# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- Ba8Rh27Si433.cif' _publ_requested_journal 'Dalton Transactions' #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# #------------------ SUBMISSION DETAILS --------------------------------------# _journal_coden_Cambridge 222 # Name and address of author for correspondence _publ_contact_author_name 'Yuri Grin' _publ_contact_author_address ; Max-Planck-Institut f\"ur Chemische Physik fester Stoffe N\"othnitzer Str. 40 D-01187 Dresden Germany ; _publ_contact_author_email grin@cpfs.mpg.de _publ_contact_author_phone 49(351)46464249 _publ_contact_author_fax 49(351)46464000 loop_ _publ_author_name _publ_author_address 'Jung, Walter' ; Department f\"ur Chemie Universit\"at zu K\"oln Greinstr. 6 50939 K\"oln, Germany ; 'Kessens, Heike' ; Department f\"ur Chemie Universit\"at zu K\"oln Greinstr. 6 50939 K\"oln, Germany ; 'Ormeci, Alim' ; MPI-CPfS N\"othnitzer Str. 40 01187 Dresden, Germany ; 'Schnelle, Walter' ; MPI-CPfS N\"othnitzer Str. 40 01187 Dresden, Germany ; 'Burkhardt, Ulrich' ; MPI-CPfS N\"othnitzer Str. 40 01187 Dresden, Germany ; 'Borrmann, Horst' ; MPI-CPfS N\"othnitzer Str. 40 01187 Dresden, Germany ; 'Nguyen, Hong Duong' ; MPI-CPfS N\"othnitzer Str. 40 01187 Dresden, Germany ; 'Baitinger, Michael' ; MPI-CPfS N\"othnitzer Str. 40 01187 Dresden, Germany ; 'Grin, Yuri' ; MPI-CPfS N\"othnitzer Str. 40 01187 Dresden, Germany ; data_Ba8Rh3Si43 _database_code_depnum_ccdc_archive 'CCDC 890537' #TrackingRef '- Ba8Rh27Si433.cif' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_sum 'Ba8 Rh2.74 Si42.61' _chemical_formula_weight 2577.3 _chemical_compound_source 'Synthesized from the elements at 1000 C' loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ba Ba 8.00 -.646 1.510 International_Tables_Vol_IV_Table_2.3.1 Rh Rh 2.70 -2.465 .600 International_Tables_Vol_IV_Table_2.3.1 Si Si 43.30 .053 .044 International_Tables_Vol_IV_Table_2.3.1 #============================================================================= #----------------------- CRYSTAL DATA --------------------------------------# #============================================================================= _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'p m -3 n' _symmetry_int_tables_number 223 loop_ _symmetry_equiv_pos_as_xyz ' x, y, z' ' z, x, y' ' y, z, x' ' x, y, -z' ' z, x, -y' ' y, z, -x' '-x, y, z' '-z, x, y' '-y, z, x' '-x, y, -z' '-z, x, -y' '-y, z, -x' ' 1/2+y, 1/2+x, 1/2+z' ' 1/2+x, 1/2+z, 1/2+y' ' 1/2+z, 1/2+y, 1/2+x' ' 1/2+y, 1/2+x, 1/2-z' ' 1/2+x, 1/2+z, 1/2-y' ' 1/2+z, 1/2+y, 1/2-x' ' 1/2+y, 1/2-x, 1/2+z' ' 1/2+x, 1/2-z, 1/2+y' ' 1/2+z, 1/2-y, 1/2+x' ' 1/2+y, 1/2-x, 1/2-z' ' 1/2+x, 1/2-z, 1/2-y' ' 1/2+z, 1/2-y, 1/2-x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' '-x, -y, z' '-z, -x, y' '-y, -z, x' ' x, -y, -z' ' z, -x, -y' ' y, -z, -x' ' x, -y, z' ' z, -x, y' ' y, -z, x' ' 1/2-y, 1/2-x, 1/2-z' ' 1/2-x, 1/2-z, 1/2-y' ' 1/2-z, 1/2-y, 1/2-x' ' 1/2-y, 1/2-x, 1/2+z' ' 1/2-x, 1/2-z, 1/2+y' ' 1/2-z, 1/2-y, 1/2+x' ' 1/2-y, 1/2+x, 1/2-z' ' 1/2-x, 1/2+z, 1/2-y' ' 1/2-z, 1/2+y, 1/2-x' ' 1/2-y, 1/2+x, 1/2+z' ' 1/2-x, 1/2+z, 1/2+y' ' 1/2-z, 1/2+y, 1/2+x' # The lattice parameters were refined from XRPD data # by using LaB6 as an internal standard. _cell_length_a 10.347(1) _cell_length_b 10.347(1) _cell_length_c 10.347(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1107.8(3) _cell_formula_units_Z 1 _cell_measurement_wavelength 1.540598 _cell_measurement_radiation CuK\a1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 50 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_colour metallic-grey _exptl_crystal_size_max 0.063 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.057 _exptl_crystal_density_diffrn 3.