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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Ming-Liang Tong'
_publ_contact_author_email       TONGML@MAIL.SYSU.EDU.CN

_publ_section_title              
;
Synthesis, Structure, Photoluminescence and Magnetic
Properties of New Three-Dimensional
Lanthanide-pyridine-2,4,6-tricarboxylate Frameworks
;
loop_
_publ_author_name
'Ming-Liang Tong.'
'Ji-Dong Leng.'
'Cui-Jin Li.'
'Zhuojia Lin.'
;
Meng-Xia Peng
;
'Ming-Mei Yang.'

data_ndm
_database_code_depnum_ccdc_archive 'CCDC 687909'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H16 N2 Nd2 O18'
_chemical_formula_weight         812.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   pc

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

_cell_length_a                   6.7735(5)
_cell_length_b                   9.3861(7)
_cell_length_c                   16.9365(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.5690(10)
_cell_angle_gamma                90.00
_cell_volume                     1075.69(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7147
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      27.47

_exptl_crystal_description       plate-like
_exptl_crystal_colour            'pale purple'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    4.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8920
_exptl_absorpt_correction_T_max  0.9574
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7147
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         27.47
_reflns_number_total             4244
_reflns_number_gt                4114
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'

_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)+(0.0153P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(15)
_refine_ls_number_reflns         4244
_refine_ls_number_parameters     343
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0564
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.26003(4) 0.43101(3) 0.780791(19) 0.01551(8) Uani 1 1 d . . .
Nd2 Nd -0.25533(4) 0.81345(3) 1.010049(19) 0.01487(8) Uani 1 1 d . . .
O1 O 0.1537(7) 0.6082(5) 0.8834(2) 0.0223(10) Uani 1 1 d . . .
O2 O 0.0336(6) 0.8156(4) 0.9220(2) 0.0228(9) Uani 1 1 d . . .
O3 O 0.1305(7) 1.2189(5) 0.7146(3) 0.0311(11) Uani 1 1 d . . .
O4 O 0.0497(6) 1.1476(5) 0.5923(2) 0.0216(10) Uani 1 1 d . . .
O5 O 0.2345(8) 0.6332(5) 0.5365(2) 0.0345(12) Uani 1 1 d . . .
O6 O 0.2982(7) 0.4944(5) 0.6409(3) 0.0218(11) Uani 1 1 d . . .
O7 O -0.2119(7) 1.0658(4) 0.9801(2) 0.0227(10) Uani 1 1 d . . .
O8 O -0.2384(10) 1.2966(5) 1.0063(4) 0.0310(11) Uani 1 1 d . . .
O9 O -0.4347(6) 1.4168(5) 1.2926(3) 0.0216(10) Uani 1 1 d . . .
O10 O -0.3822(7) 1.2396(5) 1.3772(2) 0.0287(11) Uani 1 1 d . . .
O11 O -0.4577(7) 0.7352(5) 1.2595(3) 0.0279(11) Uani 1 1 d . . .
O12 O -0.3268(6) 0.7183(5) 1.1425(2) 0.0205(10) Uani 1 1 d . . .
O1W O -0.0898(7) 0.4678(6) 0.7307(4) 0.0434(15) Uani 1 1 d D . .
H1WA H -0.1368 0.4335 0.6874 0.052 Uiso 1 1 d RD . .
H1WB H -0.1782 0.4854 0.7635 0.052 Uiso 1 1 d RD . .
O2W O 0.0170(11) 0.3001(7) 0.8697(4) 0.079(3) Uani 1 1 d D . .
H2WA H 0.1074 0.2549 0.8956 0.095 Uiso 1 1 d RD . .
H2WB H -0.0904 0.2876 0.8928 0.095 Uiso 1 1 d RD . .
O3W O 0.4215(9) 0.3514(8) 0.9052(3) 0.065(2) Uani 1 1 d DU . .
H3WA H 0.3832 0.4064 0.9414 0.078 Uiso 1 1 d RD . .
H3WB H 0.5469 0.3479 0.9096 0.078 Uiso 1 1 d RD . .
O4W O -0.5972(8) 0.9551(6) 0.9819(4) 0.0501(16) Uani 1 1 d D . .
H4WA H -0.6568 0.9176 0.9418 0.060 Uiso 1 1 d RD . .
H4WB H -0.6690 0.9422 1.0211 0.060 Uiso 1 1 d RD . .
O5W O -0.5481(8) 0.6577(6) 1.0150(3) 0.0372(14) Uani 1 1 d D . .
H5WA H -0.5900 0.6323 1.0594 0.045 Uiso 1 1 d RD . .
H5WB H -0.6288 0.6399 0.9763 0.045 Uiso 1 1 d RD . .
O6W O -0.1169(7) 0.5719(5) 1.0112(3) 0.0349(12) Uani 1 1 d D . .
H6WA H -0.1423 0.4893 1.0287 0.042 Uiso 1 1 d RD . .
H6WB H -0.0216 0.5678 0.9803 0.042 Uiso 1 1 d RD . .
N1 N 0.1792(7) 0.6940(5) 0.7377(3) 0.0135(10) Uani 1 1 d . . .
N2 N -0.3273(7) 0.9928(5) 1.1208(3) 0.0140(10) Uani 1 1 d . . .
C1 C 0.1320(8) 0.7930(6) 0.7906(3) 0.0146(12) Uani 1 1 d . . .
C2 C 0.1034(9) 0.9339(6) 0.7692(3) 0.0164(12) Uani 1 1 d . . .
H2 H 0.0709 1.0015 0.8066 0.020 Uiso 1 1 calc R . .
C3 C 0.1242(8) 0.9733(6) 0.6900(3) 0.0126(11) Uani 1 1 d . . .
C4 C 0.1630(8) 0.8664(7) 0.6368(3) 0.0176(12) Uani 1 1 d . . .
H4 H 0.1684 0.8875 0.5833 0.021 Uiso 1 1 calc R . .
C5 C 0.1933(8) 0.7303(6) 0.6622(3) 0.0145(11) Uani 1 1 d . . .
C6 C 0.1017(8) 0.7350(6) 0.8724(3) 0.0151(12) Uani 1 1 d . . .
C7 C 0.0994(8) 1.1262(6) 0.6629(3) 0.0170(12) Uani 1 1 d . . .
C8 C 0.2457(9) 0.6106(7) 0.6079(3) 0.0195(13) Uani 1 1 d . . .
C9 C -0.3057(8) 1.1318(7) 1.1081(3) 0.0143(12) Uani 1 1 d . . .
C10 C -0.3329(8) 1.2331(6) 1.1665(3) 0.0140(12) Uani 1 1 d . . .
H10 H -0.3240 1.3300 1.1558 0.017 Uiso 1 1 calc R . .
C11 C -0.3741(8) 1.1842(7) 1.2419(3) 0.0169(12) Uani 1 1 d . . .
C12 C -0.3937(8) 1.0406(7) 1.2549(3) 0.0170(12) Uani 1 1 d . . .
H12 H -0.4208 1.0068 1.3049 0.020 Uiso 1 1 calc R . .
C13 C -0.3729(8) 0.9467(6) 1.1929(3) 0.0144(12) Uani 1 1 d . . .
C14 C -0.2463(9) 1.1693(7) 1.0253(3) 0.0180(14) Uani 1 1 d . . .
C15 C -0.3986(8) 1.2891(7) 1.3103(3) 0.0156(12) Uani 1 1 d . . .
C16 C -0.3901(8) 0.7876(6) 1.1996(3) 0.0141(12) 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
Nd1 O3 2.429(4) 1_545 ?
Nd1 O3W 2.447(5) . ?
Nd1 O6 2.468(4) . ?
Nd1 O1W 2.505(5) . ?
Nd1 O11 2.506(4) 2_664 ?
Nd1 O9 2.514(4) 2_674 ?
Nd1 O1 2.533(4) . ?
Nd1 O2W 2.590(5) . ?
Nd1 N1 2.625(5) . ?
Nd2 O10 2.424(4) 2_574 ?
Nd2 O7 2.442(4) . ?
Nd2 O6W 2.453(5) . ?
Nd2 O4 2.467(4) 2_575 ?
Nd2 O5W 2.468(5) . ?
Nd2 O12 2.481(4) . ?
Nd2 O2 2.514(4) . ?
Nd2 N2 2.583(5) . ?
Nd2 O4W 2.694(6) . ?
O1 C6 1.253(7) . ?
O2 C6 1.234(7) . ?
O3 C7 1.246(7) . ?
O3 Nd1 2.429(4) 1_565 ?
O4 C7 1.244(7) . ?
O4 Nd2 2.467(4) 2_574 ?
O5 C8 1.227(7) . ?
O6 C8 1.269(8) . ?
O7 C14 1.265(7) . ?
O8 C14 1.239(8) . ?
O9 C15 1.257(7) . ?
O9 Nd1 2.514(4) 2_475 ?
O10 C15 1.224(7) . ?
O10 Nd2 2.424(4) 2_575 ?
O11 C16 1.235(7) . ?
O11 Nd1 2.506(4) 2_465 ?
O12 C16 1.256(7) . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8501 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8499 . ?
O3W H3WB 0.8500 . ?
O4W H4WA 0.8500 . ?
O4W H4WB 0.8500 . ?
O5W H5WA 0.8501 . ?
O5W H5WB 0.8499 . ?
O6W H6WA 0.8500 . ?
O6W H6WB 0.8499 . ?
N1 C5 1.332(7) . ?
N1 C1 1.339(7) . ?
N2 C9 1.331(8) . ?
N2 C13 1.344(7) . ?
C1 C2 1.382(8) . ?
C1 C6 1.512(8) . ?
C2 C3 1.405(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(8) . ?
C3 C7 1.514(8) . ?
C4 C5 1.360(8) . ?
C4 H4 0.9300 . ?
C5 C8 1.504(8) . ?
C9 C10 1.392(8) . ?
C9 C14 1.517(8) . ?
C10 C11 1.396(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.373(8) . ?
C11 C15 1.534(8) . ?
C12 C13 1.383(8) . ?
C12 H12 0.9300 . ?
C13 C16 1.503(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Nd1 O3W 106.6(2) 1_545 . ?
O3 Nd1 O6 78.81(16) 1_545 . ?
O3W Nd1 O6 146.97(18) . . ?
O3 Nd1 O1W 68.92(17) 1_545 . ?
O3W Nd1 O1W 135.5(2) . . ?
O6 Nd1 O1W 77.29(17) . . ?
O3 Nd1 O11 71.67(16) 1_545 2_664 ?
O3W Nd1 O11 67.63(16) . 2_664 ?
O6 Nd1 O11 84.17(14) . 2_664 ?
O1W Nd1 O11 138.89(17) . 2_664 ?
O3 Nd1 O9 141.37(16) 1_545 2_674 ?
O3W Nd1 O9 76.7(2) . 2_674 ?
O6 Nd1 O9 79.53(15) . 2_674 ?
O1W Nd1 O9 135.31(17) . 2_674 ?
O11 Nd1 O9 74.64(16) 2_664 2_674 ?
O3 Nd1 O1 138.30(16) 1_545 . ?
O3W Nd1 O1 74.88(17) . . ?
O6 Nd1 O1 123.09(15) . . ?
O1W Nd1 O1 81.27(16) . . ?
O11 Nd1 O1 138.54(15) 2_664 . ?
O9 Nd1 O1 80.23(14) 2_674 . ?
O3 Nd1 O2W 69.73(18) 1_545 . ?
O3W Nd1 O2W 68.0(2) . . ?
O6 Nd1 O2W 140.3(2) . . ?
O1W Nd1 O2W 69.3(2) . . ?
O11 Nd1 O2W 107.3(2) 2_664 . ?
O9 Nd1 O2W 139.92(18) 2_674 . ?
O1 Nd1 O2W 72.83(17) . . ?
O3 Nd1 N1 125.18(15) 1_545 . ?
O3W Nd1 N1 127.3(2) . . ?
O6 Nd1 N1 62.36(15) . . ?
O1W Nd1 N1 66.04(16) . . ?
O11 Nd1 N1 134.14(15) 2_664 . ?
O9 Nd1 N1 69.41(14) 2_674 . ?
O1 Nd1 N1 60.74(14) . . ?
O2W Nd1 N1 118.5(2) . . ?
O10 Nd2 O7 92.71(15) 2_574 . ?
O10 Nd2 O6W 86.41(18) 2_574 . ?
O7 Nd2 O6W 148.02(16) . . ?
O10 Nd2 O4 143.87(15) 2_574 2_575 ?
O7 Nd2 O4 82.42(15) . 2_575 ?
O6W Nd2 O4 79.75(17) . 2_575 ?
O10 Nd2 O5W 69.99(15) 2_574 . ?
O7 Nd2 O5W 133.29(18) . . ?
O6W Nd2 O5W 76.10(18) . . ?
O4 Nd2 O5W 136.27(16) 2_575 . ?
O10 Nd2 O12 133.60(15) 2_574 . ?
O7 Nd2 O12 124.52(14) . . ?
O6W Nd2 O12 75.53(16) . . ?
O4 Nd2 O12 74.65(14) 2_575 . ?
O5W Nd2 O12 64.34(14) . . ?
O10 Nd2 O2 72.77(15) 2_574 . ?
O7 Nd2 O2 76.39(13) . . ?
O6W Nd2 O2 72.83(14) . . ?
O4 Nd2 O2 71.29(14) 2_575 . ?
O5W Nd2 O2 132.30(15) . . ?
O12 Nd2 O2 136.70(15) . . ?
O10 Nd2 N2 137.51(16) 2_574 . ?
O7 Nd2 N2 63.08(14) . . ?
O6W Nd2 N2 132.91(17) . . ?
O4 Nd2 N2 70.97(14) 2_575 . ?
O5W Nd2 N2 100.57(16) . . ?
O12 Nd2 N2 61.80(14) . . ?
O2 Nd2 N2 127.09(14) . . ?
O10 Nd2 O4W 70.77(17) 2_574 . ?
O7 Nd2 O4W 66.14(16) . . ?
O6W Nd2 O4W 141.50(17) . . ?
O4 Nd2 O4W 135.94(16) 2_575 . ?
O5W Nd2 O4W 67.20(19) . . ?
O12 Nd2 O4W 97.86(17) . . ?
O2 Nd2 O4W 125.23(17) . . ?
N2 Nd2 O4W 67.57(16) . . ?
C6 O1 Nd1 127.5(4) . . ?
C6 O2 Nd2 136.3(4) . . ?
C7 O3 Nd1 160.5(4) . 1_565 ?
C7 O4 Nd2 138.6(4) . 2_574 ?
C8 O6 Nd1 126.2(4) . . ?
C14 O7 Nd2 126.3(4) . . ?
C15 O9 Nd1 135.3(4) . 2_475 ?
C15 O10 Nd2 161.8(5) . 2_575 ?
C16 O11 Nd1 132.8(4) . 2_465 ?
C16 O12 Nd2 126.6(4) . . ?
Nd1 O1W H1WA 123.5 . . ?
Nd1 O1W H1WB 119.3 . . ?
H1WA O1W H1WB 112.9 . . ?
Nd1 O2W H2WA 94.3 . . ?
Nd1 O2W H2WB 155.9 . . ?
H2WA O2W H2WB 107.8 . . ?
Nd1 O3W H3WA 107.2 . . ?
Nd1 O3W H3WB 119.5 . . ?
H3WA O3W H3WB 107.3 . . ?
Nd2 O4W H4WA 108.1 . . ?
Nd2 O4W H4WB 108.0 . . ?
H4WA O4W H4WB 107.4 . . ?
Nd2 O5W H5WA 119.8 . . ?
Nd2 O5W H5WB 125.5 . . ?
H5WA O5W H5WB 113.4 . . ?
Nd2 O6W H6WA 139.7 . . ?
Nd2 O6W H6WB 109.7 . . ?
H6WA O6W H6WB 110.2 . . ?
C5 N1 C1 119.6(5) . . ?
C5 N1 Nd1 119.0(4) . . ?
C1 N1 Nd1 121.3(4) . . ?
C9 N2 C13 119.7(5) . . ?
C9 N2 Nd2 119.7(4) . . ?
C13 N2 Nd2 120.5(4) . . ?
N1 C1 C2 121.6(5) . . ?
N1 C1 C6 114.2(5) . . ?
C2 C1 C6 124.2(5) . . ?
C1 C2 C3 118.9(5) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 117.5(5) . . ?
C4 C3 C7 120.9(5) . . ?
C2 C3 C7 121.6(5) . . ?
C5 C4 C3 120.4(5) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
N1 C5 C4 121.9(5) . . ?
N1 C5 C8 115.1(5) . . ?
C4 C5 C8 123.0(5) . . ?
O2 C6 O1 126.3(5) . . ?
O2 C6 C1 118.2(5) . . ?
O1 C6 C1 115.4(5) . . ?
O4 C7 O3 126.4(6) . . ?
O4 C7 C3 117.7(5) . . ?
O3 C7 C3 115.8(5) . . ?
O5 C8 O6 125.9(6) . . ?
O5 C8 C5 117.8(6) . . ?
O6 C8 C5 116.3(5) . . ?
N2 C9 C10 122.3(5) . . ?
N2 C9 C14 114.4(5) . . ?
C10 C9 C14 123.2(6) . . ?
C9 C10 C11 117.7(6) . . ?
C9 C10 H10 121.2 . . ?
C11 C10 H10 121.2 . . ?
C12 C11 C10 119.6(5) . . ?
C12 C11 C15 119.6(5) . . ?
C10 C11 C15 120.8(5) . . ?
C11 C12 C13 119.4(5) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
N2 C13 C12 121.3(5) . . ?
N2 C13 C16 114.2(5) . . ?
C12 C13 C16 124.4(5) . . ?
O8 C14 O7 124.9(5) . . ?
O8 C14 C9 118.7(6) . . ?
O7 C14 C9 116.4(5) . . ?
O10 C15 O9 126.2(6) . . ?
O10 C15 C11 116.5(5) . . ?
O9 C15 C11 117.2(5) . . ?
O11 C16 O12 125.4(6) . . ?
O11 C16 C13 119.4(5) . . ?
O12 C16 C13 115.2(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
O1W H1WA O12 0.85 2.04 2.765(7) 142.2 2_564
O1W H1WB O9 0.85 2.05 2.819(7) 151.1 2_574
O2W H2WA O3W 0.85 2.31 2.820(10) 118.7 .
O2W H2WB O8 0.85 2.21 2.950(8) 145.8 1_545
O3W H3WA O5 0.85 1.97 2.612(7) 131.1 2_565
O3W H3WB O8 0.85 2.19 2.855(9) 134.4 1_645
O4W H4WA O2 0.85 2.32 2.961(7) 132.9 1_455
O4W H4WB O4 0.85 2.45 3.248(7) 156.7 2_475
O5W H5WA O6 0.85 2.00 2.805(6) 158.6 2_465
O5W H5WB O1 0.85 2.13 2.976(7) 175.3 1_455
O6W H6WA O8 0.85 1.95 2.711(7) 147.9 1_545
O6W H6WB O1 0.85 2.10 2.919(6) 160.7 .

