# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global #TrackingRef 'cif-of-1a-2c.cif' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Prof. Dingxian Jia' _publ_contact_author_address ;Soochow University College of Chemistry, Chemical Engineering and Materials Science P.O. Box 174, Renai Road 199, Suzhou 215123 P.R.China. ; _publ_contact_author_email jiadingxian@suda.edu.cn _publ_contact_author_phone 86-512-65880089 _publ_contact_author_fax 86-512-65880089 loop_ _publ_author_name 'Jingjing Liang' 'Jiangfang Chen' 'Jing Zhao' 'Yingli Pan' 'Yong Zhang' 'Dingxian Jia' data_compound_1a _database_code_depnum_ccdc_archive 'CCDC 797225' #TrackingRef 'cif-of-1a-2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H64 Ce2 N16 Se8 Sn2' _chemical_formula_sum 'C16 H64 Ce2 N16 Se8 Sn2' _chemical_formula_weight 1630.14 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0942(10) _cell_length_b 16.6159(13) _cell_length_c 13.3973(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.878(3) _cell_angle_gamma 90.00 _cell_volume 2198.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10720 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 9.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1045 _exptl_absorpt_correction_T_max 0.2712 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10994 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3990 _reflns_number_gt 3471 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0315P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3990 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.55475(3) 0.440075(17) 0.40822(2) 0.01676(9) Uani 1 1 d . . . Se1 Se 0.61738(5) 0.00149(3) 0.53691(4) 0.02935(13) Uani 1 1 d . . . Se2 Se 0.43049(5) 0.40786(3) 0.23521(4) 0.02639(12) Uani 1 1 d . . . Se3 Se 0.78623(4) 0.38496(3) 0.45082(4) 0.02302(12) Uani 1 1 d . . . Se4 Se 0.55744(5) 0.59372(3) 0.43983(4) 0.02471(12) Uani 1 1 d . . . Ce1 Ce 0.56423(2) 0.093194(14) 0.32073(2) 0.01821(8) Uani 1 1 d . . . N1 N 0.8320(4) 0.0662(3) 0.3164(3) 0.0318(10) Uani 1 1 d . . . H1A H 0.8420 0.0143 0.2977 0.038 Uiso 1 1 calc R . . H1B H 0.8562 0.0986 0.2684 0.038 Uiso 1 1 calc R . . N2 N 0.7630(4) 0.1681(2) 0.4709(3) 0.0278(9) Uani 1 1 d . . . H2A H 0.7486 0.2222 0.4675 0.033 Uiso 1 1 calc R . . H2B H 0.7522 0.1513 0.5334 0.033 Uiso 1 1 calc R . . N3 N 0.4477(4) 0.1949(2) 0.4375(3) 0.0329(10) Uani 1 1 d . . . H3A H 0.4462 0.1697 0.4975 0.040 Uiso 1 1 calc R . . H3B H 0.5022 0.2388 0.4523 0.040 Uiso 1 1 calc R . . N4 N 0.3467(4) 0.1846(2) 0.2272(3) 0.0311(10) Uani 1 1 d . . . H4A H 0.3729 0.2361 0.2186 0.037 Uiso 1 1 calc R . . H4B H 0.3088 0.1637 0.1651 0.037 Uiso 1 1 calc R . . N5 N 0.5954(4) 0.0988(2) 0.1246(3) 0.0207(8) Uani 1 1 d . . . H5A H 0.6711 0.0706 0.1196 0.025 Uiso 1 1 calc R . . H5B H 0.5235 0.0737 0.0845 0.025 Uiso 1 1 calc R . . N6 N 0.6542(4) 0.2357(2) 0.2570(3) 0.0216(9) Uani 1 1 d . . . H6A H 0.5859 0.2724 0.2505 0.026 Uiso 1 1 calc R . . H6B H 0.7234 0.2539 0.3064 0.026 Uiso 1 1 calc R . . N7 N 0.6149(4) -0.0631(2) 0.2849(3) 0.0295(10) Uani 1 1 d . . . H7A H 0.6666 -0.0649 0.2368 0.035 Uiso 1 1 calc R . . H7B H 0.6647 -0.0845 0.3432 0.035 Uiso 1 1 calc R . . N8 N 0.3601(4) 0.0059(2) 0.1977(3) 0.0232(9) Uani 1 1 d . . . H8A H 0.2926 -0.0021 0.2323 0.028 Uiso 1 1 calc R . . H8B H 0.3255 0.0359 0.1415 0.028 Uiso 1 1 calc R . . C1 C 0.9237(6) 0.0814(5) 0.4159(6) 0.0370(16) Uani 1 1 d . . . H1C H 0.9142 0.0370 0.4621 0.080 Uiso 1 1 calc R . . H1D H 1.0172 0.0807 0.4059 0.080 Uiso 1 1 calc R . . C2 C 0.9025(6) 0.1525(5) 0.4624(6) 0.0370(16) Uani 1 1 d . . . H2C H 0.9326 0.1968 0.4242 0.080 Uiso 1 1 calc R . . H2D H 0.9596 0.1529 0.5311 0.080 Uiso 1 1 calc R . . C3 C 0.3106(5) 0.2231(3) 0.3945(4) 0.0372(13) Uani 1 1 d . . . H3C H 0.3129 0.2813 0.3830 0.045 Uiso 1 1 calc R . . H3D H 0.2529 0.2133 0.4438 0.045 Uiso 1 1 calc R . . C4 C 0.2499(5) 0.1822(3) 0.2957(5) 0.0360(13) Uani 1 1 d . . . H4C H 0.2282 0.1262 0.3087 0.043 Uiso 1 1 calc R . . H4D H 0.1658 0.2095 0.2634 0.043 Uiso 1 1 calc R . . C5 C 0.6065(5) 0.1803(3) 0.0850(4) 0.0233(10) Uani 1 1 d . . . H5C H 0.5166 0.2052 0.0694 0.028 Uiso 1 1 calc R . . H5D H 0.6400 0.1770 0.0214 0.028 Uiso 1 1 calc R . . C6 C 0.7010(5) 0.2324(3) 0.1603(4) 0.0244(11) Uani 1 1 d . . . H6C H 0.7928 0.2102 0.1721 0.029 Uiso 1 1 calc R . . H6D H 0.7034 0.2868 0.1326 0.029 Uiso 1 1 calc R . . C7 C 0.4939(5) -0.1147(3) 0.2504(4) 0.0341(13) Uani 1 1 d . . . H7C H 0.4471 -0.1235 0.3066 0.041 Uiso 1 1 calc R . . H7D H 0.5213 -0.1670 0.2277 0.041 Uiso 1 1 calc R . . C8 C 0.4018(5) -0.0727(3) 0.1639(4) 0.0293(12) Uani 1 1 d . . . H8C H 0.4487 -0.0651 0.1074 0.035 Uiso 1 1 calc R . . H8D H 0.3215 -0.1060 0.1394 0.035 Uiso 1 1 calc R . . 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 0.01749(15) 0.01704(16) 0.01641(18) -0.00159(12) 0.00505(13) -0.00060(12) Se1 0.0355(3) 0.0330(3) 0.0190(3) 0.0065(2) 0.0044(2) -0.0066(2) Se2 0.0283(3) 0.0292(3) 0.0196(3) -0.0047(2) -0.0001(2) 0.0020(2) Se3 0.0185(2) 0.0266(3) 0.0231(3) -0.00437(19) 0.0024(2) 0.00313(19) Se4 0.0345(3) 0.0167(2) 0.0276(3) -0.00016(19) 0.0172(2) -0.0034(2) Ce1 0.02153(13) 0.01746(14) 0.01736(15) -0.00070(10) 0.00446(10) 0.00045(10) N1 0.025(2) 0.038(2) 0.031(3) -0.006(2) 0.004(2) 0.0002(19) N2 0.041(2) 0.023(2) 0.018(2) -0.0023(17) 0.0034(19) -0.0032(18) N3 0.049(3) 0.029(2) 0.023(3) -0.0060(19) 0.012(2) 0.001(2) N4 0.036(2) 0.029(2) 0.028(3) -0.0008(19) 0.006(2) 0.003(2) N5 0.0227(19) 0.021(2) 0.018(2) -0.0033(16) 0.0026(17) -0.0028(16) N6 0.028(2) 0.021(2) 0.015(2) -0.0021(16) 0.0043(17) 0.0010(17) N7 0.034(2) 0.026(2) 0.027(3) -0.0003(18) 0.004(2) 0.0007(19) N8 0.024(2) 0.028(2) 0.019(2) 0.0009(17) 0.0073(17) -0.0028(17) C1 0.036(2) 0.037(4) 0.031(4) -0.003(3) -0.007(2) 0.005(3) C2 0.036(2) 0.037(4) 0.031(4) -0.003(3) -0.007(2) 0.005(3) C3 0.044(3) 0.035(3) 0.039(4) -0.006(3) 0.023(3) 0.009(3) C4 0.028(3) 0.033(3) 0.049(4) 0.003(3) 0.012(3) 0.008(2) C5 0.031(2) 0.022(2) 0.018(3) 0.0038(19) 0.007(2) -0.003(2) C6 0.029(2) 0.024(3) 0.022(3) 0.002(2) 0.009(2) -0.005(2) C7 0.045(3) 0.021(3) 0.038(4) -0.003(2) 0.012(3) -0.004(2) C8 0.031(3) 0.031(3) 0.027(3) -0.013(2) 0.009(2) -0.013(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 Se2 2.4567(6) . ? Sn1 Se3 2.4648(6) . ? Sn1 Se4 2.5868(6) 3_666 ? Sn1 Se4 2.5870(6) . ? Se1 Se1 2.3731(11) 3_656 ? Se1 Ce1 3.2183(6) . ? Se1 Ce1 3.3034(6) 3_656 ? Se4 Sn1 2.5868(6) 3_666 ? Ce1 N7 2.708(4) . ? Ce1 N5 2.712(4) . ? Ce1 N3 2.728(4) . ? Ce1 N6 2.735(4) . ? Ce1 N4 2.750(4) . ? Ce1 N1 2.752(4) . ? Ce1 N8 2.769(4) . ? Ce1 N2 2.822(4) . ? Ce1 Se1 3.3034(6) 3_656 ? N1 C1 1.480(8) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.459(7) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 C3 1.462(7) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C4 1.472(7) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N5 C5 1.467(6) . ? N5 H5A 0.9100 . ? N5 H5B 0.9100 . ? N6 C6 1.467(6) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N7 C7 1.486(6) . ? N7 H7A 0.9100 . ? N7 H7B 0.9100 . ? N8 C8 1.472(6) . ? N8 H8A 0.9100 . ? N8 H8B 0.9100 . ? C1 C2 1.373(9) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.502(8) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C5 C6 1.511(6) . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 C8 1.499(8) . ? C7 H7C 0.9800 . ? C7 H7D 0.9800 . ? C8 H8C 0.9800 . ? C8 H8D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 Sn1 Se3 114.40(2) . . ? Se2 Sn1 Se4 118.29(2) . 3_666 ? Se3 Sn1 Se4 106.55(2) . 3_666 ? Se2 Sn1 Se4 110.83(2) . . ? Se3 Sn1 Se4 110.565(19) . . ? Se4 Sn1 Se4 94.410(17) 3_666 . ? Se1 Se1 Ce1 70.59(2) 3_656 . ? Se1 Se1 Ce1 66.76(2) 3_656 3_656 ? Ce1 Se1 Ce1 137.349(18) . 3_656 ? Sn1 Se4 Sn1 85.590(17) 3_666 . ? N7 Ce1 N5 78.30(12) . . ? N7 Ce1 N3 144.58(13) . . ? N5 Ce1 N3 133.16(12) . . ? N7 Ce1 N6 133.45(12) . . ? N5 Ce1 N6 63.61(11) . . ? N3 Ce1 N6 81.53(12) . . ? N7 Ce1 N4 127.65(13) . . ? N5 Ce1 N4 77.33(12) . . ? N3 Ce1 N4 61.39(13) . . ? N6 Ce1 N4 70.43(12) . . ? N7 Ce1 N1 67.53(13) . . ? N5 Ce1 N1 71.03(12) . . ? N3 Ce1 N1 130.86(13) . . ? N6 Ce1 N1 75.17(12) . . ? N4 Ce1 N1 140.89(13) . . ? N7 Ce1 N8 62.41(12) . . ? N5 Ce1 N8 70.20(11) . . ? N3 Ce1 N8 108.07(12) . . ? N6 Ce1 N8 121.43(12) . . ? N4 Ce1 N8 65.89(12) . . ? N1 Ce1 N8 121.04(12) . . ? N7 Ce1 N2 114.65(12) . . ? N5 Ce1 N2 117.94(11) . . ? N3 Ce1 N2 69.20(13) . . ? N6 Ce1 N2 66.89(12) . . ? N4 Ce1 N2 117.71(12) . . ? N1 Ce1 N2 61.95(12) . . ? N8 Ce1 N2 171.25(12) . . ? N7 Ce1 Se1 72.72(10) . . ? N5 Ce1 Se1 149.00(8) . . ? N3 Ce1 Se1 77.82(10) . . ? N6 Ce1 Se1 133.35(8) . . ? N4 Ce1 Se1 129.85(9) . . ? N1 Ce1 Se1 87.66(10) . . ? N8 Ce1 Se1 104.70(8) . . ? N2 Ce1 Se1 66.73(9) . . ? N7 Ce1 Se1 78.06(9) . 3_656 ? N5 Ce1 Se1 139.87(8) . 3_656 ? N3 Ce1 Se1 66.93(9) . 3_656 ? N6 Ce1 Se1 148.43(8) . 3_656 ? N4 Ce1 Se1 92.29(9) . 3_656 ? N1 Ce1 Se1 126.77(10) . 3_656 ? N8 Ce1 Se1 70.19(8) . 3_656 ? N2 Ce1 Se1 101.32(8) . 3_656 ? Se1 Ce1 Se1 42.651(18) . 3_656 ? C1 N1 Ce1 112.8(3) . . ? C1 N1 H1A 109.0 . . ? Ce1 N1 H1A 109.0 . . ? C1 N1 H1B 109.0 . . ? Ce1 N1 H1B 109.0 . . ? H1A N1 H1B 107.8 . . ? C2 N2 Ce1 115.0(3) . . ? C2 N2 H2A 108.5 . . ? Ce1 N2 H2A 108.5 . . ? C2 N2 H2B 108.5 . . ? Ce1 N2 H2B 108.5 . . ? H2A N2 H2B 107.5 . . ? C3 N3 Ce1 117.2(3) . . ? C3 N3 H3A 108.0 . . ? Ce1 N3 H3A 108.0 . . ? C3 N3 H3B 108.0 . . ? Ce1 N3 H3B 108.0 . . ? H3A N3 H3B 107.2 . . ? C4 N4 Ce1 105.8(3) . . ? C4 N4 H4A 110.6 . . ? Ce1 N4 H4A 110.6 . . ? C4 N4 H4B 110.6 . . ? Ce1 N4 H4B 110.6 . . ? H4A N4 H4B 108.7 . . ? C5 N5 Ce1 114.5(3) . . ? C5 N5 H5A 108.6 . . ? Ce1 N5 H5A 108.6 . . ? C5 N5 H5B 108.6 . . ? Ce1 N5 H5B 108.6 . . ? H5A N5 H5B 107.6 . . ? C6 N6 Ce1 115.5(3) . . ? C6 N6 H6A 108.4 . . ? Ce1 N6 H6A 108.4 . . ? C6 N6 H6B 108.4 . . ? Ce1 N6 H6B 108.4 . . ? H6A N6 H6B 107.5 . . ? C7 N7 Ce1 115.8(3) . . ? C7 N7 H7A 108.3 . . ? Ce1 N7 H7A 108.3 . . ? C7 N7 H7B 108.3 . . ? Ce1 N7 H7B 108.3 . . ? H7A N7 H7B 107.4 . . ? C8 N8 Ce1 115.0(3) . . ? C8 N8 H8A 108.5 . . ? Ce1 N8 H8A 108.5 . . ? C8 N8 H8B 108.5 . . ? Ce1 N8 H8B 108.5 . . ? H8A N8 H8B 107.5 . . ? C2 C1 N1 115.4(6) . . ? C2 C1 H1C 108.4 . . ? N1 C1 H1C 108.4 . . ? C2 C1 H1D 108.4 . . ? N1 C1 H1D 108.4 . . ? H1C C1 H1D 107.5 . . ? C1 C2 N2 115.6(6) . . ? C1 C2 H2C 108.4 . . ? N2 C2 H2C 108.4 . . ? C1 C2 H2D 108.4 . . ? N2 C2 H2D 108.4 . . ? H2C C2 H2D 107.5 . . ? N3 C3 C4 112.6(4) . . ? N3 C3 H3C 109.1 . . ? C4 C3 H3C 109.1 . . ? N3 C3 H3D 109.1 . . ? C4 C3 H3D 109.1 . . ? H3C C3 H3D 107.8 . . ? N4 C4 C3 109.5(4) . . ? N4 C4 H4C 109.8 . . ? C3 C4 H4C 109.8 . . ? N4 C4 H4D 109.8 . . ? C3 C4 H4D 109.8 . . ? H4C C4 H4D 108.2 . . ? N5 C5 C6 111.9(4) . . ? N5 C5 H5C 109.2 . . ? C6 C5 H5C 109.2 . . ? N5 C5 H5D 109.2 . . ? C6 C5 H5D 109.2 . . ? H5C C5 H5D 107.9 . . ? N6 C6 C5 109.7(4) . . ? N6 C6 H6C 109.7 . . ? C5 C6 H6C 109.7 . . ? N6 C6 H6D 109.7 . . ? C5 C6 H6D 109.7 . . ? H6C C6 H6D 108.2 . . ? N7 C7 C8 108.2(4) . . ? N7 C7 H7C 110.1 . . ? C8 C7 H7C 110.1 . . ? N7 C7 H7D 110.1 . . ? C8 C7 H7D 110.1 . . ? H7C C7 H7D 108.4 . . ? N8 C8 C7 110.3(4) . . ? N8 C8 H8C 109.6 . . ? C7 C8 H8C 109.6 . . ? N8 C8 H8D 109.6 . . ? C7 C8 H8D 109.6 . . ? H8C C8 H8D 108.1 . . ? 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 Se4 Sn1 122.55(2) . . . 3_666 ? Se3 Sn1 Se4 Sn1 -109.51(2) . . . 3_666 ? Se4 Sn1 Se4 Sn1 0.0 3_666 . . 3_666 ? Se1 Se1 Ce1 N7 -91.03(10) 3_656 . . . ? Ce1 Se1 Ce1 N7 -91.03(10) 3_656 . . . ? Se1 Se1 Ce1 N5 -112.60(15) 3_656 . . . ? Ce1 Se1 Ce1 N5 -112.60(15) 3_656 . . . ? Se1 Se1 Ce1 N3 69.06(10) 3_656 . . . ? Ce1 Se1 Ce1 N3 69.06(10) 3_656 . . . ? Se1 Se1 Ce1 N6 134.80(11) 3_656 . . . ? Ce1 Se1 Ce1 N6 134.80(11) 3_656 . . . ? Se1 Se1 Ce1 N4 33.97(12) 3_656 . . . ? Ce1 Se1 Ce1 N4 33.97(12) 3_656 . . . ? Se1 Se1 Ce1 N1 -158.21(9) 3_656 . . . ? Ce1 Se1 Ce1 N1 -158.21(9) 3_656 . . . ? Se1 Se1 Ce1 N8 -36.69(8) 3_656 . . . ? Ce1 Se1 Ce1 N8 -36.69(8) 3_656 . . . ? Se1 Se1 Ce1 N2 141.45(9) 3_656 . . . ? Ce1 Se1 Ce1 N2 141.45(9) 3_656 . . . ? Ce1 Se1 Ce1 Se1 0.0 3_656 . . 3_656 ? N7 Ce1 N1 C1 -115.4(5) . . . . ? N5 Ce1 N1 C1 159.7(5) . . . . ? N3 Ce1 N1 C1 28.5(5) . . . . ? N6 Ce1 N1 C1 93.0(4) . . . . ? N4 Ce1 N1 C1 121.9(4) . . . . ? N8 Ce1 N1 C1 -149.0(4) . . . . ? N2 Ce1 N1 C1 21.6(4) . . . . ? Se1 Ce1 N1 C1 -43.2(4) . . . . ? Se1 Ce1 N1 C1 -61.5(5) 3_656 . . . ? N7 Ce1 N2 C2 45.2(5) . . . . ? N5 Ce1 N2 C2 -44.3(5) . . . . ? N3 Ce1 N2 C2 -173.1(5) . . . . ? N6 Ce1 N2 C2 -83.6(5) . . . . ? N4 Ce1 N2 C2 -134.2(4) . . . . ? N1 Ce1 N2 C2 1.3(4) . . . . ? N8 Ce1 N2 C2 113.6(8) . . . . ? Se1 Ce1 N2 C2 101.6(5) . . . . ? Se1 Ce1 N2 C2 127.1(4) 3_656 . . . ? N7 Ce1 N3 C3 -97.0(4) . . . . ? N5 Ce1 N3 C3 50.1(4) . . . . ? N6 Ce1 N3 C3 91.0(4) . . . . ? N4 Ce1 N3 C3 18.7(3) . . . . ? N1 Ce1 N3 C3 152.9(3) . . . . ? N8 Ce1 N3 C3 -29.4(4) . . . . ? N2 Ce1 N3 C3 159.4(4) . . . . ? Se1 Ce1 N3 C3 -131.1(4) . . . . ? Se1 Ce1 N3 C3 -87.7(3) 3_656 . . . ? N7 Ce1 N4 C4 97.0(3) . . . . ? N5 Ce1 N4 C4 161.1(3) . . . . ? N3 Ce1 N4 C4 -41.8(3) . . . . ? N6 Ce1 N4 C4 -132.7(3) . . . . ? N1 Ce1 N4 C4 -162.5(3) . . . . ? N8 Ce1 N4 C4 87.4(3) . . . . ? N2 Ce1 N4 C4 -83.8(3) . . . . ? Se1 Ce1 N4 C4 -2.0(4) . . . . ? Se1 Ce1 N4 C4 20.3(3) 3_656 . . . ? N7 Ce1 N5 C5 -168.6(3) . . . . ? N3 Ce1 N5 C5 30.1(4) . . . . ? N6 Ce1 N5 C5 -16.2(3) . . . . ? N4 Ce1 N5 C5 58.1(3) . . . . ? N1 Ce1 N5 C5 -98.6(3) . . . . ? N8 Ce1 N5 C5 126.7(3) . . . . ? N2 Ce1 N5 C5 -56.8(3) . . . . ? Se1 Ce1 N5 C5 -147.6(2) . . . . ? Se1 Ce1 N5 C5 136.3(2) 3_656 . . . ? N7 Ce1 N6 C6 24.6(4) . . . . ? N5 Ce1 N6 C6 -13.9(3) . . . . ? N3 Ce1 N6 C6 -161.7(3) . . . . ? N4 Ce1 N6 C6 -99.1(3) . . . . ? N1 Ce1 N6 C6 61.9(3) . . . . ? N8 Ce1 N6 C6 -55.7(3) . . . . ? N2 Ce1 N6 C6 127.4(3) . . . . ? Se1 Ce1 N6 C6 134.0(3) . . . . ? Se1 Ce1 N6 C6 -159.3(2) 3_656 . . . ? N5 Ce1 N7 C7 -93.8(4) . . . . ? N3 Ce1 N7 C7 62.3(4) . . . . ? N6 Ce1 N7 C7 -128.5(3) . . . . ? N4 Ce1 N7 C7 -30.0(4) . . . . ? N1 Ce1 N7 C7 -167.9(4) . . . . ? N8 Ce1 N7 C7 -20.1(3) . . . . ? N2 Ce1 N7 C7 150.7(3) . . . . ? Se1 Ce1 N7 C7 97.4(3) . . . . ? Se1 Ce1 N7 C7 53.6(3) 3_656 . . . ? N7 Ce1 N8 C8 -11.9(3) . . . . ? N5 Ce1 N8 C8 75.0(3) . . . . ? N3 Ce1 N8 C8 -154.7(3) . . . . ? N6 Ce1 N8 C8 114.3(3) . . . . ? N4 Ce1 N8 C8 159.5(4) . . . . ? N1 Ce1 N8 C8 23.3(4) . . . . ? N2 Ce1 N8 C8 -84.3(8) . . . . ? Se1 Ce1 N8 C8 -73.0(3) . . . . ? Se1 Ce1 N8 C8 -98.5(3) 3_656 . . . ? Ce1 N1 C1 C2 -47.6(8) . . . . ? N1 C1 C2 N2 50.4(10) . . . . ? Ce1 N2 C2 C1 -26.7(9) . . . . ? Ce1 N3 C3 C4 7.0(6) . . . . ? Ce1 N4 C4 C3 64.9(4) . . . . ? N3 C3 C4 N4 -49.1(6) . . . . ? Ce1 N5 C5 C6 44.8(4) . . . . ? Ce1 N6 C6 C5 41.4(4) . . . . ? N5 C5 C6 N6 -57.2(5) . . . . ? Ce1 N7 C7 C8 49.6(5) . . . . ? Ce1 N8 C8 C7 42.1(5) . . . . ? N7 C7 C8 N8 -59.9(5) . . . . ? 