Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_sm94m 
_database_code_CSD                  177867

_journal_coden_Cambridge      182

loop_
_publ_author_name
'Gunnlaugsson, Thorfinnur'
'Davies, R.J.H.'
'Mulready, Sinead'
'Nieuwenhuyzen, Mark'
'Stevenson, Clarke S.'
'Viguier, Raomain'

_publ_contact_author_name     	'Dr Thorfinnur Gunnlaugsson'  
_publ_contact_author_address 
;
Chemistry
Trinity College Dublin
Dublin
Dublin 2
REPUBLIC OF IRELAND
;

_publ_contact_author_email       'GUNNLAUT@TCD.IE'

_publ_requested_journal       'Chemical Communications'


_publ_section_title		
;
Rapid hydrolytic cleavage of the mRNA model compound HPNP by glycine
based macrocyclic lanthanide ribonuclease mimics
; 

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C33 H48 Eu F15 K2 N8 O27 S5' 
_chemical_formula_weight          1664.25 

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' 
'S'  'S'   0.1246   0.1234 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'F'  'F'   0.0171   0.0103 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'K'  'K'   0.2009   0.2494 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Tetragonal 
_symmetry_space_group_name_H-M    P4/ncc 

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

_cell_length_a                    17.2721(8) 
_cell_length_b                    17.2721(8) 
_cell_length_c                    21.0475(14) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      6279.0(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     153(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.21 
_exptl_crystal_size_mid           0.28 
_exptl_crystal_size_min           0.33 
_exptl_crystal_density_meas       not_measured 
_exptl_crystal_density_diffrn     1.761 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3336 
_exptl_absorpt_coefficient_mu     1.425 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.804 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    SADABS 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       153(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   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             51944 
_diffrn_reflns_av_R_equivalents   0.0899 
_diffrn_reflns_av_sigmaI/netI     0.0408 
_diffrn_reflns_limit_h_min        -22 
_diffrn_reflns_limit_h_max        22 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          1.67 
_diffrn_reflns_theta_max          28.76 
_reflns_number_total              3844 
_reflns_number_gt                 2661 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 

_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
; 

_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+10.3423P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3844 
_refine_ls_number_parameters      287 
_refine_ls_number_restraints      221 
_refine_ls_R_factor_all           0.0731 
_refine_ls_R_factor_gt            0.0479 
_refine_ls_wR_factor_ref          0.1366 
_refine_ls_wR_factor_gt           0.1227 
_refine_ls_goodness_of_fit_ref    1.041 
_refine_ls_restrained_S_all       1.163 
_refine_ls_shift/su_max           0.786 
_refine_ls_shift/su_mean          0.030 

