# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global #TrackingRef '- compound-20101220.cif' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Xiao-Ying Huang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. CHINA ; _publ_contact_author_email xyhuang@fjirsm.ac.cn _publ_contact_author_phone 86-59183793727 _publ_contact_author_fax 86-59183793727 loop_ _publ_author_name _publ_author_address 'Jian-Rong Li' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. CHINA ; 'Xiao-Ying Huang' ; State Key Lab of Structural Chemistry Fujian Institute of Reseach on the Structure of Matter, Chinese Academy of Sciences Fuzhou 350002 P. R. CHINA ; _publ_section_title ; [(Me)~2~NH~2~]~0.75~[Ag~1.25~SnSe~3~]: A Three-dimensionally Microporous Chalcogenide Exhibiting Framework Flexibility Upon Ion-exchange ; #===End data_Compound-1Rb _database_code_depnum_ccdc_archive 'CCDC 772737' #TrackingRef '- compound-20101220.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C0.2 H0.8 N0.1, Ag1.25 Se3 Sn, Rb0.65, H1.5 O0.75' _chemical_formula_sum 'C0.20 H2.30 Ag1.25 N0.10 O0.75 Rb0.65 Se3 Sn' _chemical_formula_weight 564.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 m' _symmetry_space_group_name_Hall 'P -4 2ab' 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' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 13.998(2) _cell_length_b 13.998(2) _cell_length_c 8.6852(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1701.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1533 _cell_measurement_theta_min 2.0574 _cell_measurement_theta_max 27.4603 _exptl_crystal_description lathe _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 22.227 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6967 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number 1192 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13288 _diffrn_reflns_av_R_equivalents 0.0888 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2066 _reflns_number_gt 1771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0700P)^2^+8.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment none _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 0.31(3) _refine_ls_number_reflns 2066 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Sn1 Sn 0.32677(8) 0.34798(7) 0.24134(14) 0.0383(3) Uani 1 1 d . . . Ag1 Ag 0.55446(11) 0.39918(10) 0.3713(2) 0.0575(4) Uani 1 1 d . . . Ag2 Ag 0.5000 0.5000 0.0000 0.0680(9) Uani 1 4 d S . . Se1 Se 0.48538(12) 0.32278(13) 0.1208(2) 0.0457(4) Uani 1 1 d . . . Se2 Se 0.29257(13) 0.49826(12) 0.3871(2) 0.0447(4) Uani 1 1 d . . . Se3 Se 0.18897(17) 0.31103(17) 0.0542(4) 0.0588(8) Uani 1 2 d S . . Se4 Se 0.28994(16) 0.21006(16) 0.4274(3) 0.0538(8) Uani 1 2 d S . . Rb1A Rb 0.1409(5) 0.6409(5) 0.1446(10) 0.099(3) Uani 0.63 2 d SP . . Rb1B Rb 0.1929(18) 0.6929(18) 0.180(2) 0.090(9) Uani 0.17 2 d SP . . Rb2 Rb 0.1200(5) 0.3800(5) 0.6587(10) 0.101(3) Uani 0.50 2 d SP . . O1 O 0.0673(10) 0.5673(10) 0.824(4) 0.105(11) Uani 1 2 d S . . O2A O 0.0000 0.5000 0.400(17) 0.18(6) Uani 0.60 4 d SP . . O2B O 0.0000 0.5000 0.28(4) 0.26(15) Uani 0.40 4 d SP . . 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 Sn1 0.0373(5) 0.0369(5) 0.0408(6) 0.0002(5) -0.0001(5) -0.0089(4) Ag1 0.0535(9) 0.0510(8) 0.0679(11) -0.0008(8) -0.0073(8) -0.0075(7) Ag2 0.0584(11) 0.0584(11) 0.087(3) 0.000 0.000 0.000 Se1 0.0475(10) 0.0499(9) 0.0397(10) -0.0022(9) 0.0084(8) 0.0029(8) Se2 0.0420(9) 0.0412(8) 0.0510(11) -0.0043(9) 0.0016(8) 0.0010(7) Se3 0.0628(11) 0.0628(11) 0.0507(17) 0.0216(11) -0.0216(11) -0.0264(14) Se4 0.0555(10) 0.0555(10) 0.0504(18) 0.0166(10) -0.0166(10) -0.0218(12) Rb1A 0.111(4) 0.111(4) 0.076(5) 0.017(4) 0.017(4) 0.035(4) Rb1B 0.123(15) 0.123(15) 0.024(9) 0.019(10) 0.019(10) 0.073(18) Rb2 0.110(4) 0.110(4) 0.083(6) -0.005(4) 0.005(4) -0.020(5) O1 0.053(8) 0.053(8) 0.21(4) 0.004(10) 0.004(10) -0.022(10) O2A 0.15(7) 0.15(7) 0.23(15) 0.000 0.000 0.10(8) O2B 0.18(12) 0.18(12) 0.4(4) 0.000 0.000 -0.14(13) _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 Sn1 Se1 2.480(2) . ? Sn1 Se2 2.501(2) . ? Sn1 Se4 2.570(2) . ? Sn1 Se3 2.575(2) . ? Ag1 Se2 2.582(2) 2_665 ? Ag1 Se1 2.610(3) . ? Ag1 Se2 2.678(3) 4_656 ? Ag1 Ag1 3.185(3) 4_656 ? Ag1 Ag1 3.185(3) 3_566 ? Ag1 Ag1 3.208(3) 2_665 ? Ag2 Se1 2.7012(19) 2_665 ? Ag2 Se1 2.7012(19) 3_565 ? Ag2 Se1 2.7012(19) . ? Ag2 Se1 2.7012(19) 4_655 ? Se2 Ag1 2.582(2) 2_665 ? Se2 Ag1 2.678(3) 3_566 ? Se3 Sn1 2.575(2) 7 ? Se4 Sn1 2.570(2) 7 ? Se1 Rb1A 3.862(5) 4_655 ? Se1 Rb2 3.908(5) 4_656 ? Se1 Rb1B 4.046(14) 4_655 ? Se2 Rb1B 3.550(12) . ? Se2 Rb1A 3.596(5) . ? Se2 Rb2 3.761(6) . ? Se3 Rb1B 3.10(3) 4_655 ? Se3 Rb2 3.696(9) 1_554 ? Se3 Rb1A 3.785(9) 4_655 ? Se4 Rb1B 3.42(2) 4_656 ? Se4 Rb2 3.918(10) . ? Se4 Rb1A 3.962(10) 4_656 ? Rb1A O2B 3.02(12) . ? Rb1A O1 3.14(3) 1_554 ? Rb1A O2A 3.56(9) . ? Rb1A Se2 3.596(5) 8_455 ? Rb1A Se3 3.785(9) 3_565 ? Rb1A Se1 3.862(5) 5 ? Rb1A Se1 3.862(5) 3_565 ? Rb1A Se4 3.962(10) 3_566 ? Rb1B Se3 3.10(3) 3_565 ? Rb1B Se4 3.42(2) 3_566 ? Rb1B Se2 3.550(12) 8_455 ? Rb1B Se1 4.046(14) 5 ? Rb1B Se1 4.046(14) 3_565 ? Rb2 O1 3.08(2) . ? Rb2 O1 3.08(2) 2_565 ? Rb2 O2A 3.27(10) . ? Rb2 Se3 3.696(9) 1_556 ? Rb2 Se2 3.761(6) 7 ? Rb2 Se1 3.908(5) 3_566 ? Rb2 Se1 3.908(5) 6_456 ? O1 Rb2 3.08(2) 2_565 ? O1 Rb1A 3.14(3) 1_556 ? O2A Rb2 3.27(10) 2_565 ? O2A Rb1A 3.56(9) 2_565 ? O2B Rb1A 3.02(12) 2_565 ? Sn1 Rb1B 4.265(18) 4_655 ? Ag1 Rb2 4.022(6) 4_656 ? Ag1 Rb1B 4.113(18) 2_665 ? Rb1B Rb2 3.96(4) 3_566 ? Rb1B Ag1 4.113(18) 7_565 ? Rb1B Ag1 4.113(18) 2_665 ? Rb1B Sn1 4.265(18) 5 ? Rb1B Sn1 4.265(18) 3_565 ? Rb2 Rb1B 3.96(4) 4_656 ? Rb2 Ag1 4.022(6) 3_566 ? Rb2 Ag1 4.022(6) 6_456 ? 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 Se1 Sn1 Se2 120.31(7) . . ? Se1 Sn1 Se4 109.77(9) . . ? Se2 Sn1 Se4 105.97(10) . . ? Se1 Sn1 Se3 112.06(10) . . ? Se2 Sn1 Se3 110.18(10) . . ? Se4 Sn1 Se3 95.49(7) . . ? Se1 Sn1 Rb1B 67.9(3) . 4_655 ? Se2 Sn1 Rb1B 148.2(5) . 4_655 ? Se4 Sn1 Rb1B 98.3(3) . 4_655 ? Se3 Sn1 Rb1B 46.2(4) . 