data_A2M4U6Q17 # SUBMISSION DETAILS _publ_contact_author_name 'James A. Ibers' # Name of author for correspondence _publ_contact_author_address # Address of author for correspondence ; Department of Chemistry Northwestern University Evanston, IL 60208-3113 ; _publ_contact_author_email 'ibers@chem.northwestern.edu' _publ_contact_author_fax '1 847 491 2976' _publ_contact_author_phone '1 847 491 5449' _publ_requested_journal 'Inorganic Chemistry' _publ_requested_category ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Syntheses and Characterization of Six Quaternary Uranium Chalcogenides A2M4U6Q17 (A = Rb or Cs; M = Pd or Pt; Q = S or Se) ; _publ_section_abstract ; The A2M4U6Q17 compounds Rb2Pd4U6S17, Rb2Pd4U6Se17, Rb2Pt4U6Se17, Cs2Pd4U6S17, Cs2Pd4U6Se17, and Cs2Pt4U6Se17 were synthesized by the high-temperature solid-state reactions of U, M, and Q in a flux of ACl or Rb2S3. These isostructural compounds crystallize in a new structure type, with two formula units in the tetragonal space group P4/mnc. This structure consists of a network of square-planar MQ4, monocapped trigonal prismatic UQ7, and square-antiprismatic UQ8 polyhedra with A atoms in the voids. Rb2Pd4U6S17 is a typical semiconductor, as deduced from electrical resistivity measurements. Magnetic susceptibility and specific heat measurements on single crystals of Rb2Pd4U6S17 show a phase transition at 13 K, the result either of antiferromagnetic ordering or of a structural phase transition. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # NB if using publCIF, the Author database tool might prove useful # (see the Tools menu in publCIF) loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Oh, George N.' ; Department of Chemistry Northwestern University Evanston, IL 60208-3113 ; . 'Choi, Eun Sang' ; Department Physics and National High Magnetic Field Laboratory Florida State University Tallahassee, FL 32310-3706 ; . 'Lu, Jun' ; Department Physics and National High Magnetic Field Laboratory Florida State University Tallahassee, FL 32310-3706 ; . 'Koscielski, Lukasz A.' ; Department of Chemistry Northwestern University Evanston, IL 60208-3113 ; . 'Ward, Matthew D.' ; Department of Chemistry Northwestern University Evanston, IL 60208-3113 ; . 'Ellis, Donald E.' ; Department of Physics and Astronomy Northwestern University Evanston, IL 60208-3113 ; . 'Ibers, James A.' ; Department of Chemistry Northwestern University Evanston, IL 60208-3113 ; . data_cs2u6pt4se17 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dicaesium tetraplatinum(II) hexauranium(IV) decaheptaselenide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cs2 Pt4 Se17 U6' _chemical_formula_sum 'Cs2 Pt4 Se17 U6' _chemical_formula_weight 3816.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cs' 'Cs' -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 '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/mnc _symmetry_space_group_name_Hall '-P 4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 10.6744(3) _cell_length_b 10.6744(3) _cell_length_c 13.3691(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1523.31(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5172 _cell_measurement_theta_min 2.442 _cell_measurement_theta_max 30.574 _exptl_crystal_description 'tetragonal prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.030 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 72.714 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2903 _exptl_absorpt_correction_T_max 0.4341 _exptl_absorpt_process_details 'face indexed, SADABS (Sheldrick, 2008b)' _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 'Bruker APEX2 CCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26292 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 31.81 _reflns_number_total 1309 _reflns_number_gt 1136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS (Sheldrick, 2008a)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008a)' _computing_molecular_graphics 'Crystalmaker (Palmer, 2009)' _computing_publication_material 'SHELXL (Sheldrick, 2008a)' _refine_special_details ; . ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0167P)^2^+0.0000sin\q/\l] where P = 1.00000Fo^2^ + 0.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000126(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1309 _refine_ls_number_parameters 43 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0396 _refine_ls_wR_factor_gt 0.0375 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _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 U1 U 0.24529(3) 0.11853(3) 0.0000 0.00964(8) Uani 1 2 d S . . U2 U 0.0000 0.5000 0.2500 0.00872(9) Uani 1 4 d S . . Pt1 Pt 0.13868(3) 0.42941(3) 0.0000 0.00849(7) Uani 1 2 d S . . Cs1 Cs 0.0000 0.0000 0.25549(10) 0.0124(3) Uani 0.50 4 d SP . . Cs2 Cs 0.0000 0.0000 0.46670(10) 0.0132(3) Uani 0.50 4 d SP . . Se1 Se 0.09113(5) 0.27708(5) 0.13428(4) 0.00943(11) Uani 1 1 d . . . Se2 Se 0.28511(5) 0.07290(5) 0.36837(4) 0.01034(11) Uani 1 1 d . . . Se3 Se 0.0000 0.0000 0.0000 0.0237(4) Uani 1 8 d S . . 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 U1 0.00723(13) 0.00710(13) 0.01460(15) 0.000 0.000 0.00021(9) U2 0.00932(12) 0.00932(12) 0.00753(17) 0.000 0.000 0.00078(14) Pt1 0.00791(13) 0.00842(14) 0.00913(14) 0.000 0.000 -0.00014(10) Cs1 0.0111(4) 0.0111(4) 0.0150(6) 0.000 0.000 0.000 Cs2 0.0103(3) 0.0103(3) 0.0189(6) 0.000 0.000 0.000 Se1 0.0097(2) 0.0090(2) 0.0096(3) 0.00053(18) -0.00001(19) 0.00149(18) Se2 0.0091(2) 0.0096(2) 0.0124(3) 0.00016(19) -0.00190(19) 0.00010(19) Se3 0.0068(4) 0.0068(4) 0.0577(12) 0.000 0.000 0.000 _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 U1 Se2 2.8144(6) 8 ? U1 Se2 2.8144(6) 15_665 ? U1 Se1 2.8891(6) 11 ? U1 Se1 2.8891(6) 4 ? U1 Se3 2.9080(3) . ? U1 Se1 2.9657(6) . ? U1 Se1 2.9657(6) 10 ? U1 Pt1 3.3765(4) 11 ? U1 Pt1 3.4790(4) 3_655 ? U1 Pt1 3.5082(4) . ? U1 Cs1 4.4859(10) . ? U1 Cs1 4.4859(10) 9 ? U2 Se2 2.8932(5) 6_455 ? U2 Se2 2.8932(5) 4_565 ? U2 Se2 2.8932(5) 5 ? U2 Se2 2.8932(5) 3 ? U2 Se1 3.0003(5) 8 ? U2 Se1 3.0003(5) 7_455 ? U2 Se1 3.0003(5) 2_565 ? U2 Se1 3.0003(5) . ? Pt1 Se2 2.4708(6) 5 ? Pt1 Se2 2.4708(6) 14_665 ? Pt1 Se1 2.4748(5) . ? Pt1 Se1 2.4748(6) 10 ? Pt1 U1 3.3765(4) 3 ? Pt1 U1 3.4790(4) 11_565 ? Pt1 Cs2 3.9549(3) 5 ? Pt1 Cs2 3.9549(3) 13_665 ? Cs1 Cs2 2.8237(18) . ? Cs1 Se3 3.4157(13) . ? Cs1 Se2 3.4850(8) . ? Cs1 Se2 3.4850(8) 3 ? Cs1 Se2 3.4850(8) 2 ? Cs1 Se2 3.4850(8) 4 ? Cs1 Se1 3.5100(8) 2 ? Cs1 Se1 3.5100(8) 3 ? Cs1 Se1 3.5100(8) 4 ? Cs1 Se1 3.5100(8) . ? Cs1 Cs2 3.7140(18) 9_556 ? Cs1 U1 4.4859(10) 9 ? Cs2 Cs2 0.890(3) 9_556 ? Cs2 Se2 3.4053(7) . ? Cs2 Se2 3.4054(7) 2 ? Cs2 Se2 3.4054(7) 4 ? Cs2 Se2 3.4054(7) 3 ? Cs2 Cs1 3.7141(18) 9_556 ? Cs2 Se2 3.8381(9) 10_556 ? Cs2 Se2 3.8381(9) 12_556 ? Cs2 Se2 3.8380(9) 9_556 ? Cs2 Se2 3.8380(9) 11_556 ? Cs2 Pt1 3.9549(3) 15_666 ? Se1 U1 2.8890(6) 3 ? Se2 Pt1 2.4708(6) 5_545 ? Se2 U1 2.8144(6) 15_666 ? Se2 U2 2.8933(5) 3_655 ? Se2 Cs2 3.8380(9) 9_556 ? Se3 U1 2.9080(3) 9 ? Se3 U1 2.9080(3) 11 ? Se3 U1 2.9080(3) 3 ? Se3 Cs1 3.4157(13) 9 ? 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 Se2 U1 Se2 77.41(2) 8 15_665 ? Se2 U1 Se1 126.203(18) 8 11 ? Se2 U1 Se1 79.253(16) 15_665 11 ? Se2 U1 Se1 79.253(16) 8 4 ? Se2 U1 Se1 126.203(18) 15_665 4 ? Se1 U1 Se1 76.84(2) 11 4 ? Se2 U1 Se3 141.246(11) 8 . ? Se2 U1 Se3 141.246(11) 15_665 . ? Se1 U1 Se3 76.627(12) 11 . ? Se1 U1 Se3 76.627(12) 4 . ? Se2 U1 Se1 78.202(15) 8 . ? Se2 U1 Se1 123.544(17) 15_665 . ? Se1 U1 Se1 152.06(2) 11 . ? Se1 U1 Se1 97.53(2) 4 . ? Se3 U1 Se1 75.445(12) . . ? Se2 U1 Se1 123.544(17) 8 10 ? Se2 U1 Se1 78.201(15) 15_665 10 ? Se1 U1 Se1 97.53(2) 11 10 ? Se1 U1 Se1 152.06(2) 4 10 ? Se3 U1 Se1 75.446(12) . 10 ? Se1 U1 Se1 74.51(2) . 10 ? Se2 U1 Pt1 84.018(13) 8 11 ? Se2 U1 Pt1 84.018(13) 15_665 11 ? Se1 U1 Pt1 45.712(11) 11 11 ? Se1 U1 Pt1 45.712(11) 4 11 ? Se3 U1 Pt1 99.805(9) . 11 ? Se1 U1 Pt1 141.908(11) . 11 ? Se1 U1 Pt1 141.907(11) 10 11 ? Se2 U1 Pt1 44.700(11) 8 3_655 ? Se2 U1 Pt1 44.700(11) 15_665 3_655 ? Se1 U1 Pt1 86.023(13) 11 3_655 ? Se1 U1 Pt1 86.023(13) 4 3_655 ? Se3 U1 Pt1 157.753(11) . 3_655 ? Se1 U1 Pt1 121.235(12) . 3_655 ? Se1 U1 Pt1 121.234(12) 10 3_655 ? Pt1 U1 Pt1 57.948(9) 11 3_655 ? Se2 U1 Pt1 82.993(13) 8 . ? Se2 U1 Pt1 82.993(13) 15_665 . ? Se1 U1 Pt1 140.431(11) 11 . ? Se1 U1 Pt1 140.431(11) 4 . ? Se3 U1 Pt1 96.862(9) . . ? Se1 U1 Pt1 43.961(11) . . ? Se1 U1 Pt1 43.961(11) 10 . ? Pt1 U1 Pt1 163.333(10) 11 . ? Pt1 U1 Pt1 105.385(12) 3_655 . ? Se2 U1 Cs1 91.686(16) 8 . ? Se2 U1 Cs1 169.009(16) 15_665 . ? Se1 U1 Cs1 108.857(14) 11 . ? Se1 U1 Cs1 51.459(11) 4 . ? Se3 U1 Cs1 49.590(11) . . ? Se1 U1 Cs1 51.404(11) . . ? Se1 U1 Cs1 107.339(14) 10 . ? Pt1 U1 Cs1 96.338(6) 11 . ? Pt1 U1 Cs1 126.870(10) 3_655 . ? Pt1 U1 Cs1 94.442(6) . . ? Se2 U1 Cs1 169.009(16) 8 9 ? Se2 U1 Cs1 91.686(16) 15_665 9 ? Se1 U1 Cs1 51.459(11) 11 9 ? Se1 U1 Cs1 108.857(14) 4 9 ? Se3 U1 Cs1 49.590(11) . 9 ? Se1 U1 Cs1 107.338(14) . 9 ? Se1 U1 Cs1 51.404(11) 10 9 ? Pt1 U1 Cs1 96.338(6) 11 9 ? Pt1 U1 Cs1 126.870(10) 3_655 9 ? Pt1 U1 Cs1 94.442(6) . 9 ? Cs1 U1 Cs1 99.18(2) . 