# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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data_a
_database_code_depnum_ccdc_archive 'CCDC 889167'
#TrackingRef '889167.CIF'
_database_code_depnum_ccdc_archive 'CCDC 913863'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H25 N6 O13 Tb'
_chemical_formula_weight         632.31
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   20.507(9)
_cell_length_b                   16.630(7)
_cell_length_c                   14.456(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.214(7)
_cell_angle_gamma                90.00
_cell_volume                     4531(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6196
_cell_measurement_theta_min      2.0997
_cell_measurement_theta_max      27.4932
_exptl_crystal_description       needlelike
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.0500
_exptl_crystal_size_min          0.0400
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2512
_exptl_absorpt_coefficient_mu    3.197
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7572
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
RIGAKU/MSC(2004), CrystalClear Version 1.3.6,
Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(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  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17596
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         27.47
_reflns_number_total             5173
_reflns_number_gt                4215
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+43.4247P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5173
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1838
_refine_ls_wR_factor_gt          0.1687
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.817256(19) -0.20862(2) 0.94796(3) 0.0227(2) Uani 1 1 d . . .
C1 C 0.8655(4) 0.2424(5) 0.6596(6) 0.0227(16) Uani 1 1 d . . .
C2 C 0.9192(6) 0.3283(7) 0.8155(8) 0.041(2) Uani 1 1 d . . .
H2A H 0.9350 0.3287 0.8875 0.061 Uiso 1 1 calc R . .
H2B H 0.8818 0.3669 0.7869 0.061 Uiso 1 1 calc R . .
H2C H 0.9581 0.3419 0.7973 0.061 Uiso 1 1 calc R . .
C3 C 1.0692(7) -0.2154(8) 0.9343(15) 0.076(5) Uani 1 1 d . . .
H3A H 1.1011 -0.2009 0.9031 0.114 Uiso 1 1 calc R . .
H3B H 1.0567 -0.2712 0.9217 0.114 Uiso 1 1 calc R . .
H3C H 1.0919 -0.2065 1.0055 0.114 Uiso 1 1 calc R . .
C4 C 0.9477(5) -0.1820(7) 0.9328(8) 0.035(2) Uani 1 1 d . . .
C5 C 0.7806(5) -0.1466(5) 0.7542(7) 0.0288(19) Uani 1 1 d . . .
C6 C 0.7360(4) 0.1013(5) 0.5673(6) 0.0265(18) Uani 1 1 d . . .
C7 C 0.8923(5) 0.2465(6) 0.7763(7) 0.031(2) Uani 1 1 d . . .
H7A H 0.8519 0.2348 0.7943 0.037 Uiso 1 1 calc R . .
C8 C 1.0030(6) -0.1646(7) 0.8911(10) 0.047(3) Uani 1 1 d . . .
H8A H 0.9809 -0.1783 0.8194 0.057 Uiso 1 1 calc R . .
C9 C 0.7823(5) -0.1080(6) 0.6569(7) 0.033(2) Uani 1 1 d . . .
H9A H 0.8191 -0.1339 0.6412 0.040 Uiso 1 1 calc R . .
H9B H 0.7373 -0.1178 0.6013 0.040 Uiso 1 1 calc R . .
C10 C 0.7362(4) 0.0320(6) 0.6368(7) 0.0296(19) Uani 1 1 d . . .
H10A H 0.7338 0.0546 0.6973 0.036 Uiso 1 1 calc R . .
H10B H 0.6933 0.0007 0.6036 0.036 Uiso 1 1 calc R . .
C11 C 0.9308(4) 0.1072(6) 0.8059(6) 0.0272(18) Uani 1 1 d . . .
C12 C 0.9702(4) -0.0254(6) 0.8408(7) 0.0294(19) Uani 1 1 d . . .
C13 C 0.8593(4) 0.0050(6) 0.7296(6) 0.0270(18) Uani 1 1 d . . .
N1 N 0.9847(4) 0.0545(5) 0.8569(6) 0.0296(17) Uani 1 1 d . . .
H1A H 1.0257 0.0713 0.8971 0.036 Uiso 1 1 calc R . .
N2 N 0.9087(4) -0.0533(5) 0.7739(6) 0.0288(16) Uani 1 1 d . . .
N3 N 0.8682(4) 0.0840(5) 0.7444(5) 0.0268(16) Uani 1 1 d . . .
N4 N 0.9462(4) 0.1851(5) 0.8230(6) 0.0304(17) Uani 1 1 d . . .
H4A H 0.9885 0.1993 0.8620 0.036 Uiso 1 1 calc R . .
N5 N 1.0199(4) -0.0792(5) 0.8950(7) 0.037(2) Uani 1 1 d . . .
H5A H 1.0619 -0.0629 0.9322 0.044 Uiso 1 1 calc R . .
N6 N 0.7957(4) -0.0216(5) 0.6663(6) 0.0276(16) Uani 1 1 d . . .
O1 O 0.9070(3) 0.2210(4) 0.6202(5) 0.0260(13) Uani 1 1 d . . .
O2 O 0.8032(3) 0.2621(4) 0.6076(4) 0.0237(12) Uani 1 1 d . . .
O3 O 0.9252(3) -0.2532(4) 0.9267(6) 0.0392(16) Uani 1 1 d . . .
O4 O 0.9211(3) -0.1261(4) 0.9686(5) 0.0324(14) Uani 1 1 d . . .
O5 O 0.7737(3) -0.1010(4) 0.8210(4) 0.0272(13) Uani 1 1 d . . .
O6 O 0.7901(4) -0.2207(4) 0.7666(5) 0.0385(17) Uani 1 1 d . . .
O7 O 0.6906(3) 0.1540(4) 0.5611(5) 0.0304(14) Uani 1 1 d . . .
O8 O 0.7784(3) 0.1027(4) 0.5245(4) 0.0263(13) Uani 1 1 d . . .
O11W O 0.7639(6) -0.3449(7) 0.6183(8) 0.080(3) Uani 1 1 d . . .
O12W O 0.6556(6) 0.0142(7) 0.8240(10) 0.096(4) Uani 1 1 d . . .
O13W O 0.9382(6) -0.4208(8) 0.8828(13) 0.122(6) Uani 1 1 d . . .
O14W O 1.1520(4) -0.0423(5) 1.0436(7) 0.065(3) Uani 1 1 d . . .
O15W O 0.5762(7) -0.0116(14) 0.4443(12) 0.163(8) Uani 1 1 d . . .
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
Tb1 0.0156(2) 0.0267(3) 0.0251(3) -0.00023(15) 0.00715(17) -0.00301(14)
C1 0.016(3) 0.022(4) 0.025(4) -0.001(3) 0.003(3) 0.000(3)
C2 0.033(5) 0.053(7) 0.031(5) -0.002(4) 0.007(4) 0.000(5)
C3 0.049(8) 0.061(9) 0.140(15) 0.035(9) 0.062(10) 0.023(6)
C4 0.019(4) 0.047(6) 0.040(5) 0.013(4) 0.010(4) 0.005(4)
C5 0.024(4) 0.030(5) 0.031(5) 0.007(4) 0.010(4) 0.005(3)
C6 0.020(4) 0.027(4) 0.027(4) -0.003(3) 0.004(3) -0.003(3)
C7 0.023(4) 0.044(6) 0.025(4) 0.000(4) 0.007(4) 0.002(4)
C8 0.034(5) 0.044(6) 0.076(8) 0.018(6) 0.035(5) 0.009(5)
C9 0.029(4) 0.034(5) 0.030(5) 0.007(4) 0.006(4) 0.003(4)
C10 0.020(4) 0.037(5) 0.027(4) 0.006(4) 0.004(3) -0.007(4)
C11 0.022(4) 0.034(5) 0.024(4) 0.008(3) 0.008(3) -0.001(3)
C12 0.020(4) 0.036(5) 0.034(5) 0.014(4) 0.012(4) 0.004(3)
C13 0.019(4) 0.038(5) 0.025(4) 0.010(4) 0.010(3) 0.000(3)
N1 0.014(3) 0.035(4) 0.034(4) 0.008(3) 0.004(3) 0.003(3)
N2 0.020(3) 0.034(4) 0.033(4) 0.012(3) 0.011(3) 0.004(3)
N3 0.014(3) 0.035(4) 0.028(4) 0.009(3) 0.005(3) -0.001(3)
N4 0.016(3) 0.034(4) 0.031(4) 0.005(3) -0.001(3) -0.004(3)
N5 0.015(3) 0.041(5) 0.053(5) 0.022(4) 0.012(3) 0.009(3)
N6 0.024(3) 0.027(4) 0.029(4) 0.004(3) 0.008(3) -0.002(3)
O1 0.016(3) 0.033(3) 0.029(3) 0.002(2) 0.008(2) 0.005(2)
O2 0.013(2) 0.029(3) 0.026(3) 0.001(2) 0.005(2) 0.005(2)
O3 0.027(3) 0.041(4) 0.053(4) 0.000(3) 0.019(3) -0.005(3)
O4 0.018(3) 0.040(4) 0.034(3) 0.005(3) 0.005(3) -0.002(3)
O5 0.026(3) 0.030(3) 0.026(3) 0.002(2) 0.010(2) 0.001(2)
O6 0.058(5) 0.028(4) 0.035(4) 0.000(3) 0.024(4) 0.000(3)
O7 0.029(3) 0.029(3) 0.037(4) 0.004(3) 0.018(3) 0.005(3)
O8 0.022(3) 0.029(3) 0.029(3) 0.007(2) 0.010(2) 0.004(2)
O11W 0.082(7) 0.072(7) 0.089(8) -0.034(6) 0.037(6) -0.023(6)
O12W 0.062(7) 0.086(8) 0.134(11) -0.013(8) 0.034(7) -0.005(6)
O13W 0.059(7) 0.097(10) 0.201(16) -0.024(10) 0.040(9) 0.024(7)
O14W 0.041(4) 0.046(5) 0.080(7) -0.003(4) -0.007(4) 0.011(4)
O15W 0.057(7) 0.28(2) 0.142(14) -0.089(15) 0.029(8) -0.002(11)
_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
Tb1 O7 2.290(7) 4_646 ?