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 
K1 K 0.17162(6) -0.17162(6) 0.2500 0.0356(4) Uani 1 2 d S . . 
Eu1 Eu 0.2500 0.2500 0.31269(2) 0.02096(16) Uani 1 4 d S . . 
C1 C 0.3749(3) 0.2702(3) 0.1842(2) 0.0288(10) Uani 1 1 d . . . 
H1A H 0.4224 0.2920 0.1648 0.035 Uiso 1 1 calc R . . 
H1B H 0.3345 0.2683 0.1509 0.035 Uiso 1 1 calc R . . 
C2 C 0.3918(3) 0.1880(3) 0.2066(2) 0.0279(10) Uani 1 1 d . . . 
H2A H 0.4091 0.1565 0.1700 0.033 Uiso 1 1 calc R . . 
H2B H 0.4344 0.1892 0.2381 0.033 Uiso 1 1 calc R . . 
N3 N 0.3224(2) 0.1513(2) 0.23589(17) 0.0245(8) Uani 1 1 d . . . 
C4 C 0.3471(3) 0.0854(3) 0.2753(2) 0.0288(10) Uani 1 1 d . . . 
H4A H 0.3976 0.0974 0.2952 0.035 Uiso 1 1 calc R . . 
H4B H 0.3539 0.0392 0.2480 0.035 Uiso 1 1 calc R . . 
O5 O 0.24161(17) 0.11873(18) 0.34456(16) 0.0278(7) Uani 1 1 d . . . 
C5 C 0.2877(3) 0.0679(3) 0.3268(2) 0.0293(10) Uani 1 1 d . . . 
N7 N 0.2886(3) -0.0008(2) 0.3528(2) 0.0408(11) Uani 1 1 d . . . 
H7 H 0.3217 -0.0359 0.3392 0.049 Uiso 1 1 calc R . . 
C8 C 0.2361(3) -0.0199(3) 0.4038(3) 0.0432(13) Uani 1 1 d . A . 
H8A H 0.2352 0.0231 0.4349 0.052 Uiso 1 1 calc R . . 
H8B H 0.2549 -0.0668 0.4260 0.052 Uiso 1 1 calc R . . 
O9 O 0.1374(3) -0.0455(2) 0.32577(19) 0.0500(10) Uani 1 1 d . A . 
C9 C 0.1547(3) -0.0341(3) 0.3797(3) 0.0415(13) Uani 1 1 d . . . 
O10 O 0.1044(3) -0.0335(3) 0.4277(2) 0.0599(12) Uani 1 1 d . A . 
C11 C 0.0249(4) -0.0530(5) 0.4119(4) 0.086(3) Uani 1 1 d . . . 
H11A H -0.0045 -0.0616 0.4512 0.129 Uiso 1 1 calc R A . 
H11B H 0.0240 -0.1002 0.3861 0.129 Uiso 1 1 calc R . . 
H11C H 0.0015 -0.0104 0.3880 0.129 Uiso 1 1 calc R . . 
O11 O 0.061(2) -0.266(2) 0.3057(17) 0.026(9) Uani 0.235(6) 1 d PD A 1 
O12 O 0.1859(10) -0.327(2) 0.3160(15) 0.027(6) Uani 0.235(6) 1 d PD . 1 
O13 O 0.0732(17) -0.3871(11) 0.3596(8) 0.041(6) Uani 0.235(6) 1 d PD A 1 
S1 S 0.10867(7) -0.32039(7) 0.33958(6) 0.0306(4) Uani 0.235(6) 1 d PD A 1 
C1S C 0.1183(10) -0.2748(8) 0.4160(7) 0.025(6) Uani 0.235(6) 1 d PD A 1 
F11 F 0.1515(10) -0.2074(7) 0.4112(7) 0.031(4) Uani 0.235(6) 1 d PD A 1 
F12 F 0.0504(10) -0.2566(9) 0.4409(10) 0.048(5) Uani 0.235(6) 1 d PD A 1 
F13 F 0.1572(12) -0.3148(8) 0.4581(8) 0.041(5) Uani 0.235(6) 1 d PD A 1 
O11' O 0.0680(9) -0.2589(8) 0.3084(7) 0.045(4) Uani 0.765(6) 1 d PD A 2 
O12' O 0.1912(4) -0.3207(8) 0.3308(6) 0.039(3) Uani 0.765(6) 1 d PD . 2 
O13' O 0.0740(5) -0.3958(4) 0.3332(4) 0.056(2) Uani 0.765(6) 1 d PD A 2 
S1' S 0.10867(7) -0.32039(7) 0.33958(6) 0.0306(4) Uani 0.76 1 d PD A 2 
C1S' C 0.0981(7) -0.2980(9) 0.4227(5) 0.106(7) Uani 0.765(6) 1 d PD A 2 
F11' F 0.1302(8) -0.2307(9) 0.4353(6) 0.220(9) Uani 0.765(6) 1 d PD A 2 