_diffrn_measured_fraction_theta_max 0.944
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.944
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.129

data_smm
_database_code_depnum_ccdc_archive 'CCDC 687910'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H15 N2 O17.50 Sm2'
_chemical_formula_weight         816.00

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'
Sm Sm -0.1638 3.4418 '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                   22.3162(11)
_cell_length_b                   9.3759(5)
_cell_length_c                   22.4546(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.0610(10)
_cell_angle_gamma                90.00
_cell_volume                     4576.7(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17304
_cell_measurement_theta_min      1.87
_cell_measurement_theta_max      26.00

_exptl_crystal_description       cuboid
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3112
_exptl_absorpt_coefficient_mu    5.174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6126
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17304
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4485
_reflns_number_gt                4292
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'

_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)+(0.0249P)²+31.6226P] where P=(Fo²+2Fc²)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4485
_refine_ls_number_parameters     344
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0618
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.109
_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
Sm1 Sm 0.046073(10) 0.27268(2) 0.432472(10) 0.01246(7) Uani 1 1 d . . .
Sm2 Sm 0.154291(9) 0.35796(2) 0.178889(9) 0.01028(7) Uani 1 1 d . . .
O1W O -0.03776(15) 0.2841(4) 0.48796(15) 0.0233(7) Uani 1 1 d D . .
H1WA H -0.0319 0.3360 0.5198 0.028 Uiso 1 1 d RD . .
H1WB H -0.0738 0.2492 0.4819 0.028 Uiso 1 1 d RD . .
O2W O 0.12524(17) 0.0957(4) 0.42622(17) 0.0339(9) Uani 1 1 d D . .
H2WA H 0.1337 0.0835 0.3915 0.041 Uiso 1 1 d RD . .
H2WB H 0.1315 0.0201 0.4476 0.041 Uiso 1 1 d RD . .
O3W O 0.05824(17) 0.0838(4) 0.51260(16) 0.0300(8) Uani 1 1 d D . .
H3WA H 0.0371 0.0610 0.5383 0.036 Uiso 1 1 d RD . .
H3WB H 0.0604 0.0071 0.4930 0.036 Uiso 1 1 d RD . .
O1 O 0.07322(15) 0.3039(4) 0.33465(14) 0.0218(7) Uani 1 1 d . . .
O2 O 0.13191(16) 0.3920(4) 0.27540(14) 0.0257(8) Uani 1 1 d . . .
O3 O 0.31830(18) 0.6822(4) 0.38638(17) 0.0366(9) Uani 1 1 d . . .
O4 O 0.35410(15) 0.6270(4) 0.48379(17) 0.0303(8) Uani 1 1 d . . .
O5 O 0.16737(15) 0.5271(4) 0.58583(14) 0.0245(8) Uani 1 1 d . . .
O6 O 0.09554(14) 0.3872(4) 0.52862(14) 0.0201(7) Uani 1 1 d . . .
O7 O 0.23337(14) 0.5360(3) 0.21702(15) 0.0217(7) Uani 1 1 d . . .
O8 O 0.26067(16) 0.7499(4) 0.25523(19) 0.0344(9) Uani 1 1 d . . .
O9 O 0.09999(15) 1.1417(3) 0.19123(16) 0.0247(8) Uani 1 1 d . . .
O10 O 0.02078(15) 1.0841(3) 0.11467(15) 0.0252(8) Uani 1 1 d . . .
O11 O -0.02800(14) 0.5423(3) 0.08641(14) 0.0192(7) Uani 1 1 d . . .
O12 O 0.04634(14) 0.4025(3) 0.13484(14) 0.0166(6) Uani 1 1 d . . .
N1 N 0.14415(16) 0.4119(4) 0.43384(16) 0.0143(8) Uani 1 1 d . . .
N2 N 0.11837(16) 0.6151(4) 0.17773(16) 0.0137(7) Uani 1 1 d . . .
C1 C 0.1636(2) 0.4284(5) 0.38219(19) 0.0170(9) Uani 1 1 d . . .
C2 C 0.2171(2) 0.4997(5) 0.3806(2) 0.0209(10) Uani 1 1 d . . .
H2 H 0.2295 0.5110 0.3440 0.025 Uiso 1 1 calc R . .
C3 C 0.2524(2) 0.5548(5) 0.4352(2) 0.0174(9) Uani 1 1 d . . .
C4 C 0.2308(2) 0.5418(5) 0.4884(2) 0.0169(9) Uani 1 1 d . . .
H4 H 0.2529 0.5797 0.5251 0.020 Uiso 1 1 calc R . .
C5 C 0.1758(2) 0.4714(5) 0.48562(19) 0.0155(9) Uani 1 1 d . . .
C6 C 0.1195(2) 0.3684(5) 0.3262(2) 0.0169(9) Uani 1 1 d . . .
C7 C 0.3132(2) 0.6277(5) 0.4353(2) 0.0194(10) Uani 1 1 d . . .
C8 C 0.1439(2) 0.4594(5) 0.5383(2) 0.0162(9) Uani 1 1 d . . .
C9 C 0.1588(2) 0.7180(5) 0.1993(2) 0.0150(9) Uani 1 1 d . . .
C10 C 0.1437(2) 0.8612(5) 0.1944(2) 0.0177(9) Uani 1 1 d . . .
H10 H 0.1728 0.9307 0.2100 0.021 Uiso 1 1 calc R . .
C11 C 0.0838(2) 0.8984(5) 0.1656(2) 0.0162(9) Uani 1 1 d . . .
C12 C 0.0414(2) 0.7921(5) 0.1427(2) 0.0177(9) Uani 1 1 d . . .
H12 H 0.0010 0.8141 0.1237 0.021 Uiso 1 1 calc R . .
C13 C 0.0615(2) 0.6522(5) 0.1494(2) 0.0147(9) Uani 1 1 d . . .
C14 C 0.2231(2) 0.6644(5) 0.2265(2) 0.0168(9) Uani 1 1 d . . .
C15 C 0.0667(2) 1.0545(5) 0.1570(2) 0.0176(9) Uani 1 1 d . . .
C16 C 0.02332(19) 0.5260(5) 0.12175(19) 0.0141(9) Uani 1 1 d . . .
O4W O 0.1528(2) 0.0302(6) 0.3201(2) 0.0670(14) Uani 1 1 d U . .
O5W O 0.0000 0.5539(14) 0.2500 0.127(4) Uani 1 2 d SU . .
O6W O 0.0000 0.0696(18) 0.2500 0.176(6) Uani 1 2 d SU . .
O7W O -0.0872(12) 0.756(3) 0.1815(12) 0.197(10) Uani 0.50 1 d PU . .


_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
Sm1 O10 2.400(3) 2_545 ?
Sm1 O1 2.425(3) . ?
Sm1 O6 2.440(3) . ?
Sm1 O2W 2.451(3) . ?
Sm1 O1W 2.473(3) . ?
Sm1 O3W 2.495(3) . ?
Sm1 N1 2.543(4) . ?
Sm1 O12 2.571(3) 2 ?
Sm1 O11 2.580(3) 2 ?
Sm1 C16 2.945(4) 2 ?
Sm2 O2 2.353(3) . ?
Sm2 O8 2.355(3) 4_545 ?
Sm2 O3 2.376(4) 4_545 ?
Sm2 O9 2.410(3) 1_545 ?
Sm2 O12 2.425(3) . ?
Sm2 O5 2.427(3) 6_565 ?
Sm2 O7 2.439(3) . ?
Sm2 N2 2.539(4) . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8499 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8500 . ?
O1 C6 1.247(6) . ?
O2 C6 1.253(5) . ?
O3 C7 1.241(6) . ?
O3 Sm2 2.376(4) 4 ?
O4 C7 1.252(6) . ?
O5 C8 1.251(5) . ?
O5 Sm2 2.427(3) 6_566 ?
O6 C8 1.250(5) . ?
O7 C14 1.252(5) . ?
O8 C14 1.232(6) . ?
O8 Sm2 2.355(3) 4 ?
O9 C15 1.246(5) . ?
O9 Sm2 2.410(3) 1_565 ?
O10 C15 1.261(5) . ?
O10 Sm1 2.400(3) 2_565 ?
O11 C16 1.247(5) . ?
O11 Sm1 2.580(3) 2 ?
O12 C16 1.274(5) . ?
O12 Sm1 2.571(3) 2 ?
N1 C1 1.336(6) . ?
N1 C5 1.338(6) . ?
N2 C13 1.330(6) . ?
N2 C9 1.336(6) . ?
C1 C2 1.376(7) . ?
C1 C6 1.519(6) . ?
C2 C3 1.399(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(6) . ?
C3 C7 1.518(6) . ?
C4 C5 1.383(6) . ?
C4 H4 0.9300 . ?
C5 C8 1.516(6) . ?
C9 C10 1.382(6) . ?
C9 C14 1.513(6) . ?
C10 C11 1.392(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.390(6) . ?
C11 C15 1.513(6) . ?
C12 C13 1.383(6) . ?
C12 H12 0.9300 . ?
C13 C16 1.507(6) . ?
C16 Sm1 2.945(4) 2 ?

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
O10 Sm1 O1 86.96(12) 2_545 . ?
O10 Sm1 O6 145.72(11) 2_545 . ?
O1 Sm1 O6 126.35(10) . . ?
O10 Sm1 O2W 81.97(13) 2_545 . ?
O1 Sm1 O2W 72.47(12) . . ?
O6 Sm1 O2W 99.25(12) . . ?
O10 Sm1 O1W 77.79(12) 2_545 . ?
O1 Sm1 O1W 145.43(11) . . ?
O6 Sm1 O1W 77.16(10) . . ?
O2W Sm1 O1W 134.05(12) . . ?
O10 Sm1 O3W 75.57(12) 2_545 . ?
O1 Sm1 O3W 136.89(12) . . ?
O6 Sm1 O3W 73.77(12) . . ?
O2W Sm1 O3W 66.32(12) . . ?
O1W Sm1 O3W 68.84(12) . . ?
O10 Sm1 N1 146.23(12) 2_545 . ?
O1 Sm1 N1 63.79(11) . . ?
O6 Sm1 N1 63.09(10) . . ?
O2W Sm1 N1 73.66(12) . . ?
O1W Sm1 N1 135.95(11) . . ?
O3W Sm1 N1 113.74(12) . . ?
O10 Sm1 O12 75.72(10) 2_545 2 ?
O1 Sm1 O12 75.03(11) . 2 ?
O6 Sm1 O12 117.01(10) . 2 ?
O2W Sm1 O12 141.23(11) . 2 ?
O1W Sm1 O12 71.22(11) . 2 ?
O3W Sm1 O12 134.59(11) . 2 ?
N1 Sm1 O12 109.75(11) . 2 ?
O10 Sm1 O11 126.22(10) 2_545 2 ?
O1 Sm1 O11 78.15(11) . 2 ?
O6 Sm1 O11 74.75(10) . 2 ?
O2W Sm1 O11 137.90(12) . 2 ?
O1W Sm1 O11 86.13(11) . 2 ?
O3W Sm1 O11 143.27(11) . 2 ?
N1 Sm1 O11 66.49(11) . 2 ?
O12 Sm1 O11 50.55(9) 2 2 ?
O10 Sm1 C16 101.27(11) 2_545 2 ?
O1 Sm1 C16 75.16(12) . 2 ?
O6 Sm1 C16 95.82(12) . 2 ?
O2W Sm1 C16 147.25(12) . 2 ?
O1W Sm1 C16 77.67(12) . 2 ?
O3W Sm1 C16 146.31(12) . 2 ?
N1 Sm1 C16 87.80(12) . 2 ?
O12 Sm1 C16 25.58(11) 2 2 ?
O11 Sm1 C16 24.98(10) 2 2 ?
O2 Sm2 O8 77.79(14) . 4_545 ?
O2 Sm2 O3 143.15(13) . 4_545 ?
O8 Sm2 O3 78.80(14) 4_545 4_545 ?
O2 Sm2 O9 77.96(12) . 1_545 ?
O8 Sm2 O9 85.45(12) 4_545 1_545 ?
O3 Sm2 O9 72.15(13) 4_545 1_545 ?
O2 Sm2 O12 87.38(11) . . ?
O8 Sm2 O12 156.28(12) 4_545 . ?
O3 Sm2 O12 103.80(12) 4_545 . ?
O9 Sm2 O12 73.31(11) 1_545 . ?
O2 Sm2 O5 145.56(12) . 6_565 ?
O8 Sm2 O5 119.68(13) 4_545 6_565 ?
O3 Sm2 O5 71.27(13) 4_545 6_565 ?
O9 Sm2 O5 129.35(12) 1_545 6_565 ?
O12 Sm2 O5 82.76(11) . 6_565 ?
O2 Sm2 O7 82.60(12) . . ?
O8 Sm2 O7 69.98(11) 4_545 . ?
O3 Sm2 O7 115.12(13) 4_545 . ?
O9 Sm2 O7 151.40(11) 1_545 . ?
O12 Sm2 O7 126.76(10) . . ?
O5 Sm2 O7 77.30(12) 6_565 . ?
O2 Sm2 N2 75.42(12) . . ?
O8 Sm2 N2 128.51(12) 4_545 . ?
O3 Sm2 N2 141.00(13) 4_545 . ?
O9 Sm2 N2 129.36(12) 1_545 . ?
O12 Sm2 N2 63.25(11) . . ?
O5 Sm2 N2 70.65(11) 6_565 . ?
O7 Sm2 N2 63.61(11) . . ?
Sm1 O1W H1WA 117.3 . . ?
Sm1 O1W H1WB 134.4 . . ?
H1WA O1W H1WB 108.3 . . ?
Sm1 O2W H2WA 117.1 . . ?
Sm1 O2W H2WB 124.2 . . ?
H2WA O2W H2WB 111.3 . . ?
Sm1 O3W H3WA 132.9 . . ?
Sm1 O3W H3WB 103.7 . . ?
H3WA O3W H3WB 104.1 . . ?
C6 O1 Sm1 125.5(3) . . ?
C6 O2 Sm2 162.0(3) . . ?
C7 O3 Sm2 157.0(3) . 4 ?
C8 O5 Sm2 148.4(3) . 6_566 ?
C8 O6 Sm1 126.3(3) . . ?
C14 O7 Sm2 124.9(3) . . ?
C14 O8 Sm2 164.9(3) . 4 ?
C15 O9 Sm2 136.6(3) . 1_565 ?
C15 O10 Sm1 144.4(3) . 2_565 ?
C16 O11 Sm1 94.1(3) . 2 ?
C16 O12 Sm2 124.2(3) . . ?
C16 O12 Sm1 93.8(2) . 2 ?
Sm2 O12 Sm1 138.52(13) . 2 ?
C1 N1 C5 119.6(4) . . ?
C1 N1 Sm1 119.8(3) . . ?
C5 N1 Sm1 120.6(3) . . ?
C13 N2 C9 118.5(4) . . ?
C13 N2 Sm2 121.2(3) . . ?
C9 N2 Sm2 119.8(3) . . ?
N1 C1 C2 122.2(4) . . ?
N1 C1 C6 113.5(4) . . ?
C2 C1 C6 124.2(4) . . ?
C1 C2 C3 118.5(4) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 119.0(4) . . ?
C4 C3 C7 121.4(4) . . ?
C2 C3 C7 119.6(4) . . ?
C5 C4 C3 118.6(4) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N1 C5 C4 121.9(4) . . ?
N1 C5 C8 113.4(4) . . ?
C4 C5 C8 124.7(4) . . ?
O1 C6 O2 125.8(4) . . ?
O1 C6 C1 117.2(4) . . ?
O2 C6 C1 116.9(4) . . ?
O3 C7 O4 125.2(4) . . ?
O3 C7 C3 116.4(4) . . ?
O4 C7 C3 118.4(4) . . ?
O6 C8 O5 126.9(4) . . ?
O6 C8 C5 116.4(4) . . ?
O5 C8 C5 116.6(4) . . ?
N2 C9 C10 122.7(4) . . ?
N2 C9 C14 114.0(4) . . ?
C10 C9 C14 123.2(4) . . ?
C9 C10 C11 118.2(4) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C12 C11 C10 119.5(4) . . ?
C12 C11 C15 121.1(4) . . ?
C10 C11 C15 119.3(4) . . ?
C13 C12 C11 117.6(4) . . ?
C13 C12 H12 121.2 . . ?
C11 C12 H12 121.2 . . ?
N2 C13 C12 123.4(4) . . ?
N2 C13 C16 112.4(4) . . ?
C12 C13 C16 124.0(4) . . ?
O8 C14 O7 125.8(4) . . ?
O8 C14 C9 117.8(4) . . ?
O7 C14 C9 116.4(4) . . ?
O9 C15 O10 126.1(4) . . ?
O9 C15 C11 117.3(4) . . ?
O10 C15 C11 116.6(4) . . ?
O11 C16 O12 121.5(4) . . ?
O11 C16 C13 121.3(4) . . ?
O12 C16 C13 117.2(4) . . ?
O11 C16 Sm1 60.9(2) . 2 ?
O12 C16 Sm1 60.6(2) . 2 ?
C13 C16 Sm1 177.4(3) . 2 ?

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
O1W H1WA O11 0.85 1.87 2.714(4) 173.5 6_566
O1W H1WB O4 0.85 1.98 2.811(5) 164.1 3_445
O2W H2WA O4W 0.85 1.82 2.663(6) 171.7 .
O2W H2WB O4 0.85 2.04 2.870(5) 165.7 7_556

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.404
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.131

data_eum
_database_code_depnum_ccdc_archive 'CCDC 687911'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H15 Eu2 N2 O17.50'
_chemical_formula_weight         819.22

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'
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   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                   22.2466(18)
_cell_length_b                   9.3529(7)
_cell_length_c                   22.4043(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.0670(10)
_cell_angle_gamma                90.00
_cell_volume                     4541.0(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11194
_cell_measurement_theta_min      1.87
_cell_measurement_theta_max      26.00

_exptl_crystal_description       cuboid
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3128
_exptl_absorpt_coefficient_mu    5.567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5452
_exptl_absorpt_correction_T_max  0.6284
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11194
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4418
_reflns_number_gt                3862
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'

_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)+(0.0415P)²+12.1770P] where P=(Fo²+2Fc²)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4418
_refine_ls_number_parameters     344
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0845
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.067
_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 0.046064(14) 0.27302(3) 0.432336(14) 0.01293(10) Uani 1 1 d . . .
Eu2 Eu 0.154393(14) 0.35922(3) 0.178937(13) 0.01021(10) Uani 1 1 d . . .
O1W O -0.0372(2) 0.2850(5) 0.4872(2) 0.0246(11) Uani 1 1 d D . .
H1WA H -0.0340 0.3269 0.5214 0.029 Uiso 1 1 d RD . .
H1WB H -0.0737 0.2531 0.4757 0.029 Uiso 1 1 d RD . .
O2W O 0.1247(2) 0.0963(6) 0.4264(2) 0.0332(13) Uani 1 1 d D . .
H2WA H 0.1337 0.0833 0.3919 0.040 Uiso 1 1 d RD . .
H2WB H 0.1354 0.0226 0.4485 0.040 Uiso 1 1 d RD . .
O3W O 0.0579(2) 0.0856(6) 0.5125(2) 0.0351(13) Uani 1 1 d D . .
H3WA H 0.0374 0.0638 0.5389 0.042 Uiso 1 1 d RD . .
H3WB H 0.0608 0.0088 0.4931 0.042 Uiso 1 1 d RD . .
O1 O 0.0723(2) 0.3032(5) 0.3345(2) 0.0238(11) Uani 1 1 d . . .
O2 O 0.1312(2) 0.3917(5) 0.2750(2) 0.0272(12) Uani 1 1 d . . .
O3 O 0.3175(3) 0.6862(6) 0.3858(2) 0.0381(14) Uani 1 1 d . . .
O4 O 0.3542(2) 0.6273(6) 0.4828(2) 0.0334(13) Uani 1 1 d . . .
O5 O 0.1676(2) 0.5252(5) 0.58599(19) 0.0230(11) Uani 1 1 d . . .
O6 O 0.0953(2) 0.3856(5) 0.52845(19) 0.0208(11) Uani 1 1 d . . .
O7 O 0.2336(2) 0.5353(5) 0.2170(2) 0.0205(11) Uani 1 1 d . . .
O8 O 0.2615(2) 0.7514(5) 0.2549(3) 0.0353(14) Uani 1 1 d . . .
O9 O 0.1011(2) 1.1429(5) 0.1909(2) 0.0262(12) Uani 1 1 d . . .
O10 O 0.0207(2) 1.0847(5) 0.1147(2) 0.0260(12) Uani 1 1 d . . .
O11 O -0.02837(19) 0.5419(5) 0.0867(2) 0.0204(10) Uani 1 1 d . . .
O12 O 0.04640(19) 0.4032(4) 0.13515(19) 0.0159(10) Uani 1 1 d . . .
N1 N 0.1438(2) 0.4108(6) 0.4335(2) 0.0155(12) Uani 1 1 d . . .
N2 N 0.1182(2) 0.6154(5) 0.1783(2) 0.0137(11) Uani 1 1 d . . .
C1 C 0.1633(3) 0.4273(7) 0.3818(3) 0.0175(14) Uani 1 1 d . . .
C2 C 0.2169(3) 0.5003(8) 0.3800(3) 0.0221(15) Uani 1 1 d . . .
H2 H 0.2293 0.5121 0.3433 0.027 Uiso 1 1 calc R . .
C3 C 0.2524(3) 0.5566(7) 0.4355(3) 0.0183(14) Uani 1 1 d . . .
C4 C 0.2307(3) 0.5403(8) 0.4887(3) 0.0216(15) Uani 1 1 d . . .
H4 H 0.2530 0.5764 0.5258 0.026 Uiso 1 1 calc R . .
C5 C 0.1756(3) 0.4696(7) 0.4854(3) 0.0147(13) Uani 1 1 d . . .
C6 C 0.1189(3) 0.3681(7) 0.3255(3) 0.0184(15) Uani 1 1 d . . .
C7 C 0.3134(3) 0.6300(7) 0.4345(3) 0.0224(16) Uani 1 1 d . . .
C8 C 0.1440(3) 0.4577(7) 0.5383(3) 0.0177(14) Uani 1 1 d . . .
C9 C 0.1591(3) 0.7187(6) 0.1995(3) 0.0142(14) Uani 1 1 d . . .
C10 C 0.1436(3) 0.8613(7) 0.1945(3) 0.0172(14) Uani 1 1 d . . .
H10 H 0.1727 0.9310 0.2103 0.021 Uiso 1 1 calc R . .
C11 C 0.0837(3) 0.8990(7) 0.1655(3) 0.0161(14) Uani 1 1 d . . .
C12 C 0.0416(3) 0.7928(7) 0.1425(3) 0.0187(15) Uani 1 1 d . . .
H12 H 0.0012 0.8149 0.1229 0.022 Uiso 1 1 calc R . .
C13 C 0.0614(3) 0.6530(7) 0.1495(3) 0.0146(14) Uani 1 1 d . . .
C14 C 0.2233(3) 0.6648(7) 0.2259(3) 0.0190(15) Uani 1 1 d . . .
C15 C 0.0672(3) 1.0561(7) 0.1569(3) 0.0192(15) Uani 1 1 d . . .
C16 C 0.0227(3) 0.5274(7) 0.1217(3) 0.0145(14) Uani 1 1 d . . .
O4W O 0.1526(4) 0.0292(9) 0.3202(3) 0.078(2) Uani 1 1 d U . .
O5W O 0.0000 0.553(2) 0.2500 0.144(6) Uani 1 2 d SU . .
O6W O 0.0000 0.069(2) 0.2500 0.177(8) Uani 1 2 d SU . .
O7W O -0.0849(14) 0.759(3) 0.1811(14) 0.188(12) Uani 0.50 1 d PU . .


