# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

 
data_Gd2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C48 H78 Cl6 Gd2 N2 O16' 
_chemical_formula_weight          1466.31
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Gd'  'Gd'  -0.1653   3.9035 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting           'Monoclinic'
_symmetry_space_group_name_H-M   'P2(1)/c'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    10.800(5) 
_cell_length_b                    15.574(5) 
_cell_length_c                    18.284(5) 
_cell_angle_alpha                 90.000(5) 
_cell_angle_beta                  95.473(5) 
_cell_angle_gamma                 90.000(5) 
_cell_volume                      3061.3(19) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     8543
_cell_measurement_theta_min        2.30
_cell_measurement_theta_max       28.26
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour            'colorless' 
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.125 
_exptl_crystal_size_min           0.105
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.591 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1476 
_exptl_absorpt_coefficient_mu     2.471 
_exptl_absorpt_correction_type    'empirical' 
_exptl_absorpt_correction_T_min   0.700446 
_exptl_absorpt_correction_T_max   1.0 
_exptl_absorpt_process_details    'sadabs' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             15200 
_diffrn_reflns_av_R_equivalents   0.0338 
_diffrn_reflns_av_sigmaI/netI     0.0358 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          4.08 
_diffrn_reflns_theta_max          25.02 
_reflns_number_total              5339 
_reflns_number_gt                 4835 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection      'Bruker SMART'
_computing_cell_refinement      'Bruker SMART'
_computing_data_reduction       'Bruker SAINT'
_computing_structure_solution   'Bruker SHELXTL'
_computing_structure_refinement 'Bruker SHELXTL'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
 
_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)+(0.0349P)²+7.5585P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5339 
_refine_ls_number_parameters      332 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0374 
_refine_ls_R_factor_gt            0.0336 
_refine_ls_wR_factor_ref          0.0822 
_refine_ls_wR_factor_gt           0.0794 
_refine_ls_goodness_of_fit_ref    1.050 
_refine_ls_restrained_S_all       1.050 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Gd1 Gd 0.150643(16) 1.048032(12) 0.531501(9) 0.01771(8) Uani 1 1 d . . . 
Cl1 Cl 0.54360(14) 0.81651(10) 0.79781(7) 0.0580(4) Uani 1 1 d . . . 
Cl2 Cl 0.4609(2) 0.94987(9) 0.88991(9) 0.0738(5) Uani 1 1 d . . . 
Cl3 Cl 0.31131(16) 0.79971(16) 0.86024(10) 0.0884(6) Uani 1 1 d . . . 
O1 O 0.0453(2) 0.91505(17) 0.52448(14) 0.0207(6) Uani 1 1 d . . . 
O2 O -0.0555(3) 0.80203(18) 0.43016(15) 0.0273(6) Uani 1 1 d . . . 
O3 O 0.3476(3) 0.9933(2) 0.48086(16) 0.0273(6) Uani 1 1 d D . . 
O4 O 0.3037(3) 1.12072(19) 0.61208(15) 0.0258(6) Uani 1 1 d D . . 
O5 O 0.0509(2) 1.03966(17) 0.64222(14) 0.0215(6) Uani 1 1 d . . . 
O6 O -0.1410(2) 1.00374(19) 0.59755(14) 0.0253(6) Uani 1 1 d . . . 
O7 O 0.2235(3) 1.16047(18) 0.45945(15) 0.0271(6) Uani 1 1 d . . . 
O8 O 0.3711(3) 1.2345(2) 0.52431(16) 0.0352(7) Uani 1 1 d . . . 
N1 N 0.2945(3) 0.9425(2) 0.62048(18) 0.0228(7) Uani 1 1 d . . . 
C1 C 0.0853(4) 0.8336(2) 0.5319(2) 0.0232(9) Uani 1 1 d . . . 
C2 C 0.1728(3) 0.8075(3) 0.5884(2) 0.0213(8) Uani 1 1 d . . . 
C3 C 0.2141(4) 0.7219(3) 0.5908(2) 0.0247(9) Uani 1 1 d . . . 
H3 H 0.2739 0.7053 0.6281 0.030 Uiso 1 1 calc R . . 
C4 C 0.1688(4) 0.6616(3) 0.5396(2) 0.0266(9) Uani 1 1 d . . . 
C5 C 0.0774(4) 0.6875(3) 0.4847(2) 0.0265(9) Uani 1 1 d . . . 
H5 H 0.0442 0.6477 0.4503 0.032 Uiso 1 1 calc R . . 
C6 C 0.0361(4) 0.7708(3) 0.4810(2) 0.0230(8) Uani 1 1 d . . . 
C7 C 0.2153(5) 0.5699(3) 0.5426(3) 0.0367(11) Uani 1 1 d . . . 
H7A H 0.2660 0.5606 0.5880 0.055 Uiso 1 1 calc R . . 
H7B H 0.2638 0.5596 0.5021 0.055 Uiso 1 1 calc R . . 
H7C H 0.1457 0.5314 0.5396 0.055 Uiso 1 1 calc R . . 
C8 C -0.0997(4) 0.7445(3) 0.3723(2) 0.0339(10) Uani 1 1 d . . . 
H8A H -0.0304 0.7227 0.3488 0.051 Uiso 1 1 calc R . . 
H8B H -0.1550 0.7747 0.3369 0.051 Uiso 1 1 calc R . . 
H8C H -0.1433 0.6977 0.3924 0.051 Uiso 1 1 calc R . . 
C9 C -0.0619(4) 1.0259(3) 0.6492(2) 0.0221(8) Uani 1 1 d . . . 
C10 C -0.1052(4) 1.0356(3) 0.7264(2) 0.0281(9) Uani 1 1 d . . . 
C11 C -0.2473(5) 1.0294(4) 0.7241(3) 0.0490(14) Uani 1 1 d . . . 
H11A H -0.2715 1.0313 0.7732 0.073 Uiso 1 1 calc R . . 
H11B H -0.2749 0.9765 0.7012 0.073 Uiso 1 1 calc R . . 
H11C H -0.2845 1.0768 0.6964 0.073 Uiso 1 1 calc R . . 
C12 C -0.0620(5) 1.1216(4) 0.7585(3) 0.0473(13) Uani 1 1 d . . . 
H12A H -0.1006 1.1671 0.7291 0.071 Uiso 1 1 calc R . . 
H12B H 0.0267 1.1258 0.7588 0.071 Uiso 1 1 calc R . . 
H12C H -0.0848 1.1262 0.8078 0.071 Uiso 1 1 calc R . . 
C13 C -0.0449(6) 0.9627(4) 0.7734(3) 0.0536(15) Uani 1 1 d . . . 
H13A H 0.0440 0.9675 0.7755 0.080 Uiso 1 1 calc R . . 
H13B H -0.0705 0.9084 0.7520 0.080 Uiso 1 1 calc R . . 
H13C H -0.0704 0.9663 0.8222 0.080 Uiso 1 1 calc R . . 
C14 C 0.2202(4) 0.8700(3) 0.6472(2) 0.0228(8) Uani 1 1 d . . . 
H14A H 0.1498 0.8936 0.6696 0.027 Uiso 1 1 calc R . . 
H14B H 0.2714 0.8391 0.6850 0.027 Uiso 1 1 calc R . . 
C15 C 0.3368(4) 0.9959(3) 0.6851(2) 0.0263(9) Uani 1 1 d . . . 
H15A H 0.3985 0.9644 0.7165 0.032 Uiso 1 1 calc R . . 
H15B H 0.2667 1.0075 0.7132 0.032 Uiso 1 1 calc R . . 
C16 C 0.3922(4) 1.0799(3) 0.6630(2) 0.0295(9) Uani 1 1 d . . . 
H16A H 0.4109 1.1161 0.7058 0.035 Uiso 1 1 calc R . . 
H16B H 0.4687 1.0696 0.6406 0.035 Uiso 1 1 calc R . . 
C17 C 0.4036(4) 0.9089(3) 0.5856(2) 0.0309(10) Uani 1 1 d . . . 
H17A H 0.4223 0.8512 0.6033 0.037 Uiso 1 1 calc R . . 
H17B H 0.4754 0.9447 0.5997 0.037 Uiso 1 1 calc R . . 
C18 C 0.3803(4) 0.9073(3) 0.5029(2) 0.0302(10) Uani 1 1 d . . . 
H18A H 0.4544 0.8890 0.4812 0.036 Uiso 1 1 calc R . . 
H18B H 0.3130 0.8680 0.4876 0.036 Uiso 1 1 calc R . . 
C19 C 0.2972(4) 1.2229(3) 0.4671(2) 0.0243(9) Uani 1 1 d . . . 
C20 C 0.2953(5) 1.2895(3) 0.4060(3) 0.0410(6) Uani 1 1 d . . . 
C21 C 0.2404(5) 1.2512(3) 0.3336(3) 0.0410(6) Uani 1 1 d . . . 
H21A H 0.1571 1.2319 0.3385 0.061 Uiso 1 1 calc R . . 
H21B H 0.2904 1.2036 0.3208 0.061 Uiso 1 1 calc R . . 
H21C H 0.2389 1.2940 0.2957 0.061 Uiso 1 1 calc R . . 
C22 C 0.4260(5) 1.3233(3) 0.3971(3) 0.0410(6) Uani 1 1 d . . . 
H22A H 0.4209 1.3694 0.3622 0.061 Uiso 1 1 calc R . . 
H22B H 0.4759 1.2778 0.3800 0.061 Uiso 1 1 calc R . . 
H22C H 0.4632 1.3438 0.4436 0.061 Uiso 1 1 calc R . . 
C23 C 0.2145(5) 1.3636(3) 0.4276(3) 0.0410(6) Uani 1 1 d . . . 
H23A H 0.1320 1.3431 0.4326 0.061 Uiso 1 1 calc R . . 
H23B H 0.2114 1.4072 0.3902 0.061 Uiso 1 1 calc R . . 
H23C H 0.2493 1.3874 0.4734 0.061 Uiso 1 1 calc R . . 
C24 C 0.4614(4) 0.8391(3) 0.8739(2) 0.0379(11) Uani 1 1 d . . . 
H24 H 0.5039 0.8108 0.9171 0.046 Uiso 1 1 calc R . . 
H111 H 0.330(5) 1.163(2) 0.590(3) 0.044(15) Uiso 1 1 d D . . 
H113 H 0.313(5) 0.990(4) 0.4387(16) 0.063(19) Uiso 1 1 d D . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Gd1 O1 2.333(3) 3_576 ? 
Gd1 O1 2.361(3) . ? 
Gd1 O7 2.370(3) . ? 
Gd1 O5 2.386(3) . ? 
Gd1 O4 2.391(3) . ? 
Gd1 O6 2.486(3) 3_576 ? 
Gd1 O3 2.546(3) . ? 
Gd1 O2 2.672(3) 3_576 ? 
Gd1 N1 2.698(3) . ? 
Gd1 Gd1 3.6658(14) 3_576 ? 
Cl1 C24 1.755(5) . ? 
Cl2 C24 1.750(5) . ? 
Cl3 C24 1.729(5) . ? 
O1 C1 1.342(5) . ? 
O1 Gd1 2.333(3) 3_576 ? 
O2 C6 1.380(5) . ? 
O2 C8 1.433(5) . ? 
O2 Gd1 2.672(3) 3_576 ? 
O3 C18 1.434(5) . ? 
O4 C16 1.419(5) . ? 
O5 C9 1.256(5) . ? 
O6 C9 1.260(5) . ? 
O6 Gd1 2.486(3) 3_576 ? 
O7 C19 1.256(5) . ? 
O8 C19 1.267(5) . ? 
N1 C15 1.482(5) . ? 
N1 C17 1.487(5) . ? 
N1 C14 1.493(5) . ? 
C1 C2 1.392(5) . ? 
C1 C6 1.419(6) . ? 
C2 C3 1.405(6) . ? 
C2 C14 1.504(6) . ? 
C3 C4 1.381(6) . ? 
C4 C5 1.399(6) . ? 
C4 C7 1.513(6) . ? 
C5 C6 1.371(6) . ? 
C9 C10 1.535(5) . ? 
C10 C12 1.518(6) . ? 
C10 C13 1.532(7) . ? 
C10 C11 1.534(6) . ? 
C15 C16 1.510(6) . ? 
C17 C18 1.508(6) . ? 
C19 C20 1.524(6) . ? 
C20 C21 1.519(7) . ? 
C20 C23 1.521(7) . ? 
C20 C22 1.529(7) . ? 
 