9 ? Se2 U2 Se2 136.52(2) 6_455 4_565 ? Se2 U2 Se2 113.69(2) 6_455 5 ? Se2 U2 Se2 82.68(2) 4_565 5 ? Se2 U2 Se2 82.68(2) 6_455 3 ? Se2 U2 Se2 113.69(2) 4_565 3 ? Se2 U2 Se2 136.52(2) 5 3 ? Se2 U2 Se1 145.442(14) 6_455 8 ? Se2 U2 Se1 76.214(14) 4_565 8 ? Se2 U2 Se1 74.958(14) 5 8 ? Se2 U2 Se1 70.990(14) 3 8 ? Se2 U2 Se1 74.958(14) 6_455 7_455 ? Se2 U2 Se1 70.990(14) 4_565 7_455 ? Se2 U2 Se1 145.442(14) 5 7_455 ? Se2 U2 Se1 76.214(14) 3 7_455 ? Se1 U2 Se1 117.92(2) 8 7_455 ? Se2 U2 Se1 70.990(14) 6_455 2_565 ? Se2 U2 Se1 74.958(14) 4_565 2_565 ? Se2 U2 Se1 76.214(14) 5 2_565 ? Se2 U2 Se1 145.442(14) 3 2_565 ? Se1 U2 Se1 141.28(2) 8 2_565 ? Se1 U2 Se1 75.615(19) 7_455 2_565 ? Se2 U2 Se1 76.213(14) 6_455 . ? Se2 U2 Se1 145.443(14) 4_565 . ? Se2 U2 Se1 70.990(14) 5 . ? Se2 U2 Se1 74.958(14) 3 . ? Se1 U2 Se1 75.616(19) 8 . ? Se1 U2 Se1 141.276(19) 7_455 . ? Se1 U2 Se1 117.92(2) 2_565 . ? Se2 Pt1 Se2 90.84(3) 5 14_665 ? Se2 Pt1 Se1 87.601(17) 5 . ? Se2 Pt1 Se1 172.53(2) 14_665 . ? Se2 Pt1 Se1 172.53(2) 5 10 ? Se2 Pt1 Se1 87.600(17) 14_665 10 ? Se1 Pt1 Se1 93.01(3) . 10 ? Se2 Pt1 U1 128.942(14) 5 3 ? Se2 Pt1 U1 128.942(14) 14_665 3 ? Se1 Pt1 U1 56.686(13) . 3 ? Se1 Pt1 U1 56.688(13) 10 3 ? Se2 Pt1 U1 53.246(13) 5 11_565 ? Se2 Pt1 U1 53.246(13) 14_665 11_565 ? Se1 Pt1 U1 130.024(13) . 11_565 ? Se1 Pt1 U1 130.024(13) 10 11_565 ? U1 Pt1 U1 122.052(9) 3 11_565 ? Se2 Pt1 U1 118.659(14) 5 . ? Se2 Pt1 U1 118.659(14) 14_665 . ? Se1 Pt1 U1 56.291(13) . . ? Se1 Pt1 U1 56.291(13) 10 . ? U1 Pt1 U1 73.332(10) 3 . ? U1 Pt1 U1 164.616(12) 11_565 . ? Se2 Pt1 Cs2 58.71(2) 5 5 ? Se2 Pt1 Cs2 68.96(2) 14_665 5 ? Se1 Pt1 Cs2 104.10(2) . 5 ? Se1 Pt1 Cs2 114.006(19) 10 5 ? U1 Pt1 Cs2 154.671(10) 3 5 ? U1 Pt1 Cs2 82.539(7) 11_565 5 ? U1 Pt1 Cs2 82.175(7) . 5 ? Se2 Pt1 Cs2 68.96(2) 5 13_665 ? Se2 Pt1 Cs2 58.71(2) 14_665 13_665 ? Se1 Pt1 Cs2 114.007(19) . 13_665 ? Se1 Pt1 Cs2 104.09(2) 10 13_665 ? U1 Pt1 Cs2 154.671(10) 3 13_665 ? U1 Pt1 Cs2 82.539(7) 11_565 13_665 ? U1 Pt1 Cs2 82.175(7) . 13_665 ? Cs2 Pt1 Cs2 12.93(4) 5 13_665 ? Cs2 Cs1 Se3 180.0 . . ? Cs2 Cs1 Se2 64.34(2) . . ? Se3 Cs1 Se2 115.66(2) . . ? Cs2 Cs1 Se2 64.34(2) . 3 ? Se3 Cs1 Se2 115.66(2) . 3 ? Se2 Cs1 Se2 79.194(17) . 3 ? Cs2 Cs1 Se2 64.34(2) . 2 ? Se3 Cs1 Se2 115.66(2) . 2 ? Se2 Cs1 Se2 128.68(4) . 2 ? Se2 Cs1 Se2 79.194(17) 3 2 ? Cs2 Cs1 Se2 64.34(2) . 4 ? Se3 Cs1 Se2 115.66(2) . 4 ? Se2 Cs1 Se2 79.193(17) . 4 ? Se2 Cs1 Se2 128.68(4) 3 4 ? Se2 Cs1 Se2 79.194(17) 2 4 ? Cs2 Cs1 Se1 117.49(2) . 2 ? Se3 Cs1 Se1 62.51(2) . 2 ? Se2 Cs1 Se1 129.057(12) . 2 ? Se2 Cs1 Se1 150.914(12) 3 2 ? Se2 Cs1 Se1 76.685(12) 2 2 ? Se2 Cs1 Se1 61.699(12) 4 2 ? Cs2 Cs1 Se1 117.49(2) . 3 ? Se3 Cs1 Se1 62.51(2) . 3 ? Se2 Cs1 Se1 150.915(12) . 3 ? Se2 Cs1 Se1 76.685(12) 3 3 ? Se2 Cs1 Se1 61.699(12) 2 3 ? Se2 Cs1 Se1 129.057(12) 4 3 ? Se1 Cs1 Se1 77.694(17) 2 3 ? Cs2 Cs1 Se1 117.49(2) . 4 ? Se3 Cs1 Se1 62.51(2) . 4 ? Se2 Cs1 Se1 61.700(12) . 4 ? Se2 Cs1 Se1 129.057(12) 3 4 ? Se2 Cs1 Se1 150.914(12) 2 4 ? Se2 Cs1 Se1 76.685(12) 4 4 ? Se1 Cs1 Se1 77.694(17) 2 4 ? Se1 Cs1 Se1 125.01(4) 3 4 ? Cs2 Cs1 Se1 117.49(2) . . ? Se3 Cs1 Se1 62.51(2) . . ? Se2 Cs1 Se1 76.687(12) . . ? Se2 Cs1 Se1 61.699(12) 3 . ? Se2 Cs1 Se1 129.057(12) 2 . ? Se2 Cs1 Se1 150.915(12) 4 . ? Se1 Cs1 Se1 125.01(4) 2 . ? Se1 Cs1 Se1 77.694(18) 3 . ? Se1 Cs1 Se1 77.695(18) 4 . ? Cs2 Cs1 Cs2 0.0 . 9_556 ? Se3 Cs1 Cs2 180.0 . 9_556 ? Se2 Cs1 Cs2 64.34(2) . 9_556 ? Se2 Cs1 Cs2 64.34(2) 3 9_556 ? Se2 Cs1 Cs2 64.34(2) 2 9_556 ? Se2 Cs1 Cs2 64.34(2) 4 9_556 ? Se1 Cs1 Cs2 117.49(2) 2 9_556 ? Se1 Cs1 Cs2 117.49(2) 3 9_556 ? Se1 Cs1 Cs2 117.49(2) 4 9_556 ? Se1 Cs1 Cs2 117.49(2) . 9_556 ? Cs2 Cs1 U1 139.590(11) . 9 ? Se3 Cs1 U1 40.410(11) . 9 ? Se2 Cs1 U1 154.48(3) . 9 ? Se2 Cs1 U1 116.466(15) 3 9 ? Se2 Cs1 U1 75.935(13) 2 9 ? Se2 Cs1 U1 102.341(14) 4 9 ? Se1 Cs1 U1 41.327(14) 2 9 ? Se1 Cs1 U1 40.076(14) 3 9 ? Se1 Cs1 U1 93.56(3) 4 9 ? Se1 Cs1 U1 92.75(3) . 9 ? Cs2 Cs1 U1 139.590(11) 9_556 9 ? Cs2 Cs2 Cs1 180.0 9_556 . ? Cs2 Cs2 Se2 112.71(2) 9_556 . ? Cs1 Cs2 Se2 67.29(2) . . ? Cs2 Cs2 Se2 112.71(2) 9_556 2 ? Cs1 Cs2 Se2 67.29(2) . 2 ? Se2 Cs2 Se2 134.58(4) . 2 ? Cs2 Cs2 Se2 112.71(2) 9_556 4 ? Cs1 Cs2 Se2 67.29(2) . 4 ? Se2 Cs2 Se2 81.429(16) . 4 ? Se2 Cs2 Se2 81.429(16) 2 4 ? Cs2 Cs2 Se2 112.71(2) 9_556 3 ? Cs1 Cs2 Se2 67.29(2) . 3 ? Se2 Cs2 Se2 81.429(16) . 3 ? Se2 Cs2 Se2 81.429(16) 2 3 ? Se2 Cs2 Se2 134.58(4) 4 3 ? Cs2 Cs2 Cs1 0.0 9_556 9_556 ? Cs1 Cs2 Cs1 180.0 . 9_556 ? Se2 Cs2 Cs1 112.71(2) . 9_556 ? Se2 Cs2 Cs1 112.71(2) 2 9_556 ? Se2 Cs2 Cs1 112.71(2) 4 9_556 ? Se2 Cs2 Cs1 112.71(2) 3 9_556 ? Cs2 Cs2 Se2 54.933(17) 9_556 10_556 ? Cs1 Cs2 Se2 125.067(17) . 10_556 ? Se2 Cs2 Se2 57.775(17) . 10_556 ? Se2 Cs2 Se2 167.64(4) 2 10_556 ? Se2 Cs2 Se2 102.815(9) 4 10_556 ? Se2 Cs2 Se2 102.815(9) 3 10_556 ? Cs1 Cs2 Se2 54.933(17) 9_556 10_556 ? Cs2 Cs2 Se2 54.933(17) 9_556 12_556 ? Cs1 Cs2 Se2 125.067(17) . 12_556 ? Se2 Cs2 Se2 102.815(9) . 12_556 ? Se2 Cs2 Se2 102.815(9) 2 12_556 ? Se2 Cs2 Se2 167.64(4) 4 12_556 ? Se2 Cs2 Se2 57.776(17) 3 12_556 ? Cs1 Cs2 Se2 54.933(17) 9_556 12_556 ? Se2 Cs2 Se2 70.726(17) 10_556 12_556 ? Cs2 Cs2 Se2 54.933(17) 9_556 9_556 ? Cs1 Cs2 Se2 125.067(17) . 9_556 ? Se2 Cs2 Se2 167.64(4) . 9_556 ? Se2 Cs2 Se2 57.776(17) 2 9_556 ? Se2 Cs2 Se2 102.815(9) 4 9_556 ? Se2 Cs2 Se2 102.815(9) 3 9_556 ? Cs1 Cs2 Se2 54.933(17) 9_556 9_556 ? Se2 Cs2 Se2 109.87(3) 10_556 9_556 ? Se2 Cs2 Se2 70.726(17) 12_556 9_556 ? Cs2 Cs2 Se2 54.933(17) 9_556 11_556 ? Cs1 Cs2 Se2 125.067(17) . 11_556 ? Se2 Cs2 Se2 102.814(9) . 11_556 ? Se2 Cs2 Se2 102.815(9) 2 11_556 ? Se2 Cs2 Se2 57.776(17) 4 11_556 ? Se2 Cs2 Se2 167.64(4) 3 11_556 ? Cs1 Cs2 Se2 54.933(17) 9_556 11_556 ? Se2 Cs2 Se2 70.726(17) 10_556 11_556 ? Se2 Cs2 Se2 109.87(3) 12_556 11_556 ? Se2 Cs2 Se2 70.726(17) 9_556 11_556 ? Cs2 Cs2 Pt1 83.537(19) 9_556 15_666 ? Cs1 Cs2 Pt1 96.463(18) . 15_666 ? Se2 Cs2 Pt1 69.533(9) . 15_666 ? Se2 Cs2 Pt1 115.886(12) 2 15_666 ? Se2 Cs2 Pt1 150.63(2) 4 15_666 ? Se2 Cs2 Pt1 38.319(9) 3 15_666 ? Cs1 Cs2 Pt1 83.537(18) 9_556 15_666 ? Se2 Cs2 Pt1 65.576(11) 10_556 15_666 ? Se2 Cs2 Pt1 36.931(9) 12_556 15_666 ? Se2 Cs2 Pt1 106.507(19) 9_556 15_666 ? Se2 Cs2 Pt1 132.07(3) 11_556 15_666 ? Pt1 Se1 U1 77.601(15) . 3 ? Pt1 Se1 U1 79.749(16) . . ? U1 Se1 U1 89.235(16) 3 . ? Pt1 Se1 U2 85.380(16) . . ? U1 Se1 U2 99.347(16) 3 . ? U1 Se1 U2 160.85(2) . . ? Pt1 Se1 Cs1 160.98(3) . . ? U1 Se1 Cs1 88.46(2) 3 . ? U1 Se1 Cs1 87.269(19) . . ? U2 Se1 Cs1 109.90(2) . . ? Pt1 Se2 U1 82.055(17) 5_545 15_666 ? Pt1 Se2 U2 87.811(16) 5_545 3_655 ? U1 Se2 U2 103.753(17) 15_666 3_655 ? Pt1 Se2 Cs2 82.97(2) 5_545 . ? U1 Se2 Cs2 104.05(2) 15_666 . ? U2 Se2 Cs2 149.12(2) 3_655 . ? Pt1 Se2 Cs1 117.23(2) 5_545 . ? U1 Se2 Cs1 138.06(2) 15_666 . ? U2 Se2 Cs1 113.29(2) 3_655 . ? Cs2 Se2 Cs1 48.37(3) . . ? Pt1 Se2 Cs2 74.108(18) 5_545 9_556 ? U1 Se2 Cs2 94.035(19) 15_666 9_556 ? U2 Se2 Cs2 152.667(17) 3_655 9_556 ? Cs2 Se2 Cs2 12.36(4) . 9_556 ? Cs1 Se2 Cs2 60.72(3) . 9_556 ? U1 Se3 U1 90.0 9 11 ? U1 Se3 U1 90.0 9 3 ? U1 Se3 U1 180.000(10) 11 3 ? U1 Se3 U1 180.0 9 . ? U1 Se3 U1 90.0 11 . ? U1 Se3 U1 90.0 3 . ? U1 Se3 Cs1 90.0 9 . ? U1 Se3 Cs1 90.0 11 . ? U1 Se3 Cs1 90.0 3 . ? U1 Se3 Cs1 90.0 . . ? U1 Se3 Cs1 90.0 9 9 ? U1 Se3 Cs1 90.0 11 9 ? U1 Se3 Cs1 90.0 3 9 ? U1 Se3 Cs1 90.0 . 9 ? Cs1 Se3 Cs1 180.0 . 9 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 31.81 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.608 _refine_diff_density_min -2.642 _refine_diff_density_rms 0.356 #===END data_cs2u6pd4se17 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dicaesium tetrapalladium(II) hexauranium(IV) decaheptaselenide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cs2 Pd4 Se17 U6' _chemical_formula_sum 'Cs2 Pd4 Se17 U6' _chemical_formula_weight 3461.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cs' 'Cs' -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/m n c' _symmetry_space_group_name_Hall '-P 4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 10.7732(2) _cell_length_b 10.7732(2) _cell_length_c 13.3032(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1543.99(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9956 _cell_measurement_theta_min 2.674 _cell_measurement_theta_max 41.137 _exptl_crystal_description 'tetragonal prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 55.968 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0138 _exptl_absorpt_correction_T_max 0.0834 _exptl_absorpt_process_details 'face-indexed, SADABS (Sheldrick, 2008b)' _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 'Bruker APEX2 CCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 47978 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 41.61 _reflns_number_total 2552 _reflns_number_gt 2486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS (Sheldrick, 2008a)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008a)' _computing_molecular_graphics 'Crystalmaker (Palmer, 2009)' _computing_publication_material 'SHELXL (Sheldrick, 2008a)' _refine_special_details ; . ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0220P)^2^+0.0000sin\q/\l] where P = 1.00000Fo^2^ + 0.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00199(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2552 _refine_ls_number_parameters 40 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.860 _refine_ls_restrained_S_all 1.860 _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 U1 U 0.242264(15) 0.116680(15) 0.0000 0.00604(5) Uani 1 2 d S . . U2 U 0.0000 0.5000 0.2500 0.00642(6) Uani 1 4 d S . . Pd1 Pd 0.14024(3) 0.42840(3) 0.0000 0.00710(7) Uani 1 2 d S . . Cs1 Cs 0.0000 0.0000 0.28021(4) 0.00983(8) Uani 1 4 d S . . Se1 Se 0.09238(3) 0.27650(3) 0.13425(3) 0.00667(7) Uani 1 1 d . . . Se2 Se 0.29112(3) 0.07528(3) 0.37007(3) 0.00720(7) Uani 1 1 d . . . Se3 Se 0.0000 0.0000 0.0000 0.00869(16) Uani 1 8 d S . . 