4_655 ? Se2 Ag1 Se1 125.40(9) 2_665 . ? Se2 Ag1 Se2 119.79(7) 2_665 4_656 ? Se1 Ag1 Se2 108.83(8) . 4_656 ? Se2 Ag1 Ag1 54.14(6) 2_665 4_656 ? Se1 Ag1 Ag1 160.09(8) . 4_656 ? Se2 Ag1 Ag1 83.49(8) 4_656 4_656 ? Se2 Ag1 Ag1 114.55(8) 2_665 3_566 ? Se1 Ag1 Ag1 114.56(8) . 3_566 ? Se2 Ag1 Ag1 51.37(7) 4_656 3_566 ? Ag1 Ag1 Ag1 60.49(6) 4_656 3_566 ? Se2 Ag1 Ag1 84.54(7) 2_665 2_665 ? Se1 Ag1 Ag1 100.63(6) . 2_665 ? Se2 Ag1 Ag1 111.06(6) 4_656 2_665 ? Ag1 Ag1 Ag1 59.76(3) 4_656 2_665 ? Ag1 Ag1 Ag1 59.76(3) 3_566 2_665 ? Se2 Ag1 Rb2 110.76(14) 2_665 4_656 ? Se1 Ag1 Rb2 68.43(13) . 4_656 ? Se2 Ag1 Rb2 64.69(14) 4_656 4_656 ? Ag1 Ag1 Rb2 131.46(14) 4_656 4_656 ? Ag1 Ag1 Rb2 113.53(14) 3_566 4_656 ? Ag1 Ag1 Rb2 164.40(14) 2_665 4_656 ? Se2 Ag1 Rb1B 58.9(5) 2_665 2_665 ? Se1 Ag1 Rb1B 81.6(3) . 2_665 ? Se2 Ag1 Rb1B 112.2(3) 4_656 2_665 ? Ag1 Ag1 Rb1B 108.8(4) 4_656 2_665 ? Ag1 Ag1 Rb1B 159.0(3) 3_566 2_665 ? Ag1 Ag1 Rb1B 133.2(4) 2_665 2_665 ? Rb2 Ag1 Rb1B 58.2(5) 4_656 2_665 ? Se1 Ag2 Se1 98.67(3) 2_665 3_565 ? Se1 Ag2 Se1 134.30(8) 2_665 . ? Se1 Ag2 Se1 98.67(3) 3_565 . ? Se1 Ag2 Se1 98.67(3) 2_665 4_655 ? Se1 Ag2 Se1 134.30(8) 3_565 4_655 ? Se1 Ag2 Se1 98.67(3) . 4_655 ? Sn1 Se1 Ag1 85.49(7) . . ? Sn1 Se1 Ag2 95.81(6) . . ? Ag1 Se1 Ag2 85.38(7) . . ? Sn1 Se1 Rb1A 86.33(13) . 4_655 ? Ag1 Se1 Rb1A 159.55(14) . 4_655 ? Ag2 Se1 Rb1A 114.10(14) . 4_655 ? Sn1 Se1 Rb2 109.16(14) . 4_656 ? Ag1 Se1 Rb2 73.17(14) . 4_656 ? Ag2 Se1 Rb2 145.15(16) . 4_656 ? Rb1A Se1 Rb2 92.0(2) 4_655 4_656 ? Sn1 Se1 Rb1B 77.5(4) . 4_655 ? Ag1 Se1 Rb1B 162.0(3) . 4_655 ? Ag2 Se1 Rb1B 102.0(4) . 4_655 ? Rb1A Se1 Rb1B 15.4(4) 4_655 4_655 ? Rb2 Se1 Rb1B 106.7(5) 4_656 4_655 ? Sn1 Se2 Ag1 106.38(8) . 2_665 ? Sn1 Se2 Ag1 93.33(7) . 3_566 ? Ag1 Se2 Ag1 74.49(8) 2_665 3_566 ? Sn1 Se2 Rb1B 117.7(4) . . ? Ag1 Se2 Rb1B 82.6(6) 2_665 . ? Ag1 Se2 Rb1B 145.8(5) 3_566 . ? Sn1 Se2 Rb1A 106.47(15) . . ? Ag1 Se2 Rb1A 98.62(16) 2_665 . ? Ag1 Se2 Rb1A 160.19(15) 3_566 . ? Rb1B Se2 Rb1A 17.3(5) . . ? Sn1 Se2 Rb2 94.02(14) . . ? Ag1 Se2 Rb2 144.18(14) 2_665 . ? Ag1 Se2 Rb2 75.23(15) 3_566 . ? Rb1B Se2 Rb2 113.8(4) . . ? Rb1A Se2 Rb2 103.5(2) . . ? Sn1 Se3 Sn1 84.41(9) . 7 ? Sn1 Se3 Rb1B 97.0(4) . 4_655 ? Sn1 Se3 Rb1B 97.0(4) 7 4_655 ? Sn1 Se3 Rb2 136.87(6) . 1_554 ? Sn1 Se3 Rb2 136.86(6) 7 1_554 ? Rb1B Se3 Rb2 70.6(6) 4_655 1_554 ? Sn1 Se3 Rb1A 86.72(14) . 4_655 ? Sn1 Se3 Rb1A 86.72(14) 7 4_655 ? Rb1B Se3 Rb1A 13.9(5) 4_655 4_655 ? Rb2 Se3 Rb1A 84.5(2) 1_554 4_655 ? Sn1 Se4 Sn1 84.61(9) 7 . ? Sn1 Se4 Rb1B 131.6(3) 7 4_656 ? Sn1 Se4 Rb1B 131.6(3) . 4_656 ? Sn1 Se4 Rb2 89.32(13) 7 . ? Sn1 Se4 Rb2 89.32(13) . . ? Rb1B Se4 Rb2 64.8(6) 4_656 . ? Sn1 Se4 Rb1A 136.43(6) 7 4_656 ? Sn1 Se4 Rb1A 136.43(6) . 4_656 ? Rb1B Se4 Rb1A 14.5(6) 4_656 4_656 ? Rb2 Se4 Rb1A 79.4(2) . 4_656 ? Rb1B Rb1A O2B 141(6) . . ? Rb1B Rb1A O1 134.4(14) . 1_554 ? O2B Rb1A O1 85(6) . 1_554 ? Rb1B Rb1A O2A 125(2) . . ? O2B Rb1A O2A 16(6) . . ? O1 Rb1A O2A 100.9(19) 1_554 . ? Rb1B Rb1A Se2 78.9(7) . 8_455 ? O2B Rb1A Se2 78(3) . 8_455 ? O1 Rb1A Se2 122.0(2) 1_554 8_455 ? O2A Rb1A Se2 69.8(9) . 8_455 ? Rb1B Rb1A Se2 78.9(7) . . ? O2B Rb1A Se2 78(3) . . ? O1 Rb1A Se2 122.0(2) 1_554 . ? O2A Rb1A Se2 69.8(9) . . ? Se2 Rb1A Se2 108.2(2) 8_455 . ? Rb1B Rb1A Se3 43.9(12) . 3_565 ? O2B Rb1A Se3 175(6) . 3_565 ? O1 Rb1A Se3 90.5(5) 1_554 3_565 ? O2A Rb1A Se3 168.6(19) . 3_565 ? Se2 Rb1A Se3 104.18(19) 8_455 3_565 ? Se2 Rb1A Se3 104.18(19) . 3_565 ? Rb1B Rb1A Se1 92.0(8) . 5 ? O2B Rb1A Se1 111(3) . 5 ? O1 Rb1A Se1 62.4(2) 1_554 5 ? O2A Rb1A Se1 118.9(8) . 5 ? Se2 Rb1A Se1 72.91(5) 8_455 5 ? Se2 Rb1A Se1 170.3(3) . 5 ? Se3 Rb1A Se1 66.48(12) 3_565 5 ? Rb1B Rb1A Se1 92.0(8) . 3_565 ? O2B Rb1A Se1 111(3) . 3_565 ? O1 Rb1A Se1 62.4(2) 1_554 3_565 ? O2A Rb1A Se1 118.9(8) . 3_565 ? Se2 Rb1A Se1 170.3(3) 8_455 3_565 ? Se2 Rb1A Se1 72.91(5) . 3_565 ? Se3 Rb1A Se1 66.48(12) 3_565 3_565 ? Se1 Rb1A Se1 104.3(2) 5 3_565 ? Rb1B Rb1A Se4 53.0(12) . 3_566 ? O2B Rb1A Se4 88(6) . 3_566 ? O1 Rb1A Se4 172.6(5) 1_554 3_566 ? O2A Rb1A Se4 71.7(18) . 3_566 ? Se2 Rb1A Se4 56.06(12) 8_455 3_566 ? Se2 Rb1A Se4 56.06(12) . 3_566 ? Se3 Rb1A Se4 96.9(2) 3_565 3_566 ? Se1 Rb1A Se4 120.70(16) 5 3_566 ? Se1 Rb1A Se4 120.70(16) 3_565 3_566 ? Rb1B Rb1A Rb2 3.1(12) . 3_566 ? O2B Rb1A Rb2 138(6) . 3_566 ? O1 Rb1A Rb2 137.5(5) 1_554 3_566 ? O2A Rb1A Rb2 121.6(19) . 3_566 ? Se2 Rb1A Rb2 77.15(17) 8_455 3_566 ? Se2 Rb1A Rb2 77.15(17) . 3_566 ? Se3 Rb1A Rb2 46.98(16) 3_565 3_566 ? Se1 Rb1A Rb2 93.93(17) 5 3_566 ? Se1 Rb1A Rb2 93.93(17) 3_565 3_566 ? Se4 Rb1A Rb2 49.93(15) 3_566 3_566 ? Rb1A Rb1B Se3 122.2(14) . 3_565 ? Rb1A Rb1B Se4 112.4(16) . 3_566 ? Se3 Rb1B Se4 125.4(11) 3_565 3_566 ? Rb1A Rb1B Se2 83.8(10) . 8_455 ? Se3 Rb1B Se2 122.2(5) 3_565 8_455 ? Se4 Rb1B Se2 61.5(3) 3_566 8_455 ? Rb1A Rb1B Se2 83.8(10) . . ? Se3 Rb1B Se2 122.2(5) 3_565 . ? Se4 Rb1B Se2 61.5(3) 3_566 . ? Se2 Rb1B Se2 110.3(6) 8_455 . ? Rb1A Rb1B Rb2 176.0(15) . 3_566 ? Se3 Rb1B Rb2 61.7(6) 3_565 3_566 ? Se4 Rb1B Rb2 63.6(5) 3_566 3_566 ? Se2 Rb1B Rb2 94.0(6) 8_455 3_566 ? Se2 Rb1B Rb2 94.0(6) . 3_566 ? Rb1A Rb1B Se1 72.6(8) . 5 ? Se3 Rb1B Se1 70.4(3) 3_565 5 ? Se4 Rb1B Se1 130.9(2) 3_566 5 ? Se2 Rb1B Se1 71.15(17) 8_455 5 ? Se2 Rb1B Se1 156.1(11) . 5 ? Rb2 Rb1B Se1 109.8(6) 3_566 5 ? Rb1A Rb1B Se1 72.6(8) . 3_565 ? Se3 Rb1B Se1 70.4(3) 3_565 3_565 ? Se4 Rb1B Se1 130.9(2) 3_566 3_565 ? Se2 Rb1B Se1 156.1(11) 8_455 3_565 ? Se2 Rb1B Se1 71.15(17) . 3_565 ? Rb2 Rb1B Se1 109.8(6) 3_566 3_565 ? Se1 Rb1B Se1 97.9(5) 5 3_565 ? Rb1A Rb1B Ag1 119.1(7) . 7_565 ? Se3 Rb1B Ag1 88.5(6) 3_565 7_565 ? Se4 Rb1B Ag1 63.9(3) 3_566 7_565 ? Se2 Rb1B Ag1 38.50(15) 8_455 7_565 ? Se2 Rb1B Ag1 125.4(6) . 7_565 ? Rb2 Rb1B Ag1 59.7(4) 3_566 7_565 ? Se1 Rb1B Ag1 71.41(11) 5 7_565 ? Se1 Rb1B Ag1 158.7(7) 3_565 7_565 ? Rb1A Rb1B Ag1 119.1(7) . 2_665 ? Se3 Rb1B Ag1 88.5(6) 3_565 2_665 ? Se4 Rb1B Ag1 63.9(3) 3_566 2_665 ? Se2 Rb1B Ag1 125.4(6) 8_455 2_665 ? Se2 Rb1B Ag1 38.50(15) . 