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 
O1 Gd1 O1 77.29(10) 3_576 . ? 
O1 Gd1 O7 84.79(10) 3_576 . ? 
O1 Gd1 O7 143.30(9) . . ? 
O1 Gd1 O5 85.51(9) 3_576 . ? 
O1 Gd1 O5 75.16(9) . . ? 
O7 Gd1 O5 135.45(9) . . ? 
O1 Gd1 O4 134.28(10) 3_576 . ? 
O1 Gd1 O4 138.59(9) . . ? 
O7 Gd1 O4 75.29(10) . . ? 
O5 Gd1 O4 81.06(10) . . ? 
O1 Gd1 O6 73.11(9) 3_576 3_576 ? 
O1 Gd1 O6 71.79(9) . 3_576 ? 
O7 Gd1 O6 72.44(10) . 3_576 ? 
O5 Gd1 O6 143.72(9) . 3_576 ? 
O4 Gd1 O6 134.60(9) . 3_576 ? 
O1 Gd1 O3 132.62(9) 3_576 . ? 
O1 Gd1 O3 95.85(10) . . ? 
O7 Gd1 O3 73.26(10) . . ? 
O5 Gd1 O3 138.66(9) . . ? 
O4 Gd1 O3 80.22(10) . . ? 
O6 Gd1 O3 60.48(9) 3_576 . ? 
O1 Gd1 O2 62.89(9) 3_576 3_576 ? 
O1 Gd1 O2 125.84(9) . 3_576 ? 
O7 Gd1 O2 69.91(10) . 3_576 ? 
O5 Gd1 O2 66.98(9) . 3_576 ? 
O4 Gd1 O2 71.64(10) . 3_576 ? 
O6 Gd1 O2 123.38(9) 3_576 3_576 ? 
O3 Gd1 O2 138.02(10) . 3_576 ? 
O1 Gd1 N1 149.39(10) 3_576 . ? 
O1 Gd1 N1 75.23(10) . . ? 
O7 Gd1 N1 125.64(10) . . ? 
O5 Gd1 N1 74.67(10) . . ? 
O4 Gd1 N1 65.97(10) . . ? 
O6 Gd1 N1 110.13(10) 3_576 . ? 
O3 Gd1 N1 64.06(10) . . ? 
O2 Gd1 N1 126.02(9) 3_576 . ? 
O1 Gd1 Gd1 38.92(7) 3_576 3_576 ? 
O1 Gd1 Gd1 38.37(6) . 3_576 ? 
O7 Gd1 Gd1 117.30(7) . 3_576 ? 
O5 Gd1 Gd1 77.60(7) . 3_576 ? 
O4 Gd1 Gd1 158.03(7) . 3_576 ? 
O6 Gd1 Gd1 67.28(6) 3_576 3_576 ? 
O3 Gd1 Gd1 119.77(7) . 3_576 ? 
O2 Gd1 Gd1 95.00(7) 3_576 3_576 ? 
N1 Gd1 Gd1 112.55(7) . 3_576 ? 
C1 O1 Gd1 123.2(2) . 3_576 ? 
C1 O1 Gd1 132.4(2) . . ? 
Gd1 O1 Gd1 102.71(10) 3_576 . ? 
C6 O2 C8 116.4(3) . . ? 
C6 O2 Gd1 113.6(2) . 3_576 ? 
C8 O2 Gd1 129.1(2) . 3_576 ? 
C18 O3 Gd1 113.7(2) . . ? 
C16 O4 Gd1 125.1(2) . . ? 
C9 O5 Gd1 128.1(2) . . ? 
C9 O6 Gd1 139.9(2) . 3_576 ? 
C19 O7 Gd1 138.6(3) . . ? 
C15 N1 C17 110.1(3) . . ? 
C15 N1 C14 107.4(3) . . ? 
C17 N1 C14 110.3(3) . . ? 
C15 N1 Gd1 104.7(2) . . ? 
C17 N1 Gd1 112.9(2) . . ? 
C14 N1 Gd1 111.2(2) . . ? 
O1 C1 C2 122.7(4) . . ? 
O1 C1 C6 119.2(3) . . ? 
C2 C1 C6 118.0(4) . . ? 
C1 C2 C3 119.5(4) . . ? 
C1 C2 C14 120.1(3) . . ? 
C3 C2 C14 120.4(3) . . ? 
C4 C3 C2 122.2(4) . . ? 
C3 C4 C5 118.1(4) . . ? 
C3 C4 C7 121.5(4) . . ? 
C5 C4 C7 120.4(4) . . ? 
C6 C5 C4 120.8(4) . . ? 
C5 C6 O2 125.1(4) . . ? 
C5 C6 C1 121.4(4) . . ? 
O2 C6 C1 113.5(3) . . ? 
O5 C9 O6 124.4(4) . . ? 
O5 C9 C10 117.5(3) . . ? 
O6 C9 C10 118.2(3) . . ? 
C12 C10 C13 109.8(4) . . ? 
C12 C10 C11 109.6(4) . . ? 
C13 C10 C11 109.9(4) . . ? 
C12 C10 C9 109.4(4) . . ? 
C13 C10 C9 107.0(4) . . ? 
C11 C10 C9 111.1(3) . . ? 
N1 C14 C2 114.4(3) . . ? 
N1 C15 C16 111.9(3) . . ? 
O4 C16 C15 107.7(3) . . ? 
N1 C17 C18 111.9(3) . . ? 
O3 C18 C17 106.2(3) . . ? 
O7 C19 O8 123.0(4) . . ? 
O7 C19 C20 118.8(4) . . ? 
O8 C19 C20 118.1(4) . . ? 
C21 C20 C23 109.8(4) . . ? 
C21 C20 C19 110.4(4) . . ? 
C23 C20 C19 107.1(4) . . ? 
C21 C20 C22 109.3(4) . . ? 
C23 C20 C22 108.9(4) . . ? 
C19 C20 C22 111.3(4) . . ? 
Cl3 C24 Cl2 110.8(3) . . ? 
Cl3 C24 Cl1 110.6(3) . . ? 
Cl2 C24 Cl1 109.9(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              25.02 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    1.484 
_refine_diff_density_min   -1.001 
_refine_diff_density_rms    0.103 