F12' F 0.0244(6) -0.2966(10) 0.4391(4) 0.166(6) Uani 0.765(6) 1 d PD A 2 
F13' F 0.1338(6) -0.3501(9) 0.4578(4) 0.170(6) Uani 0.765(6) 1 d PD A 2 
O21 O 0.2500 0.2500 0.4288(3) 0.0331(15) Uiso 1 4 d SD . 1 
O22 O 0.2500 0.2500 0.5456(5) 0.090(4) Uiso 1 4 d SD . 1 
O23 O 0.3580(19) 0.298(2) 0.490(2) 0.38(5) Uiso 0.25 1 d PD B 1 
S2 S 0.2917(3) 0.2483(7) 0.4883(2) 0.0449(15) Uani 0.25 1 d PD . 1 
C2S C 0.3220(10) 0.1529(9) 0.4990(8) 0.045(5) Uiso 0.25 1 d PD C 1 
F21 F 0.3577(7) 0.1210(7) 0.4534(6) 0.048(3) Uiso 0.25 1 d PD C 1 
F22 F 0.3629(15) 0.1416(15) 0.5508(10) 0.151(12) Uiso 0.25 1 d PD C 1 
F23 F 0.2615(13) 0.1022(12) 0.5062(14) 0.176(14) Uiso 0.25 1 d PD C 1 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
K1 0.0342(5) 0.0342(5) 0.0384(9) 0.0011(5) 0.0011(5) -0.0027(6) 
Eu1 0.02187(18) 0.02187(18) 0.0192(2) 0.000 0.000 0.000 
C1 0.029(2) 0.035(2) 0.022(2) -0.0009(19) 0.0025(18) -0.0014(18) 
C2 0.025(2) 0.033(2) 0.026(2) -0.0029(19) 0.0038(18) 0.0004(18) 
N3 0.0261(18) 0.0275(18) 0.0199(19) -0.0029(15) 0.0003(15) 0.0023(14) 
C4 0.031(2) 0.029(2) 0.027(2) -0.0024(19) -0.0023(19) 0.0014(18) 
O5 0.0323(17) 0.0253(15) 0.0258(17) 0.0000(13) 0.0013(13) 0.0023(13) 
C5 0.035(3) 0.025(2) 0.028(3) 0.0010(18) -0.007(2) 0.0023(18) 
N7 0.054(3) 0.030(2) 0.039(3) 0.0085(19) 0.007(2) 0.012(2) 
C8 0.063(4) 0.033(3) 0.034(3) 0.013(2) 0.007(3) 0.005(2) 
O9 0.068(3) 0.046(2) 0.036(2) -0.0033(18) -0.0037(19) 0.007(2) 
C9 0.060(3) 0.029(3) 0.035(3) 0.007(2) 0.003(3) 0.010(2) 
O10 0.053(3) 0.083(3) 0.043(3) -0.002(2) 0.003(2) 0.002(2) 
C11 0.058(4) 0.130(8) 0.070(5) 0.000(5) -0.002(4) -0.003(5) 
O11 0.007(10) 0.042(17) 0.028(17) 0.016(13) -0.006(10) -0.009(10) 
O12 0.025(10) 0.048(13) 0.009(12) -0.013(9) -0.004(7) 0.019(9) 
O13 0.072(14) 0.036(10) 0.014(9) -0.009(8) 0.000(10) -0.018(8) 
S1 0.0302(6) 0.0350(7) 0.0267(7) 0.0011(5) 0.0020(5) 0.0024(5) 
C1S 0.030(13) 0.008(7) 0.036(15) -0.006(8) 0.020(10) 0.005(8) 
F11 0.055(9) 0.017(6) 0.021(7) -0.004(5) 0.008(6) -0.006(5) 
F12 0.055(12) 0.044(8) 0.046(10) -0.012(7) 0.033(9) 0.009(7) 
F13 0.071(13) 0.035(7) 0.018(8) -0.003(6) -0.005(7) -0.001(7) 
O11' 0.037(8) 0.044(6) 0.054(8) 0.006(5) -0.003(5) 0.002(5) 
O12' 0.032(3) 0.055(5) 0.030(6) -0.003(4) -0.001(3) 0.001(3) 
O13' 0.049(4) 0.036(3) 0.083(7) 0.002(4) -0.008(5) -0.007(3) 
S1' 0.0302(6) 0.0350(7) 0.0267(7) 0.0011(5) 0.0020(5) 0.0024(5) 
C1S' 0.066(8) 0.22(2) 0.027(6) -0.012(9) -0.002(5) 0.063(12) 
F11' 0.180(15) 0.31(2) 0.168(13) -0.197(13) -0.097(11) 0.112(13) 
F12' 0.087(7) 0.369(17) 0.042(4) 0.031(8) 0.029(4) 0.125(9) 
F13' 0.095(7) 0.380(19) 0.035(4) 0.058(8) 0.013(4) 0.127(10) 
S2 0.035(2) 0.080(4) 0.019(2) 0.006(4) -0.0008(18) -0.011(5) 