Tb1 O2 2.328(5) 4_646 ?
Tb1 O8 2.379(6) 6_556 ?
Tb1 O4 2.451(6) . ?
Tb1 O1 2.453(6) 6_556 ?
Tb1 O6 2.464(7) . ?
Tb1 O5 2.465(6) . ?
Tb1 O3 2.466(7) . ?
Tb1 O2 2.593(6) 6_556 ?
Tb1 C5 2.796(9) . ?
Tb1 C4 2.803(9) . ?
Tb1 C1 2.876(8) 6_556 ?
C1 O2 1.244(9) . ?
C1 O1 1.249(10) . ?
C1 C7 1.556(12) . ?
C1 Tb1 2.876(8) 6 ?
C2 C7 1.494(15) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C8 1.510(16) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 O3 1.261(13) . ?
C4 O4 1.286(13) . ?
C4 C8 1.508(13) . ?
C5 O6 1.249(11) . ?
C5 O5 1.278(11) . ?
C5 C9 1.559(12) . ?
C6 O8 1.249(10) . ?
C6 O7 1.257(10) . ?
C6 C10 1.529(12) . ?
C7 N4 1.461(12) . ?
C7 H7A 0.9800 . ?
C8 N5 1.457(14) . ?
C8 H8A 0.9800 . ?
C9 N6 1.458(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N6 1.434(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N3 1.297(11) . ?
C11 N4 1.333(12) . ?
C11 N1 1.375(11) . ?
C12 N2 1.334(12) . ?
C12 N5 1.350(11) . ?
C12 N1 1.362(12) . ?
C13 N3 1.333(12) . ?
C13 N6 1.340(11) . ?
C13 N2 1.364(11) . ?
N1 H1A 0.8600 . ?
N4 H4A 0.8600 . ?
N5 H5A 0.8600 . ?
O1 Tb1 2.453(6) 6 ?
O2 Tb1 2.328(5) 4_656 ?
O2 Tb1 2.593(6) 6 ?
O7 Tb1 2.290(7) 4_656 ?
O8 Tb1 2.379(6) 6 ?
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
O7 Tb1 O2 74.4(2) 4_646 4_646 ?
O7 Tb1 O8 137.4(2) 4_646 6_556 ?
O2 Tb1 O8 79.1(2) 4_646 6_556 ?
O7 Tb1 O4 127.1(2) 4_646 . ?
O2 Tb1 O4 155.8(2) 4_646 . ?
O8 Tb1 O4 87.9(2) 6_556 . ?
O7 Tb1 O1 89.0(2) 4_646 6_556 ?
O2 Tb1 O1 127.0(2) 4_646 6_556 ?
O8 Tb1 O1 81.1(2) 6_556 6_556 ?
O4 Tb1 O1 69.8(2) . 6_556 ?
O7 Tb1 O6 82.9(2) 4_646 . ?
O2 Tb1 O6 81.5(2) 4_646 . ?
O8 Tb1 O6 125.3(2) 6_556 . ?
O4 Tb1 O6 89.8(2) . . ?
O1 Tb1 O6 146.9(2) 6_556 . ?
O7 Tb1 O5 133.2(2) 4_646 . ?
O2 Tb1 O5 82.6(2) 4_646 . ?
O8 Tb1 O5 73.7(2) 6_556 . ?
O4 Tb1 O5 74.1(2) . . ?
O1 Tb1 O5 136.3(2) 6_556 . ?
O6 Tb1 O5 53.4(2) . . ?
O7 Tb1 O3 74.9(2) 4_646 . ?
O2 Tb1 O3 141.0(2) 4_646 . ?
O8 Tb1 O3 139.7(2) 6_556 . ?
O4 Tb1 O3 53.4(2) . . ?
O1 Tb1 O3 75.5(2) 6_556 . ?
O6 Tb1 O3 71.4(3) . . ?
O5 Tb1 O3 101.8(2) . . ?
O7 Tb1 O2 71.2(2) 4_646 6_556 ?
O2 Tb1 O2 76.1(2) 4_646 6_556 ?
O8 Tb1 O2 70.4(2) 6_556 6_556 ?
O4 Tb1 O2 118.69(19) . 6_556 ?
O1 Tb1 O2 50.97(18) 6_556 6_556 ?
O6 Tb1 O2 149.4(2) . 6_556 ?
O5 Tb1 O2 141.01(19) . 6_556 ?
O3 Tb1 O2 115.3(2) . 6_556 ?
O7 Tb1 C5 109.0(2) 4_646 . ?
O2 Tb1 C5 84.4(2) 4_646 . ?
O8 Tb1 C5 100.7(2) 6_556 . ?
O4 Tb1 C5 78.0(2) . . ?
O1 Tb1 C5 147.8(2) 6_556 . ?
O6 Tb1 C5 26.5(2) . . ?
O5 Tb1 C5 27.2(2) . . ?
O3 Tb1 C5 83.5(2) . . ?
O2 Tb1 C5 159.7(2) 6_556 . ?
O7 Tb1 C4 101.6(3) 4_646 . ?
O2 Tb1 C4 157.1(3) 4_646 . ?
O8 Tb1 C4 115.1(3) 6_556 . ?
O4 Tb1 C4 27.3(3) . . ?
O1 Tb1 C4 74.6(2) 6_556 . ?
O6 Tb1 C4 75.6(3) . . ?
O5 Tb1 C4 84.5(2) . . ?
O3 Tb1 C4 26.7(3) . . ?
O2 Tb1 C4 124.6(2) 6_556 . ?
C5 Tb1 C4 75.6(3) . . ?
O7 Tb1 C1 81.5(2) 4_646 6_556 ?
O2 Tb1 C1 101.5(2) 4_646 6_556 ?
O8 Tb1 C1 71.8(2) 6_556 6_556 ?
O4 Tb1 C1 93.6(2) . 6_556 ?
O1 Tb1 C1 25.6(2) 6_556 6_556 ?
O6 Tb1 C1 162.7(2) . 6_556 ?
O5 Tb1 C1 143.7(2) . 6_556 ?
O3 Tb1 C1 97.2(2) . 6_556 ?
O2 Tb1 C1 25.6(2) 6_556 6_556 ?
C5 Tb1 C1 169.1(3) . 6_556 ?
C4 Tb1 C1 100.1(3) . 6_556 ?
O2 C1 O1 121.4(8) . . ?
O2 C1 C7 119.0(7) . . ?
O1 C1 C7 119.6(7) . . ?
O2 C1 Tb1 64.4(4) . 6 ?
O1 C1 Tb1 57.9(4) . 6 ?
C7 C1 Tb1 171.3(6) . 6 ?
C7 C2 H2A 109.5 . . ?
C7 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C7 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C8 C3 H3A 109.5 . . ?
C8 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C8 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O3 C4 O4 120.4(8) . . ?
O3 C4 C8 117.7(10) . . ?
O4 C4 C8 121.8(9) . . ?
O3 C4 Tb1 61.6(5) . . ?
O4 C4 Tb1 60.9(5) . . ?
C8 C4 Tb1 162.3(7) . . ?
O6 C5 O5 122.2(8) . . ?
O6 C5 C9 118.6(8) . . ?
O5 C5 C9 119.1(8) . . ?
O6 C5 Tb1 61.7(5) . . ?
O5 C5 Tb1 61.8(4) . . ?
C9 C5 Tb1 164.4(6) . . ?
O8 C6 O7 126.3(8) . . ?
O8 C6 C10 121.2(8) . . ?
O7 C6 C10 112.4(8) . . ?
N4 C7 C2 111.2(8) . . ?
N4 C7 C1 110.5(7) . . ?
C2 C7 C1 111.8(8) . . ?
N4 C7 H7A 107.7 . . ?
C2 C7 H7A 107.7 . . ?
C1 C7 H7A 107.7 . . ?
N5 C8 C4 112.1(9) . . ?
N5 C8 C3 111.6(10) . . ?
C4 C8 C3 115.0(10) . . ?
N5 C8 H8A 105.8 . . ?
C4 C8 H8A 105.8 . . ?
C3 C8 H8A 105.8 . . ?
N6 C9 C5 113.1(8) . . ?
N6 C9 H9A 109.0 . . ?
C5 C9 H9A 109.0 . . ?
N6 C9 H9B 109.0 . . ?
C5 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
N6 C10 C6 116.4(7) . . ?
N6 C10 H10A 108.2 . . ?
C6 C10 H10A 108.2 . . ?
N6 C10 H10B 108.2 . . ?
C6 C10 H10B 108.2 . . ?
H10A C10 H10B 107.3 . . ?
N3 C11 N4 120.9(8) . . ?
N3 C11 N1 123.1(8) . . ?
N4 C11 N1 115.9(8) . . ?
N2 C12 N5 118.2(9) . . ?
N2 C12 N1 122.9(8) . . ?
N5 C12 N1 118.9(8) . . ?
N3 C13 N6 118.0(8) . . ?
N3 C13 N2 126.6(8) . . ?
N6 C13 N2 115.4(8) . . ?
C12 N1 C11 117.1(7) . . ?
C12 N1 H1A 121.5 . . ?
C11 N1 H1A 121.5 . . ?
C12 N2 C13 114.1(8) . . ?
C11 N3 C13 116.0(8) . . ?
C11 N4 C7 120.8(7) . . ?
C11 N4 H4A 119.6 . . ?
C7 N4 H4A 119.6 . . ?
C12 N5 C8 120.6(8) . . ?
C12 N5 H5A 119.7 . . ?
C8 N5 H5A 119.7 . . ?
C13 N6 C10 118.9(8) . . ?
C13 N6 C9 119.0(8) . . ?