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 U1 0.00520(7) 0.00522(7) 0.00771(8) 0.000 0.000 0.00030(4) U2 0.00573(7) 0.00573(7) 0.00781(10) 0.000 0.000 0.00013(6) Pd1 0.00691(12) 0.00601(12) 0.00839(13) 0.000 0.000 -0.00031(9) Cs1 0.00833(10) 0.00833(10) 0.01284(18) 0.000 0.000 0.000 Se1 0.00611(12) 0.00624(12) 0.00768(13) -0.00064(9) -0.00009(9) 0.00061(10) Se2 0.00647(12) 0.00648(12) 0.00865(13) -0.00061(9) -0.00051(9) 0.00006(9) Se3 0.0060(2) 0.0060(2) 0.0141(4) 0.000 0.000 0.000 _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 U1 Se2 2.7996(4) 8 ? U1 Se2 2.7996(4) 15_665 ? U1 Se3 2.89689(17) . ? U1 Se1 2.8980(4) 11 ? U1 Se1 2.8980(4) 4 ? U1 Se1 2.9601(4) . ? U1 Se1 2.9601(4) 10 ? U1 Pd1 3.4179(4) 11 ? U1 Pd1 3.5335(4) . ? U1 Pd1 3.5571(4) 3_655 ? U1 U1 4.0968(2) 11 ? U1 U1 4.0969(2) 3 ? U2 Se2 2.8764(3) 6_455 ? U2 Se2 2.8764(4) 4_565 ? U2 Se2 2.8764(3) 5 ? U2 Se2 2.8764(3) 3 ? U2 Se1 3.0263(3) 8 ? U2 Se1 3.0263(3) . ? U2 Se1 3.0263(3) 2_565 ? U2 Se1 3.0263(3) 7_455 ? Pd1 Se2 2.4574(4) 5 ? Pd1 Se2 2.4574(4) 14_665 ? Pd1 Se1 2.4766(4) . ? Pd1 Se1 2.4766(4) 10 ? Pd1 U1 3.4179(4) 3 ? Pd1 U1 3.5570(4) 11_565 ? Cs1 Se2 3.4530(4) 3 ? Cs1 Se2 3.4530(4) 2 ? Cs1 Se2 3.4530(4) 4 ? Cs1 Se2 3.4530(4) . ? Cs1 Se1 3.6924(4) 2 ? Cs1 Se1 3.6924(4) 3 ? Cs1 Se1 3.6924(4) 4 ? Cs1 Se1 3.6924(4) . ? Cs1 Se3 3.7276(5) . ? Cs1 U1 4.7209(4) 9 ? Cs1 U1 4.7209(4) 11 ? Se1 U1 2.8980(4) 3 ? Se2 Pd1 2.4574(4) 5_545 ? Se2 U1 2.7996(4) 15_666 ? Se2 U2 2.8763(3) 3_655 ? Se3 U1 2.89691(17) 9 ? Se3 U1 2.89691(17) 11 ? Se3 U1 2.89691(17) 3 ? Se3 Cs1 3.7276(5) 9 ? 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 Se2 U1 Se2 76.253(15) 8 15_665 ? Se2 U1 Se3 141.860(7) 8 . ? Se2 U1 Se3 141.860(7) 15_665 . ? Se2 U1 Se1 124.533(11) 8 11 ? Se2 U1 Se1 78.807(10) 15_665 11 ? Se3 U1 Se1 77.141(7) . 11 ? Se2 U1 Se1 78.807(10) 8 4 ? Se2 U1 Se1 124.533(11) 15_665 4 ? Se3 U1 Se1 77.141(7) . 4 ? Se1 U1 Se1 76.092(14) 11 4 ? Se2 U1 Se1 78.702(10) 8 . ? Se2 U1 Se1 123.307(11) 15_665 . ? Se3 U1 Se1 76.168(7) . . ? Se1 U1 Se1 153.298(12) 11 . ? Se1 U1 Se1 98.606(13) 4 . ? Se2 U1 Se1 123.307(11) 8 10 ? Se2 U1 Se1 78.702(10) 15_665 10 ? Se3 U1 Se1 76.168(7) . 10 ? Se1 U1 Se1 98.606(13) 11 10 ? Se1 U1 Se1 153.298(12) 4 10 ? Se1 U1 Se1 74.223(14) . 10 ? Se2 U1 Pd1 82.843(9) 8 11 ? Se2 U1 Pd1 82.843(9) 15_665 11 ? Se3 U1 Pd1 100.207(7) . 11 ? Se1 U1 Pd1 45.249(8) 11 11 ? Se1 U1 Pd1 45.249(8) 4 11 ? Se1 U1 Pd1 142.289(7) . 11 ? Se1 U1 Pd1 142.289(7) 10 11 ? Se2 U1 Pd1 83.176(9) 8 . ? Se2 U1 Pd1 83.176(9) 15_665 . ? Se3 U1 Pd1 97.593(7) . . ? Se1 U1 Pd1 141.096(7) 11 . ? Se1 U1 Pd1 141.096(7) 4 . ? Se1 U1 Pd1 43.737(7) . . ? Se1 U1 Pd1 43.737(7) 10 . ? Pd1 U1 Pd1 162.200(9) 11 . ? Se2 U1 Pd1 43.480(8) 8 3_655 ? Se2 U1 Pd1 43.480(8) 15_665 3_655 ? Se3 U1 Pd1 158.375(8) . 3_655 ? Se1 U1 Pd1 85.899(9) 11 3_655 ? Se1 U1 Pd1 85.899(9) 4 3_655 ? Se1 U1 Pd1 120.174(9) . 3_655 ? Se1 U1 Pd1 120.174(9) 10 3_655 ? Pd1 U1 Pd1 58.168(10) 11 3_655 ? Pd1 U1 Pd1 104.032(12) . 3_655 ? Se2 U1 U1 124.525(9) 8 11 ? Se2 U1 U1 124.525(9) 15_665 11 ? Se3 U1 U1 45.0 . 11 ? Se1 U1 U1 46.249(7) 11 11 ? Se1 U1 U1 46.249(8) 4 11 ? Se1 U1 U1 111.648(7) . 11 ? Se1 U1 U1 111.648(7) 10 11 ? Pd1 U1 U1 55.206(7) 11 11 ? Pd1 U1 U1 142.593(7) . 11 ? Pd1 U1 U1 113.374(8) 3_655 11 ? Se2 U1 U1 123.060(9) 8 3 ? Se2 U1 U1 123.060(9) 15_665 3 ? Se3 U1 U1 45.0 . 3 ? Se1 U1 U1 112.135(7) 11 3 ? Se1 U1 U1 112.135(7) 4 3 ? Se1 U1 U1 45.008(7) . 3 ? Se1 U1 U1 45.008(7) 10 3 ? Pd1 U1 U1 145.207(7) 11 3 ? Pd1 U1 U1 52.593(7) . 3 ? Pd1 U1 U1 156.626(8) 3_655 3 ? U1 U1 U1 90.0 11 3 ? Se2 U2 Se2 138.557(13) 6_455 4_565 ? Se2 U2 Se2 112.533(14) 6_455 5 ? Se2 U2 Se2 82.367(14) 4_565 5 ? Se2 U2 Se2 82.367(14) 6_455 3 ? Se2 U2 Se2 112.533(14) 4_565 3 ? Se2 U2 Se2 138.557(13) 5 3 ? Se2 U2 Se1 144.319(9) 6_455 8 ? Se2 U2 Se1 75.545(9) 4_565 8 ? Se2 U2 Se1 75.690(10) 5 8 ? Se2 U2 Se1 71.610(9) 3 8 ? Se2 U2 Se1 75.545(9) 6_455 . ? Se2 U2 Se1 144.319(9) 4_565 . ? Se2 U2 Se1 71.610(9) 5 . ? Se2 U2 Se1 75.690(10) 3 . ? Se1 U2 Se1 74.669(13) 8 . ? Se2 U2 Se1 71.610(9) 6_455 2_565 ? Se2 U2 Se1 75.690(10) 4_565 2_565 ? Se2 U2 Se1 75.545(9) 5 2_565 ? Se2 U2 Se1 144.319(9) 3 2_565 ? Se1 U2 Se1 141.456(13) 8 2_565 ? Se1 U2 Se1 118.833(13) . 2_565 ? Se2 U2 Se1 75.690(10) 6_455 7_455 ? Se2 U2 Se1 71.610(9) 4_565 7_455 ? Se2 U2 Se1 144.319(9) 5 7_455 ? Se2 U2 Se1 75.545(9) 3 7_455 ? Se1 U2 Se1 118.833(13) 8 7_455 ? Se1 U2 Se1 141.457(13) . 7_455 ? Se1 U2 Se1 74.669(13) 2_565 7_455 ? Se2 Pd1 Se2 89.40(2) 5 14_665 ? Se2 Pd1 Se1 88.906(12) 5 . ? Se2 Pd1 Se1 174.501(19) 14_665 . ? Se2 Pd1 Se1 174.501(19) 5 10 ? Se2 Pd1 Se1 88.906(12) 14_665 10 ? Se1 Pd1 Se1 92.300(19) . 10 ? Se2 Pd1 U1 128.428(12) 5 3 ? Se2 Pd1 U1 128.428(12) 14_665 3 ? Se1 Pd1 U1 56.203(10) . 3 ? Se1 Pd1 U1 56.203(10) 10 3 ? Se2 Pd1 U1 121.224(12) 5 . ? Se2 Pd1 U1 121.224(12) 14_665 . ? Se1 Pd1 U1 55.722(10) . . ? Se1 Pd1 U1 55.722(10) 10 . ? U1 Pd1 U1 72.200(9) 3 . ? Se2 Pd1 U1 51.622(10) 5 11_565 ? Se2 Pd1 U1 51.622(10) 14_665 11_565 ? Se1 Pd1 U1 130.107(11) . 11_565 ? Se1 Pd1 U1 130.107(11) 10 11_565 ? U1 Pd1 U1 121.833(10) 3 11_565 ? U1 Pd1 U1 165.967(12) . 11_565 ? Se2 Cs1 Se2 83.115(6) 3 2 ? Se2 Cs1 Se2 139.487(19) 3 4 ? Se2 Cs1 Se2 83.115(6) 2 4 ? Se2 Cs1 Se2 83.116(6) 3 . ? Se2 Cs1 Se2 139.488(19) 2 . ? Se2 Cs1 Se2 83.115(6) 4 . ? Se2 Cs1 Se1 148.375(9) 3 2 ? Se2 Cs1 Se1 75.390(8) 2 2 ? Se2 Cs1 Se1 60.832(8) 4 2 ? Se2 Cs1 Se1 128.050(8) . 2 ? Se2 Cs1 Se1 75.390(8) 3 3 ? Se2 Cs1 Se1 60.832(8) 2 3 ? Se2 Cs1 Se1 128.051(8) 4 3 ? Se2 Cs1 Se1 148.375(9) . 3 ? Se1 Cs1 Se1 73.948(8) 2 3 ? Se2 Cs1 Se1 128.051(8) 3 4 ? Se2 Cs1 Se1 148.375(9) 2 4 ? Se2 Cs1 Se1 75.390(8) 4 4 ? Se2 Cs1 Se1 60.831(8) . 4 ? Se1 Cs1 Se1 73.948(8) 2 4 ? Se1 Cs1 Se1 116.550(16) 3 4 ? Se2 Cs1 Se1 60.832(8) 3 . ? Se2 Cs1 Se1 128.051(8) 2 . ? Se2 Cs1 Se1 148.375(9) 4 . ? Se2 Cs1 Se1 75.390(8) . . ? Se1 Cs1 Se1 116.550(16) 2 . ? Se1 Cs1 Se1 73.948(8) 3 . ? Se1 Cs1 Se1 73.948(8) 4 . ? Se2 Cs1 Se3 110.256(10) 3 . ? Se2 Cs1 Se3 110.256(10) 2 . ? Se2 Cs1 Se3 110.256(10) 4 . ? Se2 Cs1 Se3 110.256(10) . . ? Se1 Cs1 Se3 58.275(8) 2 . ? Se1 Cs1 Se3 58.275(8) 3 . ? Se1 Cs1 Se3 58.275(8) 4 . ? Se1 Cs1 Se3 58.275(8) . . ? Se2 Cs1 U1 99.288(8) 3 . ? Se2 Cs1 U1 146.935(12) 2 . ? Se2 Cs1 U1 112.666(8) 4 . ? Se2 Cs1 U1 73.064(7) . . ? Se1 Cs1 U1 87.054(10) 2 . ? Se1 Cs1 U1 87.653(10) 3 . ? Se1 Cs1 U1 37.866(7) 4 . ? Se1 Cs1 U1 38.829(7) . . ? Se3 Cs1 U1 37.852(4) . . ? Se2 Cs1 U1 112.666(8) 3 9 ? Se2 Cs1 U1 73.064(7) 2 9 ? Se2 Cs1 U1 99.288(8) 4 9 ? Se2 Cs1 U1 146.935(12) . 9 ? Se1 Cs1 U1 38.829(7) 2 9 ? Se1 Cs1 U1 37.866(7) 3 9 ? Se1 Cs1 U1 87.653(10) 4 9 ? Se1 Cs1 U1 87.055(10) . 9 ? Se3 Cs1 U1 37.852(4) . 9 ? U1 Cs1 U1 75.705(8) . 9 ? Se2 Cs1 U1 146.935(12) 3 11 ? Se2 Cs1 U1 112.666(8) 2 11 ? Se2 Cs1 U1 73.064(7) 4 11 ? Se2 Cs1 U1 99.287(8) . 11 ? Se1 Cs1 U1 37.866(7) 2 11 ? Se1 Cs1 U1 87.055(10) 3 11 ? Se1 Cs1 U1 38.829(7) 4 11 ? Se1 Cs1 U1 87.652(10) . 11 ? Se3 Cs1 U1 37.852(4) . 11 ? U1 Cs1 U1 51.430(5) . 11 ? U1 Cs1 U1 51.431(5) 9 11 ? Pd1 Se1 U1 78.548(12) . 3 ? Pd1 Se1 U1 80.541(12) . . ? U1 Se1 U1 88.743(11) 3 . ? Pd1 Se1 U2 84.818(12) . . ? U1 Se1 U2 99.164(10) 3 . ? U1 Se1 U2 161.654(13) . . ? Pd1 Se1 Cs1 165.555(15) . . ? U1 Se1 Cs1 90.683(10) 3 . ? U1 Se1 Cs1 89.715(10) . . ? U2 Se1 Cs1 106.599(11) . . ? Pd1 Se2 U1 84.898(13) 5_545 15_666 ? Pd1 Se2 U2 88.486(13) 5_545 3_655 ? U1 Se2 U2 105.264(11) 15_666 3_655 ? Pd1 Se2 Cs1 111.445(15) 5_545 . ? U1 Se2 Cs1 134.500(13) 15_666 . ? U2 Se2 Cs1 116.879(13) 3_655 . ? U1 Se3 U1 180.0 . 9 ? U1 Se3 U1 90.0 . 11 ? U1 Se3 U1 90.0 9 11 ? U1 Se3 U1 90.0 . 3 ? U1 Se3 U1 90.0 9 3 ? U1 Se3 U1 180.000(6) 11 3 ? U1 Se3 Cs1 90.0 . 9 ? U1 Se3 Cs1 90.0 9 9 ? U1 Se3 Cs1 90.0 11 9 ? U1 Se3 Cs1 90.0 3 9 ? U1 Se3 Cs1 90.0 . . ? U1 Se3 Cs1 90.0 9 . ? U1 Se3 Cs1 90.0 11 . ? U1 Se3 Cs1 90.0 3 . ? Cs1 Se3 Cs1 180.0 9 . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 14.337 _refine_diff_density_min -2.739 _refine_diff_density_rms 0.647 #===END data_csupds _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dirubidium tetrapalladium(II) hexauranium(IV) decaheptasulfide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cs2 Pd4 S17 U6' _chemical_formula_weight 2664.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cs' 'Cs' -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 '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/mnc _symmetry_space_group_name_Hall '-P 4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 10.42770(10) _cell_length_b 10.42770(10) _cell_length_c 12.7769(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1389.32(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4576 _cell_measurement_theta_min 2.520 _cell_measurement_theta_max 28.070 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2236 _exptl_absorpt_coefficient_mu 41.206 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0669 _exptl_absorpt_correction_T_max 0.4256 _exptl_absorpt_process_details 'face indexed, SADABS (Sheldrick, 2008b)' _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 'Bruker APEXII CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15154 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.62 _reflns_number_total 900 _reflns_number_gt 864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS (Sheldrick, 2008a)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008a)' _computing_molecular_graphics 'Crystalmaker (Palmer, 2009)' _computing_publication_material 'SHELXL (Sheldrick, 2008a)' _refine_special_details ; . ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0136P)^2^+0.0000sin\q/\l] where P = 1.00000Fo^2^ + 0.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00028(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 900 _refine_ls_number_parameters 40 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0169 _refine_ls_R_factor_gt 0.0148 _refine_ls_wR_factor_ref 0.0305 _refine_ls_wR_factor_gt 0.0301 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _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 U1 U 0.24122(2) 0.11841(2) 0.0000 0.00481(7) Uani 1 2 d S . . U2 U 0.0000 0.5000 0.2500 0.00517(8) Uani 1 4 d S . . Cs1 Cs 0.0000 0.0000 0.28522(4) 0.00753(11) Uani 1 4 d S . . Pd1 Pd 0.14308(4) 0.42962(4) 0.0000 0.00525(10) Uani 1 2 d S . . S1 S 0.09158(10) 0.27844(10) 0.13130(8) 0.0064(2) Uani 1 1 d . . . S2 S 0.29498(10) 0.07620(10) 0.37068(8) 0.0065(2) Uani 1 1 d . . . S3 S 0.0000 0.0000 0.0000 0.0068(6) Uani 1 8 d S . . 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 U1 0.00479(12) 0.00513(12) 0.00450(11) 0.000 0.000 0.00020(8) U2 0.00567(11) 0.00567(11) 0.00419(15) 0.000 0.000 0.00005(11) Cs1 0.00714(16) 0.00714(16) 0.0083(2) 0.000 0.000 0.000 Pd1 0.0060(2) 0.0048(2) 0.0049(2) 0.000 0.000 -0.00024(17) S1 0.0072(5) 0.0066(5) 0.0054(5) -0.0003(4) -0.0002(4) 0.0000(4) S2 0.0066(5) 0.0073(5) 0.0056(5) 0.0002(4) -0.0008(4) 0.0000(4) S3 0.0062(8) 0.0062(8) 0.0080(14) 0.000 0.000 0.000 _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 U1 S2 2.6777(10) 8 ? U1 S2 2.6777(10) 15_665 ? U1 S1 2.7856(10) 11 ? U1 S1 2.7856(10) 4 ? U1 S3 2.8021(2) . ? U1 S1 2.8345(10) . ? U1 S1 2.8345(10) 10 ? U1 Pd1 3.3607(5) 11 ? U1 Pd1 3.4027(5) . ? U1 Pd1 3.4420(5) 3_655 ? U1 U1 3.9628(3) 3 ? U1 U1 3.9628(3) 11 ? U2 S2 2.7531(10) 6_455 ? U2 S2 2.7531(10) 4_565 ? U2 S2 2.7531(10) 5 ? U2 S2 2.7531(10) 3 ? U2 S1 2.9240(10) 8 ? U2 S1 2.9240(10) 2_565 ? U2 S1 2.9240(10) 7_455 ? U2 S1 2.9240(10) . ? U2 Pd1 3.6010(2) 9_565 ? U2 Pd1 3.6010(2) 7_455 ? U2 Pd1 3.6010(2) 15_666 ? U2 Pd1 3.6011(2) . ? Cs1 S2 3.3594(10) 3 ? Cs1 S2 3.3594(10) 2 ? Cs1 S2 3.3594(10) 4 ? Cs1 S2 3.3594(10) . ? Cs1 S1 3.6345(11) . ? Cs1 S1 3.6345(11) 2 ? Cs1 S1 3.6345(11) 3 ? Cs1 S1 3.6345(11) 4 ? Cs1 S3 3.6442(5) . ? Cs1 U1 4.5970(4) 9 ? Cs1 U1 4.5970(4) 11 ? Cs1 U1 4.5970(4) 3 ? Pd1 S2 2.3417(10) 5 ? Pd1 S2 2.3417(10) 14_665 ? Pd1 S1 2.3639(11) 10 ? Pd1 S1 2.3639(11) . ? Pd1 U1 3.3606(5) 3 ? Pd1 U1 3.4420(5) 11_565 ? Pd1 U2 3.6011(2) 9_565 ? S1 U1 2.7856(10) 3 ? S2 Pd1 2.3417(10) 5_545 ? S2 U1 2.6777(10) 15_666 ? S2 U2 2.7531(10) 3_655 ? S3 U1 2.8021(2) 9 ? S3 U1 2.8021(2) 11 ? S3 U1 2.8021(2) 3 ? S3 Cs1 3.6442(5) 9 ? 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 S2 U1 S2 76.20(4) 8 15_665 ? S2 U1 S1 122.53(3) 8 11 ? S2 U1 S1 78.14(3) 15_665 11 ? S2 U1 S1 78.14(3) 8 4 ? S2 U1 S1 122.53(3) 15_665 4 ? S1 U1 S1 74.06(4) 11 4 ? S2 U1 S3 141.89(2) 8 . ? S2 U1 S3 141.89(2) 15_665 . ? S1 U1 S3 77.21(2) 11 . ? S1 U1 S3 77.21(2) 4 . ? S2 U1 S1 80.08(3) 8 . ? S2 U1 S1 123.92(3) 15_665 . ? S1 U1 S1 153.63(4) 11 . ? S1 U1 S1 100.55(4) 4 . ? S3 U1 S1 76.42(2) . . ? S2 U1 S1 123.92(3) 8 10 ? S2 U1 S1 80.08(3) 15_665 10 ? S1 U1 S1 100.55(4) 11 10 ? S1 U1 S1 153.63(4) 4 10 ? S3 U1 S1 76.42(2) . 10 ? S1 U1 S1 72.58(4) . 10 ? S2 U1 Pd1 81.84(2) 8 11 ? S2 U1 Pd1 81.84(2) 15_665 11 ? S1 U1 Pd1 44.01(2) 11 11 ? S1 U1 Pd1 44.01(2) 4 11 ? S3 U1 Pd1 99.627(10) . 11 ? S1 U1 Pd1 143.08(2) . 11 ? S1 U1 Pd1 143.08(2) 10 11 ? S2 U1 Pd1 83.81(2) 8 . ? S2 U1 Pd1 83.81(2) 15_665 . ? S1 U1 Pd1 142.33(2) 11 . ? S1 U1 Pd1 142.33(2) 4 . ? S3 U1 Pd1 98.641(10) . . ? S1 U1 Pd1 43.36(2) . . ? S1 U1 Pd1 43.36(2) 10 . ? Pd1 U1 Pd1 161.732(11) 11 . ? S2 U1 Pd1 42.76(2) 8 3_655 ? S2 U1 Pd1 42.76(2) 15_665 3_655 ? S1 U1 Pd1 85.40(2) 11 3_655 ? S1 U1 Pd1 85.40(2) 4 3_655 ? S3 U1 Pd1 158.140(11) . 3_655 ? S1 U1 Pd1 120.33(2) . 3_655 ? S1 U1 Pd1 120.33(2) 10 3_655 ? Pd1 U1 Pd1 58.513(13) 11 3_655 ? Pd1 U1 Pd1 103.219(16) . 3_655 ? S2 U1 U1 124.32(2) 8 3 ? S2 U1 U1 124.32(2) 15_665 3 ? S1 U1 U1 112.70(2) 11 3 ? S1 U1 U1 112.70(2) 4 3 ? S3 U1 U1 45.0 . 3 ? S1 U1 U1 44.66(2) . 3 ? S1 U1 U1 44.66(2) 10 3 ? Pd1 U1 U1 144.627(10) 11 3 ? Pd1 U1 U1 53.640(10) . 3 ? Pd1 U1 U1 156.860(11) 3_655 3 ? S2 U1 U1 123.29(2) 8 11 ? S2 U1 U1 123.29(2) 15_665 11 ? S1 U1 U1 45.66(2) 11 11 ? S1 U1 U1 45.66(2) 4 11 ? S3 U1 U1 45.0 . 11 ? S1 U1 U1 112.28(2) . 11 ? S1 U1 U1 112.29(2) 10 11 ? Pd1 U1 U1 54.627(10) 11 11 ? Pd1 U1 U1 143.640(10) . 11 ? Pd1 U1 U1 113.140(11) 3_655 11 ? U1 U1 U1 90.0 3 11 ? S2 U2 S2 139.64(4) 6_455 4_565 ? S2 U2 S2 111.88(4) 6_455 5 ? S2 U2 S2 82.27(4) 4_565 5 ? S2 U2 S2 82.27(4) 6_455 3 ? S2 U2 S2 111.88(4) 4_565 3 ? S2 U2 S2 139.64(4) 5 3 ? S2 U2 S1 144.08(3) 6_455 8 ? S2 U2 S1 74.64(3) 4_565 8 ? S2 U2 S1 76.77(3) 5 8 ? S2 U2 S1 71.58(3) 3 8 ? S2 U2 S1 71.58(3) 6_455 2_565 ? S2 U2 S1 76.77(3) 4_565 2_565 ? S2 U2 S1 74.64(3) 5 2_565 ? S2 U2 S1 144.08(3) 3 2_565 ? S1 U2 S1 141.73(4) 8 2_565 ? S2 U2 S1 76.77(3) 6_455 7_455 ? S2 U2 S1 71.58(3) 4_565 7_455 ? S2 U2 S1 144.08(3) 5 7_455 ? S2 U2 S1 74.64(3) 3 7_455 ? S1 U2 S1 117.51(4) 8 7_455 ? S1 U2 S1 75.70(4) 2_565 7_455 ? S2 U2 S1 74.64(3) 6_455 . ? S2 U2 S1 144.08(3) 4_565 . ? S2 U2 S1 71.58(3) 5 . ? S2 U2 S1 76.77(3) 3 . ? S1 U2 S1 75.70(4) 8 . ? S1 U2 S1 117.51(4) 2_565 . ? S1 U2 S1 141.73(4) 7_455 . ? S2 U2 Pd1 40.56(2) 6_455 9_565 ? S2 U2 Pd1 117.27(2) 4_565 9_565 ? S2 U2 Pd1 76.47(2) 5 9_565 ? S2 U2 Pd1 122.38(2) 3 9_565 ? S1 U2 Pd1 148.65(2) 8 9_565 ? S1 U2 Pd1 40.85(2) 2_565 9_565 ? S1 U2 Pd1 93.79(2) 7_455 9_565 ? S1 U2 Pd1 80.58(2) . 9_565 ? S2 U2 Pd1 117.27(2) 6_455 7_455 ? S2 U2 Pd1 40.56(2) 4_565 7_455 ? S2 U2 Pd1 122.38(2) 5 7_455 ? S2 U2 Pd1 76.47(2) 3 7_455 ? S1 U2 Pd1 80.58(2) 8 7_455 ? S1 U2 Pd1 93.79(2) 2_565 7_455 ? S1 U2 Pd1 40.85(2) 7_455 7_455 ? S1 U2 Pd1 148.65(2) . 7_455 ? Pd1 U2 Pd1 128.166(13) 9_565 7_455 ? S2 U2 Pd1 122.38(2) 6_455 15_666 ? S2 U2 Pd1 76.47(2) 4_565 15_666 ? S2 U2 Pd1 117.27(2) 5 15_666 ? S2 U2 Pd1 40.56(2) 3 15_666 ? S1 U2 Pd1 40.85(2) 8 15_666 ? S1 U2 Pd1 148.65(2) 2_565 15_666 ? S1 U2 Pd1 80.58(2) 7_455 15_666 ? S1 U2 Pd1 93.79(2) . 15_666 ? Pd1 U2 Pd1 162.880(14) 9_565 15_666 ? Pd1 U2 Pd1 54.996(12) 7_455 15_666 ? S2 U2 Pd1 76.47(2) 6_455 . ? S2 U2 Pd1 122.38(2) 4_565 . ? S2 U2 Pd1 40.56(2) 5 . ? S2 U2 Pd1 117.27(2) 3 . ? S1 U2 Pd1 93.79(2) 8 . ? S1 U2 Pd1 80.58(2) 2_565 . ? S1 U2 Pd1 148.65(2) 7_455 . ? S1 U2 Pd1 40.85(2) . . ? Pd1 U2 Pd1 54.997(12) 9_565 . ? Pd1 U2 Pd1 162.880(14) 7_455 . ? Pd1 U2 Pd1 128.165(13) 15_666 . ? S2 Cs1 S2 83.935(12) 3 2 ? S2 Cs1 S2 142.06(4) 3 4 ? S2 Cs1 S2 83.935(12) 2 4 ? S2 Cs1 S2 83.935(12) 3 . ? S2 Cs1 S2 142.06(4) 2 . ? S2 Cs1 S2 83.935(12) 4 . ? S2 Cs1 S1 60.43(2) 3 . ? S2 Cs1 S1 127.26(2) 2 . ? S2 Cs1 S1 147.69(2) 4 . ? S2 Cs1 S1 75.31(2) . . ? S2 Cs1 S1 147.69(2) 3 2 ? S2 Cs1 S1 75.31(2) 2 2 ? S2 Cs1 S1 60.43(2) 4 2 ? S2 Cs1 S1 127.26(2) . 2 ? S1 Cs1 S1 114.49(3) . 2 ? S2 Cs1 S1 75.31(2) 3 3 ? S2 Cs1 S1 60.43(2) 2 3 ? S2 Cs1 S1 127.26(2) 4 3 ? S2 Cs1 S1 147.69(2) . 3 ? S1 Cs1 S1 72.976(16) . 3 ? S1 Cs1 S1 72.976(16) 2 3 ? S2 Cs1 S1 127.26(2) 3 4 ? S2 Cs1 S1 147.69(2) 2 4 ? S2 Cs1 S1 75.31(2) 4 4 ? S2 Cs1 S1 60.43(2) . 4 ? S1 Cs1 S1 72.976(16) . 4 ? S1 Cs1 S1 72.976(16) 2 4 ? S1 Cs1 S1 114.49(3) 3 4 ? S2 Cs1 S3 108.968(19) 3 . ? S2 Cs1 S3 108.968(19) 2 . ? S2 Cs1 S3 108.968(19) 4 . ? S2 Cs1 S3 108.969(19) . . ? S1 Cs1 S3 57.242(17) . . ? S1 Cs1 S3 57.243(17) 2 . ? S1 Cs1 S3 57.243(17) 3 . ? S1 Cs1 S3 57.243(17) 4 . ? S2 Cs1 U1 111.974(18) 3 9 ? S2 Cs1 U1 72.128(18) 2 9 ? S2 Cs1 U1 98.116(18) 4 9 ? S2 Cs1 U1 145.31(2) . 9 ? S1 Cs1 U1 85.952(18) . 9 ? S1 Cs1 U1 38.068(17) 2 9 ? S1 Cs1 U1 37.297(16) 3 9 ? S1 Cs1 U1 86.424(19) 4 9 ? S3 Cs1 U1 37.558(4) . 9 ? S2 Cs1 U1 145.31(2) 3 11 ? S2 Cs1 U1 111.974(18) 2 11 ? S2 Cs1 U1 72.128(18) 4 11 ? S2 Cs1 U1 98.116(18) . 11 ? S1 Cs1 U1 86.424(19) . 11 ? S1 Cs1 U1 37.297(16) 2 11 ? S1 Cs1 U1 85.952(18) 3 11 ? S1 Cs1 U1 38.068(17) 4 11 ? S3 Cs1 U1 37.558(4) . 11 ? U1 Cs1 U1 51.065(5) 9 11 ? S2 Cs1 U1 72.128(18) 3 3 ? S2 Cs1 U1 98.116(18) 2 3 ? S2 Cs1 U1 145.31(2) 4 3 ? S2 Cs1 U1 111.974(18) . 3 ? S1 Cs1 U1 37.297(16) . 3 ? S1 Cs1 U1 86.424(19) 2 3 ? S1 Cs1 U1 38.068(17) 3 3 ? S1 Cs1 U1 85.952(18) 4 3 ? S3 Cs1 U1 37.558(4) . 3 ? U1 Cs1 U1 51.065(5) 9 3 ? U1 Cs1 U1 75.116(9) 11 3 ? S2 Pd1 S2 89.75(5) 5 14_665 ? S2 Pd1 S1 177.09(4) 5 10 ? S2 Pd1 S1 89.84(4) 14_665 10 ? S2 Pd1 S1 89.84(4) 5 . ? S2 Pd1 S1 177.09(4) 14_665 . ? S1 Pd1 S1 90.42(5) 10 . ? S2 Pd1 U1 127.25(3) 5 3 ? S2 Pd1 U1 127.25(3) 14_665 3 ? S1 Pd1 U1 54.96(3) 10 3 ? S1 Pd1 U1 54.96(3) . 3 ? S2 Pd1 U1 122.65(3) 5 . ? S2 Pd1 U1 122.65(3) 14_665 . ? S1 Pd1 U1 55.41(3) 10 . ? S1 Pd1 U1 55.41(3) . . ? U1 Pd1 U1 71.733(11) 3 . ? S2 Pd1 U1 50.93(3) 5 11_565 ? S2 Pd1 U1 50.93(3) 14_665 11_565 ? S1 Pd1 U1 130.39(3) 10 11_565 ? S1 Pd1 U1 130.39(3) . 