data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dingxian Jia' _publ_contact_author_address ; College of Chemistry and Chemical Engineering Suzhou University (Dushu Lake Campus) P.O. Box 174, Ren Ai Road Suzhou 215123 CHINA ; _publ_contact_author_email JIADINGXIAN@SUDA.EDU.CN _publ_section_title ; Direct Solvothermal Growth, Crystal Structures, and Optical Properties of One-Dimensional Lanthanide Selenidoarsenate (V) Polymers [Ln(dien)2(?3-AsSe4)] (Ln = Nd, Sm): The First Example of an AsSe43- Anion Acting as a Ligand to a Lanthanide Complex ; loop_ _publ_author_name 'Dingxian Jia' 'Jie Dai' 'Jie Deng' 'Yong Zhang' 'Aimei Zhu' data_1 _database_code_depnum_ccdc_archive 'CCDC 636254' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 As N6 Nd Se4' _chemical_formula_sum 'C8 H26 As N6 Nd Se4' _chemical_formula_weight 741.35 _chemical_absolute_configuration ad 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' As As 0.0499 2.0058 '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' Nd Nd -0.1943 3.0179 '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 orthorhombic _symmetry_space_group_name_H-M 'i b a 2' _symmetry_space_group_name_Hall 'i 2 -2c' _symmetry_Int_Tables_number 45 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1, z+1/2' 'x+1, -y+1, z+1/2' '-x+1/2, -y+1/2, z+1/2' _cell_length_a 16.542(2) _cell_length_b 26.674(4) _cell_length_c 8.7880(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3877.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7918 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 11.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1627 _exptl_absorpt_correction_T_max 0.3548 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 18763 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.33 _reflns_number_total 3559 _reflns_number_gt 3419 _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^)+(0.0221P)^2^+15.8142P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.033(19) _refine_ls_number_reflns 3559 _refine_ls_number_parameters 182 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0588 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 Nd1 Nd 0.25335(2) 0.633464(13) 0.13390(4) 0.01557(9) Uani 1 1 d . . . Se1 Se 0.34376(4) 0.59728(3) 0.42639(9) 0.02396(17) Uani 1 1 d . . . Se2 Se 0.17445(4) 0.68394(3) 0.42223(8) 0.02085(16) Uani 1 1 d . . . Se3 Se 0.29499(5) 0.67341(3) 0.78298(9) 0.02504(17) Uani 1 1 d . . . Se4 Se 0.16004(5) 0.56486(3) 0.65871(9) 0.02664(17) Uani 1 1 d . . . As1 As 0.24316(4) 0.62898(3) 0.58001(8) 0.01690(17) Uani 1 1 d . . . N1 N 0.4064(4) 0.6220(2) 0.0590(7) 0.0226(13) Uani 1 1 d . . . H1 H 0.4086 0.6339 -0.0403 0.027 Uiso 1 1 calc R . . N2 N 0.2891(4) 0.5492(2) -0.0123(7) 0.0258(14) Uani 1 1 d . . . H2A H 0.2776 0.5226 0.0509 0.031 Uiso 1 1 calc R . . H2B H 0.2557 0.5466 -0.0956 0.031 Uiso 1 1 calc R . . N3 N 0.3497(3) 0.7086(2) 0.1945(7) 0.0258(14) Uani 1 1 d . . . H3A H 0.3265 0.7371 0.1546 0.031 Uiso 1 1 calc R . . H3B H 0.3507 0.7126 0.2985 0.031 Uiso 1 1 calc R . . N4 N 0.1118(4) 0.6177(2) 0.0050(7) 0.0282(15) Uani 1 1 d . . . H4 H 0.1210 0.6152 -0.0991 0.034 Uiso 1 1 calc R . . N5 N 0.1669(4) 0.5617(2) 0.2562(7) 0.0280(15) Uani 1 1 d . . . H5A H 0.1894 0.5314 0.2292 0.034 Uiso 1 1 calc R . . H5B H 0.1704 0.5644 0.3603 0.034 Uiso 1 1 calc R . . N6 N 0.1777(4) 0.7164(2) 0.0567(7) 0.0277(14) Uani 1 1 d . . . H6A H 0.1672 0.7349 0.1430 0.033 Uiso 1 1 calc R . . H6B H 0.2109 0.7353 -0.0048 0.033 Uiso 1 1 calc R . . C1 C 0.4293(5) 0.5695(3) 0.0441(10) 0.036(2) Uani 1 1 d . . . H1A H 0.4266 0.5528 