_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 
K1 O11' 2.643(17) . ? 
K1 O11' 2.643(17) 8 ? 
K1 O11 2.76(4) 8 ? 
K1 O11 2.76(4) . ? 
K1 O9 2.764(4) 8 ? 
K1 O9 2.764(4) . ? 
K1 O12 2.826(15) 2_545 ? 
K1 O12 2.826(15) 7_545 ? 
K1 O12' 2.919(7) 7_545 ? 
K1 O12' 2.919(7) 2_545 ? 
K1 O12 3.04(4) . ? 
K1 O12 3.04(4) 8 ? 
Eu1 O5 2.369(3) 2 ? 
Eu1 O5 2.369(3) 4 ? 
Eu1 O5 2.369(3) . ? 
Eu1 O5 2.369(3) 3 ? 
Eu1 O21 2.445(7) . ? 
Eu1 N3 2.661(4) 2 ? 
Eu1 N3 2.661(4) 4 ? 
Eu1 N3 2.661(4) 3 ? 
Eu1 N3 2.661(4) . ? 
Eu1 C5 3.225(4) 4 ? 
Eu1 C5 3.225(4) 2 ? 
Eu1 C5 3.225(4) 3 ? 
C1 N3 1.484(6) 3 ? 
C1 C2 1.523(6) . ? 
C2 N3 1.490(5) . ? 
N3 C4 1.471(6) . ? 
N3 C1 1.484(6) 4 ? 
C4 C5 1.522(7) . ? 
O5 C5 1.243(6) . ? 
C5 N7 1.309(6) . ? 
N7 C8 1.444(7) . ? 
C8 C9 1.515(8) . ? 
O9 C9 1.189(6) . ? 
C9 O10 1.332(7) . ? 
O10 C11 1.453(8) . ? 
O11 S1 1.436(14) . ? 
O12 S1 1.428(14) . ? 
O12 K1 2.826(15) 2_545 ? 
O13 S1 1.372(13) . ? 
S1 C1S 1.799(15) . ? 
C1S F11 1.301(14) . ? 
C1S F13 1.310(15) . ? 
C1S F12 1.322(14) . ? 
O12' K1 2.919(7) 2_545 ? 
C1S' F11' 1.315(13) . ? 
C1S' F13' 1.318(11) . ? 
C1S' F12' 1.320(11) . ? 
O21 S2 1.444(7) . ? 
O21 S2 1.444(7) 2 ? 
O21 S2 1.444(7) 3 ? 
O21 S2 1.444(7) 4 ? 
O22 S2 1.405(10) 2 ? 
O22 S2 1.405(10) 4 ? 
O22 S2 1.405(10) 3 ? 
O22 S2 1.405(10) . ? 
O23 C2S 0.49(5) 3 ? 
O23 F23 0.99(5) 3 ? 
O23 F21 1.35(3) 3 ? 
O23 S2 1.427(15) . ? 
O23 F22 1.70(5) 3 ? 
O23 S2 1.84(3) 3 ? 
S2 S2 1.020(7) 4 ? 
S2 S2 1.020(7) 3 ? 
S2 S2 1.442(10) 2 ? 
S2 C2S 1.61(2) 3 ? 
S2 C2S 1.744(16) . ? 
S2 O23 1.84(3) 4 ? 
S2 F23 1.88(2) 3 ? 
C2S O23 0.49(5) 4 ? 
C2S F21 1.268(14) . ? 
C2S F22 1.313(15) . ? 
C2S F23 1.371(16) . ? 
C2S S2 1.61(2) 4 ? 
F21 O23 1.35(3) 4 ? 
F22 O23 1.70(5) 4 ? 
F23 O23 0.99(5) 4 ? 
F23 S2 1.88(2) 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 
O11' K1 O11' 171.3(4) . 8 ? 
O11' K1 O11 171.2(3) . 8 ? 
O11' K1 O11 2.6(12) 8 8 ? 
O11' K1 O11 2.6(12) . . ? 