2_665 ? Rb2 Rb1B Ag1 59.7(4) 3_566 2_665 ? Se1 Rb1B Ag1 158.7(7) 5 2_665 ? Se1 Rb1B Ag1 71.41(11) 3_565 2_665 ? Ag1 Rb1B Ag1 112.1(7) 7_565 2_665 ? Rb1A Rb1B Sn1 93.1(12) . 5 ? Se3 Rb1B Sn1 36.81(19) 3_565 5 ? Se4 Rb1B Sn1 145.4(8) 3_566 5 ? Se2 Rb1B Sn1 100.66(15) 8_455 5 ? Se2 Rb1B Sn1 148.3(4) . 5 ? Rb2 Rb1B Sn1 90.5(6) 3_566 5 ? Se1 Rb1B Sn1 34.59(13) 5 5 ? Se1 Rb1B Sn1 77.8(3) 3_565 5 ? Ag1 Rb1B Sn1 83.6(3) 7_565 5 ? Ag1 Rb1B Sn1 124.2(6) 2_665 5 ? Rb1A Rb1B Sn1 93.1(12) . 3_565 ? Se3 Rb1B Sn1 36.81(19) 3_565 3_565 ? Se4 Rb1B Sn1 145.4(8) 3_566 3_565 ? Se2 Rb1B Sn1 148.3(4) 8_455 3_565 ? Se2 Rb1B Sn1 100.66(15) . 3_565 ? Rb2 Rb1B Sn1 90.5(6) 3_566 3_565 ? Se1 Rb1B Sn1 77.8(3) 5 3_565 ? Se1 Rb1B Sn1 34.59(13) 3_565 3_565 ? Ag1 Rb1B Sn1 124.2(6) 7_565 3_565 ? Ag1 Rb1B Sn1 83.6(3) 2_665 3_565 ? Sn1 Rb1B Sn1 47.9(2) 5 3_565 ? O1 Rb2 O1 51.3(7) . 2_565 ? O1 Rb2 O2A 76.1(17) . . ? O1 Rb2 O2A 76.1(18) 2_565 . ? O1 Rb2 Se3 81.5(6) . 1_556 ? O1 Rb2 Se3 81.5(6) 2_565 1_556 ? O2A Rb2 Se3 155.1(19) . 1_556 ? O1 Rb2 Se2 137.2(5) . 7 ? O1 Rb2 Se2 94.1(5) 2_565 7 ? O2A Rb2 Se2 70.9(11) . 7 ? Se3 Rb2 Se2 122.02(17) 1_556 7 ? O1 Rb2 Se2 94.1(5) . . ? O1 Rb2 Se2 137.2(5) 2_565 . ? O2A Rb2 Se2 70.9(11) . . ? Se3 Rb2 Se2 122.02(17) 1_556 . ? Se2 Rb2 Se2 99.9(2) 7 . ? O1 Rb2 Se1 62.3(3) . 3_566 ? O1 Rb2 Se1 105.9(5) 2_565 3_566 ? O2A Rb2 Se1 117.5(5) . 3_566 ? Se3 Rb2 Se1 58.73(12) 1_556 3_566 ? Se2 Rb2 Se1 159.5(3) 7 3_566 ? Se2 Rb2 Se1 68.20(5) . 3_566 ? O1 Rb2 Se1 105.9(5) . 6_456 ? O1 Rb2 Se1 62.3(3) 2_565 6_456 ? O2A Rb2 Se1 117.5(5) . 6_456 ? Se3 Rb2 Se1 58.73(12) 1_556 6_456 ? Se2 Rb2 Se1 68.20(5) 7 6_456 ? Se2 Rb2 Se1 159.5(3) . 6_456 ? Se1 Rb2 Se1 117.4(2) 3_566 6_456 ? O1 Rb2 Se4 154.4(4) . . ? O1 Rb2 Se4 154.4(4) 2_565 . ? O2A Rb2 Se4 105.7(19) . . ? Se3 Rb2 Se4 99.2(2) 1_556 . ? Se2 Rb2 Se4 63.62(14) 7 . ? Se2 Rb2 Se4 63.62(14) . . ? Se1 Rb2 Se4 95.92(17) 3_566 . ? Se1 Rb2 Se4 95.92(17) 6_456 . ? O1 Rb2 Rb1B 123.9(6) . 4_656 ? O1 Rb2 Rb1B 123.9(6) 2_565 4_656 ? O2A Rb2 Rb1B 157.3(19) . 4_656 ? Se3 Rb2 Rb1B 47.6(3) 1_556 4_656 ? Se2 Rb2 Rb1B 95.1(3) 7 4_656 ? Se2 Rb2 Rb1B 95.1(3) . 4_656 ? Se1 Rb2 Rb1B 70.46(19) 3_566 4_656 ? Se1 Rb2 Rb1B 70.46(19) 6_456 4_656 ? Se4 Rb2 Rb1B 51.5(3) . 4_656 ? O1 Rb2 Ag1 93.9(3) . 3_566 ? O1 Rb2 Ag1 143.4(5) 2_565 3_566 ? O2A Rb2 Ag1 109.7(8) . 3_566 ? Se3 Rb2 Ag1 82.31(16) 1_556 3_566 ? Se2 Rb2 Ag1 122.2(2) 7 3_566 ? Se2 Rb2 Ag1 40.08(6) . 3_566 ? Se1 Rb2 Ag1 38.40(6) 3_566 3_566 ? Se1 Rb2 Ag1 131.8(3) 6_456 3_566 ? Se4 Rb2 Ag1 61.02(13) . 3_566 ? Rb1B Rb2 Ag1 62.05(15) 4_656 3_566 ? O1 Rb2 Ag1 143.4(5) . 6_456 ? O1 Rb2 Ag1 93.9(3) 2_565 6_456 ? O2A Rb2 Ag1 109.7(8) . 6_456 ? Se3 Rb2 Ag1 82.31(16) 1_556 6_456 ? Se2 Rb2 Ag1 40.08(6) 7 6_456 ? Se2 Rb2 Ag1 122.2(2) . 6_456 ? Se1 Rb2 Ag1 131.8(3) 3_566 6_456 ? Se1 Rb2 Ag1 38.40(6) 6_456 6_456 ? Se4 Rb2 Ag1 61.02(13) . 6_456 ? Rb1B Rb2 Ag1 62.05(15) 4_656 6_456 ? Ag1 Rb2 Ag1 116.0(2) 3_566 6_456 ? Rb2 O1 Rb2 101.0(9) 2_565 . ? Rb2 O1 Rb1A 127.9(6) 2_565 1_556 ? Rb2 O1 Rb1A 127.9(6) . 1_556 ? Rb2 O2A Rb2 93(4) 2_565 . ? O2B O2A Rb1A 51.5(18) . 2_565 ? Rb2 O2A Rb1A 115.3(2) 2_565 2_565 ? Rb2 O2A Rb1A 115.3(2) . 2_565 ? Rb2 O2A Rb1A 115.3(2) 2_565 . ? Rb2 O2A Rb1A 115.3(2) . . ? Rb1A O2A Rb1A 103(4) 2_565 . ? Rb1A O2B Rb1A 135(10) . 2_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.066 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.245 data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 772738' #TrackingRef '- compound-20101220.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C1.50 H6 N0.75, Ag1.25 Se3 Sn' _chemical_formula_sum 'C1.50 H6 Ag1.25 N0.75 Se3 Sn' _chemical_formula_weight 524.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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 21 m' _symmetry_space_group_name_Hall 'P -4 2ab' 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' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 13.8051(8) _cell_length_b 13.8051(8) _cell_length_c 9.6707(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1843.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1978 _cell_measurement_theta_min 2.0862 _cell_measurement_theta_max 27.4565 _exptl_crystal_description lathe _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 17.113 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5355 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14465 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2228 _reflns_number_gt 2068 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0360P)^2^+1.0000P] 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 constr _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 0.024(19) _refine_ls_number_reflns 2228 _refine_ls_number_parameters 86 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.003 _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 Sn1 Sn 0.15366(4) 0.17008(4) 0.73989(6) 0.03315(15) Uani 1 1 d . . . Ag1 Ag 0.10129(6) -0.05502(6) 0.62062(10) 0.0530(2) Uani 1 1 d . . . Ag2 Ag 0.0000 0.0000 1.0000 0.0576(4) Uani 1 4 d S . . Se1 Se 0.16614(7) 0.01071(7) 0.85827(9) 0.0414(2) Uani 1 1 d . . . Se2 Se 0.00683(7) 0.20791(7) 0.59732(10) 0.0414(2) Uani 1 1 d . . . Se3 Se 0.18297(8) 0.31703(8) 0.89922(15) 0.0450(3) Uani 1 2 d S . . Se4 Se 0.30477(8) 0.19523(8) 0.59081(15) 0.0435(3) Uani 1 2 d S . . N1 N 0.2862(19) 0.1413(18) 0.140(3) 0.137(6) Uani 0.50 1 d PDU . . H1A H 0.2460 0.1401 0.0668 0.164 Uiso 0.50 1 d PR . . H1B H 0.2675 0.0928 0.1964 0.164 Uiso 0.50 1 d PR . . C1 C 0.2665(13) 0.2335(13) 0.215(3) 0.138(5) Uani 1 2 d SDU . . H1C H 0.1993 0.2361 0.2396 0.207 Uiso 0.50 1 d PR . . H1D H 0.3055 0.2357 0.2968 0.207 Uiso 0.50 1 d PR . . H1E H 0.2822 0.2870 0.1561 0.207 Uiso 0.50 1 d PR . . C2 C 0.3843(14) 0.1157(14) 0.086(3) 0.141(5) Uani 1 2 d SDU . . H2C H 0.3817 0.0534 0.0409 0.211 Uiso 0.50 1 d PR . . H2D H 0.4056 0.1636 0.0214 0.211 Uiso 0.50 1 d PR . . H2E H 0.4289 0.1122 0.1621 0.211 Uiso 0.50 1 d PR . . N2 N 0.0000 0.5000 0.355(5) 0.299(7) Uani 1 4 d SDU . . H2A H 0.0156 0.5592 0.3234 0.358 Uiso 0.25 1 d PR . . H2B H -0.0592 0.4844 0.3234 0.358 Uiso 0.25 1 d PR . . C3 C 0.0000 0.5000 0.519(5) 0.290(7) Uani 1 4 d SDU . . H3A H -0.0464 0.5464 0.5516 0.435 Uiso 0.50 2 d SPR . . H3D H -0.0170 0.4367 0.5516 0.435 Uiso 0.25 1 d PR . . H3B H 0.0633 0.5170 0.5516 0.435 Uiso 0.25 1 d PR . . C4 C 0.074(2) 0.426(2) 0.312(10) 0.287(7) Uani 0.50 2 d SPDU . . H4A H 0.0756 0.4231 0.2130 0.430 Uiso 0.50 2 d SPR . . H4B H 0.1370 0.4440 0.3466 0.430 Uiso 0.25 1 d PR . . H4C H 0.0567 0.3637 0.3466 0.430 Uiso 0.25 1 d PR . . 