# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Stefanie Dehnen' _publ_contact_author_address ; University of Karlsruhe Insitute of Inorganic Chemistry Engesserstrasse 15 Karlsruhe D-76131 GERMANY ; _publ_contact_author_email DEHNEN@AOC.UKA.DE _publ_section_title ; Ternary Mn/Ge/Se Anions from Reactions of [Ba2(H2O)9][GeSe4]: Synthesis and Characterization of Compounds Containing Discrete or Polymeric [Mn6Ge4Se17]6 Units ; loop_ _publ_author_name 'Stefanie Dehnen' 'Rodolphe Clerac' 'Maike Melullis' # Attachment '3_rev.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 279906' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H38 Ba3 Ge4 Mn6 O19 Se17' _chemical_formula_weight 2716.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.184(2) _cell_length_b 15.089(3) _cell_length_c 15.868(3) _cell_angle_alpha 88.73(3) _cell_angle_beta 73.68(3) _cell_angle_gamma 71.06(3) _cell_volume 2640.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2422 _exptl_absorpt_coefficient_mu 17.580 _exptl_absorpt_correction_type semiempirical _exptl_absorpt_correction_T_min 0.32511 _exptl_absorpt_correction_T_max 0.79369 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11503 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 21.00 _reflns_number_total 5403 _reflns_number_gt 4802 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1260P)^2^+1.0635P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5403 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 0.822 _refine_ls_restrained_S_all 0.822 _refine_ls_shift/su_max 0.463 _refine_ls_shift/su_mean 0.017 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 Ba1 Ba 0.40125(6) 0.29710(4) 0.36211(5) 0.0316(10) Uani 1 1 d . . . Ba2 Ba 0.19884(6) 0.38774(5) 0.15688(5) 0.0338(10) Uani 1 1 d . . . Ba3 Ba 0.80739(6) 0.07924(5) 0.28591(5) 0.0338(10) Uani 1 1 d . . . Se1 Se 0.57888(10) 0.10623(7) 0.19680(7) 0.0290(11) Uani 1 1 d . . . Se2 Se 0.33725(11) 0.60542(7) -0.10014(7) 0.0316(11) Uani 1 1 d . . . Se3 Se 1.14574(10) 0.11920(7) 0.43609(7) 0.0298(11) Uani 1 1 d . . . Se4 Se 0.75532(10) 0.39873(7) 0.40485(7) 0.0285(11) Uani 1 1 d . . . Se5 Se 0.67847(10) -0.00744(7) 0.79928(7) 0.0252(11) Uani 1 1 d . . . Se6 Se 0.35284(10) 0.16130(7) 0.85048(7) 0.0274(11) Uani 1 1 d . . . Se7 Se 0.52857(10) 0.05613(7) 0.62157(7) 0.0266(11) Uani 1 1 d . . . Se8 Se 0.23207(10) 0.81591(7) 0.07803(7) 0.0290(11) Uani 1 1 d . . . Se9 Se 0.44815(10) 0.34147(7) -0.02956(7) 0.0261(11) Uani 1 1 d . . . Se10 Se 0.30122(10) 0.57392(7) 0.15273(7) 0.0255(11) Uani 1 1 d . . . Se11 Se 1.05385(10) -0.07977(7) 0.33103(7) 0.0249(11) Uani 1 1 d . . . Se12 Se 0.79481(10) 0.15141(7) 0.49090(7) 0.0244(11) Uani 1 1 d . . . Se13 Se 0.89346(9) 0.32068(7) 0.59589(7) 0.0249(11) Uani 1 1 d . . . Se14 Se 0.71599(10) 0.57513(7) 0.22426(7) 0.0253(11) Uani 1 1 d . . . Se15 Se 0.46335(10) 0.33130(7) 0.54680(7) 0.0244(11) Uani 1 1 d . . . Se16 Se 0.45089(9) 0.50230(7) 0.33906(7) 0.0235(11) Uani 1 1 d . . . Se17 Se 0.61641(9) 0.24593(7) 0.72746(7) 0.0228(11) Uani 1 1 d . . . Ge1 Ge 0.49059(10) 0.01989(7) 0.77116(7) 0.0242(11) Uani 1 1 d . . . Ge2 Ge 0.35645(10) 0.65836(8) 0.02997(7) 0.0258(11) Uani 1 1 d . . . Ge3 Ge 0.95665(10) 0.16207(7) 0.54011(7) 0.0237(11) Uani 1 1 d . . . Ge4 Ge 0.62314(10) 0.52735(7) 0.36151(7) 0.0231(11) Uani 1 1 d . . . Mn1 Mn 0.56858(15) 0.16928(11) 0.88312(11) 0.0286(11) Uani 1 1 d . . . Mn2 Mn 0.40683(15) 0.24663(11) 0.70010(11) 0.0278(11) Uani 1 1 d . . . Mn3 Mn 0.82296(16) 0.25340(11) 0.75734(11) 0.0303(11) Uani 1 1 d . . . Mn4 Mn 0.74404(15) 0.06552(11) 0.64130(11) 0.0283(11) Uani 1 1 d . . . Mn5 Mn 0.48868(15) 0.42457(11) 0.81844(11) 0.0298(11) Uani 1 1 d . . . Mn6 Mn 0.67789(15) 0.33056(11) 0.56724(11) 0.0287(11) Uani 1 1 d . . . O1 O 0.5120(8) 0.0958(5) 1.0073(5) 0.042(2) Uani 1 1 d . . . O2 O 0.2383(8) 0.2391(6) 0.6626(5) 0.042(2) Uani 1 1 d . . . O3 O 0.9995(8) 0.2601(6) 0.7820(6) 0.050(3) Uani 1 1 d . . . O4 O 0.1972(7) 0.4470(5) 0.3323(5) 0.039(2) Uani 1 1 d . . . O5 O 0.4271(7) 0.3294(5) 0.1885(5) 0.036(2) Uani 1 1 d . . . O6 O 0.6605(7) 0.2702(5) 0.2941(6) 0.039(2) Uani 1 1 d . . . O7 O 0.2485(8) 0.2395(5) 0.2778(6) 0.041(2) Uani 1 1 d . . . O8 O 0.7421(8) -0.0592(6) 0.3933(6) 0.047(2) Uani 1 1 d . . . O9 O 0.5410(9) 0.1358(5) 0.4189(6) 0.049(3) Uani 1 1 d . . . O10 O 0.1958(8) 0.3158(7) 0.5022(6) 0.054(3) Uani 1 1 d . . . O11 O 0.9978(10) 0.1509(7) 0.2665(7) 0.063(3) Uani 1 1 d . . . O12 O 0.2520(9) 0.2073(6) 0.0781(6) 0.058(3) Uani 1 1 d . . . O13 O -0.0020(9) 0.5458(6) 0.2292(9) 0.076(4) Uani 1 1 d . . . O14 O -0.0094(9) 0.3362(7) 0.2172(8) 0.077(4) Uani 1 1 d . . . O15 O 0.8813(12) -0.0778(8) 0.1650(8) 0.086(4) Uani 1 1 d . . . O16 O 0.8596(12) 0.1464(10) 0.1174(7) 0.091(4) Uani 1 1 d . . . O17 O 0.9524(10) 0.4964(10) 0.4264(9) 0.101(5) Uani 1 1 d . . . O18 O 1.008(3) 0.312(2) 0.966(2) 0.120(11) Uani 0.50 1 d P . . O19 O 0.1398(17) 0.4680(13) 0.0124(13) 0.053(5) Uiso 0.50 1 d P . . O20 O 0.936(3) 0.297(2) 1.080(2) 0.133(11) Uiso 0.50 1 d P . . O21 O 0.140(3) 0.0595(19) 0.0315(19) 0.101(8) Uiso 0.50 1 d P . . 