0.1446 0.043 Uiso 1 1 calc R . . H1B H 0.4855 0.5670 0.0062 0.043 Uiso 1 1 calc R . . C2 C 0.3733(5) 0.5444(3) -0.0642(10) 0.0362(19) Uani 1 1 d . . . H2C H 0.3789 0.5597 -0.1662 0.043 Uiso 1 1 calc R . . H2D H 0.3876 0.5084 -0.0726 0.043 Uiso 1 1 calc R . . C3 C 0.4643(4) 0.6548(3) 0.1422(11) 0.0315(17) Uani 1 1 d . . . H3C H 0.4704 0.6429 0.2482 0.038 Uiso 1 1 calc R . . H3D H 0.5179 0.6535 0.0923 0.038 Uiso 1 1 calc R . . C4 C 0.4334(4) 0.7068(3) 0.1416(11) 0.0318(17) Uani 1 1 d . . . H4A H 0.4676 0.7279 0.2086 0.038 Uiso 1 1 calc R . . H4B H 0.4366 0.7206 0.0372 0.038 Uiso 1 1 calc R . . C5 C 0.0728(6) 0.5691(4) 0.0538(10) 0.045(2) Uani 1 1 d . . . H5C H 0.0147 0.5698 0.0272 0.053 Uiso 1 1 calc R . . H5D H 0.0981 0.5409 -0.0018 0.053 Uiso 1 1 calc R . . C6 C 0.0814(5) 0.5612(3) 0.2135(11) 0.042(2) Uani 1 1 d . . . H6C H 0.0571 0.5285 0.2416 0.050 Uiso 1 1 calc R . . H6D H 0.0523 0.5878 0.2697 0.050 Uiso 1 1 calc R . . C7 C 0.0585(5) 0.6599(4) 0.0273(11) 0.049(2) Uani 1 1 d . . . H7A H 0.0445 0.6630 0.1365 0.059 Uiso 1 1 calc R . . H7B H 0.0078 0.6548 -0.0306 0.059 Uiso 1 1 calc R . . C8 C 0.0993(5) 0.7065(4) -0.0256(11) 0.053(3) Uani 1 1 d . . . H8A H 0.0625 0.7353 -0.0100 0.063 Uiso 1 1 calc R . . H8B H 0.1102 0.7038 -0.1360 0.063 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 Nd1 0.01412(17) 0.01466(17) 0.01793(18) -0.00121(18) -0.00073(16) -0.00045(14) Se1 0.0221(4) 0.0284(4) 0.0214(4) -0.0006(3) -0.0007(3) 0.0077(3) Se2 0.0231(4) 0.0203(3) 0.0192(3) -0.0003(3) -0.0005(3) 0.0040(3) Se3 0.0353(4) 0.0231(4) 0.0167(3) -0.0011(3) -0.0015(3) -0.0041(3) Se4 0.0349(4) 0.0224(4) 0.0226(4) 0.0010(3) 0.0027(3) -0.0099(3) As1 0.0211(4) 0.0155(3) 0.0140(3) 0.0002(3) 0.0015(3) -0.0007(3) N1 0.021(3) 0.024(3) 0.023(3) 0.000(3) -0.001(3) -0.002(3) N2 0.028(4) 0.024(3) 0.025(3) -0.003(3) 0.003(3) -0.005(3) N3 0.024(3) 0.026(3) 0.028(3) -0.002(3) 0.003(3) 0.003(3) N4 0.015(3) 0.049(4) 0.020(3) -0.007(3) -0.001(3) 0.001(3) N5 0.033(4) 0.021(3) 0.030(4) -0.005(3) 0.002(3) -0.010(3) N6 0.035(4) 0.026(3) 0.022(3) 0.005(3) 0.008(3) 0.000(3) C1 0.027(4) 0.029(4) 0.051(6) -0.009(4) 0.005(4) 0.006(4) C2 0.032(4) 0.024(4) 0.052(5) -0.008(4) 0.013(4) 0.005(3) C3 0.015(3) 0.041(4) 0.038(4) -0.007(4) -0.001(4) -0.002(3) C4 0.024(4) 0.031(4) 0.041(4) -0.005(4) 0.007(4) -0.009(3) C5 0.031(5) 0.051(6) 0.051(6) 0.006(5) -0.003(4) -0.013(4) C6 0.026(4) 0.032(5) 0.067(6) 0.008(4) 0.009(4) -0.003(4) C7 0.028(5) 0.062(6) 0.057(6) -0.010(5) -0.008(5) 0.007(4) C8 0.023(5) 0.075(7) 0.060(6) 0.045(5) 0.001(4) 0.017(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N3 2.616(6) . ? Nd1 N5 2.620(6) . ? Nd1 N6 2.632(6) . ? Nd1 N1 2.633(6) . ? Nd1 N4 2.635(6) . ? Nd1 N2 2.655(6) . ? Nd1 Se1 3.1266(9) . ? Nd1 Se2 3.1523(9) . ? Nd1 Se3 3.3347(10) 1_554 ? Se1 As1 2.3037(10) . ? Se2 As1 2.3160(10) . ? Se3 As1 2.3068(11) . ? Se3 Nd1 3.3347(10) 1_556 ? Se4 As1 2.3008(10) . ? N1 C1 1.457(9) . ? N1 C3 1.489(9) . ? N1 H1 0.9300 . ? N2 C2 1.472(10) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C4 1.462(8) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N4 C7 1.444(10) . ? N4 C5 1.509(10) . ? N4 H4 0.9300 . ? N5 C6 1.464(10) . ? N5 H5A 0.9200 . ? N5 H5B 0.9200 . ? N6 C8 1.508(11) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? C1 C2 1.488(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 C4 1.479(10) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.427(12) . ? C5 H5C 0.9900 . ? C5 H5D 0.9900 . ? C6 H6C 0.9900 . ? C6 H6D 0.9900 . ? C7 C8 1.490(13) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 