_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 O10 2.390(4) 2_545 ?
Eu1 O1 2.410(5) . ?
Eu1 O6 2.425(4) . ?
Eu1 O2W 2.432(5) . ?
Eu1 O1W 2.445(5) . ?
Eu1 O3W 2.481(5) . ?
Eu1 N1 2.522(5) . ?
Eu1 O11 2.566(5) 2 ?
Eu1 O12 2.568(4) 2 ?
Eu1 C16 2.938(6) 2 ?
Eu1 H3WB 2.8052 . ?
Eu2 O8 2.337(5) 4_545 ?
Eu2 O2 2.344(5) . ?
Eu2 O3 2.351(5) 4_545 ?
Eu2 O9 2.391(5) 1_545 ?
Eu2 O12 2.416(4) . ?
Eu2 O5 2.422(4) 6_565 ?
Eu2 O7 2.422(4) . ?
Eu2 N2 2.526(5) . ?
O1W H1WA 0.8502 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8499 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8498 . ?
O3W H3WB 0.8501 . ?
O1 C6 1.257(8) . ?
O2 C6 1.241(8) . ?
O3 C7 1.233(9) . ?
O3 Eu2 2.351(5) 4 ?
O4 C7 1.245(8) . ?
O5 C8 1.251(7) . ?
O5 Eu2 2.422(4) 6_566 ?
O6 C8 1.252(8) . ?
O7 C14 1.257(8) . ?
O8 C14 1.246(8) . ?
O8 Eu2 2.337(5) 4 ?
O9 C15 1.245(8) . ?
O9 Eu2 2.391(5) 1_565 ?
O10 C15 1.261(7) . ?
O10 Eu1 2.390(4) 2_565 ?
O11 C16 1.235(7) . ?
O11 Eu1 2.566(5) 2 ?
O12 C16 1.283(7) . ?
O12 Eu1 2.568(4) 2 ?
N1 C5 1.335(8) . ?
N1 C1 1.336(8) . ?
N2 C13 1.329(8) . ?
N2 C9 1.338(8) . ?
C1 C2 1.383(9) . ?
C1 C6 1.521(8) . ?
C2 C3 1.415(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.392(9) . ?
C3 C7 1.525(9) . ?
C4 C5 1.380(9) . ?
C4 H4 0.9300 . ?
C5 C8 1.511(9) . ?
C9 C10 1.375(8) . ?
C9 C14 1.504(9) . ?
C10 C11 1.391(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.383(9) . ?
C11 C15 1.516(9) . ?
C12 C13 1.377(9) . ?
C12 H12 0.9300 . ?
C13 C16 1.506(8) . ?
C16 Eu1 2.938(6) 2 ?

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
O10 Eu1 O1 86.49(17) 2_545 . ?
O10 Eu1 O6 145.39(16) 2_545 . ?
O1 Eu1 O6 127.11(15) . . ?
O10 Eu1 O2W 81.82(18) 2_545 . ?
O1 Eu1 O2W 72.87(17) . . ?
O6 Eu1 O2W 99.05(17) . . ?
O10 Eu1 O1W 77.88(17) 2_545 . ?
O1 Eu1 O1W 144.93(16) . . ?
O6 Eu1 O1W 77.02(15) . . ?
O2W Eu1 O1W 133.94(17) . . ?
O10 Eu1 O3W 75.68(17) 2_545 . ?
O1 Eu1 O3W 137.22(17) . . ?
O6 Eu1 O3W 73.21(17) . . ?
O2W Eu1 O3W 66.37(17) . . ?
O1W Eu1 O3W 68.71(17) . . ?
O10 Eu1 N1 146.03(18) 2_545 . ?
O1 Eu1 N1 64.19(16) . . ?
O6 Eu1 N1 63.45(15) . . ?
O2W Eu1 N1 73.68(18) . . ?
O1W Eu1 N1 136.05(16) . . ?
O3W Eu1 N1 113.75(17) . . ?
O10 Eu1 O11 126.32(14) 2_545 2 ?
O1 Eu1 O11 78.10(16) . 2 ?
O6 Eu1 O11 75.12(15) . 2 ?
O2W Eu1 O11 137.95(16) . 2 ?
O1W Eu1 O11 86.18(16) . 2 ?
O3W Eu1 O11 143.09(16) . 2 ?
N1 Eu1 O11 66.47(15) . 2 ?
O10 Eu1 O12 75.78(14) 2_545 2 ?
O1 Eu1 O12 74.63(15) . 2 ?
O6 Eu1 O12 117.26(15) . 2 ?
O2W Eu1 O12 141.31(16) . 2 ?
O1W Eu1 O12 71.19(15) . 2 ?
O3W Eu1 O12 134.52(16) . 2 ?
N1 Eu1 O12 109.76(15) . 2 ?
O11 Eu1 O12 50.60(13) 2 2 ?
O10 Eu1 C16 101.60(16) 2_545 2 ?
O1 Eu1 C16 74.95(17) . 2 ?
O6 Eu1 C16 95.92(16) . 2 ?
O2W Eu1 C16 147.36(17) . 2 ?
O1W Eu1 C16 77.72(17) . 2 ?
O3W Eu1 C16 146.19(18) . 2 ?
N1 Eu1 C16 87.60(17) . 2 ?
O11 Eu1 C16 24.75(15) 2 2 ?
O12 Eu1 C16 25.85(15) 2 2 ?
O10 Eu1 H3WB 63.8 2_545 . ?
O1 Eu1 H3WB 121.3 . . ?
O6 Eu1 H3WB 88.4 . . ?
O2W Eu1 H3WB 54.6 . . ?
O1W Eu1 H3WB 79.3 . . ?
O3W Eu1 H3WB 17.1 . . ?
N1 Eu1 H3WB 116.0 . . ?
O11 Eu1 H3WB 160.2 2 . ?
O12 Eu1 H3WB 133.9 2 . ?
C16 Eu1 H3WB 155.0 2 . ?
O8 Eu2 O2 77.6(2) 4_545 . ?
O8 Eu2 O3 78.94(19) 4_545 4_545 ?
O2 Eu2 O3 143.20(18) . 4_545 ?
O8 Eu2 O9 84.84(17) 4_545 1_545 ?
O2 Eu2 O9 77.79(17) . 1_545 ?
O3 Eu2 O9 72.24(19) 4_545 1_545 ?
O8 Eu2 O12 155.64(18) 4_545 . ?
O2 Eu2 O12 86.87(16) . . ?
O3 Eu2 O12 104.21(17) 4_545 . ?
O9 Eu2 O12 73.53(15) 1_545 . ?
O8 Eu2 O5 120.18(19) 4_545 6_565 ?
O2 Eu2 O5 145.71(17) . 6_565 ?
O3 Eu2 O5 71.07(17) 4_545 6_565 ?
O9 Eu2 O5 129.34(17) 1_545 6_565 ?
O12 Eu2 O5 82.97(15) . 6_565 ?
O8 Eu2 O7 69.83(16) 4_545 . ?
O2 Eu2 O7 83.24(17) . . ?
O3 Eu2 O7 114.29(19) 4_545 . ?
O9 Eu2 O7 151.12(15) 1_545 . ?
O12 Eu2 O7 127.23(14) . . ?
O5 Eu2 O7 77.26(16) 6_565 . ?
O8 Eu2 N2 128.38(17) 4_545 . ?
O2 Eu2 N2 75.31(17) . . ?
O3 Eu2 N2 141.09(17) 4_545 . ?
O9 Eu2 N2 129.62(17) 1_545 . ?
O12 Eu2 N2 63.28(15) . . ?
O5 Eu2 N2 70.86(16) 6_565 . ?
O7 Eu2 N2 64.06(15) . . ?
Eu1 O1W H1WA 123.8 . . ?
Eu1 O1W H1WB 127.7 . . ?
H1WA O1W H1WB 108.4 . . ?
Eu1 O2W H2WA 117.8 . . ?
Eu1 O2W H2WB 129.1 . . ?
H2WA O2W H2WB 108.6 . . ?
Eu1 O3W H3WA 133.4 . . ?
Eu1 O3W H3WB 103.6 . . ?
H3WA O3W H3WB 105.5 . . ?
C6 O1 Eu1 125.5(4) . . ?
C6 O2 Eu2 162.3(5) . . ?
C7 O3 Eu2 157.4(5) . 4 ?
C8 O5 Eu2 148.4(4) . 6_566 ?
C8 O6 Eu1 126.1(4) . . ?
C14 O7 Eu2 124.4(4) . . ?
C14 O8 Eu2 164.9(5) . 4 ?
C15 O9 Eu2 136.9(5) . 1_565 ?
C15 O10 Eu1 144.0(4) . 2_565 ?
C16 O11 Eu1 94.8(4) . 2 ?
C16 O12 Eu2 124.5(4) . . ?
C16 O12 Eu1 93.4(3) . 2 ?
Eu2 O12 Eu1 138.52(18) . 2 ?
C5 N1 C1 119.7(6) . . ?
C5 N1 Eu1 120.4(4) . . ?
C1 N1 Eu1 119.9(4) . . ?
C13 N2 C9 118.4(5) . . ?
C13 N2 Eu2 121.4(4) . . ?
C9 N2 Eu2 119.6(4) . . ?
N1 C1 C2 122.3(6) . . ?
N1 C1 C6 113.6(6) . . ?
C2 C1 C6 124.0(6) . . ?
C1 C2 C3 118.1(6) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 118.6(6) . . ?
C4 C3 C7 122.9(6) . . ?
C2 C3 C7 118.4(6) . . ?
C5 C4 C3 118.9(6) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N1 C5 C4 122.2(6) . . ?
N1 C5 C8 113.8(6) . . ?
C4 C5 C8 124.0(6) . . ?
O2 C6 O1 126.3(6) . . ?
O2 C6 C1 117.1(6) . . ?
O1 C6 C1 116.6(6) . . ?
O3 C7 O4 126.4(7) . . ?
O3 C7 C3 116.7(6) . . ?
O4 C7 C3 117.0(6) . . ?
O5 C8 O6 126.9(6) . . ?
O5 C8 C5 117.0(6) . . ?
O6 C8 C5 116.0(5) . . ?
N2 C9 C10 122.3(6) . . ?
N2 C9 C14 113.9(5) . . ?
C10 C9 C14 123.7(6) . . ?
C9 C10 C11 118.6(6) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C12 C11 C10 119.3(6) . . ?
C12 C11 C15 121.6(6) . . ?
C10 C11 C15 119.0(6) . . ?
C13 C12 C11 117.8(6) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
N2 C13 C12 123.5(6) . . ?
N2 C13 C16 112.7(5) . . ?
C12 C13 C16 123.6(5) . . ?
O8 C14 O7 125.5(6) . . ?
O8 C14 C9 117.6(6) . . ?
O7 C14 C9 116.9(6) . . ?
O9 C15 O10 127.0(6) . . ?
O9 C15 C11 117.3(6) . . ?
O10 C15 C11 115.8(6) . . ?
O11 C16 O12 121.2(6) . . ?
O11 C16 C13 122.4(6) . . ?
O12 C16 C13 116.3(5) . . ?
O11 C16 Eu1 60.5(3) . 2 ?
O12 C16 Eu1 60.7(3) . 2 ?
C13 C16 Eu1 176.6(4) . 2 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O10 Eu1 O1 C6 -162.2(5) 2_545 . . . ?
O6 Eu1 O1 C6 8.8(6) . . . . ?
O2W Eu1 O1 C6 -79.7(5) . . . . ?
O1W Eu1 O1 C6 134.8(5) . . . . ?
O3W Eu1 O1 C6 -97.7(6) . . . . ?
N1 Eu1 O1 C6 0.1(5) . . . . ?
O11 Eu1 O1 C6 69.5(5) 2 . . . ?
O12 Eu1 O1 C6 121.6(5) 2 . . . ?
C16 Eu1 O1 C6 94.8(5) 2 . . . ?
O8 Eu2 O2 C6 -61.9(15) 4_545 . . . ?
O3 Eu2 O2 C6 -10.4(17) 4_545 . . . ?
O9 Eu2 O2 C6 25.5(15) 1_545 . . . ?
O12 Eu2 O2 C6 99.3(15) . . . . ?
O5 Eu2 O2 C6 172.0(14) 6_565 . . . ?
O7 Eu2 O2 C6 -132.6(15) . . . . ?
N2 Eu2 O2 C6 162.5(16) . . . . ?
O10 Eu1 O6 C8 154.9(5) 2_545 . . . ?
O1 Eu1 O6 C8 -9.1(6) . . . . ?
O2W Eu1 O6 C8 66.2(5) . . . . ?
O1W Eu1 O6 C8 -160.6(5) . . . . ?
O3W Eu1 O6 C8 128.1(5) . . . . ?
N1 Eu1 O6 C8 -0.3(5) . . . . ?
O11 Eu1 O6 C8 -71.1(5) 2 . . . ?
O12 Eu1 O6 C8 -100.0(5) 2 . . . ?
C16 Eu1 O6 C8 -84.6(5) 2 . . . ?
O8 Eu2 O7 C14 -148.4(6) 4_545 . . . ?
O2 Eu2 O7 C14 -69.2(5) . . . . ?
O3 Eu2 O7 C14 144.6(5) 4_545 . . . ?
O9 Eu2 O7 C14 -118.2(5) 1_545 . . . ?
O12 Eu2 O7 C14 11.6(6) . . . . ?
O5 Eu2 O7 C14 82.4(5) 6_565 . . . ?
N2 Eu2 O7 C14 7.7(5) . . . . ?
O8 Eu2 O12 C16 137.4(5) 4_545 . . . ?
O2 Eu2 O12 C16 87.5(5) . . . . ?
O3 Eu2 O12 C16 -128.1(5) 4_545 . . . ?
O9 Eu2 O12 C16 165.7(5) 1_545 . . . ?
O5 Eu2 O12 C16 -59.7(5) 6_565 . . . ?
O7 Eu2 O12 C16 8.4(5) . . . . ?
N2 Eu2 O12 C16 12.4(4) . . . . ?
O8 Eu2 O12 Eu1 -70.0(5) 4_545 . . 2 ?
O2 Eu2 O12 Eu1 -119.9(3) . . . 2 ?
O3 Eu2 O12 Eu1 24.5(3) 4_545 . . 2 ?
O9 Eu2 O12 Eu1 -41.7(3) 1_545 . . 2 ?
O5 Eu2 O12 Eu1 92.9(3) 6_565 . . 2 ?
O7 Eu2 O12 Eu1 161.0(2) . . . 2 ?
N2 Eu2 O12 Eu1 165.0(4) . . . 2 ?
O10 Eu1 N1 C5 -151.2(4) 2_545 . . . ?
O1 Eu1 N1 C5 175.8(5) . . . . ?
O6 Eu1 N1 C5 3.6(4) . . . . ?
O2W Eu1 N1 C5 -105.7(5) . . . . ?
O1W Eu1 N1 C5 31.9(5) . . . . ?
O3W Eu1 N1 C5 -51.5(5) . . . . ?
O11 Eu1 N1 C5 88.1(5) 2 . . . ?
O12 Eu1 N1 C5 115.0(4) 2 . . . ?
C16 Eu1 N1 C5 101.4(5) 2 . . . ?
O10 Eu1 N1 C1 30.0(6) 2_545 . . . ?
O1 Eu1 N1 C1 -2.9(4) . . . . ?
O6 Eu1 N1 C1 -175.2(5) . . . . ?
O2W Eu1 N1 C1 75.6(5) . . . . ?
O1W Eu1 N1 C1 -146.8(4) . . . . ?
O3W Eu1 N1 C1 129.8(5) . . . . ?
O11 Eu1 N1 C1 -90.7(5) 2 . . . ?
O12 Eu1 N1 C1 -63.8(5) 2 . . . ?
C16 Eu1 N1 C1 -77.3(5) 2 . . . ?
O8 Eu2 N2 C13 -161.7(4) 4_545 . . . ?
O2 Eu2 N2 C13 -101.2(5) . . . . ?
O3 Eu2 N2 C13 72.1(6) 4_545 . . . ?
O9 Eu2 N2 C13 -41.2(5) 1_545 . . . ?
O12 Eu2 N2 C13 -7.2(5) . . . . ?
O5 Eu2 N2 C13 84.5(5) 6_565 . . . ?
O7 Eu2 N2 C13 169.3(5) . . . . ?
O8 Eu2 N2 C9 28.0(5) 4_545 . . . ?
O2 Eu2 N2 C9 88.5(5) . . . . ?
O3 Eu2 N2 C9 -98.3(5) 4_545 . . . ?
O9 Eu2 N2 C9 148.5(4) 1_545 . . . ?
O12 Eu2 N2 C9 -177.5(5) . . . . ?
O5 Eu2 N2 C9 -85.8(5) 6_565 . . . ?
O7 Eu2 N2 C9 -1.0(4) . . . . ?
C5 N1 C1 C2 2.0(10) . . . . ?
Eu1 N1 C1 C2 -179.2(5) . . . . ?
C5 N1 C1 C6 -173.9(5) . . . . ?
Eu1 N1 C1 C6 4.9(7) . . . . ?
N1 C1 C2 C3 1.2(10) . . . . ?
C6 C1 C2 C3 176.6(6) . . . . ?
C1 C2 C3 C4 -2.2(10) . . . . ?
C1 C2 C3 C7 176.6(6) . . . . ?
C2 C3 C4 C5 0.2(10) . . . . ?
C7 C3 C4 C5 -178.6(6) . . . . ?
C1 N1 C5 C4 -4.2(9) . . . . ?
Eu1 N1 C5 C4 177.0(5) . . . . ?
C1 N1 C5 C8 172.8(6) . . . . ?
Eu1 N1 C5 C8 -5.9(7) . . . . ?
C3 C4 C5 N1 3.0(10) . . . . ?
C3 C4 C5 C8 -173.7(6) . . . . ?
Eu2 O2 C6 O1 -61.4(18) . . . . ?
Eu2 O2 C6 C1 120.7(14) . . . . ?
Eu1 O1 C6 O2 -175.5(5) . . . . ?
Eu1 O1 C6 C1 2.3(8) . . . . ?
N1 C1 C6 O2 173.3(6) . . . . ?
C2 C1 C6 O2 -2.5(10) . . . . ?
N1 C1 C6 O1 -4.7(9) . . . . ?
C2 C1 C6 O1 179.5(6) . . . . ?
Eu2 O3 C7 O4 -39.2(19) 4 . . . ?
Eu2 O3 C7 C3 140.8(12) 4 . . . ?
C4 C3 C7 O3 -153.2(7) . . . . ?
C2 C3 C7 O3 27.9(10) . . . . ?
C4 C3 C7 O4 26.8(10) . . . . ?
C2 C3 C7 O4 -152.1(7) . . . . ?
Eu2 O5 C8 O6 -21.9(13) 6_566 . . . ?
Eu2 O5 C8 C5 154.8(6) 6_566 . . . ?
Eu1 O6 C8 O5 174.3(5) . . . . ?
Eu1 O6 C8 C5 -2.5(8) . . . . ?
N1 C5 C8 O5 -171.7(6) . . . . ?
C4 C5 C8 O5 5.3(10) . . . . ?
N1 C5 C8 O6 5.4(8) . . . . ?
C4 C5 C8 O6 -177.6(6) . . . . ?
C13 N2 C9 C10 2.5(9) . . . . ?
Eu2 N2 C9 C10 173.1(5) . . . . ?
C13 N2 C9 C14 -174.6(6) . . . . ?
Eu2 N2 C9 C14 -4.0(7) . . . . ?
N2 C9 C10 C11 -1.1(10) . . . . ?
C14 C9 C10 C11 175.7(6) . . . . ?
C9 C10 C11 C12 -0.1(10) . . . . ?
C9 C10 C11 C15 -176.9(6) . . . . ?
C10 C11 C12 C13 -0.1(10) . . . . ?
C15 C11 C12 C13 176.6(6) . . . . ?
C9 N2 C13 C12 -2.7(10) . . . . ?
Eu2 N2 C13 C12 -173.1(5) . . . . ?
C9 N2 C13 C16 173.3(5) . . . . ?
Eu2 N2 C13 C16 2.8(7) . . . . ?
C11 C12 C13 N2 1.5(10) . . . . ?
C11 C12 C13 C16 -174.0(6) . . . . ?
Eu2 O8 C14 O7 -24(3) 4 . . . ?
Eu2 O8 C14 C9 156.3(18) 4 . . . ?
Eu2 O7 C14 O8 167.0(6) . . . . ?
Eu2 O7 C14 C9 -12.7(8) . . . . ?
N2 C9 C14 O8 -169.3(6) . . . . ?
C10 C9 C14 O8 13.7(10) . . . . ?
N2 C9 C14 O7 10.5(9) . . . . ?
C10 C9 C14 O7 -166.6(6) . . . . ?
Eu2 O9 C15 O10 -48.9(11) 1_565 . . . ?
Eu2 O9 C15 C11 129.6(6) 1_565 . . . ?
Eu1 O10 C15 O9 -6.6(14) 2_565 . . . ?
Eu1 O10 C15 C11 174.8(5) 2_565 . . . ?
C12 C11 C15 O9 162.6(7) . . . . ?
C10 C11 C15 O9 -20.7(10) . . . . ?
C12 C11 C15 O10 -18.7(10) . . . . ?
C10 C11 C15 O10 158.0(6) . . . . ?
Eu1 O11 C16 O12 -0.1(7) 2 . . . ?
Eu1 O11 C16 C13 178.0(5) 2 . . . ?
Eu2 O12 C16 O11 162.3(5) . . . . ?
Eu1 O12 C16 O11 0.1(6) 2 . . . ?
Eu2 O12 C16 C13 -15.9(7) . . . . ?
Eu1 O12 C16 C13 -178.1(5) 2 . . . ?
Eu2 O12 C16 Eu1 162.2(4) . . . 2 ?
N2 C13 C16 O11 -170.5(6) . . . . ?
C12 C13 C16 O11 5.5(10) . . . . ?
N2 C13 C16 O12 7.7(8) . . . . ?
C12 C13 C16 O12 -176.4(6) . . . . ?
N2 C13 C16 Eu1 -22(8) . . . 2 ?
C12 C13 C16 Eu1 154(7) . . . 2 ?