C10 N6 C9 118.6(7) . . ?
C1 O1 Tb1 96.5(5) . 6 ?
C1 O2 Tb1 163.8(6) . 4_656 ?
C1 O2 Tb1 90.0(5) . 6 ?
Tb1 O2 Tb1 103.9(2) 4_656 6 ?
C4 O3 Tb1 91.7(6) . . ?
C4 O4 Tb1 91.8(6) . . ?
C5 O5 Tb1 91.0(5) . . ?
C5 O6 Tb1 91.7(6) . . ?
C6 O7 Tb1 137.2(6) . 4_656 ?
C6 O8 Tb1 132.1(6) . 6 ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.369
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.247


data_a4
_database_code_depnum_ccdc_archive 'CCDC 913863'
#TrackingRef '913865.CIF'
_database_code_depnum_ccdc_archive 'CCDC 913865'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H16 Eu N6 O11'
_chemical_formula_weight         560.26
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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   11.252(6)
_cell_length_b                   15.764(9)
_cell_length_c                   9.851(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.173(8)
_cell_angle_gamma                90.00
_cell_volume                     1744.5(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4884
_cell_measurement_theta_min      2.0707
_cell_measurement_theta_max      27.4816
_exptl_crystal_description       block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2500
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100
_exptl_absorpt_coefficient_mu    3.671
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5771
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(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  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13832
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3992
_reflns_number_gt                3470
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+3.9103P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3992
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1558
_refine_ls_wR_factor_gt          0.1464
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
Eu1 Eu 0.66460(3) 0.02223(2) -0.07132(3) 0.01708(15) Uani 1 1 d . . .
C1 C 0.7250(7) -0.3485(5) 0.3984(8) 0.0233(16) Uani 1 1 d . . .
C2 C 0.6256(7) 0.0222(4) 0.2151(7) 0.0162(14) Uani 1 1 d . . .
C3 C 0.6697(8) 0.1472(5) 0.6451(8) 0.0254(16) Uani 1 1 d . . .
C4 C 0.9477(7) 0.0974(6) 0.8965(8) 0.0280(18) Uani 1 1 d . . .
C5 C 0.7624(11) -0.2581(6) 0.3779(9) 0.044(3) Uani 1 1 d . . .
H5B H 0.8025 -0.2536 0.2935 0.053 Uiso 1 1 calc R . .
H5C H 0.6924 -0.2222 0.3707 0.053 Uiso 1 1 calc R . .
C6 C 0.5996(7) 0.0166(5) 0.3641(8) 0.0219(17) Uani 1 1 d . . .
H6B H 0.5306 0.0514 0.3801 0.026 Uiso 1 1 calc R . .
H6C H 0.5797 -0.0416 0.3853 0.026 Uiso 1 1 calc R . .
C7 C 0.7057(8) 0.1307(5) 0.4983(7) 0.0268(18) Uani 1 1 d . . .
H7A H 0.6548 0.1644 0.4365 0.032 Uiso 1 1 calc R . .
H7B H 0.7868 0.1502 0.4903 0.032 Uiso 1 1 calc R . .
C8 C 1.0318(7) 0.0744(6) 0.7898(8) 0.0282(18) Uani 1 1 d . . .
H8A H 1.0179 0.1131 0.7141 0.034 Uiso 1 1 calc R . .
H8B H 1.1121 0.0845 0.8271 0.034 Uiso 1 1 calc R . .
C9 C 0.8456(7) -0.1463(5) 0.5212(7) 0.0207(15) Uani 1 1 d . . .
C10 C 0.7794(7) -0.0119(4) 0.5063(7) 0.0160(14) Uani 1 1 d . . .
C11 C 0.9397(7) -0.0369(5) 0.6482(8) 0.0228(16) Uani 1 1 d . . .
N1 N 0.8419(6) -0.2284(4) 0.4899(7) 0.0292(16) Uani 1 1 d . . .
H1A H 0.8863 -0.2639 0.5356 0.035 Uiso 1 1 calc R . .
N2 N 0.6984(6) 0.0439(4) 0.4562(6) 0.0233(14) Uani 1 1 d . . .
N3 N 1.0270(6) -0.0121(5) 0.7357(7) 0.0231(14) Uani 1 1 d . . .
H3A H 1.0818 -0.0477 0.7611 0.028 Uiso 1 1 calc R . .
N4 N 0.9330(6) -0.1213(4) 0.6162(7) 0.0228(14) Uani 1 1 d . . .
N5 N 0.7683(6) -0.0928(4) 0.4642(6) 0.0214(13) Uani 1 1 d . . .
N6 N 0.8655(6) 0.0197(4) 0.5922(6) 0.0193(13) Uani 1 1 d . . .
O1 O 0.7287(6) -0.3815(4) 0.5145(6) 0.0396(16) Uani 1 1 d . . .
O2 O 0.6848(6) -0.3898(4) 0.2941(6) 0.0345(15) Uani 1 1 d . . .
O3 O 0.5413(5) 0.0024(4) 0.1297(5) 0.0273(12) Uani 1 1 d . . .
O4 O 0.7235(5) 0.0456(4) 0.1773(5) 0.0250(12) Uani 1 1 d . . .
O5 O 0.6431(5) 0.0847(4) 0.7144(5) 0.0315(14) Uani 1 1 d . . .
O6 O 0.6714(7) 0.2229(4) 0.6842(7) 0.0492(19) Uani 1 1 d . . .
O7 O 0.8637(5) 0.0451(5) 0.9168(6) 0.0369(15) Uani 1 1 d . . .
O8 O 0.9649(6) 0.1643(5) 0.9563(7) 0.0448(17) Uani 1 1 d . . .
O9W O 0.6152(10) 0.1626(5) -0.0214(9) 0.085(4) Uani 1 1 d . . .
H9WA H 0.6225 0.1720 0.0639 0.102 Uiso 1 1 d R . .
H9WB H 0.5434 0.1732 -0.0491 0.102 Uiso 1 1 d R . .
O10W O 0.9126(6) 0.2068(5) 0.2111(7) 0.0473(18) Uani 1 1 d . . .
H10A H 0.8467 0.2220 0.2341 0.057 Uiso 1 1 d R . .
H10B H 0.9174 0.1986 0.1317 0.057 Uiso 1 1 d R . .
O11W O 0.4531(13) 0.2745(9) -0.1351(19) 0.182(8) Uani 1 1 d . . .
H11A H 0.4486 0.3041 -0.0630 0.218 Uiso 1 1 d R . .
H11B H 0.4440 0.3074 -0.2037 0.218 Uiso 1 1 d R . .
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
Eu1 0.0151(2) 0.0241(2) 0.0118(2) 0.00164(13) -0.00106(14) -0.00461(14)
C1 0.022(4) 0.024(4) 0.023(4) 0.005(3) -0.001(3) 0.011(3)
C2 0.015(3) 0.021(4) 0.013(3) 0.003(2) -0.001(3) 0.002(3)
C3 0.029(4) 0.031(4) 0.016(3) -0.003(3) 0.000(3) -0.004(3)
C4 0.019(4) 0.047(5) 0.018(4) 0.007(3) -0.001(3) -0.001(4)
C5 0.075(8) 0.030(5) 0.027(4) -0.005(4) -0.009(5) -0.004(5)
C6 0.022(4) 0.031(5) 0.012(3) 0.002(3) -0.003(3) -0.004(3)
C7 0.042(5) 0.027(4) 0.012(3) 0.004(3) 0.000(3) 0.005(4)
C8 0.021(4) 0.047(5) 0.016(4) -0.007(3) 0.000(3) -0.010(4)
C9 0.018(4) 0.024(4) 0.020(3) 0.002(3) 0.003(3) 0.001(3)
C10 0.023(4) 0.014(3) 0.011(3) 0.000(2) 0.001(3) -0.005(3)
C11 0.021(4) 0.030(4) 0.017(3) 0.000(3) 0.001(3) -0.001(3)
N1 0.030(4) 0.025(4) 0.033(4) -0.002(3) -0.003(3) 0.006(3)
N2 0.032(4) 0.024(3) 0.013(3) 0.002(2) -0.006(3) 0.001(3)
N3 0.014(3) 0.039(4) 0.017(3) 0.008(3) 0.002(2) -0.006(3)
N4 0.016(3) 0.025(3) 0.027(3) 0.002(3) 0.000(3) -0.001(3)
N5 0.025(3) 0.019(3) 0.019(3) 0.000(2) -0.007(3) -0.005(3)
N6 0.021(3) 0.019(3) 0.017(3) -0.002(2) -0.005(3) -0.004(2)
O1 0.053(4) 0.040(4) 0.025(3) 0.006(3) -0.006(3) -0.014(3)
O2 0.057(4) 0.024(3) 0.023(3) -0.001(2) -0.002(3) -0.003(3)
O3 0.018(3) 0.053(3) 0.011(2) 0.001(3) -0.003(2) -0.007(3)
O4 0.013(3) 0.043(3) 0.019(3) 0.003(2) -0.001(2) -0.005(2)
O5 0.034(3) 0.044(4) 0.016(3) 0.010(2) -0.001(2) -0.008(3)
O6 0.071(5) 0.036(4) 0.041(4) -0.017(3) 0.017(4) -0.016(4)
O7 0.019(3) 0.062(4) 0.030(3) 0.004(3) 0.008(2) -0.017(3)
O8 0.042(4) 0.053(4) 0.040(4) -0.013(3) 0.010(3) -0.014(3)
O9W 0.135(9) 0.025(4) 0.086(6) 0.001(4) -0.074(6) 0.003(5)
O10W 0.041(4) 0.070(5) 0.030(3) 0.001(3) -0.004(3) 0.023(4)
O11W 0.149(14) 0.125(12) 0.26(2) 0.037(13) -0.121(14) 0.017(11)
_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
Eu1 O7 2.279(6) 1_554 ?