11_565 ? U1 Pd1 U1 121.486(13) 3 11_565 ? U1 Pd1 U1 166.781(16) . 11_565 ? S2 Pd1 U2 127.38(3) 5 9_565 ? S2 Pd1 U2 49.86(3) 14_665 9_565 ? S1 Pd1 U2 54.00(3) 10 9_565 ? S1 Pd1 U2 132.17(3) . 9_565 ? U1 Pd1 U2 77.466(7) 3 9_565 ? U1 Pd1 U2 108.602(7) . 9_565 ? U1 Pd1 U2 76.455(7) 11_565 9_565 ? S2 Pd1 U2 49.86(3) 5 . ? S2 Pd1 U2 127.38(3) 14_665 . ? S1 Pd1 U2 132.17(3) 10 . ? S1 Pd1 U2 54.01(2) . . ? U1 Pd1 U2 77.466(7) 3 . ? U1 Pd1 U2 108.602(7) . . ? U1 Pd1 U2 76.455(7) 11_565 . ? U2 Pd1 U2 125.003(12) 9_565 . ? Pd1 S1 U1 81.03(3) . 3 ? Pd1 S1 U1 81.23(3) . . ? U1 S1 U1 89.67(3) 3 . ? Pd1 S1 U2 85.14(3) . . ? U1 S1 U2 99.54(3) 3 . ? U1 S1 U2 162.17(4) . . ? Pd1 S1 Cs1 167.54(4) . . ? U1 S1 Cs1 90.46(3) 3 . ? U1 S1 Cs1 89.69(3) . . ? U2 S1 Cs1 105.35(3) . . ? Pd1 S2 U1 86.31(3) 5_545 15_666 ? Pd1 S2 U2 89.58(3) 5_545 3_655 ? U1 S2 U2 106.79(3) 15_666 3_655 ? Pd1 S2 Cs1 109.12(4) 5_545 . ? U1 S2 Cs1 132.65(4) 15_666 . ? U2 S2 Cs1 117.43(3) 3_655 . ? U1 S3 U1 180.0 . 9 ? U1 S3 U1 90.0 . 11 ? U1 S3 U1 90.0 9 11 ? U1 S3 U1 90.0 . 3 ? U1 S3 U1 90.0 9 3 ? U1 S3 U1 180.000(8) 11 3 ? U1 S3 Cs1 90.0 . . ? U1 S3 Cs1 90.0 9 . ? U1 S3 Cs1 90.0 11 . ? U1 S3 Cs1 90.0 3 . ? U1 S3 Cs1 90.0 . 9 ? U1 S3 Cs1 90.0 9 9 ? U1 S3 Cs1 90.0 11 9 ? U1 S3 Cs1 90.0 3 9 ? Cs1 S3 Cs1 180.0 . 9 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 28.62 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.050 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.207 #===END data_rbuptse _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dirubidium tetraplatinum(II) hexauranium(IV) decaheptaselenide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Pt4 Rb2 Se17 U6' _chemical_formula_weight 3721.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 '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/mnc _symmetry_space_group_name_Hall '-P 4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 10.55910(10) _cell_length_b 10.55910(10) _cell_length_c 13.4043(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1494.51(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3666 _cell_measurement_theta_min 2.456 _cell_measurement_theta_max 33.286 _exptl_crystal_description 'tapered needle' _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 74.950 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0260 _exptl_absorpt_correction_T_max 0.3994 _exptl_absorpt_process_details 'face indexed, SADABS (Sheldrick, 2008b)' _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 'Bruker APEXII CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20306 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 35.87 _reflns_number_total 1774 _reflns_number_gt 1457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS (Sheldrick, 2008a)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008a)' _computing_molecular_graphics 'Crystalmaker (Palmer, 2009)' _computing_publication_material 'SHELXL (Sheldrick, 2008a)' _refine_special_details ; . ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0309P)^2^+0.0000sin\q/\l] where P = 1.00000Fo^2^ + 0.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00036(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1774 _refine_ls_number_parameters 43 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 U1 U 0.24676(3) 0.12145(3) 0.0000 0.00953(8) Uani 1 2 d S . . U2 U 0.0000 0.5000 0.2500 0.00899(10) Uani 1 4 d S . . Pt1 Pt 0.14103(3) 0.42744(3) 0.0000 0.00894(8) Uani 1 2 d S . . Rb1 Rb 0.0000 0.0000 0.25144(17) 0.0102(4) Uani 0.50 4 d SP . . Rb2 Rb 0.0000 0.0000 0.47019(18) 0.0131(4) Uani 0.50 4 d SP . . Se1 Se 0.08902(6) 0.27595(6) 0.13562(4) 0.00929(12) Uani 1 1 d . . . Se2 Se 0.27906(6) 0.07031(6) 0.36827(5) 0.01009(12) Uani 1 1 d . . . Se3 Se 0.0000 0.0000 0.0000 0.0169(4) Uani 1 8 d S . . 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 U1 0.00974(15) 0.00973(15) 0.00910(14) 0.000 0.000 0.00007(11) U2 0.01060(13) 0.01060(13) 0.00576(17) 0.000 0.000 0.00036(16) Pt1 0.01044(15) 0.01031(15) 0.00608(14) 0.000 0.000 -0.00035(11) Rb1 0.0116(6) 0.0116(6) 0.0074(9) 0.000 0.000 0.000 Rb2 0.0121(6) 0.0121(6) 0.0152(10) 0.000 0.000 0.000 Se1 0.0110(3) 0.0110(3) 0.0059(3) 0.0000(2) -0.0002(2) 0.0010(2) Se2 0.0108(3) 0.0110(3) 0.0085(3) -0.0002(2) -0.0013(2) -0.0003(2) Se3 0.0112(5) 0.0112(5) 0.0284(10) 0.000 0.000 0.000 _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 U1 Se2 2.8201(7) 8 ? U1 Se2 2.8201(7) 15_665 ? U1 Se1 2.8877(6) 11 ? U1 Se1 2.8877(6) 4 ? U1 Se3 2.9040(3) . ? U1 Se1 2.9564(6) . ? U1 Se1 2.9564(6) 10 ? U1 Pt1 3.3647(5) 11 ? U1 Pt1 3.4185(5) . ? U1 Pt1 3.4464(5) 3_655 ? U1 Rb1 4.4489(17) 9 ? U1 Rb1 4.4489(17) . ? U2 Se2 2.9166(6) 6_455 ? U2 Se2 2.9166(6) 4_565 ? U2 Se2 2.9166(6) 5 ? U2 Se2 2.9166(6) 3 ? U2 Se1 2.9717(6) . ? U2 Se1 2.9717(6) 8 ? U2 Se1 2.9717(6) 2_565 ? U2 Se1 2.9717(6) 7_455 ? Pt1 Se2 2.4709(7) 5 ? Pt1 Se2 2.4709(7) 14_665 ? Pt1 Se1 2.4829(7) 10 ? Pt1 Se1 2.4829(7) . ? Pt1 U1 3.3647(5) 3 ? Pt1 U1 3.4464(5) 11_565 ? Pt1 Rb2 3.8876(4) 5 ? Pt1 Rb2 3.8876(4) 13_665 ? Rb1 Rb2 2.932(3) . ? Rb1 Se3 3.370(2) . ? Rb1 Se2 3.4185(12) . ? Rb1 Se2 3.4185(12) 3 ? Rb1 Se2 3.4185(12) 2 ? Rb1 Se2 3.4185(12) 4 ? Rb1 Se1 3.4328(12) 2 ? Rb1 Se1 3.4328(12) 3 ? Rb1 Se1 3.4328(12) . ? Rb1 Se1 3.4328(12) 4 ? Rb1 Rb2 3.731(3) 9_556 ? Rb1 U1 4.4489(17) 9 ? Rb2 Rb2 0.799(5) 9_556 ? Rb2 Se2 3.3318(12) 2 ? Rb2 Se2 3.3318(12) 4 ? Rb2 Se2 3.3318(12) . ? Rb2 Se2 3.3318(12) 3 ? Rb2 Rb1 3.731(3) 9_556 ? Rb2 Se2 3.7313(15) 10_556 ? Rb2 Se2 3.7313(15) 12_556 ? Rb2 Se2 3.7313(15) 9_556 ? Rb2 Se2 3.7313(15) 11_556 ? Rb2 Pt1 3.8876(4) 15_666 ? Se1 U1 2.8877(6) 3 ? Se2 Pt1 2.4709(7) 5_545 ? Se2 U1 2.8201(7) 15_666 ? Se2 U2 2.9166(6) 3_655 ? Se2 Rb2 3.7313(15) 9_556 ? Se3 U1 2.9040(3) 9 ? Se3 U1 2.9040(3) 11 ? Se3 U1 2.9040(3) 3 ? Se3 Rb1 3.370(2) 9 ? 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 Se2 U1 Se2 77.53(3) 8 15_665 ? Se2 U1 Se1 127.43(2) 8 11 ? Se2 U1 Se1 79.594(19) 15_665 11 ? Se2 U1 Se1 79.594(18) 8 4 ? Se2 U1 Se1 127.43(2) 15_665 4 ? Se1 U1 Se1 78.03(2) 11 4 ? Se2 U1 Se3 141.174(13) 8 . ? Se2 U1 Se3 141.174(13) 15_665 . ? Se1 U1 Se3 75.874(14) 11 . ? Se1 U1 Se3 75.874(14) 4 . ? Se2 U1 Se1 78.188(18) 8 . ? Se2 U1 Se1 124.43(2) 15_665 . ? Se1 U1 Se1 150.68(2) 11 . ? Se1 U1 Se1 95.61(2) 4 . ? Se3 U1 Se1 74.824(14) . . ? Se2 U1 Se1 124.43(2) 8 10 ? Se2 U1 Se1 78.188(18) 15_665 10 ? Se1 U1 Se1 95.61(2) 11 10 ? Se1 U1 Se1 150.68(2) 4 10 ? Se3 U1 Se1 74.824(14) . 10 ? Se1 U1 Se1 75.89(2) . 10 ? Se2 U1 Pt1 85.323(15) 8 11 ? Se2 U1 Pt1 85.323(15) 15_665 11 ? Se1 U1 Pt1 46.016(13) 11 11 ? Se1 U1 Pt1 46.016(13) 4 11 ? Se3 U1 Pt1 98.337(11) . 11 ? Se1 U1 Pt1 140.713(13) . 11 ? Se1 U1 Pt1 140.713(13) 10 11 ? Se2 U1 Pt1 82.623(15) 8 . ? Se2 U1 Pt1 82.623(15) 15_665 . ? Se1 U1 Pt1 139.664(13) 11 . ? Se1 U1 Pt1 139.664(13) 4 . ? Se3 U1 Pt1 97.144(10) . . ? Se1 U1 Pt1 45.125(13) . . ? Se1 U1 Pt1 45.125(13) 10 . ? Pt1 U1 Pt1 164.519(13) 11 . ? Se2 U1 Pt1 45.084(14) 8 3_655 ? Se2 U1 Pt1 45.084(14) 15_665 3_655 ? Se1 U1 Pt1 86.539(15) 11 3_655 ? Se1 U1 Pt1 86.539(15) 4 3_655 ? Se3 U1 Pt1 157.236(12) . 3_655 ? Se1 U1 Pt1 121.954(15) . 3_655 ? Se1 U1 Pt1 121.954(15) 10 3_655 ? Pt1 U1 Pt1 58.898(11) 11 3_655 ? Pt1 U1 Pt1 105.621(14) . 3_655 ? Se2 U1 Rb1 169.38(2) 8 9 ? Se2 U1 Rb1 91.96(2) 15_665 9 ? Se1 U1 Rb1 50.488(14) 11 9 ? Se1 U1 Rb1 108.519(19) 4 9 ? Se3 U1 Rb1 49.251(19) . 9 ? Se1 U1 Rb1 107.154(18) . 9 ? Se1 U1 Rb1 50.453(13) 10 9 ? Pt1 U1 Rb1 95.431(7) 11 9 ? Pt1 U1 Rb1 94.656(7) . 9 ? Pt1 U1 Rb1 127.006(17) 3_655 9 ? Se2 U1 Rb1 91.96(2) 8 . ? Se2 U1 Rb1 169.38(2) 15_665 . ? Se1 U1 Rb1 108.519(19) 11 . ? Se1 U1 Rb1 50.488(14) 4 . ? Se3 U1 Rb1 49.251(19) . . ? Se1 U1 Rb1 50.453(13) . . ? Se1 U1 Rb1 107.154(18) 10 . ? Pt1 U1 Rb1 95.431(7) 11 . ? Pt1 U1 Rb1 94.656(7) . . ? Pt1 U1 Rb1 127.006(17) 3_655 . ? Rb1 U1 Rb1 98.50(4) 9 . ? Se2 U2 Se2 134.64(2) 6_455 4_565 ? Se2 U2 Se2 114.15(2) 6_455 5 ? Se2 U2 Se2 83.58(2) 4_565 5 ? Se2 U2 Se2 83.58(2) 6_455 3 ? Se2 U2 Se2 114.15(2) 4_565 3 ? Se2 U2 Se2 134.64(2) 5 3 ? Se2 U2 Se1 76.700(16) 6_455 . ? Se2 U2 Se1 146.791(17) 4_565 . ? Se2 U2 Se1 70.682(16) 5 . ? Se2 U2 Se1 73.988(17) 3 . ? Se2 U2 Se1 146.791(17) 6_455 8 ? Se2 U2 Se1 76.700(16) 4_565 8 ? Se2 U2 Se1 73.988(17) 5 8 ? Se2 U2 Se1 70.682(16) 3 8 ? Se1 U2 Se1 76.26(2) . 8 ? Se2 U2 Se1 70.682(16) 6_455 2_565 ? Se2 U2 Se1 73.988(17) 4_565 2_565 ? Se2 U2 Se1 76.700(16) 5 2_565 ? Se2 U2 Se1 146.791(17) 3 2_565 ? Se1 U2 Se1 117.88(2) . 2_565 ? Se1 U2 Se1 140.34(2) 8 2_565 ? Se2 U2 Se1 73.988(17) 6_455 7_455 ? Se2 U2 Se1 70.682(16) 4_565 7_455 ? Se2 U2 Se1 146.791(17) 5 7_455 ? Se2 U2 Se1 76.700(16) 3 7_455 ? Se1 U2 Se1 140.34(2) . 7_455 ? Se1 U2 Se1 117.88(2) 8 7_455 ? Se1 U2 Se1 76.26(2) 2_565 7_455 ? Se2 Pt1 Se2 91.23(3) 5 14_665 ? Se2 Pt1 Se1 172.77(3) 5 10 ? Se2 Pt1 Se1 86.88(2) 14_665 10 ? Se2 Pt1 Se1 86.88(2) 5 . ? Se2 Pt1 Se1 172.77(3) 14_665 . ? Se1 Pt1 Se1 94.13(3) 10 . ? Se2 Pt1 U1 128.860(16) 5 3 ? Se2 Pt1 U1 128.860(16) 14_665 3 ? Se1 Pt1 U1 56.806(15) 10 3 ? Se1 Pt1 U1 56.806(15) . 3 ? Se2 Pt1 U1 117.744(17) 5 . ? Se2 Pt1 U1 117.744(17) 14_665 . ? Se1 Pt1 U1 57.543(16) 10 . ? Se1 Pt1 U1 57.543(16) . . ? U1 Pt1 U1 74.519(13) 3 . ? Se2 Pt1 U1 53.920(15) 5 11_565 ? Se2 Pt1 U1 53.920(15) 14_665 11_565 ? Se1 Pt1 U1 129.035(16) 10 11_565 ? Se1 Pt1 U1 129.035(16) . 11_565 ? U1 Pt1 U1 121.102(11) 3 11_565 ? U1 Pt1 U1 164.379(14) . 