data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(Dy6Hg5Br26)[4(HgBr2)](2Br)' ; _chemical_name_common '(Dy6Hg5Br26)[4(HgBr2)](2Br)' _chemical_melting_point 'not measured' _chemical_formula_moiety 'Br36 Dy6 Hg9' _chemical_formula_sum 'Br36 Dy6 Hg9' _chemical_formula_weight 5656.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Br' 'Br' -0.2901 2.4595 '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' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z' 'x-1/2, -y-1/2, z' _cell_length_a 13.0997(11) _cell_length_b 13.6459(13) _cell_length_c 27.906(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4988.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2768 _cell_measurement_theta_min 3.4430 _cell_measurement_theta_max 22.8610 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4722 _exptl_absorpt_coefficient_mu 31.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.090 _exptl_absorpt_correction_T_max 0.148 _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'micro-focus sealed X-ray tube' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova (Mo) X-ray Source' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1787 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14376 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4402 _reflns_number_gt 2666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _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 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^)+(0.1886P)^2^+179.1375P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4402 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1598 _refine_ls_R_factor_gt 0.1122 _refine_ls_wR_factor_ref 0.3482 _refine_ls_wR_factor_gt 0.3031 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Hg1 Hg 1.6219(3) -0.8784(3) -0.20621(8) 0.1786(14) Uani 1 1 d . . . Hg2 Hg 1.5000 -1.0000 -0.5000 0.1276(15) Uani 1 4 d S . . Hg3 Hg 0.1804(2) -1.3131(2) 0.15359(7) 0.1498(12) Uani 1 1 d . . . Dy1 Dy 1.83171(17) -1.34689(17) -0.5000 0.0676(7) Uani 1 2 d S . . Dy2 Dy 1.65842(16) -1.15476(16) -0.5000 0.0791(8) Uani 1 2 d S . . Dy3 Dy 1.5000 -1.0000 -0.37705(8) 0.0646(6) Uani 1 2 d S . . Br1 Br 1.8177(3) -1.3291(3) -0.58496(12) 0.0736(9) Uani 1 1 d . . . Br2 Br 1.5467(4) -1.2960(3) -0.5000 0.0746(12) Uani 1 2 d S . . Br3 Br 1.8057(3) -1.0505(4) -0.5000 0.0782(13) Uani 1 2 d S . . Br4 Br 1.6288(3) -1.1265(3) -0.38159(12) 