#===END

 
data_Dy2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C48 H78 Cl6 Dy2 N2 O16' 
_chemical_formula_weight          1476.82 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'Monoclinic' 
_symmetry_space_group_name_H-M    'P 21/c' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    10.758(5) 
_cell_length_b                    15.532(5) 
_cell_length_c                    18.285(5) 
_cell_angle_alpha                 90.000(5) 
_cell_angle_beta                  95.275(5) 
_cell_angle_gamma                 90.000(5) 
_cell_volume                      3042.4(19) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     7107
_cell_measurement_theta_min       2.24
_cell_measurement_theta_max       28.31
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'colorless' 
_exptl_crystal_size_max           0.148
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.092
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.612 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1484 
_exptl_absorpt_coefficient_mu     2.763 
_exptl_absorpt_correction_type    'empirical'
_exptl_absorpt_correction_T_min   0.677538
_exptl_absorpt_correction_T_max   1
_exptl_absorpt_process_details    'sadabs' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             16469 
_diffrn_reflns_av_R_equivalents   0.0414 
_diffrn_reflns_av_sigmaI/netI     0.0423 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.24 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              5905 
_reflns_number_gt                 5145 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection      'Bruker SMART'
_computing_cell_refinement      'Bruker SMART'
_computing_data_reduction       'Bruker SAINT'
_computing_structure_solution   'Bruker SHELXTL'
_computing_structure_refinement 'Bruker SHELXTL'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'