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1167.8 #------------------ ABSORPTION CORRECTION -----------------------------------# _exptl_absorpt_coefficient_mu 4.78 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8309 _exptl_absorpt_correction_T_max 1.0000 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 295(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type AgK\a _diffrn_radiation_wavelength 0.560871 _diffrn_source 'micro-focus rotating anode' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'RIGAKU Spider' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 15348 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 34.4 _reflns_number_total 9991 _reflns_number_gt ? _reflns_threshold_expression 'F~o~ > 4\s(F~o~)' #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ? _computing_cell_refinement WinCSD _computing_data_reduction WinCSD _computing_structure_solution WinCSD _computing_structure_refinement WinCSD _computing_molecular_graphics ? _computing_publication_material WinCSD #L.G. Akselrud, WINCSD, version 2011 #------------------ REFINEMENT INFORMATION ----------------------------------# _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 1/[\s(F~o~)^2^+0^.^F~o~^2^)]0.8^.^F~o~)] _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 740 _refine_ls_number_parameters 20 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max ? _refine_ls_shift/esd_mean ? _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0286 _refine_ls_goodness_of_fit_ref 1.420 _refine_diff_density_max ? _refine_diff_density_min ? #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy Ba1 Ba 0 0 0 Uani 0.01031(5) 2 1.0 Ba2 Ba 0.248(2) 0.5133(5) 0 Uani 0.0191(6) 24 0.25 Si1 Si 0.25 0 0.5 Uani 0.00874(10) 6 0.434(8) Rh1 Rh 0.25 0 0.5 Uani 0.00874(10) 6 0.4567 Si2 Si 0.18461(4) 0.18461 0.18461 Uani 0.00943(7) 16 1.0 Si3 Si 0 0.31012(5) 0.12114(6) Uani 0.0110(1) 24 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ba1 0.01031(9) 0.01031(9) 0.01031(9) 0 0 0 Ba2 0.0143(6) 0.0177(7) 0.0252(14) 0.0016(9) 0 0 Si1 0.0094(2) 0.0084(1) 0.0084(1) 0 0 0 Rh1 0.0094(2) 0.0084(1) 0.0084(1) 0 0 0 Si2 0.0094(1) 0.0094(1) 0.0094(1) -0.0009(1) -0.0009(1) -0.0009(1) Si3 0.0093(2) 0.0106(2) 0.0131(2) 0 0 0.0017(2) 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 Ba1 Si2 3.3087(4) 4_555 yes Ba1 Si3 3.4450(6) 2_555 yes Ba2 Si3 3.396(15) 25_565 yes Ba2 Si3 3.444(15) 14_554 yes Ba2 Si3 3.543(15) 20_554 yes Ba2 Si3 3.553(15) 4_555 yes Ba2 Si1 3.571(15) 13_554 yes Ba2 Si1 3.652(14) 3_555 yes Ba2 Si1 3.766(14) 2_555 yes Ba2 Si2 3.722(5) 34_565 yes Ba2 Si2 3.777(4) 43_555 yes Ba2 Si2 3.914(4) 37_555 yes Ba2 Si2 3.957(5) 4_555 yes Ba2 Si3 3.835(6) 33_565 yes Ba2 Si3 3.970(3) 37_555 yes Ba2 Si3 4.108(6) 3_555 yes Si1 Si3 2.3743(6) 2_555 yes Si2 Si2 2.3434(6) 37_555 yes Si2 Si3 2.4014(5) 2_555 yes Si3 Si3 2.5070(8) 4_555 yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si3 Si1 Si3 111.67(5) 2_555 . 5_556 yes Si3 Si1 Si3 108.38(5) 2_555 . 39_555 yes Si2 Si2 Si3 107.75(5) 37_555 . . yes Si3 Si2 Si3 111.13(5) . . 2_555 yes Si1 Si3 Si2 107.09(5) 3_555 . . yes Si1 Si3 Si3 124.16(5) 3_555 . 4_555 yes Si2 Si3 Si2 105.40(5) . . 7_555 yes Si2 Si3 Si3 105.87(5) . . 4_555 yes