# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' #TrackingRef '- cif files of 1a-3c.cif' _journal_coden_Cambridge 0222 _publ_contact_author_name '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 'Jiao Wang' 'Yingli Pan' 'Jiangfang Chen' 'Jiansheng Gu' 'Yong Zhang' ; Dingxian Jia ; data_complex_1a _database_code_depnum_ccdc_archive 'CCDC 767669' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H26 As La N6 O Se4' _chemical_formula_sum 'C6 H26 As La N6 O Se4' _chemical_formula_weight 728.00 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' La La -0.2871 2.4523 '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' Se Se -0.0929 2.2259 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3' _symmetry_space_group_name_Hall P63/m _symmetry_Int_Tables_number 147 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 19.112(2) _cell_length_b 19.112(2) _cell_length_c 9.4870(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3001.1(5) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 11577 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_absorpt_coefficient_mu 11.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1612 _exptl_absorpt_correction_T_max 0.2159 _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 29458 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3652 _reflns_number_gt 3546 _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^)+(0.0000P)^2^+411.8674P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3652 _refine_ls_number_parameters 143 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.1787 _refine_ls_wR_factor_gt 0.1778 _refine_ls_goodness_of_fit_ref 1.234 _refine_ls_restrained_S_all 1.232 _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 As1 As 0.65206(14) 0.67464(14) 0.7502(3) 0.0171(5) Uani 1 1 d . . . La1 La 0.66289(8) 0.68548(8) 0.25003(14) 0.0141(4) Uani 1 1 d D . . Se1 Se 0.71961(17) 0.75642(15) 0.5592(2) 0.0238(6) Uani 1 1 d . . . Se2 Se 0.71966(17) 0.75643(15) 0.9410(2) 0.0239(6) Uani 1 1 d . . . Se3 Se 0.51859(16) 0.63875(17) 0.7500(4) 0.0344(8) Uani 1 1 d . . . Se4 Se 0.66137(15) 0.55930(15) 0.7499(3) 0.0224(6) Uani 1 1 d . . . N1 N 0.7324(14) 0.8508(13) 0.250(3) 0.0341(3) Uani 1 1 d . . . N2 N 0.8302(14) 0.7739(12) 0.249(3) 0.0337(3) Uani 1 1 d D . . N3A N 0.5607(19) 0.727(3) 0.136(6) 0.0468(5) Uani 0.54 1 d PD . . N3B N 0.5178(19) 0.631(3) 0.121(5) 0.0471(5) Uani 0.46 1 d PD . . N4A N 0.5182(18) 0.630(3) 0.381(5) 0.0468(5) Uani 0.54 1 d PD . . N4B N 0.5615(19) 0.727(3) 0.364(7) 0.0462(5) Uani 0.46 1 d PD . . N5A N 0.728(3) 0.6038(19) 0.122(6) 0.0472(4) Uani 0.54 1 d PD . . N5B N 0.640(3) 0.553(3) 0.134(7) 0.0422(4) Uani 0.46 1 d PD . . N6A N 0.640(3) 0.553(3) 0.373(6) 0.0434(4) Uani 0.54 1 d PD . . N6B N 0.729(3) 0.604(2) 0.380(7) 0.0418(4) Uani 0.46 1 d PD . . C1 C 0.8201(16) 0.8992(16) 0.248(4) 0.0332(3) Uani 1 1 d D . . C2A C 0.867(2) 0.8590(15) 0.292(6) 0.0341(3) Uani 0.58 1 d PD . . C2B C 0.861(3) 0.855(2) 0.191(6) 0.0340(3) Uani 0.42 1 d PD . . C3 C 0.4750(17) 0.6727(18) 0.172(3) 0.0465(5) Uani 1 1 d D . . C4 C 0.4754(17) 0.6727(18) 0.330(3) 0.0472(5) Uani 1 1 d D . . C5 C 0.6929(19) 0.5194(17) 0.171(3) 0.0453(4) Uani 1 1 d D . . C6 C 0.6929(19) 0.5203(17) 0.329(3) 0.0471(4) Uani 1 1 d D . . O1A O 0.549(2) 0.560(2) 0.082(3) 0.031(8) Uani 0.48 1 d P . . O1B O 0.549(2) 0.559(2) 0.417(3) 0.032(7) Uani 0.52 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0180(12) 0.0139(11) 0.0182(12) -0.0003(9) -0.0002(10) 0.0072(10) La1 0.0141(7) 0.0147(7) 0.0123(7) 0.0002(5) -0.003(5) 0.005(5) Se1 0.0365(15) 0.0226(13) 0.0074(11) 0.0008(9) 0.0013(10) 0.0109(11) Se2 0.0371(15) 0.0232(13) 0.0068(11) -0.0007(9) -0.0011(10) 0.0116(12) Se3 0.0176(13) 0.0241(14) 0.064(2) 0.0002(13) 0.0003(13) 0.0122(11) Se4 0.0215(12) 0.0173(12) 0.0302(14) 0.0003(10) 0.0004(10) 0.0111(10) N1 0.0282(7) 0.0201(6) 0.0427(10) -0.004(6) -0.002(7) 0.008(6) N2 0.0232(7) 0.0217(6) 0.0415(10) -0.002(6) -0.001(7) 0.001(6) N3A 0.0361(9) 0.0341(9) 0.0681(13) 0.001(9) 0.003(9) 0.011(8) N3B 0.0326(9) 0.0350(9) 0.0697(13) 0.002(9) 0.005(9) 0.013(8) N4A 0.0332(9) 0.0352(9) 0.0672(13) 0.003(9) 0.006(9) 0.009(8) N4B 0.0329(9) 0.0342(9) 0.0691(13) 0.002(9) 0.002(9) 0.016(8) N5A 0.0513(10) 0.0328(9) 0.0537(12) -0.002(8) 0.002(9) 0.014(8) N5B 0.0431(10) 0.0365(9) 0.0521(12) -0.005(8) 0.003(9) 0.023(8) N6A 0.0472(10) 0.0336(9) 0.0601(12) -0.003(8) 0.006(9) 0.021(8) N6B 0.0451(10) 0.0348(9) 0.0577(12) -0.003(8) 0.002(9) 0.030(8) C1 0.026(7) 0.016(6) 0.058(10) -0.003(6) -0.001(7) 0.009(6) C2A 0.0256(7) 0.0236(6) 0.0501(10) -0.002(6) -0.001(7) 0.009(6) C2B 0.0266(7) 0.0268(6) 0.0417(10) -0.003(6) -0.003(7) 0.010(6) C3 0.0371(9) 0.0328(9) 0.0632(13) 0.001(9) 0.003(9) 0.014(8) C4 0.0353(9) 0.0313(9) 0.0673(13) 0.004(9) 0.006(9) 0.010(8) C5 0.0452(10) 0.0306(9) 0.0642(12) -0.003(8) 0.002(9) 0.020(8) C6 0.0467(10) 0.0337(9) 0.0592(12) -0.002(8) 0.007(9) 0.017(8) O1A 0.043(2) 0.025(19) 0.047(16) 0.012(14) 0.014(15) 0.020(17) O1B 0.043(2) 0.028(18) 0.042(14) -0.008(13) -0.009(13) 0.016(16) _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 As1 Se3 2.286(4) . ? As1 Se4 2.299(3) . ? As1 Se2 2.318(3) . ? As1 Se1 2.318(3) . ? La1 N5B 2.59(5) . ? La1 N6A 2.62(5) . ? La1 N4B 2.66(6) . ? La1 N3A 2.67(5) . ? La1 N3B 2.715(19) . ? La1 N4A 2.717(19) . ? La1 N5A 2.72(4) . ? La1 N6B 2.73(5) . ? La1 N1 2.75(2) . ? La1 N2 2.77(2) . ? La1 O1A 2.79(4) . ? La1 O1B 2.80(3) . ? Se2 La1 3.184(3) 1_556 ? N1 C1 1.46(3) . ? N2 C2A 1.471(10) . ? N2 C2B 1.472(10) . ? N3A C3 1.475(10) . ? N3B C3 1.486(10) . ? N4A C4 1.487(10) . ? N4B C4 1.476(10) . ? N5A C5 1.479(10) . ? N5B C5 1.484(10) . ? N6A C6 1.485(10) . ? N6B C6 1.479(10) . ? C1 C2A 1.497(10) . ? C1 C2B 1.499(10) . ? C3 C4 1.499(10) . ? C5 C6 1.502(10) . ? 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 Se3 As1 Se4 108.78(13) . . ? Se3 As1 Se2 111.41(15) . . ? Se4 As1 Se2 111.30(14) . . ? Se3 As1 Se1 111.31(15) . . ? Se4 As1 Se1 111.20(14) . . ? Se2 As1 Se1 102.77(13) . . ? N5B La1 N6A 51.6(16) . . ? N5B La1 N4B 132.3(14) . . ? N6A La1 N4B 108.4(16) . . ? N5B La1 N3A 109.1(15) . . ? N6A La1 N3A 132.2(12) . . ? N4B La1 N3A 47.6(18) . . ? N5B La1 N3B 78.0(12) . . ? N6A La1 N3B 100.5(16) . . ? N4B La1 N3B 62.8(13) . . ? N3A La1 N3B 34.6(14) . . ? N5B La1 N4A 100.1(16) . . ? N6A La1 N4A 77.1(10) . . ? N4B La1 N4A 34.9(14) . . ? N3A La1 N4A 63.0(11) . . ? N3B La1 N4A 53.8(16) . . ? N5B La1 N5A 31.9(14) . . ? N6A La1 N5A 63.1(11) . . ? N4B La1 N5A 164.2(12) . . ? N3A La1 N5A 127.0(17) . . ? N3B La1 N5A 104.5(13) . . ? N4A La1 N5A 130.6(12) . . ? N5B La1 N6B 62.5(13) . . ? N6A La1 N6B 31.9(14) . . ? N4B La1 N6B 126.6(19) . . ? N3A La1 N6B 164.2(13) . . ? N3B La1 N6B 130.9(14) . . ? N4A La1 N6B 104.0(14) . . ? N5A La1 N6B 53.5(15) . . ? N5B La1 N1 150.7(15) . . ? N6A La1 N1 149.7(13) . . ? N4B La1 N1 70.2(11) . . ? N3A La1 N1 70.4(10) . . ? N3B La1 N1 104.9(12) . . ? N4A La1 N1 104.9(10) . . ? N5A La1 N1 124.3(9) . . ? N6B La1 N1 123.9(9) . . ? N5B La1 N2 99.9(12) . . ? N6A La1 N2 100.1(10) . . ? N4B La1 N2 127.5(9) . . ? N3A La1 N2 127.5(9) . . ? N3B La1 N2 151.4(14) . . ? N4A La1 N2 151.5(13) . . ? N5A La1 N2 68.2(11) . . ? N6B La1 N2 68.3(12) . . ? N1 La1 N2 63.4(7) . . ? N5B La1 O1A 40.4(11) . . ? N6A La1 O1A 74.9(13) . . ? N4B La1 O1A 96.8(11) . . ? N3A La1 O1A 69.9(13) . . ? N3B La1 O1A 37.5(10) . . ? N4A La1 O1A 74.0(13) . . ? N5A La1 O1A 68.5(13) . . ? N6B La1 O1A 98.6(10) . . ? N1 La1 O1A 135.3(9) . . ? N2 La1 O1A 133.3(9) . . ? N5B La1 O1B 73.7(15) . . ? N6A La1 O1B 39.6(10) . . ? N4B La1 O1B 70.3(14) . . ? N3A La1 O1B 96.8(10) . . ? N3B La1 O1B 73.7(15) . . ? N4A La1 O1B 37.5(10) . . ? N5A La1 O1B 97.9(10) . . ? N6B La1 O1B 68.4(14) . . ? N1 La1 O1B 135.5(9) . . ? N2 La1 O1B 133.6(9) . . ? O1A La1 O1B 69.2(9) . . ? As1 Se1 La1 118.45(11) . . ? As1 Se2 La1 118.41(12) . 1_556 ? C1 N1 La1 118.1(15) . . ? C2A N2 C2B 38(3) . . ? C2A N2 La1 116(2) . . ? C2B N2 La1 112(3) . . ? C3 N3A La1 115(3) . . ? C3 N3B La1 112.1(19) . . ? C4 N4A La1 111.9(18) . . ? C4 N4B La1 115(3) . . ? C5 N5A La1 113(3) . . ? C5 N5B La1 120(3) . . ? C6 N6A La1 117(3) . . ? C6 N6B La1 112(3) . . ? N1 C1 C2A 118(3) . . ? N1 C1 C2B 114(3) . . ? C2A C1 C2B 38(3) . . ? N2 C2A C1 115(2) . . ? N2 C2B C1 114(2) . . ? N3A C3 N3B 66(3) . . ? N3A C3 C4 103(3) . . ? N3B C3 C4 109(3) . . ? N4B C4 N4A 66(3) . . ? N4B C4 C3 103(4) . . ? N4A C4 C3 109(3) . . ? N5A C5 N5B 59(3) . . ? N5A C5 C6 108(3) . . ? N5B C5 C6 103(3) . . ? N6B C6 N6A 60(3) . . ? N6B C6 C5 110(3) . . ? N6A C6 C5 107(3) . . ? 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 Se3 As1 Se1 La1 -61.35(17) . . . . ? Se4 As1 Se1 La1 60.12(17) . . . . ? Se2 As1 Se1 La1 179.29(12) . . . . ? N5B La1 Se1 As1 -51.9(16) . . . . ? N6A La1 Se1 As1 -36.5(8) . . . . ? N4B La1 Se1 As1 76.8(13) . . . . ? N3A La1 Se1 As1 96.1(8) . . . . ? N3B La1 Se1 As1 60.4(15) . . . . ? N4A La1 Se1 As1 41.9(7) . . . . ? N5A La1 Se1 As1 -88.9(8) . . . . ? N6B La1 Se1 As1 -67.3(12) . . . . ? N1 La1 Se1 As1 152.7(6) . . . . ? N2 La1 Se1 As1 -139.8(5) . . . . ? O1A La1 Se1 As1 8.0(13) . . . . ? O1B La1 Se1 As1 3.6(7) . . . . ? Se3 As1 Se2 La1 61.39(18) . . . 1_556 ? Se4 As1 Se2 La1 -60.22(17) . . . 1_556 ? Se1 As1 Se2 La1 -179.33(12) . . . 1_556 ? N5B La1 N1 C1 -59(3) . . . . ? N6A La1 N1 C1 63(3) . . . . ? N4B La1 N1 C1 156(3) . . . . ? N3A La1 N1 C1 -154(3) . . . . ? N3B La1 N1 C1 -151(2) . . . . ? N4A La1 N1 C1 153(2) . . . . ? N5A La1 N1 C1 -32(3) . . . . ? N6B La1 N1 C1 34(3) . . . . ? N2 La1 N1 C1 1(2) . . . . ? O1A La1 N1 C1 -125(2) . . . . ? O1B La1 N1 C1 127(2) . . . . ? N5B La1 N2 C2A 172(3) . . . . ? N6A La1 N2 C2A -135(3) . . . . ? N4B La1 N2 C2A -12(3) . . . . ? N3A La1 N2 C2A 49(3) . . . . ? N3B La1 N2 C2A 89(3) . . . . ? N4A La1 N2 C2A -54(3) . . . . ? N5A La1 N2 C2A 169(3) . . . . ? N6B La1 N2 C2A -133(3) . . . . ? N1 La1 N2 C2A 18(3) . . . . ? O1A La1 N2 C2A 146(3) . . . . ? O1B La1 N2 C2A -111(3) . . . . ? N5B La1 N2 C2B 131(3) . . . . ? N6A La1 N2 C2B -177(3) . . . . ? N4B La1 N2 C2B -54(3) . . . . ? N3A La1 N2 C2B 7(3) . . . . ? N3B La1 N2 C2B 48(3) . . . . ? N4A La1 N2 C2B -95(3) . . . . ? N5A La1 N2 C2B 128(3) . . . . ? N6B La1 N2 C2B -174(3) . . . . ? N1 La1 N2 C2B -24(3) . . . . ? O1A La1 N2 C2B 104(3) . . . . ? O1B La1 N2 C2B -153(3) . . . . ? N5B La1 N3A C3 69(4) . . . . ? N6A La1 N3A C3 14(5) . . . . ? N4B La1 N3A C3 -62(3) . . . . ? N3B La1 N3A C3 42(3) . . . . ? N4A La1 N3A C3 -23(3) . . . . ? N5A La1 N3A C3 99(3) . . . . ? N6B La1 N3A C3 14(8) . . . . ? N1 La1 N3A C3 -142(4) . . . . ? N2 La1 N3A C3 -171(3) . . . . ? O1A La1 N3A C3 59(3) . . . . ? O1B La1 N3A C3 -6(3) . . . . ? N5B La1 N3B C3 166(4) . . . . ? N6A La1 N3B C3 119(3) . . . . ? N4B La1 N3B C3 13(3) . . . . ? N3A La1 N3B C3 -40(3) . . . . ? N4A La1 N3B C3 53(3) . . . . ? N5A La1 N3B C3 -176(3) . . . . ? N6B La1 N3B C3 130(3) . . . . ? N1 La1 N3B C3 -44(4) . . . . ? N2 La1 N3B C3 -106(3) . . . . ? O1A La1 N3B C3 166(5) . . . . ? O1B La1 N3B C3 89(3) . . . . ? N5B La1 N4A C4 -120(3) . . . . ? N6A La1 N4A C4 -167(3) . . . . ? N4B La1 N4A C4 40(3) . . . . ? N3A La1 N4A C4 -14(3) . . . . ? N3B La1 N4A C4 -53(3) . . . . ? N5A La1 N4A C4 -131(3) . . . . ? N6B La1 N4A C4 176(3) . . . . ? N1 La1 N4A C4 44(3) . . . . ? N2 La1 N4A C4 106(3) . . . . ? O1A La1 N4A C4 -89(3) . . . . ? O1B La1 N4A C4 -166(5) . . . . ? N5B La1 N4B C4 -15(5) . . . . ? N6A La1 N4B C4 -69(4) . . . . ? N3A La1 N4B C4 62(4) . . . . ? N3B La1 N4B C4 24(4) . . . . ? N4A La1 N4B C4 -41(3) . . . . ? N5A La1 N4B C4 -14(9) . . . . ? N6B La1 N4B C4 -99(4) . . . . ? N1 La1 N4B C4 143(4) . . . . ? N2 La1 N4B C4 172(3) . . . . ? O1A La1 N4B C4 7(4) . . . . ? O1B La1 N4B C4 -58(4) . . . . ? N5B La1 N5A C5 -42(3) . . . . ? N6A La1 N5A C5 17(3) . . . . ? N4B La1 N5A C5 -43(8) . . . . ? N3A La1 N5A C5 -107(3) . . . . ? N3B La1 N5A C5 -77(3) . . . . ? N4A La1 N5A C5 -23(4) . . . . ? N6B La1 N5A C5 53(3) . . . . ? N1 La1 N5A C5 163(2) . . . . ? N2 La1 N5A C5 132(3) . . . . ? O1A La1 N5A C5 -66(3) . . . . ? O1B La1 N5A C5 -2(3) . . . . ? N6A La1 N5B C5 -55(3) . . . . ? N4B La1 N5B C5 -134(4) . . . . ? N3A La1 N5B C5 176(3) . . . . ? N3B La1 N5B C5 -169(4) . . . . ? N4A La1 N5B C5 -119(4) . . . . ? N5A La1 N5B C5 46(3) . . . . ? N6B La1 N5B C5 -19(3) . . . . ? N1 La1 N5B C5 92(4) . . . . ? N2 La1 N5B C5 40(4) . . . . ? O1A La1 N5B C5 -169(5) . . . . ? O1B La1 N5B C5 -92(4) . . . . ? N5B La1 N6A C6 52(3) . . . . ? N4B La1 N6A C6 -178(3) . . . . ? N3A La1 N6A C6 133(3) . . . . ? N3B La1 N6A C6 118(3) . . . . ? N4A La1 N6A C6 167(4) . . . . ? N5A La1 N6A C6 17(3) . . . . ? N6B La1 N6A C6 -47(3) . . . . ? N1 La1 N6A C6 -96(4) . . . . ? N2 La1 N6A C6 -42(3) . . . . ? O1A La1 N6A C6 90(3) . . . . ? O1B La1 N6A C6 166(5) . . . . ? N5B La1 N6B C6 -16(3) . . . . ? N6A La1 N6B C6 44(2) . . . . ? N4B La1 N6B C6 108(3) . . . . ? N3A La1 N6B C6 45(8) . . . . ? N3B La1 N6B C6 24(5) . . . . ? N4A La1 N6B C6 78(4) . . . . ? N5A La1 N6B C6 -53(3) . . . . ? N1 La1 N6B C6 -163(3) . . . . ? N2 La1 N6B C6 -131(4) . . . . ? O1A La1 N6B C6 2(4) . . . . ? O1B La1 N6B C6 66(3) . . . . ? La1 N1 C1 C2A -19(4) . . . . ? La1 N1 C1 C2B 22(4) . . . . ? C2B N2 C2A C1 58(3) . . . . ? La1 N2 C2A C1 -35(5) . . . . ? N1 C1 C2A N2 36(5) . . . . ? C2B C1 C2A N2 -58(3) . . . . ? C2A N2 C2B C1 -58(3) . . . . ? La1 N2 C2B C1 47(6) . . . . ? N1 C1 C2B N2 -47(6) . . . . ? C2A C1 C2B N2 58(3) . . . . ? La1 N3A C3 N3B -49(3) . . . . ? La1 N3A C3 C4 55(3) . . . . ? La1 N3B C3 N3A 47(3) . . . . ? La1 N3B C3 C4 -49(4) . . . . ? La1 N4B C4 N4A 49(3) . . . . ? La1 N4B C4 C3 -56(4) . . . . ? La1 N4A C4 N4B -46(3) . . . . ? La1 N4A C4 C3 49(3) . . . . ? N3A C3 C4 N4B 0(4) . . . . ? N3B C3 C4 N4B 68(4) . . . . ? N3A C3 C4 N4A -69(4) . . . . ? N3B C3 C4 N4A 0(4) . . . . ? La1 N5A C5 N5B 46(3) . . . . ? La1 N5A C5 C6 -49(3) . . . . ? La1 N5B C5 N5A -54(4) . . . . ? La1 N5B C5 C6 49(4) . . . . ? La1 N6B C6 N6A -49(3) . . . . ? La1 N6B C6 C5 49(4) . . . . ? La1 N6A C6 N6B 55(4) . . . . ? La1 N6A C6 C5 -48(4) . . . . ? N5A C5 C6 N6B -1(4) . . . . ? N5B C5 C6 N6B -62(4) . . . . ? N5A C5 C6 N6A 62(4) . . . . ? N5B C5 C6 N6A 1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.229 _refine_diff_density_min -1.737 _refine_diff_density_rms 0.405 #===END data_complex_1b _database_code_depnum_ccdc_archive 'CCDC 767670' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H26 As Ce N6 O Se4' _chemical_formula_sum 'C6 H26 As Ce N6 O Se4' _chemical_formula_weight 729.21 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' Ce Ce -0.2486 2.6331 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3' _symmetry_space_group_name_Hall P63/m _symmetry_Int_Tables_number 147 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 19.073(3) _cell_length_b 19.073(3) _cell_length_c 9.4673(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2982.6(7) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12159 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2034 _exptl_absorpt_coefficient_mu 11.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1386 _exptl_absorpt_correction_T_max 0.2116 _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 28836 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3509 _reflns_number_gt 3447 _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^)+(0.0000P)^2^+609.0761P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3509 _refine_ls_number_parameters 133 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1749 _refine_ls_wR_factor_gt 0.1746 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.189 _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 As1 As 0.34791(16) 0.32498(15) 1.2500(3) 0.0112(6) Uani 1 1 d . . . Se1 Se 0.28023(17) 0.24298(16) 1.0589(3) 0.0197(6) Uani 1 1 d . . . Se2 Se 0.28024(17) 0.24299(16) 1.4411(3) 0.0197(6) Uani 1 1 d . . . Se3 Se 0.33847(16) 0.44065(15) 1.2500(3) 0.0148(6) Uani 1 1 d . . . Se4 Se 0.48176(17) 0.36112(18) 1.2500(4) 0.0266(8) Uani 1 1 d . . . Ce1 Ce 0.33711(9) 0.31422(9) 0.74997(16) 0.0110(4) Uani 1 1 d D . . N1 N 0.2672(12) 0.1484(13) 0.750(3) 0.0211(3) Uani 1 1 d D . . N2 N 0.1694(14) 0.2253(12) 0.749(3) 0.0206(3) Uani 1 1 d D . . N3A N 0.4813(18) 0.369(3) 0.882(5) 0.0332(5) Uani 0.54 1 d PD . . N3B N 0.439(2) 0.274(3) 0.869(8) 0.0392(5) Uani 0.46 1 d PD . . N4A N 0.440(2) 0.274(3) 0.632(7) 0.0382(5) Uani 0.54 1 d PD . . N4B N 0.482(2) 0.370(3) 0.621(6) 0.0380(5) Uani 0.46 1 d PD . . N5A N 0.274(3) 0.3965(18) 0.621(5) 0.0302(4) Uani 0.54 1 d PD . . N5B N 0.361(3) 0.449(4) 0.623(6) 0.0309(4) Uani 0.46 1 d PD . . N6A N 0.362(3) 0.449(3) 0.877(5) 0.0362(4) Uani 0.54 1 d PD . . N6B N 0.273(3) 0.396(2) 0.880(5) 0.0338(4) Uani 0.46 1 d PD . . C1 C 0.1782(12) 0.1000(14) 0.751(3) 0.0215(3) Uani 1 1 d D . . C2A C 0.137(3) 0.1429(17) 0.693(5) 0.0209(3) Uani 0.54 1 d PD . . C2B C 0.136(3) 0.1429(19) 0.806(6) 0.0213(3) Uani 0.46 1 d PD . . C3 C 0.5248(19) 0.3279(19) 0.831(3) 0.0328(5) Uani 1 1 d D . . C4 C 0.5249(18) 0.3273(19) 0.673(3) 0.0379(5) Uani 1 1 d D . . C5 C 0.3082(19) 0.4809(18) 0.671(3) 0.0360(4) Uani 1 1 d D . . C6 C 0.3081(19) 0.4803(18) 0.830(3) 0.0318(4) Uani 1 1 d D . . O1A O 0.450(2) 0.440(2) 0.585(4) 0.015(8) Uiso 0.51 1 d P . . O1B O 0.451(2) 0.440(2) 0.914(4) 0.014(8) Uiso 0.49 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0118(13) 0.0082(12) 0.0123(13) 0.0003(10) 0.0002(10) 0.0040(10) Se1 0.0261(15) 0.0172(13) 0.0213(11) -0.0015(10) -0.0018(10) 0.0073(12) Se2 0.0252(15) 0.0173(13) 0.0208(11) 0.0015(9) 0.0014(10) 0.0063(12) Se3 0.0135(13) 0.0102(12) 0.0208(15) 0.0001(10) 0.0002(11) 0.0061(11) Se4 0.0109(14) 0.0163(14) 0.054(2) 0.0003(14) 0.0003(13) 0.0077(12) Ce1 0.0104(7) 0.0110(7) 0.0100(8) 0.0000(6) 0.0000(5) 0.0041(6) N1 0.0202(7) 0.0147(7) 0.0278(8) -0.002(6) -0.002(6) 0.007(6) N2 0.0195(7) 0.0192(7) 0.0292(8) -0.001(6) -0.004(6) 0.008(6) N3A 0.0235(10) 0.0247(10) 0.0478(14) -0.002(9) 0.000(10) 0.005(8) N3B 0.0267(10) 0.0237(10) 0.0516(14) -0.001(9) 0.001(10) 0.007(8) N4A 0.0271(10) 0.0252(10) 0.0602(14) -0.004(9) 0.002(10) 0.008(8) N4B 0.0282(10) 0.0228(10) 0.0519(14) -0.001(9) 0.006(10) 0.003(8) N5A 0.0301(10) 0.0321(10) 0.0339(11) 0.002(8) -0.001(8) 0.014(8) N5B 0.0318(10) 0.0357(10) 0.0326(11) 0.000(8) -0.003(8) 0.018(8) N6A 0.0328(10) 0.0338(10) 0.0345(11) 0.006(8) -0.001(8) 0.009(8) N6B 0.0297(10) 0.0309(10) 0.0370(11) 0.000(8) -0.007(8) 0.013(8) C1 0.0182(7) 0.0137(7) 0.0267(8) -0.002(6) -0.005(6) 0.005(6) C2A 0.0201(7) 0.0183(7) 0.0259(8) -0.001(6) -0.003(6) 0.008(6) C2B 0.0198(7) 0.0148(7) 0.0301(8) -0.003(6) -0.006(6) 0.007(6) C3 0.0276(10) 0.0233(10) 0.0528(14) -0.003(9) 0.000(10) 0.009(8) C4 0.0262(10) 0.0252(10) 0.0573(14) -0.001(9) 0.003(10) 0.007(8) C5 0.0334(10) 0.0318(10) 0.0338(11) 0.004(8) -0.009(8) 0.010(8) C6 0.0341(10) 0.0312(10) 0.0352(11) 0.001(8) -0.003(8) 0.018(8) _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 As1 Se4 2.288(4) . ? As1 Se3 2.301(4) . ? As1 Se2 2.316(4) . ? As1 Se1 2.317(4) . ? Se1 Ce1 3.179(3) . ? Se2 Ce1 3.179(3) 1_556 ? Ce1 N6A 2.67(5) . ? Ce1 N5B 2.67(6) . ? Ce1 N3B 2.67(7) . ? Ce1 N4A 2.67(6) . ? Ce1 N6B 2.705(19) . ? Ce1 N5A 2.707(19) . ? Ce1 N4B 2.709(19) . ? Ce1 N3A 2.711(19) . ? Ce1 N1 2.75(2) . ? Ce1 O1B 2.77(4) . ? Ce1 O1A 2.77(4) . ? Ce1 N2 2.77(2) . ? N1 C1 1.472(10) . ? N2 C2B 1.471(10) . ? N2 C2A 1.472(10) . ? N3A C3 1.486(10) . ? N3B C3 1.476(10) . ? N4A C4 1.476(10) . ? N4B C4 1.486(10) . ? N5A C5 1.479(10) . ? N5B C5 1.485(10) . ? N6A C6 1.485(10) . ? N6B C6 1.479(10) . ? C1 C2A 1.498(10) . ? C1 C2B 1.498(10) . ? C3 C4 1.502(10) . ? C5 C6 1.506(10) . ? 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 Se4 As1 Se3 108.76(14) . . ? Se4 As1 Se2 111.39(16) . . ? Se3 As1 Se2 111.28(15) . . ? Se4 As1 Se1 111.38(16) . . ? Se3 As1 Se1 111.30(15) . . ? Se2 As1 Se1 102.67(14) . . ? As1 Se1 Ce1 118.28(12) . . ? As1 Se2 Ce1 118.28(12) . 