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 N3 Nd1 N5 144.0(2) . . ? N3 Nd1 N6 72.40(19) . . ? N5 Nd1 N6 117.45(19) . . ? N3 Nd1 N1 63.56(18) . . ? N5 Nd1 N1 122.79(19) . . ? N6 Nd1 N1 119.40(19) . . ? N3 Nd1 N4 138.71(19) . . ? N5 Nd1 N4 64.8(2) . . ? N6 Nd1 N4 66.5(2) . . ? N1 Nd1 N4 136.73(19) . . ? N3 Nd1 N2 127.71(18) . . ? N5 Nd1 N2 72.61(19) . . ? N6 Nd1 N2 133.87(19) . . ? N1 Nd1 N2 64.31(19) . . ? N4 Nd1 N2 81.6(2) . . ? N3 Nd1 Se1 77.17(14) . . ? N5 Nd1 Se1 72.43(14) . . ? N6 Nd1 Se1 134.35(14) . . ? N1 Nd1 Se1 73.12(14) . . ? N4 Nd1 Se1 136.81(14) . . ? N2 Nd1 Se1 91.72(14) . . ? N3 Nd1 Se2 76.18(13) . . ? N5 Nd1 Se2 75.92(14) . . ? N6 Nd1 Se2 69.57(13) . . ? N1 Nd1 Se2 130.44(13) . . ? N4 Nd1 Se2 92.63(14) . . ? N2 Nd1 Se2 147.41(13) . . ? Se1 Nd1 Se2 70.68(2) . . ? N3 Nd1 Se3 79.48(13) . 1_554 ? N5 Nd1 Se3 136.51(14) . 1_554 ? N6 Nd1 Se3 65.87(13) . 1_554 ? N1 Nd1 Se3 66.90(14) . 1_554 ? N4 Nd1 Se3 80.63(14) . 1_554 ? N2 Nd1 Se3 77.12(13) . 1_554 ? Se1 Nd1 Se3 139.47(2) . 1_554 ? Se2 Nd1 Se3 133.82(2) . 1_554 ? As1 Se1 Nd1 91.31(3) . . ? As1 Se2 Nd1 90.44(3) . . ? As1 Se3 Nd1 118.30(3) . 1_556 ? Se4 As1 Se1 109.57(4) . . ? Se4 As1 Se3 111.81(4) . . ? Se1 As1 Se3 111.92(4) . . ? Se4 As1 Se2 110.93(4) . . ? Se1 As1 Se2 103.65(4) . . ? Se3 As1 Se2 108.67(4) . . ? C1 N1 C3 116.2(6) . . ? C1 N1 Nd1 112.7(4) . . ? C3 N1 Nd1 115.3(4) . . ? C1 N1 H1 103.5 . . ? C3 N1 H1 103.5 . . ? Nd1 N1 H1 103.5 . . ? C2 N2 Nd1 115.8(4) . . ? 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 . . ? C4 N3 Nd1 119.2(4) . . ? C4 N3 H3A 107.5 . . ? Nd1 N3 H3A 107.5 . . ? C4 N3 H3B 107.5 . . ? Nd1 N3 H3B 107.5 . . ? H3A N3 H3B 107.0 . . ? C7 N4 C5 111.7(7) . . ? C7 N4 Nd1 111.1(5) . . ? C5 N4 Nd1 113.3(5) . . ? C7 N4 H4 106.8 . . ? C5 N4 H4 106.8 . . ? Nd1 N4 H4 106.8 . . ? C6 N5 Nd1 115.4(5) . . ? C6 N5 H5A 108.4 . . ? Nd1 N5 H5A 108.4 . . ? C6 N5 H5B 108.4 . . ? Nd1 N5 H5B 108.4 . . ? H5A N5 H5B 107.5 . . ? C8 N6 Nd1 112.7(5) . . ? C8 N6 H6A 109.1 . . ? Nd1 N6 H6A 109.1 . . ? C8 N6 H6B 109.1 . . ? Nd1 N6 H6B 109.1 . . ? H6A N6 H6B 107.8 . . ? N1 C1 C2 109.1(7) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 110.6(7) . . ? N2 C2 H2C 109.5 . . ? C1 C2 H2C 109.5 . . ? N2 C2 H2D 109.5 . . ? C1 C2 H2D 109.5 . . ? H2C C2 H2D 108.1 . . ? C4 C3 N1 109.2(6) . . ? C4 C3 H3C 109.8 . . ? N1 C3 H3C 109.8 . . ? C4 C3 H3D 109.8 . . ? N1 C3 H3D 109.8 . . ? H3C C3 H3D 108.3 . . ? N3 C4 C3 110.9(6) . . ? N3 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C6 C5 N4 111.4(8) . . ? C6 C5 H5C 109.4 . . ? N4 C5 H5C 109.4 . . ? C6 C5 H5D 109.4 . . ? N4 C5 H5D 109.4 . . ? H5C C5 H5D 108.0 . . ? C5 C6 N5 110.3(8) . . ? C5 C6 H6C 109.6 . . ? N5 C6 H6C 109.6 . . ? C5 C6 H6D 109.6 . . ? N5 C6 H6D 109.6 . . ? H6C C6 H6D 108.1 . . ? N4 C7 C8 109.4(7) . . ? N4 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N4 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C7 C8 N6 112.7(7) . . ? C7 C8 H8A 109.0 . . ? N6 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? N6 C8 H8B 109.0 . . ? H8A C8 H8B 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 N3 Nd1 Se1 As1 92.62(13) . . . . ? N5 Nd1 Se1 As1 -67.87(15) . . . . ? N6 Nd1 Se1 As1 43.64(19) . . . . ? N1 Nd1 Se1 As1 158.53(13) . . . . ? N4 Nd1 Se1 As1 -59.4(2) . . . . ? N2 Nd1 Se1 As1 -139.01(14) . . . . ? Se2 Nd1 Se1 As1 12.97(3) . . . . ? Se3 Nd1 Se1 As1 148.94(3) 1_554 . . . ? N3 Nd1 Se2 As1 -93.91(14) . . . . ? N5 Nd1 Se2 As1 63.11(14) . . . . ? N6 Nd1 Se2 As1 -169.98(15) . . . . ? N1 Nd1 Se2 As1 -58.21(17) . . . . ? N4 Nd1 Se2 As1 126.33(15) . . . . ? N2 