Eu1 O5 2.330(5) 1_554 ?
Eu1 O9W 2.340(8) . ?
Eu1 O3 2.387(6) 3_655 ?
Eu1 O1 2.467(6) 4 ?
Eu1 O2 2.490(6) 4 ?
Eu1 O3 2.499(6) . ?
Eu1 O4 2.528(5) . ?
Eu1 C1 2.840(8) 4 ?
Eu1 C2 2.879(7) . ?
Eu1 Eu1 4.094(2) 3_655 ?
Eu1 H9WA 2.7647 . ?
Eu1 H9WB 2.7574 . ?
C1 O1 1.255(9) . ?
C1 O2 1.277(9) . ?
C1 C5 1.504(12) . ?
C1 Eu1 2.840(8) 4_556 ?
C2 O4 1.239(9) . ?
C2 O3 1.272(9) . ?
C2 C6 1.515(10) . ?
C3 O5 1.245(10) . ?
C3 O6 1.254(10) . ?
C3 C7 1.545(10) . ?
C4 O8 1.219(11) . ?
C4 O7 1.278(10) . ?
C4 C8 1.498(11) . ?
C5 N1 1.458(11) . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 N2 1.460(10) . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 N2 1.432(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N3 1.464(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N5 1.316(10) . ?
C9 N1 1.330(11) . ?
C9 N4 1.377(9) . ?
C10 N2 1.341(10) . ?
C10 N5 1.345(9) . ?
C10 N6 1.346(9) . ?
C11 N6 1.321(10) . ?
C11 N3 1.330(10) . ?
C11 N4 1.369(11) . ?
N1 H1A 0.8600 . ?
N3 H3A 0.8600 . ?
O1 Eu1 2.467(6) 4_556 ?
O2 Eu1 2.490(6) 4_556 ?
O3 Eu1 2.387(6) 3_655 ?
O5 Eu1 2.330(5) 1_556 ?
O7 Eu1 2.279(6) 1_556 ?
O9W H9WA 0.8536 . ?
O9W H9WB 0.8540 . ?
O10W H10A 0.8225 . ?
O10W H10B 0.7979 . ?
O11W H11A 0.8539 . ?
O11W H11B 0.8537 . ?
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
O7 Eu1 O5 86.5(2) 1_554 1_554 ?
O7 Eu1 O9W 96.2(3) 1_554 . ?
O5 Eu1 O9W 77.1(3) 1_554 . ?
O7 Eu1 O3 163.1(2) 1_554 3_655 ?
O5 Eu1 O3 78.4(2) 1_554 3_655 ?
O9W Eu1 O3 88.0(3) . 3_655 ?
O7 Eu1 O1 83.7(3) 1_554 4 ?
O5 Eu1 O1 134.8(2) 1_554 4 ?
O9W Eu1 O1 147.8(3) . 4 ?
O3 Eu1 O1 101.4(2) 3_655 4 ?
O7 Eu1 O2 89.2(2) 1_554 4 ?
O5 Eu1 O2 83.1(2) 1_554 4 ?
O9W Eu1 O2 159.1(2) . 4 ?
O3 Eu1 O2 81.5(2) 3_655 4 ?
O1 Eu1 O2 52.78(19) 4 4 ?
O7 Eu1 O3 130.63(19) 1_554 . ?
O5 Eu1 O3 137.4(2) 1_554 . ?
O9W Eu1 O3 78.7(3) . . ?
O3 Eu1 O3 66.2(2) 3_655 . ?
O1 Eu1 O3 77.3(2) 4 . ?
O2 Eu1 O3 112.8(2) 4 . ?
O7 Eu1 O4 79.7(2) 1_554 . ?
O5 Eu1 O4 145.5(2) 1_554 . ?
O9W Eu1 O4 73.2(2) . . ?
O3 Eu1 O4 117.11(18) 3_655 . ?
O1 Eu1 O4 75.1(2) 4 . ?
O2 Eu1 O4 127.66(19) 4 . ?
O3 Eu1 O4 51.56(17) . . ?
O7 Eu1 C1 84.6(2) 1_554 4 ?
O5 Eu1 C1 109.0(2) 1_554 4 ?
O9W Eu1 C1 173.9(3) . 4 ?
O3 Eu1 C1 93.0(2) 3_655 4 ?
O1 Eu1 C1 26.2(2) 4 4 ?
O2 Eu1 C1 26.70(19) 4 4 ?
O3 Eu1 C1 96.2(2) . 4 ?
O4 Eu1 C1 101.0(2) . 4 ?
O7 Eu1 C2 104.7(2) 1_554 . ?
O5 Eu1 C2 150.9(2) 1_554 . ?
O9W Eu1 C2 75.1(3) . . ?
O3 Eu1 C2 92.13(19) 3_655 . ?
O1 Eu1 C2 73.84(19) 4 . ?
O2 Eu1 C2 123.03(19) 4 . ?
O3 Eu1 C2 26.15(19) . . ?
O4 Eu1 C2 25.44(19) . . ?
C1 Eu1 C2 98.8(2) 4 . ?
O7 Eu1 Eu1 162.85(16) 1_554 3_655 ?
O5 Eu1 Eu1 109.43(15) 1_554 3_655 ?
O9W Eu1 Eu1 81.9(3) . 3_655 ?
O3 Eu1 Eu1 33.96(13) 3_655 3_655 ?
O1 Eu1 Eu1 88.93(17) 4 3_655 ?
O2 Eu1 Eu1 98.65(16) 4 3_655 ?
O3 Eu1 Eu1 32.25(12) . 3_655 ?
O4 Eu1 Eu1 83.47(12) . 3_655 ?
C1 Eu1 Eu1 95.57(16) 4 3_655 ?
C2 Eu1 Eu1 58.24(14) . 3_655 ?
O7 Eu1 H9WA 94.9 1_554 . ?
O5 Eu1 H9WA 93.6 1_554 . ?
O9W Eu1 H9WA 16.7 . . ?
O3 Eu1 H9WA 93.7 3_655 . ?
O1 Eu1 H9WA 131.1 4 . ?
O2 Eu1 H9WA 174.6 4 . ?
O3 Eu1 H9WA 66.9 . . ?
O4 Eu1 H9WA 56.7 . . ?
C1 Eu1 H9WA 157.2 4 . ?
C2 Eu1 H9WA 59.2 . . ?
Eu1 Eu1 H9WA 78.4 3_655 . ?
O7 Eu1 H9WB 111.1 1_554 . ?
O5 Eu1 H9WB 71.3 1_554 . ?
O9W Eu1 H9WB 16.9 . . ?
O3 Eu1 H9WB 71.4 3_655 . ?
O1 Eu1 H9WB 152.3 4 . ?
O2 Eu1 H9WB 145.7 4 . ?
O3 Eu1 H9WB 75.3 . . ?
O4 Eu1 H9WB 84.4 . . ?
C1 Eu1 H9WB 164.2 4 . ?
C2 Eu1 H9WB 79.6 . . ?
Eu1 Eu1 H9WB 70.1 3_655 . ?
H9WA Eu1 H9WB 29.1 . . ?
O1 C1 O2 121.0(8) . . ?
O1 C1 C5 121.3(7) . . ?
O2 C1 C5 117.7(7) . . ?
O1 C1 Eu1 60.1(4) . 4_556 ?
O2 C1 Eu1 61.2(4) . 4_556 ?
C5 C1 Eu1 176.9(7) . 4_556 ?
O4 C2 O3 121.2(7) . . ?
O4 C2 C6 122.1(6) . . ?
O3 C2 C6 116.8(7) . . ?
O4 C2 Eu1 61.2(4) . . ?
O3 C2 Eu1 60.0(4) . . ?
C6 C2 Eu1 175.9(5) . . ?
O5 C3 O6 125.8(8) . . ?
O5 C3 C7 117.6(7) . . ?
O6 C3 C7 116.6(7) . . ?
O8 C4 O7 125.6(8) . . ?
O8 C4 C8 117.3(8) . . ?
O7 C4 C8 117.0(8) . . ?
N1 C5 C1 111.6(7) . . ?
N1 C5 H5B 109.3 . . ?
C1 C5 H5B 109.3 . . ?
N1 C5 H5C 109.3 . . ?
C1 C5 H5C 109.3 . . ?
H5B C5 H5C 108.0 . . ?
N2 C6 C2 113.8(7) . . ?
N2 C6 H6B 108.8 . . ?
C2 C6 H6B 108.8 . . ?
N2 C6 H6C 108.8 . . ?
C2 C6 H6C 108.8 . . ?
H6B C6 H6C 107.7 . . ?
N2 C7 C3 114.7(7) . . ?
N2 C7 H7A 108.6 . . ?
C3 C7 H7A 108.6 . . ?
N2 C7 H7B 108.6 . . ?
C3 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
N3 C8 C4 118.0(7) . . ?
N3 C8 H8A 107.8 . . ?
C4 C8 H8A 107.8 . . ?
N3 C8 H8B 107.8 . . ?
C4 C8 H8B 107.8 . . ?
H8A C8 H8B 107.2 . . ?
N5 C9 N1 120.9(7) . . ?
N5 C9 N4 122.5(7) . . ?
N1 C9 N4 116.6(7) . . ?
N2 C10 N5 117.3(7) . . ?
N2 C10 N6 116.1(6) . . ?
N5 C10 N6 126.6(7) . . ?
N6 C11 N3 120.0(7) . . ?
N6 C11 N4 122.4(7) . . ?
N3 C11 N4 117.6(7) . . ?
C9 N1 C5 119.8(7) . . ?
C9 N1 H1A 120.1 . . ?
C5 N1 H1A 120.1 . . ?
C10 N2 C7 119.6(7) . . ?
C10 N2 C6 121.0(7) . . ?
C7 N2 C6 119.4(7) . . ?
C11 N3 C8 121.3(7) . . ?
C11 N3 H3A 119.3 . . ?