1_556 ? N6A Ce1 N5B 53.7(15) . . ? N6A Ce1 N3B 106.5(16) . . ? N5B Ce1 N3B 131.9(14) . . ? N6A Ce1 N4A 131.7(13) . . ? N5B Ce1 N4A 106.8(15) . . ? N3B Ce1 N4A 49.8(19) . . ? N6A Ce1 N6B 31.7(14) . . ? N5B Ce1 N6B 63.8(11) . . ? N3B Ce1 N6B 125(2) . . ? N4A Ce1 N6B 163.4(13) . . ? N6A Ce1 N5A 63.8(10) . . ? N5B Ce1 N5A 31.5(15) . . ? N3B Ce1 N5A 163.4(13) . . ? N4A Ce1 N5A 125.4(17) . . ? N6B Ce1 N5A 53.9(15) . . ? N6A Ce1 N4B 100.1(17) . . ? N5B Ce1 N4B 76.7(12) . . ? N3B Ce1 N4B 63.5(13) . . ? N4A Ce1 N4B 34.2(15) . . ? N6B Ce1 N4B 130.2(14) . . ? N5A Ce1 N4B 103.7(14) . . ? N6A Ce1 N3A 76.2(11) . . ? N5B Ce1 N3A 100.4(17) . . ? N3B Ce1 N3A 34.2(15) . . ? N4A Ce1 N3A 63.9(12) . . ? N6B Ce1 N3A 103.1(15) . . ? N5A Ce1 N3A 130.2(13) . . ? N4B Ce1 N3A 54.2(17) . . ? N6A Ce1 N1 149.5(13) . . ? N5B Ce1 N1 149.5(14) . . ? N3B Ce1 N1 71.0(12) . . ? N4A Ce1 N1 71.0(11) . . ? N6B Ce1 N1 124.3(9) . . ? N5A Ce1 N1 124.5(9) . . ? N4B Ce1 N1 105.2(12) . . ? N3A Ce1 N1 105.2(11) . . ? N6A Ce1 O1B 39.1(11) . . ? N5B Ce1 O1B 74.5(15) . . ? N3B Ce1 O1B 69.2(15) . . ? N4A Ce1 O1B 96.7(11) . . ? N6B Ce1 O1B 68.0(15) . . ? N5A Ce1 O1B 97.7(10) . . ? N4B Ce1 O1B 73.2(16) . . ? N3A Ce1 O1B 37.1(10) . . ? N1 Ce1 O1B 135.8(9) . . ? N6A Ce1 O1A 74.5(14) . . ? N5B Ce1 O1A 39.1(11) . . ? N3B Ce1 O1A 97.1(12) . . ? N4A Ce1 O1A 69.4(14) . . ? N6B Ce1 O1A 97.8(10) . . ? N5A Ce1 O1A 67.8(13) . . ? N4B Ce1 O1A 37.6(11) . . ? N3A Ce1 O1A 74.0(14) . . ? N1 Ce1 O1A 135.7(9) . . ? O1B Ce1 O1A 68.5(11) . . ? N6A Ce1 N2 100.6(10) . . ? N5B Ce1 N2 100.4(12) . . ? N3B Ce1 N2 127.5(10) . . ? N4A Ce1 N2 127.5(9) . . ? N6B Ce1 N2 68.9(12) . . ? N5A Ce1 N2 68.9(11) . . ? N4B Ce1 N2 151.6(15) . . ? N3A Ce1 N2 151.0(13) . . ? N1 Ce1 N2 63.2(6) . . ? O1B Ce1 N2 133.9(9) . . ? O1A Ce1 N2 133.6(9) . . ? C1 N1 Ce1 117.7(15) . . ? C2B N2 C2A 43(3) . . ? C2B N2 Ce1 114(2) . . ? C2A N2 Ce1 113(2) . . ? C3 N3A Ce1 112(2) . . ? C3 N3B Ce1 114(4) . . ? C4 N4A Ce1 114(3) . . ? C4 N4B Ce1 112(2) . . ? C5 N5A Ce1 113.6(18) . . ? C5 N5B Ce1 115(3) . . ? C6 N6A Ce1 115(3) . . ? C6 N6B Ce1 113.3(18) . . ? N1 C1 C2A 114(3) . . ? N1 C1 C2B 115(3) . . ? C2A C1 C2B 42(3) . . ? N2 C2A C1 113(2) . . ? N2 C2B C1 113(2) . . ? N3B C3 N3A 65(3) . . ? N3B C3 C4 104(4) . . ? N3A C3 C4 109(3) . . ? N4A C4 N4B 65(3) . . ? N4A C4 C3 105(3) . . ? N4B C4 C3 109(3) . . ? N5A C5 N5B 59(3) . . ? N5A C5 C6 108(3) . . ? N5B C5 C6 108(3) . . ? N6B C6 N6A 59(3) . . ? N6B C6 C5 109(3) . . ? N6A C6 C5 108(3) . . ? 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 Se4 As1 Se1 Ce1 -61.40(18) . . . . ? Se3 As1 Se1 Ce1 60.16(18) . . . . ? Se2 As1 Se1 Ce1 179.30(12) . . . . ? Se4 As1 Se2 Ce1 61.40(18) . . . 1_556 ? Se3 As1 Se2 Ce1 -60.15(18) . . . 1_556 ? Se1 As1 Se2 Ce1 -179.30(12) . . . 1_556 ? N6A Ce1 N1 C1 63(3) . . . . ? N5B Ce1 N1 C1 -63(3) . . . . ? N3B Ce1 N1 C1 153(3) . . . . ? N4A Ce1 N1 C1 -154(3) . . . . ? N6B Ce1 N1 C1 33(3) . . . . ? N5A Ce1 N1 C1 -34(3) . . . . ? N4B Ce1 N1 C1 -153(2) . . . . ? N3A Ce1 N1 C1 151(2) . . . . ? O1B Ce1 N1 C1 126(2) . . . . ? O1A Ce1 N1 C1 -127(2) . . . . ? N2 Ce1 N1 C1 -0.5(19) . . . . ? N6A Ce1 N2 C2B -129(3) . . . . ? N5B Ce1 N2 C2B 176(3) . . . . ? N3B Ce1 N2 C2B -9(3) . . . . ? N4A Ce1 N2 C2B 56(3) . . . . ? N6B Ce1 N2 C2B -127(3) . . . . ? N5A Ce1 N2 C2B 175(3) . . . . ? N4B Ce1 N2 C2B 95(3) . . . . ? N3A Ce1 N2 C2B -49(3) . . . . ? N1 Ce1 N2 C2B 24(2) . . . . ? O1B Ce1 N2 C2B -105(3) . . . . ? O1A Ce1 N2 C2B 152(3) . . . . ? N6A Ce1 N2 C2A -176(2) . . . . ? N5B Ce1 N2 C2A 129(3) . . . . ? N3B Ce1 N2 C2A -55(3) . . . . ? N4A Ce1 N2 C2A 9(3) . . . . ? N6B Ce1 N2 C2A -174(3) . . . . ? N5A Ce1 N2 C2A 128(3) . . . . ? N4B Ce1 N2 C2A 48(3) . . . . ? N3A Ce1 N2 C2A -95(3) . . . . ? N1 Ce1 N2 C2A -23(2) . . . . ? O1B Ce1 N2 C2A -152(2) . . . . ? O1A Ce1 N2 C2A 105(2) . . . . ? N6A Ce1 N3A C3 -166(4) . . . . ? N5B Ce1 N3A C3 -118(3) . . . . ? N3B Ce1 N3A C3 42(3) . . . . ? N4A Ce1 N3A C3 -14(3) . . . . ? N6B Ce1 N3A C3 177(3) . . . . ? N5A Ce1 N3A C3 -130(3) . . . . ? N4B Ce1 N3A C3 -53(3) . . . . ? N1 Ce1 N3A C3 45(3) . . . . ? O1B Ce1 N3A C3 -164(5) . . . . ? O1A Ce1 N3A C3 -89(3) . . . . ? N2 Ce1 N3A C3 107(3) . . . . ? N6A Ce1 N3B C3 -72(4) . . . . ? N5B Ce1 N3B C3 -16(5) . . . . ? N4A Ce1 N3B C3 60(4) . . . . ? N6B Ce1 N3B C3 -100(4) . . . . ? N5A Ce1 N3B C3 -20(9) . . . . ? N4B Ce1 N3B C3 22(4) . . . . ? N3A Ce1 N3B C3 -43(3) . . . . ? N1 Ce1 N3B C3 140(4) . . . . ? O1B Ce1 N3B C3 -59(4) . . . . ? O1A Ce1 N3B C3 4(4) . . . . ? N2 Ce1 N3B C3 170(3) . . . . ? N6A Ce1 N4A C4 17(5) . . . . ? N5B Ce1 N4A C4 73(4) . . . . ? N3B Ce1 N4A C4 -59(3) . . . . ? N6B Ce1 N4A C4 20(8) . . . . ? N5A Ce1 N4A C4 101(4) . . . . ? N4B Ce1 N4A C4 43(3) . . . . ? N3A Ce1 N4A C4 -21(3) . . . . ? N1 Ce1 N4A C4 -139(4) . . . . ? O1B Ce1 N4A C4 -3(4) . . . . ? O1A Ce1 N4A C4 61(3) . . . . ? N2 Ce1 N4A C4 -169(3) . . . . ? N6A Ce1 N4B C4 118(4) . . . . ? N5B Ce1 N4B C4 167(4) . . . . ? N3B Ce1 N4B C4 15(3) . . . . ? N4A Ce1 N4B C4 -42(3) . . . . ? N6B Ce1 N4B C4 130(3) . . . . ? N5A Ce1 N4B C4 -176(3) . . . . ? N3A Ce1 N4B C4 54(3) . . . . ? N1 Ce1 N4B C4 -44(4) . . . . ? O1B Ce1 N4B C4 90(4) . . . . ? O1A Ce1 N4B C4 166(6) . . . . ? N2 Ce1 N4B C4 -106(4) . . . . ? N6A Ce1 N5A C5 17(3) . . . . ? N5B Ce1 N5A C5 -46(3) . . . . ? N3B Ce1 N5A C5 -40(8) . . . . ? N4A Ce1 N5A C5 -107(3) . . . . ? N6B Ce1 N5A C5 52(3) . . . . ? N4B Ce1 N5A C5 -78(3) . . . . ? N3A Ce1 N5A C5 -23(4) . . . . ? N1 Ce1 N5A C5 163(2) . . . . ? O1B Ce1 N5A C5 -3(3) . . . . ? O1A Ce1 N5A C5 -66(3) . . . . ? N2 Ce1 N5A C5 131(3) . . . . ? N6A Ce1 N5B C5 -52(3) . . . . ? N3B Ce1 N5B C5 -131(3) . . . . ? N4A Ce1 N5B C5 178(3) . . . . ? N6B Ce1 N5B C5 -16(3) . . . . ? N5A Ce1 N5B C5 47(3) . . . . ? N4B Ce1 N5B C5 -165(4) . . . . ? N3A Ce1 N5B C5 -116(4) . . . . ? N1 Ce1 N5B C5 97(4) . . . . ? O1B Ce1 N5B C5 -89(4) . . . . ? O1A Ce1 N5B C5 -164(5) . . . . ? N2 Ce1 N5B C5 44(4) . . . . ? N5B Ce1 N6A C6 52(3) . . . . ? N3B Ce1 N6A C6 -178(3) . . . . ? N4A Ce1 N6A C6 132(3) . . . . ? N6B Ce1 N6A C6 -47(2) . . . . ? N5A Ce1 N6A C6 17(3) . . . . ? N4B Ce1 N6A C6 117(3) . . . . ? N3A Ce1 N6A C6 166(4) . . . . ? N1 Ce1 N6A C6 -97(3) . . . . ? O1B Ce1 N6A C6 164(5) . . . . ? O1A Ce1 N6A C6 89(3) . . . . ? N2 Ce1 N6A C6 -43(3) . . . . ? N6A Ce1 N6B C6 46(2) . . . . ? N5B Ce1 N6B C6 -17(3) . . . . ? N3B Ce1 N6B C6 108(3) . . . . ? N4A Ce1 N6B C6 42(8) . . . . ? N5A Ce1 N6B C6 -52(3) . . . . ? N4B Ce1 N6B C6 25(5) . . . . ? N3A Ce1 N6B C6 78(4) . . . . ? N1 Ce1 N6B C6 -163(3) . . . . ? O1B Ce1 N6B C6 66(3) . . . . ? O1A Ce1 N6B C6 3(4) . . . . ? N2 Ce1 N6B C6 -131(4) . . . . ? Ce1 N1 C1 C2A 24(3) . . . . ? Ce1 N1 C1 C2B -22(4) . . . . ? C2B N2 C2A C1 -54(3) . . . . ? Ce1 N2 C2A C1 46(4) . . . . ? N1 C1 C2A N2 -47(5) . . . . ? C2B C1 C2A N2 54(3) . . . . ? C2A N2 C2B C1 54(3) . . . . ? Ce1 N2 C2B C1 -45(5) . . . . ? N1 C1 C2B N2 45(5) . . . . ? C2A C1 C2B N2 -54(3) . . . . ? Ce1 N3B C3 N3A 51(3) . . . . ? Ce1 N3B C3 C4 -54(4) . . . . ? Ce1 N3A C3 N3B -49(4) . . . . ? Ce1 N3A C3 C4 48(4) . . . . ? Ce1 N4A C4 N4B -51(3) . . . . ? Ce1 N4A C4 C3 53(4) . . . . ? Ce1 N4B C4 N4A 49(3) . . . . ? Ce1 N4B C4 C3 -50(4) . . . . ? N3B C3 C4 N4A 0(4) . . . . ? N3A C3 C4 N4A -67(4) . . . . ? N3B C3 C4 N4B 68(4) . . . . ? N3A C3 C4 N4B 1(4) . . . . ? Ce1 N5A C5 N5B 52(3) . . . . ? Ce1 N5A C5 C6 -48(3) . . . . ? Ce1 N5B C5 N5A -54(3) . . . . ? Ce1 N5B C5 C6 47(4) . . . . ? Ce1 N6B C6 N6A -52(3) . . . . ? Ce1 N6B C6 C5 48(4) . . . . ? Ce1 N6A C6 N6B 54(3) . . . . ? Ce1 N6A C6 C5 -48(4) . . . . ? N5A C5 C6 N6B 0(4) . . . . ? N5B C5 C6 N6B -62(4) . . . . ? N5A C5 C6 N6A 63(4) . . . . ? N5B C5 C6 N6A 0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.465 _refine_diff_density_min -1.245 _refine_diff_density_rms 0.487 #===END data_complex_1c _database_code_depnum_ccdc_archive 'CCDC 767671' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H26 As N6 Nd O Se4' _chemical_formula_sum 'C6 H26 As N6 Nd O Se4' _chemical_formula_weight 733.33 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' As As 0.0499 2.0058 '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' Nd Nd -0.1943 3.0179 '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 n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x, -y+1/2, z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x, y-1/2, -z' 'x-1/2, y, -z-1/2' _cell_length_a 9.4580(16) _cell_length_b 13.545(3) _cell_length_c 14.948(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1915.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6749 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description cube _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 12.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0434 _exptl_absorpt_correction_T_max 0.1229 _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 16550 _diffrn_reflns_av_R_equivalents 0.0988 _diffrn_reflns_av_sigmaI/netI 0.0858 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1755 _reflns_number_gt 1415 _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^)+(0.0853P)^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 1755 _refine_ls_number_parameters 92 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.097 _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 As1 As 0.71829(17) 0.2500 0.53952(11) 0.0133(5) Uani 1 2 d S . . Se1 Se 0.53365(17) 0.2500 0.43899(11) 0.0189(5) Uani 1 2 d S . . Se2 Se 0.91820(19) 0.2500 0.45179(12) 0.0271(5) Uani 1 2 d S . . Se3 Se 0.70913(13) 0.11186(9) 0.63025(8) 0.0204(4) Uani 1 1 d . . . Nd1 Nd 0.23533(9) 0.2500 0.52848(6) 0.0112(3) Uani 1 2 d S . . N1 N 0.0953(11) 0.1371(7) 0.6367(7) 0.027(3) Uani 1 1 d . . . H1A H 0.1176 0.1541 0.6932 0.033 Uiso 1 1 calc R . . H1B H 0.0025 0.1490 0.6292 0.033 Uiso 1 1 calc R . . N2 N 0.3437(11) 0.0729(7) 0.5513(6) 0.022(2) Uani 1 1 d . . . H2A H 0.3365 0.0399 0.4993 0.026 Uiso 1 1 calc R . . H2B H 0.4364 0.0798 0.5633 0.026 Uiso 1 1 calc R . . N3 N 0.2142(13) 0.1438(8) 0.3775(6) 0.0264(3) Uani 1 1 d D . . C1 C 0.1203(14) 0.0284(9) 0.6259(10) 0.034(3) Uani 1 1 d . . . H1C H 0.0772 0.0052 0.5709 0.041 Uiso 1 1 calc R . . H1D H 0.0787 -0.0074 0.6755 0.041 Uiso 1 1 calc R . . C2 C 0.2792(15) 0.0111(9) 0.6233(9) 0.027(3) Uani 1 1 d . . . H2C H 0.3204 0.0282 0.6806 0.033 Uiso 1 1 calc R . . H2D H 0.2983 -0.0581 0.6117 0.033 Uiso 1 1 calc R . . C3A C 0.184(2) 0.1985(14) 0.2937(10) 0.0286(3) Uani 0.62 1 d PD . . C3B C 0.263(3) 0.199(3) 0.296(2) 0.0291(3) Uani 0.38 1 d PD . . O1 O 0.3823(14) 0.2500 0.6777(9) 0.039(3) Uani 1 2 d S . . 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 As1 0.0085(9) 0.0108(9) 0.0206(10) 0.000 0.0001(7) 0.000 Se1 0.0105(9) 0.0265(10) 0.0198(9) 0.000 -0.0006(7) 0.000 Se2 0.0100(10) 0.0478(13) 0.0234(10) 0.000 0.0006(8) 0.000 Se3 0.0225(8) 0.0103(7) 0.0285(8) 0.0032(5) -0.0024(5) 0.0017(5) Nd1 0.0119(5) 0.0053(5) 0.0163(6) 0.000 -0.0004(3) 0.005 N1 0.017(6) 0.017(6) 0.048(7) 0.005(5) 0.001(5) 0.006(5) N2 0.020(6) 0.014(5) 0.031(6) 0.003(4) -0.003(5) 0.000(5) N3 0.0382(8) 0.0202(5) 0.0181(4) -0.004(4) -0.006(5) 0.007(5) C1 0.026(8) 0.020(7) 0.058(10) 0.001(6) 0.000(7) -0.009(6) C2 0.042(9) 0.011(6) 0.029(8) 0.007(5) 0.004(6) 0.009(6) C3A 0.0378(8) 0.0253(5) 0.0226(4) -0.003(4) -0.004(5) 0.009(5) C3B 0.0325(8) 0.0268(5) 0.0281(4) -0.002(4) -0.005(5) 0.007(5) O1 0.037(9) 0.031(7) 0.048(9) 0.000 -0.001(7) 0.000 _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 As1 Se2 2.301(2) . ? As1 Se1 2.304(2) . ? As1 Se3 2.3126(16) . ? As1 Se3 2.3126(16) 3 ? Se1 Nd1 3.1225(19) . ? Se2 Nd1 3.211(2) 1_655 ? Nd1 N1 2.590(10) . ? Nd1 N1 2.590(10) 3 ? Nd1 O1 2.628(14) . ? Nd1 N2 2.630(9) 3 ? Nd1 N2 2.630(9) . ? Nd1 N3 2.684(10) . ? Nd1 N3 2.684(10) 3 ? Nd1 Se2 3.211(2) 1_455 ? N1 C1 1.501(16) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.494(15) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C3A 1.483(12) . ? N3 C3B 1.50(4) . ? C1 C2 1.521(17) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3A C3A 1.39(4) 3 ? C3A C3B 1.58(3) 3 ? C3B C3B 1.39(8) 3 ? C3B C3A 1.58(3) 3 ? 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 As1 Se1 104.54(9) . . ? Se2 As1 Se3 111.41(6) . . ? Se1 As1 Se3 110.74(6) . . ? Se2 As1 Se3 111.41(6) . 3 ? Se1 As1 Se3 110.74(6) . 3 ? Se3 As1 Se3 108.02(9) . 3 ? As1 Se1 Nd1 113.92(7) . . ? As1 Se2 Nd1 124.34(8) . 1_655 ? N1 Nd1 N1 72.3(4) . 3 ? N1 Nd1 O1 75.0(3) . . ? N1 Nd1 O1 75.0(3) 3 . ? N1 Nd1 N2 131.0(3) . 3 ? N1 Nd1 N2 65.2(3) 3 3 ? O1 Nd1 N2 71.6(2) . 3 ? N1 Nd1 N2 65.2(3) . . ? N1 Nd1 N2 131.0(3) 3 . ? O1 Nd1 N2 71.6(2) . . ? N2 Nd1 N2 131.5(5) 3 . ? N1 Nd1 N3 99.8(3) . . ? N1 Nd1 N3 143.5(3) 3 . ? O1 Nd1 N3 138.9(3) . . ? N2 Nd1 N3 128.8(3) 3 . ? N2 Nd1 N3 69.5(3) . . ? N1 Nd1 N3 143.5(3) . 3 ? N1 Nd1 N3 99.8(3) 3 3 ? O1 Nd1 N3 138.9(3) . 3 ? N2 Nd1 N3 69.5(3) 3 3 ? N2 Nd1 N3 128.8(3) . 3 ? N3 Nd1 N3 64.8(5) . 3 ? N1 Nd1 Se1 136.9(2) . . ? N1 Nd1 Se1 136.9(2) 3 . ? O1 Nd1 Se1 83.4(3) . . ? N2 Nd1 Se1 72.7(2) 3 . ? N2 Nd1 Se1 72.7(2) . . ? N3 Nd1 Se1 73.0(3) . . ? N3 Nd1 Se1 73.0(3) 3 . ? N1 Nd1 Se2 75.3(2) . 1_455 ? N1 Nd1 Se2 75.3(2) 3 1_455 ? O1 Nd1 Se2 142.9(3) . 1_455 ? N2 Nd1 Se2 114.2(2) 3 1_455 ? N2 Nd1 Se2 114.2(2) . 1_455 ? N3 Nd1 Se2 68.3(3) . 1_455 ? N3 Nd1 Se2 68.3(3) 3 1_455 ? Se1 Nd1 Se2 133.72(5) . 1_455 ? C1 N1 Nd1 115.5(8) . . ? C1 N1 H1A 108.4 . . ? Nd1 N1 H1A 108.4 . . ? C1 N1 H1B 108.4 . . ? Nd1 N1 H1B 108.4 . . ? H1A N1 H1B 107.5 . . ? C2 N2 Nd1 116.5(7) . . ? C2 N2 H2A 108.2 . . ? Nd1 N2 H2A 108.2 . . ? C2 N2 H2B 108.2 . . ? Nd1 N2 H2B 108.2 . . ? H2A N2 H2B 107.3 . . ? C3A N3 C3B 29.3(8) . . ? C3A N3 Nd1 117.1(10) . . ? C3B N3 Nd1 113.1(15) . . ? N1 C1 C2 108.0(10) . . ? N1 C1 H1C 110.1 . . ? C2 C1 H1C 110.1 . . ? N1 C1 H1D 110.1 . . ? C2 C1 H1D 110.1 . . ? H1C C1 H1D 108.4 . . ? N2 C2 C1 109.6(10) . . ? N2 C2 H2C 109.7 . . ? C1 C2 H2C 109.7 . . ? N2 C2 H2D 109.7 . . ? C1 C2 H2D 109.7 . . ? H2C C2 H2D 108.2 . . ? C3A C3A N3 120.0(9) 3 . ? C3A C3A C3B 28.4(9) 3 3 ? N3 C3A C3B 109.2(18) . 3 ? C3B C3B N3 119.8(15) 3 . ? C3B C3B C3A 28.4(9) 3 3 ? N3 C3B C3A 108(2) . 3 ? 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 As1 Se1 Nd1 180.0 . . . . ? Se3 As1 Se1 Nd1 59.90(6) . . . . ? Se3 As1 Se1 Nd1 -59.90(6) 3 . . . ? Se1 As1 Se2 Nd1 180.0 . . . 1_655 ? Se3 As1 Se2 Nd1 -60.36(6) . . . 1_655 ? Se3 As1 Se2 Nd1 60.36(6) 3 . . 1_655 ? As1 Se1 Nd1 N1 -59.7(4) . . . . ? As1 Se1 Nd1 N1 59.7(4) . . . 3 ? As1 Se1 Nd1 O1 0.000(1) . . . . ? As1 Se1 Nd1 N2 72.7(2) . . . 3 ? As1 Se1 Nd1 N2 -72.7(2) . . . . ? As1 Se1 Nd1 N3 -145.9(2) . . . . ? As1 Se1 Nd1 N3 145.9(2) . . . 3 ? As1 Se1 Nd1 Se2 180.0 . . . 1_455 ? N1 Nd1 N1 C1 -176.6(7) 3 . . . ? O1 Nd1 N1 C1 -97.9(9) . . . . ? N2 Nd1 N1 C1 -146.0(8) 3 . . . ? N2 Nd1 N1 C1 -21.6(8) . . . . ? N3 Nd1 N1 C1 40.2(9) . . . . ? N3 Nd1 N1 C1 100.8(9) 3 . . . ? Se1 Nd1 N1 C1 -35.3(10) . . . . ? Se2 Nd1 N1 C1 104.5(8) 1_455 . . . ? N1 Nd1 N2 C2 -8.9(8) . . . . ? N1 Nd1 N2 C2 23.4(10) 3 . . . ? O1 Nd1 N2 C2 72.6(9) . . . . ? N2 Nd1 N2 C2 114.9(8) 3 . . . ? N3 Nd1 N2 C2 -120.9(9) . . . . ? N3 Nd1 N2 C2 -148.8(8) 3 . . . ? Se1 Nd1 N2 C2 161.3(9) . . . . ? Se2 Nd1 N2 C2 -67.9(9) 1_455 . . . ? N1 Nd1 N3 C3A 137.4(12) . . . . ? N1 Nd1 N3 C3A 63.8(14) 3 . . . ? O1 Nd1 N3 C3A -144.3(12) . . . . ? N2 Nd1 N3 C3A -36.6(14) 3 . . . ? N2 Nd1 N3 C3A -163.9(13) . . . . ? N3 Nd1 N3 C3A -7.7(13) 3 . . . ? Se1 Nd1 N3 C3A -86.4(12) . . . . ? Se2 Nd1 N3 C3A 67.7(12) 1_455 . . . ? N1 Nd1 N3 C3B 169.5(14) . . . . ? N1 Nd1 N3 C3B 95.9(14) 3 . . . ? O1 Nd1 N3 C3B -112.2(14) . . . . ? N2 Nd1 N3 C3B -4.5(15) 3 . . . ? N2 Nd1 N3 C3B -131.8(14) . . . . ? N3 Nd1 N3 C3B 24.4(14) 3 . . . ? Se1 Nd1 N3 C3B -54.3(13) . . . . ? Se2 Nd1 N3 C3B 99.8(14) 1_455 . . . ? Nd1 N1 C1 C2 48.9(12) . . . . ? Nd1 N2 C2 C1 37.2(12) . . . . ? N1 C1 C2 N2 -55.1(14) . . . . ? C3B N3 C3A C3A -82(4) . . . 3 ? Nd1 N3 C3A C3A 7.5(13) . . . 3 ? C3B N3 C3A C3B -53(4) . . . 3 ? Nd1 N3 C3A C3B 36.5(17) . . . 3 ? C3A N3 C3B C3B 81(3) . . . 3 ? Nd1 N3 C3B C3B -23.7(13) . . . 3 ? C3A N3 C3B C3A 53(3) . . . 3 ? Nd1 N3 C3B C3A -52.1(17) . . . 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 N2 H2B Se3 0.90 2.80 3.690(11) 170.0 . N2 H2A Se3 0.90 2.86 3.726(10) 162.8 5_656 N1 H1B Se3 0.90 2.82 3.670(10) 158.1 1_455 N1 H1A Se3 0.90 2.84 3.662(11) 153.2 8_557 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.740 _refine_diff_density_min -1.460 _refine_diff_density_rms 0.382 #===END data_complex_1d _database_code_depnum_ccdc_archive 'CCDC 767672' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H36 As N9 Se4 Sm' _chemical_formula_sum 'C9 H36 As N9 Se4 Sm' _chemical_formula_weight 811.57 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' Sm Sm -0.1578 3.6682 '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' _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 11.1989(17) _cell_length_b 12.9457(19) _cell_length_c 16.241(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.360(3) _cell_angle_gamma 90.00 _cell_volume 2352.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8713 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 10.