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 Ba1 0.0384(11) 0.0291(11) 0.0285(11) 0.0033(3) -0.0121(4) -0.0108(5) Ba2 0.0342(11) 0.0307(11) 0.0342(11) 0.0018(3) -0.0064(4) -0.0106(5) Ba3 0.0394(11) 0.0280(11) 0.0353(11) 0.0019(3) -0.0160(5) -0.0083(5) Se1 0.0363(13) 0.0236(12) 0.0315(12) 0.0050(5) -0.0122(6) -0.0138(6) Se2 0.0420(13) 0.0281(12) 0.0239(12) -0.0029(5) -0.0107(6) -0.0092(6) Se3 0.0282(12) 0.0240(12) 0.0294(12) -0.0031(5) 0.0024(6) -0.0071(6) Se4 0.0282(12) 0.0256(12) 0.0273(12) 0.0059(5) -0.0070(6) -0.0044(6) Se5 0.0296(12) 0.0218(12) 0.0230(12) 0.0013(5) -0.0072(6) -0.0075(6) Se6 0.0298(12) 0.0232(12) 0.0241(12) -0.0006(5) -0.0024(6) -0.0067(6) Se7 0.0300(12) 0.0274(12) 0.0218(12) 0.0015(5) -0.0064(6) -0.0098(6) Se8 0.0351(12) 0.0239(12) 0.0267(12) 0.0009(5) -0.0100(6) -0.0069(6) Se9 0.0288(12) 0.0253(12) 0.0213(12) -0.0021(5) -0.0027(6) -0.0088(6) Se10 0.0303(12) 0.0226(12) 0.0229(12) -0.0002(5) -0.0047(6) -0.0101(6) Se11 0.0266(12) 0.0215(12) 0.0235(12) 0.0018(5) -0.0066(6) -0.0046(6) Se12 0.0274(12) 0.0214(12) 0.0227(12) -0.0009(5) -0.0061(6) -0.0068(6) Se13 0.0266(12) 0.0192(12) 0.0258(12) -0.0007(5) -0.0043(6) -0.0063(6) Se14 0.0266(12) 0.0243(12) 0.0223(12) 0.0002(5) -0.0044(6) -0.0070(6) Se15 0.0290(12) 0.0206(12) 0.0224(12) -0.0005(5) -0.0071(6) -0.0069(6) Se16 0.0266(12) 0.0198(12) 0.0235(12) 0.0011(5) -0.0067(6) -0.0072(6) Se17 0.0253(12) 0.0204(12) 0.0199(12) -0.0001(5) -0.0043(6) -0.0058(6) Ge1 0.0284(12) 0.0207(12) 0.0231(12) 0.0010(5) -0.0068(6) -0.0080(6) Ge2 0.0294(12) 0.0255(12) 0.0211(12) -0.0009(5) -0.0049(6) -0.0090(6) Ge3 0.0247(12) 0.0213(12) 0.0218(12) -0.0003(5) -0.0034(6) -0.0060(6) Ge4 0.0254(12) 0.0194(12) 0.0224(12) 0.0002(5) -0.0058(6) -0.0053(6) Mn1 0.0362(15) 0.0257(14) 0.0226(14) -0.0009(8) -0.0053(8) -0.0109(8) Mn2 0.0315(15) 0.0234(14) 0.0269(14) 0.0024(8) -0.0076(8) -0.0078(8) Mn3 0.0362(15) 0.0271(14) 0.0246(14) -0.0015(8) -0.0067(8) -0.0081(8) Mn4 0.0316(14) 0.0268(14) 0.0264(14) 0.0020(8) -0.0068(8) -0.0108(8) Mn5 0.0326(15) 0.0301(14) 0.0263(14) 0.0031(8) -0.0084(8) -0.0100(9) Mn6 0.0294(14) 0.0235(13) 0.0293(14) -0.0009(8) -0.0067(8) -0.0049(8) O1 0.069(6) 0.043(5) 0.025(5) 0.012(4) -0.019(4) -0.031(4) O2 0.044(5) 0.050(5) 0.035(5) 0.000(4) -0.011(4) -0.019(4) O3 0.049(6) 0.065(6) 0.043(6) 0.004(5) -0.016(4) -0.027(5) O4 0.035(5) 0.039(5) 0.039(5) -0.004(4) -0.010(4) -0.007(4) O5 0.045(5) 0.040(5) 0.026(5) 0.005(4) -0.008(4) -0.020(4) O6 0.038(5) 0.024(4) 0.050(6) 0.000(4) -0.013(4) -0.005(4) O7 0.052(6) 0.033(4) 0.042(5) 0.011(4) -0.015(4) -0.019(4) O8 0.049(6) 0.040(5) 0.063(6) 0.017(4) -0.027(5) -0.020(4) O9 0.083(7) 0.026(4) 0.043(6) 0.015(4) -0.032(5) -0.012(4) O10 0.048(6) 0.085(7) 0.042(6) 0.020(5) -0.017(4) -0.037(5) O11 0.066(7) 0.078(7) 0.063(7) 0.028(6) -0.032(5) -0.035(6) O12 0.061(7) 0.050(6) 0.055(6) -0.010(5) -0.002(5) -0.021(5) O13 0.047(6) 0.038(5) 0.129(11) -0.019(6) -0.015(6) -0.002(5) O14 0.042(6) 0.063(6) 0.102(9) -0.012(6) 0.018(6) -0.019(5) O15 0.094(9) 0.071(7) 0.078(8) -0.013(6) -0.046(7) 0.012(6) O16 0.101(10) 0.140(11) 0.046(7) 0.028(7) -0.018(6) -0.061(9) O17 0.039(6) 0.139(11) 0.111(10) -0.065(9) 0.006(6) -0.031(7) _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 Ba1 O5 2.735(8) . ? Ba1 O9 2.777(8) . ? Ba1 O10 2.780(9) . ? Ba1 O4 2.912(8) . ? Ba1 O7 2.917(8) . ? Ba1 O6 2.928(8) . ? Ba1 Se15 3.3157(14) . ? Ba1 Se16 3.3360(14) . ? Ba1 Se1 3.600(2) . ? Ba1 Ba2 4.5480(16) . ? Ba1 Ba3 4.797(2) . ? Ba2 O19 2.73(2) . ? Ba2 O13 2.784(9) . ? Ba2 O14 2.800(10) . ? Ba2 O5 2.817(8) . ? Ba2 O12 2.819(8) . ? Ba2 O4 2.936(8) . ? Ba2 O7 2.939(8) . ? Ba2 Se10 3.4167(14) . ? Ba2 Se9 3.4829(19) . ? Ba3 O11 2.803(10) . ? Ba3 O16 2.815(11) . ? Ba3 O15 2.820(11) . ? Ba3 O6 2.839(7) . ? Ba3 O8 2.840(8) . ? Ba3 O9 3.185(10) . ? Ba3 Se1 3.3716(15) . ? Ba3 Se12 3.3997(15) . ? Ba3 Se11 3.4266(18) . ? Se1 Ge1 2.3147(16) 2_656 ? Se2 Ge2 2.3283(16) . ? Se2 Mn5 2.840(2) 1_554 ? Se3 Ge3 2.3222(18) . ? Se3 Mn4 2.806(2) 2_756 ? Se4 Ge4 2.3168(18) . ? Se4 Mn6 2.781(2) . ? Se5 Ge1 2.3584(16) . ? Se5 Mn4 2.731(2) . ? Se5 Mn1 2.741(2) . ? Se6 Ge1 2.3581(18) . ? Se6 Mn2 