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
O1W H1WA O11 0.85 1.89 2.726(6) 167.0 6_566
O1W H1WB O4 0.85 2.02 2.815(7) 154.3 3_445
O2W H2WA O4W 0.85 1.82 2.667(9) 172.1 .
O2W H2WB O4 0.85 2.06 2.880(7) 163.1 7_556

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.454
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.188

data_GDM
_database_code_depnum_ccdc_archive 'CCDC 687912'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H15 Gd2 N2 O17.50'
_chemical_formula_weight         829.80

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'
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   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                   22.2267(16)
_cell_length_b                   9.3424(7)
_cell_length_c                   22.3427(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.1380(10)
_cell_angle_gamma                90.00
_cell_volume                     4518.0(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13472
_cell_measurement_theta_min      1.87
_cell_measurement_theta_max      26.00

_exptl_crystal_description       cuboid
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3144
_exptl_absorpt_coefficient_mu    5.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6272
_exptl_absorpt_correction_T_max  0.7330
_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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13472
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4436
_reflns_number_gt                3870
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'

_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)+(0.0359P)²+24.5562P] where P=(Fo²+2Fc²)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4436
_refine_ls_number_parameters     344
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.110
_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
Gd1 Gd 0.045996(16) 0.27324(4) 0.432302(16) 0.01223(10) Uani 1 1 d . . .
Gd2 Gd 0.154251(15) 0.35990(3) 0.179096(15) 0.00964(10) Uani 1 1 d . . .
O1W O -0.0364(2) 0.2858(6) 0.4874(2) 0.0257(13) Uani 1 1 d D . .
H1WA H -0.0332 0.3279 0.5217 0.031 Uiso 1 1 d RD . .
H1WB H -0.0730 0.2539 0.4758 0.031 Uiso 1 1 d RD . .
O2W O 0.1243(3) 0.0965(6) 0.4265(3) 0.0335(14) Uani 1 1 d D . .
H2WA H 0.1366 0.0666 0.3953 0.040 Uiso 1 1 d RD . .
H2WB H 0.1308 0.0370 0.4560 0.040 Uiso 1 1 d RD . .
O3W O 0.0579(3) 0.0858(6) 0.5122(3) 0.0355(15) Uani 1 1 d D . .
H3WA H 0.0377 0.0670 0.5394 0.043 Uiso 1 1 d RD . .
H3WB H 0.0613 0.0090 0.4929 0.043 Uiso 1 1 d RD . .
O1 O 0.0723(2) 0.3029(6) 0.3341(2) 0.0218(12) Uani 1 1 d . . .
O2 O 0.1303(2) 0.3913(6) 0.2744(2) 0.0228(12) Uani 1 1 d . . .
O3 O 0.3168(3) 0.6884(6) 0.3852(3) 0.0389(16) Uani 1 1 d . . .
O4 O 0.3548(3) 0.6268(6) 0.4826(3) 0.0327(14) Uani 1 1 d . . .
O5 O 0.1673(2) 0.5259(6) 0.5863(2) 0.0224(12) Uani 1 1 d . . .
O6 O 0.0952(2) 0.3857(5) 0.5287(2) 0.0199(12) Uani 1 1 d . . .
O7 O 0.2333(2) 0.5349(5) 0.2171(2) 0.0201(12) Uani 1 1 d . . .
O8 O 0.2622(3) 0.7504(5) 0.2545(3) 0.0326(15) Uani 1 1 d . . .
O9 O 0.1010(3) 1.1440(5) 0.1901(3) 0.0274(13) Uani 1 1 d . . .
O10 O 0.0199(2) 1.0853(5) 0.1147(2) 0.0235(12) Uani 1 1 d . . .
O11 O -0.0285(2) 0.5402(5) 0.0860(2) 0.0208(12) Uani 1 1 d . . .
O12 O 0.0465(2) 0.4023(5) 0.1347(2) 0.0147(11) Uani 1 1 d . . .
N1 N 0.1438(3) 0.4103(6) 0.4337(2) 0.0139(13) Uani 1 1 d . . .
N2 N 0.1185(3) 0.6156(6) 0.1780(3) 0.0124(12) Uani 1 1 d . . .
C1 C 0.1630(3) 0.4263(8) 0.3817(3) 0.0158(15) Uani 1 1 d . . .
C2 C 0.2168(3) 0.4984(8) 0.3800(3) 0.0209(17) Uani 1 1 d . . .
H2 H 0.2297 0.5080 0.3434 0.025 Uiso 1 1 calc R . .
C3 C 0.2518(3) 0.5574(8) 0.4356(3) 0.0175(16) Uani 1 1 d . . .
C4 C 0.2304(3) 0.5396(8) 0.4877(3) 0.0192(16) Uani 1 1 d . . .
H4 H 0.2529 0.5760 0.5248 0.023 Uiso 1 1 calc R . .
C5 C 0.1760(3) 0.4687(7) 0.4859(3) 0.0134(15) Uani 1 1 d . . .
C6 C 0.1186(3) 0.3675(7) 0.3251(3) 0.0153(15) Uani 1 1 d . . .
C7 C 0.3130(4) 0.6305(7) 0.4346(4) 0.0192(16) Uani 1 1 d . . .
C8 C 0.1437(3) 0.4585(7) 0.5387(3) 0.0158(15) Uani 1 1 d . . .
C9 C 0.1589(3) 0.7186(7) 0.1997(3) 0.0119(14) Uani 1 1 d . . .
C10 C 0.1437(3) 0.8630(7) 0.1942(3) 0.0160(15) Uani 1 1 d . . .
H10 H 0.1727 0.9335 0.2092 0.019 Uiso 1 1 calc R . .
C11 C 0.0838(3) 0.8975(7) 0.1656(3) 0.0147(15) Uani 1 1 d . . .
C12 C 0.0413(3) 0.7932(7) 0.1428(3) 0.0181(16) Uani 1 1 d . . .
H12 H 0.0007 0.8163 0.1239 0.022 Uiso 1 1 calc R . .
C13 C 0.0612(3) 0.6517(7) 0.1490(3) 0.0132(15) Uani 1 1 d . . .
C14 C 0.2240(3) 0.6639(7) 0.2261(3) 0.0172(16) Uani 1 1 d . . .
C15 C 0.0669(3) 1.0556(7) 0.1562(3) 0.0161(15) Uani 1 1 d . . .
C16 C 0.0232(3) 0.5258(7) 0.1217(3) 0.0125(14) Uani 1 1 d . . .
O4W O 0.1524(4) 0.0275(9) 0.3199(4) 0.073(2) Uani 1 1 d U . .
O5W O 0.0000 0.555(2) 0.2500 0.132(6) Uani 1 2 d SU . .
O6W O 0.0000 0.067(2) 0.2500 0.144(7) Uani 1 2 d SU . .
O7W O -0.0869(15) 0.759(3) 0.1813(15) 0.175(12) Uani 0.50 1 d PU . .


_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 O10 2.373(5) 2_545 ?
Gd1 O1 2.411(5) . ?
Gd1 O6 2.423(5) . ?
Gd1 O2W 2.425(5) . ?
Gd1 O1W 2.431(5) . ?
Gd1 O3W 2.472(6) . ?
Gd1 N1 2.518(6) . ?
Gd1 O11 2.543(5) 2 ?
Gd1 O12 2.554(4) 2 ?
Gd1 C16 2.923(7) 2 ?
Gd2 O2 2.327(5) . ?
Gd2 O8 2.333(5) 4_545 ?
Gd2 O3 2.338(6) 4_545 ?
Gd2 O9 2.380(5) 1_545 ?
Gd2 O5 2.406(5) 6_565 ?
Gd2 O12 2.407(5) . ?
Gd2 O7 2.409(5) . ?
Gd2 N2 2.516(5) . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8501 . ?
O2W H2WA 0.8502 . ?
O2W H2WB 0.8499 . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8500 . ?
O1 C6 1.248(8) . ?
O2 C6 1.240(8) . ?
O3 C7 1.250(9) . ?
O3 Gd2 2.338(6) 4 ?
O4 C7 1.250(9) . ?
O5 C8 1.246(8) . ?
O5 Gd2 2.406(5) 6_566 ?
O6 C8 1.250(8) . ?
O7 C14 1.246(8) . ?
O8 C14 1.238(9) . ?
O8 Gd2 2.333(5) 4 ?
O9 C15 1.253(8) . ?
O9 Gd2 2.380(5) 1_565 ?
O10 C15 1.260(8) . ?
O10 Gd1 2.373(5) 2_565 ?
O11 C16 1.248(8) . ?
O11 Gd1 2.543(5) 2 ?
O12 C16 1.271(8) . ?
O12 Gd1 2.554(4) 2 ?
N1 C1 1.335(9) . ?
N1 C5 1.337(8) . ?
N2 C9 1.331(9) . ?
N2 C13 1.334(9) . ?
C1 C2 1.380(10) . ?
C1 C6 1.518(10) . ?
C2 C3 1.420(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.362(10) . ?
C3 C7 1.526(10) . ?
C4 C5 1.372(9) . ?
C4 H4 0.9300 . ?
C5 C8 1.517(10) . ?
C9 C10 1.390(9) . ?
C9 C14 1.520(10) . ?
C10 C11 1.377(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.372(10) . ?
C11 C15 1.527(9) . ?
C12 C13 1.390(9) . ?
C12 H12 0.9300 . ?
C13 C16 1.496(9) . ?
C16 Gd1 2.923(7) 2 ?

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
O10 Gd1 O1 86.28(18) 2_545 . ?
O10 Gd1 O6 145.38(17) 2_545 . ?
O1 Gd1 O6 127.24(17) . . ?
O10 Gd1 O2W 81.40(19) 2_545 . ?
O1 Gd1 O2W 72.78(19) . . ?
O6 Gd1 O2W 99.11(19) . . ?
O10 Gd1 O1W 78.47(18) 2_545 . ?
O1 Gd1 O1W 145.26(18) . . ?
O6 Gd1 O1W 76.61(17) . . ?
O2W Gd1 O1W 133.87(19) . . ?
O10 Gd1 O3W 75.51(19) 2_545 . ?
O1 Gd1 O3W 136.94(19) . . ?
O6 Gd1 O3W 73.26(18) . . ?
O2W Gd1 O3W 66.2(2) . . ?
O1W Gd1 O3W 68.74(19) . . ?
O10 Gd1 N1 145.70(19) 2_545 . ?
O1 Gd1 N1 64.25(17) . . ?
O6 Gd1 N1 63.52(17) . . ?
O2W Gd1 N1 73.64(19) . . ?
O1W Gd1 N1 135.81(18) . . ?
O3W Gd1 N1 113.63(19) . . ?
O10 Gd1 O11 126.73(16) 2_545 2 ?
O1 Gd1 O11 78.48(17) . 2 ?
O6 Gd1 O11 74.91(17) . 2 ?
O2W Gd1 O11 138.12(18) . 2 ?
O1W Gd1 O11 85.93(17) . 2 ?
O3W Gd1 O11 142.97(18) . 2 ?
N1 Gd1 O11 66.61(17) . 2 ?
O10 Gd1 O12 75.90(16) 2_545 2 ?
O1 Gd1 O12 75.05(17) . 2 ?
O6 Gd1 O12 117.20(16) . 2 ?
O2W Gd1 O12 141.48(18) . 2 ?
O1W Gd1 O12 71.04(17) . 2 ?
O3W Gd1 O12 134.23(18) . 2 ?
N1 Gd1 O12 110.20(16) . 2 ?
O11 Gd1 O12 50.90(15) 2 2 ?
O10 Gd1 C16 101.58(18) 2_545 2 ?
O1 Gd1 C16 75.24(18) . 2 ?
O6 Gd1 C16 96.08(18) . 2 ?
O2W Gd1 C16 147.62(19) . 2 ?
O1W Gd1 C16 77.51(18) . 2 ?
O3W Gd1 C16 146.07(19) . 2 ?
N1 Gd1 C16 88.08(18) . 2 ?
O11 Gd1 C16 25.18(16) 2 2 ?
O12 Gd1 C16 25.72(16) 2 2 ?
O2 Gd2 O8 77.8(2) . 4_545 ?
O2 Gd2 O3 143.2(2) . 4_545 ?
O8 Gd2 O3 78.4(2) 4_545 4_545 ?
O2 Gd2 O9 77.85(19) . 1_545 ?
O8 Gd2 O9 84.54(18) 4_545 1_545 ?
O3 Gd2 O9 72.3(2) 4_545 1_545 ?
O2 Gd2 O5 146.02(18) . 6_565 ?
O8 Gd2 O5 120.5(2) 4_545 6_565 ?
O3 Gd2 O5 70.79(19) 4_545 6_565 ?
O9 Gd2 O5 128.70(19) 1_545 6_565 ?
O2 Gd2 O12 86.75(18) . . ?
O8 Gd2 O12 155.17(19) 4_545 . ?
O3 Gd2 O12 104.3(2) 4_545 . ?
O9 Gd2 O12 73.19(17) 1_545 . ?
O5 Gd2 O12 82.84(17) 6_565 . ?
O2 Gd2 O7 83.79(18) . . ?
O8 Gd2 O7 70.27(17) 4_545 . ?
O3 Gd2 O7 113.7(2) 4_545 . ?
O9 Gd2 O7 151.49(18) 1_545 . ?
O5 Gd2 O7 77.40(18) 6_565 . ?
O12 Gd2 O7 127.65(15) . . ?
O2 Gd2 N2 75.63(18) . . ?
O8 Gd2 N2 128.82(19) 4_545 . ?
O3 Gd2 N2 140.82(19) 4_545 . ?
O9 Gd2 N2 129.97(19) 1_545 . ?
O5 Gd2 N2 70.74(17) 6_565 . ?
O12 Gd2 N2 63.71(17) . . ?
O7 Gd2 N2 64.05(17) . . ?
Gd1 O1W H1WA 124.2 . . ?
Gd1 O1W H1WB 127.5 . . ?
H1WA O1W H1WB 108.3 . . ?
Gd1 O2W H2WA 129.5 . . ?
Gd1 O2W H2WB 113.6 . . ?
H2WA O2W H2WB 113.1 . . ?
Gd1 O3W H3WA 132.4 . . ?
Gd1 O3W H3WB 103.7 . . ?
H3WA O3W H3WB 108.1 . . ?
C6 O1 Gd1 125.6(5) . . ?
C6 O2 Gd2 162.4(5) . . ?
C7 O3 Gd2 157.4(5) . 4 ?
C8 O5 Gd2 148.3(5) . 6_566 ?
C8 O6 Gd1 126.2(5) . . ?
C14 O7 Gd2 125.4(5) . . ?
C14 O8 Gd2 165.1(5) . 4 ?
C15 O9 Gd2 138.0(5) . 1_565 ?
C15 O10 Gd1 144.4(5) . 2_565 ?
C16 O11 Gd1 94.7(4) . 2 ?
C16 O12 Gd2 124.0(4) . . ?
C16 O12 Gd1 93.6(4) . 2 ?
Gd2 O12 Gd1 139.17(19) . 2 ?
C1 N1 C5 120.0(6) . . ?
C1 N1 Gd1 119.5(4) . . ?
C5 N1 Gd1 120.5(4) . . ?
C9 N2 C13 119.0(6) . . ?
C9 N2 Gd2 119.8(4) . . ?
C13 N2 Gd2 120.6(4) . . ?
N1 C1 C2 121.9(6) . . ?
N1 C1 C6 114.1(6) . . ?
C2 C1 C6 123.9(7) . . ?
C1 C2 C3 118.2(7) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 118.1(7) . . ?
C4 C3 C7 123.5(7) . . ?
C2 C3 C7 118.3(6) . . ?
C3 C4 C5 120.7(7) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
N1 C5 C4 121.0(6) . . ?
N1 C5 C8 113.5(6) . . ?
C4 C5 C8 125.4(6) . . ?
O2 C6 O1 125.9(7) . . ?
O2 C6 C1 117.7(6) . . ?
O1 C6 C1 116.4(6) . . ?
O3 C7 O4 125.8(7) . . ?
O3 C7 C3 116.5(7) . . ?
O4 C7 C3 117.7(7) . . ?
O5 C8 O6 127.3(7) . . ?
O5 C8 C5 116.8(6) . . ?
O6 C8 C5 115.9(6) . . ?
N2 C9 C10 122.5(6) . . ?
N2 C9 C14 113.7(6) . . ?
C10 C9 C14 123.5(6) . . ?
C11 C10 C9 117.4(6) . . ?
C11 C10 H10 121.3 . . ?
C9 C10 H10 121.3 . . ?
C12 C11 C10 121.1(6) . . ?
C12 C11 C15 120.6(6) . . ?
C10 C11 C15 118.2(6) . . ?
C11 C12 C13 117.5(6) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 H12 121.2 . . ?
N2 C13 C12 122.4(6) . . ?
N2 C13 C16 112.8(6) . . ?
C12 C13 C16 124.8(6) . . ?
O8 C14 O7 126.4(7) . . ?
O8 C14 C9 117.4(6) . . ?
O7 C14 C9 116.1(6) . . ?
O9 C15 O10 125.9(7) . . ?
O9 C15 C11 117.3(6) . . ?
O10 C15 C11 116.8(6) . . ?
O11 C16 O12 120.8(6) . . ?
O11 C16 C13 121.9(6) . . ?
O12 C16 C13 117.2(6) . . ?
O11 C16 Gd1 60.1(4) . 2 ?
O12 C16 Gd1 60.7(3) . 2 ?
C13 C16 Gd1 177.4(5) . 2 ?