11_565 ? Se2 Pt1 Rb2 58.22(3) 5 5 ? Se2 Pt1 Rb2 67.68(3) 14_665 5 ? Se1 Pt1 Rb2 114.70(3) 10 5 ? Se1 Pt1 Rb2 105.51(3) . 5 ? U1 Pt1 Rb2 156.184(14) 3 5 ? U1 Pt1 Rb2 82.407(9) . 5 ? U1 Pt1 Rb2 82.056(9) 11_565 5 ? Se2 Pt1 Rb2 67.68(3) 5 13_665 ? Se2 Pt1 Rb2 58.22(3) 14_665 13_665 ? Se1 Pt1 Rb2 105.51(3) 10 13_665 ? Se1 Pt1 Rb2 114.70(3) . 13_665 ? U1 Pt1 Rb2 156.184(14) 3 13_665 ? U1 Pt1 Rb2 82.407(9) . 13_665 ? U1 Pt1 Rb2 82.056(9) 11_565 13_665 ? Rb2 Pt1 Rb2 11.80(7) 5 13_665 ? Rb2 Rb1 Se3 180.0 . . ? Rb2 Rb1 Se2 62.74(3) . . ? Se3 Rb1 Se2 117.26(3) . . ? Rb2 Rb1 Se2 62.74(3) . 3 ? Se3 Rb1 Se2 117.26(3) . 3 ? Se2 Rb1 Se2 77.89(3) . 3 ? Rb2 Rb1 Se2 62.74(3) . 2 ? Se3 Rb1 Se2 117.26(3) . 2 ? Se2 Rb1 Se2 125.47(7) . 2 ? Se2 Rb1 Se2 77.89(3) 3 2 ? Rb2 Rb1 Se2 62.74(3) . 4 ? Se3 Rb1 Se2 117.26(3) . 4 ? Se2 Rb1 Se2 77.89(3) . 4 ? Se2 Rb1 Se2 125.47(7) 3 4 ? Se2 Rb1 Se2 77.89(3) 2 4 ? Rb2 Rb1 Se1 116.89(3) . 2 ? Se3 Rb1 Se1 63.11(3) . 2 ? Se2 Rb1 Se1 128.868(15) . 2 ? Se2 Rb1 Se1 151.566(15) 3 2 ? Se2 Rb1 Se1 77.690(14) 2 2 ? Se2 Rb1 Se1 62.288(15) 4 2 ? Rb2 Rb1 Se1 116.89(3) . 3 ? Se3 Rb1 Se1 63.11(3) . 3 ? Se2 Rb1 Se1 151.566(14) . 3 ? Se2 Rb1 Se1 77.690(14) 3 3 ? Se2 Rb1 Se1 62.288(15) 2 3 ? Se2 Rb1 Se1 128.868(15) 4 3 ? Se1 Rb1 Se1 78.20(3) 2 3 ? Rb2 Rb1 Se1 116.89(3) . . ? Se3 Rb1 Se1 63.11(3) . . ? Se2 Rb1 Se1 77.690(14) . . ? Se2 Rb1 Se1 62.288(15) 3 . ? Se2 Rb1 Se1 128.868(15) 2 . ? Se2 Rb1 Se1 151.566(14) 4 . ? Se1 Rb1 Se1 126.22(7) 2 . ? Se1 Rb1 Se1 78.20(3) 3 . ? Rb2 Rb1 Se1 116.89(3) . 4 ? Se3 Rb1 Se1 63.11(3) . 4 ? Se2 Rb1 Se1 62.288(15) . 4 ? Se2 Rb1 Se1 128.868(15) 3 4 ? Se2 Rb1 Se1 151.566(14) 2 4 ? Se2 Rb1 Se1 77.690(14) 4 4 ? Se1 Rb1 Se1 78.20(3) 2 4 ? Se1 Rb1 Se1 126.22(7) 3 4 ? Se1 Rb1 Se1 78.20(3) . 4 ? Rb2 Rb1 Rb2 0.0 . 9_556 ? Se3 Rb1 Rb2 180.0 . 9_556 ? Se2 Rb1 Rb2 62.74(3) . 9_556 ? Se2 Rb1 Rb2 62.74(3) 3 9_556 ? Se2 Rb1 Rb2 62.74(3) 2 9_556 ? Se2 Rb1 Rb2 62.74(3) 4 9_556 ? Se1 Rb1 Rb2 116.89(3) 2 9_556 ? Se1 Rb1 Rb2 116.89(3) 3 9_556 ? Se1 Rb1 Rb2 116.89(3) . 9_556 ? Se1 Rb1 Rb2 116.89(3) 4 9_556 ? Rb2 Rb1 U1 139.251(19) . 9 ? Se3 Rb1 U1 40.749(19) . 9 ? Se2 Rb1 U1 156.13(5) . 9 ? Se2 Rb1 U1 117.92(2) 3 9 ? Se2 Rb1 U1 77.268(18) 2 9 ? Se2 Rb1 U1 103.05(2) 4 9 ? Se1 Rb1 U1 41.61(2) 2 9 ? Se1 Rb1 U1 40.46(2) 3 9 ? Se1 Rb1 U1 93.58(5) . 9 ? Se1 Rb1 U1 94.33(5) 4 9 ? Rb2 Rb1 U1 139.251(19) 9_556 9 ? Rb2 Rb2 Rb1 180.000(1) 9_556 . ? Rb2 Rb2 Se2 114.21(4) 9_556 2 ? Rb1 Rb2 Se2 65.79(4) . 2 ? Rb2 Rb2 Se2 114.21(4) 9_556 4 ? Rb1 Rb2 Se2 65.79(4) . 4 ? Se2 Rb2 Se2 80.32(3) 2 4 ? Rb2 Rb2 Se2 114.21(4) 9_556 . ? Rb1 Rb2 Se2 65.79(4) . . ? Se2 Rb2 Se2 131.58(8) 2 . ? Se2 Rb2 Se2 80.32(3) 4 . ? Rb2 Rb2 Se2 114.21(4) 9_556 3 ? Rb1 Rb2 Se2 65.79(4) . 3 ? Se2 Rb2 Se2 80.32(3) 2 3 ? Se2 Rb2 Se2 131.58(8) 4 3 ? Se2 Rb2 Se2 80.32(3) . 3 ? Rb2 Rb2 Rb1 0.000(1) 9_556 9_556 ? Rb1 Rb2 Rb1 180.0 . 9_556 ? Se2 Rb2 Rb1 114.21(4) 2 9_556 ? Se2 Rb2 Rb1 114.21(4) 4 9_556 ? Se2 Rb2 Rb1 114.21(4) . 9_556 ? Se2 Rb2 Rb1 114.21(4) 3 9_556 ? Rb2 Rb2 Se2 54.53(3) 9_556 10_556 ? Rb1 Rb2 Se2 125.47(3) . 10_556 ? Se2 Rb2 Se2 168.74(7) 2 10_556 ? Se2 Rb2 Se2 103.767(14) 4 10_556 ? Se2 Rb2 Se2 59.68(2) . 10_556 ? Se2 Rb2 Se2 103.767(14) 3 10_556 ? Rb1 Rb2 Se2 54.53(3) 9_556 10_556 ? Rb2 Rb2 Se2 54.53(3) 9_556 12_556 ? Rb1 Rb2 Se2 125.47(3) . 12_556 ? Se2 Rb2 Se2 103.767(14) 2 12_556 ? Se2 Rb2 Se2 168.74(7) 4 12_556 ? Se2 Rb2 Se2 103.767(14) . 12_556 ? Se2 Rb2 Se2 59.68(2) 3 12_556 ? Rb1 Rb2 Se2 54.53(3) 9_556 12_556 ? Se2 Rb2 Se2 70.32(3) 10_556 12_556 ? Rb2 Rb2 Se2 54.53(3) 9_556 9_556 ? Rb1 Rb2 Se2 125.47(3) . 9_556 ? Se2 Rb2 Se2 59.68(2) 2 9_556 ? Se2 Rb2 Se2 103.767(14) 4 9_556 ? Se2 Rb2 Se2 168.74(7) . 9_556 ? Se2 Rb2 Se2 103.767(14) 3 9_556 ? Rb1 Rb2 Se2 54.53(3) 9_556 9_556 ? Se2 Rb2 Se2 109.05(6) 10_556 9_556 ? Se2 Rb2 Se2 70.32(3) 12_556 9_556 ? Rb2 Rb2 Se2 54.53(3) 9_556 11_556 ? Rb1 Rb2 Se2 125.47(3) . 11_556 ? Se2 Rb2 Se2 103.767(14) 2 11_556 ? Se2 Rb2 Se2 59.68(2) 4 11_556 ? Se2 Rb2 Se2 103.767(14) . 11_556 ? Se2 Rb2 Se2 168.74(7) 3 11_556 ? Rb1 Rb2 Se2 54.53(3) 9_556 11_556 ? Se2 Rb2 Se2 70.32(3) 10_556 11_556 ? Se2 Rb2 Se2 109.05(6) 12_556 11_556 ? Se2 Rb2 Se2 70.32(3) 9_556 11_556 ? Rb2 Rb2 Pt1 84.10(3) 9_556 15_666 ? Rb1 Rb2 Pt1 95.90(3) . 15_666 ? Se2 Rb2 Pt1 115.70(2) 2 15_666 ? Se2 Rb2 Pt1 149.38(4) 4 15_666 ? Se2 Rb2 Pt1 69.550(13) . 15_666 ? Se2 Rb2 Pt1 39.083(11) 3 15_666 ? Rb1 Rb2 Pt1 84.10(3) 9_556 15_666 ? Se2 Rb2 Pt1 65.842(18) 10_556 15_666 ? Se2 Rb2 Pt1 37.778(12) 12_556 15_666 ? Se2 Rb2 Pt1 106.86(3) 9_556 15_666 ? Se2 Rb2 Pt1 132.15(6) 11_556 15_666 ? Pt1 Se1 U1 77.178(18) . 3 ? Pt1 Se1 U1 77.332(18) . . ? U1 Se1 U1 89.287(19) 3 . ? Pt1 Se1 U2 86.264(19) . . ? U1 Se1 U2 99.575(19) 3 . ? U1 Se1 U2 159.19(2) . . ? Pt1 Se1 Rb1 159.80(4) . . ? U1 Se1 Rb1 89.05(3) 3 . ? U1 Se1 Rb1 87.93(3) . . ? U2 Se1 Rb1 110.84(3) . . ? Pt1 Se2 U1 80.996(19) 5_545 15_666 ? Pt1 Se2 U2 87.70(2) 5_545 3_655 ? U1 Se2 U2 102.52(2) 15_666 3_655 ? Pt1 Se2 Rb2 82.70(3) 5_545 . ? U1 Se2 Rb2 103.02(4) 15_666 . ? U2 Se2 Rb2 150.88(3) 3_655 . ? Pt1 Se2 Rb1 119.28(3) 5_545 . ? U1 Se2 Rb1 139.17(3) 15_666 . ? U2 Se2 Rb1 112.66(3) 3_655 . ? Rb2 Se2 Rb1 51.47(5) . . ? Pt1 Se2 Rb2 74.54(3) 5_545 9_556 ? U1 Se2 Rb2 93.85(3) 15_666 9_556 ? U2 Se2 Rb2 153.69(2) 3_655 9_556 ? Rb2 Se2 Rb2 11.26(7) . 9_556 ? Rb1 Se2 Rb2 62.74(5) . 9_556 ? U1 Se3 U1 180.000(13) 9 . ? U1 Se3 U1 90.0 9 11 ? U1 Se3 U1 90.0 . 11 ? U1 Se3 U1 90.0 9 3 ? U1 Se3 U1 90.0 . 3 ? U1 Se3 U1 180.000(11) 11 3 ? U1 Se3 Rb1 90.0 9 9 ? U1 Se3 Rb1 90.0 . 9 ? U1 Se3 Rb1 90.0 11 9 ? U1 Se3 Rb1 90.0 3 9 ? U1 Se3 Rb1 90.0 9 . ? U1 Se3 Rb1 90.0 . . ? U1 Se3 Rb1 90.0 11 . ? U1 Se3 Rb1 90.0 3 . ? Rb1 Se3 Rb1 180.0 9 . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 35.87 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.352 _refine_diff_density_min -2.566 _refine_diff_density_rms 0.509 #===END data_rbupdse _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dirubidium tetrapalladium(II) hexauranium(IV) decaheptaselenide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Pd4 Rb2 Se17 U6' _chemical_formula_weight 3367.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 '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/mnc _symmetry_space_group_name_Hall '-P 4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 10.6730(2) _cell_length_b 10.6730(2) _cell_length_c 13.2822(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1513.01(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6645 _cell_measurement_theta_min 2.448 _cell_measurement_theta_max 28.244 _exptl_crystal_description 'tapered needle' _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 57.939 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0267 _exptl_absorpt_correction_T_max 0.0837 _exptl_absorpt_process_details 'face indexed, SADABS (Sheldrick, 2008b)' _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 'Bruker APEXII CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16318 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.75 _reflns_number_total 978 _reflns_number_gt 937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS (Sheldrick, 2008a)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008a)' _computing_molecular_graphics 'Crystalmaker (Palmer, 2009)' _computing_publication_material 'SHELXL (Sheldrick, 2008a)' _refine_special_details ; . ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0123P)^2^+0.0000sin\q/\l] where P = 1.00000Fo^2^ + 0.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00016(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 978 _refine_ls_number_parameters 40 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0183 _refine_ls_R_factor_gt 0.0165 _refine_ls_wR_factor_ref 0.0377 _refine_ls_wR_factor_gt 0.0375 _refine_ls_goodness_of_fit_ref 1.561 _refine_ls_restrained_S_all 1.561 _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 U1 U 0.24392(2) 0.11897(2) 0.0000 0.00582(9) Uani 1 2 d S . . U2 U 0.0000 0.5000 0.2500 0.00605(10) Uani 1 4 d S . . Pd1 Pd 0.14289(5) 0.42781(5) 0.0000 0.00673(12) Uani 1 2 d S . . Rb1 Rb 0.0000 0.0000 0.27677(8) 0.0120(2) Uani 1 4 d S . . Se1 Se 0.09102(4) 0.27614(5) 0.13523(4) 0.00653(12) Uani 1 1 d . . . Se2 Se 0.28525(5) 0.07397(4) 0.36910(4) 0.00697(12) Uani 1 1 d . . . Se3 Se 0.0000 0.0000 0.0000 0.0105(3) Uani 1 8 d S . . 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 U1 0.00526(14) 0.00527(14) 0.00694(14) 0.000 0.000 0.00032(9) U2 0.00554(12) 0.00554(12) 0.00708(18) 0.000 0.000 0.00018(13) Pd1 0.0070(3) 0.0059(3) 0.0073(3) 0.000 0.000 -0.00053(19) Rb1 0.0102(3) 0.0102(3) 0.0155(5) 0.000 0.000 0.000 Se1 0.0061(2) 0.0063(2) 0.0072(2) -0.00071(18) -0.00022(18) 0.00059(18) Se2 0.0065(2) 0.0067(2) 0.0077(2) -0.00053(18) -0.00037(18) -0.00001(18) Se3 0.0078(4) 0.0078(4) 0.0157(7) 0.000 0.000 0.000 _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 U1 Se2 2.8011(5) 8 ? U1 Se2 2.8011(5) 15_665 ? U1 Se1 2.8927(5) 11 ? U1 Se1 2.8927(5) 4 ? U1 Se3 2.8965(3) . ? U1 Se1 2.9502(5) . ? U1 Se1 2.9502(5) 10 ? U1 Pd1 3.4151(6) 11 ? U1 Pd1 3.4681(6) . ? U1 Pd1 3.5130(6) 3_655 ? U1 U1 4.0962(4) 11 ? U1 U1 4.0962(4) 3 ? U2 Se2 2.8947(5) 6_455 ? U2 Se2 2.8947(5) 4_565 ? U2 Se2 2.8947(5) 5 ? U2 Se2 2.8947(5) 3 ? U2 Se1 2.9960(5) . ? U2 Se1 2.9960(5) 8 ? U2 Se1 2.9960(5) 2_565 ? U2 Se1 2.9960(5) 7_455 ? Pd1 Se2 2.4586(6) 5 ? Pd1 Se2 2.4586(6) 14_665 ? Pd1 Se1 2.4805(6) 10 ? Pd1 Se1 2.4805(6) . ? Pd1 U1 3.4151(6) 3 ? Pd1 U1 3.5130(6) 11_565 ? Rb1 Se2 3.3758(6) . ? Rb1 Se2 3.3758(6) 3 ? Rb1 Se2 3.3758(6) 2 ? Rb1 Se2 3.3758(6) 4 ? Rb1 Se1 3.6283(7) 2 ? Rb1 Se1 3.6283(7) 3 ? Rb1 Se1 3.6283(7) . ? Rb1 Se1 3.6283(7) 4 ? Rb1 Se3 3.6762(10) . ? Rb1 U1 4.6801(8) 9 ? Rb1 U1 4.6801(8) 11 ? Rb1 U1 4.6801(8) 3 ? Se1 U1 2.8927(5) 3 ? Se2 Pd1 2.4586(6) 5_545 ? Se2 U1 2.8011(5) 15_666 ? Se2 U2 2.8947(5) 3_655 ? Se3 U1 2.8965(3) 9 ? Se3 U1 2.8965(3) 11 ? Se3 U1 2.8965(3) 3 ? Se3 Rb1 3.6762(10) 9 ? 