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1155 _exptl_absorpt_correction_T_max 0.3323 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 22515 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4304 _reflns_number_gt 4060 _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^)+(0.0215P)^2^+5.0871P] 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 4304 _refine_ls_number_parameters 221 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.170 _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 As1 As 0.50216(4) 0.72517(3) 0.31007(3) 0.01132(10) Uani 1 1 d . . . Sm1 Sm 0.517867(19) 0.266559(16) 0.325406(13) 0.01079(7) Uani 1 1 d . . . Se1 Se 0.36484(4) 0.61564(3) 0.36869(3) 0.01500(11) Uani 1 1 d . . . Se2 Se 0.67104(4) 0.74054(4) 0.39587(3) 0.01833(11) Uani 1 1 d . . . Se3 Se 0.41026(4) 0.88433(3) 0.29811(3) 0.02107(12) Uani 1 1 d . . . Se4 Se 0.55390(4) 0.65757(4) 0.18555(3) 0.01757(11) Uani 1 1 d . . . N1 N 0.7192(3) 0.3420(3) 0.2896(2) 0.0185(8) Uani 1 1 d . . . H1A H 0.7782 0.2957 0.3053 0.022 Uiso 1 1 calc R . . H1B H 0.7206 0.3495 0.2333 0.022 Uiso 1 1 calc R . . N2 N 0.5774(3) 0.4201(3) 0.4154(2) 0.0151(8) Uani 1 1 d . . . H2A H 0.5367 0.4776 0.3965 0.018 Uiso 1 1 calc R . . H2B H 0.5553 0.4076 0.4684 0.018 Uiso 1 1 calc R . . N3 N 0.3363(3) 0.3247(3) 0.4015(2) 0.0146(8) Uani 1 1 d . . . H3A H 0.3579 0.3308 0.4565 0.018 Uiso 1 1 calc R . . H3B H 0.3147 0.3894 0.3827 0.018 Uiso 1 1 calc R . . N4 N 0.3455(3) 0.1416(3) 0.3092(2) 0.0192(8) Uani 1 1 d . . . H4A H 0.3002 0.1577 0.2625 0.023 Uiso 1 1 calc R . . H4B H 0.3745 0.0756 0.3034 0.023 Uiso 1 1 calc R . . N5 N 0.5314(3) 0.2119(3) 0.1743(2) 0.0170(8) Uani 1 1 d . . . H5A H 0.6101 0.2145 0.1603 0.020 Uiso 1 1 calc R . . H5B H 0.5063 0.1445 0.1690 0.020 Uiso 1 1 calc R . . N6 N 0.4238(4) 0.3991(3) 0.2259(2) 0.0193(9) Uani 1 1 d . . . H6A H 0.3420 0.3920 0.2250 0.023 Uiso 1 1 calc R . . H6B H 0.4422 0.4645 0.2447 0.023 Uiso 1 1 calc R . . N7 N 0.5679(4) 0.1921(3) 0.4708(2) 0.0274(10) Uani 1 1 d D . . N8 N 0.6384(3) 0.0979(3) 0.3235(2) 0.0158(8) Uani 1 1 d . . . H8A H 0.5939 0.0496 0.2942 0.019 Uiso 1 1 calc R . . H8B H 0.7065 0.1098 0.2951 0.019 Uiso 1 1 calc R . . N9 N 0.4314(4) 1.0086(3) 0.1030(2) 0.0221(9) Uani 1 1 d . . . H9B H 0.4195 0.9624 0.1406 0.027 Uiso 1 1 d R . . H9A H 0.3673 1.0348 0.0905 0.027 Uiso 1 1 d R . . C1 C 0.7470(4) 0.4430(4) 0.3287(3) 0.0189(10) Uani 1 1 d . . . H1C H 0.7050 0.4989 0.2976 0.023 Uiso 1 1 calc R . . H1D H 0.8340 0.4564 0.3280 0.023 Uiso 1 1 calc R . . C2 C 0.7075(4) 0.4413(3) 0.4162(3) 0.0167(10) Uani 1 1 d . . . H2C H 0.7515 0.3869 0.4478 0.020 Uiso 1 1 calc R . . H2D H 0.7248 0.5086 0.4429 0.020 Uiso 1 1 calc R . . C3 C 0.2300(4) 0.2566(3) 0.3935(3) 0.0170(10) Uani 1 1 d . . . H3C H 0.1785 0.2784 0.3456 0.020 Uiso 1 1 calc R . . H3D H 0.1829 0.2620 0.4436 0.020 Uiso 1 1 calc R . . C4 C 0.2698(4) 0.1463(3) 0.3820(3) 0.0180(10) Uani 1 1 d . . . H4C H 0.3159 0.1224 0.4318 0.022 Uiso 1 1 calc R . . H4D H 0.1993 0.1008 0.3734 0.022 Uiso 1 1 calc R . . C5 C 0.4593(5) 0.2768(4) 0.1159(3) 0.0268(12) Uani 1 1 d . . . H5C H 0.3751 0.2534 0.1146 0.032 Uiso 1 1 calc R . . H5D H 0.4895 0.2688 0.0598 0.032 Uiso 1 1 calc R . . C6 C 0.4656(5) 0.3877(4) 0.1406(3) 0.0270(12) Uani 1 1 d . . . H6C H 0.5489 0.4128 0.1381 0.032 Uiso 1 1 calc R . . H6D H 0.4148 0.4296 0.1021 0.032 Uiso 1 1 calc R . . C7A C 0.5845(7) 0.0782(6) 0.4685(5) 0.0194(14) Uani 0.50 1 d PD . . C7B C 0.6827(7) 0.1343(6) 0.4710(5) 0.0194(14) Uani 0.50 1 d PD . . C8 C 0.6743(5) 0.0525(4) 0.4044(3) 0.0269(12) Uani 1 1 d D . . C9 C 0.4735(4) 0.9596(3) 0.0278(3) 0.0180(10) Uani 1 1 d . . . H9C H 0.4058 0.9246 -0.0018 0.022 Uiso 1 1 calc R . . H9D H 0.5346 0.9068 0.0427 0.022 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 As1 0.0107(2) 0.0132(2) 0.0101(2) 0.00090(17) 0.00066(17) 0.00014(17) Sm1 0.01040(12) 0.01188(12) 0.01012(12) -0.00196(8) 0.00087(8) 0.00037(8) Se1 0.0137(2) 0.0154(2) 0.0161(2) 0.00117(18) 0.00323(18) -0.00185(17) Se2 0.0121(2) 0.0315(3) 0.0113(2) 0.00163(19) -0.00110(18) -0.00191(19) Se3 0.0274(3) 0.0131(2) 0.0222(3) 0.00103(19) -0.0046(2) 0.00349(19) Se4 0.0127(2) 0.0271(3) 0.0130(2) -0.00433(19) 0.00136(17) 0.00024(19) N1 0.018(2) 0.023(2) 0.014(2) -0.0038(16) 0.0024(16) -0.0010(16) N2 0.0133(19) 0.0160(19) 0.0160(19) -0.0025(16) 0.0008(15) 0.0004(15) N3 0.017(2) 0.0141(18) 0.0132(19) 0.0008(15) 0.0012(15) -0.0004(15) N4 0.016(2) 0.0144(19) 0.027(2) -0.0059(17) 0.0002(17) -0.0002(16) N5 0.017(2) 0.020(2) 0.0141(19) -0.0039(16) 0.0010(15) 0.0023(16) N6 0.025(2) 0.0162(19) 0.017(2) -0.0030(16) 0.0007(17) 0.0032(16) N7 0.049(3) 0.020(2) 0.014(2) -0.0001(17) 0.0023(19) 0.021(2) N8 0.0156(19) 0.0153(19) 0.017(2) -0.0040(16) 0.0024(15) 0.0022(15) N9 0.021(2) 0.024(2) 0.022(2) 0.0034(17) 0.0038(17) -0.0023(17) C1 0.017(2) 0.022(2) 0.017(2) 0.003(2) 0.0007(19) -0.002(2) C2 0.016(2) 0.019(2) 0.015(2) -0.0020(19) -0.0011(18) -0.0049(19) C3 0.010(2) 0.026(2) 0.015(2) -0.0019(19) -0.0001(18) -0.0002(18) C4 0.015(2) 0.014(2) 0.025(3) 0.002(2) -0.0023(19) -0.0029(18) C5 0.036(3) 0.032(3) 0.013(2) -0.003(2) -0.002(2) 0.004(2) C6 0.035(3) 0.028(3) 0.018(3) 0.000(2) 0.002(2) 0.002(2) C7A 0.016(3) 0.020(3) 0.023(4) 0.001(3) 0.001(3) 0.003(3) C7B 0.016(3) 0.020(3) 0.023(4) 0.001(3) 0.001(3) 0.003(3) C8 0.034(3) 0.026(3) 0.021(3) 0.006(2) 0.005(2) 0.014(2) C9 0.015(2) 0.020(2) 0.019(2) 0.002(2) 0.0012(19) -0.0023(19) _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 As1 Se4 2.2996(7) . ? As1 Se3 2.3078(7) . ? As1 Se2 2.3112(7) . ? As1 Se1 2.3243(6) . ? Sm1 N4 2.523(4) . ? Sm1 N3 2.537(3) . ? Sm1 N2 2.540(3) . ? Sm1 N1 2.546(4) . ? Sm1 N6 2.555(4) . ? Sm1 N5 2.564(4) . ? Sm1 N8 2.568(3) . ? Sm1 N7 2.591(4) . ? N1 C1 1.480(6) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C2 1.482(5) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C3 1.483(5) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N4 C4 1.484(6) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? N5 C5 1.481(6) . ? N5 H5A 0.9200 . ? N5 H5B 0.9200 . ? N6 C6 1.487(6) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? N7 C7A 1.487(7) . ? N7 C7B 1.488(7) . ? N8 C8 1.480(6) . ? N8 H8A 0.9200 . ? N8 H8B 0.9200 . ? N9 H9A 0.8116 . ? N9 C9 1.471(6) . ? N9 H9B 0.8692 . ? N9 H9A 0.8116 . ? C1 C2 1.507(6) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 C4 1.509(6) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? C5 C6 1.492(7) . ? C5 H5C 0.9900 . ? C5 H5D 0.9900 . ? C6 H6C 0.9900 . ? C6 H6D 0.9900 . ? C7A C8 1.514(7) . ? C7B C8 1.514(7) . ? C9 C9 1.519(9) 3_675 ? C9 H9C 0.9900 . ? C9 H9D 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 Se4 As1 Se3 113.17(2) . . ? Se4 As1 Se2 109.48(2) . . ? Se3 As1 Se2 108.96(2) . . ? Se4 As1 Se1 108.84(2) . . ? Se3 As1 Se1 106.19(2) . . ? Se2 As1 Se1 110.14(2) . . ? N4 Sm1 N3 67.41(12) . . ? N4 Sm1 N2 137.99(12) . . ? N3 Sm1 N2 71.61(11) . . ? N4 Sm1 N1 154.52(12) . . ? N3 Sm1 N1 137.09(11) . . ? N2 Sm1 N1 67.49(11) . . ? N4 Sm1 N6 94.08(13) . . ? N3 Sm1 N6 77.92(12) . . ? N2 Sm1 N6 85.99(12) . . ? N1 Sm1 N6 86.77(13) . . ? N4 Sm1 N5 78.38(12) . . ? N3 Sm1 N5 128.89(12) . . ? N2 Sm1 N5 137.91(12) . . ? N1 Sm1 N5 78.44(12) . . ? N6 Sm1 N5 67.60(12) . . ? N4 Sm1 N8 81.60(12) . . ? N3 Sm1 N8 133.68(11) . . ? N2 Sm1 N8 123.13(12) . . ? N1 Sm1 N8 81.53(12) . . ? N6 Sm1 N8 140.06(11) . . ? N5 Sm1 N8 72.66(12) . . ? N4 Sm1 N7 89.54(14) . . ? N3 Sm1 N7 79.31(12) . . ? N2 Sm1 N7 74.04(12) . . ? N1 Sm1 N7 100.98(13) . . ? N6 Sm1 N7 153.50(11) . . ? N5 Sm1 N7 138.63(12) . . ? N8 Sm1 N7 66.44(11) . . ? C1 N1 Sm1 114.4(3) . . ? C1 N1 H1A 108.6 . . ? Sm1 N1 H1A 108.6 . . ? C1 N1 H1B 108.6 . . ? Sm1 N1 H1B 108.6 . . ? H1A N1 H1B 107.6 . . ? C2 N2 Sm1 112.6(2) . . ? C2 N2 H2A 109.1 . . ? Sm1 N2 H2A 109.1 . . ? C2 N2 H2B 109.1 . . ? Sm1 N2 H2B 109.1 . . ? H2A N2 H2B 107.8 . . ? C3 N3 Sm1 115.9(3) . . ? C3 N3 H3A 108.3 . . ? Sm1 N3 H3A 108.3 . . ? C3 N3 H3B 108.3 . . ? Sm1 N3 H3B 108.3 . . ? H3A N3 H3B 107.4 . . ? C4 N4 Sm1 110.5(3) . . ? C4 N4 H4A 109.5 . . ? Sm1 N4 H4A 109.5 . . ? C4 N4 H4B 109.5 . . ? Sm1 N4 H4B 109.5 . . ? H4A N4 H4B 108.1 . . ? C5 N5 Sm1 113.9(3) . . ? C5 N5 H5A 108.8 . . ? Sm1 N5 H5A 108.8 . . ? C5 N5 H5B 108.8 . . ? Sm1 N5 H5B 108.8 . . ? H5A N5 H5B 107.7 . . ? C6 N6 Sm1 112.6(3) . . ? C6 N6 H6A 109.1 . . ? Sm1 N6 H6A 109.1 . . ? C6 N6 H6B 109.1 . . ? Sm1 N6 H6B 109.1 . . ? H6A N6 H6B 107.8 . . ? C7A N7 C7B 52.6(5) . . ? C7A N7 Sm1 111.6(4) . . ? C7B N7 Sm1 110.1(4) . . ? C8 N8 Sm1 116.8(3) . . ? C8 N8 H8A 108.1 . . ? Sm1 N8 H8A 108.1 . . ? C8 N8 H8B 108.1 . . ? Sm1 N8 H8B 108.1 . . ? H8A N8 H8B 107.3 . . ? H9A N9 C9 106.4 . . ? H9A N9 H9B 107.6 . . ? C9 N9 H9B 110.5 . . ? H9A N9 H9A 0.0 . . ? C9 N9 H9A 106.4 . . ? H9B N9 H9A 107.6 . . ? N1 C1 C2 109.0(4) . . ? N1 C1 H1C 109.9 . . ? C2 C1 H1C 109.9 . . ? N1 C1 H1D 109.9 . . ? C2 C1 H1D 109.9 . . ? H1C C1 H1D 108.3 . . ? N2 C2 C1 108.7(4) . . ? 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 . . ? N3 C3 C4 109.5(3) . . ? 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 108.5(4) . . ? N4 C4 H4C 110.0 . . ? C3 C4 H4C 110.0 . . ? N4 C4 H4D 110.0 . . ? C3 C4 H4D 110.0 . . ? H4C C4 H4D 108.4 . . ? N5 C5 C6 110.8(4) . . ? N5 C5 H5C 109.5 . . ? C6 C5 H5C 109.5 . . ? N5 C5 H5D 109.5 . . ? C6 C5 H5D 109.5 . . ? H5C C5 H5D 108.1 . . ? N6 C6 C5 109.5(4) . . ? 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 . . ? N7 C7A C8 108.8(5) . . ? N7 C7B C8 108.8(5) . . ? N8 C8 C7A 111.0(5) . . ? N8 C8 C7B 111.3(5) . . ? C7A C8 C7B 51.6(5) . . ? N9 C9 C9 110.0(5) . 3_675 ? N9 C9 H9C 109.7 . . ? C9 C9 H9C 109.7 3_675 . ? N9 C9 H9D 109.7 . . ? C9 C9 H9D 109.7 3_675 . ? H9C C9 H9D 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 N4 Sm1 N1 C1 168.4(3) . . . . ? N3 Sm1 N1 C1 7.3(4) . . . . ? N2 Sm1 N1 C1 -11.3(3) . . . . ? N6 Sm1 N1 C1 75.7(3) . . . . ? N5 Sm1 N1 C1 143.5(3) . . . . ? N8 Sm1 N1 C1 -142.6(3) . . . . ? N7 Sm1 N1 C1 -78.8(3) . . . . ? N4 Sm1 N2 C2 160.1(3) . . . . ? N3 Sm1 N2 C2 173.2(3) . . . . ? N1 Sm1 N2 C2 -20.1(3) . . . . ? N6 Sm1 N2 C2 -108.2(3) . . . . ? N5 Sm1 N2 C2 -58.6(3) . . . . ? N8 Sm1 N2 C2 42.5(3) . . . . ? N7 Sm1 N2 C2 89.4(3) . . . . ? N4 Sm1 N3 C3 -1.3(3) . . . . ? N2 Sm1 N3 C3 -171.9(3) . . . . ? N1 Sm1 N3 C3 170.0(3) . . . . ? N6 Sm1 N3 C3 98.3(3) . . . . ? N5 Sm1 N3 C3 50.7(3) . . . . ? N8 Sm1 N3 C3 -53.3(3) . . . . ? N7 Sm1 N3 C3 -95.3(3) . . . . ? N3 Sm1 N4 C4 -28.4(3) . . . . ? N2 Sm1 N4 C4 -14.9(4) . . . . ? N1 Sm1 N4 C4 165.5(3) . . . . ? N6 Sm1 N4 C4 -103.5(3) . . . . ? N5 Sm1 N4 C4 -169.6(3) . . . . ? N8 Sm1 N4 C4 116.5(3) . . . . ? N7 Sm1 N4 C4 50.2(3) . . . . ? N4 Sm1 N5 C5 89.0(3) . . . . ? N3 Sm1 N5 C5 41.0(4) . . . . ? N2 Sm1 N5 C5 -65.7(4) . . . . ? N1 Sm1 N5 C5 -101.7(3) . . . . ? N6 Sm1 N5 C5 -10.4(3) . . . . ? N8 Sm1 N5 C5 173.7(3) . . . . ? N7 Sm1 N5 C5 164.8(3) . . . . ? N4 Sm1 N6 C6 -95.0(3) . . . . ? N3 Sm1 N6 C6 -160.9(3) . . . . ? N2 Sm1 N6 C6 127.1(3) . . . . ? N1 Sm1 N6 C6 59.5(3) . . . . ? N5 Sm1 N6 C6 -19.4(3) . . . . ? N8 Sm1 N6 C6 -13.2(4) . . . . ? N7 Sm1 N6 C6 167.8(3) . . . . ? N4 Sm1 N7 C7A 54.5(4) . . . . ? N3 Sm1 N7 C7A 121.6(4) . . . . ? N2 Sm1 N7 C7A -164.7(4) . . . . ? N1 Sm1 N7 C7A -102.1(4) . . . . ? N6 Sm1 N7 C7A 152.8(4) . . . . ? N5 Sm1 N7 C7A -17.2(5) . . . . ? N8 Sm1 N7 C7A -26.5(4) . . . . ? N4 Sm1 N7 C7B 111.1(4) . . . . ? N3 Sm1 N7 C7B 178.2(4) . . . . ? N2 Sm1 N7 C7B -108.1(4) . . . . ? N1 Sm1 N7 C7B -45.5(4) . . . . ? N6 Sm1 N7 C7B -150.7(4) . . . . ? N5 Sm1 N7 C7B 39.4(5) . . . . ? N8 Sm1 N7 C7B 30.1(4) . . . . ? N4 Sm1 N8 C8 -95.4(3) . . . . ? N3 Sm1 N8 C8 -48.0(4) . . . . ? N2 Sm1 N8 C8 47.8(4) . . . . ? N1 Sm1 N8 C8 103.8(3) . . . . ? N6 Sm1 N8 C8 178.3(3) . . . . ? N5 Sm1 N8 C8 -175.7(3) . . . . ? N7 Sm1 N8 C8 -2.2(3) . . . . ? Sm1 N1 C1 C2 40.6(4) . . . . ? Sm1 N2 C2 C1 48.9(4) . . . . ? N1 C1 C2 N2 -59.0(5) . . . . ? Sm1 N3 C3 C4 30.1(4) . . . . ? Sm1 N4 C4 C3 55.6(4) . . . . ? N3 C3 C4 N4 -56.4(5) . . . . ? Sm1 N5 C5 C6 39.2(5) . . . . ? Sm1 N6 C6 C5 47.2(5) . . . . ? N5 C5 C6 N6 -57.4(5) . . . . ? C7B N7 C7A C8 -47.1(6) . . . . ? Sm1 N7 C7A C8 52.3(7) . . . . ? C7A N7 C7B C8 47.1(6) . . . . ? Sm1 N7 C7B C8 -55.3(6) . . . . ? Sm1 N8 C8 C7A 30.0(6) . . . . ? Sm1 N8 C8 C7B -25.6(6) . . . . ? N7 C7A C8 N8 -54.2(7) . . . . ? N7 C7A C8 C7B 46.9(6) . . . . ? N7 C7B C8 N8 53.7(7) . . . . ? N7 C7B C8 C7A -46.8(6) . . . . ? H9A N9 C9 C9 79.2 . . . 3_675 ? 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 Se4 0.92 2.60 3.498(4) 167.2 2_645 N2 H2A Se1 0.92 2.65 3.536(4) 161.6 . N2 H2B Se1 0.92 2.77 3.570(4) 145.4 3_666 N3 H3A Se2 0.92 2.60 3.403(4) 145.8 3_666 N3 H3B Se1 0.92 2.99 3.819(4) 150.3 . N4 H4A Se1 0.92 2.82 3.668(4) 154.6 2_545 N4 H4B Se3 0.92 2.51 3.415(4) 167.7 1_545 N5 H5A Se2 0.92 2.67 3.585(4) 172.3 2_645 N5 H5B N9 0.92 2.21 3.068(5) 155.5 1_545 N6 H6A Se3 0.92 2.84 3.751(4) 172.3 2_545 N6 H6B Se1 0.92 2.96 3.715(4) 140.0 . N8 H8A Se3 0.92 2.97 3.776(4) 147.1 1_545 N8 H8B Se4 0.92 2.76 3.541(4) 143.4 2_645 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.112 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.129 #===END data_complex_1e _database_code_depnum_ccdc_archive 'CCDC 767673' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H36 As Gd N9 Se4' _chemical_formula_sum 'C9 H36 As Gd N9 Se4' _chemical_formula_weight 818.48 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' Gd Gd -0.1653 3.9035 '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' As As 0.0499 2.0058 '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 11.2363(4) _cell_length_b 12.9565(4) _cell_length_c 16.2341(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.235(2) _cell_angle_gamma 90.00 _cell_volume 2361.61(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7653 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.35 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 10.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1468 _exptl_absorpt_correction_T_max 0.2192 _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 9904 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4307 _reflns_number_gt 3931 _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^)+(0.0223P)^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 SHELXL _refine_ls_extinction_coef 0.00066(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4307 _refine_ls_number_parameters 222 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.002 _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 As1 As 0.50114(4) 0.72510(4) 0.80976(3) 0.01780(12) Uani 1 1 d . . . Se1 Se 0.40984(5) 0.88406(4) 0.79783(3) 0.03239(14) Uani 1 1 d . . . Se2 Se 0.36446(5) 0.61578(4) 0.86861(3) 0.02331(12) Uani 1 1 d . . . Se3 Se 0.66938(5) 0.74046(4) 0.89540(3) 0.02817(13) Uani 1 1 d . . . Se4 Se 0.55304(5) 0.65766(4) 0.68523(3) 0.02721(13) Uani 1 1 d . . . Gd1 Gd 0.51850(2) 0.266510(17) 0.825323(13) 0.01639(8) Uani 1 1 d . . . N1 N 0.5334(4) 0.2122(3) 0.6746(2) 0.0271(10) Uani 1 1 d . . . H1A H 0.6111 0.2144 0.6609 0.032 Uiso 1 1 calc R . . H1B H 0.5079 0.1459 0.6690 0.032 Uiso 1 1 calc R . . N2 N 0.4250(4) 0.3978(3) 0.7270(2) 0.0270(10) Uani 1 1 d . . . H2A H 0.3443 0.3916 0.7275 0.032 Uiso 1 1 calc R . . H2B H 0.4444 0.4623 0.7452 0.032 Uiso 1 1 calc R . . N3 N 0.3382(3) 0.3236(3) 0.9010(2) 0.0227(9) Uani 1 1 d . . . H3A H 0.3596 0.3295 0.9555 0.027 Uiso 1 1 calc R . . H3B H 0.3171 0.3876 0.8826 0.027 Uiso 1 1 calc R . . N4 N 0.3482(4) 0.1421(3) 0.8081(2) 0.0294(10) Uani 1 1 d . . . H4A H 0.3041 0.1580 0.7617 0.035 Uiso 1 1 calc R . . H4B H 0.3769 0.0770 0.8025 0.035 Uiso 1 1 calc R . . N5 N 0.5679(4) 0.1929(3) 0.9708(2) 0.0325(11) Uani 1 1 d D . . N6 N 0.6376(4) 0.0986(3) 0.8240(2) 0.0260(10) Uani 1 1 d . . . H6A H 0.5933 0.0508 0.7955 0.031 Uiso 1 1 calc R . . H6B H 0.7043 0.1101 0.7953 0.031 Uiso 1 1 calc R . . N7 N 0.7186(4) 0.3399(3) 0.7897(2) 0.0271(10) Uani 1 1 d . . . H7A H 0.7764 0.2942 0.8058 0.033 Uiso 1 1 calc R . . H7B H 0.7206 0.3465 0.7339 0.033 Uiso 1 1 calc R . . N8 N 0.5774(3) 0.4200(3) 0.9145(2) 0.0208(9) Uani 1 1 d . . . H8A H 0.5370 0.4768 0.8957 0.025 Uiso 1 1 calc R . . H8B H 0.5559 0.4079 0.9671 0.025 Uiso 1 1 calc R . . N9 N 0.9311(4) 0.4911(3) 0.1027(2) 0.0311(10) Uani 1 1 d D . . H9A H 0.9319 0.5443 0.1387 0.037 Uiso 1 1 d RD . . H9B H 0.8590 0.4612 0.0918 0.037 Uiso 1 1 d RD . . C1 C 0.4623(6) 0.2788(4) 0.6165(3) 0.0465(17) Uani 1 1 d . . . H1C H 0.4941 0.2728 0.5614 0.056 Uiso 1 1 calc R . . H1D H 0.3798 0.2541 0.6134 0.056 Uiso 1 1 calc R . . C2 C 0.4635(6) 0.3858(4) 0.6409(3) 0.0486(17) Uani 1 1 d . . . H2C H 0.4102 0.4253 0.6036 0.058 Uiso 1 1 calc R . . H2D H 0.5442 0.4136 0.6366 0.058 Uiso 1 1 calc R . . C3 C 0.2311(5) 0.2558(3) 0.8935(3) 0.0262(11) Uani 1 1 d . . . H3C H 0.1796 0.2779 0.8467 0.031 Uiso 1 1 calc R . . H3D H 0.1857 0.2602 0.9437 0.031 Uiso 1 1 calc R . . C4 C 0.2718(5) 0.1468(4) 0.8807(3) 0.0287(12) Uani 1 1 d . . . H4C H 0.3168 0.1226 0.9299 0.034 Uiso 1 1 calc R . . H4D H 0.2026 0.1016 0.8717 0.034 Uiso 1 1 calc R . . C5A C 0.6848(8) 0.1345(6) 0.9695(5) 0.0292(17) Uani 0.50 1 d PD . . C5B C 0.5870(9) 0.0779(6) 0.9685(5) 0.0292(17) Uani 0.50 1 d PD . . C6 C 0.6748(5) 0.0530(4) 0.9044(3) 0.0395(15) Uani 1 1 d D . . C7 C 0.7467(5) 0.4414(4) 0.8278(3) 0.0290(12) Uani 1 1 d . . . H7C H 0.7060 0.4964 0.7964 0.035 Uiso 1 1 calc R . . H7D H 0.8327 0.4541 0.8274 0.035 Uiso 1 1 calc R . . C8 C 0.7066(4) 0.4411(4) 0.9145(3) 0.0266(12) Uani 1 1 d . . . H8C H 0.7500 0.3880 0.9465 0.032 Uiso 1 1 calc R . . H8D H 0.7236 0.5082 0.9402 0.032 Uiso 1 1 calc R . . C9 C 0.9732(4) 0.5394(3) 0.0278(3) 0.0244(11) Uani 1 1 d . . . H9C H 1.0330 0.5919 0.0427 0.029 Uiso 1 1 calc R . . H9D H 0.9064 0.5738 -0.0016 0.029 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 As1 0.0145(3) 0.0209(2) 0.0180(2) 0.0014(2) 0.00063(18) 0.0002(2) Se1 0.0398(4) 0.0209(3) 0.0358(3) 0.0015(2) -0.0065(2) 0.0053(2) Se2 0.0184(3) 0.0246(3) 0.0272(3) 0.0021(2) 0.0043(2) -0.0021(2) Se3 0.0169(3) 0.0477(3) 0.0197(2) 0.0024(2) -0.0018(2) -0.0028(2) Se4 0.0169(3) 0.0422(3) 0.0227(2) -0.0067(2) 0.0019(2) 0.0006(2) Gd1 0.01323(13) 0.01847(13) 0.01749(12) -0.00277(9) 0.00093(9) 0.00051(9) N1 0.028(3) 0.027(2) 0.026(2) -0.0042(18) 0.0035(18) -0.0010(19) N2 0.031(3) 0.023(2) 0.027(2) -0.0053(18) 0.0028(19) 0.0047(19) N3 0.021(2) 0.023(2) 0.025(2) -0.0008(17) -0.0005(17) 0.0018(18) N4 0.024(3) 0.024(2) 0.040(2) -0.0103(19) -0.001(2) 0.0006(19) N5 0.049(3) 0.028(2) 0.020(2) 0.0022(18) 0.001(2) 0.023(2) N6 0.023(3) 0.027(2) 0.028(2) -0.0090(19) 0.0035(18) 0.0019(19) N7 0.022(3) 0.037(2) 0.023(2) -0.0058(19) 0.0014(17) 0.001(2) N8 0.020(2) 0.024(2) 0.0186(19) -0.0014(17) 0.0016(16) 0.0003(18) N9 0.025(3) 0.035(2) 0.033(2) -0.001(2) 0.0065(19) 0.002(2) C1 0.071(5) 0.046(4) 0.022(3) 0.002(3) -0.004(3) 0.015(3) C2 0.079(5) 0.043(3) 0.024(3) 0.001(3) 0.005(3) 0.017(3) C3 0.020(3) 0.031(3) 0.028(3) 0.000(2) -0.002(2) 0.000(2) C4 0.021(3) 0.026(3) 0.038(3) 0.005(2) -0.006(2) -0.010(2) C5A 0.031(5) 0.032(4) 0.024(3) 0.011(3) 0.001(3) 0.006(3) C5B 0.031(5) 0.032(4) 0.024(3) 0.011(3) 0.001(3) 0.006(3) C6 0.055(4) 0.031(3) 0.032(3) 0.006(2) 0.007(3) 0.019(3) C7 0.022(3) 0.031(3) 0.035(3) 0.004(2) 0.001(2) -0.002(2) C8 0.023(3) 0.026(3) 0.031(3) -0.003(2) -0.003(2) -0.006(2) C9 0.017(3) 0.024(2) 0.032(3) 0.001(2) 0.002(2) 0.003(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 As1 Se4 2.2983(6) . ? As1 Se1 2.3056(7) . ? As1 Se3 2.3110(7) . ? As1 Se2 2.3221(7) . ? Gd1 N4 2.509(4) . ? Gd1 N3 2.521(4) . ? Gd1 N7 2.529(4) . ? Gd1 N2 2.532(4) . ? Gd1 N8 2.533(3) . ? Gd1 N6 2.555(4) . ? Gd1 N1 2.557(4) . ? Gd1 N5 2.587(4) . ? N1 C1 1.488(6) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.488(6) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 C3 1.491(6) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C4 1.485(6) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N5 C5B 1.507(7) . ? N5 C5A 1.516(7) . ? N6 C6 1.479(6) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N7 C7 1.482(6) . ? N7 H7A 0.9100 . ? N7 H7B 0.9100 . ? N8 C8 1.478(6) . ? N8 H8A 0.9100 . ? N8 H8B 0.9100 . ? N9 C9 1.462(5) . ? N9 H9A 0.9046 . ? N9 H9B 0.9077 . ? C1 C2 1.442(7) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.501(6) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C5A C6 1.494(7) . ? C5B C6 1.496(7) . ? C7 C8 1.494(6) . ? C7 H7C 0.9800 . ? C7 H7D 0.9800 . ? C8 H8C 0.9800 . ? C8 H8D 0.9800 . ? C9 C9 1.504(8) 3_765 ? C9 H9C 0.9800 . ? C9 H9D 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 Se4 As1 Se1 113.14(3) . . ? Se4 As1 Se3 109.40(3) . . ? Se1 As1 Se3 108.93(3) . . ? Se4 As1 Se2 108.94(3) . . ? Se1 As1 Se2 106.27(3) . . ? Se3 As1 Se2 110.10(2) . . ? N4 Gd1 N3 67.59(12) . . ? N4 Gd1 N7 153.78(12) . . ? N3 Gd1 N7 137.70(12) . . ? N4 Gd1 N2 93.75(13) . . ? N3 Gd1 N2 77.80(12) . . ? N7 Gd1 N2 87.36(13) . . ? N4 Gd1 N8 138.52(12) . . ? N3 Gd1 N8 71.82(12) . . ? N7 Gd1 N8 67.70(12) . . ? N2 Gd1 N8 85.70(12) . . ? N4 Gd1 N6 81.35(13) . . ? N3 Gd1 N6 133.25(12) . . ? N7 Gd1 N6 81.23(13) . . ? N2 Gd1 N6 140.47(11) . . ? N8 Gd1 N6 123.26(12) . . ? N4 Gd1 N1 78.18(13) . . ? N3 Gd1 N1 129.12(13) . . ? N7 Gd1 N1 78.03(12) . . ? N2 Gd1 N1 67.85(12) . . ? N8 Gd1 N1 137.49(12) . . ? N6 Gd1 N1 72.78(12) . . ? N4 Gd1 N5 90.03(14) . . ? N3 Gd1 N5 79.10(13) . . ? N7 Gd1 N5 100.74(14) . . ? N2 Gd1 N5 153.10(12) . . ? N8 Gd1 N5 74.09(12) . . ? N6 Gd1 N5 66.43(12) . . ? N1 Gd1 N5 138.79(12) . . ? C1 N1 Gd1 113.2(3) . . ? C1 N1 H1A 108.9 . . ? Gd1 N1 H1A 108.9 . . ? C1 N1 H1B 108.9 . . ? Gd1 N1 H1B 108.9 . . ? H1A N1 H1B 107.8 . . ? C2 N2 Gd1 113.1(3) . . ? C2 N2 H2A 109.0 . . ? Gd1 N2 H2A 109.0 . . ? C2 N2 H2B 109.0 . . ? Gd1 N2 H2B 109.0 . . ? H2A N2 H2B 107.8 . . ? C3 N3 Gd1 116.6(3) . . ? C3 N3 H3A 108.1 . . ? Gd1 N3 H3A 108.1 . . ? C3 N3 H3B 108.1 . . ? Gd1 N3 H3B 108.1 . . ? H3A N3 H3B 107.3 . . ? C4 N4 Gd1 110.3(3) . . ? C4 N4 H4A 109.6 . . ? Gd1 N4 H4A 109.6 . . ? C4 N4 H4B 109.6 . . ? Gd1 N4 H4B 109.6 . . ? H4A N4 H4B 108.1 . . ? C5B N5 C5A 51.8(5) . . ? C5B N5 Gd1 111.6(4) . . ? C5A N5 Gd1 109.0(4) . . ? C6 N6 Gd1 117.6(3) . . ? C6 N6 H6A 107.9 . . ? Gd1 N6 H6A 107.9 . . ? C6 N6 H6B 107.9 . . ? Gd1 N6 H6B 107.9 . . ? H6A N6 H6B 107.2 . . ? C7 N7 Gd1 114.5(3) . . ? C7 N7 H7A 108.6 . . ? Gd1 N7 H7A 108.6 . . ? C7 N7 H7B 108.6 . . ? Gd1 N7 H7B 108.6 . . ? H7A N7 H7B 107.6 . . ? C8 N8 Gd1 112.3(3) . . ? C8 N8 H8A 109.1 . . ? Gd1 N8 H8A 109.1 . . ? C8 N8 H8B 109.1 . . ? Gd1 N8 H8B 109.1 . . ? H8A N8 H8B 107.9 . . ? C9 N9 H9A 102.4 . . ? C9 N9 H9B 109.7 . . ? H9A N9 H9B 115.9 . . ? C2 C1 N1 112.6(5) . . ? C2 C1 H1C 109.1 . . ? N1 C1 H1C 109.1 . . ? C2 C1 H1D 109.1 . . ? N1 C1 H1D 109.1 . . ? H1C C1 H1D 107.8 . . ? C1 C2 N2 111.0(5) . . ? C1 C2 H2C 109.4 . . ? N2 C2 H2C 109.4 . . ? C1 C2 H2D 109.4 . . ? N2 C2 H2D 109.4 . . ? H2C C2 H2D 108.0 . . ? N3 C3 C4 108.5(4) . . ? N3 C3 H3C 110.0 . . ? C4 C3 H3C 110.0 . . ? N3 C3 H3D 110.0 . . ? C4 C3 H3D 110.0 . . ? H3C C3 H3D 108.4 . . ? N4 C4 C3 109.7(4) . . ? 