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 Sn1 0.0297(3) 0.0319(3) 0.0378(3) 0.0015(3) 0.0010(3) -0.0048(2) Ag1 0.0465(5) 0.0478(5) 0.0645(5) -0.0051(4) -0.0007(4) -0.0038(3) Ag2 0.0571(6) 0.0571(6) 0.0588(11) 0.000 0.000 0.000 Se1 0.0444(5) 0.0370(5) 0.0427(5) 0.0074(4) 0.0013(4) 0.0012(4) Se2 0.0355(5) 0.0382(5) 0.0504(5) 0.0022(4) -0.0054(4) 0.0021(4) Se3 0.0467(5) 0.0467(5) 0.0414(7) -0.0120(4) 0.0120(4) -0.0066(6) Se4 0.0425(5) 0.0425(5) 0.0454(8) -0.0149(5) 0.0149(5) -0.0142(5) N1 0.136(7) 0.137(7) 0.137(7) 0.003(4) -0.001(4) -0.002(4) C1 0.139(5) 0.139(5) 0.137(6) 0.001(3) -0.001(3) -0.003(4) C2 0.141(5) 0.141(5) 0.141(6) 0.002(3) -0.002(3) 0.000(4) N2 0.299(7) 0.299(7) 0.298(8) 0.000 0.000 -0.001(5) C3 0.290(7) 0.290(7) 0.290(8) 0.000 0.000 -0.001(5) C4 0.287(7) 0.287(7) 0.287(8) -0.001(3) 0.001(3) 0.000(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 Sn1 Se1 2.4861(10) . ? Sn1 Se2 2.5064(11) . ? Sn1 Se4 2.5595(11) . ? Sn1 Se3 2.5795(12) . ? Ag1 Se2 2.5950(12) 2 ? Ag1 Se1 2.6281(13) . ? Ag1 Se2 2.6554(13) 3_556 ? Ag1 Ag1 3.1826(17) 2 ? Ag1 Ag1 3.2414(16) 3_556 ? Ag1 Ag1 3.2414(16) 4_556 ? Ag2 Se1 2.6759(10) 2 ? Ag2 Se1 2.6759(10) 4_557 ? Ag2 Se1 2.6759(10) 3_557 ? Ag2 Se1 2.6759(10) . ? Se2 Ag1 2.5950(12) 2 ? Se2 Ag1 2.6554(13) 4_556 ? Se3 Sn1 2.5795(12) 7 ? Se4 Sn1 2.5595(11) 7 ? N1 N1 1.42(5) 7 ? N1 C1 1.488(10) . ? N1 C2 1.494(10) . ? N1 H1A 0.9000 . ? N1 H1B 0.9001 . ? C1 N1 1.488(10) 7 ? C1 H1C 0.9597 . ? C1 H1D 0.9599 . ? C1 H1E 0.9564 . ? C2 N1 1.494(10) 7 ? C2 H2C 0.9654 . ? C2 H2D 0.9558 . ? C2 H2E 0.9603 . ? N2 C4 1.507(10) . ? N2 C4 1.507(10) 2_565 ? N2 C3 1.58(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? C3 H3A 0.9600 . ? C3 H3D 0.9600 . ? C3 H3B 0.9600 . ? C4 H4A 0.9606 . ? C4 H4B 0.9624 . ? C4 H4C 0.9516 . ? 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 Se1 Sn1 Se2 119.59(4) . . ? Se1 Sn1 Se4 108.84(4) . . ? Se2 Sn1 Se4 108.72(5) . . ? Se1 Sn1 Se3 114.21(5) . . ? Se2 Sn1 Se3 106.95(4) . . ? Se4 Sn1 Se3 95.85(3) . . ? Se2 Ag1 Se1 123.55(5) 2 . ? Se2 Ag1 Se2 116.98(4) 2 3_556 ? Se1 Ag1 Se2 114.76(4) . 3_556 ? Se2 Ag1 Ag1 83.27(4) 2 2 ? Se1 Ag1 Ag1 97.73(3) . 2 ? Se2 Ag1 Ag1 111.56(3) 3_556 2 ? Se2 Ag1 Ag1 52.72(3) 2 3_556 ? Se1 Ag1 Ag1 157.55(4) . 3_556 ? Se2 Ag1 Ag1 81.21(4) 3_556 3_556 ? Ag1 Ag1 Ag1 60.599(16) 2 3_556 ? Se2 Ag1 Ag1 111.45(4) 2 4_556 ? Se1 Ag1 Ag1 117.82(4) . 4_556 ? Se2 Ag1 Ag1 51.04(4) 3_556 4_556 ? Ag1 Ag1 Ag1 60.599(16) 2 4_556 ? Ag1 Ag1 Ag1 58.80(3) 3_556 4_556 ? Se1 Ag2 Se1 105.209(19) 2 4_557 ? Se1 Ag2 Se1 105.209(19) 2 3_557 ? Se1 Ag2 Se1 118.38(4) 4_557 3_557 ? Se1 Ag2 Se1 118.38(4) 2 . ? Se1 Ag2 Se1 105.209(19) 4_557 . ? Se1 Ag2 Se1 105.209(19) 3_557 . ? Sn1 Se1 Ag1 83.06(4) . . ? Sn1 Se1 Ag2 103.02(3) . . ? Ag1 Se1 Ag2 97.87(4) . . ? Sn1 Se2 Ag1 104.35(4) . 2 ? Sn1 Se2 Ag1 96.81(4) . 4_556 ? Ag1 Se2 Ag1 76.24(4) 2 4_556 ? Sn1 Se3 Sn1 83.68(5) . 7 ? Sn1 Se4 Sn1 84.48(5) 7 . ? N1 N1 C1 61.6(11) 7 . ? N1 N1 C2 61.7(11) 7 . ? C1 N1 C2 123(2) . . ? N1 N1 H1A 116.6 7 . ? C1 N1 H1A 106.5 . . ? C2 N1 H1A 106.2 . . ? N1 N1 H1B 136.7 7 . ? C1 N1 H1B 106.9 . . ? C2 N1 H1B 107.2 . . ? H1A N1 H1B 106.6 . . ? N1 C1 N1 57(2) 7 . ? N1 C1 H1C 162.9 7 . ? N1 C1 H1C 109.3 . . ? N1 C1 H1D 85.8 7 . ? N1 C1 H1D 109.0 . . ? H1C C1 H1D 109.5 . . ? N1 C1 H1E 70.1 7 . ? N1 C1 H1E 109.4 . . ? H1C C1 H1E 109.8 . . ? H1D C1 H1E 109.8 . . ? N1 C2 N1 57(2) . 7 ? N1 C2 H2C 109.6 . . ? N1 C2 H2C 163.2 7 . ? N1 C2 H2D 110.1 . . ? N1 C2 H2D 71.0 7 . ? H2C C2 H2D 109.4 . . ? N1 C2 H2E 109.0 . . ? N1 C2 H2E 85.9 7 . ? H2C C2 H2E 109.0 . . ? H2D C2 H2E 109.8 . . ? C4 N2 C4 148(10) . 2_565 ? C4 N2 C3 106(5) . . ? C4 N2 C3 106(5) 2_565 . ? C4 N2 H2A 111.0 . . ? C4 N2 H2A 56.7 2_565 . ? C3 N2 H2A 110.1 . . ? C4 N2 H2B 111.0 . . ? C4 N2 H2B 56.7 2_565 . ? C3 N2 H2B 110.1 . . ? H2A N2 H2B 108.4 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3D 109.5 . . ? H3A C3 H3D 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? H3D C3 H3B 109.5 . . ? N2 C4 H4A 108.5 . . ? N2 C4 H4B 109.9 . . ? H4A C4 H4B 109.7 . . ? N2 C4 H4C 110.1 . . ? H4A C4 H4C 108.6 . . ? H4B C4 H4C 110.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se2 Sn1 Se1 Ag1 43.62(5) . . . . ? Se4 Sn1 Se1 Ag1 -82.10(4) . . . . ? Se3 Sn1 Se1 Ag1 172.15(4) . . . . ? Se2 Sn1 Se1 Ag2 -52.89(5) . . . . ? Se4 Sn1 Se1 Ag2 -178.61(4) . . . . ? Se3 Sn1 Se1 Ag2 75.63(4) . . . . ? Se2 Ag1 Se1 Sn1 -148.68(5) 2 . . . ? Se2 Ag1 Se1 Sn1 56.45(5) 3_556 . . . ? Ag1 Ag1 Se1 Sn1 -61.66(4) 2 . . . ? Ag1 Ag1 Se1 Sn1 -76.03(11) 3_556 . . . ? Ag1 Ag1 Se1 Sn1 -0.90(5) 4_556 . . . ? Se2 Ag1 Se1 Ag2 -46.42(5) 2 . . . ? Se2 Ag1 Se1 Ag2 158.71(4) 3_556 . . . ? Ag1 Ag1 Se1 Ag2 40.60(4) 2 . . . ? Ag1 Ag1 Se1 Ag2 26.23(12) 3_556 . . . ? Ag1 Ag1 Se1 Ag2 101.36(4) 4_556 . . . ? Se1 Ag2 Se1 Sn1 65.65(3) 2 . . . ? Se1 Ag2 Se1 Sn1 -51.475(18) 4_557 . . . ? Se1 Ag2 Se1 Sn1 -177.23(4) 3_557 . . . ? Se1 Ag2 Se1 Ag1 -19.01(2) 2 . . . ? Se1 Ag2 Se1 Ag1 -136.13(3) 4_557 . . . ? Se1 Ag2 Se1 Ag1 98.11(2) 3_557 . . . ? Se1 Sn1 Se2 Ag1 0.94(6) . . . 2 ? Se4 Sn1 Se2 Ag1 126.71(4) . . . 2 ? Se3 Sn1 Se2 Ag1 -130.83(4) . . . 2 ? Se1 Sn1 Se2 Ag1 -76.54(5) . . . 4_556 ? Se4 Sn1 Se2 Ag1 49.23(4) . . . 4_556 ? Se3 Sn1 Se2 Ag1 151.69(4) . . . 4_556 ? Se1 Sn1 Se3 Sn1 116.50(4) . . . 7 ? Se2 Sn1 Se3 Sn1 -108.83(4) . . . 7 ? Se4 Sn1 Se3 Sn1 2.80(5) . . . 7 ? Se1 Sn1 Se4 Sn1 -120.89(4) . . . 7 ? Se2 Sn1 Se4 Sn1 107.31(4) . . . 7 ? Se3 Sn1 Se4 Sn1 -2.82(6) . . . 7 ? C2 N1 C1 N1 10(4) . . . 7 ? C1 N1 C2 N1 -10(4) . . . 