 
data_sl97 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H12 Br3 Eu O6' 
_chemical_formula_weight          499.79 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Eu'  'Eu'  -0.1578   3.6682 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.2901   2.4595 
 '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' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 
_cell_length_a                    8.1672(7) 
_cell_length_b                    6.7538(4) 
_cell_length_c                    12.5451(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  127.077(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      552.08(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.006 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              456 
_exptl_absorpt_coefficient_mu     16.520 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_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   ? 
_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             10921 
_diffrn_reflns_av_R_equivalents   0.0666 
_diffrn_reflns_av_sigmaI/netI     0.0367 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.02 
_diffrn_reflns_theta_max          30.00 
_reflns_number_total              1613 
_reflns_number_gt                 1397 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0169P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0409(10) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          1613 
_refine_ls_number_parameters      72 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0378 
_refine_ls_R_factor_gt            0.0281 
_refine_ls_wR_factor_ref          0.0489 
_refine_ls_wR_factor_gt           0.0471 
_refine_ls_goodness_of_fit_ref    1.112 
_refine_ls_restrained_S_all       1.112 
_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 
Eu1 Eu 0.5000 0.16453(4) 0.2500 0.01702(10) Uani 1 2 d S . . 
Br1 Br 0.29387(6) 0.15844(7) 0.55331(4) 0.02954(11) Uani 1 1 d . . . 
Br2 Br 0.0000 0.63151(9) 0.2500 0.03178(16) Uani 1 2 d S . . 
O1 O 0.1770(4) 0.3095(5) 0.0675(4) 0.0318(7) Uani 1 1 d . . . 
H11 H 0.141(11) 0.335(10) -0.013(8) 0.06(2) Uiso 1 1 d . . . 
H12 H 0.054(14) 0.242(15) 0.051(9) 0.10(3) Uiso 1 1 d . . . 
O2 O 0.2414(5) 0.0618(5) 0.2757(4) 0.0312(7) Uani 1 1 d . . . 
H21 H 0.253(12) 0.102(12) 0.346(9) 0.08(3) Uiso 1 1 d . . . 
H22 H 0.178(13) -0.064(14) 0.251(9) 0.09(3) Uiso 1 1 d . . . 
O3 O 0.4432(5) 0.4265(5) 0.3523(4) 0.0332(7) Uani 1 1 d . . . 
H31 H 0.534(11) 0.551(11) 0.382(8) 0.07(2) Uiso 1 1 d . . . 
H32 H 0.297(12) 0.467(13) 0.303(8) 0.09(3) Uiso 1 1 d . . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Eu1 0.01687(13) 0.01806(13) 0.01727(15) 0.000 0.01089(11) 0.000 
Br1 0.0295(2) 0.0293(2) 0.0266(3) 0.00664(17) 0.01521(19) 0.00273(16) 
Br2 0.0294(3) 0.0360(3) 0.0327(4) 0.000 0.0202(3) 0.000 
O1 0.0233(13) 0.0381(17) 0.0252(18) 0.0082(14) 0.0101(13) 0.0037(12) 
O2 0.0313(15) 0.0367(17) 0.0353(19) -0.0051(14) 0.0251(15) -0.0072(13) 
O3 0.0310(15) 0.0302(15) 0.040(2) -0.0101(14) 0.0225(15) -0.0029(12) 
 
_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 O3 2.390(3) . ? 
Eu1 O3 2.390(3) 2_655 ? 
Eu1 O2 2.422(3) . ? 
Eu1 O2 2.422(3) 2_655 ? 
Eu1 O1 2.424(3) 2_655 ? 
Eu1 O1 2.424(3) . ? 
Eu1 Br1 2.9448(5) 4 ? 
Eu1 Br1 2.9448(5) 3_656 ? 
Br1 Eu1 2.9448(5) 3_656 ? 
O1 H11 0.88(8) . ? 
O1 H12 1.00(9) . ? 
O2 H21 0.87(9) . ? 
O2 H22 0.95(9) . ? 
O3 H31 1.03(8) . ? 
O3 H32 1.00(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 Eu1 O3 84.47(17) . 2_655 ? 
O3 Eu1 O2 70.94(12) . . ? 
O3 Eu1 O2 138.64(11) 2_655 . ? 
O3 Eu1 O2 138.64(11) . 2_655 ? 
O3 Eu1 O2 70.94(11) 2_655 2_655 ? 
O2 Eu1 O2 146.72(16) . 2_655 ? 
O3 Eu1 O1 69.31(11) . 2_655 ? 
O3 Eu1 O1 75.83(12) 2_655 2_655 ? 
O2 Eu1 O1 121.99(13) . 2_655 ? 
O2 Eu1 O1 72.64(12) 2_655 2_655 ? 
O3 Eu1 O1 75.83(12) . . ? 
O3 Eu1 O1 69.31(11) 2_655 . ? 
O2 Eu1 O1 72.64(12) . . ? 
O2 Eu1 O1 121.99(13) 2_655 . ? 
O1 Eu1 O1 132.35(16) 2_655 . ? 
O3 Eu1 Br1 143.18(8) . 4 ? 
O3 Eu1 Br1 107.24(9) 2_655 4 ? 
O2 Eu1 Br1 78.20(9) . 4 ? 
O2 Eu1 Br1 77.31(8) 2_655 4 ? 
O1 Eu1 Br1 146.86(8) 2_655 4 ? 
O1 Eu1 Br1 76.18(8) . 4 ? 
O3 Eu1 Br1 107.24(9) . 3_656 ? 
O3 Eu1 Br1 143.18(8) 2_655 3_656 ? 
O2 Eu1 Br1 77.31(8) . 3_656 ? 
O2 Eu1 Br1 78.20(9) 2_655 3_656 ? 
O1 Eu1 Br1 76.18(8) 2_655 3_656 ? 
O1 Eu1 Br1 146.86(8) . 3_656 ? 
Br1 Eu1 Br1 84.41(2) 4 3_656 ? 
Eu1 O1 H11 125(4) . . ? 
Eu1 O1 H12 113(6) . . ? 
H11 O1 H12 105(7) . . ? 
Eu1 O2 H21 118(5) . . ? 
Eu1 O2 H22 124(5) . . ? 
H21 O2 H22 109(7) . . ? 
Eu1 O3 H31 118(4) . . ? 
Eu1 O3 H32 115(5) . . ? 
H31 O3 H32 109(6) . . ? 
 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              30.00 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    1.140 
_refine_diff_density_min   -1.103 
_refine_diff_density_rms    0.155 