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 . . ? C6 C5A N5 108.8(6) . . ? C6 C5B N5 109.2(6) . . ? N6 C6 C5A 110.7(5) . . ? N6 C6 C5B 110.9(5) . . ? C5A C6 C5B 52.4(5) . . ? N7 C7 C8 108.9(4) . . ? N7 C7 H7C 109.9 . . ? C8 C7 H7C 109.9 . . ? N7 C7 H7D 109.9 . . ? C8 C7 H7D 109.9 . . ? H7C C7 H7D 108.3 . . ? N8 C8 C7 109.4(4) . . ? N8 C8 H8C 109.8 . . ? C7 C8 H8C 109.8 . . ? N8 C8 H8D 109.8 . . ? C7 C8 H8D 109.8 . . ? H8C C8 H8D 108.2 . . ? N9 C9 C9 111.0(5) . 3_765 ? N9 C9 H9C 109.4 . . ? C9 C9 H9C 109.4 3_765 . ? N9 C9 H9D 109.4 . . ? C9 C9 H9D 109.4 3_765 . ? H9C C9 H9D 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 N4 Gd1 N1 C1 89.6(4) . . . . ? N3 Gd1 N1 C1 41.9(4) . . . . ? N7 Gd1 N1 C1 -101.5(4) . . . . ? N2 Gd1 N1 C1 -9.4(4) . . . . ? N8 Gd1 N1 C1 -65.1(4) . . . . ? N6 Gd1 N1 C1 174.1(4) . . . . ? N5 Gd1 N1 C1 165.8(4) . . . . ? N4 Gd1 N2 C2 -93.2(4) . . . . ? N3 Gd1 N2 C2 -159.3(4) . . . . ? N7 Gd1 N2 C2 60.5(4) . . . . ? N8 Gd1 N2 C2 128.4(4) . . . . ? N6 Gd1 N2 C2 -12.3(4) . . . . ? N1 Gd1 N2 C2 -17.6(3) . . . . ? N5 Gd1 N2 C2 169.3(4) . . . . ? N4 Gd1 N3 C3 -1.1(3) . . . . ? N7 Gd1 N3 C3 170.3(3) . . . . ? N2 Gd1 N3 C3 98.2(3) . . . . ? N8 Gd1 N3 C3 -172.3(3) . . . . ? N6 Gd1 N3 C3 -53.4(4) . . . . ? N1 Gd1 N3 C3 50.5(3) . . . . ? N5 Gd1 N3 C3 -95.7(3) . . . . ? N3 Gd1 N4 C4 -27.9(3) . . . . ? N7 Gd1 N4 C4 165.3(3) . . . . ? N2 Gd1 N4 C4 -103.0(3) . . . . ? N8 Gd1 N4 C4 -15.3(4) . . . . ? N6 Gd1 N4 C4 116.4(3) . . . . ? N1 Gd1 N4 C4 -169.5(3) . . . . ? N5 Gd1 N4 C4 50.3(3) . . . . ? N4 Gd1 N5 C5B 55.2(5) . . . . ? N3 Gd1 N5 C5B 122.4(5) . . . . ? N7 Gd1 N5 C5B -100.7(5) . . . . ? N2 Gd1 N5 C5B 153.6(5) . . . . ? N8 Gd1 N5 C5B -163.6(5) . . . . ? N6 Gd1 N5 C5B -25.3(4) . . . . ? N1 Gd1 N5 C5B -16.7(5) . . . . ? N4 Gd1 N5 C5A 110.7(4) . . . . ? N3 Gd1 N5 C5A 177.9(4) . . . . ? N7 Gd1 N5 C5A -45.2(4) . . . . ? N2 Gd1 N5 C5A -150.9(4) . . . . ? N8 Gd1 N5 C5A -108.1(4) . . . . ? N6 Gd1 N5 C5A 30.2(4) . . . . ? N1 Gd1 N5 C5A 38.8(5) . . . . ? N4 Gd1 N6 C6 -96.5(4) . . . . ? N3 Gd1 N6 C6 -48.8(4) . . . . ? N7 Gd1 N6 C6 103.2(4) . . . . ? N2 Gd1 N6 C6 178.1(3) . . . . ? N8 Gd1 N6 C6 47.2(4) . . . . ? N1 Gd1 N6 C6 -176.7(4) . . . . ? N5 Gd1 N6 C6 -2.7(4) . . . . ? N4 Gd1 N7 C7 168.0(3) . . . . ? N3 Gd1 N7 C7 6.3(4) . . . . ? N2 Gd1 N7 C7 74.9(3) . . . . ? N8 Gd1 N7 C7 -11.5(3) . . . . ? N6 Gd1 N7 C7 -143.1(3) . . . . ? N1 Gd1 N7 C7 142.8(3) . . . . ? N5 Gd1 N7 C7 -79.3(3) . . . . ? N4 Gd1 N8 C8 161.0(3) . . . . ? N3 Gd1 N8 C8 173.2(3) . . . . ? N7 Gd1 N8 C8 -19.3(3) . . . . ? N2 Gd1 N8 C8 -108.2(3) . . . . ? N6 Gd1 N8 C8 42.9(3) . . . . ? N1 Gd1 N8 C8 -58.1(4) . . . . ? N5 Gd1 N8 C8 89.7(3) . . . . ? Gd1 N1 C1 C2 37.0(6) . . . . ? N1 C1 C2 N2 -54.2(7) . . . . ? Gd1 N2 C2 C1 44.3(6) . . . . ? Gd1 N3 C3 C4 29.2(4) . . . . ? Gd1 N4 C4 C3 55.4(4) . . . . ? N3 C3 C4 N4 -55.4(5) . . . . ? C5B N5 C5A C6 46.7(6) . . . . ? Gd1 N5 C5A C6 -56.2(7) . . . . ? C5A N5 C5B C6 -46.7(6) . . . . ? Gd1 N5 C5B C6 51.1(7) . . . . ? Gd1 N6 C6 C5A -25.9(6) . . . . ? Gd1 N6 C6 C5B 30.5(6) . . . . ? N5 C5A C6 N6 54.4(8) . . . . ? N5 C5A C6 C5B -46.6(6) . . . . ? N5 C5B C6 N6 -53.4(8) . . . . ? N5 C5B C6 C5A 47.1(6) . . . . ? Gd1 N7 C7 C8 40.5(5) . . . . ? Gd1 N8 C8 C7 48.2(4) . . . . ? N7 C7 C8 N8 -58.6(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 Se3 0.91 2.69 3.588(4) 171.9 2_646 N1 H1B N9 0.91 2.23 3.085(5) 156.1 4_566 N2 H2A Se1 0.91 2.87 3.772(4) 170.8 2_546 N2 H2B Se2 0.91 2.99 3.721(4) 138.9 . N2 H2B Se4 0.91 2.99 3.734(4) 140.2 . N3 H3A Se3 0.91 2.62 3.411(4) 146.2 3_667 N4 H4A Se2 0.91 2.84 3.678(4) 154.2 2_546 N4 H4B Se1 0.91 2.53 3.420(4) 166.8 1_545 N6 H6A Se1 0.91 2.99 3.791(4) 148.2 1_545 N6 H6B Se4 0.91 2.80 3.568(4) 142.7 2_646 N7 H7A Se4 0.91 2.61 3.499(4) 166.5 2_646 N7 H7B Se3 0.91 2.83 3.545(4) 136.1 2_646 N8 H8A Se2 0.91 2.67 3.545(4) 161.7 . N8 H8B Se2 0.91 2.80 3.587(3) 145.8 3_667 N9 H9B Se2 0.91 2.80 3.644(4) 155.2 3_666 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.794 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.114 #===END data_complex_1f _database_code_depnum_ccdc_archive 'CCDC 767674' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H36 As Dy N9 Se4' _chemical_formula_sum 'C9 H36 As Dy N9 Se4' _chemical_formula_weight 823.73 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 11.239(2) _cell_length_b 12.952(3) _cell_length_c 16.241(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.262(4) _cell_angle_gamma 90.00 _cell_volume 2362.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9031 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 10.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1669 _exptl_absorpt_correction_T_max 0.2350 _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 22522 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4322 _reflns_number_gt 4020 _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^)+(0.0499P)^2^+4.5687P] 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 4322 _refine_ls_number_parameters 221 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.210 _refine_ls_restrained_S_all 1.210 _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 As1 As 0.50117(7) 0.27493(5) 0.80976(4) 0.01261(19) Uani 1 1 d . . . Se1 Se 0.66921(8) 0.25950(7) 0.89537(5) 0.0232(2) Uani 1 1 d . . . Se2 Se 0.55299(7) 0.34242(6) 0.68521(5) 0.0222(2) Uani 1 1 d . . . Se3 Se 0.36437(7) 0.38421(6) 0.86851(5) 0.0182(2) Uani 1 1 d . . . Se4 Se 0.40986(9) 0.11598(6) 0.79781(5) 0.0274(2) Uani 1 1 d . . . Dy1 Dy 0.48146(3) 0.26650(3) 0.17469(2) 0.01421(13) Uani 1 1 d . . . N1 N 0.6511(6) 0.1421(5) 0.1913(4) 0.0233(15) Uani 1 1 d . . . H1A H 0.6948 0.1575 0.2380 0.028 Uiso 1 1 calc R . . H1B H 0.6221 0.0770 0.1965 0.028 Uiso 1 1 calc R . . N2 N 0.6621(6) 0.3232(5) 0.0987(4) 0.0175(14) Uani 1 1 d . . . H2A H 0.6410 0.3287 0.0442 0.021 Uiso 1 1 calc R . . H2B H 0.6835 0.3873 0.1168 0.021 Uiso 1 1 calc R . . N3 N 0.2824(6) 0.3399(5) 0.2094(4) 0.0227(15) Uani 1 1 d . . . H3A H 0.2247 0.2943 0.1927 0.027 Uiso 1 1 calc R . . H3B H 0.2798 0.3458 0.2651 0.027 Uiso 1 1 calc R . . N4 N 0.4224(6) 0.4206(5) 0.0856(4) 0.0169(14) Uani 1 1 d . . . H4A H 0.4625 0.4774 0.1045 0.020 Uiso 1 1 calc R . . H4B H 0.4440 0.4087 0.0330 0.020 Uiso 1 1 calc R . . N5 N 0.5754(7) 0.3976(5) 0.2730(4) 0.0230(16) Uani 1 1 d . . . H5A H 0.6559 0.3901 0.2735 0.028 Uiso 1 1 calc R . . H5B H 0.5578 0.4622 0.2541 0.028 Uiso 1 1 calc R . . N6 N 0.4671(7) 0.2129(5) 0.3258(4) 0.0228(16) Uani 1 1 d . . . H6A H 0.3895 0.2151 0.3395 0.027 Uiso 1 1 calc R . . H6B H 0.4924 0.1464 0.3315 0.027 Uiso 1 1 calc R . . N7 N 0.3613(6) 0.0991(5) 0.1762(4) 0.0230(15) Uani 1 1 d . . . H7A H 0.4043 0.0516 0.2061 0.028 Uiso 1 1 calc R . . H7B H 0.2935 0.1114 0.2035 0.028 Uiso 1 1 calc R . . N8 N 0.4314(7) 0.1925(5) 0.0302(4) 0.0292(18) Uani 1 1 d D . . N9 N 0.9310(7) 0.5094(5) 0.1029(4) 0.0277(17) Uani 1 1 d D . . H9A H 0.9342 0.4637 0.1445 0.033 Uiso 1 1 d RD . . H9B H 0.8588 0.5361 0.0893 0.033 Uiso 1 1 d RD . . C1 C 0.7289(7) 0.1467(6) 0.1192(5) 0.0221(18) Uani 1 1 d . . . H1C H 0.7988 0.1024 0.1290 0.026 Uiso 1 1 calc R . . H1D H 0.6851 0.1218 0.0697 0.026 Uiso 1 1 calc R . . C2 C 0.7671(7) 0.2553(6) 0.1071(5) 0.0190(17) Uani 1 1 d . . . H2C H 0.8178 0.2775 0.1543 0.023 Uiso 1 1 calc R . . H2D H 0.8136 0.2602 0.0575 0.023 Uiso 1 1 calc R . . C3 C 0.2545(7) 0.4408(6) 0.1724(5) 0.0222(18) Uani 1 1 d . . . H3C H 0.2958 0.4954 0.2039 0.027 Uiso 1 1 calc R . . H3D H 0.1686 0.4538 0.1734 0.027 Uiso 1 1 calc R . . C4 C 0.2934(7) 0.4413(6) 0.0853(4) 0.0205(17) Uani 1 1 d . . . H4C H 0.2502 0.3882 0.0533 0.025 Uiso 1 1 calc R . . H4D H 0.2762 0.5085 0.0599 0.025 Uiso 1 1 calc R . . C5 C 0.5349(11) 0.3877(7) 0.3580(5) 0.041(3) Uani 1 1 d . . . H5C H 0.5868 0.4284 0.3955 0.050 Uiso 1 1 calc R . . H5D H 0.4537 0.4145 0.3609 0.050 Uiso 1 1 calc R . . C6 C 0.5377(11) 0.2785(7) 0.3836(5) 0.041(3) Uani 1 1 d . . . H6C H 0.5060 0.2724 0.4388 0.049 Uiso 1 1 calc R . . H6D H 0.6203 0.2542 0.3865 0.049 Uiso 1 1 calc R . . C7 C 0.3273(9) 0.0529(7) 0.0967(5) 0.035(2) Uani 1 1 d D . . C8A C 0.3178(11) 0.1340(10) 0.0310(8) 0.029(3) Uani 0.50 1 d PD . . C8B C 0.4137(14) 0.0785(8) 0.0308(9) 0.029(3) Uani 0.50 1 d PD . . C9 C 0.9734(8) 0.4604(6) 0.0280(5) 0.0236(18) Uani 1 1 d . . . H9C H 0.9069 0.4256 -0.0012 0.028 Uiso 1 1 calc R . . H9D H 1.0336 0.4083 0.0431 0.028 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 As1 0.0090(4) 0.0164(4) 0.0123(4) -0.0012(3) -0.0010(3) -0.0004(3) Se1 0.0119(5) 0.0434(5) 0.0140(4) -0.0022(3) -0.0031(3) 0.0034(4) Se2 0.0118(4) 0.0375(5) 0.0171(4) 0.0069(3) 0.0000(3) -0.0004(3) Se3 0.0136(4) 0.0198(4) 0.0212(4) -0.0016(3) 0.0030(3) 0.0023(3) Se4 0.0350(6) 0.0164(4) 0.0301(5) -0.0014(3) -0.0080(4) -0.0056(4) Dy1 0.0111(2) 0.0166(2) 0.0149(2) 0.00298(13) -0.00044(16) -0.00071(14) N1 0.021(4) 0.017(3) 0.032(4) 0.009(3) -0.006(3) 0.000(3) N2 0.016(4) 0.015(3) 0.021(3) -0.005(2) -0.001(3) -0.001(3) N3 0.019(4) 0.029(4) 0.020(3) 0.006(3) 0.001(3) 0.004(3) N4 0.014(4) 0.017(3) 0.020(3) 0.003(3) -0.003(3) 0.000(3) N5 0.033(5) 0.017(3) 0.019(3) 0.006(3) -0.002(3) -0.007(3) N6 0.025(4) 0.022(3) 0.021(3) 0.005(3) 0.001(3) -0.003(3) N7 0.021(4) 0.025(4) 0.023(3) 0.007(3) 0.003(3) -0.002(3) N8 0.045(5) 0.025(4) 0.017(3) 0.000(3) -0.003(3) -0.023(4) N9 0.022(4) 0.036(4) 0.025(4) -0.003(3) 0.001(3) -0.001(3) C1 0.009(4) 0.022(4) 0.034(5) -0.003(3) -0.007(4) 0.005(3) C2 0.010(4) 0.027(4) 0.019(4) 0.000(3) -0.006(3) 0.002(3) C3 0.013(4) 0.026(4) 0.028(4) -0.005(3) -0.002(4) 0.006(3) C4 0.018(5) 0.025(4) 0.018(4) -0.001(3) -0.007(3) 0.006(3) C5 0.059(8) 0.041(6) 0.024(5) -0.007(4) 0.004(5) -0.014(5) C6 0.065(8) 0.037(5) 0.020(4) 0.009(4) -0.001(5) -0.016(5) C7 0.045(7) 0.032(5) 0.030(5) -0.007(4) 0.007(5) -0.016(4) C8A 0.033(8) 0.025(6) 0.029(6) -0.006(5) -0.009(6) -0.008(5) C8B 0.033(8) 0.025(6) 0.029(6) -0.006(5) -0.009(6) -0.008(5) C9 0.016(5) 0.027(4) 0.027(4) 0.003(3) 0.001(4) -0.004(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 As1 Se2 2.2995(11) . ? As1 Se4 2.3052(11) . ? As1 Se1 2.3091(12) . ? As1 Se3 2.3223(11) . ? Dy1 N1 2.502(7) . ? Dy1 N3 2.516(7) . ? Dy1 N2 2.526(6) . ? Dy1 N5 2.532(6) . ? Dy1 N4 2.539(6) . ? Dy1 N7 2.555(6) . ? Dy1 N6 2.562(6) . ? Dy1 N8 2.577(6) . ? N1 C1 1.490(10) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.474(10) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 C3 1.467(10) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C4 1.473(10) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N5 C5 1.477(10) . ? N5 H5A 0.9100 . ? N5 H5B 0.9100 . ? N6 C6 1.474(11) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N7 C7 1.460(11) . ? N7 H7A 0.9100 . ? N7 H7B 0.9100 . ? N8 C8A 1.485(9) . ? N8 C8B 1.489(9) . ? N9 C9 1.468(10) . ? N9 H9A 0.8982 . ? N9 H9B 0.9011 . ? C1 C2 1.487(10) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.497(10) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C5 C6 1.474(12) . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 C8A 1.499(9) . ? C7 C8B 1.511(9) . ? C9 C9 1.509(15) 3_765 ? C9 H9C 0.9800 . ? C9 H9D 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 As1 Se4 113.13(4) . . ? Se2 As1 Se1 109.45(4) . . ? Se4 As1 Se1 108.91(4) . . ? Se2 As1 Se3 108.93(4) . . ? Se4 As1 Se3 106.21(4) . . ? Se1 As1 Se3 110.14(4) . . ? N1 Dy1 N3 154.1(2) . . ? N1 Dy1 N2 67.4(2) . . ? N3 Dy1 N2 137.6(2) . . ? N1 Dy1 N5 93.8(2) . . ? N3 Dy1 N5 87.6(2) . . ? N2 Dy1 N5 77.9(2) . . ? N1 Dy1 N4 138.5(2) . . ? N3 Dy1 N4 67.4(2) . . ? N2 Dy1 N4 71.9(2) . . ? N5 Dy1 N4 85.7(2) . . ? N1 Dy1 N7 81.6(2) . . ? N3 Dy1 N7 81.0(2) . . ? N2 Dy1 N7 133.4(2) . . ? N5 Dy1 N7 140.4(2) . . ? N4 Dy1 N7 123.1(2) . . ? N1 Dy1 N6 78.4(2) . . ? N3 Dy1 N6 78.3(2) . . ? N2 Dy1 N6 129.0(2) . . ? N5 Dy1 N6 67.6(2) . . ? N4 Dy1 N6 137.3(2) . . ? N7 Dy1 N6 73.0(2) . . ? N1 Dy1 N8 89.8(2) . . ? N3 Dy1 N8 100.4(2) . . ? N2 Dy1 N8 79.3(2) . . ? N5 Dy1 N8 153.40(19) . . ? N4 Dy1 N8 74.4(2) . . ? N7 Dy1 N8 66.2(2) . . ? N6 Dy1 N8 138.8(2) . . ? C1 N1 Dy1 111.0(4) . . ? C1 N1 H1A 109.4 . . ? Dy1 N1 H1A 109.4 . . ? C1 N1 H1B 109.4 . . ? Dy1 N1 H1B 109.4 . . ? H1A N1 H1B 108.0 . . ? C2 N2 Dy1 115.9(4) . . ? C2 N2 H2A 108.3 . . ? Dy1 N2 H2A 108.3 . . ? C2 N2 H2B 108.3 . . ? Dy1 N2 H2B 108.3 . . ? H2A N2 H2B 107.4 . . ? C3 N3 Dy1 115.0(5) . . ? C3 N3 H3A 108.5 . . ? Dy1 N3 H3A 108.5 . . ? C3 N3 H3B 108.5 . . ? Dy1 N3 H3B 108.5 . . ? H3A N3 H3B 107.5 . . ? C4 N4 Dy1 112.3(4) . . ? C4 N4 H4A 109.1 . . ? Dy1 N4 H4A 109.1 . . ? C4 N4 H4B 109.1 . . ? Dy1 N4 H4B 109.1 . . ? H4A N4 H4B 107.9 . . ? C5 N5 Dy1 113.3(5) . . ? C5 N5 H5A 108.9 . . ? Dy1 N5 H5A 108.9 . . ? C5 N5 H5B 108.9 . . ? Dy1 N5 H5B 108.9 . . ? H5A N5 H5B 107.7 . . ? C6 N6 Dy1 113.7(5) . . ? C6 N6 H6A 108.8 . . ? Dy1 N6 H6A 108.8 . . ? C6 N6 H6B 108.8 . . ? Dy1 N6 H6B 108.8 . . ? H6A N6 H6B 107.7 . . ? C7 N7 Dy1 117.3(5) . . ? C7 N7 H7A 108.0 . . ? Dy1 N7 H7A 108.0 . . ? C7 N7 H7B 108.0 . . ? Dy1 N7 H7B 108.0 . . ? H7A N7 H7B 107.2 . . ? C8A N8 C8B 51.7(9) . . ? C8A N8 Dy1 109.8(7) . . ? C8B N8 Dy1 112.8(7) . . ? C9 N9 H9A 109.5 . . ? C9 N9 H9B 106.4 . . ? H9A N9 H9B 116.5 . . ? C2 C1 N1 108.8(6) . . ? C2 C1 H1C 109.9 . . ? N1 C1 H1C 109.9 . . ? C2 C1 H1D 109.9 . . ? N1 C1 H1D 109.9 . . ? H1C C1 H1D 108.3 . . ? N2 C2 C1 110.0(7) . . ? N2 C2 H2C 109.7 . . ? C1 C2 H2C 109.7 . . ? N2 C2 H2D 109.7 . . ? C1 C2 H2D 109.7 . . ? H2C C2 H2D 108.2 . . ? N3 C3 C4 109.0(6) . . ? N3 C3 H3C 109.9 . . ? C4 C3 H3C 109.9 . . ? N3 C3 H3D 109.9 . . ? C4 C3 H3D 109.9 . . ? H3C C3 H3D 108.3 . . ? N4 C4 C3 108.7(6) . . ? 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 . . ? C6 C5 N5 110.1(7) . . ? C6 C5 H5C 109.6 . . ? N5 C5 H5C 109.6 . . ? C6 C5 H5D 109.6 . . ? N5 C5 H5D 109.6 . . ? H5C C5 H5D 108.2 . . ? C5 C6 N6 111.6(8) . . ? C5 C6 H6C 109.3 . . ? N6 C6 H6C 109.3 . . ? C5 C6 H6D 109.3 . . ? N6 C6 H6D 109.3 . . ? H6C C6 H6D 108.0 . . ? N7 C7 C8A 110.5(8) . . ? N7 C7 C8B 112.6(9) . . ? C8A C7 C8B 51.0(9) . . ? N8 C8A C7 109.1(8) . . ? N8 C8B C7 108.2(8) . . ? N9 C9 C9 110.8(8) . 3_765 ? N9 C9 H9C 109.5 . . ? C9 C9 H9C 109.5 3_765 . ? N9 C9 H9D 109.5 . . ? C9 C9 H9D 109.5 3_765 . ? H9C C9 H9D 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 N3 Dy1 N1 C1 165.1(5) . . . . ? N2 Dy1 N1 C1 -27.3(5) . . . . ? N5 Dy1 N1 C1 -102.5(5) . . . . ? N4 Dy1 N1 C1 -14.7(7) . . . . ? N7 Dy1 N1 C1 117.1(5) . . . . ? N6 Dy1 N1 C1 -168.7(5) . . . . ? N8 Dy1 N1 C1 51.1(5) . . . . ? N1 Dy1 N2 C2 -1.5(5) . . . . ? N3 Dy1 N2 C2 170.5(5) . . . . ? N5 Dy1 N2 C2 97.9(5) . . . . ? N4 Dy1 N2 C2 -172.7(5) . . . . ? N7 Dy1 N2 C2 -53.8(6) . . . . ? N6 Dy1 N2 C2 50.4(6) . . . . ? N8 Dy1 N2 C2 -95.8(5) . . . . ? N1 Dy1 N3 C3 168.1(5) . . . . ? N2 Dy1 N3 C3 5.3(7) . . . . ? N5 Dy1 N3 C3 74.4(5) . . . . ? N4 Dy1 N3 C3 -12.0(5) . . . . ? N7 Dy1 N3 C3 -143.7(6) . . . . ? N6 Dy1 N3 C3 141.9(6) . . . . ? N8 Dy1 N3 C3 -80.1(5) . . . . ? N1 Dy1 N4 C4 160.5(4) . . . . ? N3 Dy1 N4 C4 -19.4(5) . . . . ? N2 Dy1 N4 C4 172.8(5) . . . . ? N5 Dy1 N4 C4 -108.6(5) . . . . ? N7 Dy1 N4 C4 42.3(5) . . . . ? N6 Dy1 N4 C4 -58.7(6) . . . . ? N8 Dy1 N4 C4 89.2(5) . . . . ? N1 Dy1 N5 C5 -94.9(6) . . . . ? N3 Dy1 N5 C5 59.2(6) . . . . ? N2 Dy1 N5 C5 -160.8(7) . . . . ? N4 Dy1 N5 C5 126.7(6) . . . . ? N7 Dy1 N5 C5 -13.5(8) . . . . ? N6 Dy1 N5 C5 -19.1(6) . . . . ? N8 Dy1 N5 C5 167.9(6) . . . . ? N1 Dy1 N6 C6 89.7(6) . . . . ? N3 Dy1 N6 C6 -101.7(6) . . . . ? N2 Dy1 N6 C6 41.8(7) . . . . ? N5 Dy1 N6 C6 -9.4(6) . . . . ? N4 Dy1 N6 C6 -65.0(7) . . . . ? N7 Dy1 N6 C6 174.3(7) . . . . ? N8 Dy1 N6 C6 165.8(6) . . . . ? N1 Dy1 N7 C7 -94.6(6) . . . . ? N3 Dy1 N7 C7 104.6(6) . . . . ? N2 Dy1 N7 C7 -46.9(7) . . . . ? N5 Dy1 N7 C7 179.6(6) . . . . ? N4 Dy1 N7 C7 49.2(7) . . . . ? N6 Dy1 N7 C7 -174.9(7) . . . . ? N8 Dy1 N7 C7 -1.0(6) . . . . ? N1 Dy1 N8 C8A 110.1(7) . . . . ? N3 Dy1 N8 C8A -46.0(7) . . . . ? N2 Dy1 N8 C8A 177.2(7) . . . . ? N5 Dy1 N8 C8A -151.7(7) . . . . ? N4 Dy1 N8 C8A -108.8(7) . . . . ? N7 Dy1 N8 C8A 29.2(7) . . . . ? N6 Dy1 N8 C8A 38.1(8) . . . . ? N1 Dy1 N8 C8B 54.5(8) . . . . ? N3 Dy1 N8 C8B -101.6(8) . . . . ? N2 Dy1 N8 C8B 121.5(8) . . . . ? N5 Dy1 N8 C8B 152.6(8) . . . . ? N4 Dy1 N8 C8B -164.4(8) . . . . ? N7 Dy1 N8 C8B -26.4(7) . . . . ? N6 Dy1 N8 C8B -17.5(9) . . . . ? Dy1 N1 C1 C2 54.3(7) . . . . ? Dy1 N2 C2 C1 30.0(8) . . . . ? N1 C1 C2 N2 -55.3(8) . . . . ? Dy1 N3 C3 C4 41.4(8) . . . . ? Dy1 N4 C4 C3 48.2(7) . . . . ? N3 C3 C4 N4 -59.0(8) . . . . ? Dy1 N5 C5 C6 46.1(10) . . . . ? N5 C5 C6 N6 -55.5(12) . . . . ? Dy1 N6 C6 C5 37.3(10) . . . . ? Dy1 N7 C7 C8A -27.1(10) . . . . ? Dy1 N7 C7 C8B 28.0(11) . . . . ? C8B N8 C8A C7 48.5(9) . . . . ? Dy1 N8 C8A C7 -55.4(11) . . . . ? N7 C7 C8A N8 54.8(13) . . . . ? C8B C7 C8A N8 -48.2(9) . . . . ? C8A N8 C8B C7 -47.7(9) . . . . ? Dy1 N8 C8B C7 50.1(13) . . . . ? N7 C7 C8B N8 -51.1(14) . . . . ? C8A C7 C8B N8 47.7(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 N1 H1A Se3 0.91 2.85 3.688(7) 154.6 4_665 N1 H1B Se4 0.91 2.53 3.419(6) 166.6 3_656 N2 H2A Se1 0.91 2.61 3.407(6) 146.9 1_554 N3 H3A Se2 0.91 2.62 3.506(7) 165.4 4_565 N3 H3B Se1 0.91 2.84 3.563(6) 137.0 4_565 N4 H4A Se3 0.91 2.67 3.543(6) 161.2 3_666 N4 H4B Se3 0.91 2.80 3.591(6) 145.7 1_554 N5 H5A Se4 0.91 2.87 3.769(8) 171.4 4_665 N5 H5B Se3 0.91 2.97 3.721(6) 140.9 3_666 N6 H6A Se1 0.91 2.69 3.594(7) 172.3 4_565 N6 H6B N9 0.91 2.23 3.081(9) 156.4 2_645 N7 H7A Se4 0.91 3.02 3.804(7) 146.0 3_656 N7 H7B Se2 0.91 2.77 3.555(7) 144.7 4_565 N9 H9B Se3 0.90 2.82 3.641(8) 151.8 3_666 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.467 _refine_diff_density_min -2.350 _refine_diff_density_rms 0.242 #===END data_complex_2a _database_code_depnum_ccdc_archive 'CCDC 767675' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 As La N6 Se4' _chemical_formula_sum 'C8 H26 As La N6 Se4' _chemical_formula_weight 736.02 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' La La -0.2871 2.4523 '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' As As 0.0499 2.0058 '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 8.8148(12) _cell_length_b 16.607(2) _cell_length_c 26.767(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3918.3(10) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 11555 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.35 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 11.