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 Se2 0.91 3.00 3.719(4) 137.0 2_645 N2 H2A Se3 0.91 2.75 3.624(4) 162.4 . N2 H2B Se1 0.91 2.84 3.338(4) 115.6 . N4 H4A Se2 0.91 2.91 3.802(4) 166.1 . N4 H4B Se3 0.91 2.95 3.807(5) 158.4 4_565 N5 H5B Se3 0.91 2.76 3.498(4) 138.4 4_565 N6 H6A Se2 0.91 2.73 3.619(4) 166.4 . N6 H6B Se3 0.91 2.90 3.640(4) 140.0 . N7 H7A Se3 0.91 2.78 3.608(5) 151.7 2_645 N8 H8A Se2 0.91 2.81 3.627(4) 149.9 2_545 N8 H8B Se3 0.91 2.83 3.710(4) 163.8 4_565 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.717 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.165 #===END data_complex_1b _database_code_depnum_ccdc_archive 'CCDC 797226' #TrackingRef 'cif-of-1a-2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H50 N12 O2 Pr2 Se6 Sn2' _chemical_formula_sum 'C12 H50 N12 O2 Pr2 Se6 Sn2' _chemical_formula_weight 1387.60 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1968(11) _cell_length_b 11.7622(9) _cell_length_c 15.4969(16) _cell_angle_alpha 90.00 _cell_angle_beta 98.967(3) _cell_angle_gamma 90.00 _cell_volume 1835.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8748 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 9.929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1904 _exptl_absorpt_correction_T_max 0.2414 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8936 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3212 _reflns_number_gt 2829 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0319P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3212 _refine_ls_number_parameters 167 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.61016(3) 0.59685(3) 0.46073(2) 0.02081(10) Uani 1 1 d . . . Se1 Se 0.59621(6) 0.80381(4) 0.47748(4) 0.03525(16) Uani 1 1 d . . . Se2 Se 0.79712(5) 0.54347(4) 0.38537(4) 0.02950(14) Uani 1 1 d . . . Se3 Se 0.61131(5) 0.49591(4) 0.60885(3) 0.02852(14) Uani 1 1 d . . . Pr1 Pr 0.87753(3) 0.12043(2) 0.454543(18) 0.01935(9) Uani 1 1 d . . . O1 O 0.9164(3) -0.0777(3) 0.4618(2) 0.0318(9) Uani 1 1 d . . . H1 H 0.8568 -0.1325 0.4346 0.038 Uiso 1 1 calc R . . N1 N 0.8727(5) 0.2632(4) 0.5889(3) 0.0390(12) Uani 1 1 d . . . H1A H 0.9570 0.2723 0.6175 0.047 Uiso 1 1 calc R . . H1B H 0.8435 0.3323 0.5675 0.047 Uiso 1 1 calc R . . N2 N 0.7215(5) 0.0598(4) 0.5640(3) 0.0333(11) Uani 1 1 d . . . H2A H 0.6395 0.0905 0.5477 0.040 Uiso 1 1 calc R . . H2B H 0.7130 -0.0173 0.5639 0.040 Uiso 1 1 calc R . . N3 N 0.9510(5) 0.1381(4) 0.2973(3) 0.0404(12) Uani 1 1 d D . . H3 H 0.9238 0.0865 0.2535 0.048 Uiso 1 1 calc R . . N4 N 1.0122(5) 0.3065(4) 0.4300(3) 0.0358(11) Uani 1 1 d . . . H4A H 0.9582 0.3673 0.4338 0.043 Uiso 1 1 calc R . . H4B H 1.0811 0.3122 0.4748 0.043 Uiso 1 1 calc R . . N5 N 0.6795(4) 0.0306(3) 0.3425(3) 0.0275(10) Uani 1 1 d . . . H5A H 0.7109 0.0133 0.2923 0.033 Uiso 1 1 calc R . . H5B H 0.6548 -0.0359 0.3655 0.033 Uiso 1 1 calc R . . N6 N 0.6782(4) 0.2588(3) 0.4004(3) 0.0286(10) Uani 1 1 d . . . H6A H 0.6236 0.2612 0.4415 0.034 Uiso 1 1 calc R . . H6B H 0.7108 0.3300 0.3953 0.034 Uiso 1 1 calc R . . C1 C 0.7883(7) 0.2254(5) 0.6516(4) 0.0450(16) Uani 1 1 d . . . H1C H 0.6997 0.2587 0.6363 0.054 Uiso 1 1 calc R . . H1D H 0.8259 0.2520 0.7102 0.054 Uiso 1 1 calc R . . C2 C 0.7772(8) 0.0991(5) 0.6522(4) 0.0515(18) Uani 1 1 d . . . H2C H 0.8651 0.0653 0.6701 0.062 Uiso 1 1 calc R . . H2D H 0.7196 0.0756 0.6940 0.062 Uiso 1 1 calc R . . C3A C 0.9757(10) 0.2622(8) 0.2776(6) 0.041(2) Uani 0.62 1 d PD . . H3A1 H 1.0138 0.2673 0.2234 0.049 Uiso 0.62 1 calc PR . . H3A2 H 0.8910 0.3033 0.2687 0.049 Uiso 0.62 1 calc PR . . C3B C 1.0694(14) 0.2067(11) 0.2978(10) 0.047(2) Uani 0.38 1 d PD . . H3B1 H 1.0794 0.2248 0.2374 0.049 Uiso 0.38 1 calc PR . . H3B2 H 1.1471 0.1624 0.3235 0.049 Uiso 0.38 1 calc PR . . C4 C 1.0654(7) 0.3154(5) 0.3481(5) 0.0535(18) Uani 1 1 d D . . C5 C 0.5595(5) 0.1026(4) 0.3200(4) 0.0323(13) Uani 1 1 d . . . H5C H 0.5012 0.0931 0.3642 0.039 Uiso 1 1 calc R . . H5D H 0.5104 0.0793 0.2634 0.039 Uiso 1 1 calc R . . C6 C 0.6000(6) 0.2254(5) 0.3162(4) 0.0366(14) Uani 1 1 d . . . H6C H 0.6530 0.2360 0.2692 0.044 Uiso 1 1 calc R . . H6D H 0.5207 0.2734 0.3037 0.044 Uiso 1 1 calc R . . 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 0.02086(19) 0.01878(17) 0.0233(2) 0.00151(13) 0.00515(14) -0.00107(13) Se1 0.0345(3) 0.0182(3) 0.0562(4) 0.0001(2) 0.0172(3) -0.0024(2) Se2 0.0267(3) 0.0320(3) 0.0317(3) -0.0014(2) 0.0104(2) 0.0021(2) Se3 0.0274(3) 0.0334(3) 0.0229(3) 0.0054(2) -0.0017(2) -0.0074(2) Pr1 0.01784(15) 0.01821(14) 0.02156(16) 0.00046(10) 0.00164(11) 0.00042(10) O1 0.0239(19) 0.0207(17) 0.047(2) -0.0050(16) -0.0063(17) 0.0015(15) N1 0.033(3) 0.041(3) 0.041(3) -0.013(2) 0.000(2) 0.003(2) N2 0.041(3) 0.024(2) 0.037(3) 0.001(2) 0.015(2) 0.000(2) N3 0.041(3) 0.050(3) 0.032(3) -0.012(2) 0.013(2) -0.012(2) N4 0.033(3) 0.032(2) 0.039(3) 0.003(2) -0.002(2) -0.007(2) N5 0.029(2) 0.026(2) 0.029(3) 0.0015(19) 0.006(2) -0.0026(19) N6 0.022(2) 0.025(2) 0.037(3) -0.0012(19) 0.000(2) 0.0011(19) C1 0.049(4) 0.052(4) 0.032(4) -0.010(3) -0.001(3) 0.007(3) C2 0.065(5) 0.054(4) 0.038(4) 0.005(3) 0.017(4) 0.013(3) C3A 0.046(5) 0.053(6) 0.037(5) 0.010(4) 0.017(4) -0.007(4) C3B 0.045(5) 0.049(6) 0.042(5) 0.012(4) 0.011(4) -0.005(4) C4 0.066(5) 0.046(4) 0.056(5) -0.003(3) 0.034(4) -0.014(3) C5 0.029(3) 0.034(3) 0.033(3) -0.005(2) 0.002(3) -0.001(2) C6 0.031(3) 0.039(3) 0.037(4) -0.001(3) -0.003(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Se1 2.4545(6) . ? Sn1 Se2 2.4671(6) . ? Sn1 Se3 2.5826(7) . ? Sn1 Se3 2.5873(6) 3_666 ? Se3 Sn1 2.5873(6) 3_666 ? Pr1 O1 2.345(3) 3_756 ? Pr1 O1 2.363(3) . ? Pr1 N2 2.600(4) . ? Pr1 N6 2.636(4) . ? Pr1 N4 2.642(4) . ? Pr1 N3 2.667(5) . ? Pr1 N5 2.668(4) . ? Pr1 N1 2.681(4) . ? Pr1 Pr1 3.8927(6) 3_756 ? O1 Pr1 2.345(3) 3_756 ? O1 H1 0.9400 . ? N1 C1 1.464(8) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.471(8) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 C3B 1.451(12) . ? N3 C3A 1.521(9) . ? N3 H3 0.9200 . ? N4 C4 1.460(8) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N5 C5 1.485(7) . ? N5 H5A 0.9100 . ? N5 H5B 0.9100 . ? N6 C6 1.473(7) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? C1 C2 1.489(8) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3A C4 1.454(10) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3B C4 1.502(13) . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C5 C6 1.505(7) . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? 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 111.36(2) . . ? Se1 Sn1 Se3 110.75(2) . . ? Se2 Sn1 Se3 114.01(2) . . ? Se1 Sn1 Se3 113.65(2) . 3_666 ? Se2 Sn1 Se3 112.59(2) . 3_666 ? Se3 Sn1 Se3 93.400(19) . 3_666 ? Sn1 Se3 Sn1 86.600(19) . 3_666 ? O1 Pr1 O1 68.45(14) 3_756 . ? O1 Pr1 N2 99.63(14) 3_756 . ? O1 Pr1 N2 79.25(13) . . ? O1 Pr1 N6 152.65(12) 3_756 . ? O1 Pr1 N6 137.65(12) . . ? N2 Pr1 N6 81.79(15) . . ? O1 Pr1 N4 79.41(13) 3_756 . ? O1 Pr1 N4 137.43(14) . . ? N2 Pr1 N4 134.88(15) . . ? N6 Pr1 N4 80.51(14) . . ? O1 Pr1 N3 99.59(15) 3_756 . ? O1 Pr1 N3 92.95(14) . . ? N2 Pr1 N3 154.85(15) . . ? N6 Pr1 N3 88.48(15) . . ? N4 Pr1 N3 65.04(15) . . ? O1 Pr1 N5 142.83(12) 3_756 . ? O1 Pr1 N5 75.22(12) . . ? N2 Pr1 N5 80.65(14) . . ? N6 Pr1 N5 64.51(12) . . ? N4 Pr1 N5 126.32(14) . . ? N3 Pr1 N5 74.22(14) . . ? O1 Pr1 N1 80.13(14) 3_756 . ? O1 Pr1 N1 127.13(14) . . ? N2 Pr1 N1 65.04(15) . . ? N6 Pr1 N1 75.75(14) . . ? N4 Pr1 N1 70.47(15) . . ? N3 Pr1 N1 134.64(15) . . ? N5 Pr1 N1 130.52(14) . . ? O1 Pr1 Pr1 34.38(8) 3_756 3_756 ? O1 Pr1 Pr1 34.07(8) . 3_756 ? N2 Pr1 Pr1 89.29(10) . 3_756 ? N6 Pr1 Pr1 169.64(10) . 3_756 ? N4 Pr1 Pr1 109.66(10) . 3_756 ? N3 Pr1 Pr1 97.57(11) . 3_756 ? N5 Pr1 Pr1 108.97(9) . 3_756 ? N1 Pr1 Pr1 105.26(11) . 3_756 ? Pr1 O1 Pr1 111.55(14) 3_756 . ? Pr1 O1 H1 124.2 3_756 . ? Pr1 O1 H1 124.2 . . ? C1 N1 Pr1 114.2(3) . . ? C1 N1 H1A 108.7 . . ? Pr1 N1 H1A 108.7 . . ? C1 N1 H1B 108.7 . . ? Pr1 N1 H1B 108.7 . . ? H1A N1 H1B 107.6 . . ? C2 N2 Pr1 109.4(4) . . ? C2 N2 H2A 109.8 . . ? Pr1 N2 H2A 109.8 . . ? C2 N2 H2B 109.8 . . ? Pr1 N2 H2B 109.8 . . ? H2A N2 H2B 108.2 . . ? C3B N3 C3A 45.8(7) . . ? C3B N3 Pr1 113.0(6) . . ? C3A N3 Pr1 109.7(4) . . ? C3B N3 H3 121.8 . . ? C3A N3 H3 121.8 . . ? Pr1 N3 H3 121.8 . . ? C4 N4 Pr1 117.2(3) . . ? C4 N4 H4A 108.0 . . ? Pr1 N4 H4A 108.0 . . ? C4 N4 H4B 108.0 . . ? Pr1 N4 H4B 108.0 . . ? H4A N4 H4B 107.3 . . ? C5 N5 Pr1 116.0(3) . . ? C5 N5 H5A 108.3 . . ? Pr1 N5 H5A 108.3 . . ? C5 N5 H5B 108.3 . . ? Pr1 N5 H5B 108.3 . . ? H5A N5 H5B 107.4 . . ? C6 N6 Pr1 113.7(3) . . ? C6 N6 H6A 108.8 . . ? Pr1 N6 H6A 108.8 . . ? C6 N6 H6B 108.8 . . ? Pr1 N6 H6B 108.8 . . ? H6A N6 H6B 107.7 . . ? N1 C1 C2 111.1(5) . . ? N1 C1 H1C 109.4 . . ? C2 C1 H1C 109.4 . . ? N1 C1 H1D 109.4 . . ? C2 C1 H1D 109.4 . . ? H1C C1 H1D 108.0 . . ? N2 C2 C1 109.1(5) . . ? N2 C2 H2C 109.9 . . ? C1 C2 H2C 109.9 . . ? N2 C2 H2D 109.9 . . ? C1 C2 H2D 109.9 . . ? H2C C2 H2D 108.3 . . ? C4 C3A N3 111.5(7) . . ? C4 C3A H3A1 109.3 . . ? N3 C3A H3A1 109.3 . . ? C4 C3A H3A2 109.3 . . ? N3 C3A H3A2 109.3 . . ? H3A1 C3A H3A2 108.0 . . ? N3 C3B C4 112.7(10) . . ? N3 C3B H3B1 109.0 . . ? C4 C3B H3B1 109.0 . . ? N3 C3B H3B2 109.0 . . ? C4 C3B H3B2 109.0 . . ? H3B1 C3B H3B2 107.8 . . ? C3A C4 N4 110.3(6) . . ? C3A C4 C3B 46.1(7) . . ? N4 C4 C3B 115.7(7) . . ? N5 C5 C6 109.6(4) . . ? N5 C5 H5C 109.7 . . ? C6 C5 H5C 109.7 . . ? N5 C5 H5D 109.7 . . ? C6 C5 H5D 109.7 . . ? H5C C5 H5D 108.2 . . ? N6 C6 C5 109.5(5) . . ? N6 C6 H6C 109.8 . . ? C5 C6 H6C 109.8 . . ? N6 C6 H6D 109.8 . . ? C5 C6 H6D 109.8 . . ? H6C C6 H6D 108.2 . . ? 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 Se1 Sn1 Se3 Sn1 116.88(2) . . . 3_666 ? Se2 Sn1 Se3 Sn1 -116.59(2) . . . 3_666 ? Se3 Sn1 Se3 Sn1 0.0 3_666 . . 3_666 ? O1 Pr1 O1 Pr1 0.0 3_756 . . 3_756 ? N2 Pr1 O1 Pr1 -104.96(18) . . . 3_756 ? N6 Pr1 O1 Pr1 -169.86(16) . . . 3_756 ? N4 Pr1 O1 Pr1 43.8(3) . . . 3_756 ? N3 Pr1 O1 Pr1 99.15(18) . . . 3_756 ? N5 Pr1 O1 Pr1 172.0(2) . . . 3_756 ? N1 Pr1 O1 Pr1 -58.0(2) . . . 3_756 ? O1 Pr1 N1 C1 -103.3(4) 3_756 . . . ? O1 Pr1 N1 C1 -50.1(4) . . . . ? N2 Pr1 N1 C1 2.3(4) . . . . ? N6 Pr1 N1 C1 89.7(4) . . . . ? N4 Pr1 N1 C1 174.5(4) . . . . ? N3 Pr1 N1 C1 162.9(4) . . . . ? N5 Pr1 N1 C1 53.0(4) . . . . ? Pr1 Pr1 N1 C1 -79.6(4) 3_756 . . . ? O1 Pr1 N2 C2 42.6(4) 3_756 . . . ? O1 Pr1 N2 C2 108.3(4) . . . . ? N6 Pr1 N2 C2 -109.8(4) . . . . ? N4 Pr1 N2 C2 -42.1(4) . . . . ? N3 Pr1 N2 C2 -178.1(4) . . . . ? N5 Pr1 N2 C2 -175.2(4) . . . . ? N1 Pr1 N2 C2 -31.7(3) . . . . ? Pr1 Pr1 N2 C2 75.5(3) 3_756 . . . ? O1 Pr1 N3 C3B -46.8(7) 3_756 . . . ? O1 Pr1 N3 C3B -115.4(7) . . . . ? N2 Pr1 N3 C3B 173.8(7) . . . . ? N6 Pr1 N3 C3B 106.9(7) . . . . ? N4 Pr1 N3 C3B 26.7(7) . . . . ? N5 Pr1 N3 C3B 170.8(7) . . . . ? N1 Pr1 N3 C3B 38.8(8) . . . . ? Pr1 Pr1 N3 C3B -81.5(7) 3_756 . . . ? O1 Pr1 N3 C3A -96.1(5) 3_756 . . . ? O1 Pr1 N3 C3A -164.7(5) . . . . ? N2 Pr1 N3 C3A 124.5(5) . . . . ? N6 Pr1 N3 C3A 57.6(5) . . . . ? N4 Pr1 N3 C3A -22.6(5) . . . . ? N5 Pr1 N3 C3A 121.5(5) . . . . ? N1 Pr1 N3 C3A -10.5(5) . . . . ? Pr1 Pr1 N3 C3A -130.8(5) 3_756 . . . ? O1 Pr1 N4 C4 100.4(4) 3_756 . . . ? O1 Pr1 N4 C4 59.4(5) . . . . ? N2 Pr1 N4 C4 -166.5(4) . . . . ? N6 Pr1 N4 C4 -98.3(4) . . . . ? N3 Pr1 N4 C4 -5.6(4) . . . . ? N5 Pr1 N4 C4 -50.0(5) . . . . ? N1 Pr1 N4 C4 -176.5(5) . . . . ? Pr1 Pr1 N4 C4 83.8(4) 3_756 . . . ? O1 Pr1 N5 C5 171.6(3) 3_756 . . . ? O1 Pr1 N5 C5 159.2(4) . . . . ? N2 Pr1 N5 C5 78.0(4) . . . . ? N6 Pr1 N5 C5 -7.3(3) . . . . ? N4 Pr1 N5 C5 -62.1(4) . . . . ? N3 Pr1 N5 C5 -103.3(4) . . . . ? N1 Pr1 N5 C5 32.7(4) . . . . ? Pr1 Pr1 N5 C5 164.0(3) 3_756 . . . ? O1 Pr1 N6 C6 158.2(3) 3_756 . . . ? O1 Pr1 N6 C6 -42.7(4) . . . . ? N2 Pr1 N6 C6 -106.7(4) . . . . ? N4 Pr1 N6 C6 115.0(4) . . . . ? N3 Pr1 N6 C6 50.1(4) . . . . ? N5 Pr1 N6 C6 -23.2(3) . . . . ? N1 Pr1 N6 C6 -172.9(4) . . . . ? Pr1 Pr1 N6 C6 -75.9(7) 3_756 . . . ? Pr1 N1 C1 C2 27.3(6) . . . . ? Pr1 N2 C2 C1 60.4(6) . . . . ? N1 C1 C2 N2 -58.8(7) . . . . ? C3B N3 C3A C4 -51.7(9) . . . . ? Pr1 N3 C3A C4 51.6(8) . . . . ? C3A N3 C3B C4 50.0(9) . . . . ? Pr1 N3 C3B C4 -45.6(13) . . . . ? N3 C3A C4 N4 -57.7(9) . . . . ? N3 C3A C4 C3B 49.0(9) . . . . ? Pr1 N4 C4 C3A 34.5(7) . . . . ? Pr1 N4 C4 C3B -15.5(10) . . . . ? N3 C3B C4 C3A -52.9(9) . . . . ? N3 C3B C4 N4 41.2(14) . . . . ? Pr1 N5 C5 C6 35.8(6) . . . . ? Pr1 N6 C6 C5 51.6(5) . . . . ? N5 C5 C6 N6 -57.2(6) . . . . ? 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 O1 H1 Se1 0.94 2.93 3.593(4) 128.3 1_545 N2 H2A Se1 0.91 2.68 3.582(5) 171.6 3_666 N2 H2B Se1 0.91 2.67 3.458(4) 145.1 1_545 N3 H3 Se2 0.92 2.91 3.663(5) 140.4 2_645 N4 H4A Se2 0.91 2.68 3.547(5) 160.3 . N4 H4B Se2 0.91 2.88 3.653(5) 144.0 3_766 N5 H5A Se2 0.91 2.76 3.580(4) 149.8 2_645 N5 H5B Se1 0.91 2.69 3.572(4) 162.9 1_545 N6 H6A Se1 0.91 2.84 3.689(5) 155.9 3_666 N6 H6B Se2 0.91 2.67 3.581(4) 176.9 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.844 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.212 #===END data_complex_1c _database_code_depnum_ccdc_archive 'CCDC 797227' #TrackingRef 'cif-of-1a-2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H50 N12 Nd2 O2 Se6 Sn2' _chemical_formula_sum 'C12 H50 N12 Nd2 O2 Se6 Sn2' _chemical_formula_weight 1394.26 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' Nd Nd -0.1943 3.0179 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1764(18) _cell_length_b 11.7725(19) _cell_length_c 15.470(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.128(4) _cell_angle_gamma 90.00 _cell_volume 1829.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8338 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 10.