C8 N3 H3A 119.3 . . ?
C11 N4 C9 117.6(7) . . ?
C9 N5 C10 115.3(6) . . ?
C11 N6 C10 115.4(6) . . ?
C1 O1 Eu1 93.8(5) . 4_556 ?
C1 O2 Eu1 92.1(5) . 4_556 ?
C2 O3 Eu1 151.3(5) . 3_655 ?
C2 O3 Eu1 93.8(4) . . ?
Eu1 O3 Eu1 113.8(2) 3_655 . ?
C2 O4 Eu1 93.3(4) . . ?
C3 O5 Eu1 144.6(5) . 1_556 ?
C4 O7 Eu1 147.9(6) . 1_556 ?
Eu1 O9W H9WA 111.1 . . ?
Eu1 O9W H9WB 110.5 . . ?
H9WA O9W H9WB 108.6 . . ?
H10A O10W H10B 115.4 . . ?
H11A O11W H11B 108.4 . . ?
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 O8 0.86 2.02 2.782(10) 147.3 2_746
N3 H3A O4 0.86 2.24 2.937(9) 138.0 3_756
O9W H9WA O6 0.85 2.09 2.760(11) 134.7 4_565
O9W H9WB O11W 0.85 2.05 2.732(14) 136.3 .
O10W H10A O6 0.82 2.19 2.929(10) 150.4 4_565
O10W H10B O8 0.80 1.91 2.694(10) 165.5 1_554
O11W H11B O2 0.85 2.11 2.811(13) 139.4 3_655
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.519
_refine_diff_density_min         -2.008
_refine_diff_density_rms         0.216


data_a3
_database_code_depnum_ccdc_archive 'CCDC 913864'
#TrackingRef '913864.CIF'
_database_code_depnum_ccdc_archive 'CCDC 913864'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H16 Gd N6 O11'
_chemical_formula_weight         565.55
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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   11.225(4)
_cell_length_b                   15.717(5)
_cell_length_c                   9.817(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.160(5)
_cell_angle_gamma                90.00
_cell_volume                     1729.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4631
_cell_measurement_theta_min      2.0707
_cell_measurement_theta_max      27.4816
_exptl_crystal_description       block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    3.912
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
RIGAKU/MSC(2004), CrystalClear Version 1.3.6,
Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(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  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14516
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3954
_reflns_number_gt                3507
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+9.6733P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    Theo
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3954
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0724
_refine_ls_wR_factor_ref         0.1886
_refine_ls_wR_factor_gt          0.1782
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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
Gd1 Gd 0.66422(4) 0.02216(3) -0.07094(4) 0.02327(19) Uani 1 1 d . . .
C1 C 0.7217(9) -0.3502(7) 0.3972(11) 0.030(2) Uani 1 1 d . . .
C2 C 0.6241(8) 0.0233(6) 0.2157(10) 0.0244(19) Uani 1 1 d . . .
C3 C 0.6674(10) 0.1465(7) 0.6467(10) 0.031(2) Uani 1 1 d . . .
C4 C 0.9454(9) 0.0953(8) 0.8988(12) 0.036(3) Uani 1 1 d . . .
C5 C 0.7594(14) -0.2591(8) 0.3783(13) 0.048(3) Uani 1 1 d . . .
H5B H 0.7981 -0.2541 0.2927 0.058 Uiso 1 1 calc R . .
H5C H 0.6889 -0.2233 0.3725 0.058 Uiso 1 1 calc R . .
C6 C 0.5989(9) 0.0164(7) 0.3645(10) 0.028(2) Uani 1 1 d . . .
H6B H 0.5292 0.0504 0.3815 0.034 Uiso 1 1 calc R . .
H6C H 0.5803 -0.0424 0.3849 0.034 Uiso 1 1 calc R . .
C7 C 0.7039(10) 0.1311(6) 0.4985(10) 0.031(2) Uani 1 1 d . . .
H7A H 0.6521 0.1645 0.4369 0.037 Uiso 1 1 calc R . .
H7B H 0.7848 0.1515 0.4906 0.037 Uiso 1 1 calc R . .
C8 C 1.0321(9) 0.0724(8) 0.7894(11) 0.034(2) Uani 1 1 d . . .
H8A H 1.0194 0.1121 0.7143 0.041 Uiso 1 1 calc R . .
H8B H 1.1127 0.0812 0.8276 0.041 Uiso 1 1 calc R . .
C9 C 0.8447(8) -0.1468(7) 0.5205(10) 0.026(2) Uani 1 1 d . . .
C10 C 0.7774(8) -0.0107(6) 0.5051(9) 0.0207(18) Uani 1 1 d . . .
C11 C 0.9402(9) -0.0366(7) 0.6489(11) 0.029(2) Uani 1 1 d . . .
N1 N 0.8407(8) -0.2284(6) 0.4888(10) 0.036(2) Uani 1 1 d . . .
H1A H 0.8863 -0.2638 0.5335 0.043 Uiso 1 1 calc R . .
N2 N 0.6982(8) 0.0443(5) 0.4562(8) 0.0269(18) Uani 1 1 d . . .
N3 N 1.0248(8) -0.0123(6) 0.7350(9) 0.034(2) Uani 1 1 d . . .
H3A H 1.0790 -0.0484 0.7607 0.041 Uiso 1 1 calc R . .
N4 N 0.9330(7) -0.1217(6) 0.6162(9) 0.0276(18) Uani 1 1 d . . .
N5 N 0.7683(7) -0.0923(5) 0.4647(8) 0.0269(18) Uani 1 1 d . . .
N6 N 0.8649(8) 0.0197(5) 0.5926(9) 0.0269(18) Uani 1 1 d . . .
O1 O 0.7285(8) -0.3821(6) 0.5147(9) 0.047(2) Uani 1 1 d . . .
O2 O 0.6849(8) -0.3913(5) 0.2935(8) 0.0411(19) Uani 1 1 d . . .
O3 O 0.5415(6) 0.0021(5) 0.1271(7) 0.0324(16) Uani 1 1 d . . .
O4 O 0.7232(6) 0.0465(5) 0.1773(8) 0.0322(17) Uani 1 1 d . . .
O5 O 0.6439(7) 0.0842(5) 0.7150(8) 0.0367(18) Uani 1 1 d . . .
O6 O 0.6715(10) 0.2226(6) 0.6850(10) 0.060(3) Uani 1 1 d . . .
O7 O 0.8629(7) 0.0442(6) 0.9176(9) 0.044(2) Uani 1 1 d . . .
O8 O 0.9640(9) 0.1642(7) 0.9564(10) 0.055(2) Uani 1 1 d . . .
O9W O 0.6182(12) 0.1642(6) -0.0241(12) 0.082(4) Uani 1 1 d . . .
H9WA H 0.6255 0.1736 0.0613 0.098 Uiso 1 1 d R . .
H9WB H 0.5465 0.1748 -0.0518 0.098 Uiso 1 1 d R . .
O10W O 0.9123(8) 0.2073(6) 0.2104(9) 0.053(2) Uani 1 1 d . . .
H10A H 0.8464 0.2224 0.2334 0.063 Uiso 1 1 d R . .
H10B H 0.9171 0.1991 0.1310 0.063 Uiso 1 1 d R . .
O11W O 0.4517(19) 0.2717(13) -0.135(3) 0.214(14) Uani 1 1 d . . .
H11A H 0.4471 0.3013 -0.0629 0.256 Uiso 1 1 d R . .
H11B H 0.4426 0.3046 -0.2035 0.256 Uiso 1 1 d R . .
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
Gd1 0.0227(3) 0.0334(3) 0.0135(3) 0.00161(18) -0.00108(18) -0.00471(19)
C1 0.031(5) 0.033(5) 0.026(5) 0.009(4) 0.002(4) 0.003(4)
C2 0.025(5) 0.033(5) 0.015(4) -0.001(4) -0.001(4) 0.006(4)
C3 0.043(6) 0.033(5) 0.017(5) 0.000(4) 0.000(4) -0.001(4)
C4 0.023(5) 0.059(7) 0.026(6) 0.007(5) -0.001(4) 0.004(5)
C5 0.082(10) 0.035(6) 0.027(6) -0.002(5) -0.006(6) -0.009(6)
C6 0.027(5) 0.041(6) 0.017(5) -0.004(4) -0.005(4) -0.007(4)
C7 0.050(6) 0.027(5) 0.016(5) 0.008(4) 0.003(4) 0.006(4)
C8 0.031(5) 0.049(6) 0.021(5) 0.001(5) -0.004(4) -0.004(5)
C9 0.024(5) 0.033(5) 0.021(5) 0.005(4) 0.001(4) 0.001(4)
C10 0.026(5) 0.026(4) 0.010(4) 0.001(3) -0.002(3) -0.004(4)
C11 0.019(4) 0.038(6) 0.030(5) 0.011(4) 0.004(4) -0.003(4)
N1 0.042(5) 0.033(5) 0.032(5) -0.005(4) -0.008(4) 0.002(4)
N2 0.040(5) 0.029(4) 0.011(4) 0.001(3) -0.006(3) 0.001(4)
N3 0.027(5) 0.054(6) 0.020(5) 0.005(4) -0.002(4) 0.003(4)
N4 0.024(4) 0.037(5) 0.022(4) -0.003(3) 0.001(3) -0.004(3)
N5 0.026(4) 0.034(4) 0.019(4) 0.000(3) -0.007(3) -0.007(3)
N6 0.033(4) 0.030(4) 0.017(4) 0.005(3) -0.008(3) -0.008(3)
O1 0.067(6) 0.044(5) 0.029(4) 0.005(4) -0.005(4) -0.013(4)
O2 0.062(5) 0.038(4) 0.023(4) -0.007(3) -0.006(4) -0.001(4)
O3 0.026(4) 0.055(5) 0.015(3) 0.004(3) -0.005(3) -0.008(3)
O4 0.023(3) 0.049(5) 0.024(4) 0.006(3) -0.004(3) -0.008(3)
O5 0.040(4) 0.050(5) 0.020(4) 0.011(3) -0.001(3) -0.008(4)
O6 0.092(8) 0.044(5) 0.046(6) -0.021(4) 0.023(5) -0.022(5)
O7 0.024(4) 0.075(6) 0.032(4) 0.001(4) 0.005(3) -0.011(4)
O8 0.057(6) 0.067(6) 0.042(6) -0.014(5) 0.011(5) -0.019(5)
O9W 0.140(11) 0.035(5) 0.063(7) -0.003(5) -0.054(7) 0.008(6)
O10W 0.060(6) 0.069(6) 0.028(5) 0.003(4) -0.008(4) 0.028(5)
O11W 0.18(2) 0.142(19) 0.30(4) 0.06(2) -0.12(2) 0.020(16)
_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 O7 2.265(7) 1_554 ?