Nd1 Se2 As1 47.8(3) . . . . ? Se1 Nd1 Se2 As1 -12.89(3) . . . . ? Se3 Nd1 Se2 As1 -154.14(3) 1_554 . . . ? Nd1 Se1 As1 Se4 101.21(4) . . . . ? Nd1 Se1 As1 Se3 -134.17(4) . . . . ? Nd1 Se1 As1 Se2 -17.25(3) . . . . ? Nd1 Se3 As1 Se4 4.30(5) 1_556 . . . ? Nd1 Se3 As1 Se1 -119.07(4) 1_556 . . . ? Nd1 Se3 As1 Se2 127.07(4) 1_556 . . . ? Nd1 Se2 As1 Se4 -100.41(4) . . . . ? Nd1 Se2 As1 Se1 17.10(3) . . . . ? Nd1 Se2 As1 Se3 136.28(3) . . . . ? N3 Nd1 N1 C1 158.3(6) . . . . ? N5 Nd1 N1 C1 19.3(6) . . . . ? N6 Nd1 N1 C1 -153.6(5) . . . . ? N4 Nd1 N1 C1 -67.6(6) . . . . ? N2 Nd1 N1 C1 -25.9(5) . . . . ? Se1 Nd1 N1 C1 74.5(5) . . . . ? Se2 Nd1 N1 C1 119.0(5) . . . . ? Se3 Nd1 N1 C1 -112.2(5) 1_554 . . . ? N3 Nd1 N1 C3 21.7(5) . . . . ? N5 Nd1 N1 C3 -117.3(5) . . . . ? N6 Nd1 N1 C3 69.8(5) . . . . ? N4 Nd1 N1 C3 155.8(5) . . . . ? N2 Nd1 N1 C3 -162.5(6) . . . . ? Se1 Nd1 N1 C3 -62.1(5) . . . . ? Se2 Nd1 N1 C3 -17.5(6) . . . . ? Se3 Nd1 N1 C3 111.2(5) 1_554 . . . ? N3 Nd1 N2 C2 0.4(6) . . . . ? N5 Nd1 N2 C2 -145.7(6) . . . . ? N6 Nd1 N2 C2 102.7(6) . . . . ? N1 Nd1 N2 C2 -4.4(5) . . . . ? N4 Nd1 N2 C2 148.2(6) . . . . ? Se1 Nd1 N2 C2 -74.7(5) . . . . ? Se2 Nd1 N2 C2 -130.1(5) . . . . ? Se3 Nd1 N2 C2 66.0(5) 1_554 . . . ? N5 Nd1 N3 C4 116.5(6) . . . . ? N6 Nd1 N3 C4 -130.8(6) . . . . ? N1 Nd1 N3 C4 6.3(5) . . . . ? N4 Nd1 N3 C4 -125.4(5) . . . . ? N2 Nd1 N3 C4 1.6(6) . . . . ? Se1 Nd1 N3 C4 83.7(5) . . . . ? Se2 Nd1 N3 C4 156.6(6) . . . . ? Se3 Nd1 N3 C4 -63.0(5) 1_554 . . . ? N3 Nd1 N4 C7 -31.7(7) . . . . ? N5 Nd1 N4 C7 113.3(6) . . . . ? N6 Nd1 N4 C7 -26.1(5) . . . . ? N1 Nd1 N4 C7 -134.7(5) . . . . ? N2 Nd1 N4 C7 -172.0(6) . . . . ? Se1 Nd1 N4 C7 104.4(6) . . . . ? Se2 Nd1 N4 C7 40.2(6) . . . . ? Se3 Nd1 N4 C7 -93.8(6) 1_554 . . . ? N3 Nd1 N4 C5 -158.4(5) . . . . ? N5 Nd1 N4 C5 -13.3(5) . . . . ? N6 Nd1 N4 C5 -152.8(6) . . . . ? N1 Nd1 N4 C5 98.6(6) . . . . ? N2 Nd1 N4 C5 61.3(5) . . . . ? Se1 Nd1 N4 C5 -22.2(6) . . . . ? Se2 Nd1 N4 C5 -86.5(5) . . . . ? Se3 Nd1 N4 C5 139.5(5) 1_554 . . . ? N3 Nd1 N5 C6 124.5(5) . . . . ? N6 Nd1 N5 C6 26.7(6) . . . . ? N1 Nd1 N5 C6 -146.3(5) . . . . ? N4 Nd1 N5 C6 -15.5(5) . . . . ? N2 Nd1 N5 C6 -104.2(6) . . . . ? Se1 Nd1 N5 C6 158.2(6) . . . . ? Se2 Nd1 N5 C6 84.3(5) . . . . ? Se3 Nd1 N5 C6 -56.3(6) 1_554 . . . ? N3 Nd1 N6 C8 172.5(6) . . . . ? N5 Nd1 N6 C8 -45.1(6) . . . . ? N1 Nd1 N6 C8 128.2(5) . . . . ? N4 Nd1 N6 C8 -3.6(5) . . . . ? N2 Nd1 N6 C8 46.7(6) . . . . ? Se1 Nd1 N6 C8 -137.0(5) . . . . ? Se2 Nd1 N6 C8 -106.0(5) . . . . ? Se3 Nd1 N6 C8 86.4(5) 1_554 . . . ? C3 N1 C1 C2 -169.9(7) . . . . ? Nd1 N1 C1 C2 54.0(8) . . . . ? Nd1 N2 C2 C1 33.3(8) . . . . ? N1 C1 C2 N2 -57.6(9) . . . . ? C1 N1 C3 C4 177.8(7) . . . . ? Nd1 N1 C3 C4 -47.2(8) . . . . ? Nd1 N3 C4 C3 -33.2(9) . . . . ? N1 C3 C4 N3 51.3(9) . . . . ? C7 N4 C5 C6 -83.9(10) . . . . ? Nd1 N4 C5 C6 42.5(9) . . . . ? N4 C5 C6 N5 -57.1(10) . . . . ? Nd1 N5 C6 C5 44.3(9) . . . . ? C5 N4 C7 C8 -178.8(7) . . . . ? Nd1 N4 C7 C8 53.7(8) . . . . ? N4 C7 C8 N6 -58.7(10) . . . . ? Nd1 N6 C8 C7 32.8(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 C3 H3C Se1 0.99 2.88 3.545(8) 124.9 . C2 H2D Se1 0.99 2.91 3.810(8) 151.5 7_454 C1 H1B Se1 0.99 3.02 3.964(8) 159.8 6_544 C1 H1A Se1 0.99 3.07 3.720(9) 124.5 . N6 H6B Se2 0.92 2.94 3.800(6) 155.9 8_564 N6 H6B Se3 0.92 2.85 3.297(6) 111.1 1_554 N6 H6A Se2 0.92 2.81 3.327(6) 117.0 . N6 H6A Se3 0.92 2.81 3.576(6) 141.6 8_564 N5 H5B Se4 0.92 2.63 3.540(6) 171.5 . N5 H5A Se4 0.92 2.68 3.483(6) 145.7 7_454 N4 H4 Se4 0.93 2.60 3.447(6) 152.1 1_554 N3 H3A Se2 0.92 2.93 