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2363 _exptl_absorpt_correction_T_max 0.2627 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14041 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3206 _reflns_number_gt 2361 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0787P)^2^+720.2350P] 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_number_reflns 3206 _refine_ls_number_parameters 131 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1690 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.090 _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 0.6105(3) 0.0962(2) 0.46047(16) 0.0205(7) Uani 1 1 d . . . Nd1 Nd 0.6222(2) 0.12005(16) 0.04539(13) 0.0208(6) Uani 1 1 d . . . Se1 Se 0.7991(4) 0.0429(3) 0.3860(3) 0.0287(10) Uani 1 1 d . . . Se2 Se 0.5961(5) 0.3034(3) 0.4765(3) 0.0369(11) Uani 1 1 d . . . Se3 Se 0.3882(4) 0.0035(3) 0.3908(2) 0.0280(10) Uani 1 1 d . . . N1 N 0.820(4) 0.258(3) 0.099(2) 0.036(3) Uani 1 1 d . . . H1A H 0.8761 0.2578 0.0584 0.043 Uiso 1 1 calc R . . H1B H 0.7873 0.3293 0.1014 0.043 Uiso 1 1 calc R . . N2 N 0.820(4) 0.030(3) 0.157(2) 0.038(3) Uani 1 1 d . . . H2A H 0.7885 0.0111 0.2066 0.043 Uiso 1 1 calc R . . H2B H 0.8462 -0.0351 0.1330 0.043 Uiso 1 1 calc R . . N3 N 0.630(4) 0.260(3) -0.088(2) 0.035(3) Uani 1 1 d . . . H3A H 0.5452 0.2711 -0.1153 0.043 Uiso 1 1 calc R . . H3B H 0.6619 0.3278 -0.0660 0.043 Uiso 1 1 calc R . . N4 N 0.782(4) 0.059(3) -0.062(2) 0.037(3) Uani 1 1 d . . . H4A H 0.8638 0.0902 -0.0446 0.043 Uiso 1 1 calc R . . H4B H 0.7908 -0.0180 -0.0611 0.043 Uiso 1 1 calc R . . N5 N 0.550(4) 0.135(3) 0.202(2) 0.046(10) Uani 1 1 d D . . N6 N 0.487(4) 0.304(3) 0.073(2) 0.037(9) Uani 1 1 d . . . H6A H 0.5386 0.3651 0.0650 0.044 Uiso 1 1 calc R . . H6B H 0.4146 0.3073 0.0296 0.044 Uiso 1 1 calc R . . C1 C 0.895(4) 0.228(4) 0.183(3) 0.034(10) Uani 1 1 d . . . H1C H 0.8387 0.2381 0.2288 0.041 Uiso 1 1 calc R . . H1D H 0.9721 0.2784 0.1969 0.041 Uiso 1 1 calc R . . C2 C 0.941(4) 0.104(3) 0.181(3) 0.035(10) Uani 1 1 d . . . H2C H 1.0014 0.0948 0.1386 0.042 Uiso 1 1 calc R . . H2D H 0.9882 0.0818 0.2392 0.042 Uiso 1 1 calc R . . C3 C 0.705(5) 0.226(4) -0.150(3) 0.036(3) Uani 1 1 d . . . H3C H 0.7920 0.2634 -0.1380 0.043 Uiso 1 1 calc R . . H3D H 0.6608 0.2514 -0.2077 0.043 Uiso 1 1 calc R . . C4 C 0.725(5) 0.099(4) -0.152(3) 0.036(3) Uani 1 1 d . . . H4C H 0.6395 0.0611 -0.1714 0.043 Uiso 1 1 calc R . . H4D H 0.7856 0.0797 -0.1928 0.043 Uiso 1 1 calc R . . C5A C 0.447(9) 0.220(7) 0.215(6) 0.039(4) Uani 0.40 1 d PD . . C5B C 0.520(8) 0.253(4) 0.227(4) 0.036(4) Uani 0.60 1 d PD . . C6 C 0.439(4) 0.321(3) 0.154(3) 0.036(3) Uani 1 1 d D . . O1 O 0.584(3) -0.077(2) 0.038(2) 0.0415(9) Uani 1 1 d . . . H1 H 0.6439 -0.1314 0.0658 0.054 Uiso 1 1 calc R . . 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 0.0249(14) 0.0148(12) 0.0217(13) 0.0017(9) 0.0038(10) -0.0012(10) Nd1 0.0221(11) 0.0173(10) 0.0218(10) 0.0002(8) -0.0004(8) -0.0002(8) Se1 0.028(2) 0.028(2) 0.032(2) -0.0023(17) 0.0101(17) 0.0024(17) Se2 0.039(3) 0.0116(18) 0.064(3) -0.0007(18) 0.020(2) -0.0039(17) Se3 0.028(2) 0.032(2) 0.0213(18) 0.0063(16) -0.0033(15) -0.0075(17) N1 0.035(9) 0.037(8) 0.042(8) 0.005(7) 0.008(7) -0.005(7) N2 0.037(9) 0.032(8) 0.039(8) 0.0010(7) 0.007(7) -0.006(7) N3 0.034(9) 0.034(8) 0.040(8) 0.009(7) 0.006(7) -0.008(7) N4 0.034(9) 0.032(8) 0.042(8) 0.008(7) 0.004(7) -0.006(7) N5 0.07(3) 0.05(2) 0.019(18) 0.006(16) 0.020(18) 0.01(2) N6 0.03(2) 0.04(2) 0.034(19) -0.004(16) -0.004(16) 0.023(17) C1 0.03(2) 0.04(2) 0.04(2) 0.010(19) 0.001(18) -0.003(19) C2 0.009(19) 0.03(2) 0.07(3) 0.00(2) 0.001(19) -0.003(16) C3 0.036(9) 0.035(8) 0.040(8) 0.007(7) 0.008(7) -0.007(7) C4 0.034(9) 0.032(8) 0.042(8) 0.009(7) 0.005(7) -0.005(7) C5A 0.034(4) 0.026(9) 0.042(4) 0.003(5) -0.009(4) 0.006(6) C5B 0.035(4) 0.024(9) 0.044(4) 0.004(5) -0.007(4) 0.009(6) C6 0.034(9) 0.032(8) 0.042(8) 0.009(7) 0.008(7) -0.005(7) O1 0.041(2) 0.034(15) 0.041(2) 0.004(14) 0.008(17) 0.017(15) _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 Se2 2.458(4) . ? Sn1 Se1 2.471(5) . ? Sn1 Se3 2.581(4) 3_656 ? Sn1 Se3 2.588(5) . ? Nd1 O1 2.34(4) 3_655 ? Nd1 O1 2.35(3) . ? Nd1 N4 2.60(4) . ? Nd1 N1 2.61(3) . ? Nd1 N6 2.64(3) . ? Nd1 N5 2.64(3) . ? Nd1 N3 2.65(3) . ? Nd1 N2 2.66(4) . ? Nd1 Nd1 3.878(4) 3_655 ? Se3 Sn1 2.581(4) 3_656 ? N1 C1 1.45(5) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.50(5) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 C3 1.37(6) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C4 1.50(5) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N5 C5A 1.49(2) . ? N5 C5B 1.49(2) . ? N6 C6 1.44(6) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? C1 C2 1.54(6) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.51(6) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C5A C6 1.51(2) . ? C5B C6 1.51(2) . ? O1 Nd1 2.34(4) 3_655 ? O1 H1 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 Sn1 Se1 111.24(17) . . ? Se2 Sn1 Se3 110.69(18) . 3_656 ? Se1 Sn1 Se3 113.91(17) . 3_656 ? Se2 Sn1 Se3 113.51(18) . . ? Se1 Sn1 Se3 113.00(16) . . ? Se3 Sn1 Se3 93.42(14) 3_656 . ? O1 Nd1 O1 68.5(11) 3_655 . ? O1 Nd1 N4 100.6(11) 3_655 . ? O1 Nd1 N4 79.2(11) . . ? O1 Nd1 N1 152.5(10) 3_655 . ? O1 Nd1 N1 137.7(11) . . ? N4 Nd1 N1 81.0(12) . . ? O1 Nd1 N6 79.7(10) 3_655 . ? O1 Nd1 N6 136.9(12) . . ? N4 Nd1 N6 136.5(12) . . ? N1 Nd1 N6 80.6(12) . . ? O1 Nd1 N5 99.7(13) 3_655 . ? O1 Nd1 N5 92.3(12) . . ? N4 Nd1 N5 153.3(12) . . ? N1 Nd1 N5 88.9(13) . . ? N6 Nd1 N5 64.6(11) . . ? O1 Nd1 N3 80.7(11) 3_655 . ? O1 Nd1 N3 127.0(11) . . ? N4 Nd1 N3 64.9(11) . . ? N1 Nd1 N3 75.1(11) . . ? N6 Nd1 N3 72.3(12) . . ? N5 Nd1 N3 136.0(12) . . ? O1 Nd1 N2 142.6(10) 3_655 . ? O1 Nd1 N2 74.9(11) . . ? N4 Nd1 N2 79.4(11) . . ? N1 Nd1 N2 64.8(11) . . ? N6 Nd1 N2 125.8(11) . . ? N5 Nd1 N2 74.0(12) . . ? N3 Nd1 N2 129.7(11) . . ? O1 Nd1 Nd1 34.3(7) 3_655 3_655 ? O1 Nd1 Nd1 34.1(8) . 3_655 ? N4 Nd1 Nd1 89.9(8) . 3_655 ? N1 Nd1 Nd1 169.7(9) . 3_655 ? N6 Nd1 Nd1 109.6(9) . 3_655 ? N5 Nd1 Nd1 97.2(10) . 3_655 ? N3 Nd1 Nd1 105.5(8) . 3_655 ? N2 Nd1 Nd1 108.8(8) . 3_655 ? Sn1 Se3 Sn1 86.58(14) 3_656 . ? C1 N1 Nd1 114(2) . . ? C1 N1 H1A 108.8 . . ? Nd1 N1 H1A 108.8 . . ? C1 N1 H1B 108.8 . . ? Nd1 N1 H1B 108.8 . . ? H1A N1 H1B 107.7 . . ? C2 N2 Nd1 116(2) . . ? C2 N2 H2A 108.3 . . ? Nd1 N2 H2A 108.3 . . ? C2 N2 H2B 108.3 . . ? Nd1 N2 H2B 108.3 . . ? H2A N2 H2B 107.4 . . ? C3 N3 Nd1 117(3) . . ? C3 N3 H3A 108.0 . . ? Nd1 N3 H3A 108.0 . . ? C3 N3 H3B 108.0 . . ? Nd1 N3 H3B 108.0 . . ? H3A N3 H3B 107.3 . . ? C4 N4 Nd1 108(3) . . ? C4 N4 H4A 110.0 . . ? Nd1 N4 H4A 110.0 . . ? C4 N4 H4B 110.0 . . ? Nd1 N4 H4B 110.0 . . ? H4A N4 H4B 108.4 . . ? C5A N5 C5B 33(5) . . ? C5A N5 Nd1 118(4) . . ? C5B N5 Nd1 113(3) . . ? C6 N6 Nd1 121(2) . . ? C6 N6 H6A 107.2 . . ? Nd1 N6 H6A 107.2 . . ? C6 N6 H6B 107.2 . . ? Nd1 N6 H6B 107.2 . . ? H6A N6 H6B 106.8 . . ? N1 C1 C2 109(4) . . ? N1 C1 H1C 109.8 . . ? C2 C1 H1C 109.8 . . ? N1 C1 H1D 109.8 . . ? C2 C1 H1D 109.8 . . ? H1C C1 H1D 108.3 . . ? N2 C2 C1 108(3) . . ? N2 C2 H2C 110.0 . . ? C1 C2 H2C 110.0 . . ? N2 C2 H2D 110.0 . . ? C1 C2 H2D 110.0 . . ? H2C C2 H2D 108.4 . . ? N3 C3 C4 113(4) . . ? N3 C3 H3C 109.0 . . ? C4 C3 H3C 109.0 . . ? N3 C3 H3D 109.0 . . ? C4 C3 H3D 109.0 . . ? H3C C3 H3D 107.8 . . ? N4 C4 C3 109(4) . . ? N4 C4 H4C 109.9 . . ? C3 C4 H4C 109.9 . . ? N4 C4 H4D 109.9 . . ? C3 C4 H4D 109.9 . . ? H4C C4 H4D 108.3 . . ? N5 C5A C6 115(4) . . ? N5 C5B C6 114(4) . . ? N6 C6 C5B 111(4) . . ? N6 C6 C5A 116(4) . . ? C5B C6 C5A 32(4) . . ? Nd1 O1 Nd1 111.5(11) 3_655 . ? Nd1 O1 H1 124.2 3_655 . ? Nd1 O1 H1 124.2 . . ? 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 Se3 Sn1 -114.32(19) . . . 3_656 ? Se1 Sn1 Se3 Sn1 117.81(18) . . . 3_656 ? Se3 Sn1 Se3 Sn1 0.0 3_656 . . 3_656 ? O1 Nd1 N1 C1 156(3) 3_655 . . . ? O1 Nd1 N1 C1 -45(4) . . . . ? N4 Nd1 N1 C1 -108(3) . . . . ? N6 Nd1 N1 C1 112(3) . . . . ? N5 Nd1 N1 C1 47(3) . . . . ? N3 Nd1 N1 C1 -174(3) . . . . ? N2 Nd1 N1 C1 -26(3) . . . . ? Nd1 Nd1 N1 C1 -79(5) 3_655 . . . ? O1 Nd1 N2 C2 173(3) 3_655 . . . ? O1 Nd1 N2 C2 161(3) . . . . ? N4 Nd1 N2 C2 79(3) . . . . ? N1 Nd1 N2 C2 -6(3) . . . . ? N6 Nd1 N2 C2 -62(3) . . . . ? N5 Nd1 N2 C2 -102(3) . . . . ? N3 Nd1 N2 C2 35(4) . . . . ? Nd1 Nd1 N2 C2 165(3) 3_655 . . . ? O1 Nd1 N3 C3 -101(3) 3_655 . . . ? O1 Nd1 N3 C3 -47(4) . . . . ? N4 Nd1 N3 C3 5(3) . . . . ? N1 Nd1 N3 C3 92(3) . . . . ? N6 Nd1 N3 C3 177(3) . . . . ? N5 Nd1 N3 C3 164(3) . . . . ? N2 Nd1 N3 C3 54(4) . . . . ? Nd1 Nd1 N3 C3 -77(3) 3_655 . . . ? O1 Nd1 N4 C4 43(3) 3_655 . . . ? O1 Nd1 N4 C4 108(3) . . . . ? N1 Nd1 N4 C4 -110(3) . . . . ? N6 Nd1 N4 C4 -44(3) . . . . ? N5 Nd1 N4 C4 -179(3) . . . . ? N3 Nd1 N4 C4 -32(2) . . . . ? N2 Nd1 N4 C4 -175(3) . . . . ? Nd1 Nd1 N4 C4 75(2) 3_655 . . . ? O1 Nd1 N5 C5A -59(6) 3_655 . . . ? O1 Nd1 N5 C5A -127(6) . . . . ? N4 Nd1 N5 C5A 162(6) . . . . ? N1 Nd1 N5 C5A 95(6) . . . . ? N6 Nd1 N5 C5A 15(6) . . . . ? N3 Nd1 N5 C5A 28(7) . . . . ? N2 Nd1 N5 C5A 159(6) . . . . ? Nd1 Nd1 N5 C5A -93(6) 3_655 . . . ? O1 Nd1 N5 C5B -95(4) 3_655 . . . ? O1 Nd1 N5 C5B -163(4) . . . . ? N4 Nd1 N5 C5B 126(4) . . . . ? N1 Nd1 N5 C5B 59(4) . . . . ? N6 Nd1 N5 C5B -21(4) . . . . ? N3 Nd1 N5 C5B -8(5) . . . . ? N2 Nd1 N5 C5B 123(4) . . . . ? Nd1 Nd1 N5 C5B -129(4) 3_655 . . . ? O1 Nd1 N6 C6 104(3) 3_655 . . . ? O1 Nd1 N6 C6 62(4) . . . . ? N4 Nd1 N6 C6 -161(3) . . . . ? N1 Nd1 N6 C6 -95(3) . . . . ? N5 Nd1 N6 C6 -2(3) . . . . ? N3 Nd1 N6 C6 -172(3) . . . . ? N2 Nd1 N6 C6 -46(4) . . . . ? Nd1 Nd1 N6 C6 87(3) 3_655 . . . ? Nd1 N1 C1 C2 54(4) . . . . ? Nd1 N2 C2 C1 34(5) . . . . ? N1 C1 C2 N2 -57(5) . . . . ? Nd1 N3 C3 C4 23(5) . . . . ? Nd1 N4 C4 C3 57(4) . . . . ? N3 C3 C4 N4 -54(5) . . . . ? C5B N5 C5A C6 63(5) . . . . ? Nd1 N5 C5A C6 -27(11) . . . . ? C5A N5 C5B C6 -63(5) . . . . ? Nd1 N5 C5B C6 43(7) . . . . ? Nd1 N6 C6 C5B 24(5) . . . . ? Nd1 N6 C6 C5A -11(7) . . . . ? N5 C5B C6 N6 -44(8) . . . . ? N5 C5B C6 C5A 63(5) . . . . ? N5 C5A C6 N6 25(11) . . . . ? N5 C5A C6 C5B -63(5) . . . . ? O1 Nd1 O1 Nd1 0.0 3_655 . . 3_655 ? N4 Nd1 O1 Nd1 -106.0(15) . . . 3_655 ? N1 Nd1 O1 Nd1 -169.6(13) . . . 3_655 ? N6 Nd1 O1 Nd1 45(2) . . . 3_655 ? N5 Nd1 O1 Nd1 99.5(15) . . . 3_655 ? N3 Nd1 O1 Nd1 -59.1(19) . . . 3_655 ? N2 Nd1 O1 Nd1 172.2(17) . . . 3_655 ? 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 Se2 0.91 2.84 3.70(4) 158.7 4_665 N1 H1B Se1 0.91 2.68 3.59(4) 177.6 2_655 N2 H2A Se1 0.91 2.78 3.59(4) 148.0 . N2 H2B Se2 0.91 2.67 3.56(4) 164.8 2_645 N4 H4A Se2 0.91 2.65 3.55(4) 169.9 4_665 N4 H4B Se2 0.91 2.64 3.44(4) 146.2 2_645 N6 H6A Se1 0.91 2.70 3.55(4) 156.4 2_655 N6 H6B Se1 0.91 2.93 3.67(3) 139.4 4_565 O1 H1 Se2 0.94 2.93 3.59(3) 128.6 2_645 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.301 _refine_diff_density_min -1.643 _refine_diff_density_rms 0.349 #===END data_complex_1d _database_code_depnum_ccdc_archive 'CCDC 797228' #TrackingRef 'cif-of-1a-2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H50 Gd2 N12 O2 Se6 Sn2' _chemical_formula_sum 'C12 H50 Gd2 N12 O2 Se6 Sn2' _chemical_formula_weight 1420.28 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' Gd Gd -0.1653 3.9035 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9927(13) _cell_length_b 11.8421(15) _cell_length_c 15.313(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.979(3) _cell_angle_gamma 90.00 _cell_volume 1784.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6936 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 11.201 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2518 _exptl_absorpt_correction_T_max 0.4005 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17044 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3259 _reflns_number_gt 3023 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0255P)^2^+6.4696P] 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_number_reflns 3259 _refine_ls_number_parameters 173 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.88666(4) 0.90687(3) 0.54023(3) 0.01282(11) Uani 1 1 d . . . Se1 Se 0.90101(7) 0.70038(5) 0.52627(5) 0.02420(17) Uani 1 1 d . . . Se2 Se 0.69508(6) 0.96250(5) 0.61264(4) 0.01893(15) Uani 1 1 d . . . Se3 Se 0.88547(6) 1.00127(5) 0.38834(4) 0.01842(15) Uani 1 1 d . . . Gd1 Gd 0.37764(3) 0.61771(2) 0.454199(18) 0.01262(9) Uani 1 1 d . . . N1 N 0.3777(6) 0.7572(5) 0.5861(4) 0.0260(13) Uani 1 1 d . . . H1A H 0.4646 0.7620 0.6178 0.031 Uiso 1 1 calc R . . H1B H 0.3535 0.8278 0.5637 0.031 Uiso 1 1 calc R . . N2 N 0.2194(5) 0.5587(4) 0.5583(3) 0.0202(11) Uani 1 1 d . . . H2A H 0.1343 0.5881 0.5387 0.024 Uiso 1 1 calc R . . H2B H 0.2122 0.4813 0.5584 0.024 Uiso 1 1 calc R . . N3 N 0.1847(5) 0.7566(4) 0.4013(3) 0.0178(11) Uani 1 1 d . . . H3A H 0.1307 0.7618 0.4440 0.021 Uiso 1 1 calc R . . H3B H 0.2215 0.8269 0.3955 0.021 Uiso 1 1 calc R . . N4 N 0.1762(5) 0.5309(4) 0.3433(3) 0.0164(11) Uani 1 1 d . . . H4A H 0.2072 0.5119 0.2921 0.020 Uiso 1 1 calc R . . H4B H 0.1496 0.4653 0.3675 0.020 Uiso 1 1 calc R . . N5 N 0.5160(6) 0.7941(4) 0.4284(3) 0.0246(13) Uani 1 1 d . . . H5A H 0.4669 0.8567 0.4394 0.029 Uiso 1 1 calc R . . H5B H 0.5946 0.7938 0.4698 0.029 Uiso 1 1 calc R . . N6 N 0.4477(6) 0.6235(4) 0.2999(4) 0.0257(13) Uani 1 1 d D . . O1 O 0.4180(4) 0.4254(3) 0.4585(3) 0.0203(9) Uani 1 1 d . . . H1 H 0.3576 0.3709 0.4280 0.024 Uiso 1 1 calc R . . C1 C 0.2855(7) 0.7248(6) 0.6468(4) 0.0270(15) Uani 1 1 d . . . H1C H 0.1954 0.7599 0.6270 0.032 Uiso 1 1 calc R . . H1D H 0.3218 0.7529 0.7071 0.032 Uiso 1 1 calc R . . C2 C 0.2701(8) 0.5988(6) 0.6492(4) 0.0272(16) Uani 1 1 d . . . H2C H 0.3589 0.5633 0.6723 0.033 Uiso 1 1 calc R . . H2D H 0.2054 0.5780 0.6886 0.033 Uiso 1 1 calc R . . C3 C 0.0984(7) 0.7257(5) 0.3160(4) 0.0228(14) Uani 1 1 d . . . H3C H 0.1500 0.7360 0.2669 0.027 Uiso 1 1 calc R . . H3D H 0.0175 0.7753 0.3048 0.027 Uiso 1 1 calc R . . C4 C 0.0548(7) 0.6049(5) 0.3195(4) 0.0219(14) Uani 1 1 d . . . H4C H -0.0053 0.5964 0.3641 0.026 Uiso 1 1 calc R . . H4D H 0.0030 0.5822 0.2611 0.026 Uiso 1 1 calc R . . C5 C 0.5533(9) 0.8076(6) 0.3411(5) 0.043(2) Uani 1 1 d D . . C6A C 0.5653(9) 0.6963(7) 0.2974(6) 0.032(2) Uani 0.72 1 d PD . . H6A1 H 0.5747 0.7091 0.2348 0.039 Uiso 0.72 1 calc PR . . H6A2 H 0.6484 0.6575 0.3273 0.039 Uiso 0.72 1 calc PR . . C6B C 0.461(2) 0.7424(9) 0.2705(10) 0.028(6) Uani 0.28 1 d PD . . H6B1 H 0.3707 0.7786 0.2586 0.034 Uiso 0.28 1 calc PR . . H6B2 H 0.4993 0.7431 0.2150 0.034 Uiso 0.28 1 calc 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 0.0153(2) 0.0108(2) 0.0131(2) 0.00098(15) 0.00428(16) -0.00154(15) Se1 0.0242(4) 0.0106(3) 0.0406(4) 0.0005(3) 0.0135(3) -0.0017(3) Se2 0.0191(4) 0.0205(3) 0.0188(3) -0.0010(2) 0.0076(3) 0.0002(2) Se3 0.0202(4) 0.0211(3) 0.0130(3) 0.0035(2) 0.0003(2) -0.0056(3) Gd1 0.01324(17) 0.01234(15) 0.01225(16) 0.00011(11) 0.00208(11) -0.00005(11) N1 0.020(3) 0.030(3) 0.028(3) -0.014(2) 0.005(2) -0.002(2) N2 0.023(3) 0.017(3) 0.022(3) 0.001(2) 0.009(2) 0.002(2) N3 0.021(3) 0.013(2) 0.019(3) -0.002(2) 0.002(2) -0.003(2) N4 0.017(3) 0.016(3) 0.017(3) 0.001(2) 0.005(2) -0.002(2) N5 0.028(3) 0.023(3) 0.022(3) 0.000(2) 0.002(2) -0.007(2) N6 0.031(3) 0.027(3) 0.021(3) -0.003(2) 0.011(3) -0.006(2) O1 0.019(2) 0.018(2) 0.022(2) -0.0032(18) -0.0010(19) -0.0003(18) C1 0.029(4) 0.030(4) 0.021(3) -0.003(3) 0.000(3) 0.007(3) C2 0.035(4) 0.033(4) 0.013(3) 0.003(3) 0.004(3) 0.007(3) C3 0.025(4) 0.021(3) 0.021(3) 0.000(3) 0.001(3) 0.006(3) C4 0.017(3) 0.029(4) 0.019(3) 0.000(3) 0.001(3) 0.001(3) C5 0.072(6) 0.030(4) 0.040(4) -0.007(3) 0.043(4) -0.012(4) C6A 0.038(7) 0.037(6) 0.025(5) -0.007(4) 0.014(5) -0.018(5) C6B 0.026(15) 0.039(14) 0.026(13) 0.007(11) 0.013(11) 0.015(12) _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 2.4609(8) . ? Sn1 Se2 2.4626(8) . ? Sn1 Se3 2.5787(8) . ? Sn1 Se3 2.5887(8) 3_776 ? Se3 Sn1 2.5887(8) 3_776 ? Gd1 O1 2.295(4) 3_666 ? Gd1 O1 2.312(4) . ? Gd1 N2 2.530(5) . ? Gd1 N3 2.557(5) . ? Gd1 N5 2.573(5) . ? Gd1 N6 2.579(5) . ? Gd1 N4 2.609(5) . ? Gd1 N1 2.609(5) . ? Gd1 Gd1 3.8119(6) 3_666 ? N1 C1 1.468(9) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C2 1.475(8) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C3 1.481(8) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N4 C4 1.490(8) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? N5 C5 1.458(8) . ? N5 H5A 0.9200 . ? N5 H5B 0.9200 . ? N6 C6A 1.463(7) . ? N6 C6B 1.491(9) . ? O1 Gd1 2.295(4) 3_666 ? O1 H1 0.9500 . ? C1 C2 1.501(9) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 C4 1.499(9) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? C5 C6A 1.493(8) . ? C5 C6B 1.505(10) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? 