2.705(2) . ? Se6 Mn1 2.858(2) . ? Se7 Ge1 2.3742(17) . ? Se7 Mn4 2.778(2) . ? Se7 Mn2 2.893(2) . ? Se8 Ge2 2.3710(18) . ? Se8 Mn1 2.744(2) 2_666 ? Se8 Mn3 2.778(2) 2_666 ? Se9 Ge2 2.3799(17) 2_665 ? Se9 Mn5 2.689(2) 1_554 ? Se9 Mn1 2.714(2) 1_554 ? Se10 Ge2 2.3623(17) . ? Se10 Mn5 2.731(2) 2_666 ? Se10 Mn3 2.740(2) 2_666 ? Se11 Ge3 2.3629(17) 2_756 ? Se11 Mn4 2.694(2) 2_756 ? Se11 Mn3 2.740(2) 2_756 ? Se12 Ge3 2.3666(16) . ? Se12 Mn4 2.704(2) . ? Se12 Mn6 2.735(2) . ? Se13 Ge3 2.3705(16) . ? Se13 Mn6 2.746(2) . ? Se13 Mn3 2.747(2) . ? Se14 Ge4 2.3702(17) . ? Se14 Mn2 2.726(2) 2_666 ? Se14 Mn5 2.760(2) 2_666 ? Se15 Ge4 2.3650(17) 2_666 ? Se15 Mn6 2.720(2) . ? Se15 Mn2 2.741(2) . ? Se16 Ge4 2.3697(15) . ? Se16 Mn6 2.705(2) 2_666 ? Se16 Mn5 2.716(2) 2_666 ? Se17 Mn1 2.698(2) . ? Se17 Mn2 2.705(2) . ? Se17 Mn3 2.725(2) . ? Se17 Mn4 2.814(2) . ? Se17 Mn5 2.821(2) . ? Se17 Mn6 2.839(2) . ? Ge1 Se1 2.3147(16) 2_656 ? Ge2 Se9 2.3799(16) 2_665 ? Ge3 Se11 2.3629(17) 2_756 ? Ge4 Se15 2.3650(17) 2_666 ? Mn1 O1 2.286(8) . ? Mn1 Se9 2.714(2) 1_556 ? Mn1 Se8 2.744(2) 2_666 ? Mn2 O2 2.328(8) . ? Mn2 Se14 2.726(2) 2_666 ? Mn3 O3 2.324(8) . ? Mn3 Se11 2.740(2) 2_756 ? Mn3 Se10 2.740(2) 2_666 ? Mn3 Se8 2.778(2) 2_666 ? Mn4 Se11 2.694(2) 2_756 ? Mn4 Se3 2.806(2) 2_756 ? Mn5 Se9 2.689(2) 1_556 ? Mn5 Se16 2.716(2) 2_666 ? Mn5 Se10 2.731(2) 2_666 ? Mn5 Se14 2.760(2) 2_666 ? Mn5 Se2 2.840(2) 1_556 ? Mn6 Se16 2.705(2) 2_666 ? O18 O20 1.83(5) . ? 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 O5 Ba1 O9 123.5(3) . . ? O5 Ba1 O10 131.1(3) . . ? O9 Ba1 O10 93.7(3) . . ? O5 Ba1 O4 66.3(2) . . ? O9 Ba1 O4 163.0(3) . . ? O10 Ba1 O4 71.0(3) . . ? O5 Ba1 O7 62.7(2) . . ? O9 Ba1 O7 106.7(2) . . ? O10 Ba1 O7 77.9(2) . . ? O4 Ba1 O7 63.8(2) . . ? O5 Ba1 O6 77.7(2) . . ? O9 Ba1 O6 68.3(3) . . ? O10 Ba1 O6 150.6(3) . . ? O4 Ba1 O6 128.7(2) . . ? O7 Ba1 O6 128.5(2) . . ? O5 Ba1 Se15 148.58(15) . . ? O9 Ba1 Se15 65.58(17) . . ? O10 Ba1 Se15 71.86(18) . . ? O4 Ba1 Se15 114.25(15) . . ? O7 Ba1 Se15 147.88(17) . . ? O6 Ba1 Se15 79.44(16) . . ? O5 Ba1 Se16 74.58(15) . . ? O9 Ba1 Se16 126.76(19) . . ? O10 Ba1 Se16 109.7(2) . . ? O4 Ba1 Se16 67.34(15) . . ? O7 Ba1 Se16 124.34(16) . . ? O6 Ba1 Se16 68.60(14) . . ? Se15 Ba1 Se16 77.14(4) . . ? O5 Ba1 Se1 60.88(16) . . ? O9 Ba1 Se1 63.83(18) . . ? O10 Ba1 Se1 130.4(2) . . ? O4 Ba1 Se1 120.36(15) . . ? O7 Ba1 Se1 68.73(17) . . ? O6 Ba1 Se1 63.49(14) . . ? Se15 Ba1 Se1 125.16(4) . . ? Se16 Ba1 Se1 119.24(4) . . ? O5 Ba1 Ba2 35.59(17) . . ? O9 Ba1 Ba2 140.45(17) . . ? O10 Ba1 Ba2 95.54(19) . . ? O4 Ba1 Ba2 39.14(15) . . ? O7 Ba1 Ba2 39.21(15) . . ? O6 Ba1 Ba2 113.20(17) . . ? Se15 Ba1 Ba2 153.14(3) . . ? Se16 Ba1 Ba2 85.50(3) . . ? Se1 Ba1 Ba2 81.23(3) . . ? O5 Ba1 Ba3 90.08(17) . . ? O9 Ba1 Ba3 39.4(2) . . ? O10 Ba1 Ba3 133.1(2) . . ? O4 Ba1 Ba3 155.57(16) . . ? O7 Ba1 Ba3 112.04(16) . . ? O6 Ba1 Ba3 33.15(14) . . ? Se15 Ba1 Ba3 82.35(4) . . ? Se16 Ba1 Ba3 101.48(4) . . ? Se1 Ba1 Ba3 44.58(3) . . ? Ba2 Ba1 Ba3 121.58(3) . . ? O19 Ba2 O13 76.7(5) . . ? O19 Ba2 O14 94.7(5) . . ? O13 Ba2 O14 70.0(3) . . ? O19 Ba2 O5 128.1(4) . . ? O13 Ba2 O5 128.9(3) . . ? O14 Ba2 O5 134.3(3) . . ? O19 Ba2 O12 90.5(4) . . ? O13 Ba2 O12 138.9(3) . . ? O14 Ba2 O12 72.4(3) . . ? O5 Ba2 O12 89.7(3) . . ? O19 Ba2 O4 138.6(4) . . ? O13 Ba2 O4 69.2(3) . . ? O14 Ba2 O4 95.1(3) . . ? O5 Ba2 O4 65.0(2) . . ? O12 Ba2 O4 130.7(3) . . ? O19 Ba2 O7 157.0(4) . . ? O13 Ba2 O7 115.0(3) . . ? O14 Ba2 O7 72.7(3) . . ? O5 Ba2 O7 61.5(2) . . ? O12 Ba2 O7 67.6(3) . . ? O4 Ba2 O7 63.3(2) . . ? O19 Ba2 Se10 80.4(4) . . ? O13 Ba2 Se10 72.7(2) . . ? O14 Ba2 Se10 142.6(2) . . ? O5 Ba2 Se10 69.95(15) . . ? O12 Ba2 Se10 144.03(19) . . ? O4 Ba2 Se10 67.76(16) . . ? O7 Ba2 Se10 121.37(15) . . ? O19 Ba2 Se9 67.1(4) . . ? O13 Ba2 Se9 134.1(3) . . ? O14 Ba2 Se9 137.8(2) . . ? O5 Ba2 Se9 64.35(16) . . ? O12 Ba2 Se9 70.20(19) . . ? O4 Ba2 Se9 124.17(16) . . ? O7 Ba2 Se9 109.21(17) . . ? Se10 Ba2 Se9 74.23(4) . . ? O19 Ba2 Ba1 160.1(4) . . ? O13 Ba2 Ba1 107.8(3) . . ? O14 Ba2 Ba1 105.1(3) . . ? O5 Ba2 Ba1 34.41(16) . . ? O12 Ba2 Ba1 97.4(2) . . ? O4 Ba2 Ba1 38.76(15) . . ? O7 Ba2 Ba1 38.88(15) . . ? Se10 Ba2 Ba1 82.55(3) . . ? Se9 Ba2 Ba1 98.45(3) . . ? O11 Ba3 O16 71.4(3) . . ? O11 Ba3 O15 110.0(4) . . ? O16 Ba3 O15 74.0(4) . . ? O11 Ba3 O6 85.0(3) . . ? O16 Ba3 O6 70.7(3) . . ? O15 Ba3 O6 134.4(3) . . ? O11 Ba3 O8 131.2(3) . . ? O16 Ba3 O8 148.4(3) . . ? O15 Ba3 O8 76.8(3) . . ? O6 Ba3 O8 125.6(3) . . ? O11 Ba3 O9 132.7(3) . . ? O16 Ba3 O9 123.3(3) . . ? O15 Ba3 O9 117.2(3) . . ? O6 Ba3 O9 64.0(2) . . ? O8 Ba3 O9 61.7(2) . . ? O11 