_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)+(0.0414P)²+2.4971P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5905 
_refine_ls_number_parameters      348 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0395 
_refine_ls_R_factor_gt            0.0334 
_refine_ls_wR_factor_ref          0.0836 
_refine_ls_wR_factor_gt           0.0795 
_refine_ls_goodness_of_fit_ref    1.048 
_refine_ls_restrained_S_all       1.048 
_refine_ls_shift/su_max           0.003 
_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 0.149586(15) 1.047383(11) 0.531950(9) 0.01697(7) Uani 1 1 d . . . 
Cl1 Cl 0.31249(14) 0.79947(13) 0.86057(9) 0.0741(5) Uani 1 1 d . . . 
Cl2 Cl 0.54628(13) 0.81751(9) 0.79738(7) 0.0502(3) Uani 1 1 d . . . 
Cl3 Cl 0.46197(18) 0.95088(8) 0.89000(8) 0.0623(4) Uani 1 1 d . . . 
O1 O -0.0546(3) 0.80233(17) 0.42829(15) 0.0261(6) Uani 1 1 d . . . 
O2 O 0.0444(2) 0.91566(16) 0.52318(13) 0.0192(5) Uani 1 1 d . . . 
O3 O 0.3473(2) 0.99498(19) 0.48224(15) 0.0251(6) Uani 1 1 d D . . 
O4 O 0.2994(2) 1.12023(17) 0.61172(14) 0.0223(6) Uani 1 1 d D . . 
O5 O 0.0507(2) 1.03875(15) 0.64075(14) 0.0193(6) Uani 1 1 d . . . 
O6 O -0.1425(2) 1.00282(17) 0.59664(14) 0.0232(6) Uani 1 1 d . . . 
O7 O 0.2204(2) 1.15926(17) 0.46100(15) 0.0249(6) Uani 1 1 d . . . 
O8 O 0.3695(3) 1.23408(18) 0.52462(15) 0.0325(7) Uani 1 1 d . . . 
N1 N 0.2921(3) 0.94243(19) 0.62061(17) 0.0189(7) Uani 1 1 d . . . 
C1 C 0.0853(4) 0.8341(2) 0.5310(2) 0.0208(8) Uani 1 1 d . . . 
C2 C 0.1701(3) 0.8071(2) 0.5875(2) 0.0196(8) Uani 1 1 d . . . 
C3 C 0.2118(4) 0.7218(2) 0.5903(2) 0.0235(8) Uani 1 1 d . . . 
H3 H 0.2710 0.7052 0.6279 0.028 Uiso 1 1 calc R . . 
C4 C 0.1676(3) 0.6609(3) 0.5387(2) 0.0235(9) Uani 1 1 d . . . 
C5 C 0.0772(4) 0.6876(3) 0.4836(2) 0.0254(9) Uani 1 1 d . . . 
H5 H 0.0445 0.6482 0.4487 0.030 Uiso 1 1 calc R . . 
C6 C 0.0362(3) 0.7711(2) 0.4803(2) 0.0216(8) Uani 1 1 d . . . 
C7 C -0.1004(4) 0.7447(3) 0.3711(2) 0.0329(10) Uani 1 1 d . . . 
H7A H -0.0316 0.7227 0.3468 0.049 Uiso 1 1 calc R . . 
H7B H -0.1567 0.7749 0.3362 0.049 Uiso 1 1 calc R . . 
H7C H -0.1435 0.6978 0.3918 0.049 Uiso 1 1 calc R . . 
C8 C 0.2132(4) 0.5689(3) 0.5415(2) 0.0316(10) Uani 1 1 d . . . 
H8A H 0.1432 0.5306 0.5418 0.047 Uiso 1 1 calc R . . 
H8B H 0.2682 0.5603 0.5853 0.047 Uiso 1 1 calc R . . 
H8C H 0.2573 0.5573 0.4993 0.047 Uiso 1 1 calc R . . 
C9 C 0.2169(3) 0.8695(2) 0.6466(2) 0.0206(8) Uani 1 1 d . . . 
H9A H 0.1459 0.8930 0.6689 0.025 Uiso 1 1 calc R . . 
H9B H 0.2677 0.8383 0.6844 0.025 Uiso 1 1 calc R . . 
C10 C 0.4022(4) 0.9084(3) 0.5857(2) 0.0280(9) Uani 1 1 d . . . 
H10A H 0.4196 0.8502 0.6029 0.034 Uiso 1 1 calc R . . 
H10B H 0.4747 0.9435 0.6006 0.034 Uiso 1 1 calc R . . 
C11 C 0.3804(4) 0.9082(3) 0.5033(2) 0.0264(9) Uani 1 1 d . . . 
H11A H 0.4554 0.8905 0.4817 0.032 Uiso 1 1 calc R . . 
H11B H 0.3134 0.8689 0.4871 0.032 Uiso 1 1 calc R . . 
C12 C 0.3344(4) 0.9960(3) 0.6856(2) 0.0240(8) Uani 1 1 d . . . 
H12A H 0.3964 0.9645 0.7169 0.029 Uiso 1 1 calc R . . 
H12B H 0.2641 1.0075 0.7138 0.029 Uiso 1 1 calc R . . 
C13 C 0.3894(4) 1.0798(3) 0.6632(2) 0.0259(9) Uani 1 1 d . . . 
H13A H 0.4077 1.1165 0.7058 0.031 Uiso 1 1 calc R . . 
H13B H 0.4664 1.0696 0.6408 0.031 Uiso 1 1 calc R . . 
C14 C -0.0629(3) 1.0251(2) 0.6481(2) 0.0196(8) Uani 1 1 d . . . 
C15 C -0.1074(4) 1.0355(3) 0.7250(2) 0.0237(9) Uani 1 1 d . . . 
C16 C -0.0479(5) 0.9620(3) 0.7728(3) 0.0447(13) Uani 1 1 d . . . 
H16A H -0.0761 0.9651 0.8210 0.067 Uiso 1 1 calc R . . 
H16B H 0.0414 0.9674 0.7762 0.067 Uiso 1 1 calc R . . 
H16C H -0.0718 0.9076 0.7508 0.067 Uiso 1 1 calc R . . 
C17 C -0.0614(4) 1.1220(3) 0.7570(3) 0.0419(12) Uani 1 1 d . . . 
H17A H -0.1005 1.1680 0.7283 0.063 Uiso 1 1 calc R . . 
H17B H 0.0275 1.1257 0.7561 0.063 Uiso 1 1 calc R . . 
H17C H -0.0823 1.1267 0.8068 0.063 Uiso 1 1 calc R . . 
C18 C -0.2491(4) 1.0316(3) 0.7232(3) 0.0397(12) Uani 1 1 d . . . 
H18A H -0.2733 1.0352 0.7724 0.060 Uiso 1 1 calc R . . 
H18B H -0.2784 0.9783 0.7014 0.060 Uiso 1 1 calc R . . 
H18C H -0.2850 1.0789 0.6947 0.060 Uiso 1 1 calc R . . 
C19 C 0.2943(4) 1.2218(2) 0.4682(2) 0.0227(8) Uani 1 1 d . . . 
C20 C 0.2926(4) 1.2879(2) 0.4057(2) 0.0229(8) Uani 1 1 d . . . 
C21 C 0.4241(4) 1.3216(3) 0.3964(3) 0.0450(13) Uani 1 1 d . . . 
H21A H 0.4736 1.2761 0.3784 0.067 Uiso 1 1 calc R . . 
H21B H 0.4622 1.3413 0.4429 0.067 Uiso 1 1 calc R . . 
H21C H 0.4190 1.3684 0.3620 0.067 Uiso 1 1 calc R . . 
C22 C 0.2118(5) 1.3624(3) 0.4270(3) 0.0455(13) Uani 1 1 d . . . 
H22A H 0.2096 1.4061 0.3898 0.068 Uiso 1 1 calc R . . 
H22B H 0.2461 1.3861 0.4730 0.068 Uiso 1 1 calc R . . 
H22C H 0.1286 1.3422 0.4317 0.068 Uiso 1 1 calc R . . 
C23 C 0.2379(6) 1.2481(3) 0.3344(2) 0.0477(13) Uani 1 1 d . . . 
H23A H 0.1536 1.2302 0.3394 0.072 Uiso 1 1 calc R . . 
H23B H 0.2869 1.1991 0.3230 0.072 Uiso 1 1 calc R . . 
H23C H 0.2383 1.2897 0.2956 0.072 Uiso 1 1 calc R . . 
C24 C 0.4636(4) 0.8395(3) 0.8736(2) 0.0348(10) Uani 1 1 d . . . 
H24 H 0.5065 0.8112 0.9167 0.042 Uiso 1 1 calc R . . 
H201 H 0.331(4) 1.158(2) 0.587(2) 0.042 Uiso 1 1 d D . . 
H202 H 0.321(4) 0.991(3) 0.4388(12) 0.042 Uiso 1 1 d D . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Dy1 O2 2.305(3) 3_576 ? 
Dy1 O2 2.337(3) . ? 
Dy1 O7 2.338(3) . ? 
Dy1 O5 2.344(3) . ? 
Dy1 O4 2.361(3) . ? 
Dy1 O6 2.472(3) 3_576 ? 
Dy1 O3 2.524(3) . ? 
Dy1 O1 2.675(3) 3_576 ? 
Dy1 N1 2.679(3) . ? 
Dy1 Dy1 3.6331(13) 3_576 ? 
Cl1 C24 1.736(5) . ? 
Cl2 C24 1.755(4) . ? 
Cl3 C24 1.757(5) . ? 
O1 C6 1.387(5) . ? 
O1 C7 1.430(5) . ? 
O1 Dy1 2.675(3) 3_576 ? 
O2 C1 1.344(4) . ? 
O2 Dy1 2.305(3) 3_576 ? 
O3 C11 1.438(5) . ? 
O4 C13 1.432(5) . ? 
O5 C14 1.261(4) . ? 
O6 C14 1.262(4) . ? 
O6 Dy1 2.472(3) 3_576 ? 
O7 C19 1.255(4) . ? 
O8 C19 1.265(5) . ? 
N1 C12 1.488(5) . ? 
N1 C10 1.493(5) . ? 
N1 C9 1.494(5) . ? 
C1 C2 1.380(5) . ? 
C1 C6 1.417(5) . ? 
C2 C3 1.399(5) . ? 
C2 C9 1.503(5) . ? 
C3 C4 1.388(6) . ? 
C4 C5 1.397(6) . ? 
C4 C8 1.510(5) . ? 
C5 C6 1.368(5) . ? 
C10 C11 1.504(6) . ? 
C12 C13 1.503(6) . ? 
C14 C15 1.535(5) . ? 
C15 C18 1.523(6) . ? 
C15 C17 1.529(6) . ? 
C15 C16 1.541(6) . ? 
C19 C20 1.535(5) . ? 
C20 C23 1.513(6) . ? 
C20 C22 1.520(6) . ? 
C20 C21 1.532(6) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O2 Dy1 O2 76.98(10) 3_576 . ? 
O2 Dy1 O7 84.28(9) 3_576 . ? 
O2 Dy1 O7 142.50(9) . . ? 
O2 Dy1 O5 85.55(9) 3_576 . ? 
O2 Dy1 O5 75.72(9) . . ? 
O7 Dy1 O5 135.23(9) . . ? 
O2 Dy1 O4 133.63(9) 3_576 . ? 
O2 Dy1 O4 139.55(9) . . ? 
O7 Dy1 O4 75.39(9) . . ? 
O5 Dy1 O4 80.81(9) . . ? 
O2 Dy1 O6 73.45(9) 3_576 3_576 ? 
O2 Dy1 O6 71.71(9) . 3_576 ? 
O7 Dy1 O6 71.92(9) . 3_576 ? 
O5 Dy1 O6 144.35(9) . 3_576 ? 
O4 Dy1 O6 134.30(9) . 3_576 ? 
O2 Dy1 O3 132.99(9) 3_576 . ? 
O2 Dy1 O3 96.43(9) . . ? 
O7 Dy1 O3 73.22(9) . . ? 
O5 Dy1 O3 138.62(9) . . ? 
O4 Dy1 O3 80.03(10) . . ? 
O6 Dy1 O3 60.58(9) 3_576 . ? 
O2 Dy1 O1 63.17(8) 3_576 3_576 ? 
O2 Dy1 O1 126.01(9) . 3_576 ? 
O7 Dy1 O1 69.78(9) . 3_576 ? 
O5 Dy1 O1 66.74(8) . 3_576 ? 
O4 Dy1 O1 70.73(9) . 3_576 ? 
O6 Dy1 O1 123.69(9) 3_576 3_576 ? 
O3 Dy1 O1 137.29(9) . 3_576 ? 
O2 Dy1 N1 149.41(9) 3_576 . ? 
O2 Dy1 N1 75.85(9) . . ? 
O7 Dy1 N1 126.18(9) . . ? 
O5 Dy1 N1 74.38(9) . . ? 
O4 Dy1 N1 66.27(9) . . ? 
O6 Dy1 N1 110.45(9) 3_576 . ? 
O3 Dy1 N1 64.36(9) . . ? 
O1 Dy1 N1 125.31(9) 3_576 . ? 
O2 Dy1 Dy1 38.80(6) 3_576 3_576 ? 
O2 Dy1 Dy1 38.18(6) . 3_576 ? 
O7 Dy1 Dy1 116.55(7) . 3_576 ? 
O5 Dy1 Dy1 78.01(7) . 3_576 ? 
O4 Dy1 Dy1 158.01(7) . 3_576 ? 
O6 Dy1 Dy1 67.51(6) 3_576 3_576 ? 
O3 Dy1 Dy1 120.31(7) . 3_576 ? 
O1 Dy1 Dy1 95.27(6) 3_576 3_576 ? 
N1 Dy1 Dy1 112.88(7) . 3_576 ? 
C6 O1 C7 117.1(3) . . ? 
C6 O1 Dy1 112.5(2) . 3_576 ? 
C7 O1 Dy1 129.1(2) . 3_576 ? 
C1 O2 Dy1 123.8(2) . 3_576 ? 
C1 O2 Dy1 131.7(2) . . ? 
Dy1 O2 Dy1 103.02(10) 3_576 . ? 
C11 O3 Dy1 113.7(2) . . ? 
C13 O4 Dy1 125.3(2) . . ? 
C14 O5 Dy1 128.4(2) . . ? 
C14 O6 Dy1 139.1(2) . 3_576 ? 
C19 O7 Dy1 138.8(3) . . ? 
C12 N1 C10 110.1(3) . . ? 
C12 N1 C9 107.7(3) . . ? 
C10 N1 C9 110.0(3) . . ? 
C12 N1 Dy1 105.0(2) . . ? 
C10 N1 Dy1 112.9(2) . . ? 
C9 N1 Dy1 110.9(2) . . ? 
O2 C1 C2 123.6(3) . . ? 
O2 C1 C6 118.9(3) . . ? 
C2 C1 C6 117.5(3) . . ? 
C1 C2 C3 120.1(4) . . ? 
C1 C2 C9 119.8(3) . . ? 
C3 C2 C9 120.0(3) . . ? 
C4 C3 C2 122.2(4) . . ? 
C3 C4 C5 117.3(4) . . ? 
C3 C4 C8 122.1(4) . . ? 
C5 C4 C8 120.6(4) . . ? 
C6 C5 C4 120.9(4) . . ? 
C5 C6 O1 124.4(3) . . ? 
C5 C6 C1 121.8(4) . . ? 
O1 C6 C1 113.8(3) . . ? 
N1 C9 C2 114.5(3) . . ? 
N1 C10 C11 111.9(3) . . ? 
O3 C11 C10 106.2(3) . . ? 
N1 C12 C13 111.5(3) . . ? 
O4 C13 C12 107.4(3) . . ? 
O5 C14 O6 124.4(3) . . ? 
O5 C14 C15 117.9(3) . . ? 
O6 C14 C15 117.7(3) . . ? 
C18 C15 C17 109.4(4) . . ? 
C18 C15 C14 111.8(3) . . ? 
C17 C15 C14 109.0(3) . . ? 
C18 C15 C16 110.2(4) . . ? 
C17 C15 C16 109.4(4) . . ? 
C14 C15 C16 107.0(3) . . ? 
O7 C19 O8 123.6(4) . . ? 
O7 C19 C20 118.4(3) . . ? 
O8 C19 C20 118.0(3) . . ? 
C23 C20 C22 110.2(4) . . ? 
C23 C20 C21 109.5(4) . . ? 
C22 C20 C21 108.9(4) . . ? 
C23 C20 C19 110.2(3) . . ? 
C22 C20 C19 106.6(3) . . ? 
C21 C20 C19 111.3(3) . . ? 
Cl1 C24 Cl2 111.0(3) . . ? 
Cl1 C24 Cl3 110.6(2) . . ? 
Cl2 C24 Cl3 109.9(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              26.00 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    1.919 
_refine_diff_density_min   -0.816 
_refine_diff_density_rms    0.118 