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 111.50(3) . . ? Se1 Sn1 Se3 110.10(3) . . ? Se2 Sn1 Se3 114.06(3) . . ? Se1 Sn1 Se3 113.21(3) . 3_776 ? Se2 Sn1 Se3 113.13(3) . 3_776 ? Se3 Sn1 Se3 93.74(2) . 3_776 ? Sn1 Se3 Sn1 86.26(2) . 3_776 ? O1 Gd1 O1 68.36(17) 3_666 . ? O1 Gd1 N2 99.31(16) 3_666 . ? O1 Gd1 N2 80.50(16) . . ? O1 Gd1 N3 150.83(15) 3_666 . ? O1 Gd1 N3 139.57(15) . . ? N2 Gd1 N3 81.85(17) . . ? O1 Gd1 N5 79.77(16) 3_666 . ? O1 Gd1 N5 135.11(17) . . ? N2 Gd1 N5 137.03(17) . . ? N3 Gd1 N5 79.90(17) . . ? O1 Gd1 N6 100.61(17) 3_666 . ? O1 Gd1 N6 88.78(15) . . ? N2 Gd1 N6 151.99(17) . . ? N3 Gd1 N6 90.10(17) . . ? N5 Gd1 N6 66.40(16) . . ? O1 Gd1 N4 143.08(15) 3_666 . ? O1 Gd1 N4 75.03(15) . . ? N2 Gd1 N4 78.76(16) . . ? N3 Gd1 N4 65.97(15) . . ? N5 Gd1 N4 126.49(16) . . ? N6 Gd1 N4 73.47(16) . . ? O1 Gd1 N1 78.99(16) 3_666 . ? O1 Gd1 N1 128.67(16) . . ? N2 Gd1 N1 66.64(17) . . ? N3 Gd1 N1 74.76(17) . . ? N5 Gd1 N1 71.13(17) . . ? N6 Gd1 N1 136.78(17) . . ? N4 Gd1 N1 130.53(16) . . ? O1 Gd1 Gd1 34.32(10) 3_666 3_666 ? O1 Gd1 Gd1 34.04(10) . 3_666 ? N2 Gd1 Gd1 89.85(12) . 3_666 ? N3 Gd1 Gd1 170.94(12) . 3_666 ? N5 Gd1 Gd1 108.83(13) . 3_666 ? N6 Gd1 Gd1 95.62(13) . 3_666 ? N4 Gd1 Gd1 108.95(11) . 3_666 ? N1 Gd1 Gd1 105.31(13) . 3_666 ? C1 N1 Gd1 114.1(4) . . ? C1 N1 H1A 108.7 . . ? Gd1 N1 H1A 108.7 . . ? C1 N1 H1B 108.7 . . ? Gd1 N1 H1B 108.7 . . ? H1A N1 H1B 107.6 . . ? C2 N2 Gd1 110.8(4) . . ? C2 N2 H2A 109.5 . . ? Gd1 N2 H2A 109.5 . . ? C2 N2 H2B 109.5 . . ? Gd1 N2 H2B 109.5 . . ? H2A N2 H2B 108.1 . . ? C3 N3 Gd1 114.3(3) . . ? C3 N3 H3A 108.7 . . ? Gd1 N3 H3A 108.7 . . ? C3 N3 H3B 108.7 . . ? Gd1 N3 H3B 108.7 . . ? H3A N3 H3B 107.6 . . ? C4 N4 Gd1 115.6(3) . . ? C4 N4 H4A 108.4 . . ? Gd1 N4 H4A 108.4 . . ? C4 N4 H4B 108.4 . . ? Gd1 N4 H4B 108.4 . . ? H4A N4 H4B 107.5 . . ? C5 N5 Gd1 117.3(4) . . ? C5 N5 H5A 108.0 . . ? Gd1 N5 H5A 108.0 . . ? C5 N5 H5B 108.0 . . ? Gd1 N5 H5B 108.0 . . ? H5A N5 H5B 107.2 . . ? C6A N6 C6B 47.2(8) . . ? C6A N6 Gd1 112.7(4) . . ? C6B N6 Gd1 110.8(8) . . ? Gd1 O1 Gd1 111.64(17) 3_666 . ? Gd1 O1 H1 124.2 3_666 . ? Gd1 O1 H1 124.2 . . ? N1 C1 C2 110.7(5) . . ? N1 C1 H1C 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? C2 C1 H1D 109.5 . . ? H1C C1 H1D 108.1 . . ? N2 C2 C1 108.5(5) . . ? N2 C2 H2C 110.0 . . ? C1 C2 H2C 110.0 . . ? N2 C2 H2D 110.0 . . ? C1 C2 H2D 110.0 . . ? H2C C2 H2D 108.4 . . ? N3 C3 C4 109.4(5) . . ? N3 C3 H3C 109.8 . . ? C4 C3 H3C 109.8 . . ? N3 C3 H3D 109.8 . . ? C4 C3 H3D 109.8 . . ? H3C C3 H3D 108.2 . . ? N4 C4 C3 109.9(5) . . ? N4 C4 H4C 109.7 . . ? C3 C4 H4C 109.7 . . ? N4 C4 H4D 109.7 . . ? C3 C4 H4D 109.7 . . ? H4C C4 H4D 108.2 . . ? N5 C5 C6A 111.6(6) . . ? N5 C5 C6B 112.4(9) . . ? C6A C5 C6B 46.4(8) . . ? N6 C6A C5 112.4(7) . . ? N6 C6A H6A1 109.1 . . ? C5 C6A H6A1 109.1 . . ? N6 C6A H6A2 109.1 . . ? C5 C6A H6A2 109.1 . . ? H6A1 C6A H6A2 107.9 . . ? N6 C6B C5 110.2(8) . . ? N6 C6B H6B1 109.6 . . ? C5 C6B H6B1 109.6 . . ? N6 C6B H6B2 109.6 . . ? C5 C6B H6B2 109.6 . . ? H6B1 C6B H6B2 108.1 . . ? 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 Se1 Sn1 Se3 Sn1 -116.38(3) . . . 3_776 ? Se2 Sn1 Se3 Sn1 117.40(3) . . . 3_776 ? Se3 Sn1 Se3 Sn1 0.0 3_776 . . 3_776 ? O1 Gd1 N1 C1 -105.8(4) 3_666 . . . ? O1 Gd1 N1 C1 -55.4(5) . . . . ? N2 Gd1 N1 C1 -0.5(4) . . . . ? N3 Gd1 N1 C1 87.1(4) . . . . ? N5 Gd1 N1 C1 171.4(5) . . . . ? N6 Gd1 N1 C1 160.4(4) . . . . ? N4 Gd1 N1 C1 49.1(5) . . . . ? Gd1 Gd1 N1 C1 -83.6(4) 3_666 . . . ? O1 Gd1 N2 C2 44.2(4) 3_666 . . . ? O1 Gd1 N2 C2 110.2(4) . . . . ? N3 Gd1 N2 C2 -106.3(4) . . . . ? N5 Gd1 N2 C2 -40.8(5) . . . . ? N6 Gd1 N2 C2 179.1(4) . . . . ? N4 Gd1 N2 C2 -173.3(4) . . . . ? N1 Gd1 N2 C2 -29.4(4) . . . . ? Gd1 Gd1 N2 C2 77.3(4) 3_666 . . . ? O1 Gd1 N3 C3 161.8(4) 3_666 . . . ? O1 Gd1 N3 C3 -38.8(5) . . . . ? N2 Gd1 N3 C3 -103.7(4) . . . . ? N5 Gd1 N3 C3 115.4(4) . . . . ? N6 Gd1 N3 C3 49.4(4) . . . . ? N4 Gd1 N3 C3 -22.4(4) . . . . ? N1 Gd1 N3 C3 -171.6(4) . . . . ? Gd1 Gd1 N3 C3 -79.9(8) 3_666 . . . ? O1 Gd1 N4 C4 169.5(4) 3_666 . . . ? O1 Gd1 N4 C4 161.9(4) . . . . ? N2 Gd1 N4 C4 78.9(4) . . . . ? N3 Gd1 N4 C4 -7.1(4) . . . . ? N5 Gd1 N4 C4 -62.5(4) . . . . ? N6 Gd1 N4 C4 -104.8(4) . . . . ? N1 Gd1 N4 C4 33.4(5) . . . . ? Gd1 Gd1 N4 C4 164.8(4) 3_666 . . . ? O1 Gd1 N5 C5 109.8(5) 3_666 . . . ? O1 Gd1 N5 C5 65.3(6) . . . . ? N2 Gd1 N5 C5 -157.4(5) . . . . ? N3 Gd1 N5 C5 -91.2(5) . . . . ? N6 Gd1 N5 C5 3.4(5) . . . . ? N4 Gd1 N5 C5 -41.4(6) . . . . ? N1 Gd1 N5 C5 -168.4(6) . . . . ? Gd1 Gd1 N5 C5 91.3(5) 3_666 . . . ? O1 Gd1 N6 C6A -51.7(5) 3_666 . . . ? O1 Gd1 N6 C6A -119.4(5) . . . . ? N2 Gd1 N6 C6A 173.7(5) . . . . ? N3 Gd1 N6 C6A 101.1(5) . . . . ? N5 Gd1 N6 C6A 22.1(5) . . . . ? N4 Gd1 N6 C6A 165.9(6) . . . . ? N1 Gd1 N6 C6A 33.5(6) . . . . ? Gd1 Gd1 N6 C6A -86.0(5) 3_666 . . . ? O1 Gd1 N6 C6B -102.6(8) 3_666 . . . ? O1 Gd1 N6 C6B -170.3(8) . . . . ? N2 Gd1 N6 C6B 122.7(8) . . . . ? N3 Gd1 N6 C6B 50.1(8) . . . . ? N5 Gd1 N6 C6B -28.8(8) . . . . ? N4 Gd1 N6 C6B 114.9(8) . . . . ? N1 Gd1 N6 C6B -17.5(8) . . . . ? Gd1 Gd1 N6 C6B -137.0(8) 3_666 . . . ? O1 Gd1 O1 Gd1 0.0 3_666 . . 3_666 ? N2 Gd1 O1 Gd1 -104.1(2) . . . 3_666 ? N3 Gd1 O1 Gd1 -169.35(18) . . . 3_666 ? N5 Gd1 O1 Gd1 48.0(3) . . . 3_666 ? N6 Gd1 O1 Gd1 101.9(2) . . . 3_666 ? N4 Gd1 O1 Gd1 175.1(2) . . . 3_666 ? N1 Gd1 O1 Gd1 -54.5(3) . . . 3_666 ? Gd1 N1 C1 C2 29.8(7) . . . . ? Gd1 N2 C2 C1 57.2(6) . . . . ? N1 C1 C2 N2 -57.7(7) . . . . ? Gd1 N3 C3 C4 49.8(6) . . . . ? Gd1 N4 C4 C3 34.9(6) . . . . ? N3 C3 C4 N4 -55.0(7) . . . . ? Gd1 N5 C5 C6A -27.8(9) . . . . ? Gd1 N5 C5 C6B 22.5(10) . . . . ? C6B N6 C6A C5 51.7(10) . . . . ? Gd1 N6 C6A C5 -46.1(9) . . . . ? N5 C5 C6A N6 49.1(11) . . . . ? C6B C5 C6A N6 -51.9(10) . . . . ? C6A N6 C6B C5 -50.0(9) . . . . ? Gd1 N6 C6B C5 52.2(15) . . . . ? N5 C5 C6B N6 -49.6(16) . . . . ? C6A C5 C6B N6 49.5(9) . . . . ? 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 N2 H2A Se1 0.92 2.66 3.555(5) 164.0 1_455 N2 H2B Se1 0.92 2.66 3.464(5) 146.3 3_666 N3 H3A Se1 0.92 2.90 3.745(5) 154.2 1_455 N3 H3B Se2 0.92 2.64 3.555(5) 173.6 3_676 N4 H4A Se2 0.92 2.75 3.571(5) 149.7 4_575 N4 H4B Se1 0.92 2.65 3.552(5) 166.2 3_666 N5 H5A Se2 0.92 2.72 3.562(6) 152.9 3_676 O1 H1 Se1 0.95 2.92 3.563(4) 126.3 3_666 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.085 _refine_diff_density_min -1.327 _refine_diff_density_rms 0.171 #===END data_complex_2a _database_code_depnum_ccdc_archive 'CCDC 797229' #TrackingRef 'cif-of-1a-2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H104 Ce4 N24 Se15 Sn4' _chemical_formula_sum 'C32 H104 Ce4 N24 Se15 Sn4' _chemical_formula_weight 3045.04 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' Sn Sn -0.6537 1.4246 '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' Ce Ce -0.2486 2.6331 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2333(6) _cell_length_b 13.0790(9) _cell_length_c 15.7663(9) _cell_angle_alpha 80.422(4) _cell_angle_beta 73.738(3) _cell_angle_gamma 88.376(4) _cell_volume 1997.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9004 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1406 _exptl_absorpt_coefficient_mu 10.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1475 _exptl_absorpt_correction_T_max 0.3063 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15815 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6986 _reflns_number_gt 5329 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0235P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6986 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _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 0.86473(5) 0.03013(5) 0.08947(4) 0.02443(15) Uani 1 1 d . . . Sn2 Sn 0.28318(5) 0.40198(5) 0.32753(4) 0.02251(15) Uani 1 1 d . . . Ce1 Ce 0.42003(4) 0.19155(4) 0.17162(3) 0.02259(13) Uani 1 1 d . . . Ce2 Ce 0.16625(4) 0.41564(4) 0.62275(3) 0.02459(13) Uani 1 1 d . . . Se1 Se 0.62231(7) -0.00555(8) 0.10032(6) 0.0325(2) Uani 1 1 d . . . Se2 Se 0.90671(8) 0.12076(8) 0.20332(6) 0.0337(2) Uani 1 1 d . . . Se3 Se 1.01114(8) -0.13112(7) 0.06923(6) 0.0307(2) Uani 1 1 d . . . Se4 Se 0.45879(8) 0.43250(7) 0.18049(5) 0.0291(2) Uani 1 1 d . . . Se5 Se 0.15090(7) 0.24556(7) 0.32731(6) 0.0275(2) Uani 1 1 d . . . Se6 Se 0.38904(7) 0.36597(7) 0.45518(5) 0.0246(2) Uani 1 1 d . . . Se7 Se 0.15878(8) 0.57479(8) 0.33630(6) 0.0306(2) Uani 1 1 d . . . Se8 Se 0.0000 0.5000 0.5000 0.0310(3) Uani 1 2 d S . . N1 N 0.5425(6) 0.1793(6) 0.3026(5) 0.0299(19) Uani 1 1 d . . . H1A H 0.6339 0.1845 0.2764 0.036 Uiso 1 1 calc R . . H1B H 0.5186 0.2360 0.3297 0.036 Uiso 1 1 calc R . . N2 N 0.3709(6) 0.0199(6) 0.2955(4) 0.0285(18) Uani 1 1 d . . . H2 H 0.4423 -0.0225 0.2757 0.034 Uiso 1 1 calc R . . N3 N 0.2644(6) 0.0433(6) 0.1458(5) 0.0318(19) Uani 1 1 d . . . H3A H 0.1784 0.0673 0.1526 0.038 Uiso 1 1 calc R . . H3B H 0.2972 0.0319 0.0883 0.038 Uiso 1 1 calc R . . N4 N 0.2250(6) 0.2846(6) 0.1038(4) 0.0318(18) Uani 1 1 d . . . H4A H 0.1469 0.2460 0.1284 0.038 Uiso 1 1 calc R . . H4B H 0.2096 0.3475 0.1220 0.038 Uiso 1 1 calc R . . N5 N 0.4822(7) 0.2338(6) -0.0095(5) 0.039(2) Uani 1 1 d . . . H5 H 0.4567 0.1766 -0.0286 0.046 Uiso 1 1 calc R . . N6 N 0.6719(6) 0.2728(6) 0.0879(5) 0.038(2) Uani 1 1 d . . . H6A H 0.6904 0.3204 0.1191 0.046 Uiso 1 1 calc R . . H6B H 0.7335 0.2213 0.0890 0.046 Uiso 1 1 calc R . . N7 N 0.2886(6) 0.5899(6) 0.5269(4) 0.0260(17) Uani 1 1 d . . . H7A H 0.3784 0.5865 0.5246 0.031 Uiso 1 1 calc R . . H7B H 0.2827 0.5940 0.4699 0.031 Uiso 1 1 calc R . . N8 N 0.1164(6) 0.5851(6) 0.7032(4) 0.0260(17) Uani 1 1 d . . . H8 H 0.0332 0.6084 0.6974 0.031 Uiso 1 1 calc R . . N9 N 0.0603(8) 0.3788(7) 0.8050(5) 0.050(2) Uani 1 1 d . . . H9A H -0.0077 0.3301 0.8197 0.060 Uiso 1 1 calc R . . H9B H 0.1264 0.3522 0.8302 0.060 Uiso 1 1 calc R . . N10 N 0.3926(6) 0.4208(6) 0.6800(5) 0.0331(19) Uani 1 1 d . . . H10A H 0.4615 0.4521 0.6336 0.040 Uiso 1 1 calc R . . H10B H 0.3758 0.4607 0.7239 0.040 Uiso 1 1 calc R . . N11 N 0.2620(7) 0.2268(6) 0.6789(5) 0.038(2) Uani 1 1 d . . . H11 H 0.2160 0.2085 0.7385 0.046 Uiso 1 1 calc R . . N12 N 0.0608(6) 0.2476(6) 0.5822(5) 0.035(2) Uani 1 1 d . . . H12A H -0.0314 0.2528 0.5973 0.042 Uiso 1 1 calc R . . H12B H 0.0904 0.2498 0.5218 0.042 Uiso 1 1 calc R . . C1 C 0.5172(9) 0.0882(8) 0.3729(6) 0.042(3) Uani 1 1 d . . . H1C H 0.5180 0.1091 0.4297 0.050 Uiso 1 1 calc R . . H1D H 0.5903 0.0387 0.3579 0.050 Uiso 1 1 calc R . . C2 C 0.3808(9) 0.0359(9) 0.3841(6) 0.044(3) Uani 1 1 d . . . H2A H 0.3733 -0.0310 0.4240 0.052 Uiso 1 1 calc R . . H2B H 0.3063 0.0795 0.4110 0.052 Uiso 1 1 calc R . . C3 C 0.2510(8) -0.0392(7) 0.2996(6) 0.036(2) Uani 1 1 d . . . H3C H 0.1687 -0.0012 0.3237 0.043 Uiso 1 1 calc R . . H3D H 0.2477 -0.1060 0.3390 0.043 Uiso 1 1 calc R . . C4 C 0.2577(9) -0.0565(8) 0.2062(6) 0.039(2) Uani 1 1 d . . . H4C H 0.3383 -0.0969 0.1834 0.046 Uiso 1 1 calc R . . H4D H 0.1770 -0.0962 0.2079 0.046 Uiso 1 1 calc R . . C5 C 0.2517(10) 0.3010(9) 0.0054(6) 0.051(3) Uani 1 1 d . . . H5A H 0.2000 0.3602 -0.0139 0.061 Uiso 1 1 calc R . . H5B H 0.2232 0.2394 -0.0131 0.061 Uiso 1 1 calc R . . C6 C 0.4002(10) 0.3214(8) -0.0363(6) 0.048(3) Uani 1 1 d . . . H6C H 0.4188 0.3339 -0.1016 0.058 Uiso 1 1 calc R . . H6D H 0.4271 0.3841 -0.0184 0.058 Uiso 1 1 calc R . . C7 C 0.6297(10) 0.2521(9) -0.0529(6) 0.054(3) Uani 1 1 d . . . H7C H 0.6440 0.2846 -0.1155 0.065 Uiso 1 1 calc R . . H7D H 0.6764 0.1856 -0.0522 0.065 Uiso 1 1 calc R . . C8 C 0.6903(9) 0.3220(9) -0.0046(7) 0.052(3) Uani 1 1 d . . . H8A H 0.7875 0.3343 -0.0348 0.063 Uiso 1 1 calc R . . H8B H 0.6451 0.3891 -0.0061 0.063 Uiso 1 1 calc R . . C9 C 0.2343(9) 0.6865(7) 0.5598(6) 0.035(2) Uani 1 1 d . . . H9C H 0.2982 0.7445 0.5298 0.042 Uiso 1 1 calc R . . H9D H 0.1473 0.7027 0.5465 0.042 Uiso 1 1 calc R . . C10 C 0.2148(8) 0.6720(7) 0.6575(6) 0.030(2) Uani 1 1 d . . . H10C H 0.1804 0.7359 0.6800 0.036 Uiso 1 1 calc R . . H10D H 0.3022 0.6569 0.6704 0.036 Uiso 1 1 calc R . . C11 C 0.1006(8) 0.5625(8) 0.8010(5) 0.037(3) Uani 1 1 d . . . H11A H 0.0658 0.6238 0.8279 0.044 Uiso 1 1 calc R . . H11B H 0.1895 0.5467 0.8115 0.044 Uiso 1 1 calc R . . C12 C 0.0051(9) 0.4731(9) 0.8441(6) 0.054(3) Uani 1 1 d . . . H12C H -0.0842 0.4889 0.8341 0.064 Uiso 1 1 calc R . . H12D H -0.0064 0.4602 0.9088 0.064 Uiso 1 1 calc R . . C13 C 0.4388(10) 0.3172(9) 0.7152(8) 0.058(3) Uani 1 1 d . . . H13A H 0.5375 0.3208 0.7057 0.070 Uiso 1 1 calc R . . H13B H 0.3961 0.3016 0.7799 0.070 Uiso 1 1 calc R . . C14 C 0.4077(11) 0.2328(10) 0.6743(8) 0.066(3) Uani 1 1 d . . . H14A H 0.4338 0.1671 0.7048 0.079 Uiso 1 1 calc R . . H14B H 0.4618 0.2422 0.6115 0.079 Uiso 1 1 calc R . . C15 C 0.2352(10) 0.1445(9) 0.6345(8) 0.056(3) Uani 1 1 d . . . H15A H 0.2492 0.0775 0.6688 0.067 Uiso 1 1 calc R . . H15B H 0.3001 0.1509 0.5749 0.067 Uiso 1 1 calc R . . C16 C 0.0941(9) 0.1470(8) 0.6254(7) 0.048(3) Uani 1 1 d . . . H16A H 0.0840 0.0941 0.5902 0.057 Uiso 1 1 calc R . . H16B H 0.0295 0.1297 0.6850 0.057 Uiso 1 1 calc R . . 