Ba3 Se1 137.5(2) . . ? O16 Ba3 Se1 69.2(3) . . ? O15 Ba3 Se1 73.5(2) . . ? O6 Ba3 Se1 67.56(16) . . ? O8 Ba3 Se1 91.19(17) . . ? O9 Ba3 Se1 63.27(15) . . ? O11 Ba3 Se12 73.0(2) . . ? O16 Ba3 Se12 135.4(3) . . ? O15 Ba3 Se12 144.8(2) . . ? O6 Ba3 Se12 80.30(17) . . ? O8 Ba3 Se12 76.20(18) . . ? O9 Ba3 Se12 67.44(16) . . ? Se1 Ba3 Se12 129.06(4) . . ? O11 Ba3 Se11 67.7(2) . . ? O16 Ba3 Se11 113.9(3) . . ? O15 Ba3 Se11 74.2(2) . . ? O6 Ba3 Se11 147.50(16) . . ? O8 Ba3 Se11 68.40(18) . . ? O9 Ba3 Se11 122.68(15) . . ? Se1 Ba3 Se11 144.93(3) . . ? Se12 Ba3 Se11 75.10(4) . . ? O11 Ba3 Ba1 118.1(2) . . ? O16 Ba3 Ba1 91.0(3) . . ? O15 Ba3 Ba1 121.3(2) . . ? O6 Ba3 Ba1 34.33(16) . . ? O8 Ba3 Ba1 93.94(18) . . ? O9 Ba3 Ba1 33.63(14) . . ? Se1 Ba3 Ba1 48.53(3) . . ? Se12 Ba3 Ba1 82.78(4) . . ? Se11 Ba3 Ba1 154.30(3) . . ? Ge1 Se1 Ba3 108.48(5) 2_656 . ? Ge1 Se1 Ba1 109.50(5) 2_656 . ? Ba3 Se1 Ba1 86.89(4) . . ? Ge2 Se2 Mn5 120.00(7) . 1_554 ? Ge3 Se3 Mn4 120.00(7) . 2_756 ? Ge4 Se4 Mn6 119.40(7) . . ? Ge1 Se5 Mn4 85.45(6) . . ? Ge1 Se5 Mn1 83.71(6) . . ? Mn4 Se5 Mn1 90.99(6) . . ? Ge1 Se6 Mn2 87.09(6) . . ? Ge1 Se6 Mn1 81.17(6) . . ? Mn2 Se6 Mn1 89.16(6) . . ? Ge1 Se7 Mn4 84.10(6) . . ? Ge1 Se7 Mn2 82.57(6) . . ? Mn4 Se7 Mn2 89.31(6) . . ? Ge2 Se8 Mn1 84.52(6) . 2_666 ? Ge2 Se8 Mn3 84.62(6) . 2_666 ? Mn1 Se8 Mn3 85.93(6) 2_666 2_666 ? Ge2 Se9 Mn5 85.08(6) 2_665 1_554 ? Ge2 Se9 Mn1 85.03(6) 2_665 1_554 ? Mn5 Se9 Mn1 90.77(6) 1_554 1_554 ? Ge2 Se9 Ba2 124.77(5) 2_665 . ? Mn5 Se9 Ba2 132.85(6) 1_554 . ? Mn1 Se9 Ba2 123.85(6) 1_554 . ? Ge2 Se10 Mn5 84.47(6) . 2_666 ? Ge2 Se10 Mn3 85.64(6) . 2_666 ? Mn5 Se10 Mn3 91.13(6) 2_666 2_666 ? Ge2 Se10 Ba2 127.01(5) . . ? Mn5 Se10 Ba2 127.75(6) 2_666 . ? Mn3 Se10 Ba2 126.95(5) 2_666 . ? Ge3 Se11 Mn4 83.59(6) 2_756 2_756 ? Ge3 Se11 Mn3 85.30(6) 2_756 2_756 ? Mn4 Se11 Mn3 92.25(6) 2_756 2_756 ? Ge3 Se11 Ba3 123.94(6) 2_756 . ? Mn4 Se11 Ba3 133.29(5) 2_756 . ? Mn3 Se11 Ba3 123.76(6) 2_756 . ? Ge3 Se12 Mn4 83.30(6) . . ? Ge3 Se12 Mn6 84.35(6) . . ? Mn4 Se12 Mn6 95.69(6) . . ? Ge3 Se12 Ba3 127.53(5) . . ? Mn4 Se12 Ba3 127.44(5) . . ? Mn6 Se12 Ba3 125.01(6) . . ? Ge3 Se13 Mn6 84.02(6) . . ? Ge3 Se13 Mn3 85.01(6) . . ? Mn6 Se13 Mn3 89.99(6) . . ? Ge4 Se14 Mn2 85.18(6) . 2_666 ? Ge4 Se14 Mn5 84.53(6) . 2_666 ? Mn2 Se14 Mn5 88.82(6) 2_666 2_666 ? Ge4 Se15 Mn6 85.59(6) 2_666 . ? Ge4 Se15 Mn2 84.94(6) 2_666 . ? Mn6 Se15 Mn2 92.80(7) . . ? Ge4 Se15 Ba1 125.12(6) 2_666 . ? Mn6 Se15 Ba1 128.25(6) . . ? Mn2 Se15 Ba1 126.56(5) . . ? Ge4 Se16 Mn6 85.82(6) . 2_666 ? Ge4 Se16 Mn5 85.53(6) . 2_666 ? Mn6 Se16 Mn5 95.79(6) 2_666 2_666 ? Ge4 Se16 Ba1 123.47(5) . . ? Mn6 Se16 Ba1 129.41(6) 2_666 . ? Mn5 Se16 Ba1 123.89(5) 2_666 . ? Mn1 Se17 Mn2 92.59(6) . . ? Mn1 Se17 Mn3 87.88(6) . . ? Mn2 Se17 Mn3 177.49(6) . . ? Mn1 Se17 Mn4 90.10(6) . . ? Mn2 Se17 Mn4 92.46(6) . . ? Mn3 Se17 Mn4 90.00(6) . . ? Mn1 Se17 Mn5 88.32(6) . . ? Mn2 Se17 Mn5 88.02(6) . . ? Mn3 Se17 Mn5 89.54(6) . . ? Mn4 Se17 Mn5 178.37(6) . . ? Mn1 Se17 Mn6 176.22(6) . . ? Mn2 Se17 Mn6 90.98(6) . . ? Mn3 Se17 Mn6 88.50(6) . . ? Mn4 Se17 Mn6 90.99(6) . . ? Mn5 Se17 Mn6 90.56(6) . . ? Se1 Ge1 Se6 112.83(6) 2_656 . ? Se1 Ge1 Se5 111.82(6) 2_656 . ? Se6 Ge1 Se5 108.25(6) . . ? Se1 Ge1 Se7 115.18(6) 2_656 . ? Se6 Ge1 Se7 104.36(6) . . ? Se5 Ge1 Se7 103.66(6) . . ? Se2 Ge2 Se10 114.59(6) . . ? Se2 Ge2 Se8 113.48(7) . . ? Se10 Ge2 Se8 103.52(6) . . ? Se2 Ge2 Se9 117.33(7) . 2_665 ? Se10 Ge2 Se9 103.35(6) . 2_665 ? Se8 Ge2 Se9 102.88(6) . 2_665 ? Se3 Ge3 Se11 115.57(7) . 2_756 ? Se3 Ge3 Se12 116.25(6) . . ? Se11 Ge3 Se12 104.86(6) 2_756 . ? Se3 Ge3 Se13 111.32(6) . . ? Se11 Ge3 Se13 102.82(6) 2_756 . ? Se12 Ge3 Se13 104.62(6) . . ? Se4 Ge4 Se15 118.72(6) . 2_666 ? Se4 Ge4 Se16 115.04(6) . . ? Se15 Ge4 Se16 102.56(6) 2_666 . ? Se4 Ge4 Se14 112.18(7) . . ? Se15 Ge4 Se14 102.97(6) 2_666 . ? Se16 Ge4 Se14 103.56(6) . . ? O1 Mn1 Se17 172.1(2) . . ? O1 Mn1 Se9 91.8(2) . 1_556 ? Se17 Mn1 Se9 91.51(6) . 1_556 ? O1 Mn1 Se5 86.0(2) . . ? Se17 Mn1 Se5 90.43(6) . . ? Se9 Mn1 Se5 176.67(8) 1_556 . ? O1 Mn1 Se8 93.7(2) . 2_666 ? Se17 Mn1 Se8 93.69(6) . 2_666 ? Se9 Mn1 Se8 85.79(6) 1_556 2_666 ? Se5 Mn1 Se8 96.79(7) . 2_666 ? O1 Mn1 Se6 85.2(2) . . ? Se17 Mn1 Se6 87.53(6) . . ? Se9 Mn1 Se6 91.30(6) 1_556 . ? Se5 Mn1 Se6 86.08(6) . . ? Se8 Mn1 Se6 176.87(7) 2_666 . ? O2 Mn2 Se17 174.1(2) . . ? O2 Mn2 Se6 92.7(2) . . ? Se17 Mn2 Se6 90.60(7) . . ? O2 Mn2 Se14 91.5(2) . 2_666 ? Se17 Mn2 Se14 93.03(6) . 2_666 ? Se6 Mn2 Se14 95.30(7) . 