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
O1W H1WA O11 0.85 1.88 2.711(7) 166.4 6_566
O1W H1WB O4 0.85 2.03 2.820(7) 154.3 3_445
O2W H2WA O4W 0.85 1.83 2.673(10) 168.9 .
O2W H2WB O4 0.85 2.03 2.874(8) 171.9 7_556

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.392
_refine_diff_density_min         -1.572
_refine_diff_density_rms         0.202

data_tbm
_database_code_depnum_ccdc_archive 'CCDC 687913'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H13 N2 O16.50 Tb2'
_chemical_formula_weight         815.12

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'
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                   21.757(3)
_cell_length_b                   9.1657(13)
_cell_length_c                   22.457(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.886(3)
_cell_angle_gamma                90.00
_cell_volume                     4397.6(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    8050
_cell_measurement_theta_min      1.91
_cell_measurement_theta_max      26.00

_exptl_crystal_description       cuboid
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3080
_exptl_absorpt_coefficient_mu    6.470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3666
_exptl_absorpt_correction_T_max  0.5390
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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 Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8050
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4165
_reflns_number_gt                3775
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'

_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)+(0.0245P)²+59.6405P] where P=(Fo²+2Fc²)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4165
_refine_ls_number_parameters     333
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0846
_refine_ls_wR_factor_gt          0.0819
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.046
_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 0.045254(13) 0.31163(3) 0.422380(14) 0.00656(10) Uani 1 1 d . . .
Tb2 Tb 0.156559(13) 0.39137(3) 0.175579(13) 0.00581(10) Uani 1 1 d . . .
O1W O -0.0223(2) 0.2461(6) 0.4874(2) 0.0160(11) Uani 1 1 d D . .
H1WA H -0.0222 0.2919 0.5203 0.019 Uiso 1 1 d RD . .
H1WB H -0.0597 0.2200 0.4735 0.019 Uiso 1 1 d RD . .
O2W O 0.1163(2) 0.1188(5) 0.4383(2) 0.0153(11) Uani 1 1 d D . .
H2WA H 0.1330 0.0902 0.4091 0.018 Uiso 1 1 d RD . .
H2WB H 0.1168 0.0496 0.4636 0.018 Uiso 1 1 d RD . .
O1 O 0.0757(2) 0.3507(6) 0.3285(2) 0.0134(10) Uani 1 1 d . . .
O2 O 0.1410(2) 0.4407(5) 0.2717(2) 0.0133(10) Uani 1 1 d . . .
O3 O 0.3332(2) 0.7069(6) 0.3928(2) 0.0168(11) Uani 1 1 d . . .
O4 O 0.3690(2) 0.6067(6) 0.4824(2) 0.0180(11) Uani 1 1 d . . .
O5 O 0.1734(2) 0.4975(5) 0.5855(2) 0.0125(10) Uani 1 1 d . . .
O6 O 0.0947(2) 0.3899(5) 0.5218(2) 0.0102(10) Uani 1 1 d . . .
O7 O 0.23724(19) 0.5727(5) 0.2118(2) 0.0099(10) Uani 1 1 d . . .
O8 O 0.2586(2) 0.7734(5) 0.2678(2) 0.0162(11) Uani 1 1 d . . .
O9 O 0.0997(2) 1.1879(5) 0.1998(2) 0.0110(10) Uani 1 1 d . . .
O10 O 0.0153(2) 1.1290(5) 0.1298(2) 0.0129(10) Uani 1 1 d . . .
O11 O -0.0276(2) 0.5812(5) 0.0868(2) 0.0095(10) Uani 1 1 d U . .
O12 O 0.0496(2) 0.4377(5) 0.1289(2) 0.0090(9) Uani 1 1 d . . .
N1 N 0.1480(2) 0.4327(6) 0.4290(2) 0.0078(11) Uani 1 1 d . . .
N2 N 0.1210(2) 0.6522(6) 0.1751(2) 0.0057(11) Uani 1 1 d . . .
C1 C 0.1699(3) 0.4557(8) 0.3779(3) 0.0124(14) Uani 1 1 d . . .
C2 C 0.2272(3) 0.5214(7) 0.3788(3) 0.0104(14) Uani 1 1 d . . .
H2 H 0.2418 0.5391 0.3422 0.012 Uiso 1 1 calc R . .
C3 C 0.2636(3) 0.5616(8) 0.4352(3) 0.0120(14) Uani 1 1 d . . .
C4 C 0.2402(3) 0.5369(7) 0.4877(3) 0.0103(14) Uani 1 1 d . . .
H4 H 0.2637 0.5630 0.5263 0.012 Uiso 1 1 calc R . .
C5 C 0.1812(3) 0.4729(7) 0.4823(3) 0.0087(13) Uani 1 1 d . . .
C6 C 0.1255(3) 0.4125(7) 0.3216(3) 0.0090(13) Uani 1 1 d U . .
C7 C 0.3271(3) 0.6312(7) 0.4374(3) 0.0112(14) Uani 1 1 d . . .
C8 C 0.1475(3) 0.4514(7) 0.5342(3) 0.0067(13) Uani 1 1 d . . .
C9 C 0.1597(3) 0.7544(7) 0.2014(3) 0.0101(14) Uani 1 1 d U . .
C10 C 0.1434(3) 0.8999(7) 0.2006(3) 0.0100(14) Uani 1 1 d . . .
H10 H 0.1722 0.9707 0.2202 0.012 Uiso 1 1 calc R . .
C11 C 0.0840(3) 0.9412(7) 0.1706(3) 0.0090(13) Uani 1 1 d . . .
C12 C 0.0440(3) 0.8339(8) 0.1421(3) 0.0112(14) Uani 1 1 d . . .
H12 H 0.0036 0.8583 0.1201 0.013 Uiso 1 1 calc R . .
C13 C 0.0640(3) 0.6923(7) 0.1463(3) 0.0085(13) Uani 1 1 d . . .
C14 C 0.2238(3) 0.6958(7) 0.2292(3) 0.0080(13) Uani 1 1 d . . .
C15 C 0.0651(3) 1.0992(7) 0.1669(3) 0.0086(13) Uani 1 1 d . . .
C16 C 0.0260(3) 0.5648(7) 0.1183(3) 0.0060(13) Uani 1 1 d . . .
O3W O -0.0975(4) 0.7458(11) 0.1704(4) 0.071(2) Uani 1 1 d U . .
O4W O 0.1466(5) 0.0603(13) 0.3282(5) 0.0258(18) Uani 0.50 1 d PU . .
O4W' O 0.1697(5) -0.0158(13) 0.3594(5) 0.0258(18) Uani 0.50 1 d PU . .
O5W O 0.0000 0.5931(12) 0.2500 0.055(3) Uani 1 2 d SU . .


_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 O10 2.308(5) 2_545 ?
Tb1 O2W 2.331(5) . ?
Tb1 O1W 2.337(5) . ?
Tb1 O1 2.354(5) . ?
Tb1 O6 2.398(5) . ?
Tb1 O12 2.454(4) 2 ?
Tb1 N1 2.475(5) . ?
Tb1 O11 2.503(5) 2 ?
Tb1 C16 2.844(6) 2 ?
Tb2 O2 2.292(5) . ?
Tb2 O8 2.304(5) 4_545 ?
Tb2 O3 2.323(5) 4_545 ?
Tb2 O5 2.355(5) 6_565 ?
Tb2 O9 2.357(4) 1_545 ?
Tb2 O12 2.403(4) . ?
Tb2 O7 2.443(4) . ?
Tb2 N2 2.512(5) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8499 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O1 C6 1.257(8) . ?
O2 C6 1.257(8) . ?
O3 C7 1.245(8) . ?
O3 Tb2 2.323(5) 4 ?
O4 C7 1.248(8) . ?
O5 C8 1.257(8) . ?
O5 Tb2 2.355(5) 6_566 ?
O6 C8 1.263(8) . ?
O7 C14 1.246(8) . ?
O8 C14 1.258(8) . ?
O8 Tb2 2.304(5) 4 ?
O9 C15 1.251(8) . ?
O9 Tb2 2.357(4) 1_565 ?
O10 C15 1.265(8) . ?
O10 Tb1 2.308(5) 2_565 ?
O11 C16 1.254(7) . ?
O11 Tb1 2.503(5) 2 ?
O12 C16 1.277(8) . ?
O12 Tb1 2.454(4) 2 ?
N1 C5 1.328(8) . ?
N1 C1 1.340(9) . ?
N2 C9 1.322(9) . ?
N2 C13 1.337(8) . ?
C1 C2 1.381(9) . ?
C1 C6 1.493(9) . ?
C2 C3 1.410(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(10) . ?
C3 C7 1.514(9) . ?
C4 C5 1.395(9) . ?
C4 H4 0.9500 . ?
C5 C8 1.501(9) . ?
C9 C10 1.379(9) . ?
C9 C14 1.515(9) . ?
C10 C11 1.393(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(9) . ?
C11 C15 1.503(9) . ?
C12 C13 1.366(9) . ?
C12 H12 0.9500 . ?
C13 C16 1.499(9) . ?
C16 Tb1 2.844(6) 2 ?
O4W O4W' 1.046(15) . ?

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
O10 Tb1 O2W 80.02(17) 2_545 . ?
O10 Tb1 O1W 76.43(17) 2_545 . ?
O2W Tb1 O1W 100.72(18) . . ?
O10 Tb1 O1 83.43(17) 2_545 . ?
O2W Tb1 O1 87.83(17) . . ?
O1W Tb1 O1 156.27(16) . . ?
O10 Tb1 O6 143.36(16) 2_545 . ?
O2W Tb1 O6 85.17(16) . . ?
O1W Tb1 O6 73.69(15) . . ?
O1 Tb1 O6 129.49(15) . . ?
O10 Tb1 O12 75.79(15) 2_545 2 ?
O2W Tb1 O12 154.67(16) . 2 ?
O1W Tb1 O12 80.89(16) . 2 ?
O1 Tb1 O12 82.11(15) . 2 ?
O6 Tb1 O12 119.04(15) . 2 ?
O10 Tb1 N1 141.07(17) 2_545 . ?
O2W Tb1 N1 76.42(17) . . ?
O1W Tb1 N1 138.15(17) . . ?
O1 Tb1 N1 65.26(17) . . ?
O6 Tb1 N1 64.46(16) . . ?
O12 Tb1 N1 119.17(16) 2 . ?
O10 Tb1 O11 127.61(15) 2_545 2 ?
O2W Tb1 O11 148.01(15) . 2 ?
O1W Tb1 O11 101.54(17) . 2 ?
O1 Tb1 O11 80.87(16) . 2 ?
O6 Tb1 O11 79.39(15) . 2 ?
O12 Tb1 O11 52.73(14) 2 2 ?
N1 Tb1 O11 71.66(16) . 2 ?
O10 Tb1 C16 101.78(17) 2_545 2 ?
O2W Tb1 C16 166.78(17) . 2 ?
O1W Tb1 C16 92.40(18) . 2 ?
O1 Tb1 C16 79.43(17) . 2 ?
O6 Tb1 C16 100.18(17) . 2 ?
O12 Tb1 C16 26.62(16) 2 2 ?
N1 Tb1 C16 94.87(17) . 2 ?
O11 Tb1 C16 26.15(16) 2 2 ?
O2 Tb2 O8 79.54(18) . 4_545 ?
O2 Tb2 O3 144.69(18) . 4_545 ?
O8 Tb2 O3 81.77(17) 4_545 4_545 ?
O2 Tb2 O5 142.96(17) . 6_565 ?
O8 Tb2 O5 116.02(17) 4_545 6_565 ?
O3 Tb2 O5 72.35(17) 4_545 6_565 ?
O2 Tb2 O9 76.21(17) . 1_545 ?
O8 Tb2 O9 84.36(16) 4_545 1_545 ?
O3 Tb2 O9 72.35(17) 4_545 1_545 ?
O5 Tb2 O9 135.57(16) 6_565 1_545 ?
O2 Tb2 O12 94.18(16) . . ?
O8 Tb2 O12 158.89(16) 4_545 . ?
O3 Tb2 O12 92.61(16) 4_545 . ?
O5 Tb2 O12 81.01(15) 6_565 . ?
O9 Tb2 O12 74.56(15) 1_545 . ?
O2 Tb2 O7 77.11(16) . . ?
O8 Tb2 O7 71.63(16) 4_545 . ?
O3 Tb2 O7 124.26(16) 4_545 . ?
O5 Tb2 O7 76.88(16) 6_565 . ?
O9 Tb2 O7 146.79(15) 1_545 . ?
O12 Tb2 O7 126.94(15) . . ?
O2 Tb2 N2 73.48(17) . . ?
O8 Tb2 N2 131.52(17) 4_545 . ?
O3 Tb2 N2 139.26(17) 4_545 . ?
O5 Tb2 N2 71.50(17) 6_565 . ?
O9 Tb2 N2 125.40(16) 1_545 . ?
O12 Tb2 N2 63.76(16) . . ?
O7 Tb2 N2 63.60(15) . . ?
Tb1 O1W H1WA 121.2 . . ?
Tb1 O1W H1WB 121.0 . . ?
H1WA O1W H1WB 107.6 . . ?
Tb1 O2W H2WA 118.8 . . ?
Tb1 O2W H2WB 126.3 . . ?
H2WA O2W H2WB 109.5 . . ?
C6 O1 Tb1 125.0(4) . . ?
C6 O2 Tb2 155.7(5) . . ?
C7 O3 Tb2 167.2(5) . 4 ?
C8 O5 Tb2 144.8(4) . 6_566 ?
C8 O6 Tb1 124.6(4) . . ?
C14 O7 Tb2 121.6(4) . . ?
C14 O8 Tb2 163.9(5) . 4 ?
C15 O9 Tb2 131.4(4) . 1_565 ?
C15 O10 Tb1 145.7(4) . 2_565 ?
C16 O11 Tb1 92.3(4) . 2 ?
C16 O12 Tb2 124.4(4) . . ?
C16 O12 Tb1 94.0(4) . 2 ?
Tb2 O12 Tb1 141.4(2) . 2 ?
C5 N1 C1 120.5(6) . . ?
C5 N1 Tb1 120.6(4) . . ?
C1 N1 Tb1 118.9(4) . . ?
C9 N2 C13 118.4(6) . . ?
C9 N2 Tb2 120.1(4) . . ?
C13 N2 Tb2 121.4(4) . . ?
N1 C1 C2 121.4(6) . . ?
N1 C1 C6 113.9(6) . . ?
C2 C1 C6 124.6(6) . . ?
C1 C2 C3 118.7(6) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 119.0(6) . . ?
C4 C3 C7 121.4(6) . . ?
C2 C3 C7 119.6(6) . . ?
C3 C4 C5 118.3(6) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 121.9(6) . . ?
N1 C5 C8 113.7(5) . . ?
C4 C5 C8 124.3(6) . . ?
O1 C6 O2 125.8(6) . . ?
O1 C6 C1 116.8(6) . . ?
O2 C6 C1 117.4(6) . . ?
O3 C7 O4 125.4(6) . . ?
O3 C7 C3 116.4(6) . . ?
O4 C7 C3 118.2(6) . . ?
O5 C8 O6 125.7(6) . . ?
O5 C8 C5 117.8(6) . . ?
O6 C8 C5 116.4(6) . . ?
N2 C9 C10 122.6(6) . . ?
N2 C9 C14 113.1(6) . . ?
C10 C9 C14 124.2(6) . . ?
C9 C10 C11 118.8(6) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C12 C11 C10 118.3(6) . . ?
C12 C11 C15 121.1(6) . . ?
C10 C11 C15 120.5(6) . . ?
C13 C12 C11 118.6(6) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
N2 C13 C12 123.2(6) . . ?
N2 C13 C16 112.1(6) . . ?
C12 C13 C16 124.7(6) . . ?
O7 C14 O8 125.6(6) . . ?
O7 C14 C9 116.3(6) . . ?
O8 C14 C9 118.0(6) . . ?
O9 C15 O10 126.5(6) . . ?
O9 C15 C11 117.7(6) . . ?
O10 C15 C11 115.9(6) . . ?
O11 C16 O12 120.8(6) . . ?
O11 C16 C13 121.6(6) . . ?
O12 C16 C13 117.6(5) . . ?
O11 C16 Tb1 61.6(3) . 2 ?
O12 C16 Tb1 59.4(3) . 2 ?
C13 C16 Tb1 174.1(5) . 2 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O10 Tb1 O1 C6 -157.6(5) 2_545 . . . ?
O2W Tb1 O1 C6 -77.4(5) . . . . ?
O1W Tb1 O1 C6 170.5(5) . . . . ?
O6 Tb1 O1 C6 4.6(6) . . . . ?
O12 Tb1 O1 C6 125.9(5) 2 . . . ?
N1 Tb1 O1 C6 -1.3(5) . . . . ?
O11 Tb1 O1 C6 72.6(5) 2 . . . ?
C16 Tb1 O1 C6 99.1(5) 2 . . . ?
O8 Tb2 O2 C6 -75.4(11) 4_545 . . . ?
O3 Tb2 O2 C6 -16.3(12) 4_545 . . . ?
O5 Tb2 O2 C6 164.8(10) 6_565 . . . ?
O9 Tb2 O2 C6 11.3(11) 1_545 . . . ?
O12 Tb2 O2 C6 84.2(11) . . . . ?
O7 Tb2 O2 C6 -148.8(11) . . . . ?
N2 Tb2 O2 C6 145.3(11) . . . . ?
O10 Tb1 O6 C8 142.2(5) 2_545 . . . ?
O2W Tb1 O6 C8 76.1(5) . . . . ?
O1W Tb1 O6 C8 178.8(5) . . . . ?
O1 Tb1 O6 C8 -7.1(6) . . . . ?
O12 Tb1 O6 C8 -111.8(5) 2 . . . ?
N1 Tb1 O6 C8 -1.2(5) . . . . ?
O11 Tb1 O6 C8 -75.8(5) 2 . . . ?
C16 Tb1 O6 C8 -91.7(5) 2 . . . ?
O2 Tb2 O7 C14 -57.9(5) . . . . ?
O8 Tb2 O7 C14 -141.0(5) 4_545 . . . ?
O3 Tb2 O7 C14 153.2(5) 4_545 . . . ?
O5 Tb2 O7 C14 95.5(5) 6_565 . . . ?
O9 Tb2 O7 C14 -95.1(5) 1_545 . . . ?
O12 Tb2 O7 C14 27.6(6) . . . . ?
N2 Tb2 O7 C14 19.9(5) . . . . ?
O2 Tb2 O12 C16 77.9(5) . . . . ?
O8 Tb2 O12 C16 149.4(5) 4_545 . . . ?
O3 Tb2 O12 C16 -136.8(5) 4_545 . . . ?
O5 Tb2 O12 C16 -65.2(5) 6_565 . . . ?
O9 Tb2 O12 C16 152.3(5) 1_545 . . . ?
O7 Tb2 O12 C16 0.9(5) . . . . ?
N2 Tb2 O12 C16 8.6(5) . . . . ?
O2 Tb2 O12 Tb1 -110.3(3) . . . 2 ?
O8 Tb2 O12 Tb1 -38.8(7) 4_545 . . 2 ?
O3 Tb2 O12 Tb1 35.0(3) 4_545 . . 2 ?
O5 Tb2 O12 Tb1 106.7(3) 6_565 . . 2 ?
O9 Tb2 O12 Tb1 -35.9(3) 1_545 . . 2 ?
O7 Tb2 O12 Tb1 172.7(3) . . . 2 ?
N2 Tb2 O12 Tb1 -179.6(4) . . . 2 ?
O10 Tb1 N1 C5 -141.6(4) 2_545 . . . ?
O2W Tb1 N1 C5 -87.3(5) . . . . ?
O1W Tb1 N1 C5 3.7(6) . . . . ?
O1 Tb1 N1 C5 178.8(5) . . . . ?
O6 Tb1 N1 C5 3.8(4) . . . . ?
O12 Tb1 N1 C5 114.3(5) 2 . . . ?
O11 Tb1 N1 C5 90.6(5) 2 . . . ?
C16 Tb1 N1 C5 102.8(5) 2 . . . ?
O10 Tb1 N1 C1 37.8(6) 2_545 . . . ?
O2W Tb1 N1 C1 92.1(5) . . . . ?
O1W Tb1 N1 C1 -176.9(4) . . . . ?
O1 Tb1 N1 C1 -1.8(5) . . . . ?
O6 Tb1 N1 C1 -176.8(5) . . . . ?
O12 Tb1 N1 C1 -66.3(5) 2 . . . ?
O11 Tb1 N1 C1 -90.0(5) 2 . . . ?
C16 Tb1 N1 C1 -77.8(5) 2 . . . ?
O2 Tb2 N2 C9 74.5(5) . . . . ?
O8 Tb2 N2 C9 15.6(6) 4_545 . . . ?
O3 Tb2 N2 C9 -121.8(5) 4_545 . . . ?
O5 Tb2 N2 C9 -93.2(5) 6_565 . . . ?
O9 Tb2 N2 C9 133.5(5) 1_545 . . . ?
O12 Tb2 N2 C9 177.9(5) . . . . ?
O7 Tb2 N2 C9 -9.0(5) . . . . ?
O2 Tb2 N2 C13 -108.6(5) . . . . ?
O8 Tb2 N2 C13 -167.5(4) 4_545 . . . ?
O3 Tb2 N2 C13 55.2(6) 4_545 . . . ?
O5 Tb2 N2 C13 83.7(5) 6_565 . . . ?
O9 Tb2 N2 C13 -49.6(5) 1_545 . . . ?
O12 Tb2 N2 C13 -5.2(4) . . . . ?
O7 Tb2 N2 C13 167.9(5) . . . . ?
C5 N1 C1 C2 0.0(10) . . . . ?
Tb1 N1 C1 C2 -179.3(5) . . . . ?
C5 N1 C1 C6 -176.5(6) . . . . ?
Tb1 N1 C1 C6 4.1(8) . . . . ?
N1 C1 C2 C3 1.5(10) . . . . ?
C6 C1 C2 C3 177.6(6) . . . . ?
C1 C2 C3 C4 -1.4(10) . . . . ?
C1 C2 C3 C7 178.9(6) . . . . ?
C2 C3 C4 C5 0.0(10) . . . . ?
C7 C3 C4 C5 179.7(6) . . . . ?
C1 N1 C5 C4 -1.6(10) . . . . ?
Tb1 N1 C5 C4 177.8(5) . . . . ?
C1 N1 C5 C8 174.9(6) . . . . ?
Tb1 N1 C5 C8 -5.7(7) . . . . ?
C3 C4 C5 N1 1.5(10) . . . . ?
C3 C4 C5 C8 -174.6(6) . . . . ?
Tb1 O1 C6 O2 -176.2(5) . . . . ?
Tb1 O1 C6 C1 3.9(8) . . . . ?
Tb2 O2 C6 O1 -48.3(15) . . . . ?
Tb2 O2 C6 C1 131.5(9) . . . . ?
N1 C1 C6 O1 -5.2(9) . . . . ?
C2 C1 C6 O1 178.4(7) . . . . ?
N1 C1 C6 O2 174.9(6) . . . . ?
C2 C1 C6 O2 -1.4(10) . . . . ?
Tb2 O3 C7 O4 -76(2) 4 . . . ?
Tb2 O3 C7 C3 105(2) 4 . . . ?
C4 C3 C7 O3 -148.7(7) . . . . ?
C2 C3 C7 O3 31.0(9) . . . . ?
C4 C3 C7 O4 32.5(10) . . . . ?
C2 C3 C7 O4 -147.8(7) . . . . ?
Tb2 O5 C8 O6 -36.0(12) 6_566 . . . ?
Tb2 O5 C8 C5 142.8(6) 6_566 . . . ?
Tb1 O6 C8 O5 177.6(5) . . . . ?
Tb1 O6 C8 C5 -1.2(8) . . . . ?
N1 C5 C8 O5 -174.4(6) . . . . ?
C4 C5 C8 O5 2.0(10) . . . . ?
N1 C5 C8 O6 4.5(8) . . . . ?
C4 C5 C8 O6 -179.1(6) . . . . ?
C13 N2 C9 C10 0.6(10) . . . . ?
Tb2 N2 C9 C10 177.6(5) . . . . ?
C13 N2 C9 C14 -176.7(6) . . . . ?
Tb2 N2 C9 C14 0.4(7) . . . . ?
N2 C9 C10 C11 -0.5(10) . . . . ?
C14 C9 C10 C11 176.5(6) . . . . ?
C9 C10 C11 C12 -0.8(10) . . . . ?
C9 C10 C11 C15 -177.9(6) . . . . ?
C10 C11 C12 C13 2.0(10) . . . . ?
C15 C11 C12 C13 179.1(6) . . . . ?
C9 N2 C13 C12 0.7(10) . . . . ?
Tb2 N2 C13 C12 -176.3(5) . . . . ?
C9 N2 C13 C16 179.3(6) . . . . ?
Tb2 N2 C13 C16 2.3(7) . . . . ?
C11 C12 C13 N2 -2.0(10) . . . . ?
C11 C12 C13 C16 179.5(6) . . . . ?
Tb2 O7 C14 O8 151.8(5) . . . . ?
Tb2 O7 C14 C9 -27.6(8) . . . . ?
Tb2 O8 C14 O7 40(2) 4 . . . ?
Tb2 O8 C14 C9 -140.5(14) 4 . . . ?
N2 C9 C14 O7 17.1(9) . . . . ?
C10 C9 C14 O7 -160.1(6) . . . . ?
N2 C9 C14 O8 -162.3(6) . . . . ?
C10 C9 C14 O8 20.5(10) . . . . ?
Tb2 O9 C15 O10 -60.7(9) 1_565 . . . ?
Tb2 O9 C15 C11 118.6(6) 1_565 . . . ?
Tb1 O10 C15 O9 13.9(12) 2_565 . . . ?
Tb1 O10 C15 C11 -165.4(5) 2_565 . . . ?
C12 C11 C15 O9 171.1(6) . . . . ?
C10 C11 C15 O9 -12.0(9) . . . . ?
C12 C11 C15 O10 -9.5(9) . . . . ?
C10 C11 C15 O10 167.4(6) . . . . ?
Tb1 O11 C16 O12 4.3(6) 2 . . . ?
Tb1 O11 C16 C13 -174.2(5) 2 . . . ?
Tb2 O12 C16 O11 170.5(4) . . . . ?
Tb1 O12 C16 O11 -4.4(6) 2 . . . ?
Tb2 O12 C16 C13 -10.9(8) . . . . ?
Tb1 O12 C16 C13 174.2(5) 2 . . . ?
Tb2 O12 C16 Tb1 174.9(4) . . . 2 ?
N2 C13 C16 O11 -176.3(6) . . . . ?
C12 C13 C16 O11 2.3(10) . . . . ?
N2 C13 C16 O12 5.1(8) . . . . ?
C12 C13 C16 O12 -176.3(6) . . . . ?
N2 C13 C16 Tb1 63(4) . . . 2 ?
C12 C13 C16 Tb1 -119(4) . . . 2 ?