7 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Se1 0.90 2.91 3.66(3) 142.2 1_554 N1 H1B Se2 0.90 2.56 3.43(3) 164.4 3_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.037 _refine_diff_density_min -1.006 _refine_diff_density_rms 0.179 #===End data_Compound-1Cs _database_code_depnum_ccdc_archive 'CCDC 772739' #TrackingRef '- compound-20101220.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C0.10 H0.4 N 0.05, Ag1.25 Se3 Sn, Cs0.7, H0.5 O0.25' _chemical_formula_sum 'C0.10 H0.90 Ag1.25 Cs0.70 N0.05 O0.25 Se3 Sn' _chemical_formula_weight 590.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 m' _symmetry_space_group_name_Hall 'P -4 2ab' 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' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 13.9886(8) _cell_length_b 13.9886(8) _cell_length_c 8.8534(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1732.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1630 _cell_measurement_theta_min 2.0588 _cell_measurement_theta_max 27.4719 _exptl_crystal_description lathe _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2025 _exptl_absorpt_coefficient_mu 21.097 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3891 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13505 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2105 _reflns_number_gt 1886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0860P)^2^+8.6000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _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 0.02(3) _refine_ls_number_reflns 2105 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Sn1 Sn 0.33240(6) 0.34227(6) 0.24560(11) 0.0381(2) Uani 1 1 d . . . Ag1 Ag 0.55673(9) 0.40129(9) 0.36998(18) 0.0587(4) Uani 1 1 d . . . Ag2 Ag 0.5000 0.5000 0.0000 0.0687(8) Uani 1 4 d S . . Se1 Se 0.49046(10) 0.32325(11) 0.12223(18) 0.0458(4) Uani 1 1 d . . . Se2 Se 0.29440(10) 0.49091(10) 0.39148(18) 0.0448(3) Uani 1 1 d . . . Se3 Se 0.19123(14) 0.30877(14) 0.0655(3) 0.0586(6) Uani 1 2 d S . . Se4 Se 0.30140(13) 0.19860(13) 0.4212(3) 0.0569(6) Uani 1 2 d S . . Cs1A Cs 0.1365(18) 0.6365(18) 0.1566(16) 0.087(5) Uani 0.36 2 d SP . . Cs1B Cs 0.133(2) 0.633(2) 0.1179(18) 0.111(9) Uani 0.34 2 d SP . . Cs1C Cs 0.1774(12) 0.6774(12) 0.1796(19) 0.098(7) Uani 0.20 2 d SP . . Cs2 Cs 0.1137(3) 0.3863(3) 0.6610(4) 0.0833(12) Uani 0.50 2 d SP . . O1 O 0.0000 0.5000 0.901(6) 0.11(3) Uani 0.50 4 d SP . . O2 O 0.0000 0.5000 0.437(12) 0.14(3) Uani 0.50 4 d SP . . 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 Sn1 0.0372(4) 0.0364(4) 0.0408(5) 0.0002(4) -0.0009(4) -0.0083(3) Ag1 0.0542(7) 0.0512(7) 0.0707(8) -0.0030(6) -0.0080(6) -0.0063(5) Ag2 0.0581(9) 0.0581(9) 0.090(2) 0.000 0.000 0.000 Se1 0.0456(7) 0.0490(7) 0.0427(8) -0.0011(6) 0.0063(7) 0.0025(6) Se2 0.0428(7) 0.0426(7) 0.0490(8) -0.0029(6) 0.0032(6) -0.0002(6) Se3 0.0594(8) 0.0594(8) 0.0570(13) 0.0227(9) -0.0227(9) -0.0228(11) Se4 0.0570(8) 0.0570(8) 0.0567(13) 0.0221(8) -0.0221(8) -0.0228(10) Cs1A 0.117(7) 0.117(7) 0.025(7) -0.002(7) -0.002(7) 0.045(7) Cs1B 0.144(13) 0.144(13) 0.046(10) 0.042(10) 0.042(10) 0.078(13) Cs1C 0.131(11) 0.131(11) 0.032(6) 0.004(7) 0.004(7) 0.075(12) Cs2 0.0923(18) 0.0923(18) 0.065(2) -0.0078(16) 0.0078(16) -0.042(2) O1 0.14(4) 0.14(4) 0.04(3) 0.000 0.000 0.03(5) O2 0.14(5) 0.14(5) 0.16(8) 0.000 0.000 -0.05(6) _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 Sn1 Se1 2.4804(16) . ? Sn1 Se2 2.5048(16) . ? Sn1 Se4 2.5777(18) . ? Sn1 Se3 2.5809(19) . ? Sn1 Cs1B 4.37(3) 4_655 ? Sn1 Cs1C 4.417(17) 4_655 ? Ag1 Se2 2.5782(18) 2_665 ? Ag1 Se1 2.620(2) . ? Ag1 Se2 2.672(2) 4_656 ? Ag1 Ag1 3.185(2) 2_665 ? Ag1 Ag1 3.221(3) 4_656 ? Ag1 Ag1 3.221(3) 3_566 ? Ag1 Cs2 4.110(3) 4_656 ? Ag1 Cs1C 4.229(11) 2_665 ? Ag2 Se1 2.7022(15) 3_565 ? Ag2 Se1 2.7022(15) 2_665 ? Ag2 Se1 2.7022(15) . ? Ag2 Se1 2.7022(15) 4_655 ? Se1 Cs1B 3.818(12) 4_655 ? Se1 Cs2 3.905(3) 4_656 ? Se1 Cs1A 4.009(11) 4_655 ? Se1 Cs1C 4.101(11) 4_655 ? Se2 Ag1 2.5782(18) 2_665 ? Se2 Ag1 2.672(2) 3_566 ? Se2 Cs1C 3.606(10) . ? Se2 Cs1A 3.654(8) . ? Se2 Cs2 3.772(3) . ? Se2 Cs1B 3.862(10) . ? Se3 Sn1 2.5809(19) 7 ? Se3 Cs1C 3.39(2) 4_655 ? Se3 Cs1B 3.83(4) 4_655 ? Se3 Cs2 3.896(5) 1_554 ? Se3 Cs1A 3.94(3) 4_655 ? Se4 Sn1 2.5777(18) 7 ? Se4 Cs1C 3.559(16) 4_656 ? Se4 Cs1A 3.934(16) 4_656 ? Se4 Cs2 4.277(5) . ? Se4 Cs1B 4.28(2) 4_656 ? Cs1A O1 3.52(5) 1_554 ? Cs1A Se2 3.654(8) 8_455 ? Cs1A O2 3.67(8) . ? Cs1A Se4 3.934(16) 3_566 ? Cs1A Se3 3.94(3) 3_565 ? Cs1A Se1 4.009(11) 3_565 ? Cs1A Se1 4.009(11) 5 ? Cs1B O1 3.26(5) 1_554 ? Cs1B Se1 3.818(12) 3_565 ? Cs1B Se1 3.818(12) 5 ? Cs1B Se3 3.83(4) 3_565 ? Cs1B Se2 3.862(10) 8_455 ? Cs1B Se4 4.28(2) 3_566 ? Cs1B Sn1 4.37(3) 3_565 ? Cs1B Sn1 4.37(3) 5 ? Cs1C Se3 3.39(2) 3_565 ? Cs1C Se4 3.559(16) 3_566 ? Cs1C Se2 3.606(10) 8_455 ? Cs1C Se1 4.101(11) 3_565 ? Cs1C Se1 4.101(11) 5 ? Cs1C Ag1 4.229(11) 2_665 ? Cs1C Ag1 4.229(11) 7_565 ? Cs1C Cs2 4.37(2) 3_566 ? Cs1C Sn1 4.417(17) 3_565 ? Cs2 O2 3.00(7) . ? Cs2 O1 3.09(4) . ? Cs2 Se2 3.772(3) 7 ? Cs2 Se3 3.896(5) 1_556 ? Cs2 Se1 3.905(3) 3_566 ? Cs2 Se1 3.905(3) 6_456 ? Cs2 Ag1 4.110(3) 6_456 ? Cs2 Ag1 4.110(3) 3_566 ? Cs2 Cs1C 4.37(2) 4_656 ? Cs2 Cs2 4.499(10) 2_565 ? O1 Cs2 3.09(4) 2_565 ? O1 Cs1B 3.26(5) 1_556 ? O1 Cs1B 3.26(5) 2_566 ? O1 Cs1A 3.52(5) 1_556 ? O1 Cs1A 3.52(5) 2_566 ? O2 Cs2 3.00(7) 2_565 ? O2 Cs1A 3.67(8) 2_565 ? 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 Se1 Sn1 Se2 120.35(6) . . ? Se1 Sn1 Se4 109.39(7) . . ? Se2 Sn1 Se4 107.49(8) . . ? Se1 Sn1 Se3 112.99(8) . . ? Se2 Sn1 Se3 107.87(8) . . ? Se4 Sn1 Se3 95.87(5) . . ? Se1 Sn1 Cs1B 60.4(3) . 4_655 ? Se2 Sn1 Cs1B 163.2(4) . 4_655 ? Se4 Sn1 Cs1B 86.6(3) . 4_655 ? Se3 Sn1 Cs1B 60.5(5) . 4_655 ? Se1 Sn1 Cs1C 66.2(2) . 4_655 ? Se2 Sn1 Cs1C 150.0(3) . 4_655 ? Se4 Sn1 Cs1C 95.84(17) . 4_655 ? Se3 Sn1 Cs1C 49.8(3) . 4_655 ? Cs1B Sn1 Cs1C 13.4(6) 4_655 4_655 ? Se2 Ag1 Se1 126.26(8) 2_665 . ? Se2 Ag1 Se2 118.06(6) 2_665 4_656 ? Se1 Ag1 Se2 109.90(6) . 