Gd1 O5 2.317(7) 1_554 ?
Gd1 O9W 2.343(10) . ?
Gd1 O3 2.375(7) 3_655 ?
Gd1 O1 2.451(9) 4 ?
Gd1 O3 2.464(8) . ?
Gd1 O2 2.468(8) 4 ?
Gd1 O4 2.520(7) . ?
Gd1 C1 2.800(11) 4 ?
Gd1 C2 2.874(10) . ?
Gd1 Gd1 4.0724(14) 3_655 ?
C1 O2 1.256(13) . ?
C1 O1 1.256(13) . ?
C1 C5 1.508(15) . ?
C1 Gd1 2.800(11) 4_556 ?
C2 O4 1.249(12) . ?
C2 O3 1.280(12) . ?
C2 C6 1.507(14) . ?
C3 O5 1.224(13) . ?
C3 O6 1.253(14) . ?
C3 C7 1.552(14) . ?
C4 O8 1.234(15) . ?
C4 O7 1.248(14) . ?
C4 C8 1.532(15) . ?
C5 N1 1.461(14) . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 N2 1.462(12) . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 N2 1.427(13) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N3 1.435(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N5 1.311(13) . ?
C9 N1 1.320(14) . ?
C9 N4 1.385(12) . ?
C10 N2 1.311(13) . ?
C10 N5 1.345(12) . ?
C10 N6 1.356(12) . ?
C11 N3 1.294(14) . ?
C11 N6 1.323(13) . ?
C11 N4 1.376(14) . ?
N1 H1A 0.8600 . ?
N3 H3A 0.8600 . ?
O1 Gd1 2.451(9) 4_556 ?
O2 Gd1 2.468(8) 4_556 ?
O3 Gd1 2.375(7) 3_655 ?
O5 Gd1 2.317(7) 1_556 ?
O7 Gd1 2.265(7) 1_556 ?
O9W H9WA 0.8507 . ?
O9W H9WB 0.8520 . ?
O10W H10A 0.8203 . ?
O10W H10B 0.7952 . ?
O11W H11A 0.8510 . ?
O11W H11B 0.8509 . ?
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
O7 Gd1 O5 86.5(3) 1_554 1_554 ?
O7 Gd1 O9W 95.3(4) 1_554 . ?
O5 Gd1 O9W 76.4(3) 1_554 . ?
O7 Gd1 O3 163.7(3) 1_554 3_655 ?
O5 Gd1 O3 79.1(3) 1_554 3_655 ?
O9W Gd1 O3 88.7(4) . 3_655 ?
O7 Gd1 O1 83.3(3) 1_554 4 ?
O5 Gd1 O1 134.6(3) 1_554 4 ?
O9W Gd1 O1 148.5(3) . 4 ?
O3 Gd1 O1 101.5(3) 3_655 4 ?
O7 Gd1 O3 130.8(3) 1_554 . ?
O5 Gd1 O3 137.6(3) 1_554 . ?
O9W Gd1 O3 80.1(4) . . ?
O3 Gd1 O3 65.4(3) 3_655 . ?
O1 Gd1 O3 77.4(3) 4 . ?
O7 Gd1 O2 88.8(3) 1_554 4 ?
O5 Gd1 O2 82.5(3) 1_554 4 ?
O9W Gd1 O2 158.2(3) . 4 ?
O3 Gd1 O2 82.0(3) 3_655 4 ?
O1 Gd1 O2 53.3(3) 4 4 ?
O3 Gd1 O2 113.1(3) . 4 ?
O7 Gd1 O4 79.5(3) 1_554 . ?
O5 Gd1 O4 145.2(3) 1_554 . ?
O9W Gd1 O4 73.4(3) . . ?
O3 Gd1 O4 116.7(2) 3_655 . ?
O1 Gd1 O4 75.4(3) 4 . ?
O3 Gd1 O4 52.0(2) . . ?
O2 Gd1 O4 128.4(3) 4 . ?
O7 Gd1 C1 84.8(3) 1_554 4 ?
O5 Gd1 C1 108.4(3) 1_554 4 ?
O9W Gd1 C1 175.1(3) . 4 ?
O3 Gd1 C1 92.6(3) 3_655 4 ?
O1 Gd1 C1 26.6(3) 4 4 ?
O3 Gd1 C1 96.1(3) . 4 ?
O2 Gd1 C1 26.6(3) 4 4 ?
O4 Gd1 C1 101.8(3) . 4 ?
O7 Gd1 C2 104.8(3) 1_554 . ?
O5 Gd1 C2 150.8(3) 1_554 . ?
O9W Gd1 C2 75.7(4) . . ?
O3 Gd1 C2 91.5(3) 3_655 . ?
O1 Gd1 C2 74.3(3) 4 . ?
O3 Gd1 C2 26.3(2) . . ?
O2 Gd1 C2 123.9(3) 4 . ?
O4 Gd1 C2 25.7(2) . . ?
C1 Gd1 C2 99.5(3) 4 . ?
O7 Gd1 Gd1 162.8(2) 1_554 3_655 ?
O5 Gd1 Gd1 109.67(19) 1_554 3_655 ?
O9W Gd1 Gd1 83.2(4) . 3_655 ?
O3 Gd1 Gd1 33.38(18) 3_655 3_655 ?
O1 Gd1 Gd1 89.1(2) 4 3_655 ?
O3 Gd1 Gd1 32.03(16) . 3_655 ?
O2 Gd1 Gd1 99.0(2) 4 3_655 ?
O4 Gd1 Gd1 83.67(16) . 3_655 ?
C1 Gd1 Gd1 95.3(2) 4 3_655 ?
C2 Gd1 Gd1 58.17(19) . 3_655 ?
O2 C1 O1 122.7(10) . . ?
O2 C1 C5 118.1(9) . . ?
O1 C1 C5 119.2(10) . . ?
O2 C1 Gd1 61.8(6) . 4_556 ?
O1 C1 Gd1 61.0(6) . 4_556 ?
C5 C1 Gd1 176.9(9) . 4_556 ?
O4 C2 O3 119.7(9) . . ?
O4 C2 C6 122.1(9) . . ?
O3 C2 C6 118.2(9) . . ?
O4 C2 Gd1 61.1(5) . . ?
O3 C2 Gd1 58.7(5) . . ?
C6 C2 Gd1 175.1(7) . . ?
O5 C3 O6 127.2(11) . . ?
O5 C3 C7 117.6(10) . . ?
O6 C3 C7 115.1(10) . . ?
O8 C4 O7 127.3(11) . . ?
O8 C4 C8 115.5(10) . . ?
O7 C4 C8 117.2(11) . . ?
N1 C5 C1 113.0(10) . . ?
N1 C5 H5B 109.0 . . ?
C1 C5 H5B 109.0 . . ?
N1 C5 H5C 109.0 . . ?
C1 C5 H5C 109.0 . . ?
H5B C5 H5C 107.8 . . ?
N2 C6 C2 113.4(9) . . ?
N2 C6 H6B 108.9 . . ?
C2 C6 H6B 108.9 . . ?
N2 C6 H6C 108.9 . . ?
C2 C6 H6C 108.9 . . ?
H6B C6 H6C 107.7 . . ?
N2 C7 C3 114.4(8) . . ?
N2 C7 H7A 108.7 . . ?
C3 C7 H7A 108.7 . . ?
N2 C7 H7B 108.7 . . ?
C3 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N3 C8 C4 117.0(9) . . ?
N3 C8 H8A 108.0 . . ?
C4 C8 H8A 108.0 . . ?
N3 C8 H8B 108.0 . . ?
C4 C8 H8B 108.0 . . ?
H8A C8 H8B 107.3 . . ?
N5 C9 N1 121.6(9) . . ?
N5 C9 N4 121.6(9) . . ?
N1 C9 N4 116.8(9) . . ?
N2 C10 N5 118.8(8) . . ?
N2 C10 N6 116.9(9) . . ?
N5 C10 N6 124.3(9) . . ?
N3 C11 N6 120.2(10) . . ?
N3 C11 N4 118.1(9) . . ?
N6 C11 N4 121.6(10) . . ?
C9 N1 C5 120.5(9) . . ?
C9 N1 H1A 119.8 . . ?
C5 N1 H1A 119.8 . . ?
C10 N2 C7 120.3(9) . . ?
C10 N2 C6 120.4(8) . . ?
C7 N2 C6 119.1(9) . . ?
C11 N3 C8 122.9(9) . . ?
C11 N3 H3A 118.6 . . ?
C8 N3 H3A 118.6 . . ?
C11 N4 C9 117.8(9) . . ?
C9 N5 C10 117.5(8) . . ?
C11 N6 C10 116.9(9) . . ?
C1 O1 Gd1 92.4(7) . 4_556 ?
C1 O2 Gd1 91.6(6) . 4_556 ?
C2 O3 Gd1 149.1(7) . 3_655 ?
C2 O3 Gd1 95.0(6) . . ?
Gd1 O3 Gd1 114.6(3) 3_655 . ?