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
O1W H1WA O11 0.85 1.91 2.756(7) 171.2 6_566
O1W H1WB O4 0.85 1.91 2.672(6) 149.0 3_445
O2W H2WA O4W' 0.85 1.78 2.606(12) 164.0 .
O2W H2WA O4W 0.85 1.91 2.730(12) 160.6 .
O2W H2WB O4 0.85 1.86 2.707(7) 170.8 7_556

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         2.085
_refine_diff_density_min         -1.962
_refine_diff_density_rms         0.218

data_dym
_database_code_depnum_ccdc_archive 'CCDC 687914'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H12 Dy2 N2 O16'
_chemical_formula_weight         813.28

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'
Dy Dy -0.1892 4.4098 '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                   21.7769(15)
_cell_length_b                   9.2174(6)
_cell_length_c                   22.3883(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.353(2)
_cell_angle_gamma                90.00
_cell_volume                     4406.0(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6858
_cell_measurement_theta_min      1.86
_cell_measurement_theta_max      25.00

_exptl_crystal_description       rhombus
_exptl_crystal_colour            pale-orange
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3056
_exptl_absorpt_coefficient_mu    6.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7014
_exptl_absorpt_correction_T_max  0.7817
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6858
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3556
_reflns_number_gt                3225
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'

_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)+(0.0305P)²+23.3687P] where P=(Fo²+2Fc²)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3556
_refine_ls_number_parameters     333
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0672
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.044718(13) 0.30858(3) 0.423601(12) 0.01459(10) Uani 1 1 d . . .
Dy2 Dy 0.156573(13) 0.39136(3) 0.176112(11) 0.01239(9) Uani 1 1 d . . .
O1W O -0.0237(2) 0.2501(6) 0.48755(19) 0.0340(12) Uani 1 1 d D . .
H1WA H -0.0198 0.3028 0.5192 0.041 Uiso 1 1 d RD . .
H1WB H -0.0607 0.2166 0.4789 0.041 Uiso 1 1 d RD . .
O2W O 0.1155(2) 0.1165(5) 0.4414(2) 0.0339(12) Uani 1 1 d D . .
H2WA H 0.1320 0.0848 0.4126 0.041 Uiso 1 1 d RD . .
H2WB H 0.1160 0.0508 0.4682 0.041 Uiso 1 1 d RD . .
O1 O 0.0739(2) 0.3387(5) 0.32941(18) 0.0271(11) Uani 1 1 d . . .
O2 O 0.1365(2) 0.4338(5) 0.27129(18) 0.0295(11) Uani 1 1 d . . .
O3 O 0.3271(3) 0.7148(6) 0.3915(2) 0.0421(14) Uani 1 1 d . . .
O4 O 0.3676(2) 0.6091(6) 0.4785(2) 0.0460(15) Uani 1 1 d . . .
O5 O 0.1734(2) 0.4948(5) 0.58621(18) 0.0286(11) Uani 1 1 d . . .
O6 O 0.0945(2) 0.3882(5) 0.52221(18) 0.0230(10) Uani 1 1 d . . .
O7 O 0.2363(2) 0.5697(4) 0.21432(19) 0.0212(10) Uani 1 1 d . . .
O8 O 0.2598(2) 0.7752(5) 0.2647(2) 0.0350(13) Uani 1 1 d . . .
O9 O 0.1013(2) 1.1838(4) 0.1955(2) 0.0301(12) Uani 1 1 d . . .
O10 O 0.0151(2) 1.1240(5) 0.1267(2) 0.0274(11) Uani 1 1 d . . .
O11 O -0.0281(2) 0.5752(5) 0.08669(19) 0.0210(10) Uani 1 1 d . . .
O12 O 0.04956(19) 0.4346(4) 0.12978(17) 0.0173(9) Uani 1 1 d . . .
N1 N 0.1467(2) 0.4266(5) 0.4294(2) 0.0173(11) Uani 1 1 d . . .
N2 N 0.1205(2) 0.6493(5) 0.1757(2) 0.0151(11) Uani 1 1 d . . .
C1 C 0.1681(3) 0.4507(7) 0.3779(3) 0.0210(15) Uani 1 1 d . . .
C2 C 0.2246(3) 0.5179(7) 0.3783(3) 0.0250(15) Uani 1 1 d . . .
H2 H 0.2381 0.5351 0.3421 0.030 Uiso 1 1 calc R . .
C3 C 0.2612(3) 0.5600(7) 0.4339(3) 0.0218(15) Uani 1 1 d . . .
C4 C 0.2388(3) 0.5358(7) 0.4873(3) 0.0231(15) Uani 1 1 d . . .
H4 H 0.2622 0.5626 0.5250 0.028 Uiso 1 1 calc R . .
C5 C 0.1803(3) 0.4703(6) 0.4825(2) 0.0183(14) Uani 1 1 d . . .
C6 C 0.1228(3) 0.4039(7) 0.3210(3) 0.0201(15) Uani 1 1 d . . .
C7 C 0.3240(3) 0.6339(7) 0.4353(3) 0.0254(15) Uani 1 1 d . . .
C8 C 0.1474(3) 0.4488(6) 0.5352(3) 0.0196(14) Uani 1 1 d . . .
C9 C 0.1603(3) 0.7536(6) 0.2013(3) 0.0190(14) Uani 1 1 d . . .
C10 C 0.1436(3) 0.8966(7) 0.1989(3) 0.0223(15) Uani 1 1 d . . .
H10 H 0.1718 0.9662 0.2178 0.027 Uiso 1 1 calc R . .
C11 C 0.0843(3) 0.9376(7) 0.1681(3) 0.0207(14) Uani 1 1 d . . .
C12 C 0.0437(3) 0.8298(7) 0.1414(3) 0.0235(15) Uani 1 1 d . . .
H12 H 0.0038 0.8531 0.1202 0.028 Uiso 1 1 calc R . .
C13 C 0.0635(3) 0.6875(6) 0.1466(3) 0.0166(13) Uani 1 1 d . . .
C14 C 0.2245(3) 0.6954(6) 0.2289(3) 0.0173(14) Uani 1 1 d . . .
C15 C 0.0658(3) 1.0951(6) 0.1632(3) 0.0221(15) Uani 1 1 d . . .
C16 C 0.0258(3) 0.5598(6) 0.1192(2) 0.0135(13) Uani 1 1 d . . .
O3W O -0.0976(8) 0.754(2) 0.1722(8) 0.102(6) Uani 0.50 1 d P . .
O4W O 0.1463(19) 0.062(4) 0.3272(13) 0.093(8) Uani 0.50 1 d P . .
O4W' O 0.1633(19) 0.013(4) 0.3516(13) 0.093(8) Uani 0.50 1 d P . .
O5W O 0.0000 0.5837(15) 0.2500 0.105(4) Uani 1 2 d S . .