3.754(6) 149.3 8_564 N2 H2B Se4 0.92 2.72 3.618(6) 165.4 1_554 N1 H1 Se3 0.93 2.66 3.341(6) 131.0 1_554 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.039 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.135 # Attachment 'CIF-compound_2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 636255' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 As N6 Se4 Sm' _chemical_formula_sum 'C8 H26 As N6 Se4 Sm' _chemical_formula_weight 747.46 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' As As 0.0499 2.0058 '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' Sm Sm -0.1638 3.4418 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 8.8353(8) _cell_length_b 16.2766(17) _cell_length_c 26.525(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3814.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 10625 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 12.434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2131 _exptl_absorpt_correction_T_max 0.4008 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 35371 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3493 _reflns_number_gt 3166 _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^)+(0.0172P)^2^+67.7253P] 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 3493 _refine_ls_number_parameters 178 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.261 _refine_ls_restrained_S_all 1.261 _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 Sm1 Sm 0.04512(6) 0.24303(3) 0.616991(19) 0.01761(15) Uani 1 1 d . . . Se1 Se 0.32789(12) 0.16480(7) 0.56556(4) 0.0220(3) Uani 1 1 d . . . Se2 Se 0.33631(12) 0.33952(7) 0.65027(4) 0.0262(3) Uani 1 1 d . . . Se3 Se 0.69143(12) 0.28380(7) 0.57485(4) 0.0269(3) Uani 1 1 d . . . Se4 Se 0.56507(12) 0.15164(7) 0.68484(4) 0.0243(3) Uani 1 1 d . . . As1 As 0.48711(11) 0.23527(7) 0.61965(4) 0.0187(2) Uani 1 1 d . . . N1 N -0.0819(10) 0.0999(5) 0.6314(3) 0.023(2) Uani 1 1 d . . . H1 H -0.1855 0.1093 0.6340 0.028 Uiso 1 1 calc R . . N2 N -0.0347(10) 0.1691(6) 0.5341(3) 0.025(2) Uani 1 1 d . . . H2A H -0.0952 0.2041 0.5158 0.030 Uiso 1 1 calc R . . H2B H 0.0509 0.1592 0.5153 0.030 Uiso 1 1 calc R . . N3 N 0.1686(10) 0.1556(6) 0.6873(3) 0.028(2) Uani 1 1 d . . . H3A H 0.2720 0.1611 0.6848 0.033 Uiso 1 1 calc R . . H3B H 0.1400 0.1769 0.7179 0.033 Uiso 1 1 calc R . . N4 N -0.0314(11) 0.3948(6) 0.6312(3) 0.031(2) Uani 1 1 d D . . N5 N -0.1039(10) 0.2715(6) 0.7006(3) 0.026(2) Uani 1 1 d D . . N6 N 0.1004(12) 0.3395(5) 0.5420(3) 0.031(2) Uani 1 1 d . . . C1 C -0.0595(15) 0.0460(7) 0.5869(5) 0.036(3) Uani 1 1 d . . . H1A H -0.1158 -0.0061 0.5915 0.043 Uiso 1 1 calc R . . H1B H 0.0492 0.0329 0.5829 0.043 Uiso 1 1 calc R . . C2 C -0.1166(14) 0.0904(7) 0.5409(5) 0.033(3) Uani 1 1 d . . . H2C H -0.1020 0.0554 0.5108 0.039 Uiso 1 1 calc R . . H2D H -0.2263 0.1014 0.5446 0.039 Uiso 1 1 calc R . . C3 C -0.0340(13) 0.0587(7) 0.6796(4) 0.028(3) Uani 1 1 d . . . H3C H -0.0893 0.0831 0.7084 0.034 Uiso 1 1 calc R . . H3D H -0.0587 -0.0006 0.6781 0.034 Uiso 1 1 calc R . . C4 C 0.1329(13) 0.0696(7) 0.6869(4) 0.030(3) Uani 1 1 d . . . H4A H 0.1642 0.0443 0.7192 0.036 Uiso 1 1 calc R . . H4B H 0.1885 0.0420 0.6593 0.036 Uiso 1 1 calc R . . C5A C -0.060(2) 0.4138(13) 0.6846(6) 0.032(5) Uiso 0.60 1 d PD . . C5B C -0.139(4) 0.4177(19) 0.6709(12) 0.034(7) Uiso 0.40 1 d P . . C6A C -0.171(3) 0.3540(14) 0.7078(9) 0.033(6) Uiso 0.60 1 d P . . C6B C -0.116(4) 0.3592(13) 0.7146(13) 0.034(9) Uiso 0.40 1 d PD . . C7A C 0.037(2) 0.4563(10) 0.6001(7) 0.023(4) Uiso 0.60 1 d PD . . C7B C -0.030(3) 0.4474(16) 