O11' K1 O11 171.2(3) 8 . ? 
O11 K1 O11 171.9(10) 8 . ? 
O11' K1 O9 81.8(2) . 8 ? 
O11' K1 O9 92.1(4) 8 8 ? 
O11 K1 O9 94.1(9) 8 8 ? 
O11 K1 O9 80.1(5) . 8 ? 
O11' K1 O9 92.1(4) . . ? 
O11' K1 O9 81.8(2) 8 . ? 
O11 K1 O9 80.1(5) 8 . ? 
O11 K1 O9 94.1(9) . . ? 
O9 K1 O9 89.73(18) 8 . ? 
O11' K1 O12 111.0(7) . 2_545 ? 
O11' K1 O12 74.7(7) 8 2_545 ? 
O11 K1 O12 72.6(11) 8 2_545 ? 
O11 K1 O12 112.8(8) . 2_545 ? 
O9 K1 O12 166.2(7) 8 2_545 ? 
O9 K1 O12 84.7(9) . 2_545 ? 
O11' K1 O12 74.7(7) . 7_545 ? 
O11' K1 O12 111.0(7) 8 7_545 ? 
O11 K1 O12 112.8(8) 8 7_545 ? 
O11 K1 O12 72.6(11) . 7_545 ? 
O9 K1 O12 84.7(9) 8 7_545 ? 
O9 K1 O12 166.2(7) . 7_545 ? 
O12 K1 O12 103.4(17) 2_545 7_545 ? 
O11' K1 O12' 80.7(4) . 7_545 ? 
O11' K1 O12' 104.6(3) 8 7_545 ? 
O11 K1 O12' 106.5(5) 8 7_545 ? 
O11 K1 O12' 78.5(9) . 7_545 ? 
O9 K1 O12' 82.8(3) 8 7_545 ? 
O9 K1 O12' 170.2(3) . 7_545 ? 
O12 K1 O12' 104.0(6) 2_545 7_545 ? 
O12 K1 O12' 6.6(8) 7_545 7_545 ? 
O11' K1 O12' 104.6(3) . 2_545 ? 
O11' K1 O12' 80.7(4) 8 2_545 ? 
O11 K1 O12' 78.5(9) 8 2_545 ? 
O11 K1 O12' 106.5(5) . 2_545 ? 
O9 K1 O12' 170.2(3) 8 2_545 ? 
O9 K1 O12' 82.8(3) . 2_545 ? 
O12 K1 O12' 6.6(8) 2_545 2_545 ? 
O12 K1 O12' 104.0(6) 7_545 2_545 ? 
O12' K1 O12' 105.4(6) 7_545 2_545 ? 
O11' K1 O12 48.5(4) . . ? 
O11' K1 O12 140.0(4) 8 . ? 
O11 K1 O12 139.1(8) 8 . ? 
O11 K1 O12 48.8(5) . . ? 
O9 K1 O12 121.2(5) 8 . ? 
O9 K1 O12 116.8(5) . . ? 
O12 K1 O12 72.5(11) 2_545 . ? 
O12 K1 O12 56.8(12) 7_545 . ? 
O12' K1 O12 62.9(5) 7_545 . ? 
O12' K1 O12 68.1(5) 2_545 . ? 
O11' K1 O12 140.0(4) . 8 ? 
O11' K1 O12 48.5(4) 8 8 ? 
O11 K1 O12 48.8(5) 8 8 ? 
O11 K1 O12 139.1(8) . 8 ? 
O9 K1 O12 116.8(5) 8 8 ? 
O9 K1 O12 121.2(5) . 8 ? 
O12 K1 O12 56.8(12) 2_545 8 ? 
O12 K1 O12 72.5(11) 7_545 8 ? 
O12' K1 O12 68.1(5) 7_545 8 ? 
O12' K1 O12 62.9(5) 2_545 8 ? 
O12 K1 O12 93.7(5) . 8 ? 
O5 Eu1 O5 85.40(4) 2 4 ? 
O5 Eu1 O5 147.10(16) 2 . ? 
O5 Eu1 O5 85.40(4) 4 . ? 