_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
Dy1 O10 2.298(4) 2_545 ?
Dy1 O1W 2.323(4) . ?
Dy1 O2W 2.329(5) . ?
Dy1 O1 2.336(4) . ?
Dy1 O6 2.376(4) . ?
Dy1 N1 2.453(5) . ?
Dy1 O12 2.455(4) 2 ?
Dy1 O11 2.488(4) 2 ?
Dy1 C16 2.839(6) 2 ?
Dy2 O2 2.292(4) . ?
Dy2 O8 2.296(4) 4_545 ?
Dy2 O3 2.297(5) 4_545 ?
Dy2 O9 2.345(4) 1_545 ?
Dy2 O5 2.362(4) 6_565 ?
Dy2 O12 2.390(4) . ?
Dy2 O7 2.422(4) . ?
Dy2 N2 2.503(5) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8498 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8501 . ?
O1 C6 1.267(8) . ?
O2 C6 1.239(7) . ?
O3 C7 1.245(8) . ?
O3 Dy2 2.297(5) 4 ?
O4 C7 1.236(8) . ?
O5 C8 1.245(7) . ?
O5 Dy2 2.362(4) 6_566 ?
O6 C8 1.261(8) . ?
O7 C14 1.244(7) . ?
O8 C14 1.237(7) . ?
O8 Dy2 2.296(4) 4 ?
O9 C15 1.253(7) . ?
O9 Dy2 2.345(4) 1_565 ?
O10 C15 1.265(8) . ?
O10 Dy1 2.298(4) 2_565 ?
O11 C16 1.262(7) . ?
O11 Dy1 2.488(4) 2 ?
O12 C16 1.268(7) . ?
O12 Dy1 2.455(4) 2 ?
N1 C5 1.329(7) . ?
N1 C1 1.346(8) . ?
N2 C13 1.331(7) . ?
N2 C9 1.345(8) . ?
C1 C2 1.375(9) . ?
C1 C6 1.512(8) . ?
C2 C3 1.395(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.395(9) . ?
C3 C7 1.521(9) . ?
C4 C5 1.395(9) . ?
C4 H4 0.9300 . ?
C5 C8 1.509(8) . ?
C9 C10 1.364(8) . ?
C9 C14 1.511(8) . ?
C10 C11 1.392(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(9) . ?
C11 C15 1.505(8) . ?
C12 C13 1.378(8) . ?
C12 H12 0.9300 . ?
C13 C16 1.496(8) . ?
C16 Dy1 2.839(6) 2 ?
O4W O4W' 0.75(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
O10 Dy1 O1W 76.12(17) 2_545 . ?
O10 Dy1 O2W 79.24(17) 2_545 . ?
O1W Dy1 O2W 101.58(18) . . ?
O10 Dy1 O1 82.78(16) 2_545 . ?
O1W Dy1 O1 154.87(15) . . ?
O2W Dy1 O1 87.53(17) . . ?
O10 Dy1 O6 142.66(15) 2_545 . ?
O1W Dy1 O6 74.33(15) . . ?
O2W Dy1 O6 84.82(16) . . ?
O1 Dy1 O6 130.26(15) . . ?
O10 Dy1 N1 140.73(17) 2_545 . ?
O1W Dy1 N1 138.89(15) . . ?
O2W Dy1 N1 76.50(17) . . ?
O1 Dy1 N1 65.85(15) . . ?
O6 Dy1 N1 64.57(15) . . ?
O10 Dy1 O12 76.85(14) 2_545 2 ?
O1W Dy1 O12 80.41(16) . 2 ?
O2W Dy1 O12 154.77(15) . 2 ?
O1 Dy1 O12 81.63(15) . 2 ?
O6 Dy1 O12 119.43(14) . 2 ?
N1 Dy1 O12 118.55(15) . 2 ?
O10 Dy1 O11 128.88(14) 2_545 2 ?
O1W Dy1 O11 100.77(17) . 2 ?
O2W Dy1 O11 147.76(16) . 2 ?
O1 Dy1 O11 81.91(16) . 2 ?
O6 Dy1 O11 79.19(14) . 2 ?
N1 Dy1 O11 71.37(15) . 2 ?
O12 Dy1 O11 52.79(13) 2 2 ?
O10 Dy1 C16 102.80(15) 2_545 2 ?
O1W Dy1 C16 91.58(18) . 2 ?
O2W Dy1 C16 166.76(17) . 2 ?
O1 Dy1 C16 79.82(17) . 2 ?
O6 Dy1 C16 100.35(15) . 2 ?
N1 Dy1 C16 94.60(16) . 2 ?
O12 Dy1 C16 26.46(14) 2 2 ?
O11 Dy1 C16 26.36(14) 2 2 ?
O2 Dy2 O8 79.50(18) . 4_545 ?
O2 Dy2 O3 144.69(18) . 4_545 ?
O8 Dy2 O3 80.91(18) 4_545 4_545 ?
O2 Dy2 O9 76.61(16) . 1_545 ?
O8 Dy2 O9 83.71(16) 4_545 1_545 ?
O3 Dy2 O9 72.27(18) 4_545 1_545 ?
O2 Dy2 O5 143.78(17) . 6_565 ?
O8 Dy2 O5 117.43(17) 4_545 6_565 ?
O3 Dy2 O5 71.53(18) 4_545 6_565 ?
O9 Dy2 O5 133.74(16) 1_545 6_565 ?
O2 Dy2 O12 91.53(16) . . ?
O8 Dy2 O12 157.39(15) 4_545 . ?
O3 Dy2 O12 95.51(16) 4_545 . ?
O9 Dy2 O12 73.99(14) 1_545 . ?
O5 Dy2 O12 81.83(14) 6_565 . ?
O2 Dy2 O7 79.10(15) . . ?
O8 Dy2 O7 71.36(15) 4_545 . ?
O3 Dy2 O7 121.36(17) 4_545 . ?
O9 Dy2 O7 147.86(15) 1_545 . ?
O5 Dy2 O7 77.20(15) 6_565 . ?
O12 Dy2 O7 127.61(13) . . ?
O2 Dy2 N2 73.99(16) . . ?
O8 Dy2 N2 131.13(16) 4_545 . ?
O3 Dy2 N2 139.42(17) 4_545 . ?
O9 Dy2 N2 127.11(16) 1_545 . ?
O5 Dy2 N2 71.10(16) 6_565 . ?
O12 Dy2 N2 64.01(14) . . ?
O7 Dy2 N2 63.85(15) . . ?
Dy1 O1W H1WA 114.3 . . ?
Dy1 O1W H1WB 129.7 . . ?
H1WA O1W H1WB 109.4 . . ?
Dy1 O2W H2WA 119.7 . . ?
Dy1 O2W H2WB 125.4 . . ?
H2WA O2W H2WB 109.9 . . ?
C6 O1 Dy1 125.1(4) . . ?
C6 O2 Dy2 157.1(4) . . ?
C7 O3 Dy2 169.5(5) . 4 ?
C8 O5 Dy2 144.5(4) . 6_566 ?
C8 O6 Dy1 125.5(4) . . ?
C14 O7 Dy2 123.6(4) . . ?
C14 O8 Dy2 166.5(5) . 4 ?
C15 O9 Dy2 135.0(4) . 1_565 ?
C15 O10 Dy1 144.1(4) . 2_565 ?
C16 O11 Dy1 92.5(3) . 2 ?
C16 O12 Dy2 124.0(4) . . ?
C16 O12 Dy1 93.9(3) . 2 ?
Dy2 O12 Dy1 141.54(17) . 2 ?
C5 N1 C1 119.6(5) . . ?
C5 N1 Dy1 121.0(4) . . ?
C1 N1 Dy1 119.4(4) . . ?
C13 N2 C9 118.6(5) . . ?
C13 N2 Dy2 121.0(4) . . ?
C9 N2 Dy2 120.2(4) . . ?
N1 C1 C2 121.9(6) . . ?
N1 C1 C6 113.3(6) . . ?
C2 C1 C6 124.7(6) . . ?
C1 C2 C3 119.0(6) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 119.0(6) . . ?
C4 C3 C7 121.3(6) . . ?
C2 C3 C7 119.8(6) . . ?
C5 C4 C3 118.2(6) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
N1 C5 C4 122.2(5) . . ?
N1 C5 C8 113.3(5) . . ?
C4 C5 C8 124.3(5) . . ?
O2 C6 O1 126.5(6) . . ?
O2 C6 C1 117.4(6) . . ?
O1 C6 C1 116.1(5) . . ?
O4 C7 O3 125.1(7) . . ?
O4 C7 C3 118.8(6) . . ?
O3 C7 C3 116.1(6) . . ?
O5 C8 O6 126.3(6) . . ?
O5 C8 C5 118.2(6) . . ?
O6 C8 C5 115.5(5) . . ?
N2 C9 C10 122.0(6) . . ?
N2 C9 C14 112.7(5) . . ?
C10 C9 C14 125.2(5) . . ?
C9 C10 C11 119.7(6) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 118.0(6) . . ?
C12 C11 C15 121.4(6) . . ?
C10 C11 C15 120.5(6) . . ?
C13 C12 C11 118.9(6) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
N2 C13 C12 122.7(5) . . ?
N2 C13 C16 112.0(5) . . ?
C12 C13 C16 125.3(6) . . ?
O8 C14 O7 126.0(6) . . ?
O8 C14 C9 117.4(5) . . ?
O7 C14 C9 116.5(5) . . ?
O9 C15 O10 126.6(6) . . ?
O9 C15 C11 117.4(6) . . ?
O10 C15 C11 115.9(5) . . ?
O11 C16 O12 120.6(5) . . ?
O11 C16 C13 121.4(5) . . ?
O12 C16 C13 118.0(5) . . ?
O11 C16 Dy1 61.1(3) . 2 ?
O12 C16 Dy1 59.6(3) . 2 ?
C13 C16 Dy1 175.6(4) . 2 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O10 Dy1 O1 C6 -159.9(5) 2_545 . . . ?
O1W Dy1 O1 C6 167.2(5) . . . . ?
O2W Dy1 O1 C6 -80.4(5) . . . . ?
O6 Dy1 O1 C6 0.7(6) . . . . ?
N1 Dy1 O1 C6 -4.1(5) . . . . ?
O12 Dy1 O1 C6 122.4(5) 2 . . . ?
O11 Dy1 O1 C6 69.0(5) 2 . . . ?
C16 Dy1 O1 C6 95.7(5) 2 . . . ?
O8 Dy2 O2 C6 -66.7(12) 4_545 . . . ?
O3 Dy2 O2 C6 -9.4(14) 4_545 . . . ?
O9 Dy2 O2 C6 19.3(12) 1_545 . . . ?
O5 Dy2 O2 C6 170.6(11) 6_565 . . . ?
O12 Dy2 O2 C6 92.4(12) . . . . ?
O7 Dy2 O2 C6 -139.5(12) . . . . ?
N2 Dy2 O2 C6 154.8(12) . . . . ?
O10 Dy1 O6 C8 140.9(5) 2_545 . . . ?
O1W Dy1 O6 C8 179.8(5) . . . . ?
O2W Dy1 O6 C8 76.2(5) . . . . ?
O1 Dy1 O6 C8 -6.1(6) . . . . ?
N1 Dy1 O6 C8 -1.3(5) . . . . ?
O12 Dy1 O6 C8 -111.1(5) 2 . . . ?
O11 Dy1 O6 C8 -75.7(5) 2 . . . ?
C16 Dy1 O6 C8 -91.5(5) 2 . . . ?
O2 Dy2 O7 C14 -61.9(5) . . . . ?
O8 Dy2 O7 C14 -144.3(5) 4_545 . . . ?
O3 Dy2 O7 C14 149.3(4) 4_545 . . . ?
O9 Dy2 O7 C14 -103.3(5) 1_545 . . . ?
O5 Dy2 O7 C14 90.5(5) 6_565 . . . ?
O12 Dy2 O7 C14 21.6(5) . . . . ?
N2 Dy2 O7 C14 15.5(4) . . . . ?
O2 Dy2 O12 C16 80.1(4) . . . . ?
O8 Dy2 O12 C16 145.8(5) 4_545 . . . ?
O3 Dy2 O12 C16 -134.6(5) 4_545 . . . ?
O9 Dy2 O12 C16 155.7(5) 1_545 . . . ?
O5 Dy2 O12 C16 -64.2(4) 6_565 . . . ?
O7 Dy2 O12 C16 2.7(5) . . . . ?
N2 Dy2 O12 C16 8.7(4) . . . . ?
O2 Dy2 O12 Dy1 -110.5(3) . . . 2 ?
O8 Dy2 O12 Dy1 -44.7(6) 4_545 . . 2 ?
O3 Dy2 O12 Dy1 34.8(3) 4_545 . . 2 ?
O9 Dy2 O12 Dy1 -34.9(3) 1_545 . . 2 ?
O5 Dy2 O12 Dy1 105.2(3) 6_565 . . 2 ?
O7 Dy2 O12 Dy1 172.1(2) . . . 2 ?
N2 Dy2 O12 Dy1 178.1(3) . . . 2 ?
O10 Dy1 N1 C5 -141.2(4) 2_545 . . . ?
O1W Dy1 N1 C5 4.4(6) . . . . ?
O2W Dy1 N1 C5 -87.8(5) . . . . ?
O1 Dy1 N1 C5 178.8(5) . . . . ?
O6 Dy1 N1 C5 2.8(4) . . . . ?
O12 Dy1 N1 C5 114.0(4) 2 . . . ?
O11 Dy1 N1 C5 89.5(5) 2 . . . ?
C16 Dy1 N1 C5 102.1(5) 2 . . . ?
O10 Dy1 N1 C1 40.5(6) 2_545 . . . ?
O1W Dy1 N1 C1 -173.9(4) . . . . ?
O2W Dy1 N1 C1 93.9(5) . . . . ?
O1 Dy1 N1 C1 0.5(4) . . . . ?
O6 Dy1 N1 C1 -175.4(5) . . . . ?
O12 Dy1 N1 C1 -64.3(5) 2 . . . ?
O11 Dy1 N1 C1 -88.8(5) 2 . . . ?
C16 Dy1 N1 C1 -76.2(5) 2 . . . ?
O2 Dy2 N2 C13 -105.6(5) . . . . ?
O8 Dy2 N2 C13 -165.4(4) 4_545 . . . ?
O3 Dy2 N2 C13 60.4(6) 4_545 . . . ?
O9 Dy2 N2 C13 -46.8(5) 1_545 . . . ?
O5 Dy2 N2 C13 84.3(5) 6_565 . . . ?
O12 Dy2 N2 C13 -5.7(4) . . . . ?
O7 Dy2 N2 C13 168.9(5) . . . . ?
O2 Dy2 N2 C9 79.2(4) . . . . ?
O8 Dy2 N2 C9 19.4(5) 4_545 . . . ?
O3 Dy2 N2 C9 -114.8(5) 4_545 . . . ?
O9 Dy2 N2 C9 138.0(4) 1_545 . . . ?
O5 Dy2 N2 C9 -91.0(5) 6_565 . . . ?
O12 Dy2 N2 C9 179.1(5) . . . . ?
O7 Dy2 N2 C9 -6.3(4) . . . . ?
C5 N1 C1 C2 0.9(9) . . . . ?
Dy1 N1 C1 C2 179.2(5) . . . . ?
C5 N1 C1 C6 -176.1(5) . . . . ?
Dy1 N1 C1 C6 2.2(7) . . . . ?
N1 C1 C2 C3 1.2(10) . . . . ?
C6 C1 C2 C3 177.9(6) . . . . ?
C1 C2 C3 C4 -1.6(10) . . . . ?
C1 C2 C3 C7 179.7(6) . . . . ?
C2 C3 C4 C5 -0.1(9) . . . . ?
C7 C3 C4 C5 178.7(6) . . . . ?
C1 N1 C5 C4 -2.6(9) . . . . ?
Dy1 N1 C5 C4 179.1(4) . . . . ?
C1 N1 C5 C8 174.4(5) . . . . ?
Dy1 N1 C5 C8 -3.9(7) . . . . ?
C3 C4 C5 N1 2.2(9) . . . . ?
C3 C4 C5 C8 -174.5(6) . . . . ?
Dy2 O2 C6 O1 -56.5(16) . . . . ?
Dy2 O2 C6 C1 124.3(10) . . . . ?
Dy1 O1 C6 O2 -172.5(5) . . . . ?
Dy1 O1 C6 C1 6.7(8) . . . . ?
N1 C1 C6 O2 173.8(6) . . . . ?
C2 C1 C6 O2 -3.1(10) . . . . ?
N1 C1 C6 O1 -5.5(8) . . . . ?
C2 C1 C6 O1 177.6(6) . . . . ?
Dy2 O3 C7 O4 -41(3) 4 . . . ?
Dy2 O3 C7 C3 140(3) 4 . . . ?
C4 C3 C7 O4 36.1(10) . . . . ?
C2 C3 C7 O4 -145.1(7) . . . . ?
C4 C3 C7 O3 -144.5(7) . . . . ?
C2 C3 C7 O3 34.2(9) . . . . ?
Dy2 O5 C8 O6 -36.4(11) 6_566 . . . ?
Dy2 O5 C8 C5 141.5(6) 6_566 . . . ?
Dy1 O6 C8 O5 177.9(5) . . . . ?
Dy1 O6 C8 C5 -0.2(7) . . . . ?
N1 C5 C8 O5 -175.6(6) . . . . ?
C4 C5 C8 O5 1.4(9) . . . . ?
N1 C5 C8 O6 2.6(8) . . . . ?
C4 C5 C8 O6 179.6(6) . . . . ?
C13 N2 C9 C10 0.7(9) . . . . ?
Dy2 N2 C9 C10 176.1(5) . . . . ?
C13 N2 C9 C14 -176.1(5) . . . . ?
Dy2 N2 C9 C14 -0.8(7) . . . . ?
N2 C9 C10 C11 -1.4(10) . . . . ?
C14 C9 C10 C11 175.0(6) . . . . ?
C9 C10 C11 C12 0.8(10) . . . . ?
C9 C10 C11 C15 -178.1(6) . . . . ?
C10 C11 C12 C13 0.3(10) . . . . ?
C15 C11 C12 C13 179.2(6) . . . . ?
C9 N2 C13 C12 0.5(9) . . . . ?
Dy2 N2 C13 C12 -174.8(5) . . . . ?
C9 N2 C13 C16 178.3(5) . . . . ?
Dy2 N2 C13 C16 3.1(7) . . . . ?
C11 C12 C13 N2 -1.0(10) . . . . ?
C11 C12 C13 C16 -178.6(6) . . . . ?
Dy2 O8 C14 O7 27(2) 4 . . . ?
Dy2 O8 C14 C9 -154.7(16) 4 . . . ?
Dy2 O7 C14 O8 156.5(5) . . . . ?
Dy2 O7 C14 C9 -21.9(7) . . . . ?
N2 C9 C14 O8 -164.6(6) . . . . ?
C10 C9 C14 O8 18.7(10) . . . . ?
N2 C9 C14 O7 14.0(8) . . . . ?
C10 C9 C14 O7 -162.7(6) . . . . ?
Dy2 O9 C15 O10 -58.2(10) 1_565 . . . ?
Dy2 O9 C15 C11 122.2(6) 1_565 . . . ?
Dy1 O10 C15 O9 13.5(13) 2_565 . . . ?
Dy1 O10 C15 C11 -166.9(5) 2_565 . . . ?
C12 C11 C15 O9 170.3(6) . . . . ?
C10 C11 C15 O9 -10.9(10) . . . . ?
C12 C11 C15 O10 -9.4(10) . . . . ?
C10 C11 C15 O10 169.4(6) . . . . ?
Dy1 O11 C16 O12 4.0(6) 2 . . . ?
Dy1 O11 C16 C13 -175.9(5) 2 . . . ?
Dy2 O12 C16 O11 169.4(4) . . . . ?
Dy1 O12 C16 O11 -4.0(6) 2 . . . ?
Dy2 O12 C16 C13 -10.8(7) . . . . ?
Dy1 O12 C16 C13 175.8(5) 2 . . . ?
Dy2 O12 C16 Dy1 173.4(4) . . . 2 ?
N2 C13 C16 O11 -175.6(5) . . . . ?
C12 C13 C16 O11 2.2(10) . . . . ?
N2 C13 C16 O12 4.5(8) . . . . ?
C12 C13 C16 O12 -177.7(6) . . . . ?
N2 C13 C16 Dy1 61(6) . . . 2 ?
C12 C13 C16 Dy1 -122(6) . . . 2 ?

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
O1W H1WA O11 0.85 1.92 2.759(6) 169.0 6_566
O1W H1WB O4 0.85 1.85 2.674(7) 163.6 3_445
O2W H2WA O4W' 0.85 1.77 2.62(4) 177.3 .
O2W H2WA O4W 0.85 2.01 2.81(3) 158.0 .
O2W H2WB O4 0.85 1.89 2.722(7) 167.7 7_556

_diffrn_measured_fraction_theta_max 0.919
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.919
_refine_diff_density_max         1.479
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.151

data_hom
_database_code_depnum_ccdc_archive 'CCDC 687915'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H12 Ho2 N2 O16'
_chemical_formula_weight         818.14

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'
Ho Ho -0.2175 4.6783 '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                   21.721(8)
_cell_length_b                   9.202(4)
_cell_length_c                   22.347(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.243(6)
_cell_angle_gamma                90.00
_cell_volume                     4381(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14590
_cell_measurement_theta_min      1.86
_cell_measurement_theta_max      26.00

_exptl_crystal_description       rhombus
_exptl_crystal_colour            pale-pink
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3072
_exptl_absorpt_coefficient_mu    7.259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6157
_exptl_absorpt_correction_T_max  0.6537
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14590
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4289
_reflns_number_gt                3939
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'

_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)+(0.0261P)²+18.4749P] where P=(Fo²+2Fc²)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4289
_refine_ls_number_parameters     339
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0564
_refine_ls_wR_factor_gt          0.0549
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.057
_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
Ho1 Ho 0.045266(9) 0.31018(2) 0.423288(9) 0.01310(7) Uani 1 1 d . . .
Ho2 Ho 0.156078(9) 0.39203(2) 0.176175(8) 0.01148(6) Uani 1 1 d . . .
O1W O -0.02207(16) 0.2498(4) 0.48728(15) 0.0295(8) Uani 1 1 d D . .
H1WA H -0.0251 0.2970 0.5193 0.035 Uiso 1 1 d RD . .
H1WB H -0.0550 0.1994 0.4755 0.035 Uiso 1 1 d RD . .
O2W O 0.11525(17) 0.1180(4) 0.44166(16) 0.0301(8) Uani 1 1 d D . .
H2WA H 0.1288 0.0910 0.4102 0.036 Uiso 1 1 d RD . .
H2WB H 0.1202 0.0516 0.4686 0.036 Uiso 1 1 d RD . .
O1 O 0.07407(16) 0.3422(4) 0.32927(14) 0.0243(8) Uani 1 1 d . . .
O2 O 0.13697(17) 0.4360(4) 0.27124(14) 0.0273(8) Uani 1 1 d . . .
O3 O 0.32871(18) 0.7149(4) 0.39173(17) 0.0363(9) Uani 1 1 d . . .
O4 O 0.36866(17) 0.6084(5) 0.47890(18) 0.0401(10) Uani 1 1 d . . .
O5 O 0.17399(15) 0.4950(4) 0.58654(14) 0.0256(8) Uani 1 1 d . . .
O6 O 0.09465(15) 0.3889(4) 0.52240(14) 0.0214(7) Uani 1 1 d . . .
O7 O 0.23636(14) 0.5692(3) 0.21415(14) 0.0186(7) Uani 1 1 d . . .
O8 O 0.25997(16) 0.7749(4) 0.26560(17) 0.0312(9) Uani 1 1 d . . .
O9 O 0.10035(16) 1.1859(3) 0.19662(16) 0.0256(8) Uani 1 1 d . . .
O10 O 0.01441(16) 1.1262(4) 0.12784(16) 0.0262(8) Uani 1 1 d . . .
O11 O -0.02820(14) 0.5759(3) 0.08615(14) 0.0184(7) Uani 1 1 d . . .
O12 O 0.04944(14) 0.4352(3) 0.12951(14) 0.0177(7) Uani 1 1 d . . .
N1 N 0.14737(17) 0.4278(4) 0.42923(16) 0.0140(8) Uani 1 1 d . . .
N2 N 0.12040(17) 0.6501(4) 0.17600(16) 0.0137(8) Uani 1 1 d . . .
C1 C 0.1688(2) 0.4528(5) 0.3778(2) 0.0181(10) Uani 1 1 d . . .
C2 C 0.2254(2) 0.5201(5) 0.3783(2) 0.0217(10) Uani 1 1 d . . .
H2 H 0.2389 0.5381 0.3420 0.026 Uiso 1 1 calc R . .
C3 C 0.2625(2) 0.5610(5) 0.4343(2) 0.0196(10) Uani 1 1 d . . .
C4 C 0.2395(2) 0.5362(5) 0.4875(2) 0.0186(10) Uani 1 1 d . . .
H4 H 0.2628 0.5629 0.5253 0.022 Uiso 1 1 calc R . .
C5 C 0.1811(2) 0.4713(5) 0.48289(19) 0.0156(9) Uani 1 1 d . . .
C6 C 0.1234(2) 0.4062(5) 0.3209(2) 0.0190(10) Uani 1 1 d . . .
C7 C 0.3254(2) 0.6344(5) 0.4357(2) 0.0200(10) Uani 1 1 d . . .
C8 C 0.1476(2) 0.4495(5) 0.5352(2) 0.0179(10) Uani 1 1 d . . .
C9 C 0.1600(2) 0.7540(5) 0.2017(2) 0.0173(9) Uani 1 1 d . . .
C10 C 0.1434(2) 0.8988(5) 0.1999(2) 0.0205(10) Uani 1 1 d . . .
H10 H 0.1715 0.9687 0.2187 0.025 Uiso 1 1 calc R . .
C11 C 0.0836(2) 0.9383(5) 0.1692(2) 0.0183(10) Uani 1 1 d . . .
C12 C 0.0425(2) 0.8314(5) 0.1415(2) 0.0198(10) Uani 1 1 d . . .
H12 H 0.0025 0.8552 0.1204 0.024 Uiso 1 1 calc R . .
C13 C 0.0628(2) 0.6884(5) 0.1464(2) 0.0150(9) Uani 1 1 d . . .
C14 C 0.2241(2) 0.6960(5) 0.2294(2) 0.0166(9) Uani 1 1 d . . .
C15 C 0.0643(2) 1.0972(5) 0.1644(2) 0.0185(10) Uani 1 1 d . . .
C16 C 0.0253(2) 0.5608(5) 0.11916(19) 0.0149(9) Uani 1 1 d . . .
O3W O -0.0975(7) 0.7530(16) 0.1703(7) 0.111(5) Uani 0.50 1 d P . .
O4W O 0.1460(9) 0.060(2) 0.3300(7) 0.054(4) Uani 0.50 1 d P . .
O4W' O 0.1651(11) 0.018(3) 0.3522(10) 0.122(9) Uani 0.50 1 d P . .
O5W O 0.0000 0.5842(13) 0.2500 0.116(4) Uani 1 2 d S . .