0.5860(8) 0.027(7) Uiso 0.40 1 d PD . . C8A C 0.038(3) 0.4247(12) 0.5456(7) 0.022(5) Uiso 0.60 1 d P . . C8B C 0.096(3) 0.4271(18) 0.5494(10) 0.020(7) Uiso 0.40 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 Sm1 0.0205(3) 0.0181(3) 0.0143(3) 0.0006(2) 0.0014(2) 0.0006(2) Se1 0.0200(5) 0.0267(6) 0.0194(5) -0.0041(4) -0.0020(4) 0.0006(5) Se2 0.0261(6) 0.0241(6) 0.0284(6) -0.0070(5) -0.0013(5) 0.0025(5) Se3 0.0210(5) 0.0388(7) 0.0209(6) 0.0040(5) 0.0010(5) -0.0032(5) Se4 0.0227(5) 0.0308(6) 0.0194(5) 0.0049(5) -0.0013(4) 0.0025(5) As1 0.0172(5) 0.0242(6) 0.0148(5) -0.0004(4) -0.0005(4) 0.0011(4) N1 0.021(5) 0.021(5) 0.028(5) 0.003(4) -0.001(4) 0.001(4) N2 0.018(4) 0.030(5) 0.026(5) -0.002(4) -0.004(4) 0.000(4) N3 0.027(5) 0.030(6) 0.026(5) 0.000(4) -0.002(4) 0.000(4) N4 0.040(6) 0.028(5) 0.026(5) 0.006(4) 0.001(4) 0.008(5) N5 0.029(5) 0.026(5) 0.022(5) -0.003(4) -0.004(4) 0.003(4) N6 0.057(7) 0.013(5) 0.024(5) 0.003(4) 0.008(5) 0.003(5) C1 0.044(7) 0.023(6) 0.041(8) -0.001(5) 0.000(6) -0.005(6) C2 0.037(7) 0.027(7) 0.034(7) -0.005(5) -0.007(6) -0.001(6) C3 0.035(7) 0.028(6) 0.022(6) 0.008(5) 0.004(5) -0.007(5) C4 0.036(7) 0.027(7) 0.027(6) -0.003(5) -0.005(5) 0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N6 2.582(9) . ? Sm1 N3 2.586(9) . ? Sm1 N4 2.589(9) . ? Sm1 N2 2.605(9) . ? Sm1 N1 2.614(9) . ? Sm1 N5 2.620(9) . ? Sm1 Se1 3.1183(12) . ? Sm1 Se2 3.1408(13) . ? Sm1 Se3 3.3845(12) 1_455 ? Se1 As1 2.3138(15) . ? Se2 As1 2.3052(15) . ? Se3 As1 2.3010(15) . ? Se3 Sm1 3.3845(12) 1_655 ? Se4 As1 2.3059(15) . ? N1 C1 1.484(14) . ? N1 C3 1.505(13) . ? N1 H1 0.9300 . ? N2 C2 1.482(14) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C4 1.435(14) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N4 C7A 1.429(15) . ? N4 C5B 1.47(3) . ? N4 C5A 1.470(15) . ? N4 C7B 1.474(17) . ? N5 C6B 1.479(18) . ? N5 C6A 1.48(2) . ? N6 C8B 1.44(3) . ? N6 C8A 1.50(2) . ? C1 C2 1.505(16) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 C4 1.498(16) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5A C6A 1.51(3) . ? C5B C6B 1.52(5) . ? C7A C8A 1.54(3) . ? C7B C8B 1.516(18) . ? 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 N6 Sm1 N3 144.1(3) . . ? N6 Sm1 N4 65.2(3) . . ? N3 Sm1 N4 122.0(3) . . ? N6 Sm1 N2 71.4(3) . . ? N3 Sm1 N2 117.9(3) . . ? N4 Sm1 N2 119.6(3) . . ? N6 Sm1 N1 137.4(3) . . ? N3 Sm1 N1 65.5(3) . . ? N4 Sm1 N1 135.8(3) . . ? N2 Sm1 N1 66.1(3) . . ? N6 Sm1 N5 129.8(3) . . ? N3 Sm1 N5 72.5(3) . . ? N4 Sm1 N5 64.9(3) . . ? N2 Sm1 N5 131.3(3) . . ? N1 Sm1 N5 79.5(3) . . ? N6 Sm1 Se1 76.1(2) . . ? N3 Sm1 Se1 75.7(2) . . ? N4 Sm1 Se1 131.5(2) . . ? N2 Sm1 Se1 70.0(2) . . ? N1 Sm1 Se1 92.5(2) . . ? N5 Sm1 Se1 147.7(2) . . ? N6 Sm1 Se2 76.0(2) . . ? N3 Sm1 Se2 74.2(2) . . ? N4 Sm1 Se2 72.3(2) . . ? N2 Sm1 Se2 133.6(2) . . ? N1 Sm1 Se2 139.15(19) . . ? N5 Sm1 Se2 94.9(2) . . ? Se1 Sm1 Se2 70.78(3) . . ? N6 Sm1 Se3 78.5(2) . 1_455 ? N3 Sm1 Se3 137.3(2) . 1_455 ? N4 Sm1 Se3 67.7(2) . 1_455 ? N2 Sm1 Se3 64.0(2) . 1_455 ? N1 Sm1 Se3 80.0(2) . 1_455 ? N5 Sm1 Se3 77.3(2) . 1_455 ? Se1 Sm1 Se3 132.48(3) . 1_455 ? Se2 Sm1 Se3 138.68(3) . 1_455 ? As1 Se1 Sm1 90.77(4) . . ? As1 Se2 Sm1 90.37(4) . . ? As1 Se3 Sm1 119.11(5) . 