4_656 ? Se2 Ag1 Ag1 83.99(6) 2_665 2_665 ? Se1 Ag1 Ag1 100.66(5) . 2_665 ? Se2 Ag1 Ag1 111.16(5) 4_656 2_665 ? Se2 Ag1 Ag1 53.49(5) 2_665 4_656 ? Se1 Ag1 Ag1 160.80(7) . 4_656 ? Se2 Ag1 Ag1 81.86(7) 4_656 4_656 ? Ag1 Ag1 Ag1 60.36(3) 2_665 4_656 ? Se2 Ag1 Ag1 112.70(6) 2_665 3_566 ? Se1 Ag1 Ag1 115.82(6) . 3_566 ? Se2 Ag1 Ag1 50.86(6) 4_656 3_566 ? Ag1 Ag1 Ag1 60.36(3) 2_665 3_566 ? Ag1 Ag1 Ag1 59.27(5) 4_656 3_566 ? Se2 Ag1 Cs2 114.88(8) 2_665 4_656 ? Se1 Ag1 Cs2 66.72(7) . 4_656 ? Se2 Ag1 Cs2 63.48(7) 4_656 4_656 ? Ag1 Ag1 Cs2 160.95(8) 2_665 4_656 ? Ag1 Ag1 Cs2 132.31(8) 4_656 4_656 ? Ag1 Ag1 Cs2 110.93(8) 3_566 4_656 ? Se2 Ag1 Cs1C 58.1(3) 2_665 2_665 ? Se1 Ag1 Cs1C 82.5(3) . 2_665 ? Se2 Ag1 Cs1C 112.9(2) 4_656 2_665 ? Ag1 Ag1 Cs1C 131.6(2) 2_665 2_665 ? Ag1 Ag1 Cs1C 107.5(3) 4_656 2_665 ? Ag1 Ag1 Cs1C 157.8(2) 3_566 2_665 ? Cs2 Ag1 Cs1C 63.1(3) 4_656 2_665 ? Se1 Ag2 Se1 99.23(2) 3_565 2_665 ? Se1 Ag2 Se1 99.23(2) 3_565 . ? Se1 Ag2 Se1 132.79(7) 2_665 . ? Se1 Ag2 Se1 132.79(7) 3_565 4_655 ? Se1 Ag2 Se1 99.23(3) 2_665 4_655 ? Se1 Ag2 Se1 99.23(2) . 4_655 ? Sn1 Se1 Ag1 84.38(6) . . ? Sn1 Se1 Ag2 97.02(5) . . ? Ag1 Se1 Ag2 86.36(5) . . ? Sn1 Se1 Cs1B 85.2(5) . 4_655 ? Ag1 Se1 Cs1B 156.4(3) . 4_655 ? Ag2 Se1 Cs1B 115.9(4) . 4_655 ? Sn1 Se1 Cs2 104.93(8) . 4_656 ? Ag1 Se1 Cs2 75.23(8) . 4_656 ? Ag2 Se1 Cs2 149.53(9) . 4_656 ? Cs1B Se1 Cs2 87.2(6) 4_655 4_656 ? Sn1 Se1 Cs1A 86.9(4) . 4_655 ? Ag1 Se1 Cs1A 160.7(2) . 4_655 ? Ag2 Se1 Cs1A 111.8(3) . 4_655 ? Cs1B Se1 Cs1A 4.3(4) 4_655 4_655 ? Cs2 Se1 Cs1A 90.5(4) 4_656 4_655 ? Sn1 Se1 Cs1C 80.2(3) . 4_655 ? Ag1 Se1 Cs1C 162.9(2) . 4_655 ? Ag2 Se1 Cs1C 102.9(2) . 4_655 ? Cs1B Se1 Cs1C 14.4(7) 4_655 4_655 ? Cs2 Se1 Cs1C 101.5(3) 4_656 4_655 ? Cs1A Se1 Cs1C 11.8(4) 4_655 4_655 ? Sn1 Se2 Ag1 106.02(6) . 2_665 ? Sn1 Se2 Ag1 94.69(6) . 3_566 ? Ag1 Se2 Ag1 75.65(7) 2_665 3_566 ? Sn1 Se2 Cs1C 115.4(2) . . ? Ag1 Se2 Cs1C 84.6(4) 2_665 . ? Ag1 Se2 Cs1C 147.7(3) 3_566 . ? Sn1 Se2 Cs1A 107.3(3) . . ? Ag1 Se2 Cs1A 96.9(6) 2_665 . ? Ag1 Se2 Cs1A 158.0(3) 3_566 . ? Cs1C Se2 Cs1A 13.2(5) . . ? Sn1 Se2 Cs2 98.42(8) . . ? Ag1 Se2 Cs2 144.58(8) 2_665 . ? Ag1 Se2 Cs2 77.18(8) 3_566 . ? Cs1C Se2 Cs2 107.8(3) . . ? Cs1A Se2 Cs2 99.8(5) . . ? Sn1 Se2 Cs1B 103.2(3) . . ? Ag1 Se2 Cs1B 97.1(6) 2_665 . ? Ag1 Se2 Cs1B 162.0(4) 3_566 . ? Cs1C Se2 Cs1B 15.4(8) . . ? Cs1A Se2 Cs1B 4.3(4) . . ? Cs2 Se2 Cs1B 101.9(5) . . ? Sn1 Se3 Sn1 84.05(8) . 7 ? Sn1 Se3 Cs1C 94.5(2) . 4_655 ? Sn1 Se3 Cs1C 94.5(2) 7 4_655 ? Sn1 Se3 Cs1B 83.6(3) . 4_655 ? Sn1 Se3 Cs1B 83.6(3) 7 4_655 ? Cs1C Se3 Cs1B 14.8(5) 4_655 4_655 ? Sn1 Se3 Cs2 136.91(5) . 1_554 ? Sn1 Se3 Cs2 136.91(5) 7 1_554 ? Cs1C Se3 Cs2 73.3(3) 4_655 1_554 ? Cs1B Se3 Cs2 88.1(3) 4_655 1_554 ? Sn1 Se3 Cs1A 87.2(2) . 4_655 ? Sn1 Se3 Cs1A 87.2(2) 7 4_655 ? Cs1C Se3 Cs1A 9.9(3) 4_655 4_655 ? Cs1B Se3 Cs1A 4.9(6) 4_655 4_655 ? Cs2 Se3 Cs1A 83.2(3) 1_554 4_655 ? Sn1 Se4 Sn1 84.18(7) 7 . ? Sn1 Se4 Cs1C 130.54(19) 7 4_656 ? Sn1 Se4 Cs1C 130.54(19) . 4_656 ? Sn1 Se4 Cs1A 135.08(17) 7 4_656 ? Sn1 Se4 Cs1A 135.08(17) . 4_656 ? Cs1C Se4 Cs1A 11.4(5) 4_656 4_656 ? Sn1 Se4 Cs2 85.65(8) 7 . ? Sn1 Se4 Cs2 85.65(8) . . ? Cs1C Se4 Cs2 67.0(4) 4_656 . ? Cs1A Se4 Cs2 78.4(5) 4_656 . ? Sn1 Se4 Cs1B 134.87(19) 7 4_656 ? Sn1 Se4 Cs1B 134.87(19) . 4_656 ? Cs1C Se4 Cs1B 10.8(8) 4_656 4_656 ? Cs1A Se4 Cs1B 0.6(11) 4_656 4_656 ? Cs2 Se4 Cs1B 77.8(6) . 4_656 ? Cs1C Cs1A O1 154(2) . 1_554 ? Cs1C Cs1A Se2 80.1(9) . . ? O1 Cs1A Se2 113.0(7) 1_554 . ? Cs1C Cs1A Se2 80.1(9) . 8_455 ? O1 Cs1A Se2 113.0(7) 1_554 8_455 ? Se2 Cs1A Se2 110.5(4) . 8_455 ? Cs1C Cs1A O2 123(2) . . ? O1 Cs1A O2 82.6(16) 1_554 . ? Se2 Cs1A O2 68.9(7) . . ? Se2 Cs1A O2 68.9(7) 8_455 . ? Cs1C Cs1A Se4 57.7(16) . 3_566 ? O1 Cs1A Se4 148.2(12) 1_554 3_566 ? Se2 Cs1A Se4 56.56(19) . 3_566 ? Se2 Cs1A Se4 56.56(19) 8_455 3_566 ? O2 Cs1A Se4 65.6(13) . 3_566 ? Cs1C Cs1A Se3 44.1(18) . 3_565 ? O1 Cs1A Se3 110.0(8) 1_554 3_565 ? Se2 Cs1A Se3 104.8(6) . 3_565 ? Se2 Cs1A Se3 104.8(6) 8_455 3_565 ? O2 Cs1A Se3 167.4(14) . 3_565 ? Se4 Cs1A Se3 101.8(7) 3_566 3_565 ? Cs1C Cs1A Se1 90.4(14) . 3_565 ? O1 Cs1A Se1 73.6(5) 1_554 3_565 ? Se2 Cs1A Se1 73.12(9) . 3_565 ? Se2 Cs1A Se1 168.9(10) 8_455 3_565 ? O2 Cs1A Se1 121.7(8) . 3_565 ? Se4 Cs1A Se1 122.6(4) 3_566 3_565 ? Se3 Cs1A Se1 64.2(4) 3_565 3_565 ? Cs1C Cs1A Se1 90.4(14) . 5 ? O1 Cs1A Se1 73.6(5) 1_554 5 ? Se2 Cs1A Se1 168.9(10) . 5 ? Se2 Cs1A Se1 73.12(9) 8_455 5 ? O2 Cs1A Se1 121.7(8) . 5 ? Se4 Cs1A Se1 122.6(4) 3_566 5 ? Se3 Cs1A Se1 64.2(4) 3_565 5 ? Se1 Cs1A Se1 101.4(4) 3_565 5 ? Cs1C Cs1A Cs2 4.0(17) . 3_566 ? O1 Cs1A Cs2 158.1(10) 1_554 3_566 ? Se2 Cs1A Cs2 78.0(5) . 3_566 ? Se2 Cs1A Cs2 78.0(5) 8_455 3_566 ? O2 Cs1A Cs2 119.3(13) . 3_566 ? Se4 Cs1A Cs2 53.7(4) 3_566 3_566 ? Se3 Cs1A Cs2 48.1(4) 3_565 3_566 ? Se1 Cs1A Cs2 92.9(6) 3_565 3_566 ? Se1 Cs1A Cs2 92.9(6) 5 3_566 ? Cs1C Cs1A Cs1B 169.6(19) . 2_565 ? O1 Cs1A Cs1B 36.3(8) 1_554 2_565 ? Se2 Cs1A Cs1B 94.0(6) . 2_565 ? Se2 Cs1A Cs1B 94.0(6) 8_455 2_565 ? O2 Cs1A Cs1B 46.3(13) . 2_565 ? Se4 Cs1A Cs1B 111.9(6) 3_566 2_565 ? Se3 Cs1A Cs1B 146.3(5) 3_565 2_565 ? Se1 Cs1A Cs1B 96.2(5) 3_565 2_565 ? Se1 Cs1A Cs1B 96.2(5) 5 2_565 ? Cs2 Cs1A Cs1B 165.6(5) 3_566 2_565 ? Cs1C Cs1A Cs1A 165.9(18) . 2_565 ? O1 Cs1A Cs1A 40.0(8) 1_554 2_565 ? Se2 Cs1A Cs1A 91.9(5) . 2_565 ? Se2 Cs1A Cs1A 91.9(5) 8_455 2_565 ? O2 Cs1A Cs1A 42.6(13) . 2_565 ? Se4 Cs1A Cs1A 108.2(5) 3_566 2_565 ? Se3 Cs1A Cs1A 150.0(3) 3_565 2_565 ? Se1 Cs1A Cs1A 98.5(5) 3_565 2_565 ? Se1 Cs1A Cs1A 98.5(5) 5 2_565 ? Cs2 Cs1A Cs1A 161.9(2) 3_566 2_565 ? Cs1B Cs1A Cs1A 3.7(3) 2_565 2_565 ? Cs1C Cs1B O1 176(3) . 1_554 ? Cs1C Cs1B Se1 98.6(16) . 3_565 ? O1 Cs1B Se1 79.1(6) 1_554 3_565 ? Cs1C Cs1B Se1 98.6(16) . 5 ? O1 Cs1B Se1 79.1(6) 1_554 5 ? Se1 Cs1B Se1 108.7(5) 3_565 5 ? Cs1C Cs1B Se3 57(2) . 3_565 ? O1 Cs1B Se3 118.9(9) 1_554 3_565 ? Se1 Cs1B Se3 67.0(5) 3_565 3_565 ? Se1 Cs1B Se3 67.0(5) 5 3_565 ? Cs1C Cs1B Se2 68.1(9) . 