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 0.0175(3) 0.0277(4) 0.0291(3) -0.0125(3) -0.0035(2) 0.0008(2) Sn2 0.0163(3) 0.0298(4) 0.0229(3) -0.0110(3) -0.0042(2) 0.0023(2) Ce1 0.0191(2) 0.0253(3) 0.0238(3) -0.0076(2) -0.00459(19) 0.0002(2) Ce2 0.0198(2) 0.0238(3) 0.0317(3) -0.0099(2) -0.0068(2) 0.0023(2) Se1 0.0172(4) 0.0406(6) 0.0416(5) -0.0215(5) -0.0029(4) -0.0007(4) Se2 0.0269(4) 0.0421(7) 0.0372(5) -0.0230(5) -0.0080(4) 0.0027(4) Se3 0.0275(4) 0.0264(6) 0.0341(5) -0.0057(5) -0.0018(4) 0.0033(4) Se4 0.0295(4) 0.0287(6) 0.0251(5) -0.0087(4) 0.0015(4) -0.0011(4) Se5 0.0194(4) 0.0308(6) 0.0330(5) -0.0123(5) -0.0042(3) 0.0002(4) Se6 0.0201(4) 0.0327(6) 0.0231(4) -0.0090(4) -0.0069(3) 0.0023(4) Se7 0.0214(4) 0.0328(6) 0.0398(5) -0.0140(5) -0.0080(4) 0.0064(4) Se8 0.0228(6) 0.0348(9) 0.0401(7) -0.0114(7) -0.0136(5) 0.0045(6) N1 0.025(4) 0.031(5) 0.039(4) -0.016(4) -0.012(3) 0.005(3) N2 0.026(4) 0.028(5) 0.026(4) -0.009(4) 0.003(3) 0.003(3) N3 0.024(4) 0.039(5) 0.034(4) -0.015(4) -0.005(3) 0.001(3) N4 0.036(4) 0.026(5) 0.032(4) 0.003(4) -0.010(3) 0.000(3) N5 0.049(5) 0.036(5) 0.029(4) -0.013(4) -0.002(4) -0.004(4) N6 0.024(4) 0.031(5) 0.059(5) -0.020(5) -0.002(4) 0.003(3) N7 0.017(3) 0.037(5) 0.028(4) -0.013(4) -0.009(3) 0.003(3) N8 0.018(3) 0.028(5) 0.033(4) -0.011(4) -0.006(3) 0.002(3) N9 0.054(5) 0.044(6) 0.040(5) -0.003(5) 0.004(4) -0.003(4) N10 0.023(4) 0.044(6) 0.033(4) -0.009(4) -0.008(3) 0.002(3) N11 0.037(4) 0.033(5) 0.045(5) -0.005(4) -0.014(4) 0.011(4) N12 0.024(4) 0.034(5) 0.044(5) -0.008(4) -0.002(3) 0.002(3) C1 0.044(5) 0.046(7) 0.047(6) -0.011(6) -0.030(5) 0.008(5) C2 0.045(6) 0.054(8) 0.028(5) -0.001(5) -0.008(4) -0.003(5) C3 0.038(5) 0.014(5) 0.049(6) 0.002(5) -0.004(4) -0.013(4) C4 0.033(5) 0.032(7) 0.050(6) -0.006(5) -0.009(4) -0.012(4) C5 0.057(6) 0.053(8) 0.057(7) -0.013(6) -0.035(5) -0.003(6) C6 0.079(8) 0.038(7) 0.026(5) 0.007(5) -0.017(5) -0.007(6) C7 0.062(7) 0.054(8) 0.033(6) -0.017(6) 0.018(5) -0.011(6) C8 0.033(5) 0.048(8) 0.057(7) -0.011(6) 0.021(5) -0.003(5) C9 0.033(5) 0.029(6) 0.040(5) -0.003(5) -0.006(4) -0.001(4) C10 0.024(4) 0.019(5) 0.049(6) -0.016(5) -0.006(4) -0.007(4) C11 0.032(5) 0.055(7) 0.025(5) -0.016(5) -0.005(4) 0.001(5) C12 0.044(6) 0.074(9) 0.041(6) -0.028(7) 0.003(5) 0.001(6) C13 0.050(6) 0.057(9) 0.079(8) -0.018(7) -0.032(6) 0.008(6) C14 0.065(7) 0.049(9) 0.093(9) 0.001(7) -0.045(7) 0.007(6) C15 0.048(6) 0.035(7) 0.078(8) -0.007(6) -0.008(6) 0.009(5) C16 0.043(6) 0.033(7) 0.064(7) -0.010(6) -0.008(5) -0.008(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 Se2 2.4455(9) . ? Sn1 Se1 2.4905(9) . ? Sn1 Se3 2.5635(11) . ? Sn1 Se3 2.6142(11) 2_755 ? Sn2 Se4 2.4825(9) . ? Sn2 Se5 2.4860(10) . ? Sn2 Se6 2.5145(10) . ? Sn2 Se7 2.5671(11) . ? Ce1 N2 2.676(7) . ? Ce1 N1 2.682(6) . ? Ce1 N4 2.689(7) . ? Ce1 N3 2.695(6) . ? Ce1 N6 2.702(6) . ? Ce1 N5 2.710(7) . ? Ce1 Se4 3.2182(10) . ? Ce1 Se5 3.2847(8) . ? Ce1 Se1 3.3989(10) . ? Ce2 N7 2.647(7) . ? Ce2 N8 2.700(6) . ? Ce2 N10 2.717(6) . ? Ce2 N12 2.719(7) . ? Ce2 N11 2.732(8) . ? Ce2 N9 2.737(7) . ? Ce2 Se8 2.9806(5) . ? Ce2 Se6 3.1167(8) . ? Ce2 Se7 3.2088(9) 2_566 ? Se3 Sn1 2.6142(11) 2_755 ? Se7 Se8 2.6757(9) . ? Se7 Ce2 3.2088(9) 2_566 ? Se8 Se7 2.6757(9) 2_566 ? Se8 Ce2 2.9806(5) 2_566 ? N1 C1 1.460(12) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C3 1.449(9) . ? N2 C2 1.478(10) . ? N2 H2 0.9200 . ? N3 C4 1.472(12) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C5 1.477(11) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N5 C6 1.476(13) . ? N5 C7 1.481(11) . ? N5 H5 0.9200 . ? N6 C8 1.454(13) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N7 C9 1.481(10) . ? N7 H7A 0.9100 . ? N7 H7B 0.9100 . ? N8 C11 1.484(10) . ? N8 C10 1.488(10) . ? N8 H8 0.9200 . ? N9 C12 1.496(12) . ? N9 H9A 0.9100 . ? N9 H9B 0.9100 . ? N10 C13 1.493(13) . ? N10 H10A 0.9100 . ? N10 H10B 0.9100 . ? N11 C15 1.448(11) . ? N11 C14 1.476(11) . ? N11 H11 0.9200 . ? N12 C16 1.455(13) . ? N12 H12A 0.9100 . ? N12 H12B 0.9100 . ? C1 C2 1.524(11) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.509(11) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C5 C6 1.490(12) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 C8 1.527(12) . ? C7 H7C 0.9800 . ? C7 H7D 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.477(11) . ? C9 H9C 0.9800 . ? C9 H9D 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C11 C12 1.488(13) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12C 0.9800 . ? C12 H12D 0.9800 . ? C13 C14 1.452(13) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.489(13) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 Sn1 Se1 116.66(3) . . ? Se2 Sn1 Se3 112.34(4) . . ? Se1 Sn1 Se3 112.09(4) . . ? Se2 Sn1 Se3 109.01(4) . 2_755 ? Se1 Sn1 Se3 110.45(4) . 2_755 ? Se3 Sn1 Se3 93.93(3) . 2_755 ? Se4 Sn2 Se5 105.94(3) . . ? Se4 Sn2 Se6 111.56(3) . . ? Se5 Sn2 Se6 108.69(4) . . ? Se4 Sn2 Se7 104.28(4) . . ? Se5 Sn2 Se7 118.18(3) . . ? Se6 Sn2 Se7 108.13(3) . . ? N2 Ce1 N1 63.0(2) . . ? N2 Ce1 N4 122.4(2) . . ? N1 Ce1 N4 145.38(19) . . ? N2 Ce1 N3 63.7(2) . . ? N1 Ce1 N3 126.6(2) . . ? N4 Ce1 N3 71.7(2) . . ? N2 Ce1 N6 123.6(2) . . ? N1 Ce1 N6 75.7(2) . . ? N4 Ce1 N6 113.5(2) . . ? N3 Ce1 N6 135.21(19) . . ? N2 Ce1 N5 135.7(2) . . ? N1 Ce1 N5 139.7(2) . . ? N4 Ce1 N5 64.2(2) . . ? N3 Ce1 N5 81.3(2) . . ? N6 Ce1 N5 64.7(2) . . ? N2 Ce1 Se4 133.25(13) . . ? N1 Ce1 Se4 78.30(16) . . ? N4 Ce1 Se4 76.63(15) . . ? N3 Ce1 Se4 147.70(16) . . ? N6 Ce1 Se4 64.71(15) . . ? N5 Ce1 Se4 90.80(16) . . ? N2 Ce1 Se5 75.37(13) . . ? N1 Ce1 Se5 83.55(13) . . ? N4 Ce1 Se5 67.22(13) . . ? N3 Ce1 Se5 86.67(13) . . ? N6 Ce1 Se5 137.59(14) . . ? N5 Ce1 Se5 131.28(17) . . ? Se4 Ce1 Se5 75.16(2) . . ? N2 Ce1 Se1 68.54(13) . . ? N1 Ce1 Se1 86.67(14) . . ? N4 Ce1 Se1 127.87(14) . . ? N3 Ce1 Se1 71.10(14) . . ? N6 Ce1 Se1 72.60(15) . . ? N5 Ce1 Se1 75.18(17) . . ? Se4 Ce1 Se1 136.98(2) . . ? Se5 Ce1 Se1 143.15(3) . . ? N7 Ce2 N8 64.07(19) . . ? N7 Ce2 N10 78.0(2) . . ? N8 Ce2 N10 79.8(2) . . ? N7 Ce2 N12 134.0(2) . . ? N8 Ce2 N12 147.04(18) . . ? N10 Ce2 N12 126.5(2) . . ? N7 Ce2 N11 132.8(2) . . ? N8 Ce2 N11 129.8(2) . . ? N10 Ce2 N11 64.4(2) . . ? N12 Ce2 N11 63.5(2) . . ? N7 Ce2 N9 125.5(2) . . ? N8 Ce2 N9 64.1(2) . . ? N10 Ce2 N9 77.8(2) . . ? N12 Ce2 N9 99.3(2) . . ? N11 Ce2 N9 74.5(2) . . ? N7 Ce2 Se8 73.27(14) . . ? N8 Ce2 Se8 90.53(15) . . ? N10 Ce2 Se8 151.02(17) . . ? N12 Ce2 Se8 74.25(17) . . ? N11 Ce2 Se8 136.94(15) . . ? N9 Ce2 Se8 122.29(18) . . ? N7 Ce2 Se6 70.44(12) . . ? N8 Ce2 Se6 132.88(14) . . ? N10 Ce2 Se6 79.46(14) . . ? N12 Ce2 Se6 76.62(13) . . ? N11 Ce2 Se6 75.35(15) . . ? N9 Ce2 Se6 147.88(19) . . ? Se8 Ce2 Se6 87.73(2) . . ? N7 Ce2 Se7 112.26(14) . 2_566 ? N8 Ce2 Se7 79.54(13) . 2_566 ? N10 Ce2 Se7 149.42(14) . 2_566 ? N12 Ce2 Se7 68.09(14) . 2_566 ? N11 Ce2 Se7 114.64(15) . 2_566 ? N9 Ce2 Se7 72.92(18) . 2_566 ? Se8 Ce2 Se7 51.065(19) . 2_566 ? Se6 Ce2 Se7 130.94(2) . 2_566 ? Sn1 Se1 Ce1 111.31(3) . . ? Sn1 Se3 Sn1 86.07(3) . 2_755 ? Sn2 Se4 Ce1 87.00(3) . . ? Sn2 Se5 Ce1 85.48(3) . . ? Sn2 Se6 Ce2 105.69(3) . . ? Sn2 Se7 Se8 90.93(3) . . ? Sn2 Se7 Ce2 121.27(3) . 2_566 ? Se8 Se7 Ce2 60.055(18) . 2_566 ? Se7 Se8 Se7 180.0 2_566 . ? Se7 Se8 Ce2 111.12(2) 2_566 2_566 ? Se7 Se8 Ce2 68.88(2) . 2_566 ? Se7 Se8 Ce2 68.88(2) 2_566 . ? Se7 Se8 Ce2 111.12(2) . . ? Ce2 Se8 Ce2 180.000(1) 2_566 . ? C1 N1 Ce1 119.3(5) . . ? C1 N1 H1A 107.5 . . ? Ce1 N1 H1A 107.5 . . ? C1 N1 H1B 107.5 . . ? Ce1 N1 H1B 107.5 . . ? H1A N1 H1B 107.0 . . ? C3 N2 C2 113.7(6) . . ? C3 N2 Ce1 114.6(6) . . ? C2 N2 Ce1 113.9(5) . . ? C3 N2 H2 104.3 . . ? C2 N2 H2 104.3 . . ? Ce1 N2 H2 104.3 . . ? C4 N3 Ce1 115.0(5) . . ? C4 N3 H3A 108.5 . . ? Ce1 N3 H3A 108.5 . . ? C4 N3 H3B 108.5 . . ? Ce1 N3 H3B 108.5 . . ? H3A N3 H3B 107.5 . . ? C5 N4 Ce1 117.0(5) . . ? C5 N4 H4A 108.0 . . ? Ce1 N4 H4A 108.0 . . ? C5 N4 H4B 108.0 . . ? Ce1 N4 H4B 108.0 . . ? H4A N4 H4B 107.3 . . ? C6 N5 C7 112.2(8) . . ? C6 N5 Ce1 109.3(5) . . ? C7 N5 Ce1 113.0(6) . . ? C6 N5 H5 107.4 . . ? C7 N5 H5 107.4 . . ? Ce1 N5 H5 107.4 . . ? C8 N6 Ce1 114.4(5) . . ? C8 N6 H6A 108.7 . . ? Ce1 N6 H6A 108.7 . . ? C8 N6 H6B 108.7 . . ? Ce1 N6 H6B 108.7 . . ? H6A N6 H6B 107.6 . . ? C9 N7 Ce2 115.8(5) . . ? C9 N7 H7A 108.3 . . ? Ce2 N7 H7A 108.3 . . ? C9 N7 H7B 108.3 . . ? Ce2 N7 H7B 108.3 . . ? H7A N7 H7B 107.4 . . ? C11 N8 C10 112.1(6) . . ? C11 N8 Ce2 113.7(5) . . ? C10 N8 Ce2 113.1(4) . . ? C11 N8 H8 105.7 . . ? C10 N8 H8 105.7 . . ? Ce2 N8 H8 105.7 . . ? C12 N9 Ce2 113.8(6) . . ? C12 N9 H9A 108.8 . . ? Ce2 N9 H9A 108.8 . . ? C12 N9 H9B 108.8 . . ? Ce2 N9 H9B 108.8 . . ? H9A N9 H9B 107.7 . . ? C13 N10 Ce2 114.8(5) . . ? C13 N10 H10A 108.6 . . ? Ce2 N10 H10A 108.6 . . ? C13 N10 H10B 108.6 . . ? Ce2 N10 H10B 108.6 . . ? H10A N10 H10B 107.5 . . ? C15 N11 C14 111.2(7) . . ? C15 N11 Ce2 114.3(6) . . ? C14 N11 Ce2 111.7(6) . . ? C15 N11 H11 106.3 . . ? C14 N11 H11 106.3 . . ? Ce2 N11 H11 106.3 . . ? C16 N12 Ce2 116.0(5) . . ? C16 N12 H12A 108.3 . . ? Ce2 N12 H12A 108.3 . . ? C16 N12 H12B 108.3 . . ? Ce2 N12 H12B 108.3 . . ? H12A N12 H12B 107.4 . . ? N1 C1 C2 111.6(8) . . ? N1 C1 H1C 109.3 . . ? C2 C1 H1C 109.3 . . ? N1 C1 H1D 109.3 . . ? C2 C1 H1D 109.3 . . ? H1C C1 H1D 108.0 . . ? N2 C2 C1 109.2(7) . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? N2 C3 C4 108.6(7) . . ? N2 C3 H3C 110.0 . . ? C4 C3 H3C 110.0 . . ? N2 C3 H3D 110.0 . . ? C4 C3 H3D 110.0 . . ? H3C C3 H3D 108.4 . . ? N3 C4 C3 110.6(7) . . ? N3 C4 H4C 109.5 . . ? C3 C4 H4C 109.5 . . ? N3 C4 H4D 109.5 . . ? C3 C4 H4D 109.5 . . ? H4C C4 H4D 108.1 . . ? N4 C5 C6 108.6(7) . . ? N4 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? N4 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N5 C6 C5 111.9(9) . . ? N5 C6 H6C 109.2 . . ? C5 C6 H6C 109.2 . . ? N5 C6 H6D 109.2 . . ? C5 C6 H6D 109.2 . . ? H6C C6 H6D 107.9 . . ? N5 C7 C8 110.9(6) . . ? N5 C7 H7C 109.5 . . ? C8 C7 H7C 109.5 . . ? N5 C7 H7D 109.5 . . ? C8 C7 H7D 109.5 . . ? H7C C7 H7D 108.0 . . ? N6 C8 C7 109.5(8) . . ? N6 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? N6 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C10 C9 N7 108.8(8) . . ? C10 C9 H9C 109.9 . . ? N7 C9 H9C 109.9 . . ? C10 C9 H9D 109.9 . . ? N7 C9 H9D 109.9 . . ? H9C C9 H9D 108.3 . . ? C9 C10 N8 110.0(6) . . ? C9 C10 H10C 109.7 . . ? N8 C10 H10C 109.7 . . ? C9 C10 H10D 109.7 . . ? N8 C10 H10D 109.7 . . ? H10C C10 H10D 108.2 . . ? N8 C11 C12 110.6(7) . . ? N8 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N8 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 N9 109.6(7) . . ? C11 C12 H12C 109.8 . . ? N9 C12 H12C 109.8 . . ? C11 C12 H12D 109.8 . . ? N9 C12 H12D 109.8 . . ? H12C C12 H12D 108.2 . . ? C14 C13 N10 114.3(9) . . ? C14 C13 H13A 108.7 . . ? N10 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? N10 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 N11 112.5(9) . . ? C13 C14 H14A 109.1 . . ? N11 C14 H14A 109.1 . . ? C13 C14 H14B 109.1 . . ? N11 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N11 C15 C16 112.4(8) . . ? N11 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N11 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? N12 C16 C15 112.6(8) . . ? N12 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? N12 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? 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 Ce1 36.15(6) . . . . ? Se3 Sn1 Se1 Ce1 167.66(3) . . . . ? Se3 Sn1 Se1 Ce1 -89.03(4) 2_755 . . . ? N2 Ce1 Se1 Sn1 -111.13(15) . . . . ? N1 Ce1 Se1 Sn1 -48.88(16) . . . . ? N4 Ce1 Se1 Sn1 133.83(19) . . . . ? N3 Ce1 Se1 Sn1 -179.49(17) . . . . ? N6 Ce1 Se1 Sn1 27.20(18) . . . . ? N5 Ce1 Se1 Sn1 94.79(16) . . . . ? Se4 Ce1 Se1 Sn1 20.01(6) . . . . ? Se5 Ce1 Se1 Sn1 -123.49(4) . . . . ? Se2 Sn1 Se3 Sn1 -112.41(4) . . . 2_755 ? Se1 Sn1 Se3 Sn1 113.94(4) . . . 2_755 ? Se3 Sn1 Se3 Sn1 0.0 2_755 . . 2_755 ? Se5 Sn2 Se4 Ce1 -22.13(4) . . . . ? Se6 Sn2 Se4 Ce1 95.99(3) . . . . ? Se7 Sn2 Se4 Ce1 -147.54(3) . . . . ? N2 Ce1 Se4 Sn2 -36.08(19) . . . . ? N1 Ce1 Se4 Sn2 -69.87(14) . . . . ? N4 Ce1 Se4 Sn2 86.06(14) . . . . ? N3 Ce1 Se4 Sn2 74.4(3) . . . . ? N6 Ce1 Se4 Sn2 -149.5(2) . . . . ? N5 Ce1 Se4 Sn2 149.23(16) . . . . ? Se5 Ce1 Se4 Sn2 16.47(3) . . . . ? Se1 Ce1 Se4 Sn2 -141.87(4) . . . . ? Se4 Sn2 Se5 Ce1 21.69(4) . . . . ? Se6 Sn2 Se5 Ce1 -98.31(3) . . . . ? Se7 Sn2 Se5 Ce1 138.05(3) . . . . ? N2 Ce1 Se5 Sn2 126.82(14) . . . . ? N1 Ce1 Se5 Sn2 63.09(16) . . . . ? N4 Ce1 Se5 Sn2 -97.95(17) . . . . ? N3 Ce1 Se5 Sn2 -169.51(17) . . . . ? N6 Ce1 Se5 Sn2 2.5(3) . . . . ? N5 Ce1 Se5 Sn2 -94.2(2) . . . . ? Se4 Ce1 Se5 Sn2 -16.48(3) . . . . ? Se1 Ce1 Se5 Sn2 138.70(4) . . . . ? Se4 Sn2 Se6 Ce2 158.65(3) . . . . ? Se5 Sn2 Se6 Ce2 -84.91(4) . . . . ? Se7 Sn2 Se6 Ce2 44.54(4) . . . . ? N7 Ce2 Se6 Sn2 -80.69(15) . . . . ? N8 Ce2 Se6 Sn2 -96.3(2) . . . . ? N10 Ce2 Se6 Sn2 -161.53(18) . . . . ? N12 Ce2 Se6 Sn2 66.69(18) . . . . ? N11 Ce2 Se6 Sn2 132.35(16) . . . . ? N9 Ce2 Se6 Sn2 152.8(3) . . . . ? Se8 Ce2 Se6 Sn2 -7.66(3) . . . . ? Se7 Ce2 Se6 Sn2 22.25(5) 2_566 . . . ? Se4 Sn2 Se7 Se8 -178.21(3) . . . . ? Se5 Sn2 Se7 Se8 64.55(4) . . . . ? Se6 Sn2 Se7 Se8 -59.37(3) . . . . ? Se4 Sn2 Se7 Ce2 126.84(4) . . . 2_566 ? Se5 Sn2 Se7 Ce2 9.60(6) . . . 2_566 ? Se6 Sn2 Se7 Ce2 -114.32(4) . . . 2_566 ? Sn2 Se7 Se8 Se7 74(100) . . . 2_566 ? Ce2 Se7 Se8 Se7 -160(100) 2_566 . . 2_566 ? Sn2 Se7 Se8 Ce2 -126.14(3) . . . 2_566 ? Sn2 Se7 Se8 Ce2 53.86(3) . . . . ? Ce2 Se7 Se8 Ce2 180.0 2_566 . . . ? N7 Ce2 Se8 Se7 -138.71(13) . . . 2_566 ? N8 Ce2 Se8 Se7 -76.06(13) . . . 2_566 ? N10 Ce2 Se8 Se7 -145.7(3) . . . 2_566 ? N12 Ce2 Se8 Se7 74.30(14) . . . 2_566 ? N11 Ce2 Se8 Se7 85.4(2) . . . 2_566 ? N9 Ce2 Se8 Se7 -16.8(2) . . . 2_566 ? Se6 Ce2 Se8 Se7 151.04(3) . . . 2_566 ? N7 Ce2 Se8 Se7 41.29(13) . . . . ? N8 Ce2 Se8 Se7 103.94(13) . . . . ? N10 Ce2 Se8 Se7 34.3(3) . . . . ? N12 Ce2 Se8 Se7 -105.70(14) . . . . ? N11 Ce2 Se8 Se7 -94.6(2) . . . . ? N9 Ce2 Se8 Se7 163.2(2) . . . . ? Se6 Ce2 Se8 Se7 -28.96(3) . . . . ? Se7 Ce2 Se8 Se7 180.0 2_566 . . . ? N7 Ce2 Se8 Ce2 113(100) . . . 2_566 ? N8 Ce2 Se8 Ce2 176(100) . . . 2_566 ? N10 Ce2 Se8 Ce2 106(100) . . . 2_566 ? N12 Ce2 Se8 Ce2 -34(100) . . . 2_566 ? N11 Ce2 Se8 Ce2 -23(100) . . . 2_566 ? N9 Ce2 Se8 Ce2 -125(100) . . . 2_566 ? Se6 Ce2 Se8 Ce2 43(100) . . . 2_566 ? Se7 Ce2 Se8 Ce2 -108(100) 2_566 . . 