96(3) 2.799(4) 146(4) .
O12 H122 N18 0.97(3) 1.79(3) 2.750(3) 175(4) 2_666
O13 H131 N22 0.80(3) 2.06(4) 2.805(3) 155(4) 1_565
O13 H132 O13 0.88(8) 2.00(8) 2.856(5) 166(9) 2_575
O14 H141 N12 0.92(3) 1.94(3) 2.840(3) 165(4) 2_566
O15 H151 N21 0.89(3) 1.90(3) 2.792(3) 174(4) 1_565
O15 H152 O11 0.83(3) 2.06(4) 2.791(3) 147(4) .
O15 H153 O15 0.92(9) 1.94(9) 2.828(5) 161(9) 2_675

_diffrn_measured_fraction_theta_max 0.878
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         2.120
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.106