#===END

 
data_Tb2
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C48 H78 Cl6 N2 O16 Tb2' 
_chemical_formula_weight          1469.68 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'monoclinic' 
_symmetry_space_group_name_H-M   'P 21/c' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    10.789(5) 
_cell_length_b                    15.561(5) 
_cell_length_c                    18.269(5) 
_cell_angle_alpha                 90.000(5) 
_cell_angle_beta                  95.279(5) 
_cell_angle_gamma                 90.000(5) 
_cell_volume                      3054.1(19) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     5763
_cell_measurement_theta_min        2.30
_cell_measurement_theta_max       28.18
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'colorless' 
_exptl_crystal_size_max           0.128
_exptl_crystal_size_mid           0.107 
_exptl_crystal_size_min           0.089
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.598 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1480 
_exptl_absorpt_coefficient_mu     2.621 
_exptl_absorpt_correction_type    'empirical' 
_exptl_absorpt_correction_T_min   0.715345 
_exptl_absorpt_correction_T_max   1.0 
_exptl_absorpt_process_details    'sadabs' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             15921 
_diffrn_reflns_av_R_equivalents   0.0369 
_diffrn_reflns_av_sigmaI/netI     0.0419 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.64 
_diffrn_reflns_theta_max          25.50 
_reflns_number_total              5611 
_reflns_number_gt                 4799 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection      'Bruker SMART'
_computing_cell_refinement      'Bruker SMART'
_computing_data_reduction       'Bruker SAINT'
_computing_structure_solution   'Bruker SHELXTL'
_computing_structure_refinement 'Bruker SHELXTL'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
 