0.0732(9) Uani 1 1 d . . . Br5 Br 1.6278(4) -0.8886(4) -0.29204(13) 0.1052(14) Uani 1 1 d . . . Br6 Br 1.5000 -1.0000 -0.15248(17) 0.0786(14) Uani 1 2 d S . . Br7 Br 1.5712(3) -0.7206(3) -0.15857(15) 0.0914(11) Uani 1 1 d . . . Br8 Br 1.7986(4) -0.9378(4) -0.1603(2) 0.1214(17) Uani 1 1 d . . . Br9 Br 2.0000 -1.0000 -0.1441(5) 0.196(6) Uani 1 2 d S . . Br10 Br 0.1688(3) -1.3269(4) 0.23806(15) 0.0984(13) Uani 1 1 d . . . Br11 Br 0.1822(4) -1.3114(4) 0.06771(15) 0.1086(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.239(3) 0.227(3) 0.0696(13) -0.0079(15) 0.0326(16) -0.031(3) Hg2 0.114(3) 0.121(3) 0.148(4) 0.000 0.000 -0.006(2) Hg3 0.159(2) 0.229(3) 0.0608(11) -0.0034(13) 0.0013(11) -0.0528(19) Dy1 0.0800(14) 0.0785(14) 0.0444(11) 0.000 0.000 0.0218(11) Dy2 0.0545(12) 0.0570(12) 0.126(2) 0.000 0.000 -0.0070(9) Dy3 0.0549(11) 0.0660(12) 0.0728(14) 0.000 0.000 0.0217(9) Br1 0.080(2) 0.082(2) 0.059(2) 0.0108(15) 0.0005(15) 0.0204(17) Br2 0.077(3) 0.059(2) 0.088(3) 0.000 0.000 -0.002(2) Br3 0.056(2) 0.077(3) 0.102(4) 0.000 0.000 -0.004(2) Br4 0.072(2) 0.081(2) 0.067(2) 0.0011(16) -0.0008(15) 0.0188(16) Br5 0.124(3) 0.140(4) 0.051(2) -0.015(2) -0.007(2) -0.027(3) Br6 0.085(3) 0.091(3) 0.059(3) 0.000 0.000 -0.015(2) Br7 0.079(2) 0.098(3) 0.098(3) -0.009(2) -0.001(2) -0.0063(19) Br8 0.117(3) 0.114(3) 0.133(4) 0.008(3) -0.040(3) -0.014(3) Br9 0.098(6) 0.277(16) 0.211(12) 0.000 0.000 0.034(7) Br10 0.096(3) 0.137(3) 0.062(2) -0.003(2) 0.0012(19) 0.001(2) Br11 0.110(3) 0.154(4) 0.062(2) 0.000(2) -0.006(2) -0.038(3) _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 Hg1 Br5 2.400(4) . ? Hg1 Br7 2.617(5) . ? Hg1 Br6 2.748(4) . ? Hg1 Br8 2.767(6) . ? Hg2 Dy2 2.961(2) . ? Hg2 Dy2 2.961(2) 5_834 ? Hg2 Dy1 3.037(2) 7_965 ? Hg2 Dy1 3.037(2) 3_424 ? Hg2 Dy3 3.431(2) 5_834 ? Hg2 Dy3 3.431(2) . ? Hg3 Br10 2.370(4) . ? Hg3 Br11 2.397(4) . ? Hg3 Br7 3.289(5) 5_735 ? Dy1 Br1 2.390(3) 6_554 ? Dy1 Br1 2.390(3) . ? Dy1 Hg2 3.037(2) 3_524 ? Dy1 Br3 3.310(6) 7_955 ? Dy1 Br2 3.425(6) 3_524 ? Dy1 Dy2 3.468(3) . ? Dy2 Br3 2.398(5) . ? Dy2 Br2 2.420(5) . ? Dy2 Br4 3.349(3) 6_554 ? Dy2 Br4 3.349(3) . ? Dy3 Br4 2.417(3) . ? Dy3 Br4 2.417(3) 2_835 ? Dy3 Br5 3.278(4) . ? Dy3 Br5 3.278(4) 2_835 ? Br2 Dy1 3.425(6) 3_424 ? Br3 Dy1 3.310(5) 7_965 ? Br6 Hg1 2.748(4) 2_835 ? Br7 Hg3 3.289(5) 5_735 ? Br8 Br9 2.808(6) . ? Br9 Br8 2.808(6) 2_935 ? 