C2 O4 Gd1 93.2(6) . . ?
C3 O5 Gd1 145.1(7) . 1_556 ?
C4 O7 Gd1 147.9(9) . 1_556 ?
Gd1 O9W H9WA 110.4 . . ?
Gd1 O9W H9WB 109.8 . . ?
H9WA O9W H9WB 108.6 . . ?
H10A O10W H10B 115.3 . . ?
H11A O11W H11B 108.4 . . ?
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 O8 0.86 2.02 2.794(13) 148.9 2_746
N3 H3A O4 0.86 2.27 2.960(11) 137.3 3_756
O9W H9WA O6 0.85 2.08 2.757(15) 135.9 4_565
O9W H9WB O11W 0.85 2.00 2.70(2) 138.6 .
O10W H10A O6 0.82 2.17 2.917(13) 150.8 4_565
O10W H10B O8 0.80 1.90 2.678(13) 165.5 1_554
O11W H11B O2 0.85 2.13 2.836(19) 139.9 3_655
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.244
_refine_diff_density_min         -2.042
_refine_diff_density_rms         0.198


data_a2
_database_code_depnum_ccdc_archive 'CCDC 913865'
#TrackingRef '913863.CIF'
_database_code_depnum_ccdc_archive 'CCDC 913863'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H16 N6 O11 Tb'
_chemical_formula_weight         567.22
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   11.1943(6)
_cell_length_b                   15.6877(13)
_cell_length_c                   9.8087(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.125(6)
_cell_angle_gamma                90.00
_cell_volume                     1720.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5190
_cell_measurement_theta_min      2.0793
_cell_measurement_theta_max      27.4835
_exptl_crystal_description       block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1108
_exptl_absorpt_coefficient_mu    4.189
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5452
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
RIGAKU/MSC(2004), CrystalClear Version 1.3.6,
Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(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  'Mercury2 (1x1 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13312
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.52
_reflns_number_total             3883
_reflns_number_gt                3672
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+2.7101P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    Theo
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3883
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0962
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
Tb1 Tb 0.663812(18) 0.022281(12) -0.070428(19) 0.01976(10) Uani 1 1 d . . .
C1 C 0.7221(4) -0.3510(3) 0.3971(5) 0.0300(10) Uani 1 1 d . . .
C2 C 0.6240(4) 0.0231(2) 0.2146(4) 0.0205(9) Uani 1 1 d . . .
C3 C 0.6683(4) 0.1476(3) 0.6467(5) 0.0264(9) Uani 1 1 d . . .
C4 C 0.9457(4) 0.0963(4) 0.8976(5) 0.0304(10) Uani 1 1 d . . .
C5 C 0.7611(6) -0.2599(3) 0.3769(6) 0.0451(14) Uani 1 1 d . . .
H5B H 0.8011 -0.2559 0.2918 0.054 Uiso 1 1 calc R . .
H5C H 0.6907 -0.2238 0.3690 0.054 Uiso 1 1 calc R . .
C6 C 0.5978(5) 0.0178(3) 0.3641(5) 0.0271(11) Uani 1 1 d . . .
H6B H 0.5286 0.0530 0.3799 0.032 Uiso 1 1 calc R . .
H6C H 0.5773 -0.0406 0.3855 0.032 Uiso 1 1 calc R . .
C7 C 0.7027(5) 0.1325(3) 0.4992(4) 0.0277(10) Uani 1 1 d . . .
H7A H 0.6501 0.1660 0.4385 0.033 Uiso 1 1 calc R . .
H7B H 0.7836 0.1530 0.4900 0.033 Uiso 1 1 calc R . .
C8 C 1.0316(4) 0.0748(4) 0.7891(4) 0.0295(10) Uani 1 1 d . . .
H8A H 1.0172 0.1137 0.7131 0.035 Uiso 1 1 calc R . .
H8B H 1.1124 0.0849 0.8263 0.035 Uiso 1 1 calc R . .
C9 C 0.8443(4) -0.1466(3) 0.5195(5) 0.0257(9) Uani 1 1 d . . .
C10 C 0.7780(4) -0.0114(3) 0.5055(4) 0.0208(9) Uani 1 1 d . . .
C11 C 0.9396(4) -0.0367(3) 0.6470(5) 0.0246(9) Uani 1 1 d . . .
N1 N 0.8408(4) -0.2284(3) 0.4871(4) 0.0334(9) Uani 1 1 d . . .
H1A H 0.8867 -0.2636 0.5323 0.040 Uiso 1 1 calc R . .
N2 N 0.6966(4) 0.0448(3) 0.4560(4) 0.0238(8) Uani 1 1 d . . .
N3 N 1.0248(4) -0.0115(3) 0.7372(4) 0.0302(9) Uani 1 1 d . . .
H3A H 1.0780 -0.0478 0.7659 0.036 Uiso 1 1 calc R . .
N4 N 0.9323(3) -0.1214(3) 0.6149(4) 0.0266(8) Uani 1 1 d . . .
N5 N 0.7668(4) -0.0923(2) 0.4632(4) 0.0244(8) Uani 1 1 d . . .
N6 N 0.8645(4) 0.0204(2) 0.5926(4) 0.0235(8) Uani 1 1 d . . .
O1 O 0.7257(4) -0.3828(3) 0.5131(4) 0.0409(9) Uani 1 1 d . . .
O2 O 0.6839(4) -0.3929(2) 0.2930(4) 0.0397(9) Uani 1 1 d . . .
O3 O 0.5404(3) 0.0027(3) 0.1280(3) 0.0291(7) Uani 1 1 d . . .
O4 O 0.7235(3) 0.0460(2) 0.1762(3) 0.0279(7) Uani 1 1 d . . .
O5 O 0.6424(3) 0.0843(2) 0.7161(3) 0.0328(8) Uani 1 1 d . . .
O6 O 0.6712(4) 0.2229(3) 0.6877(4) 0.0527(12) Uani 1 1 d . . .
O7 O 0.8617(3) 0.0443(3) 0.9168(4) 0.0380(9) Uani 1 1 d . . .
O8 O 0.9629(4) 0.1642(3) 0.9584(4) 0.0473(10) Uani 1 1 d . . .
O9W O 0.6180(6) 0.1638(3) -0.0231(6) 0.0770(18) Uani 1 1 d . . .
H9WA H 0.6253 0.1732 0.0623 0.092 Uiso 1 1 d R . .
H9WB H 0.5462 0.1744 -0.0508 0.092 Uiso 1 1 d R . .
O10W O 0.9123(4) 0.2074(3) 0.2133(4) 0.0498(11) Uani 1 1 d . . .
H10A H 0.8464 0.2226 0.2362 0.060 Uiso 1 1 d R . .
H10B H 0.9171 0.1992 0.1338 0.060 Uiso 1 1 d R . .
O11W O 0.4532(10) 0.2725(7) -0.1374(14) 0.203(6) Uani 1 1 d . . .
H11A H 0.4486 0.3021 -0.0653 0.243 Uiso 1 1 d R . .
H11B H 0.4441 0.3054 -0.2059 0.243 Uiso 1 1 d R . .
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
Tb1 0.01836(15) 0.02477(14) 0.01598(13) 0.00099(6) -0.00049(9) -0.00355(7)
C1 0.031(2) 0.032(2) 0.027(2) -0.0025(18) -0.0005(18) 0.005(2)
C2 0.022(2) 0.025(2) 0.0145(19) -0.0005(13) -0.0019(16) 0.0033(15)
C3 0.030(2) 0.027(2) 0.022(2) -0.0014(17) 0.0006(16) -0.0028(19)
C4 0.020(2) 0.047(3) 0.024(2) 0.0011(19) -0.0019(17) -0.002(2)
C5 0.075(4) 0.027(3) 0.033(3) -0.003(2) -0.008(3) -0.005(3)
C6 0.024(2) 0.043(3) 0.014(2) 0.0023(16) -0.0035(17) -0.0005(18)
C7 0.042(3) 0.023(2) 0.017(2) 0.0055(15) -0.0022(18) 0.004(2)
C8 0.020(2) 0.050(3) 0.019(2) -0.0052(19) 0.0012(16) -0.011(2)
C9 0.029(2) 0.022(2) 0.026(2) 0.0006(17) 0.0023(17) -0.0006(18)
C10 0.026(2) 0.020(2) 0.0156(19) 0.0007(15) 0.0015(16) -0.0019(18)
C11 0.020(2) 0.029(2) 0.025(2) 0.0008(17) 0.0031(18) -0.0015(18)
N1 0.039(2) 0.023(2) 0.037(2) -0.0009(16) -0.0086(18) 0.0013(18)
N2 0.032(2) 0.0235(17) 0.0148(16) -0.0032(14) -0.0078(15) 0.0006(17)
N3 0.018(2) 0.042(3) 0.030(2) -0.0016(18) -0.0095(16) 0.0012(17)
N4 0.0234(19) 0.025(2) 0.031(2) 0.0015(15) -0.0018(15) 0.0012(16)
N5 0.029(2) 0.0191(18) 0.0241(18) -0.0031(14) -0.0030(15) -0.0015(16)
N6 0.027(2) 0.024(2) 0.0187(17) 0.0010(12) -0.0041(15) -0.0059(14)
O1 0.055(2) 0.037(2) 0.0294(18) 0.0027(15) -0.0036(16) -0.0113(18)
O2 0.060(3) 0.0270(19) 0.0312(18) -0.0003(14) -0.0074(17) -0.0030(18)
O3 0.0169(16) 0.0542(19) 0.0157(14) 0.0026(16) -0.0033(11) -0.0060(17)
O4 0.0195(16) 0.0406(18) 0.0233(16) 0.0011(14) -0.0014(12) -0.0044(15)
O5 0.038(2) 0.038(2) 0.0224(16) 0.0095(14) -0.0001(14) -0.0063(16)
O6 0.081(3) 0.034(2) 0.044(2) -0.0117(17) 0.018(2) -0.011(2)
O7 0.0220(18) 0.058(2) 0.0344(19) 0.0010(17) 0.0053(15) -0.0151(17)
O8 0.046(2) 0.053(2) 0.044(2) -0.0148(18) 0.0106(18) -0.011(2)
O9W 0.126(5) 0.026(2) 0.073(3) -0.007(2) -0.053(3) 0.012(3)
O10W 0.054(3) 0.059(3) 0.035(2) -0.0015(18) -0.0067(18) 0.017(2)
O11W 0.177(11) 0.162(11) 0.254(14) 0.060(10) -0.119(10) 0.023(9)
_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
Tb1 O7 2.253(3) 1_554 ?