1_655 ? Se3 As1 Se2 112.50(6) . . ? Se3 As1 Se4 110.82(6) . . ? Se2 As1 Se4 110.06(6) . . ? Se3 As1 Se1 109.08(6) . . ? Se2 As1 Se1 103.41(5) . . ? Se4 As1 Se1 110.73(6) . . ? C1 N1 C3 112.0(9) . . ? C1 N1 Sm1 110.7(6) . . ? C3 N1 Sm1 113.6(6) . . ? C1 N1 H1 106.7 . . ? C3 N1 H1 106.7 . . ? Sm1 N1 H1 106.7 . . ? C2 N2 Sm1 115.3(7) . . ? C2 N2 H2A 108.4 . . ? Sm1 N2 H2A 108.4 . . ? C2 N2 H2B 108.4 . . ? Sm1 N2 H2B 108.4 . . ? H2A N2 H2B 107.5 . . ? C4 N3 Sm1 116.1(7) . . ? C4 N3 H3A 108.3 . . ? Sm1 N3 H3A 108.3 . . ? C4 N3 H3B 108.3 . . ? Sm1 N3 H3B 108.3 . . ? H3A N3 H3B 107.4 . . ? C7A N4 C5B 120.6(16) . . ? C7A N4 C5A 118.8(13) . . ? C5B N4 C5A 31.2(13) . . ? C7A N4 C7B 28.4(11) . . ? C5B N4 C7B 116.1(17) . . ? C5A N4 C7B 131.5(15) . . ? C7A N4 Sm1 118.3(9) . . ? C5B N4 Sm1 121.1(13) . . ? C5A N4 Sm1 112.7(9) . . ? C7B N4 Sm1 115.7(11) . . ? C6B N5 C6A 20.5(15) . . ? C6B N5 Sm1 114.8(15) . . ? C6A N5 Sm1 118.1(10) . . ? C8B N6 C8A 20.4(12) . . ? C8B N6 Sm1 119.5(11) . . ? C8A N6 Sm1 116.4(9) . . ? N1 C1 C2 108.4(9) . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 110.6(9) . . ? N2 C2 H2C 109.5 . . ? C1 C2 H2C 109.5 . . ? N2 C2 H2D 109.5 . . ? C1 C2 H2D 109.5 . . ? H2C C2 H2D 108.1 . . ? C4 C3 N1 109.5(9) . . ? C4 C3 H3C 109.8 . . ? N1 C3 H3C 109.8 . . ? C4 C3 H3D 109.8 . . ? N1 C3 H3D 109.8 . . ? H3C C3 H3D 108.2 . . ? N3 C4 C3 109.5(9) . . ? N3 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? N3 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? N4 C5A C6A 111.7(16) . . ? N4 C5B C6B 107(2) . . ? N5 C6A C5A 105.8(17) . . ? N5 C6B C5B 115(2) . . ? N4 C7A C8A 108.3(14) . . ? N4 C7B C8B 113.6(19) . . ? N6 C8A C7A 111.9(15) . . ? N6 C8B C7B 109(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 N6 Sm1 Se1 As1 93.8(2) . . . . ? N3 Sm1 Se1 As1 -63.8(2) . . . . ? N4 Sm1 Se1 As1 56.5(3) . . . . ? N2 Sm1 Se1 As1 168.8(2) . . . . ? N1 Sm1 Se1 As1 -127.76(19) . . . . ? N5 Sm1 Se1 As1 -53.5(4) . . . . ? Se2 Sm1 Se1 As1 14.09(4) . . . . ? Se3 Sm1 Se1 As1 153.49(5) 1_455 . . . ? N6 Sm1 Se2 As1 -94.1(2) . . . . ? N3 Sm1 Se2 As1 65.9(2) . . . . ? N4 Sm1 Se2 As1 -162.1(2) . . . . ? N2 Sm1 Se2 As1 -47.9(3) . . . . ? N1 Sm1 Se2 As1 56.5(3) . . . . ? N5 Sm1 Se2 As1 136.1(2) . . . . ? Se1 Sm1 Se2 As1 -14.14(4) . . . . ? Se3 Sm1 Se2 As1 -147.51(5) 1_455 . . . ? Sm1 Se3 As1 Se2 117.72(6) 1_655 . . . ? Sm1 Se3 As1 Se4 -5.98(8) 1_655 . . . ? Sm1 Se3 As1 Se1 -128.14(5) 1_655 . . . ? Sm1 Se2 As1 Se3 136.19(5) . . . . ? Sm1 Se2 As1 Se4 -99.68(5) . . . . ? Sm1 Se2 As1 Se1 18.64(5) . . . . ? Sm1 Se1 As1 Se3 -138.70(5) . . . . ? Sm1 Se1 As1 Se2 -18.78(5) . . . . ? Sm1 Se1 As1 Se4 99.08(5) . . . . ? N6 Sm1 N1 C1 31.7(9) . . . . ? N3 Sm1 N1 C1 -113.4(8) . . . . ? N4 Sm1 N1 C1 135.1(7) . . . . ? N2 Sm1 N1 C1 26.5(7) . . . . ? N5 Sm1 N1 C1 171.2(8) . . . . ? Se1 Sm1 N1 C1 -40.4(7) . . . . ? Se2 Sm1 N1 C1 -103.5(7) . . . . ? Se3 Sm1 N1 C1 92.4(7) 1_455 . . . ? N6 Sm1 N1 C3 158.7(7) . . . . ? N3 Sm1 N1 C3 13.6(7) . . . . ? N4 Sm1 N1 C3 -97.9(7) . . . . ? N2 Sm1 N1 C3 153.5(8) . . . . ? N5 Sm1 N1 C3 -61.8(7) . . . . ? Se1 Sm1 N1 C3 86.6(7) . . . . ? Se2 Sm1 N1 C3 23.5(8) . . . . ? Se3 Sm1 N1 C3 -140.6(7) 1_455 . . . ? N6 Sm1 N2 C2 -172.2(8) . . . . ? N3 Sm1 N2 C2 45.6(8) . . . . ? N4 Sm1 N2 C2 -126.5(7) . . . . ? N1 Sm1 N2 C2 4.0(7) . . . . ? N5 Sm1 N2 C2 -45.1(9) . . . . ? Se1 Sm1 N2 C2 106.3(7) . . . . ? Se2 Sm1 N2 C2 140.2(6) . . . . ? Se3 Sm1 N2 C2 -86.2(7) 1_455 . . . ? N6 Sm1 N3 C4 -121.4(8) . . . . ? N4 Sm1 N3 C4 147.3(7) . . . . ? N2 Sm1 N3 C4 -24.6(9) . . . . ? N1 Sm1 N3 C4 17.2(7) . . . . ? N5 Sm1 N3 C4 103.4(8) . . . . ? Se1 Sm1 N3 C4 -82.3(8) . . . . ? Se2 Sm1 N3 C4 -156.0(8) . . . . ? Se3 Sm1 N3 C4 56.4(9) 1_455 . . . ? N6 Sm1 N4 C7A -19.9(11) . . . . ? N3 Sm1 N4 C7A 119.9(11) . . . . ? N2 Sm1 N4 C7A -68.2(11) . . . . ? N1 Sm1 N4 C7A -153.4(10) . . . . ? N5 Sm1 N4 C7A 166.9(12) . . . . ? Se1 Sm1 N4 C7A 20.5(12) . . . . ? Se2 Sm1 N4 C7A 62.5(11) . . . . ? Se3 