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 Se2 U1 Se2 76.74(2) 8 15_665 ? Se2 U1 Se1 125.853(17) 8 11 ? Se2 U1 Se1 79.330(15) 15_665 11 ? Se2 U1 Se1 79.330(15) 8 4 ? Se2 U1 Se1 125.853(17) 15_665 4 ? Se1 U1 Se1 76.77(2) 11 4 ? Se2 U1 Se3 141.599(10) 8 . ? Se2 U1 Se3 141.599(10) 15_665 . ? Se1 U1 Se3 76.540(11) 11 . ? Se1 U1 Se3 76.540(11) 4 . ? Se2 U1 Se1 78.368(14) 8 . ? Se2 U1 Se1 123.656(16) 15_665 . ? Se1 U1 Se1 152.177(19) 11 . ? Se1 U1 Se1 97.370(19) 4 . ? Se3 U1 Se1 75.647(11) . . ? Se2 U1 Se1 123.656(16) 8 10 ? Se2 U1 Se1 78.368(14) 15_665 10 ? Se1 U1 Se1 97.370(19) 11 10 ? Se1 U1 Se1 152.177(19) 4 10 ? Se3 U1 Se1 75.647(11) . 10 ? Se1 U1 Se1 75.012(19) . 10 ? Se2 U1 Pd1 84.256(14) 8 11 ? Se2 U1 Pd1 84.256(14) 15_665 11 ? Se1 U1 Pd1 45.381(11) 11 11 ? Se1 U1 Pd1 45.381(11) 4 11 ? Se3 U1 Pd1 99.079(11) . 11 ? Se1 U1 Pd1 141.558(10) . 11 ? Se1 U1 Pd1 141.558(10) 10 11 ? Se2 U1 Pd1 82.464(13) 8 . ? Se2 U1 Pd1 82.464(13) 15_665 . ? Se1 U1 Pd1 140.656(10) 11 . ? Se1 U1 Pd1 140.656(10) 4 . ? Se3 U1 Pd1 97.886(11) . . ? Se1 U1 Pd1 44.567(11) . . ? Se1 U1 Pd1 44.567(11) 10 . ? Pd1 U1 Pd1 163.036(13) 11 . ? Se2 U1 Pd1 44.061(11) 8 3_655 ? Se2 U1 Pd1 44.061(11) 15_665 3_655 ? Se1 U1 Pd1 86.430(13) 11 3_655 ? Se1 U1 Pd1 86.430(13) 4 3_655 ? Se3 U1 Pd1 158.169(12) . 3_655 ? Se1 U1 Pd1 120.687(13) . 3_655 ? Se1 U1 Pd1 120.687(13) 10 3_655 ? Pd1 U1 Pd1 59.090(16) 11 3_655 ? Pd1 U1 Pd1 103.946(18) . 3_655 ? Se2 U1 U1 124.821(13) 8 11 ? Se2 U1 U1 124.821(13) 15_665 11 ? Se1 U1 U1 46.064(11) 11 11 ? Se1 U1 U1 46.064(11) 4 11 ? Se3 U1 U1 45.0 . 11 ? Se1 U1 U1 110.950(10) . 11 ? Se1 U1 U1 110.950(10) 10 11 ? Pd1 U1 U1 54.079(11) 11 11 ? Pd1 U1 U1 142.886(11) . 11 ? Pd1 U1 U1 113.169(12) 3_655 11 ? Se2 U1 U1 122.498(13) 8 3 ? Se2 U1 U1 122.498(13) 15_665 3 ? Se1 U1 U1 111.387(11) 11 3 ? Se1 U1 U1 111.387(11) 4 3 ? Se3 U1 U1 45.0 . 3 ? Se1 U1 U1 44.916(11) . 3 ? Se1 U1 U1 44.916(11) 10 3 ? Pd1 U1 U1 144.079(11) 11 3 ? Pd1 U1 U1 52.886(11) . 3 ? Pd1 U1 U1 156.831(12) 3_655 3 ? U1 U1 U1 90.0 11 3 ? Se2 U2 Se2 136.933(19) 6_455 4_565 ? Se2 U2 Se2 113.75(2) 6_455 5 ? Se2 U2 Se2 82.342(19) 4_565 5 ? Se2 U2 Se2 82.342(19) 6_455 3 ? Se2 U2 Se2 113.75(2) 4_565 3 ? Se2 U2 Se2 136.933(19) 5 3 ? Se2 U2 Se1 76.184(13) 6_455 . ? Se2 U2 Se1 145.192(13) 4_565 . ? Se2 U2 Se1 71.500(13) 5 . ? Se2 U2 Se1 74.635(14) 3 . ? Se2 U2 Se1 145.192(13) 6_455 8 ? Se2 U2 Se1 76.184(13) 4_565 8 ? Se2 U2 Se1 74.635(14) 5 8 ? Se2 U2 Se1 71.500(13) 3 8 ? Se1 U2 Se1 75.031(18) . 8 ? Se2 U2 Se1 71.500(13) 6_455 2_565 ? Se2 U2 Se1 74.635(14) 4_565 2_565 ? Se2 U2 Se1 76.184(13) 5 2_565 ? Se2 U2 Se1 145.192(13) 3 2_565 ? Se1 U2 Se1 118.832(18) . 2_565 ? Se1 U2 Se1 140.901(18) 8 2_565 ? Se2 U2 Se1 74.635(14) 6_455 7_455 ? Se2 U2 Se1 71.500(13) 4_565 7_455 ? Se2 U2 Se1 145.192(13) 5 7_455 ? Se2 U2 Se1 76.184(13) 3 7_455 ? Se1 U2 Se1 140.901(18) . 7_455 ? Se1 U2 Se1 118.832(18) 8 7_455 ? Se1 U2 Se1 75.031(18) 2_565 7_455 ? Se2 Pd1 Se2 90.01(3) 5 14_665 ? Se2 Pd1 Se1 174.72(3) 5 10 ? Se2 Pd1 Se1 88.373(16) 14_665 10 ? Se2 Pd1 Se1 88.373(16) 5 . ? Se2 Pd1 Se1 174.72(3) 14_665 . ? Se1 Pd1 Se1 92.79(3) 10 . ? Se2 Pd1 U1 128.313(17) 5 3 ? Se2 Pd1 U1 128.312(17) 14_665 3 ? Se1 Pd1 U1 56.105(15) 10 3 ? Se1 Pd1 U1 56.105(15) . 3 ? Se2 Pd1 U1 120.403(18) 5 . ? Se2 Pd1 U1 120.403(18) 14_665 . ? Se1 Pd1 U1 56.576(16) 10 . ? Se1 Pd1 U1 56.576(16) . . ? U1 Pd1 U1 73.036(13) 3 . ? Se2 Pd1 U1 52.399(15) 5 11_565 ? Se2 Pd1 U1 52.399(15) 14_665 11_565 ? Se1 Pd1 U1 129.391(16) 10 11_565 ? Se1 Pd1 U1 129.391(16) . 11_565 ? U1 Pd1 U1 120.910(16) 3 11_565 ? U1 Pd1 U1 166.054(18) . 11_565 ? Se2 Rb1 Se2 82.417(12) . 3 ? Se2 Rb1 Se2 137.40(4) . 2 ? Se2 Rb1 Se2 82.417(12) 3 2 ? Se2 Rb1 Se2 82.417(12) . 4 ? Se2 Rb1 Se2 137.40(4) 3 4 ? Se2 Rb1 Se2 82.417(12) 2 4 ? Se2 Rb1 Se1 128.292(13) . 2 ? Se2 Rb1 Se1 149.114(15) 3 2 ? Se2 Rb1 Se1 75.923(12) 2 2 ? Se2 Rb1 Se1 61.201(12) 4 2 ? Se2 Rb1 Se1 149.114(15) . 3 ? Se2 Rb1 Se1 75.923(12) 3 3 ? Se2 Rb1 Se1 61.201(12) 2 3 ? Se2 Rb1 Se1 128.292(13) 4 3 ? Se1 Rb1 Se1 74.427(14) 2 3 ? Se2 Rb1 Se1 75.923(12) . . ? Se2 Rb1 Se1 61.201(12) 3 . ? Se2 Rb1 Se1 128.292(13) 2 . ? Se2 Rb1 Se1 149.114(15) 4 . ? Se1 Rb1 Se1 117.59(3) 2 . ? Se1 Rb1 Se1 74.427(14) 3 . ? Se2 Rb1 Se1 61.201(12) . 4 ? Se2 Rb1 Se1 128.292(13) 3 4 ? Se2 Rb1 Se1 149.114(15) 2 4 ? Se2 Rb1 Se1 75.923(12) 4 4 ? Se1 Rb1 Se1 74.427(14) 2 4 ? Se1 Rb1 Se1 117.59(3) 3 4 ? Se1 Rb1 Se1 74.427(14) . 4 ? Se2 Rb1 Se3 111.301(18) . . ? Se2 Rb1 Se3 111.301(18) 3 . ? Se2 Rb1 Se3 111.301(18) 2 . ? Se2 Rb1 Se3 111.301(18) 4 . ? Se1 Rb1 Se3 58.793(16) 2 . ? Se1 Rb1 Se3 58.793(16) 3 . ? Se1 Rb1 Se3 58.793(16) . . ? Se1 Rb1 Se3 58.793(16) 4 . ? Se2 Rb1 U1 148.26(2) . 9 ? Se2 Rb1 U1 113.573(15) 3 9 ? Se2 Rb1 U1 73.754(12) 2 9 ? Se2 Rb1 U1 99.832(13) 4 9 ? Se1 Rb1 U1 39.077(11) 2 9 ? Se1 Rb1 U1 38.169(11) 3 9 ? Se1 Rb1 U1 87.84(2) . 9 ? Se1 Rb1 U1 88.41(2) 4 9 ? Se3 Rb1 U1 38.235(8) . 9 ? Se2 Rb1 U1 99.832(13) . 11 ? Se2 Rb1 U1 148.26(2) 3 11 ? Se2 Rb1 U1 113.573(15) 2 11 ? Se2 Rb1 U1 73.754(12) 4 11 ? Se1 Rb1 U1 38.169(11) 2 11 ? Se1 Rb1 U1 87.84(2) 3 11 ? Se1 Rb1 U1 88.41(2) . 11 ? Se1 Rb1 U1 39.077(11) 4 11 ? Se3 Rb1 U1 38.235(8) . 11 ? U1 Rb1 U1 51.904(10) 9 11 ? Se2 Rb1 U1 113.573(15) . 3 ? Se2 Rb1 U1 73.754(12) 3 3 ? Se2 Rb1 U1 99.832(13) 2 3 ? Se2 Rb1 U1 148.26(2) 4 3 ? Se1 Rb1 U1 88.41(2) 2 3 ? Se1 Rb1 U1 39.077(11) 3 3 ? Se1 Rb1 U1 38.169(11) . 3 ? Se1 Rb1 U1 87.84(2) 4 3 ? Se3 Rb1 U1 38.235(8) . 3 ? U1 Rb1 U1 51.904(10) 9 3 ? U1 Rb1 U1 76.470(16) 11 3 ? Pd1 Se1 U1 78.513(17) . 3 ? Pd1 Se1 U1 78.857(18) . . ? U1 Se1 U1 89.020(15) 3 . ? Pd1 Se1 U2 85.434(18) . . ? U1 Se1 U2 99.180(15) 3 . ? U1 Se1 U2 160.495(19) . . ? Pd1 Se1 Rb1 164.80(2) . . ? U1 Se1 Rb1 91.015(16) 3 . ? U1 Se1 Rb1 90.095(16) . . ? U2 Se1 Rb1 107.299(18) . . ? Pd1 Se2 U1 83.540(18) 5_545 15_666 ? Pd1 Se2 U2 88.074(18) 5_545 3_655 ? U1 Se2 U2 103.855(16) 15_666 3_655 ? Pd1 Se2 Rb1 112.94(2) 5_545 . ? U1 Se2 Rb1 135.80(2) 15_666 . ? U2 Se2 Rb1 116.86(2) 3_655 . ? U1 Se3 U1 180.000(10) 9 . ? U1 Se3 U1 90.0 9 11 ? U1 Se3 U1 90.0 . 11 ? U1 Se3 U1 90.0 9 3 ? U1 Se3 U1 90.0 . 3 ? U1 Se3 U1 180.000(9) 11 3 ? U1 Se3 Rb1 90.0 9 9 ? U1 Se3 Rb1 90.0 . 9 ? U1 Se3 Rb1 90.0 11 9 ? U1 Se3 Rb1 90.0 3 9 ? U1 Se3 Rb1 90.0 9 . ? U1 Se3 Rb1 90.0 . . ? U1 Se3 Rb1 90.0 11 . ? U1 Se3 Rb1 90.0 3 . ? Rb1 Se3 Rb1 180.0 9 . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 4.438 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.239 #===END data_rbupds _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dirubidium tetrapalladium(II) hexauranium(IV) decaheptasulfide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Pd4 Rb2 S17 U6' _chemical_formula_weight 2569.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 '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/mnc _symmetry_space_group_name_Hall '-P 4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 10.32180(10) _cell_length_b 10.32180(10) _cell_length_c 12.7302(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1356.27(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9668 _cell_measurement_theta_min 2.540 _cell_measurement_theta_max 28.710 _exptl_crystal_description 'truncated rectangular prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 43.131 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0315 _exptl_absorpt_correction_T_max 0.0542 _exptl_absorpt_process_details 'face indexed, SADABS (Sheldrick, 2008b)' _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 'Bruker APEXII CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14860 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 28.93 _reflns_number_total 914 _reflns_number_gt 906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS (Sheldrick, 2008a)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008a)' _computing_molecular_graphics 'Crystalmaker (Palmer, 2009)' _computing_publication_material 'SHELXL (Sheldrick, 2008a)' _refine_special_details ; . ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0106P)^2^+0.0000sin\q/\l] where P = 1.00000Fo^2^ + 0.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00107(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 914 _refine_ls_number_parameters 40 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 2.414 _refine_ls_restrained_S_all 2.414 _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 U1 U 0.24264(3) 0.12061(3) 0.0000 0.00453(12) Uani 1 2 d S . . U2 U 0.0000 0.5000 0.2500 0.00469(13) Uani 1 4 d S . . Pd1 Pd 0.14550(6) 0.42931(6) 0.0000 0.00529(15) Uani 1 2 d S . . Rb1 Rb 0.0000 0.0000 0.28191(9) 0.0087(2) Uani 1 4 d S . . S1 S 0.09028(13) 0.27859(13) 0.13232(11) 0.0060(3) Uani 1 1 d . . . S2 S 0.28937(13) 0.07483(13) 0.36926(11) 0.0057(3) Uani 1 1 d . . . S3 S 0.0000 0.0000 0.0000 0.0062(7) Uani 1 8 d S . . 