2_566 ? N2 Ce1 N1 C1 -1.1(5) . . . . ? N4 Ce1 N1 C1 107.5(6) . . . . ? N3 Ce1 N1 C1 -5.3(6) . . . . ? N6 Ce1 N1 C1 -141.6(6) . . . . ? N5 Ce1 N1 C1 -131.0(6) . . . . ? Se4 Ce1 N1 C1 151.8(6) . . . . ? Se5 Ce1 N1 C1 75.7(6) . . . . ? Se1 Ce1 N1 C1 -68.7(6) . . . . ? N1 Ce1 N2 C3 161.7(5) . . . . ? N4 Ce1 N2 C3 21.3(6) . . . . ? N3 Ce1 N2 C3 -22.0(5) . . . . ? N6 Ce1 N2 C3 -150.5(5) . . . . ? N5 Ce1 N2 C3 -63.6(6) . . . . ? Se4 Ce1 N2 C3 124.0(4) . . . . ? Se5 Ce1 N2 C3 71.6(5) . . . . ? Se1 Ce1 N2 C3 -100.8(5) . . . . ? N1 Ce1 N2 C2 28.3(5) . . . . ? N4 Ce1 N2 C2 -112.1(5) . . . . ? N3 Ce1 N2 C2 -155.4(6) . . . . ? N6 Ce1 N2 C2 76.1(5) . . . . ? N5 Ce1 N2 C2 163.0(5) . . . . ? Se4 Ce1 N2 C2 -9.4(6) . . . . ? Se5 Ce1 N2 C2 -61.8(5) . . . . ? Se1 Ce1 N2 C2 125.8(5) . . . . ? N2 Ce1 N3 C4 -9.6(5) . . . . ? N1 Ce1 N3 C4 -5.5(6) . . . . ? N4 Ce1 N3 C4 -152.0(6) . . . . ? N6 Ce1 N3 C4 102.7(6) . . . . ? N5 Ce1 N3 C4 142.4(5) . . . . ? Se4 Ce1 N3 C4 -140.1(5) . . . . ? Se5 Ce1 N3 C4 -84.9(5) . . . . ? Se1 Ce1 N3 C4 65.2(5) . . . . ? N2 Ce1 N4 C5 -124.6(6) . . . . ? N1 Ce1 N4 C5 146.9(6) . . . . ? N3 Ce1 N4 C5 -84.3(6) . . . . ? N6 Ce1 N4 C5 47.9(6) . . . . ? N5 Ce1 N4 C5 4.7(6) . . . . ? Se4 Ce1 N4 C5 102.3(6) . . . . ? Se5 Ce1 N4 C5 -178.4(6) . . . . ? Se1 Ce1 N4 C5 -37.8(7) . . . . ? N2 Ce1 N5 C6 136.0(6) . . . . ? N1 Ce1 N5 C6 -122.3(6) . . . . ? N4 Ce1 N5 C6 25.1(5) . . . . ? N3 Ce1 N5 C6 99.0(6) . . . . ? N6 Ce1 N5 C6 -110.9(6) . . . . ? Se4 Ce1 N5 C6 -49.6(6) . . . . ? Se5 Ce1 N5 C6 21.3(7) . . . . ? Se1 Ce1 N5 C6 171.6(6) . . . . ? N2 Ce1 N5 C7 -98.3(6) . . . . ? N1 Ce1 N5 C7 3.4(8) . . . . ? N4 Ce1 N5 C7 150.8(7) . . . . ? N3 Ce1 N5 C7 -135.3(6) . . . . ? N6 Ce1 N5 C7 14.8(6) . . . . ? Se4 Ce1 N5 C7 76.1(6) . . . . ? Se5 Ce1 N5 C7 146.9(5) . . . . ? Se1 Ce1 N5 C7 -62.7(6) . . . . ? N2 Ce1 N6 C8 146.3(6) . . . . ? N1 Ce1 N6 C8 -170.7(6) . . . . ? N4 Ce1 N6 C8 -26.1(7) . . . . ? N3 Ce1 N6 C8 61.2(7) . . . . ? N5 Ce1 N6 C8 16.8(6) . . . . ? Se4 Ce1 N6 C8 -87.1(6) . . . . ? Se5 Ce1 N6 C8 -107.5(6) . . . . ? Se1 Ce1 N6 C8 98.3(6) . . . . ? N8 Ce2 N7 C9 -15.7(5) . . . . ? N10 Ce2 N7 C9 -100.1(5) . . . . ? N12 Ce2 N7 C9 130.1(5) . . . . ? N11 Ce2 N7 C9 -137.1(5) . . . . ? N9 Ce2 N7 C9 -34.8(6) . . . . ? Se8 Ce2 N7 C9 83.3(5) . . . . ? Se6 Ce2 N7 C9 176.9(5) . . . . ? Se7 Ce2 N7 C9 49.6(5) 2_566 . . . ? N7 Ce2 N8 C11 -144.9(5) . . . . ? N10 Ce2 N8 C11 -63.5(5) . . . . ? N12 Ce2 N8 C11 83.0(6) . . . . ? N11 Ce2 N8 C11 -19.6(6) . . . . ? N9 Ce2 N8 C11 17.9(5) . . . . ? Se8 Ce2 N8 C11 144.0(5) . . . . ? Se6 Ce2 N8 C11 -128.6(4) . . . . ? Se7 Ce2 N8 C11 93.9(5) 2_566 . . . ? N7 Ce2 N8 C10 -15.7(5) . . . . ? N10 Ce2 N8 C10 65.7(6) . . . . ? N12 Ce2 N8 C10 -147.8(5) . . . . ? N11 Ce2 N8 C10 109.6(6) . . . . ? N9 Ce2 N8 C10 147.1(6) . . . . ? Se8 Ce2 N8 C10 -86.8(5) . . . . ? Se6 Ce2 N8 C10 0.6(6) . . . . ? Se7 Ce2 N8 C10 -136.9(6) 2_566 . . . ? N7 Ce2 N9 C12 32.3(7) . . . . ? N8 Ce2 N9 C12 13.3(6) . . . . ? N10 Ce2 N9 C12 97.7(6) . . . . ? N12 Ce2 N9 C12 -136.7(6) . . . . ? N11 Ce2 N9 C12 164.2(6) . . . . ? Se8 Ce2 N9 C12 -59.6(6) . . . . ? Se6 Ce2 N9 C12 143.7(5) . . . . ? Se7 Ce2 N9 C12 -73.2(6) 2_566 . . . ? N7 Ce2 N10 C13 -154.0(6) . . . . ? N8 Ce2 N10 C13 140.6(6) . . . . ? N12 Ce2 N10 C13 -17.5(7) . . . . ? N11 Ce2 N10 C13 -3.3(6) . . . . ? N9 Ce2 N10 C13 75.1(6) . . . . ? Se8 Ce2 N10 C13 -147.2(5) . . . . ? Se6 Ce2 N10 C13 -82.0(6) . . . . ? Se7 Ce2 N10 C13 92.4(7) 2_566 . . . ? N7 Ce2 N11 C15 -109.3(6) . . . . ? N8 Ce2 N11 C15 160.9(5) . . . . ? N10 Ce2 N11 C15 -150.0(6) . . . . ? N12 Ce2 N11 C15 17.3(5) . . . . ? N9 Ce2 N11 C15 126.3(6) . . . . ? Se8 Ce2 N11 C15 5.3(7) . . . . ? Se6 Ce2 N11 C15 -64.9(6) . . . . ? Se7 Ce2 N11 C15 63.8(6) 2_566 . . . ? N7 Ce2 N11 C14 18.0(7) . . . . ? N8 Ce2 N11 C14 -71.7(6) . . . . ? N10 Ce2 N11 C14 -22.6(6) . . . . ? N12 Ce2 N11 C14 144.6(7) . . . . ? N9 Ce2 N11 C14 -106.4(6) . . . . ? Se8 Ce2 N11 C14 132.7(6) . . . . ? Se6 Ce2 N11 C14 62.5(6) . . . . ? Se7 Ce2 N11 C14 -168.8(6) 2_566 . . . ? N7 Ce2 N12 C16 135.3(6) . . . . ? N8 Ce2 N12 C16 -112.8(6) . . . . ? N10 Ce2 N12 C16 24.6(7) . . . . ? N11 Ce2 N12 C16 10.3(5) . . . . ? N9 Ce2 N12 C16 -57.1(6) . . . . ? Se8 Ce2 N12 C16 -178.1(6) . . . . ? Se6 Ce2 N12 C16 90.4(6) . . . . ? Se7 Ce2 N12 C16 -124.3(6) 2_566 . . . ? Ce1 N1 C1 C2 -24.7(9) . . . . ? C3 N2 C2 C1 173.9(8) . . . . ? Ce1 N2 C2 C1 -52.3(9) . . . . ? N1 C1 C2 N2 49.9(10) . . . . ? C2 N2 C3 C4 -176.1(8) . . . . ? Ce1 N2 C3 C4 50.4(8) . . . . ? Ce1 N3 C4 C3 38.9(8) . . . . ? N2 C3 C4 N3 -59.0(9) . . . . ? Ce1 N4 C5 C6 -33.6(10) . . . . ? C7 N5 C6 C5 178.3(7) . . . . ? Ce1 N5 C6 C5 -55.6(8) . . . . ? N4 C5 C6 N5 60.2(10) . . . . ? C6 N5 C7 C8 80.0(11) . . . . ? Ce1 N5 C7 C8 -44.1(11) . . . . ? Ce1 N6 C8 C7 -45.7(9) . . . . ? N5 C7 C8 N6 60.4(12) . . . . ? Ce2 N7 C9 C10 45.7(7) . . . . ? N7 C9 C10 N8 -60.3(9) . . . . ? C11 N8 C10 C9 176.0(7) . . . . ? Ce2 N8 C10 C9 46.0(8) . . . . ? C10 N8 C11 C12 -178.2(8) . . . . ? Ce2 N8 C11 C12 -48.4(8) . . . . ? N8 C11 C12 N9 60.9(11) . . . . ? Ce2 N9 C12 C11 -43.0(10) . . . . ? Ce2 N10 C13 C14 30.2(11) . . . . ? N10 C13 C14 N11 -53.7(13) . . . . ? C15 N11 C14 C13 177.8(10) . . . . ? Ce2 N11 C14 C13 48.7(11) . . . . ? C14 N11 C15 C16 -171.0(9) . . . . ? Ce2 N11 C15 C16 -43.4(10) . . . . ? Ce2 N12 C16 C15 -36.5(9) . . . . ? N11 C15 C16 N12 53.6(12) . . . . ? 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 Se2 0.91 2.86 3.728(6) 159.0 . N1 H1B Se6 0.91 2.84 3.719(6) 161.9 . N2 H2 Se1 0.92 2.84 3.473(6) 127.2 . N3 H3A Se2 0.91 2.77 3.673(6) 170.0 1_455 N3 H3B Se1 0.91 2.93 3.838(6) 174.1 2_655 N4 H4A Se2 0.91 2.84 3.752(7) 178.4 1_455 N5 H5 Se1 0.92 2.90 3.816(7) 176.1 2_655 N6 H6A Se4 0.91 2.77 3.198(7) 109.8 . N7 H7A Se6 0.91 2.59 3.462(6) 159.7 2_666 N7 H7B Se7 0.91 2.79 3.644(6) 156.4 . N8 H8 Se5 0.92 2.70 3.558(7) 154.9 2_566 N9 H9A Se3 0.91 2.88 3.484(9) 125.2 2_656 N10 H10A Se6 0.91 2.80 3.609(8) 148.2 2_666 N10 H10B Se4 0.91 3.06 3.779(6) 137.3 2_666 N12 H12A Se7 0.91 2.78 3.343(7) 121.1 2_566 N12 H12B Se5 0.91 2.96 3.868(7) 172.4 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.398 _refine_diff_density_min -1.377 _refine_diff_density_rms 0.196 #===END data_complex_2b _database_code_depnum_ccdc_archive 'CCDC 797230' #TrackingRef 'cif-of-1a-2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H104 N24 Nd4 Se15 Sn4' _chemical_formula_sum 'C32 H104 N24 Nd4 Se15 Sn4' _chemical_formula_weight 3061.51 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1844(11) _cell_length_b 12.9795(17) _cell_length_c 15.7510(16) _cell_angle_alpha 80.448(6) _cell_angle_beta 73.991(6) _cell_angle_gamma 88.552(7) _cell_volume 1973.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9030 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1414 _exptl_absorpt_coefficient_mu 10.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0422 _exptl_absorpt_correction_T_max 0.2946 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16306 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6899 _reflns_number_gt 4932 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0233P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6899 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 1.36530(5) 0.02923(5) 0.09014(4) 0.02383(15) Uani 1 1 d . . . Sn2 Sn 0.78271(5) 0.40300(5) 0.32787(3) 0.02111(14) Uani 1 1 d . . . Se1 Se 1.12143(8) -0.00677(8) 0.10159(6) 0.0263(2) Uani 1 1 d . . . Se2 Se 1.40878(8) 0.12042(8) 0.20416(6) 0.0329(2) Uani 1 1 d . . . Se3 Se 1.51118(8) -0.13246(8) 0.06806(6) 0.0307(2) Uani 1 1 d . . . Se4 Se 0.65157(8) 0.24458(7) 0.32719(5) 0.0262(2) Uani 1 1 d . . . Se5 Se 0.95891(8) 0.43294(7) 0.18120(5) 0.0274(2) Uani 1 1 d . . . Se6 Se 0.88718(7) 0.36654(7) 0.45685(5) 0.0228(2) Uani 1 1 d . . . Se7 Se 0.65753(7) 0.57590(7) 0.33611(5) 0.0250(2) Uani 1 1 d . . . Se8 Se 0.5000 0.5000 0.5000 0.0244(3) Uani 1 2 d S . . Nd1 Nd 0.91940(4) 0.19256(4) 0.17230(3) 0.02132(12) Uani 1 1 d . . . Nd2 Nd 0.66680(4) 0.41568(4) 0.62145(3) 0.01974(12) Uani 1 1 d . . . N1 N 0.7288(7) 0.2867(6) 0.1087(4) 0.0342(19) Uani 1 1 d . . . H1A H 0.6488 0.2501 0.1349 0.041 Uiso 1 1 calc R . . H1B H 0.7176 0.3512 0.1247 0.041 Uiso 1 1 calc R . . N2 N 0.9808(7) 0.2317(6) -0.0049(4) 0.0367(19) Uani 1 1 d . . . H2 H 0.9558 0.1735 -0.0236 0.044 Uiso 1 1 calc R . . N3 N 1.1669(7) 0.2718(6) 0.0939(5) 0.041(2) Uani 1 1 d . . . H3A H 1.1834 0.3214 0.1246 0.049 Uiso 1 1 calc R . . H3B H 1.2283 0.2203 0.0978 0.049 Uiso 1 1 calc R . . N4 N 0.7682(6) 0.0493(6) 0.1432(5) 0.0310(18) Uani 1 1 d . . . H4A H 0.6828 0.0748 0.1482 0.037 Uiso 1 1 calc R . . H4B H 0.8031 0.0386 0.0857 0.037 Uiso 1 1 calc R . . N5 N 0.8717(6) 0.0243(6) 0.2923(4) 0.0275(17) Uani 1 1 d . . . H5 H 0.9439 -0.0174 0.2716 0.033 Uiso 1 1 calc R . . N6 N 1.0424(6) 0.1825(6) 0.2992(4) 0.0318(19) Uani 1 1 d . . . H6A H 1.1339 0.1881 0.2725 0.038 Uiso 1 1 calc R . . H6B H 1.0186 0.2397 0.3261 0.038 Uiso 1 1 calc R . . N7 N 0.7879(6) 0.5870(5) 0.5262(4) 0.0238(16) Uani 1 1 d . . . H7A H 0.8781 0.5835 0.5241 0.029 Uiso 1 1 calc R . . H7B H 0.7820 0.5901 0.4692 0.029 Uiso 1 1 calc R . . N8 N 0.6163(6) 0.5820(6) 0.7015(4) 0.0248(17) Uani 1 1 d . . . H8 H 0.5327 0.6049 0.6952 0.030 Uiso 1 1 calc R . . N9 N 0.5647(7) 0.3730(6) 0.7991(4) 0.041(2) Uani 1 1 d . . . H9A H 0.4981 0.3228 0.8127 0.049 Uiso 1 1 calc R . . H9B H 0.6321 0.3467 0.8237 0.049 Uiso 1 1 calc R . . N10 N 0.8892(6) 0.4243(6) 0.6769(4) 0.0320(19) Uani 1 1 d . . . H10A H 0.9586 0.4537 0.6296 0.038 Uiso 1 1 calc R . . H10B H 0.8732 0.4674 0.7185 0.038 Uiso 1 1 calc R . . N11 N 0.7629(6) 0.2309(6) 0.6760(4) 0.0303(18) Uani 1 1 d . . . H11 H 0.7169 0.2132 0.7357 0.036 Uiso 1 1 calc R . . N12 N 0.5597(6) 0.2498(6) 0.5829(4) 0.0284(18) Uani 1 1 d . . . H12A H 0.4673 0.2557 0.5980 0.034 Uiso 1 1 calc R . . H12B H 0.5887 0.2518 0.5225 0.034 Uiso 1 1 calc R . . C1 C 0.7550(10) 0.2988(10) 0.0099(7) 0.059(3) Uani 1 1 d . . . H1C H 0.7255 0.2351 -0.0061 0.071 Uiso 1 1 calc R . . H1D H 0.7025 0.3571 -0.0109 0.071 Uiso 1 1 calc R . . C2 C 0.9008(10) 0.3187(9) -0.0337(6) 0.053(3) Uani 1 1 d . . . H2A H 0.9171 0.3282 -0.0988 0.064 Uiso 1 1 calc R . . H2B H 0.9297 0.3831 -0.0185 0.064 Uiso 1 1 calc R . . C3 C 1.1311(10) 0.2507(9) -0.0474(6) 0.052(3) Uani 1 1 d . . . H3C H 1.1776 0.1836 -0.0465 0.062 Uiso 1 1 calc R . . H3D H 1.1463 0.2836 -0.1100 0.062 Uiso 1 1 calc R . . C4 C 1.1903(9) 0.3186(8) 0.0000(6) 0.049(3) Uani 1 1 d . . . H4C H 1.2887 0.3283 -0.0284 0.058 Uiso 1 1 calc R . . H4D H 1.1483 0.3874 -0.0041 0.058 Uiso 1 1 calc R . . C5 C 0.7557(8) -0.0530(8) 0.2028(6) 0.038(2) Uani 1 1 d . . . H5A H 0.8334 -0.0961 0.1794 0.045 Uiso 1 1 calc R . . H5B H 0.6719 -0.0894 0.2040 0.045 Uiso 1 1 calc R . . C6 C 0.7521(8) -0.0388(8) 0.2963(6) 0.038(2) Uani 1 1 d . . . H6C H 0.6682 -0.0038 0.3230 0.045 Uiso 1 1 calc R . . H6D H 0.7533 -0.1071 0.3336 0.045 Uiso 1 1 calc R . . C7 C 0.8843(8) 0.0369(8) 0.3810(5) 0.038(2) Uani 1 1 d . . . H7C H 0.8788 -0.0317 0.4189 0.045 Uiso 1 1 calc R . . H7D H 0.8092 0.0789 0.4100 0.045 Uiso 1 1 calc R . . C8 C 1.0179(8) 0.0895(8) 0.3706(6) 0.039(3) Uani 1 1 d . . . H8A H 1.0183 0.1108 0.4274 0.047 Uiso 1 1 calc R . . H8B H 1.0919 0.0401 0.3558 0.047 Uiso 1 1 calc R . . C9 C 0.7347(8) 0.6857(7) 0.5575(5) 0.032(2) Uani 1 1 d . . . H9C H 0.8003 0.7434 0.5282 0.038 Uiso 1 1 calc R . . H9D H 0.6482 0.7028 0.5432 0.038 Uiso 1 1 calc R . . C10 C 0.7138(7) 0.6695(7) 0.6554(5) 0.029(2) Uani 1 1 d . . . H10C H 0.6789 0.7336 0.6782 0.035 Uiso 1 1 calc R . . H10D H 0.8016 0.6548 0.6687 0.035 Uiso 1 1 calc R . . C11 C 0.5990(8) 0.5588(8) 0.7992(5) 0.036(2) Uani 1 1 d . . . H11A H 0.5596 0.6190 0.8266 0.043 Uiso 1 1 calc R . . H11B H 0.6883 0.5458 0.8106 0.043 Uiso 1 1 calc R . . C12 C 0.5071(9) 0.4648(9) 0.8400(6) 0.043(3) Uani 1 1 d . . . H12C H 0.4964 0.4499 0.9046 0.051 Uiso 1 1 calc R . . H12D H 0.4167 0.4790 0.8307 0.051 Uiso 1 1 calc R . . C13 C 0.9355(10) 0.3223(9) 0.7164(7) 0.051(3) Uani 1 1 d . . . H13A H 1.0336 0.3273 0.7104 0.061 Uiso 1 1 calc R . . H13B H 0.8878 0.3070 0.7805 0.061 Uiso 1 1 calc R . . C14 C 0.9095(9) 0.2367(9) 0.6728(7) 0.052(3) Uani 1 1 d . . . H14A H 0.9358 0.1704 0.7031 0.062 Uiso 1 1 calc R . . H14B H 0.9651 0.2477 0.6103 0.062 Uiso 1 1 calc R . . C15 C 0.7340(9) 0.1460(8) 0.6334(7) 0.050(3) Uani 1 1 d . . . H15A H 0.7491 0.0791 0.6682 0.060 Uiso 1 1 calc R . . H15B H 0.7975 0.1515 0.5733 0.060 Uiso 1 1 calc R . . C16 C 0.5920(9) 0.1479(8) 0.6263(7) 0.043(3) Uani 1 1 d . . . H16A H 0.5797 0.0943 0.5918 0.052 Uiso 1 1 calc R . . H16B H 0.5286 0.1312 0.6864 0.052 Uiso 1 1 calc R . . 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 0.0192(3) 0.0255(4) 0.0270(3) -0.0118(3) -0.0023(2) 0.0000(3) Sn2 0.0169(3) 0.0257(4) 0.0216(3) -0.0093(3) -0.0038(2) 0.0026(2) Se1 0.0207(4) 0.0221(7) 0.0279(5) -0.0049(5) -0.0018(4) -0.0028(4) Se2 0.0269(4) 0.0407(7) 0.0354(5) -0.0220(5) -0.0067(4) 0.0023(4) Se3 0.0300(5) 0.0248(6) 0.0322(5) -0.0042(4) -0.0007(4) 0.0026(4) Se4 0.0210(4) 0.0260(6) 0.0324(5) -0.0108(4) -0.0050(4) 0.0004(4) Se5 0.0287(4) 0.0244(6) 0.0251(4) -0.0085(4) 0.0020(4) -0.0002(4) Se6 0.0178(4) 0.0290(6) 0.0229(4) -0.0085(4) -0.0056(3) 0.0029(4) Se7 0.0193(4) 0.0259(6) 0.0290(4) -0.0082(4) -0.0034(3) 0.0040(4) Se8 0.0184(5) 0.0253(8) 0.0324(6) -0.0078(6) -0.0102(5) 0.0032(5) Nd1 0.0205(2) 0.0218(3) 0.0220(2) -0.0062(2) -0.00478(18) -0.00103(19) Nd2 0.0186(2) 0.0187(3) 0.0219(2) -0.0052(2) -0.00468(18) 0.00107(19) N1 0.047(4) 0.027(5) 0.034(4) -0.006(4) -0.019(4) -0.001(4) N2 0.053(5) 0.028(5) 0.026(4) -0.008(4) -0.003(4) 0.004(4) N3 0.029(4) 0.027(5) 0.071(6) -0.026(5) -0.009(4) 0.003(4) N4 0.022(4) 0.033(5) 0.037(4) -0.004(4) -0.006(3) -0.009(3) N5 0.029(4) 0.027(5) 0.027(4) -0.010(3) -0.007(3) 0.004(3) N6 0.019(3) 0.042(6) 0.038(4) -0.018(4) -0.007(3) 0.004(3) N7 0.022(3) 0.019(4) 0.031(4) -0.006(3) -0.008(3) -0.001(3) N8 0.019(3) 0.030(5) 0.027(4) -0.007(3) -0.006(3) -0.002(3) N9 0.053(5) 0.040(6) 0.023(4) 0.001(4) -0.001(4) -0.006(4) N10 0.025(4) 0.053(6) 0.017(3) -0.012(4) -0.001(3) 0.000(4) N11 0.032(4) 0.031(5) 0.029(4) -0.006(4) -0.010(3) 0.006(3) N12 0.019(3) 0.032(5) 0.033(4) -0.007(4) -0.005(3) 0.008(3) C1 0.059(7) 0.068(10) 0.056(7) 0.005(6) -0.032(6) -0.016(6) C2 0.073(7) 0.058(9) 0.026(5) 0.003(5) -0.014(5) -0.005(6) C3 0.066(7) 0.050(8) 0.024(5) -0.019(5) 0.022(5) -0.017(6) C4 0.043(6) 0.033(7) 0.052(6) 0.000(5) 0.014(5) -0.009(5) C5 0.026(5) 0.038(7) 0.050(6) -0.028(5) -0.001(4) -0.005(4) C6 0.035(5) 0.034(7) 0.040(5) -0.007(5) -0.001(4) -0.016(4) C7 0.038(5) 0.046(7) 0.029(5) 0.001(5) -0.013(4) -0.005(5) C8 0.040(5) 0.053(8) 0.031(5) -0.012(5) -0.018(4) 0.006(5) C9 0.030(5) 0.031(6) 0.028(5) -0.003(4) 0.002(4) -0.005(4) C10 0.020(4) 0.021(6) 0.045(5) -0.013(4) -0.002(4) -0.001(4) C11 0.035(5) 0.047(7) 0.028(5) -0.017(5) -0.005(4) 0.000(5) C12 0.045(5) 0.062(8) 0.019(5) -0.012(5) -0.003(4) 0.010(5) C13 0.056(6) 0.056(8) 0.050(6) -0.011(6) -0.031(5) 0.019(6) C14 0.047(6) 0.060(9) 0.051(6) 0.000(6) -0.026(5) 0.021(6) C15 0.046(6) 0.023(7) 0.078(8) 0.003(6) -0.019(5) 0.001(5) C16 0.040(5) 0.032(7) 0.059(6) -0.021(5) -0.010(5) -0.005(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 Se2 2.4481(10) . ? Sn1 Se1 2.4906(10) . ? Sn1 Se3 2.5559(11) . ? Sn1 Se3 2.6143(11) 2_855 ? Sn2 Se5 2.4817(10) . ? Sn2 Se4 2.4831(11) . ? Sn2 Se6 2.5162(9) . ? Sn2 Se7 2.5572(10) . ? Se1 Nd1 3.4046(11) . ? Se3 Sn1 2.6143(11) 2_855 ? Se4 Nd1 3.2605(9) . ? Se5 Nd1 3.1867(11) . ? Se6 Nd2 3.0712(9) . ? Se7 Se8 2.6758(9) . ? Se7 Nd2 3.1871(9) 2_666 ? Se8 Se7 2.6758(9) 2_666 ? Se8 Nd2 2.9575(5) . ? Se8 Nd2 2.9575(5) 2_666 ? Nd1 N5 2.599(7) . ? Nd1 N1 2.610(6) . ? Nd1 N4 2.618(7) . ? Nd1 N6 2.620(6) . ? Nd1 N3 2.632(7) . ? Nd1 N2 2.651(6) . ? Nd2 N7 2.594(7) . ? Nd2 N8 2.646(7) . ? Nd2 N10 2.654(6) . ? Nd2 N11 2.666(7) . ? Nd2 N12 2.667(7) . ? Nd2 N9 2.670(6) . ? Nd2 Se7 3.1871(9) 2_666 ? N1 C1 1.486(11) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.460(12) . ? N2 C3 1.500(11) . ? N2 H2 0.9200 . ? N3 C4 1.459(11) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C5 1.479(11) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N5 C6 1.466(10) . ? N5 C7 1.473(9) . ? N5 H5 0.9200 . ? N6 C8 1.481(11) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N7 C9 1.485(10) . ? N7 H7A 0.9100 . ? N7 H7B 0.9100 . ? N8 C11 1.479(9) . ? N8 C10 1.480(10) . ? N8 H8 0.9200 . ? N9 C12 1.479(12) . ? N9 H9A 0.9100 . ? N9 H9B 0.9100 . ? N10 C13 1.490(12) . ? N10 H10A 0.9100 . ? N10 H10B 0.9100 . ? N11 C15 1.457(12) . ? N11 C14 1.483(10) . ? N11 H11 0.9200 . ? N12 C16 1.459(11) . ? N12 H12A 0.9100 . ? N12 H12B 0.9100 . ? C1 C2 1.463(13) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.481(13) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C5 C6 1.506(11) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 C8 1.494(12) . ? C7 H7C 0.9800 . ? C7 H7D 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.477(10) . ? C9 H9C 0.9800 . ? C9 H9D 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C11 C12 1.498(13) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12C 0.9800 . ? C12 H12D 0.9800 . ? C13 C14 1.465(14) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.480(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 Sn1 Se1 116.50(3) . . ? Se2 Sn1 Se3 112.86(4) . . ? Se1 Sn1 Se3 111.97(4) . . ? Se2 Sn1 Se3 108.69(4) . 