O5 Eu1 O5 85.40(4) 2 3 ? 
O5 Eu1 O5 147.10(16) 4 3 ? 
O5 Eu1 O5 85.40(4) . 3 ? 
O5 Eu1 O21 73.55(8) 2 . ? 
O5 Eu1 O21 73.55(8) 4 . ? 
O5 Eu1 O21 73.55(8) . . ? 
O5 Eu1 O21 73.55(8) 3 . ? 
O5 Eu1 N3 65.65(11) 2 2 ? 
O5 Eu1 N3 71.52(11) 4 2 ? 
O5 Eu1 N3 139.14(11) . 2 ? 
O5 Eu1 N3 131.37(11) 3 2 ? 
O21 Eu1 N3 127.40(8) . 2 ? 
O5 Eu1 N3 131.37(11) 2 4 ? 
O5 Eu1 N3 65.65(11) 4 4 ? 
O5 Eu1 N3 71.52(11) . 4 ? 
O5 Eu1 N3 139.14(11) 3 4 ? 
O21 Eu1 N3 127.40(8) . 4 ? 
N3 Eu1 N3 68.35(8) 2 4 ? 
O5 Eu1 N3 71.52(11) 2 3 ? 
O5 Eu1 N3 139.14(11) 4 3 ? 
O5 Eu1 N3 131.37(11) . 3 ? 
O5 Eu1 N3 65.65(11) 3 3 ? 
O21 Eu1 N3 127.40(8) . 3 ? 
N3 Eu1 N3 68.35(8) 2 3 ? 
N3 Eu1 N3 105.20(16) 4 3 ? 
O5 Eu1 N3 139.14(11) 2 . ? 
O5 Eu1 N3 131.37(11) 4 . ? 
O5 Eu1 N3 65.65(11) . . ? 
O5 Eu1 N3 71.52(11) 3 . ? 
O21 Eu1 N3 127.40(8) . . ? 
N3 Eu1 N3 105.20(16) 2 . ? 
N3 Eu1 N3 68.35(8) 4 . ? 
N3 Eu1 N3 68.35(8) 3 . ? 
O5 Eu1 C5 103.12(12) 2 4 ? 
O5 Eu1 C5 18.75(12) 4 4 ? 
O5 Eu1 C5 73.80(11) . 4 ? 
O5 Eu1 C5 153.50(11) 3 4 ? 
O21 Eu1 C5 84.73(8) . 4 ? 
N3 Eu1 C5 74.16(11) 2 4 ? 
N3 Eu1 C5 48.42(12) 4 4 ? 
N3 Eu1 C5 140.83(12) 3 4 ? 
N3 Eu1 C5 112.62(12) . 4 ? 
O5 Eu1 C5 18.75(12) 2 2 ? 
O5 Eu1 C5 73.80(11) 4 2 ? 
O5 Eu1 C5 153.50(11) . 2 ? 
O5 Eu1 C5 103.12(12) 3 2 ? 
O21 Eu1 C5 84.73(8) . 2 ? 
N3 Eu1 C5 48.42(12) 2 2 ? 
N3 Eu1 C5 112.62(12) 4 2 ? 
N3 Eu1 C5 74.16(11) 3 2 ? 
N3 Eu1 C5 140.83(12) . 2 ? 
C5 Eu1 C5 89.517(16) 4 2 ? 
O5 Eu1 C5 73.80(11) 2 3 ? 
O5 Eu1 C5 153.50(11) 4 3 ? 
O5 Eu1 C5 103.12(12) . 3 ? 
O5 Eu1 C5 18.75(12) 3 3 ? 
O21 Eu1 C5 84.73(8) . 3 ? 
N3 Eu1 C5 112.62(12) 2 3 ? 
N3 Eu1 C5 140.83(12) 4 3 ? 
N3 Eu1 C5 48.42(12) 3 3 ? 
N3 Eu1 C5 74.15(11) . 3 ? 
C5 Eu1 C5 169.46(17) 4 3 ? 
C5 Eu1 C5 89.517(16) 2 3 ? 
N3 C1 C2 113.4(4) 3 . ? 
N3 C2 C1 111.7(4) . . ? 
C4 N3 C1 110.7(4) . 4 ? 
C4 N3 C2 109.2(3) . . ? 
C1 N3 C2 108.4(3) 4 . ? 
C4 N3 Eu1 106.8(3) . . ? 
C1 N3 Eu1 110.8(3) 4 . ? 