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 Br5 Hg1 Br7 124.2(2) . . ? Br5 Hg1 Br6 121.91(18) . . ? Br7 Hg1 Br6 94.15(14) . . ? Br5 Hg1 Br8 114.7(2) . . ? Br7 Hg1 Br8 102.60(18) . . ? Br6 Hg1 Br8 93.27(16) . . ? Dy2 Hg2 Dy2 180.0 . 5_834 ? Dy2 Hg2 Dy1 88.96(6) . 7_965 ? Dy2 Hg2 Dy1 91.04(6) 5_834 7_965 ? Dy2 Hg2 Dy1 91.04(6) . 3_424 ? Dy2 Hg2 Dy1 88.96(6) 5_834 3_424 ? Dy1 Hg2 Dy1 180.0 7_965 3_424 ? Dy2 Hg2 Dy3 90.0 . 5_834 ? Dy2 Hg2 Dy3 90.0 5_834 5_834 ? Dy1 Hg2 Dy3 90.0 7_965 5_834 ? Dy1 Hg2 Dy3 90.0 3_424 5_834 ? Dy2 Hg2 Dy3 90.0 . . ? Dy2 Hg2 Dy3 90.0 5_834 . ? Dy1 Hg2 Dy3 90.0 7_965 . ? Dy1 Hg2 Dy3 90.0 3_424 . ? Dy3 Hg2 Dy3 180.0 5_834 . ? Br10 Hg3 Br11 174.89(19) . . ? Br10 Hg3 Br7 91.88(15) . 5_735 ? Br11 Hg3 Br7 91.79(15) . 5_735 ? Br1 Dy1 Br1 165.34(18) 6_554 . ? Br1 Dy1 Hg2 97.23(9) 6_554 3_524 ? Br1 Dy1 Hg2 97.23(9) . 3_524 ? Br1 Dy1 Br3 92.50(11) 6_554 7_955 ? Br1 Dy1 Br3 92.50(11) . 7_955 ? Hg2 Dy1 Br3 79.48(9) 3_524 7_955 ? Br1 Dy1 Br2 90.30(11) 6_554 3_524 ? Br1 Dy1 Br2 90.30(11) . 3_524 ? Hg2 Dy1 Br2 78.16(10) 3_524 3_524 ? Br3 Dy1 Br2 157.64(13) 7_955 3_524 ? Br1 Dy1 Dy2 82.69(9) 6_554 . ? Br1 Dy1 Dy2 82.69(9) . . ? Hg2 Dy1 Dy2 174.35(10) 3_524 . ? Br3 Dy1 Dy2 106.17(11) 7_955 . ? Br2 Dy1 Dy2 96.19(10) 3_524 . ? Br3 Dy2 Br2 163.63(19) . . ? Br3 Dy2 Hg2 98.09(14) . . ? Br2 Dy2 Hg2 98.28(13) . . ? Br3 Dy2 Br4 91.43(8) . 6_554 ? Br2 Dy2 Br4 91.23(8) . 6_554 ? Hg2 Dy2 Br4 80.59(6) . 6_554 ? Br3 Dy2 Br4 91.43(8) . . ? Br2 Dy2 Br4 91.23(8) . . ? Hg2 Dy2 Br4 80.59(6) . . ? Br4 Dy2 Br4 161.19(13) 6_554 . ? Br3 Dy2 Dy1 85.52(14) . . ? Br2 Dy2 Dy1 78.11(14) . . ? Hg2 Dy2 Dy1 176.39(9) . . ? Br4 Dy2 Dy1 99.38(6) 6_554 . ? Br4 Dy2 Dy1 99.38(6) . . ? Br4 Dy3 Br4 173.99(19) . 2_835 ? Br4 Dy3 Br5 90.74(13) . . ? Br4 Dy3 Br5 93.61(13) 2_835 . ? Br4 Dy3 Br5 93.61(13) . 2_835 ? Br4 Dy3 Br5 90.74(13) 2_835 2_835 ? Br5 Dy3 Br5 87.27(16) . 2_835 ? Br4 Dy3 Hg2 86.99(9) . . ? Br4 Dy3 Hg2 86.99(9) 2_835 . ? Br5 Dy3 Hg2 136.37(8) . . ? Br5 Dy3 Hg2 136.37(8) 2_835 . ? Dy2 Br2 Dy1 92.53(15) . 3_424 ? Dy2 Br3 Dy1 93.46(15) . 7_965 ? Dy3 Br4 Dy2 102.41(12) . . ? Hg1 Br5 Dy3 137.09(19) . . ? Hg1 Br6 Hg1 113.9(2) 2_835 . ? Hg1 Br7 Hg3 83.42(14) . 5_735 ? Hg1 Br8 Br9 161.7(4) . . ? Br8 Br9 Br8 161.4(6) 2_935 . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 3.287 _refine_diff_density_min -6.423 _refine_diff_density_rms 0.439