_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
Ho1 O10 2.296(3) 2_545 ?
Ho1 O1W 2.304(3) . ?
Ho1 O2W 2.316(3) . ?
Ho1 O1 2.325(3) . ?
Ho1 O6 2.378(3) . ?
Ho1 N1 2.448(4) . ?
Ho1 O12 2.450(3) 2 ?
Ho1 O11 2.476(3) 2 ?
Ho1 C16 2.829(4) 2 ?
Ho2 O2 2.279(3) . ?
Ho2 O8 2.293(3) 4_545 ?
Ho2 O3 2.294(3) 4_545 ?
Ho2 O9 2.343(3) 1_545 ?
Ho2 O5 2.356(3) 6_565 ?
Ho2 O12 2.381(3) . ?
Ho2 O7 2.417(3) . ?
Ho2 N2 2.498(4) . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8502 . ?
O2W H2WB 0.8499 . ?
O1 C6 1.268(6) . ?
O2 C6 1.234(5) . ?
O3 C7 1.245(6) . ?
O3 Ho2 2.294(3) 4 ?
O4 C7 1.232(6) . ?
O5 C8 1.250(5) . ?
O5 Ho2 2.356(3) 6_566 ?
O6 C8 1.260(6) . ?
O7 C14 1.258(5) . ?
O8 C14 1.241(5) . ?
O8 Ho2 2.293(3) 4 ?
O9 C15 1.257(5) . ?
O9 Ho2 2.343(3) 1_565 ?
O10 C15 1.251(6) . ?
O10 Ho1 2.296(3) 2_565 ?
O11 C16 1.257(5) . ?
O11 Ho1 2.476(3) 2 ?
O12 C16 1.272(5) . ?
O12 Ho1 2.450(3) 2 ?
N1 C5 1.339(5) . ?
N1 C1 1.340(6) . ?
N2 C9 1.338(6) . ?
N2 C13 1.342(6) . ?
C1 C2 1.375(6) . ?
C1 C6 1.512(6) . ?
C2 C3 1.401(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(6) . ?
C3 C7 1.517(6) . ?
C4 C5 1.387(6) . ?
C4 H4 0.9300 . ?
C5 C8 1.506(6) . ?
C9 C10 1.379(6) . ?
C9 C14 1.507(6) . ?
C10 C11 1.392(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.390(6) . ?
C11 C15 1.520(6) . ?
C12 C13 1.386(6) . ?
C12 H12 0.9300 . ?
C13 C16 1.490(6) . ?
C16 Ho1 2.829(4) 2 ?
O4W O4W' 0.70(2) . ?

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
O10 Ho1 O1W 76.46(13) 2_545 . ?
O10 Ho1 O2W 79.21(13) 2_545 . ?
O1W Ho1 O2W 100.36(13) . . ?
O10 Ho1 O1 82.47(12) 2_545 . ?
O1W Ho1 O1 155.05(12) . . ?
O2W Ho1 O1 88.51(13) . . ?
O10 Ho1 O6 142.79(12) 2_545 . ?
O1W Ho1 O6 73.80(11) . . ?
O2W Ho1 O6 84.62(12) . . ?
O1 Ho1 O6 130.63(11) . . ?
O10 Ho1 N1 140.40(13) 2_545 . ?
O1W Ho1 N1 138.67(12) . . ?
O2W Ho1 N1 76.80(13) . . ?
O1 Ho1 N1 65.95(11) . . ?
O6 Ho1 N1 64.87(11) . . ?
O10 Ho1 O12 76.53(11) 2_545 2 ?
O1W Ho1 O12 80.64(12) . 2 ?
O2W Ho1 O12 154.77(12) . 2 ?
O1 Ho1 O12 81.59(11) . 2 ?
O6 Ho1 O12 119.30(11) . 2 ?
N1 Ho1 O12 119.02(11) . 2 ?
O10 Ho1 O11 128.67(11) 2_545 2 ?
O1W Ho1 O11 100.87(12) . 2 ?
O2W Ho1 O11 148.37(12) . 2 ?
O1 Ho1 O11 81.96(12) . 2 ?
O6 Ho1 O11 79.13(11) . 2 ?
N1 Ho1 O11 71.75(11) . 2 ?
O12 Ho1 O11 52.94(10) 2 2 ?
O10 Ho1 C16 102.58(12) 2_545 2 ?
O1W Ho1 C16 92.11(13) . 2 ?
O2W Ho1 C16 167.45(13) . 2 ?
O1 Ho1 C16 79.48(13) . 2 ?
O6 Ho1 C16 100.39(12) . 2 ?
N1 Ho1 C16 94.79(12) . 2 ?
O12 Ho1 C16 26.66(11) 2 2 ?
O11 Ho1 C16 26.34(11) 2 2 ?
O2 Ho2 O8 79.84(14) . 4_545 ?
O2 Ho2 O3 144.94(14) . 4_545 ?
O8 Ho2 O3 80.80(14) 4_545 4_545 ?
O2 Ho2 O9 76.52(12) . 1_545 ?
O8 Ho2 O9 83.83(12) 4_545 1_545 ?
O3 Ho2 O9 72.56(14) 4_545 1_545 ?
O2 Ho2 O5 143.59(13) . 6_565 ?
O8 Ho2 O5 116.44(13) 4_545 6_565 ?
O3 Ho2 O5 71.46(14) 4_545 6_565 ?
O9 Ho2 O5 134.47(12) 1_545 6_565 ?
O2 Ho2 O12 92.30(12) . . ?
O8 Ho2 O12 157.72(12) 4_545 . ?
O3 Ho2 O12 94.72(12) 4_545 . ?
O9 Ho2 O12 74.04(11) 1_545 . ?
O5 Ho2 O12 82.05(11) 6_565 . ?
O2 Ho2 O7 78.65(12) . . ?
O8 Ho2 O7 71.24(11) 4_545 . ?
O3 Ho2 O7 121.62(13) 4_545 . ?
O9 Ho2 O7 147.42(11) 1_545 . ?
O5 Ho2 O7 76.90(12) 6_565 . ?
O12 Ho2 O7 127.94(10) . . ?
O2 Ho2 N2 73.73(12) . . ?
O8 Ho2 N2 131.32(12) 4_545 . ?
O3 Ho2 N2 139.38(13) 4_545 . ?
O9 Ho2 N2 126.74(12) 1_545 . ?
O5 Ho2 N2 71.44(12) 6_565 . ?
O12 Ho2 N2 64.25(11) . . ?
O7 Ho2 N2 64.00(11) . . ?
Ho1 O1W H1WA 124.1 . . ?
Ho1 O1W H1WB 122.4 . . ?
H1WA O1W H1WB 110.0 . . ?
Ho1 O2W H2WA 113.4 . . ?
Ho1 O2W H2WB 131.5 . . ?
H2WA O2W H2WB 111.0 . . ?
C6 O1 Ho1 125.1(3) . . ?
C6 O2 Ho2 156.7(3) . . ?
C7 O3 Ho2 169.6(4) . 4 ?
C8 O5 Ho2 143.7(3) . 6_566 ?
C8 O6 Ho1 124.9(3) . . ?
C14 O7 Ho2 123.0(3) . . ?
C14 O8 Ho2 166.7(3) . 4 ?
C15 O9 Ho2 134.6(3) . 1_565 ?
C15 O10 Ho1 144.6(3) . 2_565 ?
C16 O11 Ho1 92.7(3) . 2 ?
C16 O12 Ho2 124.3(3) . . ?
C16 O12 Ho1 93.5(3) . 2 ?
Ho2 O12 Ho1 141.84(14) . 2 ?
C5 N1 C1 119.7(4) . . ?
C5 N1 Ho1 120.8(3) . . ?
C1 N1 Ho1 119.4(3) . . ?
C9 N2 C13 118.9(4) . . ?
C9 N2 Ho2 120.3(3) . . ?
C13 N2 Ho2 120.6(3) . . ?
N1 C1 C2 122.0(4) . . ?
N1 C1 C6 113.2(4) . . ?
C2 C1 C6 124.8(4) . . ?
C1 C2 C3 119.1(4) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 118.5(4) . . ?
C4 C3 C7 121.7(4) . . ?
C2 C3 C7 119.8(4) . . ?
C5 C4 C3 118.9(4) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 121.8(4) . . ?
N1 C5 C8 113.1(4) . . ?
C4 C5 C8 125.0(4) . . ?
O2 C6 O1 126.3(4) . . ?
O2 C6 C1 117.6(4) . . ?
O1 C6 C1 116.1(4) . . ?
O4 C7 O3 125.5(5) . . ?
O4 C7 C3 118.4(4) . . ?
O3 C7 C3 116.1(4) . . ?
O5 C8 O6 126.2(4) . . ?
O5 C8 C5 117.6(4) . . ?
O6 C8 C5 116.1(4) . . ?
N2 C9 C10 122.3(4) . . ?
N2 C9 C14 112.9(4) . . ?
C10 C9 C14 124.7(4) . . ?
C9 C10 C11 118.7(4) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C12 C11 C10 119.4(4) . . ?
C12 C11 C15 120.2(4) . . ?
C10 C11 C15 120.3(4) . . ?
C13 C12 C11 118.0(4) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
N2 C13 C12 122.7(4) . . ?
N2 C13 C16 112.2(4) . . ?
C12 C13 C16 125.1(4) . . ?
O8 C14 O7 125.4(4) . . ?
O8 C14 C9 118.2(4) . . ?
O7 C14 C9 116.4(4) . . ?
O10 C15 O9 126.8(4) . . ?
O10 C15 C11 116.4(4) . . ?
O9 C15 C11 116.8(4) . . ?
O11 C16 O12 120.5(4) . . ?
O11 C16 C13 121.5(4) . . ?
O12 C16 C13 117.9(4) . . ?
O11 C16 Ho1 61.0(2) . 2 ?
O12 C16 Ho1 59.8(2) . 2 ?
C13 C16 Ho1 175.5(3) . 2 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O10 Ho1 O1 C6 -158.8(4) 2_545 . . . ?
O1W Ho1 O1 C6 168.7(4) . . . . ?
O2W Ho1 O1 C6 -79.5(4) . . . . ?
O6 Ho1 O1 C6 2.1(4) . . . . ?
N1 Ho1 O1 C6 -3.3(4) . . . . ?
O12 Ho1 O1 C6 123.7(4) 2 . . . ?
O11 Ho1 O1 C6 70.2(4) 2 . . . ?
C16 Ho1 O1 C6 96.8(4) 2 . . . ?
O8 Ho2 O2 C6 -67.3(9) 4_545 . . . ?
O3 Ho2 O2 C6 -9.9(10) 4_545 . . . ?
O9 Ho2 O2 C6 18.7(8) 1_545 . . . ?
O5 Ho2 O2 C6 171.4(8) 6_565 . . . ?
O12 Ho2 O2 C6 91.7(9) . . . . ?
O7 Ho2 O2 C6 -140.0(9) . . . . ?
N2 Ho2 O2 C6 154.0(9) . . . . ?
O10 Ho1 O6 C8 140.9(3) 2_545 . . . ?
O1W Ho1 O6 C8 179.2(4) . . . . ?
O2W Ho1 O6 C8 76.7(4) . . . . ?
O1 Ho1 O6 C8 -6.7(4) . . . . ?
N1 Ho1 O6 C8 -1.2(3) . . . . ?
O12 Ho1 O6 C8 -111.8(4) 2 . . . ?
O11 Ho1 O6 C8 -76.0(4) 2 . . . ?
C16 Ho1 O6 C8 -91.7(4) 2 . . . ?
O2 Ho2 O7 C14 -61.2(3) . . . . ?
O8 Ho2 O7 C14 -144.2(4) 4_545 . . . ?
O3 Ho2 O7 C14 149.9(3) 4_545 . . . ?
O9 Ho2 O7 C14 -102.1(4) 1_545 . . . ?
O5 Ho2 O7 C14 91.7(3) 6_565 . . . ?
O12 Ho2 O7 C14 22.8(4) . . . . ?
N2 Ho2 O7 C14 16.1(3) . . . . ?
O2 Ho2 O12 C16 79.0(3) . . . . ?
O8 Ho2 O12 C16 147.4(4) 4_545 . . . ?
O3 Ho2 O12 C16 -135.4(3) 4_545 . . . ?
O9 Ho2 O12 C16 154.3(4) 1_545 . . . ?
O5 Ho2 O12 C16 -64.9(3) 6_565 . . . ?
O7 Ho2 O12 C16 1.6(4) . . . . ?
N2 Ho2 O12 C16 8.3(3) . . . . ?
O2 Ho2 O12 Ho1 -110.1(2) . . . 2 ?
O8 Ho2 O12 Ho1 -41.7(5) 4_545 . . 2 ?
O3 Ho2 O12 Ho1 35.5(2) 4_545 . . 2 ?
O9 Ho2 O12 Ho1 -34.8(2) 1_545 . . 2 ?
O5 Ho2 O12 Ho1 106.0(2) 6_565 . . 2 ?
O7 Ho2 O12 Ho1 172.50(18) . . . 2 ?
N2 Ho2 O12 Ho1 179.2(3) . . . 2 ?
O10 Ho1 N1 C5 -141.4(3) 2_545 . . . ?
O1W Ho1 N1 C5 3.5(4) . . . . ?
O2W Ho1 N1 C5 -87.3(3) . . . . ?
O1 Ho1 N1 C5 178.4(4) . . . . ?
O6 Ho1 N1 C5 2.9(3) . . . . ?
O12 Ho1 N1 C5 113.9(3) 2 . . . ?
O11 Ho1 N1 C5 89.2(3) 2 . . . ?
C16 Ho1 N1 C5 102.2(3) 2 . . . ?
O10 Ho1 N1 C1 40.5(4) 2_545 . . . ?
O1W Ho1 N1 C1 -174.5(3) . . . . ?
O2W Ho1 N1 C1 94.7(3) . . . . ?
O1 Ho1 N1 C1 0.4(3) . . . . ?
O6 Ho1 N1 C1 -175.1(4) . . . . ?
O12 Ho1 N1 C1 -64.1(4) 2 . . . ?
O11 Ho1 N1 C1 -88.8(3) 2 . . . ?
C16 Ho1 N1 C1 -75.8(3) 2 . . . ?
O2 Ho2 N2 C9 78.4(3) . . . . ?
O8 Ho2 N2 C9 18.4(4) 4_545 . . . ?
O3 Ho2 N2 C9 -115.8(3) 4_545 . . . ?
O9 Ho2 N2 C9 137.0(3) 1_545 . . . ?
O5 Ho2 N2 C9 -90.9(3) 6_565 . . . ?
O12 Ho2 N2 C9 179.1(4) . . . . ?
O7 Ho2 N2 C9 -6.7(3) . . . . ?
O2 Ho2 N2 C13 -106.4(3) . . . . ?
O8 Ho2 N2 C13 -166.4(3) 4_545 . . . ?
O3 Ho2 N2 C13 59.4(4) 4_545 . . . ?
O9 Ho2 N2 C13 -47.8(4) 1_545 . . . ?
O5 Ho2 N2 C13 84.4(3) 6_565 . . . ?
O12 Ho2 N2 C13 -5.6(3) . . . . ?
O7 Ho2 N2 C13 168.5(4) . . . . ?
C5 N1 C1 C2 1.2(7) . . . . ?
Ho1 N1 C1 C2 179.2(3) . . . . ?
C5 N1 C1 C6 -176.2(4) . . . . ?
Ho1 N1 C1 C6 1.8(5) . . . . ?
N1 C1 C2 C3 1.4(7) . . . . ?
C6 C1 C2 C3 178.5(4) . . . . ?
C1 C2 C3 C4 -2.2(7) . . . . ?
C1 C2 C3 C7 179.6(4) . . . . ?
C2 C3 C4 C5 0.5(7) . . . . ?
C7 C3 C4 C5 178.7(4) . . . . ?
C1 N1 C5 C4 -2.9(7) . . . . ?
Ho1 N1 C5 C4 179.1(3) . . . . ?
C1 N1 C5 C8 173.9(4) . . . . ?
Ho1 N1 C5 C8 -4.1(5) . . . . ?
C3 C4 C5 N1 2.0(7) . . . . ?
C3 C4 C5 C8 -174.4(4) . . . . ?
Ho2 O2 C6 O1 -56.3(11) . . . . ?
Ho2 O2 C6 C1 125.2(7) . . . . ?
Ho1 O1 C6 O2 -173.1(4) . . . . ?
Ho1 O1 C6 C1 5.5(6) . . . . ?
N1 C1 C6 O2 174.2(4) . . . . ?
C2 C1 C6 O2 -3.1(7) . . . . ?
N1 C1 C6 O1 -4.5(6) . . . . ?
C2 C1 C6 O1 178.2(5) . . . . ?
Ho2 O3 C7 O4 -46(2) 4 . . . ?
Ho2 O3 C7 C3 135.3(18) 4 . . . ?
C4 C3 C7 O4 36.4(7) . . . . ?
C2 C3 C7 O4 -145.4(5) . . . . ?
C4 C3 C7 O3 -144.9(5) . . . . ?
C2 C3 C7 O3 33.3(7) . . . . ?
Ho2 O5 C8 O6 -36.7(9) 6_566 . . . ?
Ho2 O5 C8 C5 141.9(4) 6_566 . . . ?
Ho1 O6 C8 O5 178.2(4) . . . . ?
Ho1 O6 C8 C5 -0.4(6) . . . . ?
N1 C5 C8 O5 -175.8(4) . . . . ?
C4 C5 C8 O5 0.9(7) . . . . ?
N1 C5 C8 O6 2.9(6) . . . . ?
C4 C5 C8 O6 179.6(4) . . . . ?
C13 N2 C9 C10 1.2(7) . . . . ?
Ho2 N2 C9 C10 176.5(3) . . . . ?
C13 N2 C9 C14 -176.0(4) . . . . ?
Ho2 N2 C9 C14 -0.7(5) . . . . ?
N2 C9 C10 C11 -1.1(7) . . . . ?
C14 C9 C10 C11 175.7(4) . . . . ?
C9 C10 C11 C12 0.1(7) . . . . ?
C9 C10 C11 C15 -178.0(4) . . . . ?
C10 C11 C12 C13 0.7(7) . . . . ?
C15 C11 C12 C13 178.9(4) . . . . ?
C9 N2 C13 C12 -0.2(7) . . . . ?
Ho2 N2 C13 C12 -175.5(3) . . . . ?
C9 N2 C13 C16 178.6(4) . . . . ?
Ho2 N2 C13 C16 3.3(5) . . . . ?
C11 C12 C13 N2 -0.7(7) . . . . ?
C11 C12 C13 C16 -179.3(4) . . . . ?
Ho2 O8 C14 O7 31.0(18) 4 . . . ?
Ho2 O8 C14 C9 -150.0(13) 4 . . . ?
Ho2 O7 C14 O8 156.2(4) . . . . ?
Ho2 O7 C14 C9 -22.8(5) . . . . ?
N2 C9 C14 O8 -164.5(4) . . . . ?
C10 C9 C14 O8 18.4(7) . . . . ?
N2 C9 C14 O7 14.5(6) . . . . ?
C10 C9 C14 O7 -162.5(4) . . . . ?
Ho1 O10 C15 O9 12.6(9) 2_565 . . . ?
Ho1 O10 C15 C11 -166.1(4) 2_565 . . . ?
Ho2 O9 C15 O10 -57.5(7) 1_565 . . . ?
Ho2 O9 C15 C11 121.3(4) 1_565 . . . ?
C12 C11 C15 O10 -9.8(7) . . . . ?
C10 C11 C15 O10 168.4(4) . . . . ?
C12 C11 C15 O9 171.3(4) . . . . ?
C10 C11 C15 O9 -10.5(7) . . . . ?
Ho1 O11 C16 O12 5.3(4) 2 . . . ?
Ho1 O11 C16 C13 -175.7(4) 2 . . . ?
Ho2 O12 C16 O11 169.0(3) . . . . ?
Ho1 O12 C16 O11 -5.4(4) 2 . . . ?
Ho2 O12 C16 C13 -10.0(5) . . . . ?
Ho1 O12 C16 C13 175.6(3) 2 . . . ?
Ho2 O12 C16 Ho1 174.4(3) . . . 2 ?
N2 C13 C16 O11 -175.1(4) . . . . ?
C12 C13 C16 O11 3.7(7) . . . . ?
N2 C13 C16 O12 3.9(6) . . . . ?
C12 C13 C16 O12 -177.4(4) . . . . ?
N2 C13 C16 Ho1 62(4) . . . 2 ?
C12 C13 C16 Ho1 -119(4) . . . 2 ?

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
O1W H1WA O11 0.85 1.91 2.755(5) 172.7 6_566
O1W H1WB O4 0.85 1.87 2.681(5) 158.3 3_445
O2W H2WA O4W' 0.85 1.78 2.62(2) 171.3 .
O2W H2WA O4W 0.85 1.92 2.759(19) 167.4 .
O2W H2WB O4 0.85 1.87 2.715(5) 173.9 7_556

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.145