8_455 ? O1 Cs1B Se2 114.1(9) 1_554 8_455 ? Se1 Cs1B Se2 166.6(12) 3_565 8_455 ? Se1 Cs1B Se2 73.10(11) 5 8_455 ? Se3 Cs1B Se2 102.8(8) 3_565 8_455 ? Cs1C Cs1B Se2 68.1(9) . . ? O1 Cs1B Se2 114.1(9) 1_554 . ? Se1 Cs1B Se2 73.10(11) 3_565 . ? Se1 Cs1B Se2 166.6(12) 5 . ? Se3 Cs1B Se2 102.8(8) 3_565 . ? Se2 Cs1B Se2 102.0(4) 8_455 . ? Cs1C Cs1B Se4 40.4(18) . 3_566 ? O1 Cs1B Se4 143.7(13) 1_554 3_566 ? Se1 Cs1B Se4 118.6(5) 3_565 3_566 ? Se1 Cs1B Se4 118.6(5) 5 3_566 ? Se3 Cs1B Se4 97.5(8) 3_565 3_566 ? Se2 Cs1B Se4 52.2(2) 8_455 3_566 ? Se2 Cs1B Se4 52.2(2) . 3_566 ? Cs1C Cs1B Sn1 86(2) . 3_565 ? O1 Cs1B Sn1 90.6(8) 1_554 3_565 ? Se1 Cs1B Sn1 34.4(2) 3_565 3_565 ? Se1 Cs1B Sn1 79.5(5) 5 3_565 ? Se3 Cs1B Sn1 35.9(3) 3_565 3_565 ? Se2 Cs1B Sn1 137.9(10) 8_455 3_565 ? Se2 Cs1B Sn1 97.4(4) . 3_565 ? Se4 Cs1B Sn1 122.4(9) 3_566 3_565 ? Cs1C Cs1B Sn1 86(2) . 5 ? O1 Cs1B Sn1 90.6(8) 1_554 5 ? Se1 Cs1B Sn1 79.5(5) 3_565 5 ? Se1 Cs1B Sn1 34.4(2) 5 5 ? Se3 Cs1B Sn1 35.9(3) 3_565 5 ? Se2 Cs1B Sn1 97.4(4) 8_455 5 ? Se2 Cs1B Sn1 137.9(10) . 5 ? Se4 Cs1B Sn1 122.4(9) 3_566 5 ? Sn1 Cs1B Sn1 46.5(3) 3_565 5 ? Cs1C Cs1B Cs1B 148(2) . 2_565 ? O1 Cs1B Cs1B 36.1(9) 1_554 2_565 ? Se1 Cs1B Cs1B 99.9(6) 3_565 2_565 ? Se1 Cs1B Cs1B 99.9(6) 5 2_565 ? Se3 Cs1B Cs1B 154.9(3) 3_565 2_565 ? Se2 Cs1B Cs1B 92.7(7) 8_455 2_565 ? Se2 Cs1B Cs1B 92.7(7) . 2_565 ? Se4 Cs1B Cs1B 107.6(6) 3_566 2_565 ? Sn1 Cs1B Cs1B 123.4(5) 3_565 2_565 ? Sn1 Cs1B Cs1B 123.4(5) 5 2_565 ? Cs1C Cs1B Cs2 145.4(17) . 1_554 ? O1 Cs1B Cs2 32.1(5) 1_554 1_554 ? Se1 Cs1B Cs2 47.1(3) 3_565 1_554 ? Se1 Cs1B Cs2 90.3(4) 5 1_554 ? Se3 Cs1B Cs2 97.3(3) 3_565 1_554 ? Se2 Cs1B Cs2 145.9(8) 8_455 1_554 ? Se2 Cs1B Cs2 99.9(3) . 1_554 ? Se4 Cs1B Cs2 150.8(4) 3_566 1_554 ? Sn1 Cs1B Cs2 63.06(19) 3_565 1_554 ? Sn1 Cs1B Cs2 83.1(3) 5 1_554 ? Cs1B Cs1B Cs2 60.3(4) 2_565 1_554 ? Cs1A Cs1C Cs1B 18(3) . . ? Cs1A Cs1C Se3 126.0(19) . 3_565 ? Cs1B Cs1C Se3 108(2) . 3_565 ? Cs1A Cs1C Se4 111(2) . 3_566 ? Cs1B Cs1C Se4 129(2) . 3_566 ? Se3 Cs1C Se4 123.1(6) 3_565 3_566 ? Cs1A Cs1C Se2 86.7(11) . 8_455 ? Cs1B Cs1C Se2 96.6(14) . 8_455 ? Se3 Cs1C Se2 118.7(4) 3_565 8_455 ? Se4 Cs1C Se2 60.4(2) 3_566 8_455 ? Cs1A Cs1C Se2 86.7(11) . . ? Cs1B Cs1C Se2 96.6(13) . . ? Se3 Cs1C Se2 118.7(4) 3_565 . ? Se4 Cs1C Se2 60.4(2) 3_566 . ? Se2 Cs1C Se2 112.7(5) 8_455 . ? Cs1A Cs1C Se1 77.9(11) . 3_565 ? Cs1B Cs1C Se1 67.0(11) . 3_565 ? Se3 Cs1C Se1 67.9(3) 3_565 3_565 ? Se4 Cs1C Se1 130.79(17) 3_566 3_565 ? Se2 Cs1C Se1 163.5(6) 8_455 3_565 ? Se2 Cs1C Se1 72.48(8) . 3_565 ? Cs1A Cs1C Se1 77.9(11) . 5 ? Cs1B Cs1C Se1 67.0(11) . 5 ? Se3 Cs1C Se1 67.9(3) 3_565 5 ? Se4 Cs1C Se1 130.79(17) 3_566 5 ? Se2 Cs1C Se1 72.48(8) 8_455 5 ? Se2 Cs1C Se1 163.5(6) . 5 ? Se1 Cs1C Se1 98.3(3) 3_565 5 ? Cs1A Cs1C Ag1 121.4(7) . 2_665 ? Cs1B Cs1C Ag1 125.6(4) . 2_665 ? Se3 Cs1C Ag1 85.4(4) 3_565 2_665 ? Se4 Cs1C Ag1 63.4(2) 3_566 2_665 ? Se2 Cs1C Ag1 123.2(4) 8_455 2_665 ? Se2 Cs1C Ag1 37.37(10) . 2_665 ? Se1 Cs1C Ag1 70.92(11) 3_565 2_665 ? Se1 Cs1C Ag1 153.2(6) 5 2_665 ? Cs1A Cs1C Ag1 121.4(7) . 7_565 ? Cs1B Cs1C Ag1 125.6(4) . 7_565 ? Se3 Cs1C Ag1 85.4(4) 3_565 7_565 ? Se4 Cs1C Ag1 63.4(2) 3_566 7_565 ? Se2 Cs1C Ag1 37.37(10) 8_455 7_565 ? Se2 Cs1C Ag1 123.2(4) . 7_565 ? Se1 Cs1C Ag1 153.2(6) 3_565 7_565 ? Se1 Cs1C Ag1 70.92(11) 5 7_565 ? Ag1 Cs1C Ag1 107.4(4) 2_665 7_565 ? Cs1A Cs1C Cs2 175(2) . 3_566 ? Cs1B Cs1C Cs2 167(2) . 3_566 ? Se3 Cs1C Cs2 58.7(4) 3_565 3_566 ? Se4 Cs1C Cs2 64.4(3) 3_566 3_566 ? Se2 Cs1C Cs2 90.7(3) 8_455 3_566 ? Se2 Cs1C Cs2 90.7(3) . 3_566 ? Se1 Cs1C Cs2 105.1(4) 3_565 3_566 ? Se1 Cs1C Cs2 105.1(4) 5 3_566 ? Ag1 Cs1C Cs2 57.1(2) 2_665 3_566 ? Ag1 Cs1C Cs2 57.1(2) 7_565 3_566 ? Cs1A Cs1C Sn1 97.4(16) . 3_565 ? Cs1B Cs1C Sn1 80.9(19) . 3_565 ? Se3 Cs1C Sn1 35.63(17) 3_565 3_565 ? Se4 Cs1C Sn1 143.6(5) 3_566 3_565 ? Se2 Cs1C Sn1 146.6(4) 8_455 3_565 ? Se2 Cs1C Sn1 100.60(16) . 3_565 ? Se1 Cs1C Sn1 33.60(12) 3_565 3_565 ? Se1 Cs1C Sn1 76.1(3) 5 3_565 ? Ag1 Cs1C Sn1 82.7(2) 2_665 3_565 ? Ag1 Cs1C Sn1 120.2(5) 7_565 3_565 ? Cs2 Cs1C Sn1 86.9(4) 3_566 3_565 ? O2 Cs2 O1 84.8(18) . . ? O2 Cs2 Se2 74.4(10) . 7 ? O1 Cs2 Se2 125.4(3) . 7 ? O2 Cs2 Se2 74.4(10) . . ? O1 Cs2 Se2 125.4(3) . . ? Se2 Cs2 Se2 96.88(10) 7 . ? O2 Cs2 Se3 154.6(16) . 1_556 ? O1 Cs2 Se3 69.8(8) . 1_556 ? Se2 Cs2 Se3 120.20(9) 7 1_556 ? Se2 Cs2 Se3 120.20(9) . 1_556 ? O2 Cs2 Se1 119.3(4) . 3_566 ? O1 Cs2 Se1 79.7(4) . 3_566 ? Se2 Cs2 Se1 153.91(14) 7 3_566 ? Se2 Cs2 Se1 68.69(4) . 3_566 ? Se3 Cs2 Se1 57.47(6) 1_556 3_566 ? O2 Cs2 Se1 119.3(4) . 6_456 ? O1 Cs2 Se1 79.7(4) . 6_456 ? Se2 Cs2 Se1 68.69(4) 7 6_456 ? Se2 Cs2 Se1 153.91(14) . 6_456 ? Se3 Cs2 Se1 57.47(6) 1_556 6_456 ? Se1 Cs2 Se1 114.92(11) 3_566 6_456 ? O2 Cs2 Ag1 111.8(7) . 6_456 ? O1 Cs2 Ag1 116.7(3) . 6_456 ? Se2 Cs2 Ag1 39.34(4) 7 6_456 ? Se2 Cs2 Ag1 117.87(11) . 6_456 ? Se3 Cs2 Ag1 80.96(8) 1_556 6_456 ? Se1 Cs2 Ag1 127.63(13) 3_566 6_456 ? Se1 Cs2 Ag1 38.05(4) 6_456 6_456 ? O2 Cs2 Ag1 111.8(7) . 3_566 ? O1 Cs2 Ag1 116.7(3) . 3_566 ? Se2 Cs2 Ag1 117.87(11) 7 3_566 ? Se2 Cs2 Ag1 39.34(4) . 3_566 ? Se3 Cs2 Ag1 80.96(8) 1_556 3_566 ? Se1 Cs2 Ag1 38.05(4) 3_566 3_566 ? Se1 Cs2 Ag1 127.63(13) 6_456 3_566 ? Ag1 Cs2 Ag1 112.03(12) 6_456 3_566 ? O2 Cs2 Se4 108.8(16) . . ? O1 Cs2 Se4 166.4(8) . . ? Se2 Cs2 Se4 60.84(6) 7 . ? Se2 Cs2 Se4 60.84(6) . . ? Se3 Cs2 Se4 96.58(12) 1_556 . ? Se1 Cs2 Se4 93.11(9) 3_566 . ? Se1 Cs2 Se4 93.11(9) 6_456 . ? Ag1 Cs2 Se4 59.01(6) 6_456 . ? Ag1 Cs2 Se4 59.01(6) 3_566 . ? O2 Cs2 Cs1C 157.4(16) . 4_656 ? O1 Cs2 Cs1C 117.8(8) . 4_656 ? Se2 Cs2 Cs1C 90.89(18) 7 4_656 ? Se2 Cs2 Cs1C 90.89(19) . 4_656 ? Se3 Cs2 Cs1C 48.0(3) 1_556 4_656 ? Se1 Cs2 Cs1C 68.55(13) 3_566 4_656 ? Se1 Cs2 Cs1C 68.55(13) 6_456 4_656 ? Ag1 Cs2 Cs1C 59.76(9) 6_456 4_656 ? Ag1 Cs2 Cs1C 59.76(9) 3_566 4_656 ? Se4 Cs2 Cs1C 48.6(3) . 4_656 ? O2 Cs2 Cs2 41.4(16) . 2_565 ? O1 Cs2 Cs2 43.3(8) . 2_565 ? Se2 Cs2 Cs2 101.51(8) 7 2_565 ? Se2 Cs2 Cs2 101.51(8) . 2_565 ? Se3 Cs2 Cs2 113.18(8) 1_556 2_565 ? Se1 Cs2 Cs2 102.63(8) 3_566 2_565 ? Se1 Cs2 Cs2 102.63(8) 6_456 2_565 ? Ag1 Cs2 Cs2 123.71(6) 6_456 2_565 ? Ag1 Cs2 Cs2 123.71(6) 3_566 2_565 ? Se4 Cs2 Cs2 150.24(6) . 