2_666 ? O2 Mn2 Se15 87.4(2) . . ? Se17 Mn2 Se15 89.25(6) . . ? Se6 Mn2 Se15 179.38(8) . . ? Se14 Mn2 Se15 85.31(6) 2_666 . ? O2 Mn2 Se7 86.7(2) . . ? Se17 Mn2 Se7 88.91(6) . . ? Se6 Mn2 Se7 83.73(6) . . ? Se14 Mn2 Se7 177.84(7) 2_666 . ? Se15 Mn2 Se7 95.67(6) . . ? O3 Mn3 Se17 179.6(2) . . ? O3 Mn3 Se11 90.7(2) . 2_756 ? Se17 Mn3 Se11 89.30(6) . 2_756 ? O3 Mn3 Se10 89.5(2) . 2_666 ? Se17 Mn3 Se10 90.57(7) . 2_666 ? Se11 Mn3 Se10 179.38(8) 2_756 2_666 ? O3 Mn3 Se13 87.9(2) . . ? Se17 Mn3 Se13 91.75(7) . . ? Se11 Mn3 Se13 84.79(6) 2_756 . ? Se10 Mn3 Se13 95.82(7) 2_666 . ? O3 Mn3 Se8 88.0(2) . 2_666 ? Se17 Mn3 Se8 92.33(7) . 2_666 ? Se11 Mn3 Se8 94.68(7) 2_756 2_666 ? Se10 Mn3 Se8 84.71(6) 2_666 2_666 ? Se13 Mn3 Se8 175.87(8) . 2_666 ? Se11 Mn4 Se12 87.96(6) 2_756 . ? Se11 Mn4 Se5 93.13(7) 2_756 . ? Se12 Mn4 Se5 175.27(7) . . ? Se11 Mn4 Se7 176.90(7) 2_756 . ? Se12 Mn4 Se7 93.73(7) . . ? Se5 Mn4 Se7 84.98(6) . . ? Se11 Mn4 Se3 95.18(7) 2_756 2_756 ? Se12 Mn4 Se3 96.42(7) . 2_756 ? Se5 Mn4 Se3 88.07(6) . 2_756 ? Se7 Mn4 Se3 87.22(6) . 2_756 ? Se11 Mn4 Se17 88.40(6) 2_756 . ? Se12 Mn4 Se17 87.19(6) . . ? Se5 Mn4 Se17 88.23(6) . . ? Se7 Mn4 Se17 89.08(6) . . ? Se3 Mn4 Se17 174.99(7) 2_756 . ? Se9 Mn5 Se16 175.10(8) 1_556 2_666 ? Se9 Mn5 Se10 86.68(6) 1_556 2_666 ? Se16 Mn5 Se10 90.03(6) 2_666 2_666 ? Se9 Mn5 Se14 97.52(7) 1_556 2_666 ? Se16 Mn5 Se14 85.68(6) 2_666 2_666 ? Se10 Mn5 Se14 175.55(8) 2_666 2_666 ? Se9 Mn5 Se17 89.40(6) 1_556 . ? Se16 Mn5 Se17 86.90(6) 2_666 . ? Se10 Mn5 Se17 88.76(6) 2_666 . ? Se14 Mn5 Se17 89.81(6) 2_666 . ? Se9 Mn5 Se2 93.01(7) 1_556 1_556 ? Se16 Mn5 Se2 91.05(6) 2_666 1_556 ? Se10 Mn5 Se2 98.12(6) 2_666 1_556 ? Se14 Mn5 Se2 83.18(6) 2_666 1_556 ? Se17 Mn5 Se2 172.83(7) . 1_556 ? Se16 Mn6 Se15 85.83(6) 2_666 . ? Se16 Mn6 Se12 172.66(8) 2_666 . ? Se15 Mn6 Se12 92.18(6) . . ? Se16 Mn6 Se13 95.23(6) 2_666 . ? Se15 Mn6 Se13 176.11(8) . . ? Se12 Mn6 Se13 86.30(6) . . ? Se16 Mn6 Se4 98.01(7) 2_666 . ? Se15 Mn6 Se4 95.23(7) . . ? Se12 Mn6 Se4 89.20(6) . . ? Se13 Mn6 Se4 88.34(6) . . ? Se16 Mn6 Se17 86.73(6) 2_666 . ? Se15 Mn6 Se17 86.95(6) . . ? Se12 Mn6 Se17 86.11(6) . . ? Se13 Mn6 Se17 89.37(6) . . ? Se4 Mn6 Se17 174.90(7) . . ? Ba1 O4 Ba2 102.1(2) . . ? Ba1 O5 Ba2 110.0(3) . . ? Ba3 O6 Ba1 112.5(3) . . ? Ba1 O7 Ba2 101.9(2) . . ? Ba1 O9 Ba3 106.9(3) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.321 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.126 # Attachment '1_rev.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 284719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H18 Ba2 Ge O9 Se4' _chemical_formula_weight 825.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.3016 1.1903 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se 0.2367 1.4831 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.6940 1.5004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.916(3) _cell_length_b 15.097(3) _cell_length_c 16.116(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3385.9(12) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour light_yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 7.926 _exptl_absorpt_correction_type semiempirical _exptl_absorpt_correction_T_min 0.24665 _exptl_absorpt_correction_T_max 0.27764 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.56086 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11556 _diffrn_reflns_av_R_equivalents 0.1392 _diffrn_reflns_av_sigmaI/netI 0.1452 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 23.00 _reflns_number_total 4530 _reflns_number_gt 2380 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4530 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1562 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.002 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 Ba1 Ba 0.11777(6) 0.02506(7) 0.61011(5) 0.0394(5) Uani 1 1 d . . . Ba2 Ba -0.02342(5) 0.00684(6) 0.85755(4) 0.0356(5) Uani 1 1 d . . . Ge1 Ge 0.20176(10) 0.22933(11) 0.40088(8) 0.0345(6) Uani 1 1 d . . . Se1 Se 0.19999(10) 0.07391(10) 0.41683(7) 0.0361(6) Uani 1 1 d . . . Se2 Se 0.04166(10) 0.22554(11) 0.87656(8) 0.0404(6) Uani 1 1 d . . . Se3 Se 0.30550(12) 0.25994(12) 0.29011(9) 0.0461(6) Uani 1 1 d . . . Se4 Se 0.26465(11) 0.29704(12) 0.51893(9) 0.0450(6) Uani 1 1 d . . . O1 O -0.1132(7) -0.0274(8) 1.0109(5) 0.039(2) Uani 1 1 d . . . O2 O -0.1958(7) 0.1124(7) 0.8755(6) 0.040(2) Uani 1 1 d . . . O3 O 0.0265(8) -0.1574(8) 0.9241(6) 0.049(3) Uani 1 1 d . . . O4 O -0.0635(7) 0.0564(8) 0.6935(5) 0.040(2) Uani 1 1 d . . . O5 O 0.0276(8) -0.1020(8) 0.5002(6) 0.044(2) Uani 1 1 d . . . O6 O 0.1658(7) 0.0447(8) 0.7835(5) 0.041(3) Uani 1 1 d . . . O7 O -0.1989(9) -0.0878(9) 0.8225(7) 0.055(3) Uani 1 1 d . . . O8 O 