C2 N3 Eu1 110.9(3) . . ? 
N3 C4 C5 111.1(4) . . ? 
C5 O5 Eu1 123.4(3) . . ? 
O5 C5 N7 121.5(5) . . ? 
O5 C5 C4 120.4(4) . . ? 
N7 C5 C4 118.1(4) . . ? 
O5 C5 Eu1 37.8(2) . . ? 
N7 C5 Eu1 157.8(4) . . ? 
C4 C5 Eu1 82.9(2) . . ? 
C5 N7 C8 120.7(4) . . ? 
N7 C8 C9 111.8(5) . . ? 
C9 O9 K1 128.8(4) . . ? 
O9 C9 O10 124.1(6) . . ? 
O9 C9 C8 125.5(5) . . ? 
O10 C9 C8 110.4(5) . . ? 
C9 O10 C11 116.2(5) . . ? 
S1 O11 K1 102(2) . . ? 
S1 O12 K1 170(2) . 2_545 ? 
S1 O12 K1 90.5(17) . . ? 
K1 O12 K1 81.4(9) 2_545 . ? 
O13 S1 O12 117.0(17) . . ? 
O13 S1 O11 116.8(19) . . ? 
O12 S1 O11 114.4(18) . . ? 
O13 S1 C1S 97.7(8) . . ? 
O12 S1 C1S 105.2(13) . . ? 
O11 S1 C1S 102.0(17) . . ? 
O13 S1 K1 163.2(8) . . ? 
O12 S1 K1 64.4(17) . . ? 
O11 S1 K1 53.4(18) . . ? 
C1S S1 K1 97.8(5) . . ? 
F11 C1S F13 107.4(14) . . ? 
F11 C1S F12 102.1(13) . . ? 
F13 C1S F12 108.2(16) . . ? 
F11 C1S S1 111.3(11) . . ? 
F13 C1S S1 114.9(12) . . ? 
F12 C1S S1 112.2(13) . . ? 
K1 O12' K1 78.9(3) 2_545 . ? 
F11' C1S' F13' 107.0(12) . . ? 
F11' C1S' F12' 109.8(12) . . ? 
F13' C1S' F12' 108.5(10) . . ? 
S2 O21 S2 59.9(5) . 2 ? 
S2 O21 S2 41.4(3) . 3 ? 
S2 O21 S2 41.4(3) 2 3 ? 
S2 O21 S2 41.4(3) . 4 ? 
S2 O21 S2 41.4(3) 2 4 ? 
S2 O21 S2 59.9(5) 3 4 ? 
S2 O21 Eu1 150.0(2) . . ? 
S2 O21 Eu1 150.0(2) 2 . ? 
S2 O21 Eu1 150.0(2) 3 . ? 
S2 O21 Eu1 150.0(2) 4 . ? 
S2 O22 S2 42.5(4) 2 4 ? 
S2 O22 S2 42.5(4) 2 3 ? 
S2 O22 S2 61.7(6) 4 3 ? 
S2 O22 S2 61.7(6) 2 . ? 
S2 O22 S2 42.5(4) 4 . ? 
S2 O22 S2 42.5(4) 3 . ? 
C2S O23 F23 133(7) 3 3 ? 
C2S O23 F21 70(4) 3 3 ? 
F23 O23 F21 120(3) 3 3 ? 
C2S O23 S2 102(4) 3 . ? 
F23 O23 S2 101(3) 3 . ? 
F21 O23 S2 131(3) 3 . ? 
C2S O23 F22 33(4) 3 3 ? 
F23 O23 F22 99(3) 3 3 ? 
F21 O23 F22 85(2) 3 3 ? 
S2 O23 F22 115(3) . 3 ? 
C2S O23 S2 71(4) 3 3 ? 
F23 O23 S2 132(3) 3 3 ? 
F21 O23 S2 107(3) 3 3 ? 
S2 O23 S2 33.5(9) . 3 ? 
F22 O23 S2 93(2) 3 3 ? 
S2 S2 S2 90.000(1) 4 3 ? 
S2 S2 O22 68.7(2) 4 . ? 