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0706 _exptl_absorpt_correction_T_max 0.2113 _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 31570 _diffrn_reflns_av_R_equivalents 0.1296 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3589 _reflns_number_gt 3159 _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^)+(0.0253P)^2^+36.6483P] 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 3589 _refine_ls_number_parameters 182 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.156 _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 As1 As 0.49237(11) 0.26635(6) 0.38012(4) 0.0251(2) Uani 1 1 d . . . Se1 Se 0.33442(11) 0.33468(6) 0.43456(4) 0.0308(3) Uani 1 1 d . . . Se2 Se 0.34374(12) 0.16375(7) 0.34911(4) 0.0361(3) Uani 1 1 d . . . Se3 Se 0.69597(11) 0.21749(7) 0.42485(4) 0.0364(3) Uani 1 1 d . . . Se4 Se 0.57001(12) 0.34852(7) 0.31598(4) 0.0363(3) Uani 1 1 d . . . La1 La 0.04424(6) 0.25773(3) 0.38294(2) 0.02266(16) Uani 1 1 d . . . N1 N -0.0811(10) 0.4048(5) 0.3696(3) 0.038(2) Uani 1 1 d . . . H1 H -0.1830 0.3972 0.3668 0.045 Uiso 1 1 calc R . . N2 N -0.0315(9) 0.3368(5) 0.4674(3) 0.037(2) Uani 1 1 d . . . H2A H -0.0895 0.3043 0.4863 0.045 Uiso 1 1 calc R . . H2B H 0.0537 0.3476 0.4847 0.045 Uiso 1 1 calc R . . N3 N 0.1673(10) 0.3487(5) 0.3112(3) 0.039(2) Uani 1 1 d . . . H3A H 0.2686 0.3425 0.3124 0.047 Uiso 1 1 calc R . . H3B H 0.1356 0.3298 0.2815 0.047 Uiso 1 1 calc R . . N4 N -0.0288(11) 0.1028(5) 0.3679(3) 0.040(2) Uani 1 1 d D . . N5 N -0.1015(10) 0.2223(5) 0.2960(3) 0.041(2) Uani 1 1 d . . . H5A H -0.1869 0.2520 0.2949 0.049 Uiso 1 1 calc R . . H5B H -0.0422 0.2387 0.2707 0.049 Uiso 1 1 calc R . . N6 N 0.0949(11) 0.1565(5) 0.4582(3) 0.045(2) Uani 1 1 d . . . H6A H 0.1929 0.1618 0.4670 0.054 Uiso 1 1 calc R . . H6B H 0.0390 0.1734 0.4843 0.054 Uiso 1 1 calc R . . C1 C -0.0574(17) 0.4549(7) 0.4135(5) 0.061(4) Uani 1 1 d . . . H1A H -0.1108 0.5055 0.4095 0.073 Uiso 1 1 calc R . . H1B H 0.0499 0.4665 0.4172 0.073 Uiso 1 1 calc R . . C2 C -0.1138(15) 0.4127(7) 0.4586(5) 0.055(4) Uani 1 1 d . . . H2C H -0.1020 0.4475 0.4874 0.066 Uiso 1 1 calc R . . H2D H -0.2211 0.4013 0.4546 0.066 Uiso 1 1 calc R . . C3 C -0.0297(13) 0.4453(7) 0.3219(5) 0.053(3) Uani 1 1 d . . . H3C H -0.0862 0.4235 0.2939 0.063 Uiso 1 1 calc R . . H3D H -0.0512 0.5025 0.3239 0.063 Uiso 1 1 calc R . . C4 C 0.1339(14) 0.4334(7) 0.3134(5) 0.049(3) Uani 1 1 d . . . H4A H 0.1635 0.4589 0.2823 0.059 Uiso 1 1 calc R . . H4B H 0.1911 0.4581 0.3403 0.059 Uiso 1 1 calc R . . C5A C -0.130(4) 0.0791(15) 0.3282(9) 0.074(4) Uani 0.50 1 d PD . . C5B C -0.048(3) 0.0826(14) 0.3146(7) 0.074(4) Uani 0.50 1 d PD . . C6 C -0.1436(19) 0.1380(7) 0.2865(5) 0.074(4) Uani 1 1 d D . . C7A C -0.033(3) 0.0461(14) 0.4097(8) 0.052(6) Uani 0.50 1 d PD . . C7B C 0.047(3) 0.0450(13) 0.3996(7) 0.052(6) Uani 0.50 1 d PD . . C8 C 0.066(2) 0.0722(7) 0.4520(4) 0.071(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0208(5) 0.0321(6) 0.0225(5) -0.0003(4) 0.0007(4) -0.0016(4) Se1 0.0251(5) 0.0385(6) 0.0287(6) -0.0081(5) 0.0014(4) -0.0014(5) Se2 0.0316(6) 0.0328(6) 0.0438(7) -0.0123(5) 0.0022(5) -0.0028(5) Se3 0.0239(5) 0.0523(7) 0.0331(6) 0.0082(5) -0.0004(4) 0.0035(5) Se4 0.0326(6) 0.0467(7) 0.0295(6) 0.0076(5) 0.0028(5) -0.0056(5) La1 0.0227(3) 0.0231(3) 0.0222(3) 0.0007(2) -0.0011(2) -0.0012(2) N1 0.031(5) 0.038(5) 0.044(6) -0.002(4) -0.006(4) -0.003(4) N2 0.023(4) 0.053(6) 0.036(5) -0.008(4) -0.003(4) -0.003(4) N3 0.046(6) 0.031(5) 0.039(5) 0.001(4) -0.003(4) -0.003(4) N4 0.060(6) 0.035(5) 0.025(5) 0.007(4) -0.004(4) -0.010(5) N5 0.042(5) 0.048(6) 0.032(5) 0.003(4) 0.003(4) 0.000(5) N6 0.052(6) 0.048(6) 0.034(5) 0.004(4) -0.006(5) 0.001(5) C1 0.073(10) 0.039(7) 0.070(10) -0.009(7) 0.000(8) 0.004(7) C2 0.065(9) 0.045(8) 0.055(8) -0.011(6) 0.027(7) 0.004(7) C3 0.046(8) 0.043(7) 0.070(9) 0.021(6) -0.010(7) 0.002(6) C4 0.060(8) 0.043(7) 0.045(7) 0.005(6) 0.009(6) -0.006(6) C5A 0.122(12) 0.044(6) 0.057(8) 0.007(5) -0.034(8) -0.040(7) C5B 0.122(12) 0.044(6) 0.057(8) 0.007(5) -0.034(8) -0.040(7) C6 0.122(12) 0.044(6) 0.057(8) 0.007(5) -0.034(8) -0.040(7) C7A 0.034(14) 0.040(8) 0.082(14) 0.017(9) -0.040(13) -0.016(13) C7B 0.034(14) 0.040(8) 0.082(14) 0.017(9) -0.040(13) -0.016(13) C8 0.143(15) 0.030(7) 0.040(8) 0.010(6) -0.012(9) -0.008(8) _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 As1 Se4 2.2975(14) . ? As1 Se2 2.3041(14) . ? As1 Se3 2.3049(14) . ? As1 Se1 2.3128(14) . ? Se1 La1 3.1757(12) . ? Se2 La1 3.1977(12) . ? Se3 La1 3.3361(12) 1_655 ? La1 N6 2.661(9) . ? La1 N3 2.673(8) . ? La1 N4 2.683(9) . ? La1 N2 2.697(8) . ? La1 N1 2.704(9) . ? La1 N5 2.722(9) . ? La1 Se3 3.3361(12) 1_455 ? N1 C1 1.455(14) . ? N1 C3 1.511(14) . ? N1 H1 0.9100 . ? N2 C2 1.474(14) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C4 1.438(13) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C5A 1.444(16) . ? N4 C7B 1.444(17) . ? N4 C7A 1.464(17) . ? N4 C5B 1.475(17) . ? N5 C6 1.470(14) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 C8 1.432(14) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? C1 C2 1.482(17) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.474(16) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5A C6 1.489(17) . ? C5B C6 1.454(18) . ? C7A C8 1.493(17) . ? C7B C8 1.484(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 Se4 As1 Se2 109.84(6) . . ? Se4 As1 Se3 111.43(6) . . ? Se2 As1 Se3 111.69(6) . . ? Se4 As1 Se1 111.02(6) . . ? Se2 As1 Se1 104.33(5) . . ? Se3 As1 Se1 108.32(5) . . ? As1 Se1 La1 90.77(4) . . ? As1 Se2 La1 90.37(4) . . ? As1 Se3 La1 118.12(5) . 1_655 ? N6 La1 N3 146.4(3) . . ? N6 La1 N4 63.1(3) . . ? N3 La1 N4 122.1(3) . . ? N6 La1 N2 73.4(3) . . ? N3 La1 N2 115.3(3) . . ? N4 La1 N2 122.2(3) . . ? N6 La1 N1 137.7(3) . . ? N3 La1 N1 63.9(3) . . ? N4 La1 N1 138.4(3) . . ? N2 La1 N1 64.5(3) . . ? N6 La1 N5 126.1(3) . . ? N3 La1 N5 72.5(3) . . ? N4 La1 N5 63.3(3) . . ? N2 La1 N5 134.8(3) . . ? N1 La1 N5 83.6(3) . . ? N6 La1 Se1 77.9(2) . . ? N3 La1 Se1 76.01(19) . . ? N4 La1 Se1 130.14(19) . . ? N2 La1 Se1 68.84(18) . . ? N1 La1 Se1 91.33(19) . . ? N5 La1 Se1 147.05(19) . . ? N6 La1 Se2 76.6(2) . . ? N3 La1 Se2 74.78(19) . . ? N4 La1 Se2 71.8(2) . . ? N2 La1 Se2 132.77(18) . . ? N1 La1 Se2 137.78(19) . . ? N5 La1 Se2 92.4(2) . . ? Se1 La1 Se2 69.79(3) . . ? N6 La1 Se3 76.9(2) . 1_455 ? N3 La1 Se3 136.7(2) . 1_455 ? N4 La1 Se3 68.7(2) . 1_455 ? N2 La1 Se3 65.67(18) . 1_455 ? N1 La1 Se3 81.35(19) . 1_455 ? N5 La1 Se3 79.02(19) . 1_455 ? Se1 La1 Se3 132.49(3) . 1_455 ? Se2 La1 Se3 139.22(3) . 1_455 ? C1 N1 C3 112.6(9) . . ? C1 N1 La1 110.5(7) . . ? C3 N1 La1 113.1(7) . . ? C1 N1 H1 106.7 . . ? C3 N1 H1 106.7 . . ? La1 N1 H1 106.7 . . ? C2 N2 La1 113.9(7) . . ? C2 N2 H2A 108.8 . . ? La1 N2 H2A 108.8 . . ? C2 N2 H2B 108.8 . . ? La1 N2 H2B 108.8 . . ? H2A N2 H2B 107.7 . . ? C4 N3 La1 116.1(7) . . ? C4 N3 H3A 108.3 . . ? La1 N3 H3A 108.3 . . ? C4 N3 H3B 108.3 . . ? La1 N3 H3B 108.3 . . ? H3A N3 H3B 107.4 . . ? C5A N4 C7B 122.5(14) . . ? C5A N4 C7A 111.8(12) . . ? C7B N4 C7A 30.0(12) . . ? C5A N4 C5B 32.2(17) . . ? C7B N4 C5B 118.1(13) . . ? C7A N4 C5B 126.2(15) . . ? C5A N4 La1 121.4(10) . . ? C7B N4 La1 116.0(10) . . ? C7A N4 La1 120.6(10) . . ? C5B N4 La1 113.0(11) . . ? C6 N5 La1 118.2(7) . . ? C6 N5 H5A 107.8 . . ? La1 N5 H5A 107.8 . . ? C6 N5 H5B 107.8 . . ? La1 N5 H5B 107.8 . . ? H5A N5 H5B 107.1 . . ? C8 N6 La1 120.0(7) . . ? C8 N6 H6A 107.3 . . ? La1 N6 H6A 107.3 . . ? C8 N6 H6B 107.3 . . ? La1 N6 H6B 107.3 . . ? H6A N6 H6B 106.9 . . ? N1 C1 C2 109.9(10) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 111.6(10) . . ? N2 C2 H2C 109.3 . . ? C1 C2 H2C 109.3 . . ? N2 C2 H2D 109.3 . . ? C1 C2 H2D 109.3 . . ? H2C C2 H2D 108.0 . . ? C4 C3 N1 111.3(9) . . ? C4 C3 H3C 109.4 . . ? N1 C3 H3C 109.4 . . ? C4 C3 H3D 109.4 . . ? N1 C3 H3D 109.4 . . ? H3C C3 H3D 108.0 . . ? N3 C4 C3 109.8(10) . . ? N3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N4 C5A C6 114.8(14) . . ? C6 C5B N4 115.0(16) . . ? C5B C6 N5 111.6(14) . . ? C5B C6 C5A 32.0(17) . . ? N5 C6 C5A 118.5(12) . . ? N4 C7A C8 112.3(13) . . ? N4 C7B C8 114.0(15) . . ? N6 C8 C7B 115.2(12) . . ? N6 C8 C7A 118.4(13) . . ? C7B C8 C7A 29.3(12) . . ? 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 Se4 As1 Se1 La1 99.19(5) . . . . ? Se2 As1 Se1 La1 -19.07(5) . . . . ? Se3 As1 Se1 La1 -138.17(5) . . . . ? Se4 As1 Se2 La1 -100.13(5) . . . . ? Se3 As1 Se2 La1 135.72(5) . . . . ? Se1 As1 Se2 La1 18.93(5) . . . . ? Se4 As1 Se3 La1 -5.94(8) . . . 1_655 ? Se2 As1 Se3 La1 117.32(6) . . . 1_655 ? Se1 As1 Se3 La1 -128.34(5) . . . 1_655 ? As1 Se1 La1 N6 94.0(2) . . . . ? As1 Se1 La1 N3 -64.6(2) . . . . ? As1 Se1 La1 N4 55.8(2) . . . . ? As1 Se1 La1 N2 170.8(2) . . . . ? As1 Se1 La1 N1 -127.27(19) . . . . ? As1 Se1 La1 N5 -46.9(4) . . . . ? As1 Se1 La1 Se2 14.06(4) . . . . ? As1 Se1 La1 Se3 153.27(4) . . . 1_455 ? As1 Se2 La1 N6 -95.9(2) . . . . ? As1 Se2 La1 N3 66.3(2) . . . . ? As1 Se2 La1 N4 -161.70(18) . . . . ? As1 Se2 La1 N2 -44.3(3) . . . . ? As1 Se2 La1 N1 54.2(3) . . . . ? As1 Se2 La1 N5 137.45(19) . . . . ? As1 Se2 La1 Se1 -14.12(4) . . . . ? As1 Se2 La1 Se3 -146.60(5) . . . 1_455 ? N6 La1 N1 C1 32.2(9) . . . . ? N3 La1 N1 C1 -114.8(8) . . . . ? N4 La1 N1 C1 135.3(7) . . . . ? N2 La1 N1 C1 24.6(7) . . . . ? N5 La1 N1 C1 171.5(8) . . . . ? Se1 La1 N1 C1 -41.1(8) . . . . ? Se2 La1 N1 C1 -101.9(8) . . . . ? Se3 La1 N1 C1 91.7(8) 1_455 . . . ? N6 La1 N1 C3 159.4(7) . . . . ? N3 La1 N1 C3 12.4(7) . . . . ? N4 La1 N1 C3 -97.5(7) . . . . ? N2 La1 N1 C3 151.8(8) . . . . ? N5 La1 N1 C3 -61.3(7) . . . . ? Se1 La1 N1 C3 86.1(7) . . . . ? Se2 La1 N1 C3 25.3(8) . . . . ? Se3 La1 N1 C3 -141.1(7) 1_455 . . . ? N6 La1 N2 C2 -168.6(8) . . . . ? N3 La1 N2 C2 46.3(8) . . . . ? N4 La1 N2 C2 -126.7(7) . . . . ? N1 La1 N2 C2 6.1(7) . . . . ? N5 La1 N2 C2 -43.8(9) . . . . ? Se1 La1 N2 C2 108.3(7) . . . . ? Se2 La1 N2 C2 138.7(7) . . . . ? Se3 La1 N2 C2 -85.8(7) 1_455 . . . ? N6 La1 N3 C4 -120.8(8) . . . . ? N4 La1 N3 C4 150.4(7) . . . . ? N2 La1 N3 C4 -22.7(9) . . . . ? N1 La1 N3 C4 17.8(7) . . . . ? N5 La1 N3 C4 109.2(8) . . . . ? Se1 La1 N3 C4 -80.7(8) . . . . ? Se2 La1 N3 C4 -153.2(8) . . . . ? Se3 La1 N3 C4 57.9(9) 1_455 . . . ? N6 La1 N4 C5A 161.9(19) . . . . ? N3 La1 N4 C5A -56.5(19) . . . . ? N2 La1 N4 C5A 116.1(18) . . . . ? N1 La1 N4 C5A 29.3(19) . . . . ? N5 La1 N4 C5A -11.8(18) . . . . ? Se1 La1 N4 C5A -155.4(18) . . . . ? Se2 La1 N4 C5A -114.3(18) . . . . ? Se3 La1 N4 C5A 76.3(18) 1_455 . . . ? N6 La1 N4 C7B -21.9(12) . . . . ? N3 La1 N4 C7B 119.7(12) . . . . ? N2 La1 N4 C7B -67.7(13) . . . . ? N1 La1 N4 C7B -154.6(12) . . . . ? N5 La1 N4 C7B 164.3(13) . . . . ? Se1 La1 N4 C7B 20.7(13) . . . . ? Se2 La1 N4 C7B 61.9(12) . . . . ? Se3 La1 N4 C7B -107.6(12) 1_455 . . . ? N6 La1 N4 C7A 11.9(14) . . . . ? N3 La1 N4 C7A 153.5(14) . . . . ? N2 La1 N4 C7A -34.0(15) . . . . ? N1 La1 N4 C7A -120.8(14) . . . . ? N5 La1 N4 C7A -161.9(15) . . . . ? Se1 La1 N4 C7A 54.5(15) . . . . ? Se2 La1 N4 C7A 95.7(14) . . . . ? Se3 La1 N4 C7A -73.8(14) 1_455 . . . ? N6 La1 N4 C5B -162.9(14) . . . . ? N3 La1 N4 C5B -21.3(14) . . . . ? N2 La1 N4 C5B 151.3(13) . . . . ? N1 La1 N4 C5B 64.5(14) . . . . ? N5 La1 N4 C5B 23.3(13) . . . . ? Se1 La1 N4 C5B -120.2(13) . . . . ? Se2 La1 N4 C5B -79.1(13) . . . . ? Se3 La1 N4 C5B 111.4(13) 1_455 . . . ? N6 La1 N5 C6 -6.8(11) . . . . ? N3 La1 N5 C6 141.5(10) . . . . ? N4 La1 N5 C6 0.1(9) . . . . ? N2 La1 N5 C6 -109.9(10) . . . . ? N1 La1 N5 C6 -153.9(10) . . . . ? Se1 La1 N5 C6 123.5(9) . . . . ? Se2 La1 N5 C6 68.3(9) . . . . ? Se3 La1 N5 C6 -71.5(9) 1_455 . . . ? N3 La1 N6 C8 -105.1(11) . . . . ? N4 La1 N6 C8 3.2(10) . . . . ? N2 La1 N6 C8 143.9(11) . . . . ? N1 La1 N6 C8 136.8(10) . . . . ? N5 La1 N6 C8 10.1(11) . . . . ? Se1 La1 N6 C8 -144.8(10) . . . . ? Se2 La1 N6 C8 -73.0(10) . . . . ? Se3 La1 N6 C8 75.8(10) 1_455 . . . ? C3 N1 C1 C2 178.4(10) . . . . ? La1 N1 C1 C2 -54.1(12) . . . . ? La1 N2 C2 C1 -36.3(12) . . . . ? N1 C1 C2 N2 61.7(14) . . . . ? C1 N1 C3 C4 84.8(13) . . . . ? La1 N1 C3 C4 -41.3(12) . . . . ? La1 N3 C4 C3 -46.5(12) . . . . ? N1 C3 C4 N3 58.1(13) . . . . ? C7B N4 C5A C6 -154(2) . . . . ? C7A N4 C5A C6 174(2) . . . . ? C5B N4 C5A C6 -62(2) . . . . ? La1 N4 C5A C6 22(3) . . . . ? C5A N4 C5B C6 65(2) . . . . ? C7B N4 C5B C6 171.8(19) . . . . ? C7A N4 C5B C6 137(2) . . . . ? La1 N4 C5B C6 -48(2) . . . . ? N4 C5B C6 N5 48(3) . . . . ? N4 C5B C6 C5A -62(2) . . . . ? La1 N5 C6 C5B -23.6(18) . . . . ? La1 N5 C6 C5A 11(2) . . . . ? N4 C5A C6 C5B 64(2) . . . . ? N4 C5A C6 N5 -21(4) . . . . ? C5A N4 C7A C8 -177(2) . . . . ? C7B N4 C7A C8 65(2) . . . . ? C5B N4 C7A C8 150(2) . . . . ? La1 N4 C7A C8 -24(3) . . . . ? C5A N4 C7B C8 -145(2) . . . . ? C7A N4 C7B C8 -68(2) . . . . ? C5B N4 C7B C8 177.9(19) . . . . ? La1 N4 C7B C8 39(2) . . . . ? La1 N6 C8 C7B 15.1(19) . . . . ? La1 N6 C8 C7A -18(2) . . . . ? N4 C7B C8 N6 -36(2) . . . . ? N4 C7B C8 C7A 68(2) . . . . ? N4 C7A C8 N6 27(3) . . . . ? N4 C7A C8 C7B -65(2) . . . . ? 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 H1 Se4 0.91 2.69 3.520(9) 151.9 1_455 N2 H2B Se3 0.90 2.93 3.627(9) 135.1 6_566 N3 H3A Se4 0.90 2.66 3.553(9) 171.3 . N3 H3B Se4 0.90 2.69 3.511(9) 152.2 8_556 N5 H5A Se4 0.90 2.74 3.614(9) 165.7 1_455 N6 H6B Se1 0.90 2.83 3.679(10) 158.6 6_566 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.820 _refine_diff_density_min -1.088 _refine_diff_density_rms 0.200 #===END data_complex_2b _database_code_depnum_ccdc_archive 'CCDC 767676' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 As Ce N6 Se4' _chemical_formula_sum 'C8 H26 As Ce N6 Se4' _chemical_formula_weight 737.24 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' Ce Ce -0.2871 2.4523 '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' _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 8.8021(9) _cell_length_b 16.5022(14) _cell_length_c 26.691(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3877.0(7) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12052 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 11.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2087 _exptl_absorpt_correction_T_max 0.3414 _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 36022 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.0365 _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 -28 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3548 _reflns_number_gt 3247 _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^)+(0.0079P)^2^+44.1402P] 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 3548 _refine_ls_number_parameters 176 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.169 _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 Ce1 Ce 0.04323(5) 0.24176(3) 0.617129(17) 0.01677(13) Uani 1 1 d . . . Se1 Se 0.33301(9) 0.16434(5) 0.56517(3) 0.0219(2) Uani 1 1 d . . . Se2 Se 0.34300(10) 0.33706(5) 0.65043(3) 0.0250(2) Uani 1 1 d . . . Se4 Se 0.56887(10) 0.15082(6) 0.68409(3) 0.0256(2) Uani 1 1 d . . . Se3 Se 0.69549(9) 0.28156(6) 0.57455(3) 0.0251(2) Uani 1 1 d . . . As1 As 0.49117(9) 0.23340(5) 0.61948(3) 0.01809(19) Uani 1 1 d . . . N1 N -0.0820(9) 0.0933(4) 0.6309(3) 0.0270(17) Uani 1 1 d . . . H1 H -0.1863 0.1013 0.6335 0.032 Uiso 1 1 calc R . . N2 N -0.0333(8) 0.1625(5) 0.5320(3) 0.0271(17) Uani 1 1 d . . . H2A H -0.0928 0.1960 0.5126 0.033 Uiso 1 1 calc R . . H2B H 0.0537 0.1514 0.5142 0.033 Uiso 1 1 calc R . . N3 N 0.1670(8) 0.1504(4) 0.6889(3) 0.0284(17) Uani 1 1 d . . . H3A H 0.2707 0.1570 0.6877 0.034 Uiso 1 1 calc R . . H3B H 0.1346 0.1697 0.7194 0.034 Uiso 1 1 calc R . . N4 N -0.0325(9) 0.3973(4) 0.6320(2) 0.0289(18) Uani 1 1 d D . . N5 N -0.1059(9) 0.2759(4) 0.7048(3) 0.0307(18) Uani 1 1 d D . . N6 N 0.0939(9) 0.3430(4) 0.5406(3) 0.0314(18) Uani 1 1 d D . . C1 C -0.0579(12) 0.0420(5) 0.5868(3) 0.034(2) Uani 1 1 d . . . H1A H -0.1122 -0.0101 0.5910 0.041 Uiso 1 1 calc R . . H1B H 0.0518 0.0302 0.5828 0.041 Uiso 1 1 calc R . . C2 C -0.1166(11) 0.0855(5) 0.5408(4) 0.032(2) Uani 1 1 d . . . H2C H -0.1052 0.0498 0.5112 0.039 Uiso 1 1 calc R . . H2D H -0.2261 0.0972 0.5452 0.039 Uiso 1 1 calc R . . C3 C -0.0331(10) 0.0533(5) 0.6788(3) 0.029(2) Uani 1 1 d . . . H3C H -0.0894 0.0772 0.7073 0.035 Uiso 1 1 calc R . . H3D H -0.0575 -0.0053 0.6773 0.035 Uiso 1 1 calc R . . C4 C 0.1340(11) 0.0641(5) 0.6867(4) 0.031(2) Uani 1 1 d . . . H4A H 0.1653 0.0377 0.7184 0.037 Uiso 1 1 calc R . . H4B H 0.1911 0.0388 0.6589 0.037 Uiso 1 1 calc R . . C5A C -0.146(2) 0.4197(12) 0.6703(6) 0.036(3) Uani 0.45 1 d PD . . C5B C -0.064(2) 0.4145(9) 0.6856(4) 0.036(3) Uani 0.55 1 d PD . . C6A C -0.114(3) 0.3649(6) 0.7141(8) 0.036(3) Uani 0.47 1 d PD . . C6B C -0.1730(19) 0.3574(6) 0.7107(8) 0.036(3) Uani 0.53 1 d PD . . C7A C 0.047(2) 0.4601(9) 0.6015(6) 0.036(3) Uani 0.48 1 d PD . . C7B C -0.024(2) 0.4512(10) 0.5879(5) 0.036(3) Uani 0.52 1 d PD . . C8A C 0.040(2) 0.4267(7) 0.5484(7) 0.036(3) Uani 0.56 1 d PD . . C8B C 0.095(3) 0.4322(7) 0.5491(10) 0.036(3) Uani 0.44 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 Ce1 0.0179(2) 0.0172(2) 0.0152(2) 0.00026(19) 0.00056(19) 0.00133(19) Se1 0.0195(4) 0.0264(5) 0.0198(4) -0.0055(4) -0.0014(3) 0.0013(4) Se2 0.0227(5) 0.0230(5) 0.0294(5) -0.0074(4) -0.0013(4) 0.0017(4) Se4 0.0249(5) 0.0316(5) 0.0203(4) 0.0050(4) -0.0019(4) 0.0040(4) Se3 0.0183(4) 0.0353(5) 0.0216(4) 0.0048(4) 0.0000(4) -0.0012(4) As1 0.0170(4) 0.0216(4) 0.0156(4) -0.0002(3) -0.0006(3) 0.0010(3) N1 0.027(4) 0.024(4) 0.030(4) 0.003(3) 0.006(3) 0.003(3) N2 0.019(4) 0.039(5) 0.023(4) -0.004(3) -0.003(3) -0.001(3) N3 0.031(4) 0.031(4) 0.023(4) 0.000(3) 0.002(3) 0.001(3) N4 0.046(5) 0.024(4) 0.017(4) 0.002(3) 0.004(3) 0.012(4) N5 0.039(5) 0.027(4) 0.026(4) -0.004(3) 0.001(4) 0.003(4) N6 0.046(5) 0.023(4) 0.026(4) 0.004(3) 0.009(4) 0.000(4) C1 0.042(6) 0.023(5) 0.037(6) -0.004(4) 0.006(5) 0.001(4) C2 0.036(6) 0.026(5) 0.035(6) -0.007(4) -0.008(5) -0.006(4) C3 0.032(5) 0.024(5) 0.031(5) 0.010(4) 0.006(4) 0.000(4) C4 0.034(5) 0.025(5) 0.033(5) 0.000(4) 0.000(4) 0.004(4) C5A 0.050(8) 0.024(3) 0.033(4) 0.003(3) 0.017(4) 0.009(4) C5B 0.050(8) 0.024(3) 0.033(4) 0.003(3) 0.017(4) 0.009(4) C6A 0.050(8) 0.024(3) 0.033(4) 0.003(3) 0.017(4) 0.009(4) C6B 0.050(8) 0.024(3) 0.033(4) 0.003(3) 0.017(4) 0.009(4) C7A 0.050(8) 0.024(3) 0.033(4) 0.003(3) 0.017(4) 0.009(4) C7B 0.050(8) 0.024(3) 0.033(4) 0.003(3) 0.017(4) 0.009(4) C8A 0.050(8) 0.024(3) 0.033(4) 0.003(3) 0.017(4) 0.009(4) C8B 0.050(8) 0.024(3) 0.033(4) 0.003(3) 0.017(4) 0.009(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 Ce1 N3 2.670(7) . ? Ce1 N6 2.676(7) . ? Ce1 N4 2.682(7) . ? Ce1 N2 2.708(7) . ? Ce1 N1 2.711(7) . ? Ce1 N5 2.741(7) . ? Ce1 Se1 3.1720(10) . ? Ce1 Se2 3.1978(10) . ? Ce1 Se3 3.3304(10) 1_455 ? Se1 As1 2.3104(12) . ? Se2 As1 2.3044(12) . ? Se4 As1 2.3021(12) . ? Se3 As1 2.3030(12) . ? Se3 Ce1 3.3304(10) 1_655 ? N1 C1 1.467(11) . ? N1 C3 1.501(11) . ? N1 H1 0.9300 . ? N2 C2 1.486(11) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C4 1.455(11) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N4 C5A 1.473(9) . ? N4 C7B 1.478(9) . ? N4 C5B 1.484(9) . ? N4 C7A 1.495(9) . ? N5 C6B 1.478(9) . ? N5 C6A 1.491(9) . ? N6 C8A 1.477(9) . ? N6 C8B 1.490(10) . ? C1 C2 1.512(13) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 C4 1.497(13) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5A C6A 1.502(10) . ? C5B C6B 1.500(10) . ? C7A C8A 1.520(10) . ? C7B C8B 1.505(10) . ? 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 Ce1 N6 146.3(2) . . ? N3 Ce1 N4 122.4(2) . . ? N6 Ce1 N4 63.7(2) . . ? N3 Ce1 N2 115.5(2) . . ? N6 Ce1 N2 72.7(2) . . ? N4 Ce1 N2 121.7(2) . . ? N3 Ce1 N1 63.8(2) . . ? N6 Ce1 N1 137.3(2) . . ? N4 Ce1 N1 138.0(2) . . ? N2 Ce1 N1 64.9(2) . . ? N3 Ce1 N5 72.5(2) . . ? N6 Ce1 N5 127.1(2) . . ? N4 Ce1 N5 63.74(19) . . ? N2 Ce1 N5 134.2(2) . . ? N1 Ce1 N5 82.8(2) . . ? N3 Ce1 Se1 76.01(16) . . ? N6 Ce1 Se1 77.51(16) . . ? N4 Ce1 Se1 130.57(16) . . ? N2 Ce1 Se1 68.81(15) . . ? N1 Ce1 Se1 91.28(16) . . ? N5 Ce1 Se1 147.25(16) . . ? N3 Ce1 Se2 75.03(16) . . ? N6 Ce1 Se2 76.57(18) . . ? N4 Ce1 Se2 72.14(17) . . ? N2 Ce1 Se2 132.56(15) . . ? N1 Ce1 Se2 137.90(16) . . ? N5 Ce1 Se2 93.25(16) . . ? Se1 Ce1 Se2 69.89(2) . . ? N3 Ce1 Se3 136.98(16) . 1_455 ? N6 Ce1 Se3 76.68(18) . 1_455 ? N4 Ce1 Se3 68.48(17) . 1_455 ? N2 Ce1 Se3 65.18(16) . 1_455 ? N1 Ce1 Se3 81.43(16) . 1_455 ? N5 Ce1 Se3 79.08(16) . 1_455 ? Se1 Ce1 Se3 132.01(3) . 1_455 ? Se2 Ce1 Se3 139.13(3) . 1_455 ? As1 Se1 Ce1 90.66(3) . . ? As1 Se2 Ce1 90.13(3) . . ? As1 Se3 Ce1 118.16(4) . 1_655 ? Se4 As1 Se3 111.24(5) . . ? Se4 As1 Se2 109.82(5) . . ? Se3 As1 Se2 111.87(5) . . ? Se4 As1 Se1 110.92(5) . . ? Se3 As1 Se1 108.31(5) . . ? Se2 As1 Se1 104.48(4) . . ? C1 N1 C3 112.8(7) . . ? C1 N1 Ce1 110.7(5) . . ? C3 N1 Ce1 113.4(5) . . ? C1 N1 H1 106.5 . . ? C3 N1 H1 106.5 . . ? Ce1 N1 H1 106.5 . . ? C2 N2 Ce1 113.7(5) . . ? C2 N2 H2A 108.8 . . ? Ce1 N2 H2A 108.8 . . ? C2 N2 H2B 108.8 . . ? Ce1 N2 H2B 108.8 . . ? H2A N2 H2B 107.7 . . ? C4 N3 Ce1 116.3(5) . . ? C4 N3 H3A 108.2 . . ? Ce1 N3 H3A 108.2 . . ? C4 N3 H3B 108.2 . . ? Ce1 N3 H3B 108.2 . . ? H3A N3 H3B 107.4 . . ? C5A N4 C7B 115.8(10) . . ? C5A N4 C5B 32.5(10) . . ? C7B N4 C5B 131.5(10) . . ? C5A N4 C7A 121.5(12) . . ? C7B N4 C7A 28.9(10) . . ? C5B N4 C7A 118.8(10) . . ? C5A N4 Ce1 120.7(9) . . ? C7B N4 Ce1 116.5(8) . . ? C5B N4 Ce1 111.9(7) . . ? C7A N4 Ce1 117.8(8) . . ? C6B N5 C6A 20.9(12) . . ? C6B N5 Ce1 118.1(8) . . ? C6A N5 Ce1 111.6(9) . . ? C8A N6 C8B 19.2(12) . . ? C8A N6 Ce1 115.0(8) . . ? C8B N6 Ce1 120.1(10) . . ? 