0.0481(8) -0.1052(8) 0.7239(5) 0.042(2) Uani 1 1 d . . . O9 O 0.0915(8) 0.1962(9) 0.6619(7) 0.055(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0404(6) 0.0440(7) 0.0337(6) 0.0018(3) 0.0011(3) -0.0020(4) Ba2 0.0374(6) 0.0372(7) 0.0321(6) 0.0011(3) 0.0004(3) 0.0001(3) Ge1 0.0341(8) 0.0320(10) 0.0373(8) 0.0012(6) -0.0007(5) 0.0007(5) Se1 0.0403(8) 0.0312(9) 0.0367(8) 0.0012(5) -0.0004(5) 0.0021(6) Se2 0.0383(8) 0.0331(10) 0.0499(9) 0.0002(6) -0.0041(5) -0.0024(5) Se3 0.0514(10) 0.0408(11) 0.0460(9) 0.0082(6) 0.0099(6) 0.0014(7) Se4 0.0483(9) 0.0411(11) 0.0455(8) -0.0026(6) -0.0071(6) -0.0023(7) O1 0.031(4) 0.051(7) 0.035(4) -0.004(4) -0.005(3) -0.001(4) O2 0.041(5) 0.035(6) 0.043(5) 0.003(4) -0.001(4) -0.001(4) O3 0.052(6) 0.043(7) 0.051(5) 0.005(5) 0.004(4) 0.009(5) O4 0.043(5) 0.041(7) 0.037(4) 0.000(4) -0.006(4) 0.002(4) O5 0.055(6) 0.035(6) 0.042(4) 0.006(4) 0.001(4) -0.001(5) O6 0.035(5) 0.051(8) 0.037(4) 0.000(4) -0.001(3) -0.002(4) O7 0.057(7) 0.057(9) 0.052(5) 0.007(6) -0.014(5) -0.009(6) O8 0.050(6) 0.035(7) 0.042(4) 0.004(4) 0.006(4) 0.003(4) O9 0.056(7) 0.037(8) 0.071(7) 0.009(6) -0.011(5) -0.002(5) _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 Ba1 O9 2.740(14) . ? Ba1 O8 2.858(10) . ? Ba1 O6 2.888(9) . ? Ba1 O4 2.897(10) . ? Ba1 O5 2.897(11) . ? Ba1 O2 2.920(10) 6_657 ? Ba1 O5 2.933(10) 5_556 ? Ba1 O7 3.255(14) 6_657 ? Ba1 Se1 3.3993(16) . ? Ba1 Ba2 4.4540(12) . ? Ba2 O3 2.790(12) . ? Ba2 O4 2.803(9) . ? Ba2 O1 2.817(8) . ? Ba2 O1 2.864(8) 5_557 ? Ba2 O7 2.885(12) . ? Ba2 O2 2.894(10) . ? Ba2 O8 2.915(10) . ? Ba2 O6 2.947(9) . ? Ba2 Se2 3.4374(19) . ? Ba2 Ba2 4.6420(16) 5_557 ? Ge1 Se4 2.330(2) . ? Ge1 Se3 2.342(2) . ? Ge1 Se1 2.361(2) . ? Ge1 Se2 2.363(2) 7_565 ? Se2 Ge1 2.363(2) 7_566 ? O1 Ba2 2.864(8) 5_557 ? O2 Ba1 2.920(10) 6_557 ? O5 Ba1 2.933(10) 5_556 ? O7 Ba1 3.255(14) 6_557 ? 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 O9 Ba1 O8 114.1(3) . . ? O9 Ba1 O6 68.8(3) . . ? O8 Ba1 O6 61.9(3) . . ? O9 Ba1 O4 65.7(3) . . ? O8 Ba1 O4 61.3(3) . . ? O6 Ba1 O4 74.7(3) . . ? O9 Ba1 O5 138.9(3) . . ? O8 Ba1 O5 77.9(3) . . ? O6 Ba1 O5 139.5(3) . . ? O4 Ba1 O5 90.9(3) . . ? O9 Ba1 O2 70.6(3) . 6_657 ? O8 Ba1 O2 124.1(3) . 6_657 ? O6 Ba1 O2 70.8(3) . 6_657 ? O4 Ba1 O2 131.5(3) . 6_657 ? O5 Ba1 O2 137.1(3) . 6_657 ? O9 Ba1 O5 73.7(3) . 5_556 ? O8 Ba1 O5 115.3(3) . 5_556 ? O6 Ba1 O5 134.8(3) . 5_556 ? O4 Ba1 O5 67.4(3) . 5_556 ? O5 Ba1 O5 66.0(4) . 5_556 ? O2 Ba1 O5 118.8(3) 6_657 5_556 ? O9 Ba1 O7 119.8(3) . 6_657 ? O8 Ba1 O7 72.0(3) . 6_657 ? O6 Ba1 O7 63.3(3) . 6_657 ? O4 Ba1 O7 127.8(3) . 6_657 ? O5 Ba1 O7 101.3(3) . 6_657 ? O2 Ba1 O7 60.9(3) 6_657 6_657 ? O5 Ba1 O7 161.9(3) 5_556 6_657 ? O9 Ba1 Se1 96.9(2) . . ? O8 Ba1 Se1 148.3(2) . . ? O6 Ba1 Se1 141.8(2) . . ? O4 Ba1 Se1 133.06(19) . . ? O5 Ba1 Se1 74.3(2) . . ? O2 Ba1 Se1 71.08(18) 6_657 . ? O5 Ba1 Se1 65.9(2) 5_556 . ? O7 Ba1 Se1 98.94(18) 6_657 . ? O9 Ba1 Ba2 74.1(2) . . ? O8 Ba1 Ba2 40.0(2) . . ? O6 Ba1 Ba2 40.73(19) . . ? O4 Ba1 Ba2 37.87(17) . . ? O5 Ba1 Ba2 108.4(2) . . ? O2 Ba1 Ba2 110.41(18) 6_657 . ? O5 Ba1 Ba2 105.2(2) 5_556 . ? O7 Ba1 Ba2 90.85(18) 6_657 . ? Se1 Ba1 Ba2 169.20(4) . . ? O3 Ba2 O4 130.5(3) . . ? O3 Ba2 O1 67.1(3) . . ? O4 Ba2 O1 142.0(3) . . ? O3 Ba2 O1 69.3(3) . 5_557 ? O4 Ba2 O1 143.2(3) . 5_557 ? O1 Ba2 O1 70.4(3) . 5_557 ? O3 Ba2 O7 81.1(4) . . ? O4 Ba2 O7 77.3(3) . . ? O1 Ba2 O7 72.9(3) . . ? O1 Ba2 O7 139.5(3) 5_557 . ? O3 Ba2 O2 131.1(3) . . ? O4 Ba2 O2 77.4(3) . . ? O1 Ba2 O2 69.3(3) . . ? O1 Ba2 O2 114.6(3) 5_557 . ? O7 Ba2 O2 65.9(3) . . ? O3 Ba2 O8 71.5(3) . . ? O4 Ba2 O8 61.7(3) . . ? O1 Ba2 O8 133.9(3) . . ? O1 Ba2 O8 112.5(3) 5_557 . ? O7 Ba2 O8 81.8(3) . . ? O2 Ba2 O8 132.6(3) . . ? O3 Ba2 O6 96.1(3) . . ? O4 Ba2 O6 75.2(3) . . ? O1 Ba2 O6 141.9(2) . . ? O1 Ba2 O6 71.7(2) 5_557 . ? O7 Ba2 O6 140.6(3) . . ? O2 Ba2 O6 132.4(3) . . ? O8 Ba2 O6 60.5(3) . . ? O3 Ba2 Se2 138.9(2) . . ? O4 Ba2 Se2 83.1(2) . . ? O1 Ba2 Se2 102.4(2) . . ? O1 Ba2 Se2 69.8(2) 5_557 . ? O7 Ba2 Se2 135.7(3) . . ? O2 Ba2 Se2 71.4(2) . . ? O8 Ba2 Se2 122.2(2) . . ? O6 Ba2 Se2 67.3(2) . . ? O3 Ba2 Ba1 106.8(2) . . ? O4 Ba2 Ba1 39.4(2) . . ? O1 Ba2 Ba1 173.0(2) . . ? O1 Ba2 Ba1 111.29(18) 5_557 . ? O7 Ba2 Ba1 103.2(2) . . ? O2 Ba2 Ba1 114.89(18) . . ? O8 Ba2 Ba1 39.0(2) . . ? O6 Ba2 Ba1 39.75(17) . . ? Se2 Ba2 Ba1 84.51(3) . . ? O3 Ba2 Ba2 63.0(2) . 5_557 ? O4 Ba2 Ba2 166.5(2) . 5_557 ? O1 Ba2 Ba2 35.54(18) . 5_557 ? O1 Ba2 Ba2 34.87(18) 5_557 5_557 ? O7 Ba2 Ba2 106.9(2) . 5_557 ? O2 Ba2 Ba2 92.41(18) . 5_557 ? O8 Ba2 Ba2 131.1(2) . 5_557 ? O6 Ba2 Ba2 106.49(17) . 5_557 ? Se2 Ba2 Ba2 85.27(3) . 