Sm1 N4 C7A -107.2(11) 1_455 . . . ? N6 Sm1 N4 C5B 161.4(17) . . . . ? N3 Sm1 N4 C5B -58.8(17) . . . . ? N2 Sm1 N4 C5B 113.0(17) . . . . ? N1 Sm1 N4 C5B 27.8(18) . . . . ? N5 Sm1 N4 C5B -11.9(16) . . . . ? Se1 Sm1 N4 C5B -158.2(16) . . . . ? Se2 Sm1 N4 C5B -116.3(17) . . . . ? Se3 Sm1 N4 C5B 74.1(17) 1_455 . . . ? N6 Sm1 N4 C5A -164.8(12) . . . . ? N3 Sm1 N4 C5A -25.0(12) . . . . ? N2 Sm1 N4 C5A 146.9(11) . . . . ? N1 Sm1 N4 C5A 61.7(12) . . . . ? N5 Sm1 N4 C5A 22.0(11) . . . . ? Se1 Sm1 N4 C5A -124.4(10) . . . . ? Se2 Sm1 N4 C5A -82.4(11) . . . . ? Se3 Sm1 N4 C5A 108.0(11) 1_455 . . . ? N6 Sm1 N4 C7B 12.0(14) . . . . ? N3 Sm1 N4 C7B 151.8(14) . . . . ? N2 Sm1 N4 C7B -36.3(15) . . . . ? N1 Sm1 N4 C7B -121.5(14) . . . . ? N5 Sm1 N4 C7B -161.3(15) . . . . ? Se1 Sm1 N4 C7B 52.4(15) . . . . ? Se2 Sm1 N4 C7B 94.3(14) . . . . ? Se3 Sm1 N4 C7B -75.3(14) 1_455 . . . ? N6 Sm1 N5 C6B -21.8(18) . . . . ? N3 Sm1 N5 C6B 125.7(18) . . . . ? N4 Sm1 N5 C6B -13.9(17) . . . . ? N2 Sm1 N5 C6B -122.2(17) . . . . ? N1 Sm1 N5 C6B -166.9(18) . . . . ? Se1 Sm1 N5 C6B 115.1(17) . . . . ? Se2 Sm1 N5 C6B 54.0(17) . . . . ? Se3 Sm1 N5 C6B -84.9(17) 1_455 . . . ? N6 Sm1 N5 C6A 0.9(14) . . . . ? N3 Sm1 N5 C6A 148.3(13) . . . . ? N4 Sm1 N5 C6A 8.8(12) . . . . ? N2 Sm1 N5 C6A -99.5(13) . . . . ? N1 Sm1 N5 C6A -144.2(13) . . . . ? Se1 Sm1 N5 C6A 137.8(12) . . . . ? Se2 Sm1 N5 C6A 76.7(13) . . . . ? Se3 Sm1 N5 C6A -62.2(13) 1_455 . . . ? N3 Sm1 N6 C8B -96.7(16) . . . . ? N4 Sm1 N6 C8B 14.3(15) . . . . ? N2 Sm1 N6 C8B 151.1(16) . . . . ? N1 Sm1 N6 C8B 146.0(15) . . . . ? N5 Sm1 N6 C8B 22.3(17) . . . . ? Se1 Sm1 N6 C8B -135.7(16) . . . . ? Se2 Sm1 N6 C8B -62.4(16) . . . . ? Se3 Sm1 N6 C8B 84.9(16) 1_455 . . . ? N3 Sm1 N6 C8A -119.6(11) . . . . ? N4 Sm1 N6 C8A -8.6(11) . . . . ? N2 Sm1 N6 C8A 128.1(12) . . . . ? N1 Sm1 N6 C8A 123.1(11) . . . . ? N5 Sm1 N6 C8A -0.7(13) . . . . ? Se1 Sm1 N6 C8A -158.6(11) . . . . ? Se2 Sm1 N6 C8A -85.3(11) . . . . ? Se3 Sm1 N6 C8A 61.9(11) 1_455 . . . ? C3 N1 C1 C2 177.5(9) . . . . ? Sm1 N1 C1 C2 -54.6(11) . . . . ? Sm1 N2 C2 C1 -33.8(12) . . . . ? N1 C1 C2 N2 58.9(13) . . . . ? C1 N1 C3 C4 84.5(11) . . . . ? Sm1 N1 C3 C4 -41.8(11) . . . . ? Sm1 N3 C4 C3 -45.8(11) . . . . ? N1 C3 C4 N3 57.4(12) . . . . ? C7A N4 C5A C6A 163.4(16) . . . . ? C5B N4 C5A C6A 61(3) . . . . ? C7B N4 C5A C6A 132(2) . . . . ? Sm1 N4 C5A C6A -51.9(19) . . . . ? C7A N4 C5B C6B -145(2) . . . . ? C5A N4 C5B C6B -49(3) . . . . ? C7B N4 C5B C6B -177(2) . . . . ? Sm1 N4 C5B C6B 34(3) . . . . ? C6B N5 C6A C5A 50(5) . . . . ? Sm1 N5 C6A C5A -36(2) . . . . ? N4 C5A C6A N5 57(2) . . . . ? C6A N5 C6B C5B -66(5) . . . . ? Sm1 N5 C6B C5B 38(3) . . . . ? N4 C5B C6B N5 -46(4) . . . . ? C5B N4 C7A C8A -138(2) . . . . ? C5A N4 C7A C8A -173.8(16) . . . . ? C7B N4 C7A C8A -49(2) . . . . ? Sm1 N4 C7A C8A 43.4(18) . . . . ? C7A N4 C7B C8B 66(3) . . . . ? C5B N4 C7B C8B 173(2) . . . . ? C5A N4 C7B C8B 140(2) . . . . ? Sm1 N4 C7B C8B -36(3) . . . . ? C8B N6 C8A C7A -70(4) . . . . ? Sm1 N6 C8A C7A 33.8(19) . . . . ? N4 C7A C8A N6 -49(2) . . . . ? C8A N6 C8B C7B 50(3) . . . . ? Sm1 N6 C8B C7B -37(3) . . . . ? N4 C7B C8B N6 47(3) . . . . ? 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 N3 H3B Se4 0.92 2.69 3.515(9) 148.9 8_557 N3 H3A Se4 0.92 2.59 3.504(9) 170.1 . N2 H2B Se3 0.92 2.85 3.595(9) 139.1 6_566 N2 H2B Se1 0.92 2.79 3.311(9) 117.1 . N2 H2A Se3 0.92 2.77 3.242(9) 112.8 1_455 N1 H1 Se4 0.93 2.67 3.528(9) 152.9 1_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.283 _refine_diff_density_min -1.454 _refine_diff_density_rms 0.233