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 111.5(7) . . ? N2 C2 H2C 109.3 . . ? C1 C2 H2C 109.3 . . ? N2 C2 H2D 109.3 . . ? C1 C2 H2D 109.3 . . ? H2C C2 H2D 108.0 . . ? C4 C3 N1 110.5(7) . . ? C4 C3 H3C 109.6 . . ? N1 C3 H3C 109.6 . . ? C4 C3 H3D 109.6 . . ? N1 C3 H3D 109.6 . . ? H3C C3 H3D 108.1 . . ? N3 C4 C3 108.6(7) . . ? N3 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? N3 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? N4 C5A C6A 105.3(14) . . ? N4 C5B C6B 115.5(14) . . ? N5 C6A C5A 118.2(15) . . ? N5 C6B C5B 105.6(11) . . ? N4 C7A C8A 103.6(12) . . ? N4 C7B C8B 117.2(15) . . ? N6 C8A C7A 117.2(14) . . ? N6 C8B C7B 107.9(13) . . ? 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 Ce1 Se1 As1 -64.70(16) . . . . ? N6 Ce1 Se1 As1 94.29(17) . . . . ? N4 Ce1 Se1 As1 56.2(2) . . . . ? N2 Ce1 Se1 As1 170.35(17) . . . . ? N1 Ce1 Se1 As1 -127.24(16) . . . . ? N5 Ce1 Se1 As1 -48.5(3) . . . . ? Se2 Ce1 Se1 As1 14.21(3) . . . . ? Se3 Ce1 Se1 As1 153.15(4) 1_455 . . . ? N3 Ce1 Se2 As1 66.04(17) . . . . ? N6 Ce1 Se2 As1 -95.67(16) . . . . ? N4 Ce1 Se2 As1 -161.99(14) . . . . ? N2 Ce1 Se2 As1 -45.1(2) . . . . ? N1 Ce1 Se2 As1 54.1(2) . . . . ? N5 Ce1 Se2 As1 136.95(15) . . . . ? Se1 Ce1 Se2 As1 -14.25(3) . . . . ? Se3 Ce1 Se2 As1 -146.01(4) 1_455 . . . ? Ce1 Se3 As1 Se4 -6.46(6) 1_655 . . . ? Ce1 Se3 As1 Se2 116.77(5) 1_655 . . . ? Ce1 Se3 As1 Se1 -128.61(4) 1_655 . . . ? Ce1 Se2 As1 Se4 -99.89(4) . . . . ? Ce1 Se2 As1 Se3 136.09(4) . . . . ? Ce1 Se2 As1 Se1 19.13(4) . . . . ? Ce1 Se1 As1 Se4 98.97(4) . . . . ? Ce1 Se1 As1 Se3 -138.68(4) . . . . ? Ce1 Se1 As1 Se2 -19.30(4) . . . . ? N3 Ce1 N1 C1 -114.5(6) . . . . ? N6 Ce1 N1 C1 32.1(7) . . . . ? N4 Ce1 N1 C1 135.3(6) . . . . ? N2 Ce1 N1 C1 25.1(6) . . . . ? N5 Ce1 N1 C1 171.6(6) . . . . ? Se1 Ce1 N1 C1 -40.8(6) . . . . ? Se2 Ce1 N1 C1 -101.5(6) . . . . ? Se3 Ce1 N1 C1 91.6(6) 1_455 . . . ? N3 Ce1 N1 C3 13.5(5) . . . . ? N6 Ce1 N1 C3 160.0(5) . . . . ? N4 Ce1 N1 C3 -96.7(6) . . . . ? N2 Ce1 N1 C3 153.0(6) . . . . ? N5 Ce1 N1 C3 -60.5(5) . . . . ? Se1 Ce1 N1 C3 87.2(5) . . . . ? Se2 Ce1 N1 C3 26.4(6) . . . . ? Se3 Ce1 N1 C3 -140.5(5) 1_455 . . . ? N3 Ce1 N2 C2 46.4(6) . . . . ? N6 Ce1 N2 C2 -168.8(6) . . . . ? N4 Ce1 N2 C2 -126.3(6) . . . . ? N1 Ce1 N2 C2 6.2(5) . . . . ? N5 Ce1 N2 C2 -43.5(7) . . . . ? Se1 Ce1 N2 C2 108.2(6) . . . . ? Se2 Ce1 N2 C2 139.3(5) . . . . ? Se3 Ce1 N2 C2 -85.8(6) 1_455 . . . ? N6 Ce1 N3 C4 -119.6(6) . . . . ? N4 Ce1 N3 C4 150.1(6) . . . . ? N2 Ce1 N3 C4 -22.6(7) . . . . ? N1 Ce1 N3 C4 18.1(6) . . . . ? N5 Ce1 N3 C4 108.6(6) . . . . ? Se1 Ce1 N3 C4 -80.5(6) . . . . ? Se2 Ce1 N3 C4 -153.0(6) . . . . ? Se3 Ce1 N3 C4 57.6(7) 1_455 . . . ? N3 Ce1 N4 C5A -60.8(12) . . . . ? N6 Ce1 N4 C5A 157.4(12) . . . . ? N2 Ce1 N4 C5A 111.4(12) . . . . ? N1 Ce1 N4 C5A 24.8(13) . . . . ? N5 Ce1 N4 C5A -16.0(12) . . . . ? Se1 Ce1 N4 C5A -160.3(11) . . . . ? Se2 Ce1 N4 C5A -119.1(12) . . . . ? Se3 Ce1 N4 C5A 72.1(12) 1_455 . . . ? N3 Ce1 N4 C7B 149.7(10) . . . . ? N6 Ce1 N4 C7B 7.9(10) . . . . ? N2 Ce1 N4 C7B -38.1(11) . . . . ? N1 Ce1 N4 C7B -124.7(10) . . . . ? N5 Ce1 N4 C7B -165.6(11) . . . . ? Se1 Ce1 N4 C7B 50.1(11) . . . . ? Se2 Ce1 N4 C7B 91.4(10) . . . . ? Se3 Ce1 N4 C7B -77.4(10) 1_455 . . . ? N3 Ce1 N4 C5B -25.7(10) . . . . ? N6 Ce1 N4 C5B -167.5(9) . . . . ? N2 Ce1 N4 C5B 146.5(9) . . . . ? N1 Ce1 N4 C5B 59.8(10) . . . . ? N5 Ce1 N4 C5B 19.0(9) . . . . ? Se1 Ce1 N4 C5B -125.3(9) . . . . ? Se2 Ce1 N4 C5B -84.0(9) . . . . ? Se3 Ce1 N4 C5B 107.1(9) 1_455 . . . ? N3 Ce1 N4 C7A 117.2(10) . . . . ? N6 Ce1 N4 C7A -24.6(10) . . . . ? N2 Ce1 N4 C7A -70.6(11) . . . . ? N1 Ce1 N4 C7A -157.2(10) . . . . ? N5 Ce1 N4 C7A 162.0(11) . . . . ? Se1 Ce1 N4 C7A 17.6(11) . . . . ? Se2 Ce1 N4 C7A 58.9(10) . . . . ? Se3 Ce1 N4 C7A -109.9(10) 1_455 . . . ? N3 Ce1 N5 C6B 151.8(11) . . . . ? N6 Ce1 N5 C6B 3.0(11) . . . . ? N4 Ce1 N5 C6B 10.3(10) . . . . ? N2 Ce1 N5 C6B -99.4(10) . . . . ? N1 Ce1 N5 C6B -143.5(10) . . . . ? Se1 Ce1 N5 C6B 135.3(10) . . . . ? Se2 Ce1 N5 C6B 78.6(10) . . . . ? Se3 Ce1 N5 C6B -60.9(10) 1_455 . . . ? N3 Ce1 N5 C6A 129.8(11) . . . . ? N6 Ce1 N5 C6A -19.0(11) . . . . ? N4 Ce1 N5 C6A -11.7(10) . . . . ? N2 Ce1 N5 C6A -121.4(10) . . . . ? N1 Ce1 N5 C6A -165.5(11) . . . . ? Se1 Ce1 N5 C6A 113.3(10) . . . . ? Se2 Ce1 N5 C6A 56.6(11) . . . . ? Se3 Ce1 N5 C6A -82.9(11) 1_455 . . . ? N3 Ce1 N6 C8A -114.4(10) . . . . ? N4 Ce1 N6 C8A -4.7(10) . . . . ? N2 Ce1 N6 C8A 135.4(10) . . . . ? N1 Ce1 N6 C8A 128.7(10) . . . . ? N5 Ce1 N6 C8A 2.6(11) . . . . ? Se1 Ce1 N6 C8A -153.2(10) . . . . ? Se2 Ce1 N6 C8A -81.2(10) . . . . ? Se3 Ce1 N6 C8A 67.6(10) 1_455 . . . ? N3 Ce1 N6 C8B -93.5(13) . . . . ? N4 Ce1 N6 C8B 16.2(12) . . . . ? N2 Ce1 N6 C8B 156.3(13) . . . . ? N1 Ce1 N6 C8B 149.6(12) . . . . ? N5 Ce1 N6 C8B 23.5(13) . . . . ? Se1 Ce1 N6 C8B -132.3(13) . . . . ? Se2 Ce1 N6 C8B -60.3(12) . . . . ? Se3 Ce1 N6 C8B 88.5(13) 1_455 . . . ? C3 N1 C1 C2 177.5(7) . . . . ? Ce1 N1 C1 C2 -54.3(9) . . . . ? Ce1 N2 C2 C1 -36.6(9) . . . . ? N1 C1 C2 N2 61.8(10) . . . . ? C1 N1 C3 C4 83.7(9) . . . . ? Ce1 N1 C3 C4 -43.2(8) . . . . ? Ce1 N3 C4 C3 -47.3(9) . . . . ? N1 C3 C4 N3 59.4(10) . . . . ? C7B N4 C5A C6A -171.0(15) . . . . ? C5B N4 C5A C6A -43.4(15) . . . . ? C7A N4 C5A C6A -138.6(16) . . . . ? Ce1 N4 C5A C6A 39(2) . . . . ? C5A N4 C5B C6B 63(2) . . . . ? C7B N4 C5B C6B 135.3(16) . . . . ? C7A N4 C5B C6B 167.3(15) . . . . ? Ce1 N4 C5B C6B -50.2(16) . . . . ? C6B N5 C6A C5A -72(4) . . . . ? Ce1 N5 C6A C5A 40(2) . . . . ? N4 C5A C6A N5 -52(2) . . . . ? C6A N5 C6B C5B 40(3) . . . . ? Ce1 N5 C6B C5B -36.4(18) . . . . ? N4 C5B C6B N5 57(2) . . . . ? C5A N4 C7A C8A -134.8(16) . . . . ? C7B N4 C7A C8A -47.8(17) . . . . ? C5B N4 C7A C8A -172.4(13) . . . . ? Ce1 N4 C7A C8A 47.3(16) . . . . ? C5A N4 C7B C8B 177.3(18) . . . . ? C5B N4 C7B C8B 142.7(17) . . . . ? C7A N4 C7B C8B 68(3) . . . . ? Ce1 N4 C7B C8B -32(2) . . . . ? C8B N6 C8A C7A -76(5) . . . . ? Ce1 N6 C8A C7A 33.9(18) . . . . ? N4 C7A C8A N6 -52(2) . . . . ? C8A N6 C8B C7B 43(3) . . . . ? Ce1 N6 C8B C7B -36(2) . . . . ? N4 C7B C8B N6 44(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 2.66 3.498(7) 152.2 8_557 N3 H3A Se4 0.92 2.63 3.540(8) 171.0 . N2 H2B Se3 0.92 2.90 3.605(7) 134.8 6_566 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.887 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.192 #===END data_complex_2c _database_code_depnum_ccdc_archive 'CCDC 767677' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 As N6 Pr Se4' _chemical_formula_sum 'C8 H26 As N6 Pr Se4' _chemical_formula_weight 738.02 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' As As 0.0499 2.0058 '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 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 8.8169(13) _cell_length_b 16.489(3) _cell_length_c 26.719(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3884.4(10) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 11570 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.00 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 11.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0892 _exptl_absorpt_correction_T_max 0.1829 _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 31064 _diffrn_reflns_av_R_equivalents 0.1140 _diffrn_reflns_av_sigmaI/netI 0.0988 _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 -26 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3424 _reflns_number_gt 2803 _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^)+(0.0958P)^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 3424 _refine_ls_number_parameters 188 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.210 _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 As1 As 0.49074(18) 0.26545(10) 0.11986(6) 0.0286(4) Uani 1 1 d . . . Se1 Se 0.34067(18) 0.16286(10) 0.15081(6) 0.0393(5) Uani 1 1 d . . . Se2 Se 0.33245(16) 0.33450(10) 0.06559(6) 0.0341(4) Uani 1 1 d . . . Se3 Se 0.69501(18) 0.21696(11) 0.07542(6) 0.0405(5) Uani 1 1 d . . . Se4 Se 0.56792(17) 0.34835(11) 0.18452(6) 0.0385(5) Uani 1 1 d . . . Pr1 Pr 0.04528(9) 0.25713(5) 0.11686(3) 0.0265(3) Uani 1 1 d . . . N1 N -0.0807(15) 0.4019(9) 0.1315(5) 0.040(3) Uani 1 1 d . . . H1 H -0.1824 0.3935 0.1342 0.048 Uiso 1 1 calc R . . N2 N 0.1698(16) 0.3468(8) 0.1882(5) 0.042(3) Uani 1 1 d . . . H2A H 0.1410 0.3269 0.2181 0.051 Uiso 1 1 calc R . . H2B H 0.2713 0.3419 0.1862 0.051 Uiso 1 1 calc R . . N3 N -0.0325(14) 0.3334(9) 0.0332(5) 0.041(3) Uani 1 1 d . . . H3A H 0.0520 0.3440 0.0155 0.049 Uiso 1 1 calc R . . H3B H -0.0910 0.3002 0.0147 0.049 Uiso 1 1 calc R . . N4 N -0.0288(16) 0.1045(9) 0.1320(5) 0.043(4) Uani 1 1 d D . . N5 N -0.1008(16) 0.2235(9) 0.2024(5) 0.045(3) Uani 1 1 d . . . H5A H -0.0415 0.2400 0.2279 0.053 Uiso 1 1 calc R . . H5B H -0.1854 0.2541 0.2032 0.053 Uiso 1 1 calc R . . N6 N 0.0972(17) 0.1569(8) 0.0419(5) 0.049(4) Uani 1 1 d . . . H6A H 0.0454 0.1756 0.0153 0.059 Uiso 1 1 calc R . . H6B H 0.1964 0.1606 0.0343 0.059 Uiso 1 1 calc R . . C1 C -0.0317(19) 0.4442(10) 0.1788(6) 0.043(4) Uani 1 1 d . . . H1A H -0.0526 0.5018 0.1762 0.051 Uiso 1 1 calc R . . H1B H -0.0877 0.4229 0.2071 0.051 Uiso 1 1 calc R . . C2 C 0.132(2) 0.4312(12) 0.1862(7) 0.057(5) Uani 1 1 d . . . H2C H 0.1868 0.4566 0.1590 0.068 Uiso 1 1 calc R . . H2D H 0.1626 0.4570 0.2172 0.068 Uiso 1 1 calc R . . C3 C -0.057(3) 0.4508(12) 0.0863(8) 0.074(7) Uani 1 1 d . . . H3C H -0.1067 0.5029 0.0904 0.089 Uiso 1 1 calc R . . H3D H 0.0508 0.4607 0.0820 0.089 Uiso 1 1 calc R . . C4 C -0.116(2) 0.4109(11) 0.0417(7) 0.058(5) Uani 1 1 d . . . H4A H -0.1039 0.4461 0.0129 0.070 Uiso 1 1 calc R . . H4B H -0.2233 0.3998 0.0460 0.070 Uiso 1 1 calc R . . C5A C -0.039(5) 0.084(2) 0.1856(9) 0.084(18) Uani 0.50 1 d PD . . C5B C -0.132(6) 0.078(2) 0.1717(15) 0.084(18) Uani 0.50 1 d PD . . C7A C 0.053(5) 0.046(2) 0.1013(9) 0.074(17) Uani 0.50 1 d PD . . C7B C -0.028(6) 0.045(2) 0.0917(12) 0.074(17) Uani 0.50 1 d PD . . C6 C -0.144(3) 0.1411(12) 0.2122(8) 0.087(8) Uani 1 1 d D . . C8 C 0.062(2) 0.0717(10) 0.0471(6) 0.055(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0206(8) 0.0363(10) 0.0288(8) 0.0012(7) -0.0004(6) -0.0018(7) Se1 0.0303(9) 0.0357(10) 0.0518(10) 0.0111(8) -0.0034(7) -0.0034(7) Se2 0.0236(8) 0.0405(10) 0.0382(9) 0.0081(7) -0.0009(6) -0.0017(7) Se3 0.0218(8) 0.0580(12) 0.0417(9) -0.0057(8) 0.0008(7) 0.0033(8) Se4 0.0275(8) 0.0486(11) 0.0396(9) -0.0077(8) -0.0025(7) -0.0044(8) Pr1 0.0222(5) 0.0267(5) 0.0305(5) -0.0014(3) 0.0014(3) -0.0007(3) N1 0.029(7) 0.046(9) 0.044(8) 0.000(7) 0.007(6) -0.007(7) N2 0.051(9) 0.031(8) 0.045(8) -0.014(6) 0.003(7) -0.013(7) N3 0.021(7) 0.055(10) 0.048(8) 0.007(7) 0.000(6) -0.008(7) N4 0.044(9) 0.039(9) 0.047(8) -0.012(7) 0.008(6) 0.002(7) N5 0.039(8) 0.050(9) 0.044(8) 0.001(7) 0.001(7) 0.002(7) N6 0.063(10) 0.038(9) 0.046(8) -0.011(7) 0.032(8) -0.015(8) C1 0.049(11) 0.035(10) 0.045(9) -0.003(8) 0.011(8) 0.001(8) C2 0.066(14) 0.059(14) 0.045(10) -0.005(9) -0.003(9) -0.026(11) C3 0.093(17) 0.042(13) 0.086(16) 0.011(12) -0.017(13) 0.004(12) C4 0.065(13) 0.044(12) 0.066(12) 0.017(10) -0.025(10) -0.005(10) C5A 0.12(5) 0.027(15) 0.11(3) 0.002(17) 0.05(3) -0.02(3) C5B 0.12(5) 0.027(15) 0.11(3) 0.002(17) 0.05(3) -0.02(3) C7A 0.11(4) 0.036(14) 0.08(2) -0.020(14) 0.05(3) -0.03(2) C7B 0.11(4) 0.036(14) 0.08(2) -0.020(14) 0.05(3) -0.03(2) C6 0.13(2) 0.047(13) 0.081(16) -0.005(12) 0.035(16) -0.050(14) C8 0.108(17) 0.021(9) 0.036(9) 0.000(7) -0.001(10) -0.009(10) _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 As1 Se3 2.301(2) . ? As1 Se1 2.301(2) . ? As1 Se4 2.306(2) . ? As1 Se2 2.312(2) . ? Se1 Pr1 3.1657(19) . ? Se2 Pr1 3.1487(17) . ? Se3 Pr1 3.3470(18) 1_655 ? Pr1 N4 2.631(14) . ? Pr1 N6 2.636(13) . ? Pr1 N2 2.650(12) . ? Pr1 N3 2.654(13) . ? Pr1 N1 2.661(15) . ? Pr1 N5 2.681(13) . ? Pr1 Se3 3.3470(18) 1_455 ? N1 C3 1.47(2) . ? N1 C1 1.51(2) . ? N1 H1 0.9100 . ? N2 C2 1.43(2) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C4 1.49(2) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C7B 1.461(19) . ? N4 C7A 1.462(19) . ? N4 C5B 1.467(19) . ? N4 C5A 1.477(19) . ? N5 C6 1.44(2) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 C8 1.45(2) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? C1 C2 1.47(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.46(3) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5A C6 1.50(2) . ? C5B C6 1.504(19) . ? C7A C8 1.51(2) . ? C7B C8 1.501(19) . ? 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 Se3 As1 Se1 112.33(9) . . ? Se3 As1 Se4 111.21(9) . . ? Se1 As1 Se4 109.65(9) . . ? Se3 As1 Se2 108.66(8) . . ? Se1 As1 Se2 103.90(8) . . ? Se4 As1 Se2 110.86(9) . . ? As1 Se1 Pr1 90.52(7) . . ? As1 Se2 Pr1 90.75(6) . . ? As1 Se3 Pr1 118.87(7) . 1_655 ? N4 Pr1 N6 63.9(4) . . ? N4 Pr1 N2 121.7(4) . . ? N6 Pr1 N2 145.5(5) . . ? N4 Pr1 N3 121.2(4) . . ? N6 Pr1 N3 72.7(5) . . ? N2 Pr1 N3 116.6(4) . . ? N4 Pr1 N1 137.0(4) . . ? N6 Pr1 N1 138.3(4) . . ? N2 Pr1 N1 64.3(4) . . ? N3 Pr1 N1 65.9(4) . . ? N4 Pr1 N5 63.4(4) . . ? N6 Pr1 N5 127.0(4) . . ? N2 Pr1 N5 72.6(4) . . ? N3 Pr1 N5 133.7(4) . . ? N1 Pr1 N5 81.9(4) . . ? N4 Pr1 Se2 130.8(3) . . ? N6 Pr1 Se2 77.5(3) . . ? N2 Pr1 Se2 75.7(3) . . ? N3 Pr1 Se2 69.5(3) . . ? N1 Pr1 Se2 92.1(3) . . ? N5 Pr1 Se2 147.2(3) . . ? N4 Pr1 Se1 72.0(3) . . ? N6 Pr1 Se1 76.5(4) . . ? N2 Pr1 Se1 74.1(3) . . ? N3 Pr1 Se1 133.3(3) . . ? N1 Pr1 Se1 137.9(3) . . ? N5 Pr1 Se1 92.8(3) . . ? Se2 Pr1 Se1 70.25(5) . . ? N4 Pr1 Se3 68.4(3) . 1_455 ? N6 Pr1 Se3 77.6(3) . 1_455 ? N2 Pr1 Se3 136.9(3) . 1_455 ? N3 Pr1 Se3 65.0(3) . 1_455 ? N1 Pr1 Se3 80.9(3) . 1_455 ? N5 Pr1 Se3 78.3(3) . 1_455 ? Se2 Pr1 Se3 132.71(5) . 1_455 ? Se1 Pr1 Se3 139.18(5) . 1_455 ? C3 N1 C1 113.2(14) . . ? C3 N1 Pr1 108.2(11) . . ? C1 N1 Pr1 114.8(10) . . ? C3 N1 H1 106.7 . . ? C1 N1 H1 106.7 . . ? Pr1 N1 H1 106.7 . . ? C2 N2 Pr1 114.7(10) . . ? C2 N2 H2A 108.6 . . ? Pr1 N2 H2A 108.6 . . ? C2 N2 H2B 108.6 . . ? Pr1 N2 H2B 108.6 . . ? H2A N2 H2B 107.6 . . ? C4 N3 Pr1 113.9(10) . . ? C4 N3 H3A 108.8 . . ? Pr1 N3 H3A 108.8 . . ? C4 N3 H3B 108.8 . . ? Pr1 N3 H3B 108.8 . . ? H3A N3 H3B 107.7 . . ? C7B N4 C7A 30(3) . . ? C7B N4 C5B 109.5(17) . . ? C7A N4 C5B 121(2) . . ? C7B N4 C5A 124(3) . . ? C7A N4 C5A 114.9(18) . . ? C5B N4 C5A 36(3) . . ? C7B N4 Pr1 122.3(15) . . ? C7A N4 Pr1 115.3(17) . . ? C5B N4 Pr1 123.3(15) . . ? C5A N4 Pr1 113(2) . . ? C6 N5 Pr1 118.7(11) . . ? C6 N5 H5A 107.6 . . ? Pr1 N5 H5A 107.6 . . ? C6 N5 H5B 107.6 . . ? Pr1 N5 H5B 107.6 . . ? H5A N5 H5B 107.1 . . ? C8 N6 Pr1 119.9(9) . . ? C8 N6 H6A 107.3 . . ? Pr1 N6 H6A 107.3 . . ? C8 N6 H6B 107.3 . . ? Pr1 N6 H6B 107.3 . . ? H6A N6 H6B 106.9 . . ? C2 C1 N1 109.0(14) . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? N1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 112.2(14) . . ? N2 C2 H2C 109.2 . . ? C1 C2 H2C 109.2 . . ? N2 C2 H2D 109.2 . . ? C1 C2 H2D 109.2 . . ? H2C C2 H2D 107.9 . . ? C4 C3 N1 111.9(17) . . ? C4 C3 H3C 109.2 . . ? N1 C3 H3C 109.2 . . ? C4 C3 H3D 109.2 . . ? N1 C3 H3D 109.2 . . ? H3C C3 H3D 107.9 . . ? C3 C4 N3 109.6(16) . . ? C3 C4 H4A 109.8 . . ? N3 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? N3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? N4 C5A C6 111(2) . . ? N4 C5B C6 111.1(19) . . ? N4 C7A C8 111.9(19) . . ? N4 C7B C8 112.6(19) . . ? N5 C6 C5A 110(2) . . ? N5 C6 C5B 120(2) . . ? C5A C6 C5B 35(3) . . ? N6 C8 C7B 118.7(18) . . ? N6 C8 C7A 112.3(19) . . ? C7B C8 C7A 29(3) . . ? 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 Se3 As1 Se1 Pr1 -135.82(8) . . . . ? Se4 As1 Se1 Pr1 99.99(8) . . . . ? Se2 As1 Se1 Pr1 -18.56(8) . . . . ? Se3 As1 Se2 Pr1 138.45(8) . . . . ? Se1 As1 Se2 Pr1 18.66(8) . . . . ? Se4 As1 Se2 Pr1 -99.05(8) . . . . ? Se1 As1 Se3 Pr1 -117.47(9) . . . 1_655 ? Se4 As1 Se3 Pr1 5.85(12) . . . 1_655 ? Se2 As1 Se3 Pr1 128.14(8) . . . 1_655 ? As1 Se2 Pr1 N4 -55.7(4) . . . . ? As1 Se2 Pr1 N6 -93.8(4) . . . . ? As1 Se2 Pr1 N2 64.1(3) . . . . ? As1 Se2 Pr1 N3 -169.8(3) . . . . ? As1 Se2 Pr1 N1 126.9(3) . . . . ? As1 Se2 Pr1 N5 48.7(6) . . . . ? As1 Se2 Pr1 Se1 -13.88(6) . . . . ? As1 Se2 Pr1 Se3 -153.59(7) . . . 1_455 ? As1 Se1 Pr1 N4 161.9(3) . . . . ? As1 Se1 Pr1 N6 95.3(3) . . . . ? As1 Se1 Pr1 N2 -66.3(3) . . . . ? As1 Se1 Pr1 N3 45.6(4) . . . . ? As1 Se1 Pr1 N1 -56.2(4) . . . . ? As1 Se1 Pr1 N5 -137.3(3) . . . . ? As1 Se1 Pr1 Se2 13.95(6) . . . . ? As1 Se1 Pr1 Se3 147.32(7) . . . 1_455 ? N4 Pr1 N1 C3 -135.2(12) . . . . ? N6 Pr1 N1 C3 -31.6(14) . . . . ? N2 Pr1 N1 C3 114.9(12) . . . . ? N3 Pr1 N1 C3 -24.5(11) . . . . ? N5 Pr1 N1 C3 -170.5(12) . . . . ? Se2 Pr1 N1 C3 41.9(12) . . . . ? Se1 Pr1 N1 C3 104.2(11) . . . . ? Se3 Pr1 N1 C3 -91.1(12) 1_455 . . . ? N4 Pr1 N1 C1 97.4(11) . . . . ? N6 Pr1 N1 C1 -159.1(9) . . . . ? N2 Pr1 N1 C1 -12.5(9) . . . . ? N3 Pr1 N1 C1 -152.0(11) . . . . ? N5 Pr1 N1 C1 62.0(10) . . . . ? Se2 Pr1 N1 C1 -85.6(10) . . . . ? Se1 Pr1 N1 C1 -23.3(12) . . . . ? Se3 Pr1 N1 C1 141.4(10) 1_455 . . . ? N4 Pr1 N2 C2 -148.1(11) . . . . ? N6 Pr1 N2 C2 122.7(12) . . . . ? N3 Pr1 N2 C2 24.5(13) . . . . ? N1 Pr1 N2 C2 -17.1(11) . . . . ? N5 Pr1 N2 C2 -106.3(12) . . . . ? Se2 Pr1 N2 C2 82.4(11) . . . . ? Se1 Pr1 N2 C2 155.5(12) . . . . ? Se3 Pr1 N2 C2 -56.5(13) 1_455 . . . ? N4 Pr1 N3 C4 126.3(11) . . . . ? N6 Pr1 N3 C4 169.6(12) . . . . ? N2 Pr1 N3 C4 -46.4(12) . . . . ? N1 Pr1 N3 C4 -5.4(11) . . . . ? N5 Pr1 N3 C4 44.6(13) . . . . ? Se2 Pr1 N3 C4 -107.5(11) . . . . ? Se1 Pr1 N3 C4 -139.4(10) . . . . ? Se3 Pr1 N3 C4 85.6(11) 1_455 . . . ? N6 Pr1 N4 C7B -9(3) . . . . ? N2 Pr1 N4 C7B -150(3) . . . . ? N3 Pr1 N4 C7B 37(3) . . . . ? N1 Pr1 N4 C7B 124(3) . . . . ? N5 Pr1 N4 C7B 164(3) . . . . ? Se2 Pr1 N4 C7B -52(3) . . . . ? Se1 Pr1 N4 C7B -93(3) . . . . ? Se3 Pr1 N4 C7B 77(3) 1_455 . . . ? N6 Pr1 N4 C7A 24(2) . . . . ? N2 Pr1 N4 C7A -117(2) . . . . ? N3 Pr1 N4 C7A 71(2) . . . . ? N1 Pr1 N4 C7A 158(2) . . . . ? N5 Pr1 N4 C7A -162(2) . . . . ? Se2 Pr1 N4 C7A -18(2) . . . . ? Se1 Pr1 N4 C7A -59(2) . . . . ? Se3 Pr1 N4 C7A 110(2) 1_455 . . . ? N6 Pr1 N4 C5B -162(3) . . . . ? N2 Pr1 N4 C5B 57(3) . . . . ? N3 Pr1 N4 C5B -115(3) . . . . ? N1 Pr1 N4 C5B -28(3) . . . . ? N5 Pr1 N4 C5B 12(3) . . . . ? Se2 Pr1 N4 C5B 156(3) . . . . ? Se1 Pr1 N4 C5B 114(3) . . . . ? Se3 Pr1 N4 C5B -76(3) 1_455 . . . ? N6 Pr1 N4 C5A 159(2) . . . . ? N2 Pr1 N4 C5A 18(2) . . . . ? N3 Pr1 N4 C5A -154.3(18) . . . . ? N1 Pr1 N4 C5A -67(2) . . . . ? N5 Pr1 N4 C5A -27.4(18) . . . . ? Se2 Pr1 N4 C5A 116.7(18) . . . . ? Se1 Pr1 N4 C5A 75.4(18) . . . . ? Se3 Pr1 N4 C5A -114.8(19) 1_455 . . . ? N4 Pr1 N5 C6 -0.3(15) . . . . ? N6 Pr1 N5 C6 6.7(17) . . . . ? N2 Pr1 N5 C6 -141.0(16) . . . . ? N3 Pr1 N5 C6 108.5(16) . . . . ? N1 Pr1 N5 C6 153.5(16) . . . . ? Se2 Pr1 N5 C6 -125.3(15) . . . . ? Se1 Pr1 N5 C6 -68.5(16) . . . . ? Se3 Pr1 N5 C6 71.2(16) 1_455 . . . ? N4 Pr1 N6 C8 -0.7(13) . . . . ? N2 Pr1 N6 C8 108.0(14) . . . . ? N3 Pr1 N6 C8 -139.9(15) . . . . ? N1 Pr1 N6 C8 -133.1(13) . . . . ? N5 Pr1 N6 C8 -7.7(16) . . . . ? Se2 Pr1 N6 C8 147.9(14) . . . . ? Se1 Pr1 N6 C8 75.6(14) . . . . ? Se3 Pr1 N6 C8 -72.6(14) 1_455 . . . ? C3 N1 C1 C2 -85.0(19) . . . . ? Pr1 N1 C1 C2 40.0(16) . . . . ? Pr1 N2 C2 C1 46.5(17) . . . . ? N1 C1 C2 N2 -57.1(18) . . . . ? C1 N1 C3 C4 -175.6(16) . . . . ? Pr1 N1 C3 C4 56(2) . . . . ? N1 C3 C4 N3 -63(2) . . . . ? Pr1 N3 C4 C3 35.4(19) . . . . ? C7B N4 C5A C6 -138(4) . . . . ? C7A N4 C5A C6 -171(3) . . . . ? C5B N4 C5A C6 -62(3) . . . . ? Pr1 N4 C5A C6 54(4) . . . . ? C7B N4 C5B C6 -176(4) . . . . ? C7A N4 C5B C6 153(4) . . . . ? C5A N4 C5B C6 63(3) . . . . ? Pr1 N4 C5B C6 -20(6) . . . . ? C7B N4 C7A C8 66(3) . . . . ? C5B N4 C7A C8 141(4) . . . . ? C5A N4 C7A C8 -179(3) . . . . ? Pr1 N4 C7A C8 -45(4) . . . . ? C7A N4 C7B C8 -68(3) . . . . ? C5B N4 C7B C8 174(4) . . . . ? C5A N4 C7B C8 -149(3) . . . . ? Pr1 N4 C7B C8 18(6) . . . . ? Pr1 N5 C6 C5A 27(3) . . . . ? Pr1 N5 C6 C5B -10(4) . . . . ? N4 C5A C6 N5 -53(4) . . . . ? N4 C5A C6 C5B 62(3) . . . . ? N4 C5B C6 N5 19(6) . . . . ? N4 C5B C6 C5A -63(3) . . . . ? Pr1 N6 C8 C7B 10(4) . . . . ? Pr1 N6 C8 C7A -21(3) . . . . ? N4 C7B C8 N6 -18(6) . . . . ? N4 C7B C8 C7A 67(3) . . . . ? N4 C7A C8 N6 43(4) . . . . ? N4 C7A C8 C7B -66(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 N6 H6A Se2 0.90 2.87 3.704(16) 155.3 6_565 N5 H5B Se4 0.90 2.72 3.605(14) 167.9 1_455 N3 H3A Se3 0.90 2.92 3.625(13) 136.8 6_565 N2 H2B Se4 0.90 2.62 3.511(14) 172.1 . N2 H2A Se4 0.90 2.70 3.518(13) 151.0 8_556 N1 H1 Se4 0.91 2.69 3.519(13) 152.7 1_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.831 _refine_diff_density_min -1.242 _refine_diff_density_rms 0.265 #===END data_complex_3a _database_code_depnum_ccdc_archive 'CCDC 767678' #TrackingRef '- cif files of 1a-3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 As La N6 Se4' _chemical_formula_sum 'C8 H26 As La N6 Se4' _chemical_formula_weight 736.02 _chemical_absolute_configuration unk 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' As As 0.0499 2.0058 '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' La La -0.2871 2.4523 '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 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 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' _cell_length_a 8.7554(15) _cell_length_b 11.3211(18) _cell_length_c 19.807(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1963.