5_557 ? Ba1 Ba2 Ba2 145.72(3) . 5_557 ? Se4 Ge1 Se3 107.72(8) . . ? Se4 Ge1 Se1 110.55(8) . . ? Se3 Ge1 Se1 106.60(8) . . ? Se4 Ge1 Se2 111.29(8) . 7_565 ? Se3 Ge1 Se2 113.45(7) . 7_565 ? Se1 Ge1 Se2 107.15(8) . 7_565 ? Ge1 Se1 Ba1 108.60(6) . . ? Ge1 Se2 Ba2 122.70(7) 7_566 . ? Ba2 O1 Ba2 109.6(3) . 5_557 ? Ba2 O2 Ba1 119.7(4) . 6_557 ? Ba2 O4 Ba1 102.8(3) . . ? Ba1 O5 Ba1 114.0(4) . 5_556 ? Ba1 O6 Ba2 99.5(3) . . ? Ba2 O7 Ba1 109.8(4) . 6_557 ? Ba1 O8 Ba2 101.0(4) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.476 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.104 # Attachment '2_rev.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 284720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H60 Ba3 Ge4 Mn6 O30 Se17' _chemical_formula_weight 2914.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 20.463(3) _cell_length_b 20.463(3) _cell_length_c 25.119(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9109(3) _cell_formula_units_Z 6 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment_of_an_rhombic_dodecahedron_ _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7944 _exptl_absorpt_coefficient_mu 15.313 _exptl_absorpt_correction_type semiempirical _exptl_absorpt_correction_T_min 0.21290 _exptl_absorpt_correction_T_max 0.31967 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40197 _diffrn_reflns_av_R_equivalents 0.1120 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3786 _reflns_number_gt 3413 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+3.5508P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 3786 _refine_ls_number_parameters 184 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 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 Ba1 Ba -0.67079(4) -0.61111(4) -0.09876(3) 0.0339(5) Uani 1 1 d . . . Se1 Se -0.6667 -0.3333 0.25486(7) 0.0352(6) Uani 1 3 d S . . Se2 Se -0.84669(6) -0.65281(6) -0.07191(5) 0.0337(5) Uani 1 1 d . . . Se3 Se -0.72941(6) -0.45664(6) -0.11562(4) 0.0303(5) Uani 1 1 d . . . Se4 Se -0.67548(6) -0.52413(6) 0.01339(4) 0.0294(5) Uani 1 1 d . . . Se5 Se -0.81528(6) -0.79769(6) -0.15184(4) 0.0301(5) Uani 1 1 d . . . Se6 Se -0.80053(6) -0.39308(6) 0.13713(4) 0.0300(5) Uani 1 1 d . . . Se7 Se -0.6667 -0.3333 0.01362(8) 0.0280(5) Uani 1 3 d S . . Mn1 Mn -0.60357(9) -0.20927(9) -0.04985(7) 0.0312(5) Uani 1 1 d . . . Mn2 Mn -0.72149(9) -0.26403(9) 0.07659(7) 0.0315(5) Uani 1 1 d . . . O1 O -0.5627(4) -0.4559(4) -0.1090(3) 0.0331(16) Uani 1 1 d . . . O2 O -0.7667(5) -0.2035(4) 0.1259(3) 0.0388(18) Uani 1 1 d . . . Ge1 Ge -0.6667 -0.3333 -0.15246(7) 0.0280(6) Uani 1 3 d S . . Ge2 Ge -0.56670(6) -0.45585(6) 0.06654(4) 0.0276(5) Uani 1 1 d . . . O11 O -0.9657(5) -0.5923(4) -0.1052(3) 0.0381(18) Uani 1 1 d . . . O22 O -0.7748(5) -0.5220(5) 0.2371(3) 0.044(2) Uani 1 1 d . . . O33 O -0.6428(5) -0.8451(5) -0.1034(4) 0.053(2) Uani 1 1 d . . . O44 O -0.5986(5) -0.6710(6) -0.1544(4) 0.054(2) Uani 1 1 d . . . O55 O -0.5393(6) -0.3989(5) -0.2139(4) 0.047(2) Uani 1 1 d . . . O66 O -0.7250(5) -0.7231(5) -0.0199(3) 0.042(2) Uani 1 1 d . . . O77 O -0.5435(5) -0.5901(6) -0.0408(4) 0.049(2) Uani 1 1 d . . . O88 O -0.6676(5) -0.5758(5) -0.2058(3) 0.045(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0336(5) 0.0359(5) 0.0318(5) -0.0026(3) 0.0006(2) 0.0172(4) Se1 0.0397(7) 0.0397(7) 0.0264(10) 0.000 0.000 0.0198(4) Se2 0.0323(7) 0.0278(7) 0.0394(7) -0.0042(4) -0.0006(4) 0.0138(5) Se3 0.0312(7) 0.0286(7) 0.0299(7) 0.0001(4) -0.0002(4) 0.0139(5) Se4 0.0300(7) 0.0295(7) 0.0288(6) -0.0013(4) 0.0000(4) 0.0149(5) Se5 0.0290(6) 0.0324(7) 0.0283(6) -0.0008(4) 0.0016(4) 0.0149(5) Se6 0.0308(7) 0.0332(7) 0.0272(6) -0.0005(4) -0.0011(4) 0.0168(5) Se7 0.0283(6) 0.0283(6) 0.0274(8) 0.000 0.000 0.0142(3) Mn1 0.0321(9) 0.0300(9) 0.0289(9) -0.0013(6) -0.0006(6) 0.0136(7) Mn2 0.0292(9) 0.0307(9) 0.0326(9) -0.0025(7) 0.0008(7) 0.0135(7) O1 0.031(4) 0.030(4) 0.035(4) 0.000(3) -0.001(3) 0.013(3) O2 0.044(4) 0.038(4) 0.040(4) -0.006(3) -0.003(4) 0.024(4) Ge1 0.0292(7) 0.0292(7) 0.0257(10) 0.000 0.000 0.0146(3) Ge2 0.0286(7) 0.0285(7) 0.0271(7) 0.0008(4) 0.0009(4) 0.0154(5) O11 0.038(4) 0.038(4) 0.039(4) -0.003(3) -0.009(3) 0.019(4) O22 0.052(5) 0.041(4) 0.034(4) 0.003(3) -0.001(4) 0.018(4) O33 0.045(5) 0.043(5) 0.071(7) -0.008(5) -0.017(5) 0.022(4) O44 0.050(5) 0.057(6) 0.062(6) -0.023(5) -0.005(4) 0.031(5) O55 0.065(6) 0.040(4) 0.041(4) 0.000(4) 0.006(4) 0.029(4) O66 0.052(5) 0.035(4) 0.042(5) -0.003(3) -0.013(4) 0.024(4) O77 0.042(5) 0.065(6) 0.041(5) -0.007(4) 0.001(4) 0.027(4) O88 0.049(5) 0.047(5) 0.037(4) -0.001(4) -0.002(4) 