_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)+(0.0387P)²+3.8542P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5611 
_refine_ls_number_parameters      350 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0403 
_refine_ls_R_factor_gt            0.0332 
_refine_ls_wR_factor_ref          0.0828 
_refine_ls_wR_factor_gt           0.0782 
_refine_ls_goodness_of_fit_ref    1.039 
_refine_ls_restrained_S_all       1.039 
_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 
C1 C 0.8907(4) -0.0799(3) 0.6632(2) 0.0273(10) Uani 1 1 d . . . 
H1A H 0.9677 -0.0698 0.6409 0.033 Uiso 1 1 calc R . . 
H1B H 0.9085 -0.1162 0.7060 0.033 Uiso 1 1 calc R . . 
C2 C 0.8349(4) 0.0046(3) 0.6850(2) 0.0246(9) Uani 1 1 d . . . 
H2A H 0.7649 -0.0068 0.7133 0.030 Uiso 1 1 calc R . . 
H2B H 0.8966 0.0364 0.7162 0.030 Uiso 1 1 calc R . . 
C3 C 0.9021(4) 0.0914(3) 0.5856(2) 0.0285(10) Uani 1 1 d . . . 
H3A H 0.9742 0.0561 0.6003 0.034 Uiso 1 1 calc R . . 
H3B H 0.9198 0.1494 0.6029 0.034 Uiso 1 1 calc R . . 
C4 C 0.8799(4) 0.0919(3) 0.5026(2) 0.0268(10) Uani 1 1 d . . . 
H4A H 0.8125 0.1308 0.4866 0.032 Uiso 1 1 calc R . . 
H4B H 0.9543 0.1100 0.4809 0.032 Uiso 1 1 calc R . . 
C5 C 0.7177(4) 0.1302(3) 0.6466(2) 0.0222(9) Uani 1 1 d . . . 
H5A H 0.7684 0.1611 0.6845 0.027 Uiso 1 1 calc R . . 
H5B H 0.6469 0.1066 0.6688 0.027 Uiso 1 1 calc R . . 
C6 C 0.6711(4) 0.1927(2) 0.5878(2) 0.0190(8) Uani 1 1 d . . . 
C7 C 0.7120(4) 0.2782(3) 0.5900(2) 0.0234(9) Uani 1 1 d . . . 
H7 H 0.7714 0.2951 0.6274 0.028 Uiso 1 1 calc R . . 
C8 C 0.6671(4) 0.3383(3) 0.5386(2) 0.0229(9) Uani 1 1 d . . . 
C9 C 0.7140(5) 0.4307(3) 0.5418(3) 0.0329(11) Uani 1 1 d . . . 
H9A H 0.7598 0.4410 0.5885 0.049 Uiso 1 1 calc R . . 
H9B H 0.6444 0.4693 0.5357 0.049 Uiso 1 1 calc R . . 
H9C H 0.7672 0.4401 0.5032 0.049 Uiso 1 1 calc R . . 
C10 C 0.5764(4) 0.3121(3) 0.4836(2) 0.0249(9) Uani 1 1 d . . . 
H10 H 0.5434 0.3516 0.4489 0.030 Uiso 1 1 calc R . . 
C11 C 0.5356(4) 0.2285(2) 0.4805(2) 0.0199(9) Uani 1 1 d . . . 
C12 C 0.5846(4) 0.1660(2) 0.5311(2) 0.0209(9) Uani 1 1 d . . . 
C13 C 0.3992(5) 0.2552(3) 0.3712(2) 0.0320(11) Uani 1 1 d . . . 
H13A H 0.3573 0.3026 0.3918 0.048 Uiso 1 1 calc R . . 
H13B H 0.3420 0.2252 0.3369 0.048 Uiso 1 1 calc R . . 
H13C H 0.4676 0.2763 0.3463 0.048 Uiso 1 1 calc R . . 
C14 C 0.2872(5) 0.3631(3) 0.5723(3) 0.0444(14) Uani 1 1 d . . . 
H14A H 0.2907 0.4066 0.6097 0.067 Uiso 1 1 calc R . . 
H14B H 0.2519 0.3870 0.5266 0.067 Uiso 1 1 calc R . . 
H14C H 0.3697 0.3427 0.5667 0.067 Uiso 1 1 calc R . . 
C15 C 0.2626(6) 0.2499(3) 0.6660(3) 0.0445(13) Uani 1 1 d . . . 
H15A H 0.3456 0.2305 0.6603 0.067 Uiso 1 1 calc R . . 
H15B H 0.2127 0.2021 0.6789 0.067 Uiso 1 1 calc R . . 
H15C H 0.2650 0.2924 0.7041 0.067 Uiso 1 1 calc R . . 
C16 C 0.2065(4) 0.2887(3) 0.5943(2) 0.0222(9) Uani 1 1 d . . . 
C17 C 0.0754(5) 0.3223(3) 0.6033(3) 0.0479(14) Uani 1 1 d . . . 
H17A H 0.0266 0.2774 0.6223 0.072 Uiso 1 1 calc R . . 
H17B H 0.0370 0.3407 0.5564 0.072 Uiso 1 1 calc R . . 
H17C H 0.0805 0.3700 0.6368 0.072 Uiso 1 1 calc R . . 
C18 C 0.2046(4) 0.2220(3) 0.5322(2) 0.0230(9) Uani 1 1 d . . . 
C19 C 0.5611(5) 0.1207(3) 0.2420(3) 0.0445(13) Uani 1 1 d . . . 
H19A H 0.6024 0.1667 0.2694 0.067 Uiso 1 1 calc R . . 
H19B H 0.4729 0.1253 0.2445 0.067 Uiso 1 1 calc R . . 
H19C H 0.5793 0.1242 0.1916 0.067 Uiso 1 1 calc R . . 
C20 C 0.7472(5) 0.0310(4) 0.2760(3) 0.0435(13) Uani 1 1 d . . . 
H20A H 0.7716 0.0356 0.2269 0.065 Uiso 1 1 calc R . . 
H20B H 0.7755 -0.0228 0.2970 0.065 Uiso 1 1 calc R . . 
H20C H 0.7834 0.0774 0.3053 0.065 Uiso 1 1 calc R . . 
C21 C 0.6064(4) 0.0357(3) 0.2739(2) 0.0259(10) Uani 1 1 d . . . 
C22 C 0.5470(6) -0.0381(3) 0.2272(3) 0.0478(14) Uani 1 1 d . . . 
H22A H 0.4580 -0.0339 0.2254 0.072 Uiso 1 1 calc R . . 
H22B H 0.5736 -0.0921 0.2486 0.072 Uiso 1 1 calc R . . 
H22C H 0.5723 -0.0343 0.1782 0.072 Uiso 1 1 calc R . . 
C23 C 0.9637(5) 0.3398(3) 0.3737(3) 0.0360(11) Uani 1 1 d . . . 
H23 H 1.0062 0.3114 0.4169 0.043 Uiso 1 1 calc R . . 
C24 C 0.5626(4) 0.0251(2) 0.3516(2) 0.0195(9) Uani 1 1 d . . . 
N1 N 0.7926(3) 0.0576(2) 0.62017(18) 0.0197(7) Uani 1 1 d . . . 
O1 O 0.5439(2) 0.08431(17) 0.52379(15) 0.0193(6) Uani 1 1 d . . . 
O2 O 0.8018(3) -0.12022(18) 0.61178(15) 0.0236(6) Uani 1 1 d . . . 
O3 O 0.8481(3) 0.0058(2) 0.48174(18) 0.0252(7) Uani 1 1 d . . . 
O4 O 0.6420(3) 0.00320(18) 0.40303(15) 0.0238(6) Uani 1 1 d . . . 
O5 O 0.4500(3) 0.03876(16) 0.35866(15) 0.0199(6) Uani 1 1 d . . . 
O6 O 0.2780(3) 0.15924(18) 0.54000(15) 0.0242(6) Uani 1 1 d . . . 
O7 O 0.1295(3) 0.23396(19) 0.47518(16) 0.0321(7) Uani 1 1 d . . . 
O8 O 0.4449(3) 0.19771(17) 0.42893(16) 0.0256(7) Uani 1 1 d . . . 
Cl1 Cl 1.04497(14) 0.31674(9) 0.29728(8) 0.0533(4) Uani 1 1 d . . . 
Cl2 Cl 0.81215(16) 0.30057(14) 0.36054(10) 0.0789(5) Uani 1 1 d . . . 
Cl3 Cl 0.96303(19) 0.45064(9) 0.38983(9) 0.0652(5) Uani 1 1 d . . . 
Tb1 Tb 0.349790(17) 0.047523(11) 0.468267(10) 0.01649(8) Uani 1 1 d . . . 
H111 H 0.838(9) -0.171(6) 0.585(5) 0.15(4) Uiso 1 1 d . . . 
H112 H 0.816(5) 0.008(3) 0.444(3) 0.027(15) Uiso 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 
C1 O2 1.425(5) . ? 
C1 C2 1.515(6) . ? 
C2 N1 1.481(5) . ? 
C3 N1 1.486(5) . ? 
C3 C4 1.512(6) . ? 
C4 O3 1.426(5) . ? 
C5 N1 1.495(5) . ? 
C5 C6 1.501(6) . ? 
C6 C12 1.392(6) . ? 
C6 C7 1.401(6) . ? 
C7 C8 1.380(6) . ? 
C8 C10 1.397(6) . ? 
C8 C9 1.525(6) . ? 
C10 C11 1.373(6) . ? 
C11 O8 1.380(5) . ? 
C11 C12 1.411(6) . ? 
C12 O1 1.348(5) . ? 
C13 O8 1.435(5) . ? 
C14 C16 1.524(6) . ? 
C15 C16 1.517(6) . ? 
C16 C17 1.531(6) . ? 
C16 C18 1.536(6) . ? 
C18 O6 1.258(5) . ? 
C18 O7 1.274(5) . ? 
C19 C21 1.509(6) . ? 
C20 C21 1.517(6) . ? 
C21 C22 1.535(6) . ? 
C21 C24 1.545(6) . ? 
C23 Cl2 1.741(6) . ? 
C23 Cl3 1.750(5) . ? 
C23 Cl1 1.753(5) . ? 
C24 O5 1.253(5) . ? 
C24 O4 1.259(5) . ? 
N1 Tb1 2.682(3) 3_656 ? 
O1 Tb1 2.313(3) . ? 
O1 Tb1 2.348(3) 3_656 ? 
O2 Tb1 2.378(3) 3_656 ? 
O3 Tb1 2.538(3) 3_656 ? 
O4 Tb1 2.474(3) 3_656 ? 
O5 Tb1 2.365(3) . ? 
O6 Tb1 2.351(3) . ? 
O8 Tb1 2.677(3) . ? 
Tb1 O1 2.348(3) 3_656 ? 
Tb1 O2 2.378(3) 3_656 ? 
Tb1 O4 2.474(3) 3_656 ? 
Tb1 O3 2.538(3) 3_656 ? 
Tb1 N1 2.682(3) 3_656 ? 
Tb1 Tb1 3.6532(14) 3_656 ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O2 C1 C2 107.2(3) . . ? 
N1 C2 C1 111.9(3) . . ? 
N1 C3 C4 111.7(3) . . ? 
O3 C4 C3 106.0(3) . . ? 
N1 C5 C6 114.4(3) . . ? 
C12 C6 C7 119.5(4) . . ? 
C12 C6 C5 119.8(3) . . ? 
C7 C6 C5 120.7(4) . . ? 
C8 C7 C6 122.2(4) . . ? 
C7 C8 C10 118.0(4) . . ? 
C7 C8 C9 121.2(4) . . ? 
C10 C8 C9 120.7(4) . . ? 
C11 C10 C8 120.5(4) . . ? 
C10 C11 O8 124.2(4) . . ? 
C10 C11 C12 121.7(4) . . ? 
O8 C11 C12 114.1(3) . . ? 
O1 C12 C6 123.0(4) . . ? 
O1 C12 C11 119.1(4) . . ? 
C6 C12 C11 117.9(4) . . ? 
C15 C16 C14 109.8(4) . . ? 
C15 C16 C17 110.1(4) . . ? 
C14 C16 C17 108.9(4) . . ? 
C15 C16 C18 110.2(3) . . ? 
C14 C16 C18 106.7(3) . . ? 
C17 C16 C18 111.1(4) . . ? 
O6 C18 O7 123.5(4) . . ? 
O6 C18 C16 118.4(4) . . ? 
O7 C18 C16 118.1(4) . . ? 
C19 C21 C20 109.8(4) . . ? 
C19 C21 C22 109.6(4) . . ? 
C20 C21 C22 110.1(4) . . ? 
C19 C21 C24 109.5(4) . . ? 
C20 C21 C24 111.2(4) . . ? 
C22 C21 C24 106.5(4) . . ? 
Cl2 C23 Cl3 110.5(3) . . ? 
Cl2 C23 Cl1 110.5(3) . . ? 
Cl3 C23 Cl1 110.2(3) . . ? 
O5 C24 O4 124.7(4) . . ? 
O5 C24 C21 117.3(4) . . ? 
O4 C24 C21 118.0(4) . . ? 
C2 N1 C3 109.8(3) . . ? 
C2 N1 C5 107.4(3) . . ? 
C3 N1 C5 110.2(3) . . ? 
C2 N1 Tb1 105.0(2) . 3_656 ? 
C3 N1 Tb1 113.1(2) . 3_656 ? 
C5 N1 Tb1 111.0(2) . 3_656 ? 
C12 O1 Tb1 123.4(2) . . ? 
C12 O1 Tb1 131.7(2) . 3_656 ? 
Tb1 O1 Tb1 103.19(10) . 3_656 ? 
C1 O2 Tb1 125.4(2) . 3_656 ? 
C4 O3 Tb1 113.6(2) . 3_656 ? 
C24 O4 Tb1 139.3(3) . 3_656 ? 
C24 O5 Tb1 128.4(3) . . ? 
C18 O6 Tb1 138.4(3) . . ? 
C11 O8 C13 117.3(3) . . ? 
C11 O8 Tb1 112.7(2) . . ? 
C13 O8 Tb1 128.8(2) . . ? 
O1 Tb1 O1 76.81(10) . 3_656 ? 
O1 Tb1 O6 84.49(10) . . ? 
O1 Tb1 O6 142.72(9) 3_656 . ? 
O1 Tb1 O5 85.40(10) . . ? 
O1 Tb1 O5 75.13(9) 3_656 . ? 
O6 Tb1 O5 135.58(9) . . ? 
O1 Tb1 O2 134.08(10) . 3_656 ? 
O1 Tb1 O2 139.29(10) 3_656 3_656 ? 
O6 Tb1 O2 75.39(10) . 3_656 ? 
O5 Tb1 O2 81.30(10) . 3_656 ? 
O1 Tb1 O4 73.18(9) . 3_656 ? 
O1 Tb1 O4 71.82(9) 3_656 3_656 ? 
O6 Tb1 O4 72.00(10) . 3_656 ? 
O5 Tb1 O4 143.81(9) . 3_656 ? 
O2 Tb1 O4 134.32(10) 3_656 3_656 ? 
O1 Tb1 O3 132.90(10) . 3_656 ? 
O1 Tb1 O3 96.58(10) 3_656 3_656 ? 
O6 Tb1 O3 73.13(10) . 3_656 ? 
O5 Tb1 O3 138.67(10) . 3_656 ? 
O2 Tb1 O3 79.81(11) 3_656 3_656 ? 
O4 Tb1 O3 60.74(10) 3_656 3_656 ? 
O1 Tb1 O8 63.11(9) . . ? 
O1 Tb1 O8 125.59(10) 3_656 . ? 
O6 Tb1 O8 70.01(10) . . ? 
O5 Tb1 O8 66.85(9) . . ? 
O2 Tb1 O8 71.25(10) 3_656 . ? 
O4 Tb1 O8 123.54(9) 3_656 . ? 
O3 Tb1 O8 137.56(9) 3_656 . ? 
O1 Tb1 N1 149.38(10) . 3_656 ? 
O1 Tb1 N1 75.75(10) 3_656 3_656 ? 
O6 Tb1 N1 125.96(10) . 3_656 ? 
O5 Tb1 N1 74.68(10) . 3_656 ? 
O2 Tb1 N1 66.18(10) 3_656 3_656 ? 
O4 Tb1 N1 110.26(10) 3_656 3_656 ? 
O3 Tb1 N1 64.09(10) 3_656 3_656 ? 
O8 Tb1 N1 125.69(9) . 3_656 ? 
O1 Tb1 Tb1 38.75(7) . 3_656 ? 
O1 Tb1 Tb1 38.06(7) 3_656 3_656 ? 
O6 Tb1 Tb1 116.79(7) . 3_656 ? 
O5 Tb1 Tb1 77.54(7) . 3_656 ? 
O2 Tb1 Tb1 158.10(7) 3_656 3_656 ? 
O4 Tb1 Tb1 67.43(6) 3_656 3_656 ? 
O3 Tb1 Tb1 120.31(8) 3_656 3_656 ? 
O8 Tb1 Tb1 95.04(7) . 3_656 ? 
N1 Tb1 Tb1 112.74(7) 3_656 3_656 ? 
 