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 U1 0.00446(16) 0.00475(17) 0.00438(17) 0.000 0.000 0.00033(10) U2 0.00512(16) 0.00512(16) 0.0038(2) 0.000 0.000 0.00004(13) Pd1 0.0060(3) 0.0055(3) 0.0044(3) 0.000 0.000 -0.0004(2) Rb1 0.0083(3) 0.0083(3) 0.0096(5) 0.000 0.000 0.000 S1 0.0064(6) 0.0060(6) 0.0057(7) -0.0001(5) -0.0001(5) 0.0005(5) S2 0.0059(6) 0.0063(6) 0.0048(7) -0.0001(5) -0.0006(5) 0.0004(5) S3 0.0049(10) 0.0049(10) 0.0089(19) 0.000 0.000 0.000 _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 U1 S2 2.6801(14) 8 ? U1 S2 2.6801(14) 15_665 ? U1 S1 2.7773(14) 11 ? U1 S1 2.7773(14) 4 ? U1 S3 2.7968(3) . ? U1 S1 2.8231(14) . ? U1 S1 2.8231(14) 10 ? U1 Pd1 3.3404(7) . ? U1 Pd1 3.3551(6) 11 ? U1 Pd1 3.3959(7) 3_655 ? U1 U1 3.9552(4) 11 ? U1 U1 3.9552(4) 3 ? U2 S2 2.7619(14) 6_455 ? U2 S2 2.7619(14) 4_565 ? U2 S2 2.7619(14) 5 ? U2 S2 2.7619(14) 3 ? U2 S1 2.8871(14) . ? U2 S1 2.8871(14) 8 ? U2 S1 2.8871(14) 2_565 ? U2 S1 2.8871(14) 7_455 ? U2 Pd1 3.5940(3) 9_565 ? U2 Pd1 3.5940(3) 7_455 ? U2 Pd1 3.5940(3) . ? U2 Pd1 3.5940(3) 15_666 ? Pd1 S2 2.3406(14) 5 ? Pd1 S2 2.3406(14) 14_665 ? Pd1 S1 2.3628(14) 10 ? Pd1 S1 2.3628(14) . ? Pd1 U1 3.3551(6) 3 ? Pd1 U1 3.3959(7) 11_565 ? Pd1 U2 3.5940(3) 9_565 ? Rb1 S2 3.2794(14) . ? Rb1 S2 3.2794(14) 3 ? Rb1 S2 3.2794(14) 2 ? Rb1 S2 3.2794(14) 4 ? Rb1 S1 3.5726(15) 2 ? Rb1 S1 3.5726(15) 3 ? Rb1 S1 3.5726(15) . ? Rb1 S1 3.5726(15) 4 ? Rb1 S3 3.5888(11) . ? Rb1 U1 4.5499(9) 9 ? Rb1 U1 4.5499(9) 11 ? Rb1 U1 4.5499(9) 3 ? S1 U1 2.7773(14) 3 ? S2 Pd1 2.3406(14) 5_545 ? S2 U1 2.6801(14) 15_666 ? S2 U2 2.7619(14) 3_655 ? S3 U1 2.7968(3) 9 ? S3 U1 2.7968(3) 11 ? S3 U1 2.7968(3) 3 ? S3 Rb1 3.5888(11) 9 ? 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 S2 U1 S2 76.78(6) 8 15_665 ? S2 U1 S1 123.67(4) 8 11 ? S2 U1 S1 78.53(4) 15_665 11 ? S2 U1 S1 78.53(4) 8 4 ? S2 U1 S1 123.67(4) 15_665 4 ? S1 U1 S1 74.68(6) 11 4 ? S2 U1 S3 141.61(3) 8 . ? S2 U1 S3 141.61(3) 15_665 . ? S1 U1 S3 76.75(3) 11 . ? S1 U1 S3 76.75(3) 4 . ? S2 U1 S1 79.68(4) 8 . ? S2 U1 S1 124.19(4) 15_665 . ? S1 U1 S1 152.76(5) 11 . ? S1 U1 S1 99.51(6) 4 . ? S3 U1 S1 76.01(3) . . ? S2 U1 S1 124.19(4) 8 10 ? S2 U1 S1 79.68(4) 15_665 10 ? S1 U1 S1 99.51(6) 11 10 ? S1 U1 S1 152.76(5) 4 10 ? S3 U1 S1 76.01(3) . 10 ? S1 U1 S1 73.27(6) . 10 ? S2 U1 Pd1 83.12(3) 8 . ? S2 U1 Pd1 83.12(3) 15_665 . ? S1 U1 Pd1 141.97(3) 11 . ? S1 U1 Pd1 141.97(3) 4 . ? S3 U1 Pd1 98.964(12) . . ? S1 U1 Pd1 44.09(3) . . ? S1 U1 Pd1 44.09(3) 10 . ? S2 U1 Pd1 83.12(3) 8 11 ? S2 U1 Pd1 83.12(3) 15_665 11 ? S1 U1 Pd1 44.08(3) 11 11 ? S1 U1 Pd1 44.08(3) 4 11 ? S3 U1 Pd1 98.619(13) . 11 ? S1 U1 Pd1 142.45(3) . 11 ? S1 U1 Pd1 142.45(3) 10 11 ? Pd1 U1 Pd1 162.417(15) . 11 ? S2 U1 Pd1 43.35(3) 8 3_655 ? S2 U1 Pd1 43.35(3) 15_665 3_655 ? S1 U1 Pd1 85.76(3) 11 3_655 ? S1 U1 Pd1 85.76(3) 4 3_655 ? S3 U1 Pd1 157.910(14) . 3_655 ? S1 U1 Pd1 120.78(3) . 3_655 ? S1 U1 Pd1 120.78(3) 10 3_655 ? Pd1 U1 Pd1 103.13(2) . 3_655 ? Pd1 U1 Pd1 59.291(18) 11 3_655 ? S2 U1 U1 123.54(3) 8 11 ? S2 U1 U1 123.54(3) 15_665 11 ? S1 U1 U1 45.54(3) 11 11 ? S1 U1 U1 45.54(3) 4 11 ? S3 U1 U1 45.0 . 11 ? S1 U1 U1 111.73(3) . 11 ? S1 U1 U1 111.73(3) 10 11 ? Pd1 U1 U1 143.964(13) . 11 ? Pd1 U1 U1 53.619(13) 11 11 ? Pd1 U1 U1 112.910(14) 3_655 11 ? S2 U1 U1 123.78(3) 8 3 ? S2 U1 U1 123.78(3) 15_665 3 ? S1 U1 U1 112.10(3) 11 3 ? S1 U1 U1 112.10(3) 4 3 ? S3 U1 U1 45.0 . 3 ? S1 U1 U1 44.60(3) . 3 ? S1 U1 U1 44.60(3) 10 3 ? Pd1 U1 U1 53.964(12) . 3 ? Pd1 U1 U1 143.619(13) 11 3 ? Pd1 U1 U1 157.090(14) 3_655 3 ? U1 U1 U1 90.0 11 3 ? S2 U2 S2 137.94(6) 6_455 4_565 ? S2 U2 S2 113.31(6) 6_455 5 ? S2 U2 S2 82.06(6) 4_565 5 ? S2 U2 S2 82.06(6) 6_455 3 ? S2 U2 S2 113.31(6) 4_565 3 ? S2 U2 S2 137.94(6) 5 3 ? S2 U2 S1 75.37(4) 6_455 . ? S2 U2 S1 144.89(4) 4_565 . ? S2 U2 S1 71.46(4) 5 . ? S2 U2 S1 75.66(4) 3 . ? S2 U2 S1 144.89(4) 6_455 8 ? S2 U2 S1 75.37(4) 4_565 8 ? S2 U2 S1 75.66(4) 5 8 ? S2 U2 S1 71.46(4) 3 8 ? S1 U2 S1 76.01(6) . 8 ? S2 U2 S1 71.46(4) 6_455 2_565 ? S2 U2 S1 75.66(4) 4_565 2_565 ? S2 U2 S1 75.37(4) 5 2_565 ? S2 U2 S1 144.89(4) 3 2_565 ? S1 U2 S1 117.49(6) . 2_565 ? S1 U2 S1 141.28(5) 8 2_565 ? S2 U2 S1 75.66(4) 6_455 7_455 ? S2 U2 S1 71.46(4) 4_565 7_455 ? S2 U2 S1 144.89(4) 5 7_455 ? S2 U2 S1 75.37(4) 3 7_455 ? S1 U2 S1 141.28(5) . 7_455 ? S1 U2 S1 117.49(6) 8 7_455 ? S1 U2 S1 76.01(6) 2_565 7_455 ? S2 U2 Pd1 40.63(3) 6_455 9_565 ? S2 U2 Pd1 116.35(3) 4_565 9_565 ? S2 U2 Pd1 77.61(3) 5 9_565 ? S2 U2 Pd1 121.99(3) 3 9_565 ? S1 U2 Pd1 80.57(3) . 9_565 ? S1 U2 Pd1 148.85(3) 8 9_565 ? S1 U2 Pd1 40.97(3) 2_565 9_565 ? S1 U2 Pd1 93.62(3) 7_455 9_565 ? S2 U2 Pd1 116.35(3) 6_455 7_455 ? S2 U2 Pd1 40.63(3) 4_565 7_455 ? S2 U2 Pd1 121.99(3) 5 7_455 ? S2 U2 Pd1 77.61(3) 3 7_455 ? S1 U2 Pd1 148.85(3) . 7_455 ? S1 U2 Pd1 80.57(3) 8 7_455 ? S1 U2 Pd1 93.62(3) 2_565 7_455 ? S1 U2 Pd1 40.97(3) 7_455 7_455 ? Pd1 U2 Pd1 127.914(17) 9_565 7_455 ? S2 U2 Pd1 77.61(3) 6_455 . ? S2 U2 Pd1 121.99(3) 4_565 . ? S2 U2 Pd1 40.63(3) 5 . ? S2 U2 Pd1 116.35(3) 3 . ? S1 U2 Pd1 40.97(3) . . ? S1 U2 Pd1 93.62(3) 8 . ? S1 U2 Pd1 80.57(3) 2_565 . ? S1 U2 Pd1 148.85(3) 7_455 . ? Pd1 U2 Pd1 55.367(16) 9_565 . ? Pd1 U2 Pd1 162.523(19) 7_455 . ? S2 U2 Pd1 121.99(3) 6_455 15_666 ? S2 U2 Pd1 77.61(3) 4_565 15_666 ? S2 U2 Pd1 116.35(3) 5 15_666 ? S2 U2 Pd1 40.63(3) 3 15_666 ? S1 U2 Pd1 93.62(3) . 15_666 ? S1 U2 Pd1 40.97(3) 8 15_666 ? S1 U2 Pd1 148.85(3) 2_565 15_666 ? S1 U2 Pd1 80.57(3) 7_455 15_666 ? Pd1 U2 Pd1 162.523(19) 9_565 15_666 ? Pd1 U2 Pd1 55.367(16) 7_455 15_666 ? Pd1 U2 Pd1 127.914(17) . 15_666 ? S2 Pd1 S2 90.65(7) 5 14_665 ? S2 Pd1 S1 177.20(6) 5 10 ? S2 Pd1 S1 89.13(5) 14_665 10 ? S2 Pd1 S1 89.13(5) 5 . ? S2 Pd1 S1 177.20(6) 14_665 . ? S1 Pd1 S1 90.95(7) 10 . ? S2 Pd1 U1 121.73(4) 5 . ? S2 Pd1 U1 121.73(4) 14_665 . ? S1 Pd1 U1 56.24(4) 10 . ? S1 Pd1 U1 56.24(4) . . ? S2 Pd1 U1 127.13(4) 5 3 ? S2 Pd1 U1 127.13(4) 14_665 3 ? S1 Pd1 U1 54.86(3) 10 3 ? S1 Pd1 U1 54.86(3) . 3 ? U1 Pd1 U1 72.417(15) . 3 ? S2 Pd1 U1 51.82(3) 5 11_565 ? S2 Pd1 U1 51.82(3) 14_665 11_565 ? S1 Pd1 U1 129.66(4) 10 11_565 ? S1 Pd1 U1 129.66(4) . 11_565 ? U1 Pd1 U1 166.87(2) . 11_565 ? U1 Pd1 U1 120.709(18) 3 11_565 ? S2 Pd1 U2 128.27(4) 5 9_565 ? S2 Pd1 U2 50.21(3) 14_665 9_565 ? S1 Pd1 U2 53.24(3) 10 9_565 ? S1 Pd1 U2 131.62(4) . 9_565 ? U1 Pd1 U2 108.608(10) . 9_565 ? U1 Pd1 U2 76.967(10) 3 9_565 ? U1 Pd1 U2 76.463(10) 11_565 9_565 ? S2 Pd1 U2 50.21(3) 5 . ? S2 Pd1 U2 128.27(4) 14_665 . ? S1 Pd1 U2 131.62(4) 10 . ? S1 Pd1 U2 53.24(3) . . ? U1 Pd1 U2 108.608(10) . . ? U1 Pd1 U2 76.967(10) 3 . ? U1 Pd1 U2 76.463(10) 11_565 . ? U2 Pd1 U2 124.633(16) 9_565 . ? S2 Rb1 S2 83.398(19) . 3 ? S2 Rb1 S2 140.36(6) . 2 ? S2 Rb1 S2 83.398(19) 3 2 ? S2 Rb1 S2 83.398(19) . 4 ? S2 Rb1 S2 140.36(6) 3 4 ? S2 Rb1 S2 83.398(19) 2 4 ? S2 Rb1 S1 127.44(3) . 2 ? S2 Rb1 S1 148.47(4) 3 2 ? S2 Rb1 S1 75.73(3) 2 2 ? S2 Rb1 S1 60.60(3) 4 2 ? S2 Rb1 S1 148.47(4) . 3 ? S2 Rb1 S1 75.73(3) 3 3 ? S2 Rb1 S1 60.60(3) 2 3 ? S2 Rb1 S1 127.44(3) 4 3 ? S1 Rb1 S1 73.49(3) 2 3 ? S2 Rb1 S1 75.73(3) . . ? S2 Rb1 S1 60.60(3) 3 . ? S2 Rb1 S1 127.44(3) 2 . ? S2 Rb1 S1 148.47(4) 4 . ? S1 Rb1 S1 115.58(5) 2 . ? S1 Rb1 S1 73.49(3) 3 . ? S2 Rb1 S1 60.60(3) . 4 ? S2 Rb1 S1 127.44(3) 3 4 ? S2 Rb1 S1 148.47(4) 2 4 ? S2 Rb1 S1 75.73(3) 4 4 ? S1 Rb1 S1 73.49(3) 2 4 ? S1 Rb1 S1 115.58(5) 3 4 ? S1 Rb1 S1 73.49(3) . 4 ? S2 Rb1 S3 109.82(3) . . ? S2 Rb1 S3 109.82(3) 3 . ? S2 Rb1 S3 109.82(3) 2 . ? S2 Rb1 S3 109.82(3) 4 . ? S1 Rb1 S3 57.79(3) 2 . ? S1 Rb1 S3 57.79(3) 3 . ? S1 Rb1 S3 57.79(3) . . ? S1 Rb1 S3 57.79(3) 4 . ? S2 Rb1 U1 146.43(4) . 9 ? S2 Rb1 U1 112.77(3) 3 9 ? S2 Rb1 U1 72.64(3) 2 9 ? S2 Rb1 U1 98.51(3) 4 9 ? S1 Rb1 U1 38.35(2) 2 9 ? S1 Rb1 U1 37.62(2) 3 9 ? S1 Rb1 U1 86.75(3) . 9 ? S1 Rb1 U1 87.21(3) 4 9 ? S3 Rb1 U1 37.930(9) . 9 ? S2 Rb1 U1 98.51(3) . 11 ? S2 Rb1 U1 146.43(4) 3 11 ? S2 Rb1 U1 112.77(3) 2 11 ? S2 Rb1 U1 72.64(3) 4 11 ? S1 Rb1 U1 37.62(2) 2 11 ? S1 Rb1 U1 86.75(3) 3 11 ? S1 Rb1 U1 87.21(3) . 11 ? S1 Rb1 U1 38.35(2) 4 11 ? S3 Rb1 U1 37.930(9) . 11 ? U1 Rb1 U1 51.527(11) 9 11 ? S2 Rb1 U1 112.77(3) . 3 ? S2 Rb1 U1 72.64(3) 3 3 ? S2 Rb1 U1 98.51(3) 2 3 ? S2 Rb1 U1 146.43(4) 4 3 ? S1 Rb1 U1 87.21(3) 2 3 ? S1 Rb1 U1 38.35(2) 3 3 ? S1 Rb1 U1 37.62(2) . 3 ? S1 Rb1 U1 86.75(3) 4 3 ? S3 Rb1 U1 37.930(9) . 3 ? U1 Rb1 U1 51.527(11) 9 3 ? U1 Rb1 U1 75.859(18) 11 3 ? Pd1 S1 U1 81.06(4) . 3 ? Pd1 S1 U1 79.66(4) . . ? U1 S1 U1 89.86(4) 3 . ? Pd1 S1 U2 85.79(4) . . ? U1 S1 U2 99.64(4) 3 . ? U1 S1 U2 161.20(5) . . ? Pd1 S1 Rb1 166.63(6) . . ? U1 S1 Rb1 90.65(4) 3 . ? U1 S1 Rb1 89.91(4) . . ? U2 S1 Rb1 106.04(4) . . ? Pd1 S2 U1 84.83(4) 5_545 15_666 ? Pd1 S2 U2 89.16(4) 5_545 3_655 ? U1 S2 U2 105.37(5) 15_666 3_655 ? Pd1 S2 Rb1 110.58(5) 5_545 . ? U1 S2 Rb1 133.78(5) 15_666 . ? U2 S2 Rb1 117.69(5) 3_655 . ? U1 S3 U1 180.000(12) 9 . ? U1 S3 U1 90.0 9 11 ? U1 S3 U1 90.0 . 11 ? U1 S3 U1 90.0 9 3 ? U1 S3 U1 90.0 . 3 ? U1 S3 U1 180.000(11) 11 3 ? U1 S3 Rb1 90.0 9 9 ? U1 S3 Rb1 90.0 . 9 ? U1 S3 Rb1 90.0 11 9 ? U1 S3 Rb1 90.0 3 9 ? U1 S3 Rb1 90.0 9 . ? U1 S3 Rb1 90.0 . . ? U1 S3 Rb1 90.0 11 . ? U1 S3 Rb1 90.0 3 . ? Rb1 S3 Rb1 180.0 9 . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.93 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 2.841 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.291