2_855 ? Se1 Sn1 Se3 110.65(3) . 2_855 ? Se3 Sn1 Se3 93.81(3) . 2_855 ? Se5 Sn2 Se4 105.47(3) . . ? Se5 Sn2 Se6 112.00(3) . . ? Se4 Sn2 Se6 108.22(4) . . ? Se5 Sn2 Se7 104.62(4) . . ? Se4 Sn2 Se7 118.35(3) . . ? Se6 Sn2 Se7 108.19(3) . . ? Sn1 Se1 Nd1 111.37(4) . . ? Sn1 Se3 Sn1 86.19(3) . 2_855 ? Sn2 Se4 Nd1 85.58(3) . . ? Sn2 Se5 Nd1 87.23(3) . . ? Sn2 Se6 Nd2 106.05(3) . . ? Sn2 Se7 Se8 90.72(3) . . ? Sn2 Se7 Nd2 121.43(4) . 2_666 ? Se8 Se7 Nd2 59.834(18) . 2_666 ? Se7 Se8 Se7 180.0 2_666 . ? Se7 Se8 Nd2 68.702(19) 2_666 . ? Se7 Se8 Nd2 111.298(19) . . ? Se7 Se8 Nd2 111.298(19) 2_666 2_666 ? Se7 Se8 Nd2 68.702(19) . 2_666 ? Nd2 Se8 Nd2 180.0 . 2_666 ? N5 Nd1 N1 122.6(2) . . ? N5 Nd1 N4 64.8(2) . . ? N1 Nd1 N4 72.0(2) . . ? N5 Nd1 N6 63.8(2) . . ? N1 Nd1 N6 144.1(2) . . ? N4 Nd1 N6 128.5(2) . . ? N5 Nd1 N3 122.8(2) . . ? N1 Nd1 N3 114.3(2) . . ? N4 Nd1 N3 135.1(2) . . ? N6 Nd1 N3 73.9(2) . . ? N5 Nd1 N2 134.9(2) . . ? N1 Nd1 N2 65.5(2) . . ? N4 Nd1 N2 79.6(2) . . ? N6 Nd1 N2 139.0(2) . . ? N3 Nd1 N2 65.8(2) . . ? N5 Nd1 Se5 133.35(14) . . ? N1 Nd1 Se5 75.58(17) . . ? N4 Nd1 Se5 147.24(15) . . ? N6 Nd1 Se5 77.72(17) . . ? N3 Nd1 Se5 64.55(17) . . ? N2 Nd1 Se5 91.50(18) . . ? N5 Nd1 Se4 75.07(14) . . ? N1 Nd1 Se4 66.54(15) . . ? N4 Nd1 Se4 87.08(15) . . ? N6 Nd1 Se4 83.88(14) . . ? N3 Nd1 Se4 137.41(16) . . ? N2 Nd1 Se4 132.02(15) . . ? Se5 Nd1 Se4 75.59(2) . . ? N5 Nd1 Se1 68.26(14) . . ? N1 Nd1 Se1 129.19(15) . . ? N4 Nd1 Se1 70.95(15) . . ? N6 Nd1 Se1 86.68(15) . . ? N3 Nd1 Se1 72.77(17) . . ? N2 Nd1 Se1 74.59(16) . . ? Se5 Nd1 Se1 137.08(3) . . ? Se4 Nd1 Se1 142.55(3) . . ? N7 Nd2 N8 65.2(2) . . ? N7 Nd2 N10 77.3(2) . . ? N8 Nd2 N10 79.3(2) . . ? N7 Nd2 N11 132.1(2) . . ? N8 Nd2 N11 129.5(2) . . ? N10 Nd2 N11 64.9(2) . . ? N7 Nd2 N12 133.9(2) . . ? N8 Nd2 N12 145.92(18) . . ? N10 Nd2 N12 127.8(2) . . ? N11 Nd2 N12 64.2(2) . . ? N7 Nd2 N9 127.7(2) . . ? N8 Nd2 N9 65.3(2) . . ? N10 Nd2 N9 78.1(2) . . ? N11 Nd2 N9 73.0(2) . . ? N12 Nd2 N9 97.4(2) . . ? N7 Nd2 Se8 73.17(13) . . ? N8 Nd2 Se8 90.43(13) . . ? N10 Nd2 Se8 150.33(16) . . ? N11 Nd2 Se8 137.38(15) . . ? N12 Nd2 Se8 74.15(14) . . ? N9 Nd2 Se8 122.79(16) . . ? N7 Nd2 Se6 69.90(14) . . ? N8 Nd2 Se6 133.39(14) . . ? N10 Nd2 Se6 79.41(14) . . ? N11 Nd2 Se6 75.00(14) . . ? N12 Nd2 Se6 77.37(13) . . ? N9 Nd2 Se6 146.44(17) . . ? Se8 Nd2 Se6 88.105(19) . . ? N7 Nd2 Se7 112.80(13) . 2_666 ? N8 Nd2 Se7 78.96(13) . 2_666 ? N10 Nd2 Se7 148.85(14) . 2_666 ? N11 Nd2 Se7 114.85(15) . 2_666 ? N12 Nd2 Se7 67.59(13) . 2_666 ? N9 Nd2 Se7 72.66(16) . 2_666 ? Se8 Nd2 Se7 51.464(17) . 2_666 ? Se6 Nd2 Se7 131.60(2) . 2_666 ? C1 N1 Nd1 115.2(6) . . ? C1 N1 H1A 108.5 . . ? Nd1 N1 H1A 108.5 . . ? C1 N1 H1B 108.5 . . ? Nd1 N1 H1B 108.5 . . ? H1A N1 H1B 107.5 . . ? C2 N2 C3 111.8(8) . . ? C2 N2 Nd1 110.0(5) . . ? C3 N2 Nd1 112.3(5) . . ? C2 N2 H2 107.5 . . ? C3 N2 H2 107.5 . . ? Nd1 N2 H2 107.5 . . ? C4 N3 Nd1 114.8(5) . . ? C4 N3 H3A 108.6 . . ? Nd1 N3 H3A 108.6 . . ? C4 N3 H3B 108.6 . . ? Nd1 N3 H3B 108.6 . . ? H3A N3 H3B 107.5 . . ? C5 N4 Nd1 116.4(5) . . ? C5 N4 H4A 108.2 . . ? Nd1 N4 H4A 108.2 . . ? C5 N4 H4B 108.2 . . ? Nd1 N4 H4B 108.2 . . ? H4A N4 H4B 107.3 . . ? C6 N5 C7 113.6(6) . . ? C6 N5 Nd1 115.8(5) . . ? C7 N5 Nd1 115.3(6) . . ? C6 N5 H5 103.3 . . ? C7 N5 H5 103.3 . . ? Nd1 N5 H5 103.3 . . ? C8 N6 Nd1 119.0(5) . . ? C8 N6 H6A 107.6 . . ? Nd1 N6 H6A 107.6 . . ? C8 N6 H6B 107.6 . . ? Nd1 N6 H6B 107.6 . . ? H6A N6 H6B 107.0 . . ? C9 N7 Nd2 116.3(5) . . ? C9 N7 H7A 108.2 . . ? Nd2 N7 H7A 108.2 . . ? C9 N7 H7B 108.2 . . ? Nd2 N7 H7B 108.2 . . ? H7A N7 H7B 107.4 . . ? C11 N8 C10 113.2(7) . . ? C11 N8 Nd2 113.9(5) . . ? C10 N8 Nd2 112.4(4) . . ? C11 N8 H8 105.5 . . ? C10 N8 H8 105.5 . . ? Nd2 N8 H8 105.5 . . ? C12 N9 Nd2 113.7(5) . . ? C12 N9 H9A 108.8 . . ? Nd2 N9 H9A 108.8 . . ? C12 N9 H9B 108.8 . . ? Nd2 N9 H9B 108.8 . . ? H9A N9 H9B 107.7 . . ? C13 N10 Nd2 115.6(6) . . ? C13 N10 H10A 108.4 . . ? Nd2 N10 H10A 108.4 . . ? C13 N10 H10B 108.4 . . ? Nd2 N10 H10B 108.4 . . ? H10A N10 H10B 107.4 . . ? C15 N11 C14 111.8(7) . . ? C15 N11 Nd2 114.8(5) . . ? C14 N11 Nd2 112.6(6) . . ? C15 N11 H11 105.6 . . ? C14 N11 H11 105.6 . . ? Nd2 N11 H11 105.6 . . ? C16 N12 Nd2 116.3(5) . . ? C16 N12 H12A 108.2 . . ? Nd2 N12 H12A 108.2 . . ? C16 N12 H12B 108.2 . . ? Nd2 N12 H12B 108.2 . . ? H12A N12 H12B 107.4 . . ? C2 C1 N1 109.9(7) . . ? C2 C1 H1C 109.7 . . ? N1 C1 H1C 109.7 . . ? C2 C1 H1D 109.7 . . ? N1 C1 H1D 109.7 . . ? H1C C1 H1D 108.2 . . ? N2 C2 C1 110.6(9) . . ? N2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 N2 111.5(7) . . ? C4 C3 H3C 109.3 . . ? N2 C3 H3C 109.3 . . ? C4 C3 H3D 109.3 . . ? N2 C3 H3D 109.3 . . ? H3C C3 H3D 108.0 . . ? N3 C4 C3 110.3(8) . . ? N3 C4 H4C 109.6 . . ? C3 C4 H4C 109.6 . . ? N3 C4 H4D 109.6 . . ? C3 C4 H4D 109.6 . . ? H4C C4 H4D 108.1 . . ? N4 C5 C6 110.6(8) . . ? N4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? N5 C6 C5 108.8(7) . . ? N5 C6 H6C 109.9 . . ? C5 C6 H6C 109.9 . . ? N5 C6 H6D 109.9 . . ? C5 C6 H6D 109.9 . . ? H6C C6 H6D 108.3 . . ? N5 C7 C8 109.6(7) . . ? N5 C7 H7C 109.8 . . ? C8 C7 H7C 109.8 . . ? N5 C7 H7D 109.8 . . ? C8 C7 H7D 109.8 . . ? H7C C7 H7D 108.2 . . ? N6 C8 C7 111.2(6) . . ? N6 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? N6 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 N7 107.4(7) . . ? C10 C9 H9C 110.2 . . ? N7 C9 H9C 110.2 . . ? C10 C9 H9D 110.2 . . ? N7 C9 H9D 110.2 . . ? H9C C9 H9D 108.5 . . ? C9 C10 N8 111.5(7) . . ? C9 C10 H10C 109.3 . . ? N8 C10 H10C 109.3 . . ? C9 C10 H10D 109.3 . . ? N8 C10 H10D 109.3 . . ? H10C C10 H10D 108.0 . . ? N8 C11 C12 110.1(7) . . ? N8 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? N8 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.2 . . ? N9 C12 C11 110.4(7) . . ? N9 C12 H12C 109.6 . . ? C11 C12 H12C 109.6 . . ? N9 C12 H12D 109.6 . . ? C11 C12 H12D 109.6 . . ? H12C C12 H12D 108.1 . . ? C14 C13 N10 111.9(7) . . ? C14 C13 H13A 109.2 . . ? N10 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? N10 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 N11 110.6(8) . . ? C13 C14 H14A 109.5 . . ? N11 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? N11 C15 C16 112.0(8) . . ? N11 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N11 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? N12 C16 C15 111.5(8) . . ? N12 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? N12 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? 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 Nd1 36.54(5) . . . . ? Se3 Sn1 Se1 Nd1 168.54(3) . . . . ? Se3 Sn1 Se1 Nd1 -88.25(4) 2_855 . . . ? Se2 Sn1 Se3 Sn1 -112.12(4) . . . 2_855 ? Se1 Sn1 Se3 Sn1 114.08(4) . . . 2_855 ? Se3 Sn1 Se3 Sn1 0.0 2_855 . . 2_855 ? Se5 Sn2 Se4 Nd1 21.08(3) . . . . ? Se6 Sn2 Se4 Nd1 -98.93(3) . . . . ? Se7 Sn2 Se4 Nd1 137.63(3) . . . . ? Se4 Sn2 Se5 Nd1 -21.55(3) . . . . ? Se6 Sn2 Se5 Nd1 95.94(4) . . . . ? Se7 Sn2 Se5 Nd1 -147.10(3) . . . . ? Se5 Sn2 Se6 Nd2 158.93(3) . . . . ? Se4 Sn2 Se6 Nd2 -85.24(4) . . . . ? Se7 Sn2 Se6 Nd2 44.13(4) . . . . ? Se5 Sn2 Se7 Se8 -178.00(3) . . . . ? Se4 Sn2 Se7 Se8 64.99(4) . . . . ? Se6 Sn2 Se7 Se8 -58.45(3) . . . . ? Se5 Sn2 Se7 Nd2 127.54(4) . . . 2_666 ? Se4 Sn2 Se7 Nd2 10.54(5) . . . 2_666 ? Se6 Sn2 Se7 Nd2 -112.91(4) . . . 2_666 ? Sn2 Se7 Se8 Se7 -103(100) . . . 2_666 ? Nd2 Se7 Se8 Se7 23(100) 2_666 . . 2_666 ? Sn2 Se7 Se8 Nd2 53.42(3) . . . . ? Nd2 Se7 Se8 Nd2 180.0 2_666 . . . ? Sn2 Se7 Se8 Nd2 -126.58(3) . . . 2_666 ? Sn2 Se5 Nd1 N5 -36.36(19) . . . . ? Sn2 Se5 Nd1 N1 85.17(15) . . . . ? Sn2 Se5 Nd1 N4 76.4(3) . . . . ? Sn2 Se5 Nd1 N6 -70.58(14) . . . . ? Sn2 Se5 Nd1 N3 -148.44(19) . . . . ? Sn2 Se5 Nd1 N2 149.37(15) . . . . ? Sn2 Se5 Nd1 Se4 16.17(2) . . . . ? Sn2 Se5 Nd1 Se1 -141.86(3) . . . . ? Sn2 Se4 Nd1 N5 127.14(14) . . . . ? Sn2 Se4 Nd1 N1 -96.48(19) . . . . ? Sn2 Se4 Nd1 N4 -168.13(15) . . . . ? Sn2 Se4 Nd1 N6 62.67(18) . . . . ? Sn2 Se4 Nd1 N3 4.6(3) . . . . ? Sn2 Se4 Nd1 N2 -94.9(2) . . . . ? Sn2 Se4 Nd1 Se5 -16.19(2) . . . . ? Sn2 Se4 Nd1 Se1 139.03(4) . . . . ? Sn1 Se1 Nd1 N5 -111.52(15) . . . . ? Sn1 Se1 Nd1 N1 133.4(2) . . . . ? Sn1 Se1 Nd1 N4 178.75(16) . . . . ? Sn1 Se1 Nd1 N6 -48.45(16) . . . . ? Sn1 Se1 Nd1 N3 25.73(18) . . . . ? Sn1 Se1 Nd1 N2 94.65(18) . . . . ? Sn1 Se1 Nd1 Se5 19.51(5) . . . . ? Sn1 Se1 Nd1 Se4 -123.89(4) . . . . ? Se7 Se8 Nd2 N7 -139.32(15) 2_666 . . . ? Se7 Se8 Nd2 N7 40.68(15) . . . . ? Nd2 Se8 Nd2 N7 118(100) 2_666 . . . ? Se7 Se8 Nd2 N8 -75.48(14) 2_666 . . . ? Se7 Se8 Nd2 N8 104.52(14) . . . . ? Nd2 Se8 Nd2 N8 -178(100) 2_666 . . . ? Se7 Se8 Nd2 N10 -144.3(3) 2_666 . . . ? Se7 Se8 Nd2 N10 35.7(3) . . . . ? Nd2 Se8 Nd2 N10 113(100) 2_666 . . . ? Se7 Se8 Nd2 N11 85.9(2) 2_666 . . . ? Se7 Se8 Nd2 N11 -94.1(2) . . . . ? Nd2 Se8 Nd2 N11 -16(100) 2_666 . . . ? Se7 Se8 Nd2 N12 73.71(14) 2_666 . . . ? Se7 Se8 Nd2 N12 -106.29(14) . . . . ? Nd2 Se8 Nd2 N12 -29(100) 2_666 . . . ? Se7 Se8 Nd2 N9 -14.9(2) 2_666 . . . ? Se7 Se8 Nd2 N9 165.1(2) . . . . ? Nd2 Se8 Nd2 N9 -117(100) 2_666 . . . ? Se7 Se8 Nd2 Se6 151.12(3) 2_666 . . . ? Se7 Se8 Nd2 Se6 -28.88(3) . . . . ? Nd2 Se8 Nd2 Se6 49(100) 2_666 . . . ? Se7 Se8 Nd2 Se7 180.0 . . . 2_666 ? Nd2 Se8 Nd2 Se7 -102(100) 2_666 . . 2_666 ? Sn2 Se6 Nd2 N7 -80.18(14) . . . . ? Sn2 Se6 Nd2 N8 -96.22(18) . . . . ? Sn2 Se6 Nd2 N10 -160.37(18) . . . . ? Sn2 Se6 Nd2 N11 133.04(16) . . . . ? Sn2 Se6 Nd2 N12 66.76(14) . . . . ? Sn2 Se6 Nd2 N9 151.1(3) . . . . ? Sn2 Se6 Nd2 Se8 -7.42(3) . . . . ? Sn2 Se6 Nd2 Se7 22.93(5) . . . 2_666 ? N5 Nd1 N1 C1 -122.6(7) . . . . ? N4 Nd1 N1 C1 -80.2(7) . . . . ? N6 Nd1 N1 C1 148.0(6) . . . . ? N3 Nd1 N1 C1 51.9(7) . . . . ? N2 Nd1 N1 C1 6.4(6) . . . . ? Se5 Nd1 N1 C1 104.8(7) . . . . ? Se4 Nd1 N1 C1 -174.9(7) . . . . ? Se1 Nd1 N1 C1 -35.2(7) . . . . ? N5 Nd1 N2 C2 136.2(6) . . . . ? N1 Nd1 N2 C2 23.8(6) . . . . ? N4 Nd1 N2 C2 98.6(6) . . . . ? N6 Nd1 N2 C2 -122.6(6) . . . . ? N3 Nd1 N2 C2 -110.8(7) . . . . ? Se5 Nd1 N2 C2 -49.6(6) . . . . ? Se4 Nd1 N2 C2 22.2(7) . . . . ? Se1 Nd1 N2 C2 171.5(7) . . . . ? N5 Nd1 N2 C3 -98.6(7) . . . . ? N1 Nd1 N2 C3 148.9(7) . . . . ? N4 Nd1 N2 C3 -136.2(6) . . . . ? N6 Nd1 N2 C3 2.6(8) . . . . ? N3 Nd1 N2 C3 14.4(6) . . . . ? Se5 Nd1 N2 C3 75.5(6) . . . . ? Se4 Nd1 N2 C3 147.3(5) . . . . ? Se1 Nd1 N2 C3 -63.3(6) . . . . ? N5 Nd1 N3 C4 144.3(6) . . . . ? N1 Nd1 N3 C4 -30.2(7) . . . . ? N4 Nd1 N3 C4 58.3(7) . . . . ? N6 Nd1 N3 C4 -172.8(7) . . . . ? N2 Nd1 N3 C4 15.2(6) . . . . ? Se5 Nd1 N3 C4 -89.0(6) . . . . ? Se4 Nd1 N3 C4 -111.4(6) . . . . ? Se1 Nd1 N3 C4 95.7(6) . . . . ? N5 Nd1 N4 C5 -8.6(5) . . . . ? N1 Nd1 N4 C5 -149.7(6) . . . . ? N6 Nd1 N4 C5 -3.6(6) . . . . ? N3 Nd1 N4 C5 103.6(6) . . . . ? N2 Nd1 N4 C5 142.9(6) . . . . ? Se5 Nd1 N4 C5 -140.8(4) . . . . ? Se4 Nd1 N4 C5 -83.4(5) . . . . ? Se1 Nd1 N4 C5 65.7(5) . . . . ? N1 Nd1 N5 C6 24.1(6) . . . . ? N4 Nd1 N5 C6 -21.1(5) . . . . ? N6 Nd1 N5 C6 163.3(6) . . . . ? N3 Nd1 N5 C6 -149.9(5) . . . . ? N2 Nd1 N5 C6 -62.6(6) . . . . ? Se5 Nd1 N5 C6 125.5(5) . . . . ? Se4 Nd1 N5 C6 72.8(5) . . . . ? Se1 Nd1 N5 C6 -99.5(5) . . . . ? N1 Nd1 N5 C7 -112.0(5) . . . . ? N4 Nd1 N5 C7 -157.1(6) . . . . ? N6 Nd1 N5 C7 27.2(5) . . . . ? N3 Nd1 N5 C7 74.0(6) . . . . ? N2 Nd1 N5 C7 161.4(5) . . . . ? Se5 Nd1 N5 C7 -10.6(6) . . . . ? Se4 Nd1 N5 C7 -63.3(5) . . . . ? Se1 Nd1 N5 C7 124.5(5) . . . . ? N5 Nd1 N6 C8 -1.0(5) . . . . ? N1 Nd1 N6 C8 109.2(6) . . . . ? N4 Nd1 N6 C8 -6.0(7) . . . . ? N3 Nd1 N6 C8 -141.4(6) . . . . ? N2 Nd1 N6 C8 -130.2(6) . . . . ? Se5 Nd1 N6 C8 151.9(6) . . . . ? Se4 Nd1 N6 C8 75.3(5) . . . . ? Se1 Nd1 N6 C8 -68.4(5) . . . . ? N8 Nd2 N7 C9 -15.9(5) . . . . ? N10 Nd2 N7 C9 -99.9(5) . . . . ? N11 Nd2 N7 C9 -137.7(5) . . . . ? N12 Nd2 N7 C9 129.3(5) . . . . ? N9 Nd2 N7 C9 -36.1(6) . . . . ? Se8 Nd2 N7 C9 82.6(5) . . . . ? Se6 Nd2 N7 C9 176.9(5) . . . . ? Se7 Nd2 N7 C9 49.1(5) 2_666 . . . ? N7 Nd2 N8 C11 -145.6(5) . . . . ? N10 Nd2 N8 C11 -64.8(5) . . . . ? N11 Nd2 N8 C11 -20.4(6) . . . . ? N12 Nd2 N8 C11 81.7(6) . . . . ? N9 Nd2 N8 C11 16.9(5) . . . . ? Se8 Nd2 N8 C11 143.3(5) . . . . ? Se6 Nd2 N8 C11 -129.0(4) . . . . ? Se7 Nd2 N8 C11 92.8(5) 2_666 . . . ? N7 Nd2 N8 C10 -15.1(5) . . . . ? N10 Nd2 N8 C10 65.7(5) . . . . ? N11 Nd2 N8 C10 110.0(5) . . . . ? N12 Nd2 N8 C10 -147.9(5) . . . . ? N9 Nd2 N8 C10 147.4(5) . . . . ? Se8 Nd2 N8 C10 -86.3(5) . . . . ? Se6 Nd2 N8 C10 1.5(6) . . . . ? Se7 Nd2 N8 C10 -136.8(5) 2_666 . . . ? N7 Nd2 N9 C12 33.9(7) . . . . ? N8 Nd2 N9 C12 13.7(5) . . . . ? N10 Nd2 N9 C12 97.3(6) . . . . ? N11 Nd2 N9 C12 164.4(6) . . . . ? N12 Nd2 N9 C12 -135.6(6) . . . . ? Se8 Nd2 N9 C12 -59.7(6) . . . . ? Se6 Nd2 N9 C12 146.2(5) . . . . ? Se7 Nd2 N9 C12 -71.9(6) 2_666 . . . ? N7 Nd2 N10 C13 -156.0(6) . . . . ? N8 Nd2 N10 C13 137.3(6) . . . . ? N11 Nd2 N10 C13 -6.1(5) . . . . ? N12 Nd2 N10 C13 -19.6(6) . . . . ? N9 Nd2 N10 C13 70.5(6) . . . . ? Se8 Nd2 N10 C13 -151.1(5) . . . . ? Se6 Nd2 N10 C13 -84.4(6) . . . . ? Se7 Nd2 N10 C13 90.8(6) 2_666 . . . ? N7 Nd2 N11 C15 -110.1(6) . . . . ? N8 Nd2 N11 C15 159.3(6) . . . . ? N10 Nd2 N11 C15 -151.4(6) . . . . ? N12 Nd2 N11 C15 16.8(6) . . . . ? N9 Nd2 N11 C15 124.0(6) . . . . ? Se8 Nd2 N11 C15 3.8(7) . . . . ? Se6 Nd2 N11 C15 -66.2(6) . . . . ? Se7 Nd2 N11 C15 63.1(6) 2_666 . . . ? N7 Nd2 N11 C14 19.3(7) . . . . ? N8 Nd2 N11 C14 -71.3(6) . . . . ? N10 Nd2 N11 C14 -22.0(5) . . . . ? N12 Nd2 N11 C14 146.2(6) . . . . ? N9 Nd2 N11 C14 -106.6(6) . . . . ? Se8 Nd2 N11 C14 133.2(5) . . . . ? Se6 Nd2 N11 C14 63.2(5) . . . . ? Se7 Nd2 N11 C14 -167.5(5) 2_666 . . . ? N7 Nd2 N12 C16 135.6(5) . . . . ? N8 Nd2 N12 C16 -112.0(6) . . . . ? N10 Nd2 N12 C16 24.6(7) . . . . ? N11 Nd2 N12 C16 11.0(5) . . . . ? N9 Nd2 N12 C16 -56.0(6) . . . . ? Se8 Nd2 N12 C16 -178.1(6) . . . . ? Se6 Nd2 N12 C16 90.3(6) . . . . ? Se7 Nd2 N12 C16 -123.8(6) 2_666 . . . ? Nd1 N1 C1 C2 -36.1(11) . . . . ? C3 N2 C2 C1 -179.0(8) . . . . ? Nd1 N2 C2 C1 -53.6(9) . . . . ? N1 C1 C2 N2 60.5(12) . . . . ? C2 N2 C3 C4 81.0(10) . . . . ? Nd1 N2 C3 C4 -43.1(10) . . . . ? Nd1 N3 C4 C3 -43.6(9) . . . . ? N2 C3 C4 N3 58.0(11) . . . . ? Nd1 N4 C5 C6 36.0(8) . . . . ? C7 N5 C6 C5 -175.8(8) . . . . ? Nd1 N5 C6 C5 47.4(9) . . . . ? N4 C5 C6 N5 -53.8(9) . . . . ? C6 N5 C7 C8 172.4(8) . . . . ? Nd1 N5 C7 C8 -50.7(8) . . . . ? Nd1 N6 C8 C7 -24.0(9) . . . . ? N5 C7 C8 N6 47.4(10) . . . . ? Nd2 N7 C9 C10 44.6(7) . . . . ? N7 C9 C10 N8 -59.2(8) . . . . ? C11 N8 C10 C9 176.3(7) . . . . ? Nd2 N8 C10 C9 45.6(7) . . . . ? C10 N8 C11 C12 -175.9(7) . . . . ? Nd2 N8 C11 C12 -45.9(8) . . . . ? Nd2 N9 C12 C11 -42.7(8) . . . . ? N8 C11 C12 N9 59.1(9) . . . . ? Nd2 N10 C13 C14 34.3(10) . . . . ? N10 C13 C14 N11 -55.6(11) . . . . ? C15 N11 C14 C13 -179.8(8) . . . . ? Nd2 N11 C14 C13 49.3(9) . . . . ? C14 N11 C15 C16 -172.9(8) . . . . ? Nd2 N11 C15 C16 -43.1(10) . . . . ? Nd2 N12 C16 C15 -37.2(9) . . . . ? N11 C15 C16 N12 53.1(11) . . . . ? 