_diffrn_measured_fraction_theta_max    0.989 
_diffrn_reflns_theta_full              25.50 
_diffrn_measured_fraction_theta_full   0.989 
_refine_diff_density_max    1.761 
_refine_diff_density_min   -0.798 
_refine_diff_density_rms    0.112 

#===END

 
data_Eu2
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C48 H78 Cl6 Eu2 N2 O16' 
_chemical_formula_weight          1455.74 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting           'Monoclinic'
_symmetry_space_group_name_H-M   'P2(1)/c'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    10.8414(14) 
_cell_length_b                    15.569(2) 
_cell_length_c                    18.273(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.541(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      3070.0(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     5160
_cell_measurement_theta_min       2.24
_cell_measurement_theta_max       27.63
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'colorless' 
_exptl_crystal_size_max           0.15 
_exptl_crystal_size_mid           0.13 
_exptl_crystal_size_min           0.105
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.575 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1472 
_exptl_absorpt_coefficient_mu     2.347 
_exptl_absorpt_correction_type    'empirical' 
_exptl_absorpt_correction_T_min   0.480131 
_exptl_absorpt_correction_T_max   1.0 
_exptl_absorpt_process_details    'sadabs' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             15898 
_diffrn_reflns_av_R_equivalents   0.0476 
_diffrn_reflns_av_sigmaI/netI     0.0512 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          1.89 
_diffrn_reflns_theta_max          25.50 
_reflns_number_total              5665 
_reflns_number_gt                 4696 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection      'Bruker SMART'
_computing_cell_refinement      'Bruker SMART'
_computing_data_reduction       'Bruker SAINT'
_computing_structure_solution   'Bruker SHELXTL'
_computing_structure_refinement 'Bruker SHELXTL'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL' 
 
_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)+(0.0562P)²+4.8198P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5663 
_refine_ls_number_parameters      318 
_refine_ls_number_restraints      4 
_refine_ls_R_factor_all           0.0512 
_refine_ls_R_factor_gt            0.0415 
_refine_ls_wR_factor_ref          0.1102 
_refine_ls_wR_factor_gt           0.1022 
_refine_ls_goodness_of_fit_ref    1.041 
_refine_ls_restrained_S_all       1.040 
_refine_ls_shift/su_max           0.009 
_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 0.84903(2) 0.951804(14) 0.468678(12) 0.01952(10) Uani 1 1 d . . . 
Cl2 Cl 0.45729(18) 0.18370(12) 0.20189(10) 0.0646(5) Uani 1 1 d . . . 
Cl3 Cl 0.5397(3) 0.05049(11) 0.11021(12) 0.0836(7) Uani 1 1 d . . . 
Cl1 Cl 0.6880(2) 0.2002(2) 0.13980(13) 0.0990(8) Uani 1 1 d . . . 
O5 O 0.9487(3) 0.95988(19) 0.35752(18) 0.0233(7) Uani 1 1 d . . . 
O2 O 0.6955(3) 0.8791(2) 0.38774(19) 0.0275(8) Uani 1 1 d D . . 
H2 H 0.665(3) 0.836(2) 0.408(3) 0.041 Uiso 1 1 d D . . 
O8 O 0.8600(3) 1.0049(2) 0.59785(18) 0.0287(8) Uani 1 1 d . . . 
O1 O 0.9553(3) 1.0852(2) 0.47492(18) 0.0231(7) Uani 1 1 d . . . 
O4 O 0.9446(3) 0.8018(2) 0.43064(19) 0.0296(8) Uani 1 1 d . . . 
O6 O 0.7753(3) 0.8394(2) 0.54108(19) 0.0290(8) Uani 1 1 d . . . 
O3 O 0.6524(3) 1.0075(2) 0.51998(19) 0.0284(8) Uani 1 1 d D . . 
H3 H 0.692(5) 1.0088(18) 0.5622(15) 0.043 Uiso 1 1 d D . . 
O7 O 0.6284(3) 0.7655(2) 0.4759(2) 0.0371(9) Uani 1 1 d . . . 
N1 N 0.7051(4) 1.0577(2) 0.3795(2) 0.0234(9) Uani 1 1 d . . . 
C1 C 0.9138(5) 1.1662(3) 0.4676(3) 0.0234(11) Uani 1 1 d . . . 
C19 C 0.7021(5) 0.7771(3) 0.5326(3) 0.0258(11) Uani 1 1 d . . . 
C14 C 1.0610(4) 0.9739(3) 0.3501(3) 0.0230(10) Uani 1 1 d . . . 
C2 C 0.9638(4) 1.2293(3) 0.5182(3) 0.0249(11) Uani 1 1 d . . . 
C4 C 0.8308(5) 1.3393(3) 0.4603(3) 0.0274(11) Uani 1 1 d . . . 
C3 C 0.9225(5) 1.3128(3) 0.5150(3) 0.0295(12) Uani 1 1 d . . . 
H3A H 0.9559 1.3523 0.5496 0.035 Uiso 1 1 calc R . . 
C7 C 0.8271(4) 1.1925(3) 0.4114(3) 0.0240(11) Uani 1 1 d . . . 
C8 C 0.7791(4) 1.1296(3) 0.3531(3) 0.0254(11) Uani 1 1 d . . . 
H8A H 0.7283 1.1604 0.3152 0.030 Uiso 1 1 calc R . . 
H8B H 0.8491 1.1057 0.3307 0.030 Uiso 1 1 calc R . . 
C6 C 0.7850(4) 1.2781(3) 0.4088(3) 0.0264(11) Uani 1 1 d . . . 
H6 H 0.7249 1.2944 0.3717 0.032 Uiso 1 1 calc R . . 
C15 C 1.1045(6) 0.9648(4) 0.2735(3) 0.0467(8) Uani 1 1 d . . . 
C23 C 0.7854(6) 0.6362(4) 0.5726(4) 0.0536(18) Uani 1 1 d . . . 
H23A H 0.8684 0.6565 0.5694 0.080 Uiso 1 1 calc R . . 
H23B H 0.7527 0.6139 0.5257 0.080 Uiso 1 1 calc R . . 
H23C H 0.7862 0.5917 0.6089 0.080 Uiso 1 1 calc R . . 
C20 C 0.7044(6) 0.7103(4) 0.5943(3) 0.0421(8) Uani 1 1 d . . . 
C11 C 0.5965(5) 1.0909(3) 0.4141(3) 0.0313(12) Uani 1 1 d . . . 
H11A H 0.5252 1.0548 0.4001 0.038 Uiso 1 1 calc R . . 
H11B H 0.5775 1.1485 0.3961 0.038 Uiso 1 1 calc R . . 
C9 C 0.6622(5) 1.0037(3) 0.3150(3) 0.0304(12) Uani 1 1 d . . . 
H9A H 0.7319 0.9916 0.2870 0.037 Uiso 1 1 calc R . . 
H9B H 0.6011 1.0353 0.2834 0.037 Uiso 1 1 calc R . . 
C10 C 0.6061(5) 0.9201(3) 0.3372(3) 0.0314(12) Uani 1 1 d D . . 
H10A H 0.5306 0.9308 0.3602 0.038 Uiso 1 1 calc R . . 
H10B H 0.5863 0.8840 0.2944 0.038 Uiso 1 1 calc R . . 
C12 C 0.6196(5) 1.0931(3) 0.4970(3) 0.0323(12) Uani 1 1 d D . . 
H12A H 0.6863 1.1327 0.5123 0.039 Uiso 1 1 calc R . . 
H12B H 0.5456 1.1116 0.5185 0.039 Uiso 1 1 calc R . . 
C5 C 0.7831(6) 1.4298(4) 0.4572(3) 0.0412(14) Uani 1 1 d . . . 
H5A H 0.7363 1.4401 0.4983 0.062 Uiso 1 1 calc R . . 
H5B H 0.7308 1.4382 0.4123 0.062 Uiso 1 1 calc R . . 
H5C H 0.8517 1.4690 0.4589 0.062 Uiso 1 1 calc R . . 
C22 C 0.5735(6) 0.6763(4) 0.6030(3) 0.0421(8) Uani 1 1 d . . . 
H22A H 0.5333 0.6613 0.5556 0.063 Uiso 1 1 calc R . . 
H22B H 0.5263 0.7199 0.6249 0.063 Uiso 1 1 calc R . . 
H22C H 0.5791 0.6264 0.6340 0.063 Uiso 1 1 calc R . . 
C13 C 0.9006(5) 0.7444(4) 0.3728(3) 0.0381(14) Uani 1 1 d . . . 
H13A H 0.9688 0.7260 0.3468 0.057 Uiso 1 1 calc R . . 
H13B H 0.8407 0.7735 0.3394 0.057 Uiso 1 1 calc R . . 
H13C H 0.8627 0.6954 0.3932 0.057 Uiso 1 1 calc R . . 
C24 C 0.5389(6) 0.1608(4) 0.1267(3) 0.0431(15) Uani 1 1 d . . . 
H24 H 0.4966 0.1890 0.0833 0.052 Uiso 1 1 calc R . . 
C18 C 1.0442(6) 1.0372(4) 0.2261(3) 0.0467(8) Uani 1 1 d . . . 
H18A H 1.0684 1.0916 0.2477 0.070 Uiso 1 1 calc R . . 
H18B H 0.9557 1.0316 0.2234 0.070 Uiso 1 1 calc R . . 
H18C H 1.0707 1.0338 0.1776 0.070 Uiso 1 1 calc R . . 
C21 C 0.7588(6) 0.7485(4) 0.6666(3) 0.0421(8) Uani 1 1 d . . . 
H21A H 0.7616 0.7054 0.7043 0.063 Uiso 1 1 calc R . . 
H21B H 0.7081 0.7956 0.6797 0.063 Uiso 1 1 calc R . . 
H21C H 0.8412 0.7688 0.6615 0.063 Uiso 1 1 calc R . . 
C17 C 1.2445(6) 0.9705(4) 0.2747(3) 0.0467(8) Uani 1 1 d . . . 
H17A H 1.2728 1.0232 0.2980 0.070 Uiso 1 1 calc R . . 
H17B H 1.2675 0.9693 0.2253 0.070 Uiso 1 1 calc R . . 
H17C H 1.2819 0.9228 0.3017 0.070 Uiso 1 1 calc R . . 
C16 C 1.0618(6) 0.8778(4) 0.2413(3) 0.0467(8) Uani 1 1 d . . . 
H16A H 1.0858 0.8726 0.1923 0.070 Uiso 1 1 calc R . . 
H16B H 0.9732 0.8737 0.2401 0.070 Uiso 1 1 calc R . . 
H16C H 1.0994 0.8326 0.2714 0.070 Uiso 1 1 calc R . . 
 