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.35 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 11.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0565 _exptl_absorpt_correction_T_max 0.3988 _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 10006 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.1130 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3582 _reflns_number_gt 2686 _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^)+(0.0437P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.17(2) _refine_ls_number_reflns 3582 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0708 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _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 As1 As 1.22469(8) 0.50068(6) 0.90809(6) 0.01982(19) Uani 1 1 d . . . Se1 Se 1.42589(8) 0.63326(6) 0.90841(6) 0.0251(2) Uani 1 1 d . . . Se2 Se 1.07132(9) 0.53550(9) 1.00093(5) 0.0284(2) Uani 1 1 d . . . Se3 Se 1.07368(9) 0.53674(9) 0.81487(5) 0.0280(2) Uani 1 1 d . . . Se4 Se 1.31300(8) 0.30985(6) 0.90757(6) 0.0257(2) Uani 1 1 d . . . La1 La 0.77739(4) 0.53348(3) 0.90844(3) 0.01726(12) Uani 1 1 d . . . N1 N 0.6268(8) 0.4026(6) 0.9990(4) 0.025(2) Uani 1 1 d . . . H1A H 0.5439 0.3704 0.9783 0.030 Uiso 1 1 calc R . . H1B H 0.6886 0.3420 1.0119 0.030 Uiso 1 1 calc R . . N2 N 0.7129(8) 0.6403(6) 1.0237(4) 0.0240(17) Uani 1 1 d . . . H2A H 0.7904 0.6908 1.0339 0.029 Uiso 1 1 calc R . . H2B H 0.6268 0.6843 1.0180 0.029 Uiso 1 1 calc R . . N3 N 0.8419(8) 0.7662(5) 0.9000(5) 0.0301(19) Uani 1 1 d . . . H3A H 0.8040 0.8021 0.9375 0.036 Uiso 1 1 calc R . . H3B H 0.9452 0.7747 0.9010 0.036 Uiso 1 1 calc R . . N4 N 0.7030(8) 0.6435(6) 0.7928(4) 0.0255(19) Uani 1 1 d . . . H4 H 0.6036 0.6663 0.8002 0.031 Uiso 1 1 calc R . . N5 N 0.6390(7) 0.3969(6) 0.8131(4) 0.0232(19) Uani 1 1 d . . . H5 H 0.5511 0.3685 0.8328 0.028 Uiso 1 1 calc R . . N6 N 0.8712(7) 0.3057(5) 0.9031(5) 0.0296(18) Uani 1 1 d . . . H6A H 0.9698 0.3038 0.8886 0.036 Uiso 1 1 calc R . . H6B H 0.8689 0.2749 0.9455 0.036 Uiso 1 1 calc R . . C1 C 0.5745(9) 0.4642(8) 1.0601(5) 0.029(2) Uani 1 1 d . . . H1C H 0.5610 0.4068 1.0967 0.035 Uiso 1 1 calc R . . H1D H 0.4754 0.5013 1.0513 0.035 Uiso 1 1 calc R . . C2 C 0.6893(9) 0.5588(7) 1.0821(5) 0.030(2) Uani 1 1 d . . . H2C H 0.6497 0.6026 1.1210 0.036 Uiso 1 1 calc R . . H2D H 0.7863 0.5219 1.0950 0.036 Uiso 1 1 calc R . . C3 C 0.7847(13) 0.8289(7) 0.8414(5) 0.038(2) Uani 1 1 d . . . H3C H 0.8490 0.8984 0.8335 0.046 Uiso 1 1 calc R . . H3D H 0.6810 0.8569 0.8510 0.046 Uiso 1 1 calc R . . C4 C 0.7813(13) 0.7571(7) 0.7795(6) 0.040(3) Uani 1 1 d . . . H4A H 0.8859 0.7420 0.7641 0.048 Uiso 1 1 calc R . . H4B H 0.7274 0.8001 0.7438 0.048 Uiso 1 1 calc R . . C5 C 0.6899(12) 0.5654(7) 0.7365(6) 0.041(3) Uani 1 1 d . . . H5A H 0.7917 0.5370 0.7238 0.049 Uiso 1 1 calc R . . H5B H 0.6476 0.6086 0.6979 0.049 Uiso 1 1 calc R . . C6 C 0.5897(10) 0.4622(9) 0.7522(5) 0.037(2) Uani 1 1 d . . . H6C H 0.5897 0.4082 0.7135 0.044 Uiso 1 1 calc R . . H6D H 0.4848 0.4901 0.7588 0.044 Uiso 1 1 calc R . . C7 C 0.7317(12) 0.2926(7) 0.7965(6) 0.042(3) Uani 1 1 d . . . H7A H 0.8228 0.3171 0.7714 0.050 Uiso 1 1 calc R . . H7B H 0.6725 0.2390 0.7678 0.050 Uiso 1 1 calc R . . C8 C 0.7780(13) 0.2304(7) 0.8584(6) 0.044(3) Uani 1 1 d . . . H8A H 0.6865 0.2045 0.8828 0.053 Uiso 1 1 calc R . . H8B H 0.8367 0.1599 0.8461 0.053 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 As1 0.0124(3) 0.0223(4) 0.0248(5) -0.0015(4) -0.0003(4) 0.0000(3) Se1 0.0146(3) 0.0198(3) 0.0409(6) -0.0027(5) 0.0017(5) -0.0002(3) Se2 0.0175(4) 0.0445(5) 0.0231(6) -0.0051(5) 0.0004(4) 0.0000(5) Se3 0.0186(4) 0.0417(5) 0.0236(6) 0.0014(5) -0.0002(4) 0.0035(5) Se4 0.0229(4) 0.0196(3) 0.0345(6) 0.0003(4) 0.0011(5) -0.0016(3) La1 0.01447(18) 0.01768(19) 0.0196(3) -0.0009(3) -0.0003(2) 0.00008(17) N1 0.021(4) 0.020(3) 0.035(6) -0.001(3) -0.003(3) -0.004(3) N2 0.021(4) 0.028(3) 0.023(5) 0.000(3) 0.000(3) 0.000(4) N3 0.047(4) 0.024(3) 0.019(5) 0.001(4) -0.005(4) -0.008(3) N4 0.025(4) 0.031(4) 0.021(5) 0.002(3) -0.004(3) -0.005(4) N5 0.016(4) 0.024(4) 0.030(6) 0.001(3) -0.001(3) 0.001(3) N6 0.026(3) 0.028(3) 0.035(6) -0.001(5) 0.000(4) 0.003(3) C1 0.028(4) 0.024(4) 0.034(6) 0.002(4) 0.005(4) 0.002(5) C2 0.031(4) 0.038(5) 0.022(7) 0.003(5) -0.003(5) 0.001(4) C3 0.060(6) 0.024(4) 0.031(7) 0.005(4) -0.004(6) -0.011(5) C4 0.066(7) 0.027(4) 0.026(7) 0.008(4) -0.011(6) -0.006(5) C5 0.055(6) 0.037(5) 0.032(8) -0.002(5) -0.011(6) 0.000(5) C6 0.031(5) 0.052(6) 0.028(7) -0.004(5) -0.009(5) -0.004(5) C7 0.046(6) 0.034(5) 0.046(8) -0.019(5) -0.006(6) 0.011(5) C8 0.046(6) 0.020(4) 0.067(9) -0.006(5) -0.008(6) 0.011(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 As1 Se4 2.2945(10) . ? As1 Se3 2.3074(14) . ? As1 Se2 2.3109(14) . ? As1 Se1 2.3143(10) . ? Se1 La1 3.2783(9) 1_655 ? Se2 La1 3.1590(11) . ? Se3 La1 3.1885(11) . ? La1 N2 2.645(7) . ? La1 N1 2.674(8) . ? La1 N3 2.699(6) . ? La1 N4 2.688(7) . ? La1 N5 2.725(8) . ? La1 N6 2.709(6) . ? La1 Se1 3.2783(9) 1_455 ? N1 C1 1.470(11) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.494(12) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 C3 1.450(12) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C5 1.427(12) . ? N4 C4 1.480(10) . ? N4 H4 0.9200 . ? N5 C7 1.470(10) . ? N5 C6 1.479(12) . ? N5 H5 0.9200 . ? N6 C8 1.476(12) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? C1 C2 1.532(11) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.471(13) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.494(13) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 C8 1.469(14) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 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 Se4 As1 Se3 110.86(5) . . ? Se4 As1 Se2 111.10(5) . . ? Se3 As1 Se2 105.88(4) . . ? Se4 As1 Se1 110.74(4) . . ? Se3 As1 Se1 108.88(5) . . ? Se2 As1 Se1 109.23(5) . . ? As1 Se1 La1 119.41(3) . 1_655 ? As1 Se2 La1 90.61(4) . . ? As1 Se3 La1 89.94(4) . . ? N2 La1 N1 64.5(2) . . ? N2 La1 N3 69.6(2) . . ? N1 La1 N3 133.3(2) . . ? N2 La1 N4 118.16(19) . . ? N1 La1 N4 135.2(2) . . ? N3 La1 N4 63.0(2) . . ? N2 La1 N5 139.7(2) . . ? N1 La1 N5 86.1(2) . . ? N3 La1 N5 127.2(2) . . ? N4 La1 N5 64.2(2) . . ? N2 La1 N6 122.3(3) . . ? N1 La1 N6 69.4(2) . . ? N3 La1 N6 149.7(2) . . ? N4 La1 N6 118.8(3) . . ? N5 La1 N6 64.4(2) . . ? N2 La1 Se2 70.74(16) . . ? N1 La1 Se2 90.95(17) . . ? N3 La1 Se2 81.86(16) . . ? N4 La1 Se2 133.49(15) . . ? N5 La1 Se2 140.19(13) . . ? N6 La1 Se2 77.44(17) . . ? N2 La1 Se3 132.09(15) . . ? N1 La1 Se3 142.89(15) . . ? N3 La1 Se3 77.44(18) . . ? N4 La1 Se3 72.31(16) . . ? N5 La1 Se3 88.02(16) . . ? N6 La1 Se3 75.03(17) . . ? Se2 La1 Se3 70.99(3) . . ? N2 La1 Se1 69.02(16) . 1_455 ? N1 La1 Se1 74.23(16) . 1_455 ? N3 La1 Se1 81.95(16) . 1_455 ? N4 La1 Se1 67.22(16) . 1_455 ? N5 La1 Se1 77.18(14) . 1_455 ? N6 La1 Se1 127.79(13) . 1_455 ? Se2 La1 Se1 139.67(3) . 1_455 ? Se3 La1 Se1 139.44(3) . 1_455 ? C1 N1 La1 116.3(5) . . ? C1 N1 H1A 108.2 . . ? La1 N1 H1A 108.2 . . ? C1 N1 H1B 108.2 . . ? La1 N1 H1B 108.2 . . ? H1A N1 H1B 107.4 . . ? C2 N2 La1 114.5(5) . . ? C2 N2 H2A 108.6 . . ? La1 N2 H2A 108.6 . . ? C2 N2 H2B 108.6 . . ? La1 N2 H2B 108.6 . . ? H2A N2 H2B 107.6 . . ? C3 N3 La1 117.1(5) . . ? C3 N3 H3A 108.0 . . ? La1 N3 H3A 108.0 . . ? C3 N3 H3B 108.0 . . ? La1 N3 H3B 108.0 . . ? H3A N3 H3B 107.3 . . ? C5 N4 C4 115.9(8) . . ? C5 N4 La1 113.4(5) . . ? C4 N4 La1 116.2(6) . . ? C5 N4 H4 102.9 . . ? C4 N4 H4 102.9 . . ? La1 N4 H4 102.9 . . ? C7 N5 C6 112.4(8) . . ? C7 N5 La1 111.4(5) . . ? C6 N5 La1 114.3(5) . . ? C7 N5 H5 106.0 . . ? C6 N5 H5 106.0 . . ? La1 N5 H5 106.0 . . ? C8 N6 La1 113.9(5) . . ? C8 N6 H6A 108.8 . . ? La1 N6 H6A 108.8 . . ? C8 N6 H6B 108.8 . . ? La1 N6 H6B 108.8 . . ? H6A N6 H6B 107.7 . . ? N1 C1 C2 111.2(7) . . ? 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 107.6(8) . . ? N2 C2 H2C 110.2 . . ? C1 C2 H2C 110.2 . . ? N2 C2 H2D 110.2 . . ? C1 C2 H2D 110.2 . . ? H2C C2 H2D 108.5 . . ? N3 C3 C4 113.8(8) . . ? N3 C3 H3C 108.8 . . ? C4 C3 H3C 108.8 . . ? N3 C3 H3D 108.8 . . ? C4 C3 H3D 108.8 . . ? H3C C3 H3D 107.7 . . ? C3 C4 N4 110.0(9) . . ? C3 C4 H4A 109.7 . . ? N4 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? N4 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N4 C5 C6 111.7(9) . . ? N4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C5 C6 N5 112.9(7) . . ? C5 C6 H6C 109.0 . . ? N5 C6 H6C 109.0 . . ? C5 C6 H6D 109.0 . . ? N5 C6 H6D 109.0 . . ? H6C C6 H6D 107.8 . . ? N5 C7 C8 110.6(9) . . ? N5 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N5 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N6 C8 C7 112.1(8) . . ? N6 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N6 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? 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 Se4 As1 Se1 La1 -0.14(8) . . . 1_655 ? Se3 As1 Se1 La1 -122.27(5) . . . 1_655 ? Se2 As1 Se1 La1 122.54(5) . . . 1_655 ? Se4 As1 Se2 La1 -106.26(4) . . . . ? Se3 As1 Se2 La1 14.17(4) . . . . ? Se1 As1 Se2 La1 131.28(4) . . . . ? Se4 As1 Se3 La1 106.55(4) . . . . ? Se2 As1 Se3 La1 -14.04(4) . . . . ? Se1 As1 Se3 La1 -131.38(4) . . . . ? As1 Se2 La1 N2 -161.01(16) . . . . ? As1 Se2 La1 N1 136.53(16) . . . . ? As1 Se2 La1 N3 -89.84(19) . . . . ? As1 Se2 La1 N4 -50.1(2) . . . . ? As1 Se2 La1 N5 51.5(3) . . . . ? As1 Se2 La1 N6 67.9(2) . . . . ? As1 Se2 La1 Se3 -10.39(3) . . . . ? As1 Se2 La1 Se1 -157.07(4) . . . 1_455 ? As1 Se3 La1 N2 49.0(2) . . . . ? As1 Se3 La1 N1 -54.4(3) . . . . ? As1 Se3 La1 N3 96.01(18) . . . . ? As1 Se3 La1 N4 161.32(16) . . . . ? As1 Se3 La1 N5 -135.18(14) . . . . ? As1 Se3 La1 N6 -71.2(2) . . . . ? As1 Se3 La1 Se2 10.40(3) . . . . ? As1 Se3 La1 Se1 157.27(4) . . . 1_455 ? N2 La1 N1 C1 6.8(6) . . . . ? N3 La1 N1 C1 -4.9(7) . . . . ? N4 La1 N1 C1 -98.4(6) . . . . ? N5 La1 N1 C1 -144.9(6) . . . . ? N6 La1 N1 C1 151.0(6) . . . . ? Se2 La1 N1 C1 74.8(6) . . . . ? Se3 La1 N1 C1 133.6(5) . . . . ? Se1 La1 N1 C1 -67.1(6) 1_455 . . . ? N1 La1 N2 C2 23.9(5) . . . . ? N3 La1 N2 C2 -165.2(6) . . . . ? N4 La1 N2 C2 153.3(5) . . . . ? N5 La1 N2 C2 70.9(6) . . . . ? N6 La1 N2 C2 -16.4(6) . . . . ? Se2 La1 N2 C2 -76.9(5) . . . . ? Se3 La1 N2 C2 -115.6(5) . . . . ? Se1 La1 N2 C2 105.8(5) 1_455 . . . ? N2 La1 N3 C3 -131.4(7) . . . . ? N1 La1 N3 C3 -120.2(7) . . . . ? N4 La1 N3 C3 7.6(7) . . . . ? N5 La1 N3 C3 6.3(8) . . . . ? N6 La1 N3 C3 109.0(8) . . . . ? Se2 La1 N3 C3 156.2(7) . . . . ? Se3 La1 N3 C3 84.0(7) . . . . ? Se1 La1 N3 C3 -60.9(7) 1_455 . . . ? N2 La1 N4 C5 -158.5(6) . . . . ? N1 La1 N4 C5 -77.4(7) . . . . ? N3 La1 N4 C5 157.3(7) . . . . ? N5 La1 N4 C5 -23.9(6) . . . . ? N6 La1 N4 C5 11.7(7) . . . . ? Se2 La1 N4 C5 112.0(6) . . . . ? Se3 La1 N4 C5 72.7(6) . . . . ? Se1 La1 N4 C5 -110.2(6) 1_455 . . . ? N2 La1 N4 C4 63.4(7) . . . . ? N1 La1 N4 C4 144.5(6) . . . . ? N3 La1 N4 C4 19.2(6) . . . . ? N5 La1 N4 C4 -162.0(7) . . . . ? N6 La1 N4 C4 -126.4(6) . . . . ? Se2 La1 N4 C4 -26.1(7) . . . . ? Se3 La1 N4 C4 -65.4(6) . . . . ? Se1 La1 N4 C4 111.7(7) 1_455 . . . ? N2 La1 N5 C7 -131.6(6) . . . . ? N1 La1 N5 C7 -90.1(6) . . . . ? N3 La1 N5 C7 125.8(6) . . . . ? N4 La1 N5 C7 124.5(6) . . . . ? N6 La1 N5 C7 -21.1(6) . . . . ? Se2 La1 N5 C7 -3.4(8) . . . . ? Se3 La1 N5 C7 53.2(6) . . . . ? Se1 La1 N5 C7 -164.8(6) 1_455 . . . ? N2 La1 N5 C6 99.7(6) . . . . ? N1 La1 N5 C6 141.2(6) . . . . ? N3 La1 N5 C6 -2.9(7) . . . . ? N4 La1 N5 C6 -4.2(6) . . . . ? N6 La1 N5 C6 -149.8(6) . . . . ? Se2 La1 N5 C6 -132.1(5) . . . . ? Se3 La1 N5 C6 -75.5(6) . . . . ? Se1 La1 N5 C6 66.5(5) 1_455 . . . ? N2 La1 N6 C8 125.4(7) . . . . ? N1 La1 N6 C8 86.8(7) . . . . ? N3 La1 N6 C8 -129.3(7) . . . . ? N4 La1 N6 C8 -44.3(8) . . . . ? N5 La1 N6 C8 -8.8(7) . . . . ? Se2 La1 N6 C8 -177.3(7) . . . . ? Se3 La1 N6 C8 -103.9(7) . . . . ? Se1 La1 N6 C8 38.1(8) 1_455 . . . ? La1 N1 C1 C2 -35.5(9) . . . . ? La1 N2 C2 C1 -50.6(7) . . . . ? N1 C1 C2 N2 56.0(9) . . . . ? La1 N3 C3 C4 -34.0(12) . . . . ? N3 C3 C4 N4 50.6(12) . . . . ? C5 N4 C4 C3 179.3(9) . . . . ? La1 N4 C4 C3 -43.7(10) . . . . ? C4 N4 C5 C6 -171.5(8) . . . . ? La1 N4 C5 C6 50.3(9) . . . . ? N4 C5 C6 N5 -54.7(11) . . . . ? C7 N5 C6 C5 -97.4(10) . . . . ? La1 N5 C6 C5 30.8(10) . . . . ? C6 N5 C7 C8 -180.0(8) . . . . ? La1 N5 C7 C8 50.3(9) . . . . ? La1 N6 C8 C7 38.8(11) . . . . ? N5 C7 C8 N6 -60.7(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 Se4 0.91 2.55 3.454(7) 170.6 1_455 N1 H1B Se4 0.91 2.59 3.445(8) 157.5 2_457 N2 H2A Se1 0.91 2.58 3.443(7) 157.6 2_467 N2 H2B Se1 0.91 2.85 3.396(8) 119.6 1_455 N3 H3A N2 0.91 2.63 3.051(11) 109.2 . N4 H4 Se1 0.92 2.67 3.339(8) 129.8 1_455 N5 H5 Se4 0.92 2.64 3.552(7) 170.0 1_455 N6 H6A Se4 0.91 3.03 3.869(6) 154.3 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.990 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.217 #===END data_complex_3b _database_code_depnum_ccdc_archive 'CCDC 767679' #TrackingRef '- cif files of 1a-3c.cif' _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 unk 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' Nd Nd -0.1943 3.0179 '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' 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 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 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' _cell_length_a 8.746(2) _cell_length_b 11.277(3) _cell_length_c 19.717(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1944.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6102 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 26.30 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 11.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2004 _exptl_absorpt_correction_T_max 0.4508 _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 6741 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.1112 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 26.30 _reflns_number_total 3816 _reflns_number_gt 2947 _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^)+(0.0902P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(6) _refine_ls_number_reflns 3816 _refine_ls_number_parameters 128 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1426 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 As1 As 0.77584(18) 0.49908(14) 0.90777(12) 0.0285(4) Uani 1 1 d . . . Se1 Se 0.57357(17) 0.36651(14) 0.90816(13) 0.0323(4) Uani 1 1 d . . . Se2 Se 0.9280(2) 0.4630(2) 0.81396(10) 0.0353(5) Uani 1 1 d . . . Se3 Se 0.9322(2) 0.4629(2) 1.00056(10) 0.0361(5) Uani 1 1 d . . . Se4 Se 0.6896(2) 0.69145(14) 0.90769(13) 0.0336(4) Uani 1 1 d . . . Nd1 Nd 0.22176(10) 0.46583(7) 0.90771(6) 0.0268(3) Uani 1 1 d . . . N1 N 0.2816(16) 0.3602(12) 1.0208(8) 0.028(3) Uani 1 1 d . . . H1A H 0.2044 0.3085 1.0298 0.033 Uiso 1 1 calc R . . H1B H 0.3686 0.3169 1.0153 0.033 Uiso 1 1 calc R . . N2 N 0.3661(16) 0.5969(13) 0.9962(9) 0.029(4) Uani 1 1 d . . . H2A H 0.4446 0.6339 0.9745 0.035 Uiso 1 1 calc R . . H2B H 0.3008 0.6542 1.0108 0.035 Uiso 1 1 calc R . . N3 N 0.1509(19) 0.2391(13) 0.8994(9) 0.0372(13) Uani 1 1 d . . . H3A H 0.1815 0.2035 0.9385 0.045 Uiso 1 1 calc R . . H3B H 0.0472 0.2333 0.8975 0.045 Uiso 1 1 calc R . . N4 N 0.296(2) 0.3573(13) 0.7961(7) 0.0372(13) Uani 1 1 d D . . H4 H 0.3951 0.3326 0.8041 0.045 Uiso 1 1 calc R . . N5 N 0.3598(19) 0.6026(14) 0.8158(9) 0.0372(13) Uani 1 1 d . . . H5 H 0.4477 0.6292 0.8365 0.045 Uiso 1 1 calc R . . N6 N 0.1269(18) 0.6884(12) 0.9060(10) 0.0372(13) Uani 1 1 d . . . H6A H 0.0289 0.6898 0.8904 0.045 Uiso 1 1 calc R . . H6B H 0.1258 0.7161 0.9493 0.045 Uiso 1 1 calc R . . C1 C 0.303(3) 0.4424(18) 1.0833(15) 0.062(7) Uani 1 1 d . . . H1C H 0.3385 0.3976 1.1228 0.075 Uiso 1 1 calc R . . H1D H 0.2072 0.4830 1.0949 0.075 Uiso 1 1 calc R . . C2 C 0.430(2) 0.5348(17) 1.0578(12) 0.040(5) Uani 1 1 d . . . H2C H 0.4534 0.5925 1.0935 0.048 Uiso 1 1 calc R . . H2D H 0.5249 0.4929 1.0460 0.048 Uiso 1 1 calc R . . C3 C 0.213(2) 0.1708(16) 0.8428(10) 0.0372(13) Uani 1 1 d . . . H3C H 0.1513 0.0996 0.8357 0.045 Uiso 1 1 calc R . . H3D H 0.3178 0.1457 0.8537 0.045 Uiso 1 1 calc R . . C4 C 0.215(2) 0.2450(15) 0.7784(11) 0.0372(13) Uani 1 1 d . . . H4A H 0.2682 0.2030 0.7419 0.045 Uiso 1 1 calc R . . H4B H 0.1100 0.2619 0.7635 0.045 Uiso 1 1 calc R . . C5 C 0.312(2) 0.4350(13) 0.7365(8) 0.0372(13) Uani 1 1 d D . . H5A H 0.2109 0.4634 0.7223 0.045 Uiso 1 1 calc R . . H5B H 0.3568 0.3904 0.6987 0.045 Uiso 1 1 calc R . . C6 C 0.412(2) 0.5381(15) 0.7539(10) 0.0372(13) Uani 1 1 d D . . H6C H 0.5166 0.5097 0.7611 0.045 Uiso 1 1 calc R . . H6D H 0.4136 0.5933 0.7156 0.045 Uiso 1 1 calc R . . C7 C 0.273(3) 0.7075(16) 0.8004(10) 0.0372(13) Uani 1 1 d . . . H7A H 0.1849 0.6860 0.7724 0.045 Uiso 1 1 calc R . . H7B H 0.3372 0.7623 0.7742 0.045 Uiso 1 1 calc R . . C8 C 0.218(3) 0.7692(16) 0.8646(10) 0.0372(13) Uani 1 1 d . . . H8A H 0.3064 0.7968 0.8909 0.045 Uiso 1 1 calc R . . H8B H 0.1564 0.8385 0.8524 0.045 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 As1 0.0237(8) 0.0272(8) 0.0346(10) 0.0025(8) -0.0002(10) -0.0009(7) Se1 0.0238(8) 0.0253(8) 0.0478(12) 0.0040(10) -0.0005(10) -0.0012(7) Se2 0.0267(9) 0.0424(11) 0.0369(12) -0.0027(11) 0.0013(8) 0.0007(10) Se3 0.0265(9) 0.0472(11) 0.0348(12) 0.0041(11) 0.0005(8) 0.0010(11) Se4 0.0333(9) 0.0258(7) 0.0415(11) 0.0012(9) -0.0006(10) -0.0009(7) Nd1 0.0265(5) 0.0242(4) 0.0298(5) 0.0002(5) 0.0001(5) -0.0006(4) N1 0.012(6) 0.023(6) 0.049(10) 0.004(7) 0.000(7) -0.004(6) N2 0.017(7) 0.032(8) 0.038(10) -0.002(7) -0.010(7) -0.001(6) N3 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(3) N4 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(3) N5 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(3) N6 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(3) C1 0.069(15) 0.039(11) 0.08(2) -0.005(13) -0.020(16) 0.004(12) C2 0.031(10) 0.030(9) 0.059(14) 0.004(10) 0.004(10) -0.017(9) C3 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(3) C4 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(3) C5 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(3) C6 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(3) C7 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(3) C8 0.047(3) 0.036(3) 0.028(3) 0.003(3) 0.001(3) -0.001(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 As1 Se4 2.297(2) . ? As1 Se2 2.315(3) . ? As1 Se1 2.316(2) . ? As1 Se3 2.320(3) . ? Se1 Nd1 3.2745(19) . ? Se2 Nd1 3.165(2) 1_655 ? Se3 Nd1 3.125(2) 1_655 ? Nd1 N1 2.581(16) . ? Nd1 N4 2.602(16) . ? Nd1 N2 2.613(15) . ? Nd1 N3 2.636(14) . ? Nd1 N6 2.644(14) . ? Nd1 N5 2.668(17) . ? Nd1 Se3 3.125(2) 1_455 ? Nd1 Se2 3.165(2) 1_455 ? N1 C1 1.55(3) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.51(3) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 C3 1.46(2) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C5 1.472(9) . ? N4 C4 1.50(2) . ? N4 H4 0.9200 . ? N5 C7 1.44(2) . ? N5 C6 1.49(3) . ? N5 H5 0.9200 . ? N6 C8 1.46(2) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? C1 C2 1.61(3) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.52(3) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.495(10) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 C8 1.52(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 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 Se4 As1 Se2 110.75(11) . . ? Se4 As1 Se1 111.02(9) . . ? Se2 As1 Se1 109.17(11) . . ? Se4 As1 Se3 111.11(12) . . ? Se2 As1 Se3 105.10(9) . . ? Se1 As1 Se3 109.51(11) . . ? As1 Se1 Nd1 119.80(7) . . ? As1 Se2 Nd1 89.90(8) . 