2_565 ? Cs1C Cs2 Cs2 161.2(2) 4_656 2_565 ? Cs2 O1 Cs2 93.3(15) . 2_565 ? Cs2 O1 Cs1B 113.8(3) . 1_556 ? Cs2 O1 Cs1B 113.8(3) 2_565 1_556 ? Cs2 O1 Cs1B 113.8(3) . 2_566 ? Cs2 O1 Cs1B 113.8(3) 2_565 2_566 ? Cs1B O1 Cs1B 107.8(19) 1_556 2_566 ? Cs2 O1 Cs1A 116.2(3) . 1_556 ? Cs2 O1 Cs1A 116.2(3) 2_565 1_556 ? Cs1B O1 Cs1A 3.9(9) 1_556 1_556 ? Cs1B O1 Cs1A 103.9(15) 2_566 1_556 ? Cs2 O1 Cs1A 116.2(3) . 2_566 ? Cs2 O1 Cs1A 116.2(3) 2_565 2_566 ? Cs1B O1 Cs1A 103.9(15) 1_556 2_566 ? Cs1B O1 Cs1A 3.9(9) 2_566 2_566 ? Cs1A O1 Cs1A 100.0(17) 1_556 2_566 ? Cs2 O2 Cs2 97(3) . 2_565 ? Cs2 O2 Cs1A 116.6(3) . 2_565 ? Cs2 O2 Cs1A 116.6(3) 2_565 2_565 ? Cs2 O2 Cs1A 116.6(3) . . ? Cs2 O2 Cs1A 116.6(3) 2_565 . ? Cs1A O2 Cs1A 95(3) 2_565 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.021 _refine_diff_density_min -1.583 _refine_diff_density_rms 0.269 #==== End data_Compound-1NH4 _database_code_depnum_ccdc_archive 'CCDC 772740' #TrackingRef '- compound-20101220.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C0.50 H2 N0.25, H2 N0.5, Ag1.25 Se3 Sn, H O0.5' _chemical_formula_sum 'C0.50 H5 Ag1.25 N0.75 O0.50 Se3 Sn' _chemical_formula_weight 519.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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 21 m' _symmetry_space_group_name_Hall 'P -4 2ab' 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' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 13.9087(6) _cell_length_b 13.9087(6) _cell_length_c 8.8618(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1714.33(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3815 _cell_measurement_theta_min 3.275 _cell_measurement_theta_max 27.4565 _exptl_crystal_description lathe _exptl_crystal_colour red _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 18.400 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7039 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13455 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2056 _reflns_number_gt 1973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2005)' _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^)+(0.0300P)^2^+10.9989P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment none _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 0.19(2) _refine_ls_number_reflns 2056 _refine_ls_number_parameters 84 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.138 _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 Sn1 Sn 0.14986(5) 0.17462(5) 0.75682(9) 0.03326(18) Uani 1 1 d . . . Ag1 Ag 0.10327(7) -0.05294(7) 0.62720(14) 0.0554(3) Uani 1 1 d . . . Ag2 Ag 0.0000 0.0000 1.0000 0.0641(6) Uani 1 4 d S . . Se1 Se 0.17602(8) 0.01578(8) 0.87702(15) 0.0422(3) Uani 1 1 d . . . Se2 Se -0.00086(8) 0.20747(8) 0.61115(14) 0.0401(3) Uani 1 1 d . . . Se3 Se 0.18329(10) 0.31671(10) 0.9357(2) 0.0490(5) Uani 1 2 d S . . Se4 Se 0.29086(10) 0.20914(10) 0.5774(2) 0.0467(5) Uani 1 2 d S . . N1 N -0.331(2) 0.831(2) 0.162(3) 0.174(16) Uani 1 2 d S . . O1 O 0.120(4) 0.380(4) 0.360(9) 0.205(14) Uani 0.50 2 d SPU . . O2 O 0.078(3) 0.578(3) 0.066(8) 0.206(14) Uani 0.50 2 d SPU . . N2 N 0.0460(7) 0.5460(7) 0.441(6) 0.208(14) Uani 0.50 2 d SPDU . . C1 C 0.0000 0.5000 0.306(6) 0.209(14) Uani 1 4 d SDU . . C2 C 0.0000 0.5000 0.577(6) 0.209(14) Uani 1 4 d SDU . . 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 Sn1 0.0292(4) 0.0309(4) 0.0397(4) 0.0011(3) -0.0003(3) -0.0070(3) Ag1 0.0482(6) 0.0468(6) 0.0711(7) -0.0075(5) -0.0003(5) -0.0064(4) Ag2 0.0534(8) 0.0534(8) 0.0854(17) 0.000 0.000 0.000 Se1 0.0429(6) 0.0405(6) 0.0433(6) 0.0091(5) -0.0006(6) 0.0041(5) Se2 0.0347(6) 0.0361(6) 0.0495(7) 0.0023(5) -0.0060(6) 0.0007(5) Se3 0.0486(6) 0.0486(6) 0.0499(10) -0.0164(6) 0.0164(6) -0.0167(8) Se4 0.0465(6) 0.0465(6) 0.0470(10) -0.0161(6) 0.0161(6) -0.0201(8) N1 0.20(2) 0.20(2) 0.11(2) -0.09(2) 0.09(2) -0.11(3) O1 0.199(18) 0.199(18) 0.22(3) 0.000(4) 0.000(4) -0.07(2) O2 0.198(18) 0.198(18) 0.22(3) -0.001(5) -0.001(5) -0.07(2) N2 0.201(18) 0.201(18) 0.22(3) -0.001(4) -0.001(4) -0.07(2) C1 0.202(18) 0.202(18) 0.22(3) 0.000 0.000 -0.07(2) C2 0.202(18) 0.202(18) 0.22(3) 0.000 0.000 -0.07(2) _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 Sn1 Se1 2.4795(13) . ? Sn1 Se2 2.5040(14) . ? Sn1 Se4 2.5701(14) . ? Sn1 Se3 2.5756(15) . ? Ag1 Se2 2.5823(15) 2 ? Ag1 Se1 2.6151(17) . ? Ag1 Se2 2.6687(17) 3_556 ? Ag1 Ag1 3.208(2) 3_556 ? Ag1 Ag1 3.208(2) 4_556 ? Ag1 Ag1 3.228(2) 2 ? Ag2 Se1 2.6888(12) 2 ? Ag2 Se1 2.6888(12) 4_557 ? Ag2 Se1 2.6888(12) . ? Ag2 Se1 2.6888(12) 3_557 ? Se2 Ag1 2.5823(15) 2 ? Se2 Ag1 2.6687(17) 4_556 ? Se3 Sn1 2.5756(15) 7 ? Se4 Sn1 2.5701(14) 7 ? N2 C1 1.501(10) . ? N2 C2 1.504(10) . ? C1 N2 1.501(10) 2_565 ? C2 N2 1.504(10) 2_565 ? 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 Se1 Sn1 Se2 120.46(5) . . ? Se1 Sn1 Se4 108.68(6) . . ? Se2 Sn1 Se4 106.61(6) . . ? Se1 Sn1 Se3 113.13(6) . . ? Se2 Sn1 Se3 109.17(6) . . ? Se4 Sn1 Se3 95.72(4) . . ? Se2 Ag1 Se1 124.35(6) 2 . ? Se2 Ag1 Se2 119.30(5) 2 3_556 ? Se1 Ag1 Se2 110.94(5) . 3_556 ? Se2 Ag1 Ag1 53.57(4) 2 3_556 ? Se1 Ag1 Ag1 159.50(6) . 3_556 ? Se2 Ag1 Ag1 82.69(6) 3_556 3_556 ? Se2 Ag1 Ag1 113.87(5) 2 4_556 ? Se1 Ag1 Ag1 115.58(5) . 4_556 ? Se2 Ag1 Ag1 51.13(5) 3_556 4_556 ? Ag1 Ag1 Ag1 60.41(4) 3_556 4_556 ? Se2 Ag1 Ag1 83.62(5) 2 2 ? Se1 Ag1 Ag1 100.23(4) . 2 ? Se2 Ag1 Ag1 110.81(4) 3_556 2 ? Ag1 Ag1 Ag1 59.80(2) 3_556 2 ? Ag1 Ag1 Ag1 59.80(2) 4_556 2 ? Se1 Ag2 Se1 99.45(2) 2 4_557 ? Se1 Ag2 Se1 132.18(6) 2 . ? Se1 Ag2 Se1 99.45(2) 4_557 . ? Se1 Ag2 Se1 99.45(2) 2 3_557 ? Se1 Ag2 Se1 132.18(6) 4_557 3_557 ? Se1 Ag2 Se1 99.45(2) . 3_557 ? Sn1 Se1 Ag1 84.56(5) . . ? Sn1 Se1 Ag2 96.50(4) . . ? Ag1 Se1 Ag2 87.76(4) . . ? Sn1 Se2 Ag1 106.35(5) . 2 ? Sn1 Se2 Ag1 94.25(5) . 4_556 ? Ag1 Se2 Ag1 75.30(6) 2 4_556 ? Sn1 Se3 Sn1 84.16(6) 7 . ? Sn1 Se4 Sn1 84.39(6) 7 . ? C1 N2 C2 106.0(9) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.961 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.200 #==== End