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 Se2 0.91 2.85 3.757(7) 173.9 1_455 N2 H2 Se1 0.92 2.88 3.798(8) 173.3 2_755 N3 H3B Se2 0.91 2.95 3.732(7) 144.5 . N4 H4A Se2 0.91 2.77 3.655(6) 165.8 1_455 N4 H4B Se1 0.91 2.93 3.837(7) 172.4 2_755 N5 H5 Se1 0.92 2.77 3.434(6) 129.9 . N6 H6A Se2 0.91 2.88 3.739(6) 157.9 . N6 H6B Se6 0.91 2.87 3.740(7) 160.4 . N7 H7A Se6 0.91 2.60 3.468(6) 159.5 2_766 N7 H7B Se7 0.91 2.76 3.618(6) 156.7 . N8 H8 Se4 0.92 2.72 3.570(6) 153.5 2_666 N9 H9A Se3 0.91 2.83 3.433(8) 124.9 2_756 N10 H10A Se6 0.91 2.78 3.572(7) 146.5 2_766 N10 H10B Se5 0.91 3.06 3.774(7) 136.6 2_766 N12 H12A Se7 0.91 2.71 3.285(6) 121.9 2_666 N12 H12B Se4 0.91 2.98 3.887(6) 173.0 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.962 _refine_diff_density_min -1.525 _refine_diff_density_rms 0.219 #===END data_complex_2c _database_code_depnum_ccdc_archive 'CCDC 797231' #TrackingRef 'cif-of-1a-2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H40 Gd N9 Se4 Sn' _chemical_formula_sum 'C12 H40 Gd N9 Se4 Sn' _chemical_formula_weight 902.31 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c ' _symmetry_space_group_name_Hall '-P 2yc' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 10.3004(15) _cell_length_b 9.4257(11) _cell_length_c 13.875(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.678(4) _cell_angle_gamma 90.00 _cell_volume 1319.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5973 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 8.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1738 _exptl_absorpt_correction_T_max 0.2126 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6439 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2405 _reflns_number_gt 2043 _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^+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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2405 _refine_ls_number_parameters 120 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.056 _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 0.5000 0.65993(5) 0.7500 0.03921(17) Uani 1 2 d S . . Se1 Se 0.67712(7) 0.49572(6) 0.84366(5) 0.04523(19) Uani 1 1 d . . . Se2 Se 0.38773(7) 0.79957(6) 0.86284(4) 0.04873(19) Uani 1 1 d . . . Gd1 Gd 0.5000 0.26937(4) 0.7500 0.03170(14) Uani 1 2 d S . . N1 N 0.4085(5) 0.3461(5) 0.9035(4) 0.0431(12) Uani 1 1 d . . . H1A H 0.4765 0.3465 0.9568 0.052 Uiso 1 1 calc R . . H1B H 0.3775 0.4365 0.8942 0.052 Uiso 1 1 calc R . . N2 N 0.2824(5) 0.1424(5) 0.7657(4) 0.0396(11) Uani 1 1 d . . . H2 H 0.3066 0.0552 0.7934 0.048 Uiso 1 1 calc R . . N3 N 0.4066(5) 0.0970(5) 0.6087(3) 0.0390(11) Uani 1 1 d . . . H3A H 0.3994 0.1450 0.5510 0.047 Uiso 1 1 calc R . . H3B H 0.4674 0.0269 0.6088 0.047 Uiso 1 1 calc R . . C1 C 0.3011(7) 0.2545(7) 0.9255(5) 0.0527(17) Uani 1 1 d . . . H1C H 0.2528 0.3052 0.9690 0.063 Uiso 1 1 calc R . . H1D H 0.3395 0.1686 0.9597 0.063 Uiso 1 1 calc R . . C2 C 0.2071(6) 0.2144(7) 0.8319(5) 0.0529(17) Uani 1 1 d . . . H2A H 0.1384 0.1509 0.8466 0.063 Uiso 1 1 calc R . . H2B H 0.1640 0.2996 0.7998 0.063 Uiso 1 1 calc R . . C3 C 0.1998(6) 0.1144(7) 0.6688(5) 0.0505(16) Uani 1 1 d . . . H3C H 0.1720 0.2042 0.6353 0.061 Uiso 1 1 calc R . . H3D H 0.1202 0.0620 0.6761 0.061 Uiso 1 1 calc R . . C4 C 0.2775(6) 0.0292(6) 0.6092(5) 0.0473(15) Uani 1 1 d . . . H4A H 0.2920 -0.0665 0.6368 0.057 Uiso 1 1 calc R . . H4B H 0.2270 0.0209 0.5415 0.057 Uiso 1 1 calc R . . N4 N 0.028(3) 0.797(3) 0.889(3) 0.216(7) Uani 0.50 1 d PD . . N5 N 0.086(3) 0.634(4) 0.803(3) 0.216(7) Uani 0.50 1 d PD . . N6 N -0.107(3) 0.637(4) 0.573(3) 0.216(7) Uani 0.50 1 d PD . . C5 C 0.023(4) 0.666(4) 0.945(3) 0.216(7) Uani 0.50 1 d PD . . C6 C 0.048(4) 0.544(3) 0.883(3) 0.216(7) Uani 0.50 1 d PD . . C7 C 0.052(3) 0.712(4) 0.715(3) 0.216(7) Uani 0.50 1 d PD . . C8 C 0.019(3) 0.710(4) 0.604(3) 0.216(7) Uani 0.50 1 d PD . . 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 0.0686(4) 0.0206(3) 0.0287(3) 0.000 0.0105(3) 0.000 Se1 0.0602(4) 0.0297(3) 0.0406(4) 0.0001(2) -0.0020(3) -0.0055(3) Se2 0.0793(5) 0.0351(3) 0.0357(4) -0.0032(3) 0.0208(3) 0.0007(3) Gd1 0.0447(2) 0.02341(19) 0.0283(2) 0.000 0.01034(17) 0.000 N1 0.057(3) 0.039(3) 0.035(3) -0.007(2) 0.015(2) 0.001(2) N2 0.043(3) 0.037(2) 0.040(3) -0.002(2) 0.012(2) 0.002(2) N3 0.055(3) 0.032(2) 0.032(3) -0.002(2) 0.014(2) -0.002(2) C1 0.068(4) 0.055(4) 0.043(4) -0.003(3) 0.029(4) 0.003(3) C2 0.048(4) 0.061(4) 0.054(4) -0.011(3) 0.023(3) -0.001(3) C3 0.047(4) 0.046(3) 0.058(4) -0.006(3) 0.007(3) 0.000(3) C4 0.057(4) 0.039(3) 0.046(4) -0.011(3) 0.011(3) -0.002(3) N4 0.181(13) 0.186(16) 0.280(18) -0.051(13) 0.042(15) 0.052(12) N5 0.181(13) 0.186(16) 0.280(18) -0.051(13) 0.042(15) 0.052(12) N6 0.181(13) 0.186(16) 0.280(18) -0.051(13) 0.042(15) 0.052(12) C5 0.181(13) 0.186(16) 0.280(18) -0.051(13) 0.042(15) 0.052(12) C6 0.181(13) 0.186(16) 0.280(18) -0.051(13) 0.042(15) 0.052(12) C7 0.181(13) 0.186(16) 0.280(18) -0.051(13) 0.042(15) 0.052(12) C8 0.181(13) 0.186(16) 0.280(18) -0.051(13) 0.042(15) 0.052(12) _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 Se2 2.5009(7) . ? Sn1 Se2 2.5009(7) 2_656 ? Sn1 Se1 2.5403(7) 2_656 ? Sn1 Se1 2.5403(7) . ? Se1 Gd1 2.9341(7) . ? Gd1 N3 2.578(4) . ? Gd1 N3 2.578(4) 2_656 ? Gd1 N2 2.589(5) . ? Gd1 N2 2.589(4) 2_656 ? Gd1 N1 2.600(4) . ? Gd1 N1 2.600(4) 2_656 ? Gd1 Se1 2.9341(7) 2_656 ? N1 C1 1.482(8) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C3 1.462(8) . ? N2 C2 1.482(7) . ? N2 H2 0.9200 . ? N3 C4 1.476(7) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? C1 C2 1.503(10) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.495(8) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? N4 C8 0.96(5) 2_556 ? N4 C5 1.47(2) . ? N4 C7 1.71(5) 2_556 ? N4 N6 1.74(4) 2_556 ? N5 C7 1.403(19) . ? N5 C6 1.507(19) . ? N5 C7 1.57(3) 2_556 ? N5 N6 1.68(5) 2_556 ? N6 C5 0.98(4) 2_556 ? N6 C6 1.17(4) 2_556 ? N6 C8 1.458(19) . ? N6 N5 1.68(5) 2_556 ? N6 N4 1.74(5) 2_556 ? C5 C8 0.84(5) 2_556 ? C5 N6 0.98(4) 2_556 ? C5 C6 1.488(19) . ? C6 N6 1.17(4) 2_556 ? C6 C8 1.74(5) 2_556 ? C7 C8 1.51(2) . ? C7 N5 1.57(3) 2_556 ? C7 C7 1.58(8) 2_556 ? C7 N4 1.71(5) 2_556 ? C8 C5 0.84(5) 2_556 ? C8 N4 0.96(5) 2_556 ? C8 C6 1.74(5) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 Sn1 Se2 116.49(3) . 2_656 ? Se2 Sn1 Se1 105.41(2) . 2_656 ? Se2 Sn1 Se1 112.06(2) 2_656 2_656 ? Se2 Sn1 Se1 112.06(2) . . ? Se2 Sn1 Se1 105.41(2) 2_656 . ? Se1 Sn1 Se1 104.92(3) 2_656 . ? Sn1 Se1 Gd1 84.18(2) . . ? N3 Gd1 N3 101.8(2) . 2_656 ? N3 Gd1 N2 64.91(14) . . ? N3 Gd1 N2 80.84(15) 2_656 . ? N3 Gd1 N2 80.84(15) . 2_656 ? N3 Gd1 N2 64.91(14) 2_656 2_656 ? N2 Gd1 N2 124.9(2) . 2_656 ? N3 Gd1 N1 131.05(15) . . ? N3 Gd1 N1 72.17(15) 2_656 . ? N2 Gd1 N1 66.18(15) . . ? N2 Gd1 N1 131.37(16) 2_656 . ? N3 Gd1 N1 72.17(15) . 2_656 ? N3 Gd1 N1 131.05(15) 2_656 2_656 ? N2 Gd1 N1 131.37(16) . 2_656 ? N2 Gd1 N1 66.18(15) 2_656 2_656 ? N1 Gd1 N1 147.7(2) . 2_656 ? N3 Gd1 Se1 153.91(10) . . ? N3 Gd1 Se1 91.07(11) 2_656 . ? N2 Gd1 Se1 140.39(10) . . ? N2 Gd1 Se1 84.39(11) 2_656 . ? N1 Gd1 Se1 74.40(11) . . ? N1 Gd1 Se1 82.22(11) 2_656 . ? N3 Gd1 Se1 91.07(11) . 2_656 ? N3 Gd1 Se1 153.91(10) 2_656 2_656 ? N2 Gd1 Se1 84.39(11) . 2_656 ? N2 Gd1 Se1 140.39(10) 2_656 2_656 ? N1 Gd1 Se1 82.22(11) . 2_656 ? N1 Gd1 Se1 74.40(11) 2_656 2_656 ? Se1 Gd1 Se1 86.71(3) . 2_656 ? C1 N1 Gd1 114.6(3) . . ? C1 N1 H1A 108.6 . . ? Gd1 N1 H1A 108.6 . . ? C1 N1 H1B 108.6 . . ? Gd1 N1 H1B 108.6 . . ? H1A N1 H1B 107.6 . . ? C3 N2 C2 111.9(5) . . ? C3 N2 Gd1 111.0(4) . . ? C2 N2 Gd1 114.2(4) . . ? C3 N2 H2 106.4 . . ? C2 N2 H2 106.4 . . ? Gd1 N2 H2 106.4 . . ? C4 N3 Gd1 117.9(3) . . ? C4 N3 H3A 107.8 . . ? Gd1 N3 H3A 107.8 . . ? C4 N3 H3B 107.8 . . ? Gd1 N3 H3B 107.8 . . ? H3A N3 H3B 107.2 . . ? N1 C1 C2 110.2(5) . . ? N1 C1 H1C 109.6 . . ? C2 C1 H1C 109.6 . . ? N1 C1 H1D 109.6 . . ? C2 C1 H1D 109.6 . . ? H1C C1 H1D 108.1 . . ? N2 C2 C1 109.0(5) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N2 C3 C4 109.2(5) . . ? N2 C3 H3C 109.8 . . ? C4 C3 H3C 109.8 . . ? N2 C3 H3D 109.8 . . ? C4 C3 H3D 109.8 . . ? H3C C3 H3D 108.3 . . ? N3 C4 C3 110.7(5) . . ? N3 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C8 N4 C5 33(3) 2_556 . ? C8 N4 C7 62(3) 2_556 2_556 ? C5 N4 C7 89(2) . 2_556 ? C8 N4 N6 57(2) 2_556 2_556 ? C5 N4 N6 34.4(17) . 2_556 ? C7 N4 N6 88.2(15) 2_556 2_556 ? C7 N5 C6 151(4) . . ? C7 N5 C7 64(3) . 2_556 ? C6 N5 C7 91(3) . 2_556 ? C7 N5 N6 147(3) . 2_556 ? C6 N5 N6 42.7(17) . 2_556 ? C7 N5 N6 95(2) 2_556 2_556 ? C5 N6 C6 87(3) 2_556 2_556 ? C5 N6 C8 34(3) 2_556 . ? C6 N6 C8 82(3) 2_556 . ? C5 N6 N5 109(3) 2_556 2_556 ? C6 N6 N5 61(2) 2_556 2_556 ? C8 N6 N5 77.4(16) . 2_556 ? C5 N6 N4 57(2) 2_556 2_556 ? C6 N6 N4 109(3) 2_556 2_556 ? C8 N6 N4 33.6(19) . 2_556 ? N5 N6 N4 75(2) 2_556 2_556 ? C8 C5 N6 106(5) 2_556 2_556 ? C8 C5 N4 39(3) 2_556 . ? N6 C5 N4 88(3) 2_556 . ? C8 C5 C6 92(4) 2_556 . ? N6 C5 C6 52(3) 2_556 . ? N4 C5 C6 108.3(18) . . ? N6 C6 C5 41(2) 2_556 . ? N6 C6 N5 77(3) 2_556 . ? C5 C6 N5 94.9(19) . . ? N6 C6 C8 56.2(18) 2_556 2_556 ? C5 C6 C8 29(2) . 2_556 ? N5 C6 C8 75(2) . 2_556 ? N5 C7 C8 148(4) . . ? N5 C7 N5 88(4) . 2_556 ? C8 C7 N5 80(2) . 2_556 ? N5 C7 C7 63(2) . 2_556 ? C8 C7 C7 126(3) . 2_556 ? N5 C7 C7 52.9(17) 2_556 2_556 ? N5 C7 N4 166(4) . 2_556 ? C8 C7 N4 34(2) . 2_556 ? N5 C7 N4 79(2) 2_556 2_556 ? C7 C7 N4 104(3) 2_556 2_556 ? C5 C8 N4 108(5) 2_556 2_556 ? C5 C8 N6 41(3) 2_556 . ? N4 C8 N6 89(3) 2_556 . ? C5 C8 C7 143(4) 2_556 . ? N4 C8 C7 84(4) 2_556 . ? N6 C8 C7 107.9(19) . . ? C5 C8 C6 59(3) 2_556 2_556 ? N4 C8 C6 122(4) 2_556 2_556 ? N6 C8 C6 42(2) . 2_556 ? C7 C8 C6 85(3) . 2_556 ? 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 Gd1 113.88(2) . . . . ? Se2 Sn1 Se1 Gd1 -118.47(2) 2_656 . . . ? Se1 Sn1 Se1 Gd1 0.0 2_656 . . . ? Sn1 Se1 Gd1 N3 85.7(2) . . . . ? Sn1 Se1 Gd1 N3 -153.98(10) . . . 2_656 ? Sn1 Se1 Gd1 N2 -77.11(17) . . . . ? Sn1 Se1 Gd1 N2 141.36(11) . . . 2_656 ? Sn1 Se1 Gd1 N1 -82.84(12) . . . . ? Sn1 Se1 Gd1 N1 74.69(11) . . . 2_656 ? Sn1 Se1 Gd1 Se1 0.0 . . . 2_656 ? N3 Gd1 N1 C1 14.8(5) . . . . ? N3 Gd1 N1 C1 -75.5(4) 2_656 . . . ? N2 Gd1 N1 C1 12.2(4) . . . . ? N2 Gd1 N1 C1 -104.2(4) 2_656 . . . ? N1 Gd1 N1 C1 143.0(4) 2_656 . . . ? Se1 Gd1 N1 C1 -171.8(4) . . . . ? Se1 Gd1 N1 C1 99.4(4) 2_656 . . . ? N3 Gd1 N2 C3 -31.8(3) . . . . ? N3 Gd1 N2 C3 -139.5(4) 2_656 . . . ? N2 Gd1 N2 C3 -89.0(4) 2_656 . . . ? N1 Gd1 N2 C3 146.0(4) . . . . ? N1 Gd1 N2 C3 -1.4(4) 2_656 . . . ? Se1 Gd1 N2 C3 140.0(3) . . . . ? Se1 Gd1 N2 C3 62.1(4) 2_656 . . . ? N3 Gd1 N2 C2 -159.4(5) . . . . ? N3 Gd1 N2 C2 92.8(4) 2_656 . . . ? N2 Gd1 N2 C2 143.3(4) 2_656 . . . ? N1 Gd1 N2 C2 18.4(4) . . . . ? N1 Gd1 N2 C2 -129.1(4) 2_656 . . . ? Se1 Gd1 N2 C2 12.3(5) . . . . ? Se1 Gd1 N2 C2 -65.6(4) 2_656 . . . ? N3 Gd1 N3 C4 78.4(4) 2_656 . . . ? N2 Gd1 N3 C4 4.5(4) . . . . ? N2 Gd1 N3 C4 140.2(4) 2_656 . . . ? N1 Gd1 N3 C4 1.8(5) . . . . ? N1 Gd1 N3 C4 -152.0(4) 2_656 . . . ? Se1 Gd1 N3 C4 -163.5(3) . . . . ? Se1 Gd1 N3 C4 -78.8(4) 2_656 . . . ? Gd1 N1 C1 C2 -40.9(6) . . . . ? C3 N2 C2 C1 -173.6(5) . . . . ? Gd1 N2 C2 C1 -46.4(6) . . . . ? N1 C1 C2 N2 57.3(7) . . . . ? C2 N2 C3 C4 -174.4(5) . . . . ? Gd1 N2 C3 C4 56.6(5) . . . . ? Gd1 N3 C4 C3 22.3(7) . . . . ? N2 C3 C4 N3 -51.7(7) . . . . ? C7 N4 C5 C8 -31(4) 2_556 . . 2_556 ? N6 N4 C5 C8 -118(7) 2_556 . . 2_556 ? C8 N4 C5 N6 118(7) 2_556 . . 2_556 ? C7 N4 C5 N6 88(4) 2_556 . . 2_556 ? C8 N4 C5 C6 69(6) 2_556 . . . ? C7 N4 C5 C6 39(4) 2_556 . . . ? N6 N4 C5 C6 -49(3) 2_556 . . . ? C8 C5 C6 N6 108(6) 2_556 . . 2_556 ? N4 C5 C6 N6 72(4) . . . 2_556 ? C8 C5 C6 N5 45(5) 2_556 . . . ? N6 C5 C6 N5 -63(4) 2_556 . . . ? N4 C5 C6 N5 9(4) . . . . ? N6 C5 C6 C8 -108(6) 2_556 . . 2_556 ? N4 C5 C6 C8 -36(3) . . . 2_556 ? C7 N5 C6 N6 -126(7) . . . 2_556 ? C7 N5 C6 N6 -96(3) 2_556 . . 2_556 ? C7 N5 C6 C5 -89(7) . . . . ? C7 N5 C6 C5 -59(3) 2_556 . . . ? N6 N5 C6 C5 37(2) 2_556 . . . ? C7 N5 C6 C8 -68(7) . . . 2_556 ? C7 N5 C6 C8 -38(2) 2_556 . . 2_556 ? N6 N5 C6 C8 58.1(19) 2_556 . . 2_556 ? C6 N5 C7 C8 -82(9) . . . . ? C7 N5 C7 C8 -115(6) 2_556 . . . ? N6 N5 C7 C8 -171(4) 2_556 . . . ? C6 N5 C7 N5 -15(7) . . . 2_556 ? C7 N5 C7 N5 -49(2) 2_556 . . 2_556 ? N6 N5 C7 N5 -104(6) 2_556 . . 2_556 ? C6 N5 C7 C7 34(6) . . . 2_556 ? N6 N5 C7 C7 -55(5) 2_556 . . 2_556 ? C6 N5 C7 N4 7(19) . . . 2_556 ? C7 N5 C7 N4 -27(14) 2_556 . . 2_556 ? N6 N5 C7 N4 -82(16) 2_556 . . 2_556 ? C6 N6 C8 C5 96(5) 2_556 . . 2_556 ? N5 N6 C8 C5 158(6) 2_556 . . 2_556 ? N4 N6 C8 C5 -120(7) 2_556 . . 2_556 ? C5 N6 C8 N4 120(7) 2_556 . . 2_556 ? C6 N6 C8 N4 -144(5) 2_556 . . 2_556 ? N5 N6 C8 N4 -82(4) 2_556 . . 2_556 ? C5 N6 C8 C7 -157(7) 2_556 . . . ? C6 N6 C8 C7 -60(4) 2_556 . . . ? N5 N6 C8 C7 1(3) 2_556 . . . ? N4 N6 C8 C7 84(4) 2_556 . . . ? C5 N6 C8 C6 -96(5) 2_556 . . 2_556 ? N5 N6 C8 C6 62(2) 2_556 . . 2_556 ? N4 N6 C8 C6 144(5) 2_556 . . 2_556 ? N5 C7 C8 C5 42(12) . . . 2_556 ? N5 C7 C8 C5 -27(9) 2_556 . . 2_556 ? C7 C7 C8 C5 -55(10) 2_556 . . 2_556 ? N4 C7 C8 C5 -113(9) 2_556 . . 2_556 ? N5 C7 C8 N4 155(7) . . . 2_556 ? N5 C7 C8 N4 86(3) 2_556 . . 2_556 ? C7 C7 C8 N4 59(4) 2_556 . . 2_556 ? N5 C7 C8 N6 67(7) . . . . ? N5 C7 C8 N6 -1(3) 2_556 . . . ? C7 C7 C8 N6 -29(4) 2_556 . . . ? N4 C7 C8 N6 -88(3) 2_556 . . . ? N5 C7 C8 C6 32(7) . . . 2_556 ? N5 C7 C8 C6 -37(2) 2_556 . . 2_556 ? C7 C7 C8 C6 -65(3) 2_556 . . 2_556 ? N4 C7 C8 C6 -123(4) 2_556 . . 2_556 ? 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 N2 H2 Se2 0.92 2.67 3.584(5) 175.5 1_545 N3 H3A Se2 0.91 2.64 3.516(5) 161.4 4_565 N3 H3B Se2 0.91 2.60 3.488(5) 166.8 2_646 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.107 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.199