S2 S2 O22 68.7(2) 3 . ? 
S2 S2 O23 174(2) 4 . ? 
S2 S2 O23 96(2) 3 . ? 
O22 S2 O23 111.8(19) . . ? 
S2 S2 S2 45.000(3) 4 2 ? 
S2 S2 S2 45.000(2) 3 2 ? 
O22 S2 S2 59.1(3) . 2 ? 
O23 S2 S2 141(2) . 2 ? 
S2 S2 O21 69.32(16) 4 . ? 
S2 S2 O21 69.32(16) 3 . ? 
O22 S2 O21 119.2(5) . . ? 
O23 S2 O21 114.6(18) . . ? 
S2 S2 O21 60.0(2) 2 . ? 
S2 S2 C2S 166.9(11) 4 3 ? 
S2 S2 C2S 79.8(13) 3 3 ? 
O22 S2 C2S 99.7(8) . 3 ? 
O23 S2 C2S 17.5(19) . 3 ? 
S2 S2 C2S 124.3(13) 2 3 ? 
O21 S2 C2S 113.8(8) . 3 ? 
S2 S2 C2S 65.1(13) 4 . ? 
S2 S2 C2S 153.9(12) 3 . ? 
O22 S2 C2S 93.5(7) . . ? 
O23 S2 C2S 108.6(19) . . ? 
S2 S2 C2S 109.7(12) 2 . ? 
O21 S2 C2S 106.3(8) . . ? 
C2S S2 C2S 123.4(5) 3 . ? 
S2 S2 O23 50.5(15) 4 4 ? 
S2 S2 O23 140.5(15) 3 4 ? 
O22 S2 O23 91.6(13) . 4 ? 
O23 S2 O23 123.4(9) . 4 ? 
S2 S2 O23 95.5(15) 2 4 ? 
O21 S2 O23 94.0(14) . 4 ? 
C2S S2 O23 138.9(13) 3 4 ? 
C2S S2 O23 15.6(14) . 4 ? 
S2 S2 F23 142.8(15) 4 3 ? 
S2 S2 F23 124.8(15) 3 3 ? 
O22 S2 F23 108.9(10) . 3 ? 
O23 S2 F23 30.9(19) . 3 ? 
S2 S2 F23 165.1(12) 2 3 ? 
O21 S2 F23 131.0(10) . 3 ? 
C2S S2 F23 45.4(7) 3 3 ? 
C2S S2 F23 78.3(7) . 3 ? 
O23 S2 F23 93.5(15) 4 3 ? 
O23 C2S F21 88(5) 4 . ? 
O23 C2S F22 135(5) 4 . ? 
F21 C2S F22 107.6(17) . . ? 
O23 C2S F23 32(5) 4 . ? 
F21 C2S F23 100.2(16) . . ? 
F22 C2S F23 102.9(17) . . ? 
O23 C2S S2 60(3) 4 4 ? 
F21 C2S S2 122.5(13) . 4 ? 
F22 C2S S2 129.1(16) . 4 ? 
F23 C2S S2 78.1(13) . 4 ? 
O23 C2S S2 93(3) 4 . ? 
F21 C2S S2 117.3(12) . . ? 
F22 C2S S2 114.1(15) . . ? 
F23 C2S S2 112.9(14) . . ? 
S2 C2S S2 35.1(4) 4 . ? 
C2S F21 O23 22(2) . 4 ? 
C2S F22 O23 11.9(16) . 4 ? 
O23 F23 C2S 15(3) 4 . ? 
O23 F23 S2 48.0(14) 4 4 ? 
C2S F23 S2 56.6(11) . 4 ? 

_diffrn_measured_fraction_theta_max    0.939 
_diffrn_reflns_theta_full              28.76 
_diffrn_measured_fraction_theta_full   0.939 
_refine_diff_density_max    1.259 
_refine_diff_density_min   -1.006 
_refine_diff_density_rms    0.123