0.023(4) _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 Ba1 O44 2.730(9) . ? Ba1 O88 2.777(8) . ? Ba1 O66 2.804(8) . ? Ba1 O77 2.824(9) . ? Ba1 O1 2.831(7) . ? Ba1 Se2 3.3268(13) . ? Ba1 Se4 3.3590(14) . ? Ba1 Se5 3.7160(14) . ? Se1 Ge1 2.328(3) 4_445 ? Se2 Ge2 2.3281(15) 12_444 ? Se3 Ge1 2.3732(13) . ? Se3 Mn1 2.745(2) 2_455 ? Se3 Mn1 2.745(2) 3_445 ? Se4 Ge2 2.3623(15) . ? Se4 Mn2 2.757(2) 2_455 ? Se4 Mn1 2.767(2) 3_445 ? Se5 Ge2 2.3626(15) 12_444 ? Se5 Mn1 2.750(2) 11_344 ? Se5 Mn2 2.824(2) 11_344 ? Se6 Ge2 2.3700(15) 3_445 ? Se6 Mn2 2.745(2) 2_455 ? Se6 Mn2 2.762(2) . ? Se7 Mn2 2.713(2) . ? Se7 Mn2 2.713(2) 2_455 ? Se7 Mn2 2.713(2) 3_445 ? Se7 Mn1 2.7158(19) 2_455 ? Se7 Mn1 2.7158(19) . ? Se7 Mn1 2.7158(19) 3_445 ? Mn1 O1 2.353(8) 2_455 ? Mn1 Se3 2.745(2) 3_445 ? Mn1 Se3 2.745(2) 2_455 ? Mn1 Se5 2.750(2) 17_454 ? Mn1 Se4 2.767(2) 2_455 ? Mn2 O2 2.251(8) . ? Mn2 Se6 2.745(2) 3_445 ? Mn2 Se4 2.757(2) 3_445 ? Mn2 Se5 2.824(2) 17_454 ? O1 Mn1 2.353(8) 3_445 ? Ge1 Se1 2.328(3) 4_444 ? Ge1 Se3 2.3732(13) 3_445 ? Ge1 Se3 2.3732(13) 2_455 ? Ge2 Se2 2.3282(15) 18_544 ? Ge2 Se5 2.3625(15) 18_544 ? Ge2 Se6 2.3700(15) 2_455 ? 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 O44 Ba1 O88 70.9(3) . . ? O44 Ba1 O66 94.4(3) . . ? O88 Ba1 O66 147.6(2) . . ? O44 Ba1 O77 70.6(3) . . ? O88 Ba1 O77 124.0(3) . . ? O66 Ba1 O77 73.6(3) . . ? O44 Ba1 O1 99.3(3) . . ? O88 Ba1 O1 73.5(2) . . ? O66 Ba1 O1 138.5(2) . . ? O77 Ba1 O1 74.5(3) . . ? O44 Ba1 Se2 138.4(2) . . ? O88 Ba1 Se2 98.34(19) . . ? O66 Ba1 Se2 73.27(18) . . ? O77 Ba1 Se2 137.07(18) . . ? O1 Ba1 Se2 116.38(16) . . ? O44 Ba1 Se4 146.4(2) . . ? O88 Ba1 Se4 132.68(19) . . ? O66 Ba1 Se4 74.73(17) . . ? O77 Ba1 Se4 75.85(18) . . ? O1 Ba1 Se4 72.27(16) . . ? Se2 Ba1 Se4 69.64(3) . . ? O44 Ba1 Se5 71.7(2) . . ? O88 Ba1 Se5 79.79(19) . . ? O66 Ba1 Se5 68.11(17) . . ? O77 Ba1 Se5 122.8(2) . . ? O1 Ba1 Se5 153.32(16) . . ? Se2 Ba1 Se5 66.81(3) . . ? Se4 Ba1 Se5 128.79(3) . . ? Ge2 Se2 Ba1 94.22(4) 12_444 . ? Ge1 Se3 Mn1 82.56(6) . 2_455 ? Ge1 Se3 Mn1 82.54(6) . 3_445 ? Mn1 Se3 Mn1 87.84(8) 2_455 3_445 ? Ge2 Se4 Mn2 84.57(5) . 2_455 ? Ge2 Se4 Mn1 82.95(6) . 3_445 ? Mn2 Se4 Mn1 90.61(6) 2_455 3_445 ? Ge2 Se4 Ba1 121.29(5) . . ? Mn2 Se4 Ba1 152.11(5) 2_455 . ? Mn1 Se4 Ba1 83.17(5) 3_445 . ? Ge2 Se5 Mn1 83.33(6) 12_444 11_344 ? Ge2 Se5 Mn2 81.92(5) 12_444 11_344 ? Mn1 Se5 Mn2 86.02(5) 11_344 11_344 ? Ge2 Se5 Ba1 84.24(4) 12_444 . ? Mn1 Se5 Ba1 146.96(5) 11_344 . ? Mn2 Se5 Ba1 122.23(5) 11_344 . ? Ge2 Se6 Mn2 83.52(5) 3_445 2_455 ? Ge2 Se6 Mn2 84.31(6) 3_445 . ? Mn2 Se6 Mn2 87.80(8) 2_455 . ? Mn2 Se7 Mn2 89.44(7) . 2_455 ? Mn2 Se7 Mn2 89.44(7) . 3_445 ? Mn2 Se7 Mn2 89.44(7) 2_455 3_445 ? Mn2 Se7 Mn1 92.66(5) . 2_455 ? Mn2 Se7 Mn1 88.92(5) 2_455 2_455 ? Mn2 Se7 Mn1 177.32(5) 3_445 2_455 ? Mn2 Se7 Mn1 88.92(5) . . ? Mn2 Se7 Mn1 177.32(5) 2_455 . ? Mn2 Se7 Mn1 92.66(5) 3_445 . ? Mn1 Se7 Mn1 89.03(7) 2_455 . ? Mn2 Se7 Mn1 177.32(5) . 3_445 ? Mn2 Se7 Mn1 92.66(5) 2_455 3_445 ? Mn2 Se7 Mn1 88.92(5) 3_445 3_445 ? Mn1 Se7 Mn1 89.03(7) 2_455 3_445 ? Mn1 Se7 Mn1 89.03(7) . 3_445 ? O1 Mn1 Se7 175.0(2) 2_455 . ? O1 Mn1 Se3 88.58(19) 2_455 3_445 ? Se7 Mn1 Se3 91.56(6) . 3_445 ? O1 Mn1 Se3 83.50(19) 2_455 2_455 ? Se7 Mn1 Se3 91.54(6) . 2_455 ? Se3 Mn1 Se3 87.18(7) 3_445 2_455 ? O1 Mn1 Se5 91.68(19) 2_455 17_454 ? Se7 Mn1 Se5 93.23(6) . 17_454 ? Se3 Mn1 Se5 96.81(6) 3_445 17_454 ? Se3 Mn1 Se5 173.68(8) 2_455 17_454 ? O1 Mn1 Se4 91.36(19) 2_455 2_455 ? Se7 Mn1 Se4 88.24(6) . 2_455 ? Se3 Mn1 Se4 176.99(8) 3_445 2_455 ? Se3 Mn1 Se4 89.83(6) 2_455 2_455 ? Se5 Mn1 Se4 86.20(6) 17_454 2_455 ? O2 Mn2 Se7 177.6(2) . . ? O2 Mn2 Se6 89.5(2) . 3_445 ? Se7 Mn2 Se6 91.45(6) . 3_445 ? O2 Mn2 Se4 90.5(2) . 3_445 ? Se7 Mn2 Se4 88.49(6) . 3_445 ? Se6 Mn2 Se4 177.96(8) 3_445 3_445 ? O2 Mn2 Se6 91.1(2) . . ? Se7 Mn2 Se6 91.07(6) . . ? Se6 Mn2 Se6 96.75(7) 3_445 . ? Se4 Mn2 Se6 85.28(5) 3_445 . ? O2 Mn2 Se5 86.2(2) . 17_454 ? Se7 Mn2 Se5 91.64(6) . 17_454 ? Se6 Mn2 Se5 85.73(5) 3_445 17_454 ? Se4 Mn2 Se5 92.24(6) 3_445 17_454 ? Se6 Mn2 Se5 176.28(8) . 17_454 ? Mn1 O1 Ba1 103.8(3) 3_445 . ? Se1 Ge1 Se3 112.95(5) 4_444 3_445 ? Se1 Ge1 Se3 112.95(5) 4_444 2_455 ? Se3 Ge1 Se3 105.78(5) 3_445 2_455 ? Se1 Ge1 Se3 112.95(5) 4_444 . ? Se3 Ge1 Se3 105.78(5) 3_445 . ? Se3 Ge1 Se3 105.78(5) 2_455 . ? Se2 Ge2 Se4 113.56(6) 18_544 . ? Se2 Ge2 Se5 112.09(6) 18_544 18_544 ? Se4 Ge2 Se5 105.85(6) . 18_544 ? Se2 Ge2 Se6 113.84(6) 18_544 2_455 ? Se4 Ge2 Se6 104.39(5) . 2_455 ? Se5 Ge2 Se6 106.39(6) 18_544 2_455 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.360 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.077