Tb1 O5 2.310(3) 1_554 ?
Tb1 O9W 2.331(5) . ?
Tb1 O3 2.357(3) 3_655 ?
Tb1 O1 2.425(4) 4 ?
Tb1 O2 2.449(4) 4 ?
Tb1 O3 2.467(3) . ?
Tb1 O4 2.502(3) . ?
Tb1 C1 2.788(5) 4 ?
Tb1 C2 2.855(4) . ?
C1 O1 1.241(6) . ?
C1 O2 1.269(6) . ?
C1 C5 1.510(8) . ?
C1 Tb1 2.788(5) 4_556 ?
C2 O4 1.248(6) . ?
C2 O3 1.270(6) . ?
C2 C6 1.513(6) . ?
C3 O5 1.246(6) . ?
C3 O6 1.247(6) . ?
C3 C7 1.536(6) . ?
C4 O8 1.230(7) . ?
C4 O7 1.266(6) . ?
C4 C8 1.512(6) . ?
C5 N1 1.451(7) . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 N2 1.452(6) . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 N2 1.440(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N3 1.447(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N5 1.315(6) . ?
C9 N1 1.323(6) . ?
C9 N4 1.379(6) . ?
C10 N5 1.339(6) . ?
C10 N2 1.340(6) . ?
C10 N6 1.351(6) . ?
C11 N6 1.321(6) . ?
C11 N3 1.326(6) . ?
C11 N4 1.367(6) . ?
N1 H1A 0.8600 . ?
N3 H3A 0.8600 . ?
O1 Tb1 2.425(4) 4_556 ?
O2 Tb1 2.449(4) 4_556 ?
O3 Tb1 2.357(3) 3_655 ?
O5 Tb1 2.310(3) 1_556 ?
O7 Tb1 2.253(3) 1_556 ?
O9W H9WA 0.8500 . ?
O9W H9WB 0.8500 . ?
O10W H10A 0.8181 . ?
O10W H10B 0.7945 . ?
O11W H11A 0.8500 . ?
O11W H11B 0.8499 . ?
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
O7 Tb1 O5 86.48(13) 1_554 1_554 ?
O7 Tb1 O9W 95.3(2) 1_554 . ?
O5 Tb1 O9W 76.49(17) 1_554 . ?
O7 Tb1 O3 162.96(12) 1_554 3_655 ?
O5 Tb1 O3 78.56(12) 1_554 3_655 ?
O9W Tb1 O3 89.14(19) . 3_655 ?
O7 Tb1 O1 83.89(15) 1_554 4 ?
O5 Tb1 O1 134.43(13) 1_554 4 ?
O9W Tb1 O1 148.68(15) . 4 ?
O3 Tb1 O1 100.74(15) 3_655 4 ?
O7 Tb1 O2 88.70(15) 1_554 4 ?
O5 Tb1 O2 82.02(13) 1_554 4 ?
O9W Tb1 O2 157.83(15) . 4 ?
O3 Tb1 O2 81.24(14) 3_655 4 ?
O1 Tb1 O2 53.39(12) 4 4 ?
O7 Tb1 O3 131.13(12) 1_554 . ?
O5 Tb1 O3 137.14(12) 1_554 . ?
O9W Tb1 O3 79.8(2) . . ?
O3 Tb1 O3 65.85(12) 3_655 . ?
O1 Tb1 O3 77.48(14) 4 . ?
O2 Tb1 O3 113.60(14) 4 . ?
O7 Tb1 O4 79.57(12) 1_554 . ?
O5 Tb1 O4 145.40(13) 1_554 . ?
O9W Tb1 O4 73.51(15) . . ?
O3 Tb1 O4 117.44(10) 3_655 . ?
O1 Tb1 O4 75.58(12) 4 . ?
O2 Tb1 O4 128.63(12) 4 . ?
O3 Tb1 O4 52.21(10) . . ?
O7 Tb1 C1 84.53(16) 1_554 4 ?
O5 Tb1 C1 108.40(13) 1_554 4 ?
O9W Tb1 C1 175.07(16) . 4 ?
O3 Tb1 C1 92.43(15) 3_655 4 ?
O1 Tb1 C1 26.38(13) 4 4 ?
O2 Tb1 C1 27.07(13) 4 4 ?
O3 Tb1 C1 96.60(15) . 4 ?
O4 Tb1 C1 101.64(13) . 4 ?
O7 Tb1 C2 105.08(14) 1_554 . ?
O5 Tb1 C2 150.70(12) 1_554 . ?
O9W Tb1 C2 75.70(17) . . ?
O3 Tb1 C2 91.96(12) 3_655 . ?
O1 Tb1 C2 74.34(11) 4 . ?
O2 Tb1 C2 124.27(12) 4 . ?
O3 Tb1 C2 26.34(12) . . ?
O4 Tb1 C2 25.89(12) . . ?
C1 Tb1 C2 99.57(12) 4 . ?
O1 C1 O2 121.5(5) . . ?
O1 C1 C5 120.4(5) . . ?
O2 C1 C5 118.1(4) . . ?
O1 C1 Tb1 60.3(3) . 4_556 ?
O2 C1 Tb1 61.4(3) . 4_556 ?
C5 C1 Tb1 176.5(4) . 4_556 ?
O4 C2 O3 120.5(4) . . ?
O4 C2 C6 122.1(4) . . ?
O3 C2 C6 117.3(4) . . ?
O4 C2 Tb1 61.1(2) . . ?
O3 C2 Tb1 59.5(2) . . ?
C6 C2 Tb1 176.0(3) . . ?
O5 C3 O6 125.5(4) . . ?
O5 C3 C7 118.0(4) . . ?
O6 C3 C7 116.5(4) . . ?
O8 C4 O7 125.7(5) . . ?
O8 C4 C8 116.5(4) . . ?
O7 C4 C8 117.8(5) . . ?
N1 C5 C1 113.2(5) . . ?
N1 C5 H5B 108.9 . . ?
C1 C5 H5B 108.9 . . ?
N1 C5 H5C 108.9 . . ?
C1 C5 H5C 108.9 . . ?
H5B C5 H5C 107.7 . . ?
N2 C6 C2 113.9(4) . . ?
N2 C6 H6B 108.8 . . ?
C2 C6 H6B 108.8 . . ?
N2 C6 H6C 108.8 . . ?
C2 C6 H6C 108.8 . . ?
H6B C6 H6C 107.7 . . ?
N2 C7 C3 114.4(4) . . ?
N2 C7 H7A 108.6 . . ?
C3 C7 H7A 108.6 . . ?
N2 C7 H7B 108.6 . . ?
C3 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
N3 C8 C4 115.7(4) . . ?
N3 C8 H8A 108.4 . . ?
C4 C8 H8A 108.4 . . ?
N3 C8 H8B 108.4 . . ?
C4 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
N5 C9 N1 121.2(4) . . ?
N5 C9 N4 122.0(4) . . ?
N1 C9 N4 116.9(4) . . ?
N5 C10 N2 117.5(4) . . ?
N5 C10 N6 126.7(4) . . ?
N2 C10 N6 115.9(4) . . ?
N6 C11 N3 119.1(5) . . ?
N6 C11 N4 122.5(4) . . ?
N3 C11 N4 118.4(5) . . ?
C9 N1 C5 121.2(4) . . ?
C9 N1 H1A 119.4 . . ?
C5 N1 H1A 119.4 . . ?
C10 N2 C7 120.1(4) . . ?
C10 N2 C6 120.9(4) . . ?
C7 N2 C6 119.0(4) . . ?
C11 N3 C8 122.4(4) . . ?
C11 N3 H3A 118.8 . . ?
C8 N3 H3A 118.8 . . ?
C11 N4 C9 117.8(4) . . ?
C9 N5 C10 115.8(4) . . ?
C11 N6 C10 115.1(4) . . ?
C1 O1 Tb1 93.3(3) . 4_556 ?
C1 O2 Tb1 91.5(3) . 4_556 ?
C2 O3 Tb1 150.7(3) . 3_655 ?
C2 O3 Tb1 94.1(3) . . ?
Tb1 O3 Tb1 114.15(12) 3_655 . ?
C2 O4 Tb1 93.0(3) . . ?
C3 O5 Tb1 144.5(3) . 1_556 ?
C4 O7 Tb1 147.9(4) . 1_556 ?
Tb1 O9W H9WA 110.6 . . ?
Tb1 O9W H9WB 109.7 . . ?
H9WA O9W H9WB 108.6 . . ?
H10A O10W H10B 115.3 . . ?
H11A O11W H11B 108.4 . . ?
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 O8 0.86 2.03 2.797(6) 148.5 2_746
N3 H3A O4 0.86 2.26 2.948(5) 136.6 3_756
O9W H9WA O6 0.85 2.09 2.767(7) 136.3 4_565
O9W H9WB O11W 0.85 2.02 2.709(10) 137.8 .
O10W H10A O6 0.82 2.17 2.910(6) 150.7 4_565
O10W H10B O8 0.79 1.90 2.680(6) 165.8 1_554
O11W H11B O2 0.85 2.13 2.828(10) 139.4 3_655
_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.064
_refine_diff_density_min         -2.271
_refine_diff_density_rms         0.149