 
_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 O1 2.340(3) 3_776 ? 
Eu1 O1 2.372(3) . ? 
Eu1 O6 2.378(3) . ? 
Eu1 O5 2.394(3) . ? 
Eu1 O2 2.401(3) . ? 
Eu1 O8 2.493(3) . ? 
Eu1 O3 2.561(3) . ? 
Eu1 O4 2.674(3) . ? 
Eu1 N1 2.704(4) . ? 
Eu1 Eu1 3.6816(6) 3_776 ? 
Cl2 C24 1.742(6) . ? 
Cl3 C24 1.744(6) . ? 
Cl1 C24 1.724(7) . ? 
O5 C14 1.257(6) . ? 
O2 C10 1.423(6) . ? 
O8 C14 1.261(6) 3_776 ? 
O1 C1 1.341(6) . ? 
O1 Eu1 2.340(3) 3_776 ? 
O4 C2 1.384(6) 3_776 ? 
O4 C13 1.430(6) . ? 
O6 C19 1.254(6) . ? 
O3 C12 1.432(7) . ? 
O7 C19 1.259(6) . ? 
N1 C11 1.483(6) . ? 
N1 C8 1.485(6) . ? 
N1 C9 1.485(6) . ? 
C1 C7 1.384(7) . ? 
C1 C2 1.420(7) . ? 
C19 C20 1.532(7) . ? 
C14 O8 1.261(5) 3_776 ? 
C14 C15 1.527(8) . ? 
C2 C3 1.374(7) . ? 
C2 O4 1.384(6) 3_776 ? 
C4 C6 1.395(7) . ? 
C4 C3 1.402(7) . ? 
C4 C5 1.501(7) . ? 
C7 C6 1.408(7) . ? 
C7 C8 1.503(7) . ? 
C15 C17 1.519(9) . ? 
C15 C18 1.529(9) . ? 
C15 C16 1.529(8) . ? 
C23 C20 1.525(8) . ? 
C20 C21 1.515(8) . ? 
C20 C22 1.538(8) . ? 
C11 C12 1.512(7) . ? 
C9 C10 1.509(7) . ? 
 
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 
O1 Eu1 O1 77.24(12) 3_776 . ? 
O1 Eu1 O6 85.00(11) 3_776 . ? 
O1 Eu1 O6 143.63(11) . . ? 
O1 Eu1 O5 85.54(12) 3_776 . ? 
O1 Eu1 O5 74.82(11) . . ? 
O6 Eu1 O5 135.56(11) . . ? 
O1 Eu1 O2 134.46(11) 3_776 . ? 
O1 Eu1 O2 138.32(11) . . ? 
O6 Eu1 O2 75.25(11) . . ? 
O5 Eu1 O2 81.09(12) . . ? 
O1 Eu1 O8 72.92(11) 3_776 . ? 
O1 Eu1 O8 71.67(11) . . ? 
O6 Eu1 O8 72.86(12) . . ? 
O5 Eu1 O8 143.28(11) . . ? 
O2 Eu1 O8 134.95(12) . . ? 
O1 Eu1 O3 132.34(11) 3_776 . ? 
O1 Eu1 O3 95.92(11) . . ? 
O6 Eu1 O3 73.10(12) . . ? 
O5 Eu1 O3 138.80(11) . . ? 
O2 Eu1 O3 80.40(12) . . ? 
O8 Eu1 O3 60.43(11) . . ? 
O1 Eu1 O4 62.73(10) 3_776 . ? 
O1 Eu1 O4 125.37(11) . . ? 
O6 Eu1 O4 70.20(12) . . ? 
O5 Eu1 O4 66.89(11) . . ? 
O2 Eu1 O4 71.99(11) . . ? 
O8 Eu1 O4 123.47(11) . . ? 
O3 Eu1 O4 138.40(11) . . ? 
O1 Eu1 N1 149.47(12) 3_776 . ? 
O1 Eu1 N1 75.20(11) . . ? 
O6 Eu1 N1 125.32(12) . . ? 
O5 Eu1 N1 74.83(12) . . ? 
O2 Eu1 N1 65.85(12) . . ? 
O8 Eu1 N1 109.89(12) . . ? 
O3 Eu1 N1 64.03(12) . . ? 
O4 Eu1 N1 126.24(11) . . ? 
O1 Eu1 Eu1 38.94(8) 3_776 3_776 ? 
O1 Eu1 Eu1 38.30(7) . 3_776 ? 
O6 Eu1 Eu1 117.62(8) . 3_776 ? 
O5 Eu1 Eu1 77.40(8) . 3_776 ? 
O2 Eu1 Eu1 157.89(9) . 3_776 ? 
O8 Eu1 Eu1 67.09(8) . 3_776 ? 
O3 Eu1 Eu1 119.64(8) . 3_776 ? 
O4 Eu1 Eu1 94.69(7) . 3_776 ? 
N1 Eu1 Eu1 112.51(8) . 3_776 ? 
C14 O5 Eu1 128.5(3) . . ? 
C10 O2 Eu1 125.2(3) . . ? 
C14 O8 Eu1 140.2(3) 3_776 . ? 
C1 O1 Eu1 123.8(3) . 3_776 ? 
C1 O1 Eu1 131.4(3) . . ? 
Eu1 O1 Eu1 102.76(12) 3_776 . ? 
C2 O4 C13 116.6(4) 3_776 . ? 
C2 O4 Eu1 113.6(3) 3_776 . ? 
C13 O4 Eu1 128.9(3) . . ? 
C19 O6 Eu1 138.0(3) . . ? 
C12 O3 Eu1 113.6(3) . . ? 
C11 N1 C8 110.6(4) . . ? 
C11 N1 C9 109.6(4) . . ? 
C8 N1 C9 107.8(4) . . ? 
C11 N1 Eu1 113.1(3) . . ? 
C8 N1 Eu1 110.9(3) . . ? 
C9 N1 Eu1 104.6(3) . . ? 
O1 C1 C7 123.3(4) . . ? 
O1 C1 C2 118.8(4) . . ? 
C7 C1 C2 117.9(4) . . ? 
O6 C19 O7 123.8(5) . . ? 
O6 C19 C20 117.9(4) . . ? 
O7 C19 C20 118.3(4) . . ? 
O5 C14 O8 124.0(5) . 3_776 ? 
O5 C14 C15 118.1(4) . . ? 
O8 C14 C15 117.9(5) 3_776 . ? 
C3 C2 O4 124.6(4) . 3_776 ? 
C3 C2 C1 121.6(5) . . ? 
O4 C2 C1 113.7(4) 3_776 . ? 
C6 C4 C3 117.5(4) . . ? 
C6 C4 C5 121.1(5) . . ? 
C3 C4 C5 121.4(5) . . ? 
C2 C3 C4 120.9(5) . . ? 
C1 C7 C6 119.9(4) . . ? 
C1 C7 C8 119.8(4) . . ? 
C6 C7 C8 120.3(4) . . ? 
N1 C8 C7 114.9(4) . . ? 
C4 C6 C7 122.0(5) . . ? 
C17 C15 C14 112.2(5) . . ? 
C17 C15 C18 109.7(6) . . ? 
C14 C15 C18 107.3(5) . . ? 
C17 C15 C16 108.9(5) . . ? 
C14 C15 C16 109.0(5) . . ? 
C18 C15 C16 109.8(5) . . ? 
C21 C20 C23 109.8(5) . . ? 
C21 C20 C19 110.7(5) . . ? 
C23 C20 C19 106.9(5) . . ? 
C21 C20 C22 109.3(5) . . ? 
C23 C20 C22 109.1(5) . . ? 
C19 C20 C22 111.1(5) . . ? 
N1 C11 C12 111.9(4) . . ? 
N1 C9 C10 112.2(4) . . ? 
O2 C10 C9 107.1(4) . . ? 
O3 C12 C11 106.5(4) . . ? 
Cl1 C24 Cl2 111.0(3) . . ? 
Cl1 C24 Cl3 110.7(4) . . ? 
Cl2 C24 Cl3 110.4(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.994 
_diffrn_reflns_theta_full              25.50 
_diffrn_measured_fraction_theta_full   0.994 
_refine_diff_density_max    1.524 
_refine_diff_density_min   -1.091 
_refine_diff_density_rms    0.130 