1_655 ? As1 Se3 Nd1 90.79(8) . 1_655 ? N1 Nd1 N4 117.5(4) . . ? N1 Nd1 N2 65.5(5) . . ? N4 Nd1 N2 135.2(5) . . ? N1 Nd1 N3 69.7(5) . . ? N4 Nd1 N3 63.3(5) . . ? N2 Nd1 N3 134.7(5) . . ? N1 Nd1 N6 120.9(6) . . ? N4 Nd1 N6 121.0(5) . . ? N2 Nd1 N6 67.9(5) . . ? N3 Nd1 N6 147.8(5) . . ? N1 Nd1 N5 139.6(5) . . ? N4 Nd1 N5 65.4(5) . . ? N2 Nd1 N5 84.7(5) . . ? N3 Nd1 N5 128.7(5) . . ? N6 Nd1 N5 65.4(5) . . ? N1 Nd1 Se3 69.7(3) . 1_455 ? N4 Nd1 Se3 134.0(4) . 1_455 ? N2 Nd1 Se3 90.4(4) . 1_455 ? N3 Nd1 Se3 80.6(4) . 1_455 ? N6 Nd1 Se3 76.3(4) . 1_455 ? N5 Nd1 Se3 140.4(4) . 1_455 ? N1 Nd1 Se2 131.6(3) . 1_455 ? N4 Nd1 Se2 72.8(4) . 1_455 ? N2 Nd1 Se2 142.0(3) . 1_455 ? N3 Nd1 Se2 76.3(4) . 1_455 ? N6 Nd1 Se2 75.4(4) . 1_455 ? N5 Nd1 Se2 88.7(4) . 1_455 ? Se3 Nd1 Se2 71.59(5) 1_455 1_455 ? N1 Nd1 Se1 69.5(3) . . ? N4 Nd1 Se1 66.8(4) . . ? N2 Nd1 Se1 74.8(3) . . ? N3 Nd1 Se1 83.6(4) . . ? N6 Nd1 Se1 128.3(3) . . ? N5 Nd1 Se1 77.0(4) . . ? Se3 Nd1 Se1 139.14(6) 1_455 . ? Se2 Nd1 Se1 139.54(6) 1_455 . ? C1 N1 Nd1 115.7(11) . . ? C1 N1 H1A 108.4 . . ? Nd1 N1 H1A 108.4 . . ? C1 N1 H1B 108.4 . . ? Nd1 N1 H1B 108.4 . . ? H1A N1 H1B 107.4 . . ? C2 N2 Nd1 117.1(11) . . ? C2 N2 H2A 108.0 . . ? Nd1 N2 H2A 108.0 . . ? C2 N2 H2B 108.0 . . ? Nd1 N2 H2B 108.0 . . ? H2A N2 H2B 107.3 . . ? C3 N3 Nd1 118.1(11) . . ? C3 N3 H3A 107.8 . . ? Nd1 N3 H3A 107.8 . . ? C3 N3 H3B 107.8 . . ? Nd1 N3 H3B 107.8 . . ? H3A N3 H3B 107.1 . . ? C5 N4 C4 111.2(14) . . ? C5 N4 Nd1 114.8(11) . . ? C4 N4 Nd1 118.4(12) . . ? C5 N4 H4 103.4 . . ? C4 N4 H4 103.4 . . ? Nd1 N4 H4 103.4 . . ? C7 N5 C6 112.9(17) . . ? C7 N5 Nd1 112.4(12) . . ? C6 N5 Nd1 114.3(11) . . ? C7 N5 H5 105.4 . . ? C6 N5 H5 105.4 . . ? Nd1 N5 H5 105.4 . . ? C8 N6 Nd1 115.3(12) . . ? C8 N6 H6A 108.4 . . ? Nd1 N6 H6A 108.4 . . ? C8 N6 H6B 108.4 . . ? Nd1 N6 H6B 108.4 . . ? H6A N6 H6B 107.5 . . ? N1 C1 C2 103(2) . . ? N1 C1 H1C 111.2 . . ? C2 C1 H1C 111.2 . . ? N1 C1 H1D 111.2 . . ? C2 C1 H1D 111.2 . . ? H1C C1 H1D 109.1 . . ? N2 C2 C1 107.1(15) . . ? N2 C2 H2C 110.3 . . ? C1 C2 H2C 110.3 . . ? N2 C2 H2D 110.3 . . ? C1 C2 H2D 110.3 . . ? H2C C2 H2D 108.6 . . ? N3 C3 C4 110.5(16) . . ? N3 C3 H3C 109.5 . . ? C4 C3 H3C 109.5 . . ? N3 C3 H3D 109.5 . . ? C4 C3 H3D 109.5 . . ? H3C C3 H3D 108.1 . . ? N4 C4 C3 105.9(16) . . ? N4 C4 H4A 110.6 . . ? C3 C4 H4A 110.6 . . ? N4 C4 H4B 110.6 . . ? C3 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? N4 C5 C6 109.4(14) . . ? N4 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? N4 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? N5 C6 C5 112.9(15) . . ? N5 C6 H6C 109.0 . . ? C5 C6 H6C 109.0 . . ? N5 C6 H6D 109.0 . . ? C5 C6 H6D 109.0 . . ? H6C C6 H6D 107.8 . . ? N5 C7 C8 111.5(17) . . ? N5 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N5 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N6 C8 C7 110.6(16) . . ? N6 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N6 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 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 Se4 As1 Se1 Nd1 0.32(18) . . . . ? Se2 As1 Se1 Nd1 -122.05(11) . . . . ? Se3 As1 Se1 Nd1 123.38(11) . . . . ? Se4 As1 Se2 Nd1 106.03(10) . . . 1_655 ? Se1 As1 Se2 Nd1 -131.44(9) . . . 1_655 ? Se3 As1 Se2 Nd1 -14.05(8) . . . 1_655 ? Se4 As1 Se3 Nd1 -105.61(10) . . . 1_655 ? Se2 As1 Se3 Nd1 14.23(8) . . . 1_655 ? Se1 As1 Se3 Nd1 131.39(9) . . . 1_655 ? As1 Se1 Nd1 N1 -113.2(4) . . . . ? As1 Se1 Nd1 N4 112.5(4) . . . . ? As1 Se1 Nd1 N2 -44.1(4) . . . . ? As1 Se1 Nd1 N3 176.1(4) . . . . ? As1 Se1 Nd1 N6 0.5(6) . . . . ? As1 Se1 Nd1 N5 43.9(4) . . . . ? As1 Se1 Nd1 Se3 -116.34(13) . . . 1_455 ? As1 Se1 Nd1 Se2 115.95(13) . . . 1_455 ? N4 Nd1 N1 C1 154.6(14) . . . . ? N2 Nd1 N1 C1 24.6(14) . . . . ? N3 Nd1 N1 C1 -162.6(15) . . . . ? N6 Nd1 N1 C1 -16.5(15) . . . . ? N5 Nd1 N1 C1 71.0(16) . . . . ? Se3 Nd1 N1 C1 -75.5(13) 1_455 . . . ? Se2 Nd1 N1 C1 -114.4(13) 1_455 . . . ? Se1 Nd1 N1 C1 106.7(14) . . . . ? N1 Nd1 N2 C2 11.1(12) . . . . ? N4 Nd1 N2 C2 -94.1(14) . . . . ? N3 Nd1 N2 C2 1.6(16) . . . . ? N6 Nd1 N2 C2 153.6(14) . . . . ? N5 Nd1 N2 C2 -140.8(13) . . . . ? Se3 Nd1 N2 C2 78.6(12) 1_455 . . . ? Se2 Nd1 N2 C2 138.2(10) 1_455 . . . ? Se1 Nd1 N2 C2 -62.9(12) . . . . ? N1 Nd1 N3 C3 -127.4(15) . . . . ? N4 Nd1 N3 C3 10.1(14) . . . . ? N2 Nd1 N3 C3 -118.2(15) . . . . ? N6 Nd1 N3 C3 116.4(15) . . . . ? N5 Nd1 N3 C3 10.7(17) . . . . ? Se3 Nd1 N3 C3 160.8(15) 1_455 . . . ? Se2 Nd1 N3 C3 87.6(14) 1_455 . . . ? Se1 Nd1 N3 C3 -57.0(14) . . . . ? N1 Nd1 N4 C5 -159.1(12) . . . . ? N2 Nd1 N4 C5 -76.9(15) . . . . ? N3 Nd1 N4 C5 155.4(14) . . . . ? N6 Nd1 N4 C5 12.0(15) . . . . ? N5 Nd1 N4 C5 -24.2(12) . . . . ? Se3 Nd1 N4 C5 113.2(12) 1_455 . . . ? Se2 Nd1 N4 C5 72.4(12) 1_455 . . . ? Se1 Nd1 N4 C5 -109.9(13) . . . . ? N1 Nd1 N4 C4 66.4(14) . . . . ? N2 Nd1 N4 C4 148.5(12) . . . . ? N3 Nd1 N4 C4 20.8(12) . . . . ? N6 Nd1 N4 C4 -122.6(12) . . . . ? N5 Nd1 N4 C4 -158.7(14) . . . . ? Se3 Nd1 N4 C4 -21.3(15) 1_455 . . . ? Se2 Nd1 N4 C4 -62.1(13) 1_455 . . . ? Se1 Nd1 N4 C4 115.5(13) . . . . ? N1 Nd1 N5 C7 -129.3(12) . . . . ? N4 Nd1 N5 C7 126.4(14) . . . . ? N2 Nd1 N5 C7 -87.8(13) . . . . ? N3 Nd1 N5 C7 125.9(13) . . . . ? N6 Nd1 N5 C7 -19.8(12) . . . . ? Se3 Nd1 N5 C7 -3.7(17) 1_455 . . . ? Se2 Nd1 N5 C7 54.7(13) 1_455 . . . ? Se1 Nd1 N5 C7 -163.4(13) . . . . ? N1 Nd1 N5 C6 100.3(14) . . . . ? N4 Nd1 N5 C6 -4.0(12) . . . . ? N2 Nd1 N5 C6 141.7(13) . . . . ? N3 Nd1 N5 C6 -4.5(15) . . . . ? N6 Nd1 N5 C6 -150.2(14) . . . . ? Se3 Nd1 N5 C6 -134.1(10) 1_455 . . . ? Se2 Nd1 N5 C6 -75.7(12) 1_455 . . . ? Se1 Nd1 N5 C6 66.2(12) . . . . ? N1 Nd1 N6 C8 124.5(14) . . . . ? N4 Nd1 N6 C8 -46.2(16) . . . . ? N2 Nd1 N6 C8 84.3(14) . . . . ? N3 Nd1 N6 C8 -134.4(14) . . . . ? N5 Nd1 N6 C8 -10.1(13) . . . . ? Se3 Nd1 N6 C8 -179.6(15) 1_455 . . . ? Se2 Nd1 N6 C8 -105.4(14) 1_455 . . . ? Se1 Nd1 N6 C8 37.3(16) . . . . ? Nd1 N1 C1 C2 -53.3(17) . . . . ? Nd1 N2 C2 C1 -42.6(19) . . . . ? N1 C1 C2 N2 59.7(19) . . . . ? Nd1 N3 C3 C4 -38(2) . . . . ? C5 N4 C4 C3 177.2(16) . . . . ? Nd1 N4 C4 C3 -46.7(19) . . . . ? N3 C3 C4 N4 53(2) . . . . ? C4 N4 C5 C6 -172.5(16) . . . . ? Nd1 N4 C5 C6 49.8(19) . . . . ? C7 N5 C6 C5 -99(2) . . . . ? Nd1 N5 C6 C5 31.2(19) . . . . ? N4 C5 C6 N5 -53(2) . . . . ? C6 N5 C7 C8 178.4(16) . . . . ? Nd1 N5 C7 C8 47(2) . . . . ? Nd1 N6 C8 C7 37(2) . . . . ? N5 C7 C8 N6 -57(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Se1 0.91 2.59 3.436(14) 155.4 2_457 N1 H1B Se1 0.91 2.83 3.384(15) 120.8 . N2 H2A Se4 0.91 2.60 3.491(16) 167.2 . N2 H2B Se4 0.91 2.56 3.416(16) 157.0 2_467 N4 H4 Se1 0.92 2.61 3.281(17) 130.8 . N5 H5 Se4 0.92 2.63 3.550(18) 173.5 . N6 H6A Se4 0.91 2.99 3.825(16) 153.8 1_455 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.648 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.316 #===END data_complex_3c _database_code_depnum_ccdc_archive 'CCDC 767680' #TrackingRef '- cif files of 1a-3c.cif' _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' N N 0.0061 0.0033 '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' Se Se -0.0929 2.2259 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.009(2) _cell_length_b 13.427(2) _cell_length_c 14.821(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.201(7) _cell_angle_gamma 90.00 _cell_volume 1971.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8866 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 12.029 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1529 _exptl_absorpt_correction_T_max 0.2656 _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 9869 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3582 _reflns_number_gt 2848 _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^)+(0.0415P)^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 3582 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 As1 As 1.21669(8) 0.51308(6) 0.74221(5) 0.0200(2) Uani 1 1 d . . . Se1 Se 1.09110(9) 0.37614(7) 0.68259(6) 0.0266(2) Uani 1 1 d . . . Se2 Se 1.05803(9) 0.60557(7) 0.80701(6) 0.0288(2) Uani 1 1 d . . . Se3 Se 1.28519(9) 0.60452(7) 0.62560(6) 0.0309(2) Uani 1 1 d . . . Se4 Se 1.38904(9) 0.46792(7) 0.85216(6) 0.0301(2) Uani 1 1 d . . . Sm1 Sm 0.83362(4) 0.47861(3) 0.71503(3) 0.01747(13) Uani 1 1 d . . . N1 N 0.7748(7) 0.3251(5) 0.6123(5) 0.0257(16) Uani 1 1 d . . . H1A H 0.7909 0.3402 0.5550 0.031 Uiso 1 1 calc R . . H1B H 0.8314 0.2745 0.6333 0.031 Uiso 1 1 calc R . . N2 N 0.5781(7) 0.4483(6) 0.6700(4) 0.0263(16) Uani 1 1 d . . . H2A H 0.5440 0.4258 0.7200 0.032 Uiso 1 1 calc R . . H2B H 0.5378 0.5077 0.6540 0.032 Uiso 1 1 calc R . . N3 N 0.8564(8) 0.5649(6) 0.5630(5) 0.0347(18) Uani 1 1 d . . . H3A H 0.9444 0.5622 0.5541 0.042 Uiso 1 1 calc R . . H3B H 0.8075 0.5299 0.5171 0.042 Uiso 1 1 calc R . . N4 N 0.7445(7) 0.6571(5) 0.7056(4) 0.0253(16) Uani 1 1 d . . . H4 H 0.8190 0.6961 0.7239 0.030 Uiso 1 1 calc R . . N5 N 0.7263(7) 0.5304(5) 0.8542(4) 0.0256(16) Uani 1 1 d . . . H5 H 0.6411 0.5032 0.8460 0.031 Uiso 1 1 calc R . . N6 N 0.8654(8) 0.3489(6) 0.8449(5) 0.038(2) Uani 1 1 d . . . H6A H 0.8320 0.2896 0.8220 0.045 Uiso 1 1 calc R . . H6B H 0.9555 0.3406 0.8629 0.045 Uiso 1 1 calc R . . C1 C 0.6339(9) 0.2894(7) 0.6072(7) 0.036(2) Uani 1 1 d . . . H1C H 0.6224 0.2537 0.6632 0.043 Uiso 1 1 calc R . . H1D H 0.6129 0.2435 0.5557 0.043 Uiso 1 1 calc R . . C2 C 0.5409(9) 0.3773(7) 0.5950(6) 0.029(2) Uani 1 1 d . . . H2C H 0.5473 0.4097 0.5366 0.035 Uiso 1 1 calc R . . H2D H 0.4475 0.3552 0.5947 0.035 Uiso 1 1 calc R . . C3 C 0.8116(10) 0.6700(7) 0.5565(6) 0.035(2) Uani 1 1 d . . . H3C H 0.7815 0.6870 0.4925 0.041 Uiso 1 1 calc R . . H3D H 0.8877 0.7135 0.5791 0.041 Uiso 1 1 calc R . . C4 C 0.6978(9) 0.6877(7) 0.6113(5) 0.033(2) Uani 1 1 d . . . H4A H 0.6730 0.7584 0.6093 0.039 Uiso 1 1 calc R . . H4B H 0.6184 0.6488 0.5861 0.039 Uiso 1 1 calc R . . C5 C 0.6487(9) 0.6808(7) 0.7711(6) 0.027(2) Uani 1 1 d . . . H5A H 0.5603 0.6508 0.7505 0.033 Uiso 1 1 calc R . . H5B H 0.6372 0.7530 0.7754 0.033 Uiso 1 1 calc R . . C6 C 0.7072(9) 0.6388(7) 0.8630(6) 0.031(2) Uani 1 1 d . . . H6C H 0.7940 0.6707 0.8844 0.037 Uiso 1 1 calc R . . H6D H 0.6459 0.6520 0.9076 0.037 Uiso 1 1 calc R . . C7 C 0.7981(10) 0.4840(7) 0.9382(6) 0.034(2) Uani 1 1 d . . . H7A H 0.7515 0.5001 0.9902 0.041 Uiso 1 1 calc R . . H7B H 0.8903 0.5101 0.9507 0.041 Uiso 1 1 calc R . . C8 C 0.8019(11) 0.3724(7) 0.9258(6) 0.039(2) Uani 1 1 d . . . H8A H 0.8533 0.3416 0.9798 0.046 Uiso 1 1 calc R . . H8B H 0.7099 0.3456 0.9183 0.046 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 As1 0.0135(5) 0.0228(5) 0.0240(4) -0.0003(4) 0.0035(3) 0.0004(3) Se1 0.0182(5) 0.0236(5) 0.0383(5) -0.0076(4) 0.0050(4) 0.0009(4) Se2 0.0157(5) 0.0303(5) 0.0402(5) -0.0152(4) 0.0036(4) -0.0013(4) Se3 0.0295(6) 0.0342(6) 0.0297(5) 0.0083(4) 0.0068(4) -0.0004(4) Se4 0.0169(5) 0.0433(6) 0.0297(5) 0.0084(4) 0.0022(3) 0.0010(4) Sm1 0.0136(2) 0.0194(2) 0.0194(2) -0.00153(18) 0.00262(15) 0.00025(18) N1 0.026(4) 0.020(4) 0.032(4) -0.005(3) 0.006(3) 0.004(3) N2 0.020(4) 0.032(4) 0.028(4) -0.009(3) 0.007(3) 0.000(3) N3 0.038(5) 0.032(5) 0.036(4) -0.002(4) 0.011(3) -0.001(4) N4 0.016(4) 0.031(4) 0.028(4) -0.009(3) 0.001(3) 0.005(3) N5 0.019(4) 0.029(4) 0.028(4) -0.004(3) 0.005(3) 0.000(3) N6 0.049(6) 0.032(5) 0.033(4) 0.003(4) 0.006(4) 0.000(4) C1 0.026(5) 0.030(5) 0.051(6) -0.019(5) 0.005(4) -0.016(4) C2 0.019(5) 0.032(5) 0.036(5) -0.006(4) 0.004(4) -0.004(4) C3 0.052(7) 0.023(5) 0.028(5) 0.004(4) 0.002(4) -0.005(5) C4 0.038(6) 0.029(5) 0.029(5) 0.000(4) -0.003(4) 0.006(4) C5 0.020(5) 0.025(5) 0.038(5) -0.001(4) 0.009(4) 0.001(4) C6 0.025(5) 0.032(5) 0.038(5) -0.010(4) 0.012(4) -0.004(4) C7 0.037(6) 0.043(6) 0.024(5) 0.010(4) 0.003(4) -0.002(5) C8 0.052(7) 0.039(6) 0.026(5) 0.004(5) 0.010(4) -0.007(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 As1 Se4 2.2797(12) . ? As1 Se3 2.3027(12) . ? As1 Se2 2.3285(12) . ? As1 Se1 2.3291(12) . ? Se1 Sm1 3.0199(11) . ? Se2 Sm1 2.9894(10) . ? Sm1 N5 2.554(7) . ? Sm1 N4 2.554(7) . ? Sm1 N3 2.572(7) . ? Sm1 N1 2.580(7) . ? Sm1 N2 2.582(7) . ? Sm1 N6 2.582(7) . ? N1 C1 1.482(11) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.471(11) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 C3 1.481(12) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C4 1.468(10) . ? N4 C5 1.493(10) . ? N4 H4 0.9200 . ? N5 C6 1.476(11) . ? N5 C7 1.483(11) . ? N5 H5 0.9200 . ? N6 C8 1.469(12) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? C1 C2 1.498(13) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.509(13) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.512(12) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 C8 1.510(13) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 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 Se4 As1 Se3 113.72(5) . . ? Se4 As1 Se2 109.76(5) . . ? Se3 As1 Se2 108.59(5) . . ? Se4 As1 Se1 111.94(5) . . ? Se3 As1 Se1 109.79(5) . . ? Se2 As1 Se1 102.39(4) . . ? As1 Se1 Sm1 90.38(4) . . ? As1 Se2 Sm1 91.15(4) . . ? N5 Sm1 N4 66.7(2) . . ? N5 Sm1 N3 133.2(2) . . ? N4 Sm1 N3 66.6(2) . . ? N5 Sm1 N1 127.4(2) . . ? N4 Sm1 N1 132.0(2) . . ? N3 Sm1 N1 83.3(2) . . ? N5 Sm1 N2 74.7(2) . . ? N4 Sm1 N2 79.0(2) . . ? N3 Sm1 N2 93.0(2) . . ? N1 Sm1 N2 65.6(2) . . ? N5 Sm1 N6 66.6(2) . . ? N4 Sm1 N6 132.8(2) . . ? N3 Sm1 N6 160.0(2) . . ? N1 Sm1 N6 83.9(2) . . ? N2 Sm1 N6 95.6(2) . . ? N5 Sm1 Se2 81.46(16) . . ? N4 Sm1 Se2 73.96(16) . . ? N3 Sm1 Se2 89.32(18) . . ? N1 Sm1 Se2 144.88(15) . . ? N2 Sm1 Se2 149.32(16) . . ? N6 Sm1 Se2 92.30(19) . . ? N5 Sm1 Se1 135.99(16) . . ? N4 Sm1 Se1 135.90(16) . . ? N3 Sm1 Se1 83.19(18) . . ? N1 Sm1 Se1 70.73(15) . . ? N2 Sm1 Se1 136.34(15) . . ? N6 Sm1 Se1 78.11(18) . . ? Se2 Sm1 Se1 74.31(3) . . ? C1 N1 Sm1 115.1(5) . . ? C1 N1 H1A 108.5 . . ? Sm1 N1 H1A 108.5 . . ? C1 N1 H1B 108.5 . . ? Sm1 N1 H1B 108.5 . . ? H1A N1 H1B 107.5 . . ? C2 N2 Sm1 115.6(5) . . ? C2 N2 H2A 108.4 . . ? Sm1 N2 H2A 108.4 . . ? C2 N2 H2B 108.4 . . ? Sm1 N2 H2B 108.4 . . ? H2A N2 H2B 107.4 . . ? C3 N3 Sm1 115.0(5) . . ? C3 N3 H3A 108.5 . . ? Sm1 N3 H3A 108.5 . . ? C3 N3 H3B 108.5 . . ? Sm1 N3 H3B 108.5 . . ? H3A N3 H3B 107.5 . . ? C4 N4 C5 114.4(7) . . ? C4 N4 Sm1 112.1(5) . . ? C5 N4 Sm1 114.6(5) . . ? C4 N4 H4 104.8 . . ? C5 N4 H4 104.8 . . ? Sm1 N4 H4 104.8 . . ? C6 N5 C7 113.2(7) . . ? C6 N5 Sm1 114.5(5) . . ? C7 N5 Sm1 110.8(5) . . ? C6 N5 H5 105.9 . . ? C7 N5 H5 105.9 . . ? Sm1 N5 H5 105.9 . . ? C8 N6 Sm1 116.2(6) . . ? C8 N6 H6A 108.2 . . ? Sm1 N6 H6A 108.2 . . ? C8 N6 H6B 108.2 . . ? Sm1 N6 H6B 108.2 . . ? H6A N6 H6B 107.4 . . ? N1 C1 C2 108.8(7) . . ? N1 C1 H1C 109.9 . . ? C2 C1 H1C 109.9 . . ? N1 C1 H1D 109.9 . . ? C2 C1 H1D 109.9 . . ? H1C C1 H1D 108.3 . . ? N2 C2 C1 109.5(7) . . ? N2 C2 H2C 109.8 . . ? C1 C2 H2C 109.8 . . ? N2 C2 H2D 109.8 . . ? C1 C2 H2D 109.8 . . ? H2C C2 H2D 108.2 . . ? N3 C3 C4 111.1(8) . . ? N3 C3 H3C 109.4 . . ? C4 C3 H3C 109.4 . . ? N3 C3 H3D 109.4 . . ? C4 C3 H3D 109.4 . . ? H3C C3 H3D 108.0 . . ? N4 C4 C3 107.8(7) . . ? N4 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? N4 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.5 . . ? N4 C5 C6 107.7(7) . . ? N4 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? N4 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? N5 C6 C5 109.1(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 109.4(8) . . ? N5 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N5 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? 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 . . ? 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 Se4 As1 Se1 Sm1 128.77(4) . . . . ? Se3 As1 Se1 Sm1 -103.93(4) . . . . ? Se2 As1 Se1 Sm1 11.28(4) . . . . ? Se4 As1 Se2 Sm1 -130.44(4) . . . . ? Se3 As1 Se2 Sm1 104.68(4) . . . . ? Se1 As1 Se2 Sm1 -11.40(4) . . . . ? As1 Se2 Sm1 N5 151.80(16) . . . . ? As1 Se2 Sm1 N4 -140.07(16) . . . . ? As1 Se2 Sm1 N3 -74.22(18) . . . . ? As1 Se2 Sm1 N1 3.2(3) . . . . ? As1 Se2 Sm1 N2 -169.0(3) . . . . ? As1 Se2 Sm1 N6 85.87(18) . . . . ? As1 Se2 Sm1 Se1 8.89(3) . . . . ? As1 Se1 Sm1 N5 -68.0(2) . . . . ? As1 Se1 Sm1 N4 36.5(2) . . . . ? As1 Se1 Sm1 N3 82.32(18) . . . . ? As1 Se1 Sm1 N1 167.62(17) . . . . ? As1 Se1 Sm1 N2 169.6(2) . . . . ? As1 Se1 Sm1 N6 -104.73(19) . . . . ? As1 Se1 Sm1 Se2 -8.89(3) . . . . ? N5 Sm1 N1 C1 28.1(7) . . . . ? N4 Sm1 N1 C1 -63.0(7) . . . . ? N3 Sm1 N1 C1 -113.0(6) . . . . ? N2 Sm1 N1 C1 -16.6(6) . . . . ? N6 Sm1 N1 C1 82.4(6) . . . . ? Se2 Sm1 N1 C1 167.7(5) . . . . ? Se1 Sm1 N1 C1 161.9(6) . . . . ? N5 Sm1 N2 C2 -158.6(6) . . . . ? N4 Sm1 N2 C2 132.7(6) . . . . ? N3 Sm1 N2 C2 67.2(6) . . . . ? N1 Sm1 N2 C2 -14.1(6) . . . . ? N6 Sm1 N2 C2 -94.8(6) . . . . ? Se2 Sm1 N2 C2 161.0(4) . . . . ? Se1 Sm1 N2 C2 -16.1(7) . . . . ? N5 Sm1 N3 C3 7.5(8) . . . . ? N4 Sm1 N3 C3 2.7(6) . . . . ? N1 Sm1 N3 C3 144.3(6) . . . . ? N2 Sm1 N3 C3 79.3(6) . . . . ? N6 Sm1 N3 C3 -165.0(7) . . . . ? Se2 Sm1 N3 C3 -70.1(6) . . . . ? Se1 Sm1 N3 C3 -144.4(6) . . . . ? N5 Sm1 N4 C4 -148.8(6) . . . . ? N3 Sm1 N4 C4 27.4(6) . . . . ? N1 Sm1 N4 C4 -28.7(7) . . . . ? N2 Sm1 N4 C4 -70.8(6) . . . . ? N6 Sm1 N4 C4 -158.3(5) . . . . ? Se2 Sm1 N4 C4 123.7(6) . . . . ? Se1 Sm1 N4 C4 78.2(6) . . . . ? N5 Sm1 N4 C5 -16.3(5) . . . . ? N3 Sm1 N4 C5 159.9(6) . . . . ? N1 Sm1 N4 C5 103.9(5) . . . . ? N2 Sm1 N4 C5 61.7(5) . . . . ? N6 Sm1 N4 C5 -25.8(7) . . . . ? Se2 Sm1 N4 C5 -103.7(5) . . . . ? Se1 Sm1 N4 C5 -149.2(4) . . . . ? N4 Sm1 N5 C6 -15.6(5) . . . . ? N3 Sm1 N5 C6 -20.4(7) . . . . ? N1 Sm1 N5 C6 -141.6(5) . . . . ? N2 Sm1 N5 C6 -99.9(6) . . . . ? N6 Sm1 N5 C6 156.8(6) . . . . ? Se2 Sm1 N5 C6 60.6(5) . . . . ? Se1 Sm1 N5 C6 117.3(5) . . . . ? N4 Sm1 N5 C7 -145.0(6) . . . . ? N3 Sm1 N5 C7 -149.8(5) . . . . ? N1 Sm1 N5 C7 89.0(6) . . . . ? N2 Sm1 N5 C7 130.6(6) . . . . ? N6 Sm1 N5 C7 27.4(6) . . . . ? Se2 Sm1 N5 C7 -68.9(5) . . . . ? Se1 Sm1 N5 C7 -12.2(7) . . . . ? N5 Sm1 N6 C8 2.1(6) . . . . ? N4 Sm1 N6 C8 11.6(8) . . . . ? N3 Sm1 N6 C8 176.1(7) . . . . ? N1 Sm1 N6 C8 -133.2(7) . . . . ? N2 Sm1 N6 C8 -68.5(7) . . . . ? Se2 Sm1 N6 C8 81.8(6) . . . . ? Se1 Sm1 N6 C8 155.2(7) . . . . ? Sm1 N1 C1 C2 44.6(9) . . . . ? Sm1 N2 C2 C1 42.5(9) . . . . ? N1 C1 C2 N2 -56.5(10) . . . . ? Sm1 N3 C3 C4 -31.6(9) . . . . ? C5 N4 C4 C3 173.4(7) . . . . ? Sm1 N4 C4 C3 -54.0(8) . . . . ? N3 C3 C4 N4 56.4(10) . . . . ? C4 N4 C5 C6 176.4(8) . . . . ? Sm1 N4 C5 C6 45.0(8) . . . . ? C7 N5 C6 C5 173.3(7) . . . . ? Sm1 N5 C6 C5 45.1(8) . . . . ? N4 C5 C6 N5 -58.6(9) . . . . ? C6 N5 C7 C8 175.0(8) . . . . ? Sm1 N5 C7 C8 -54.9(8) . . . . ? Sm1 N6 C8 C7 -30.6(10) . . . . ? N5 C7 C8 N6 56.5(10) . . . . ? 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 Se3 0.91 2.78 3.617(7) 154.0 3_766 N1 H1B Se2 0.91 2.62 3.513(7) 166.7 2_746 N2 H2A Se4 0.91 2.73 3.521(7) 146.5 1_455 N2 H2B Se3 0.91 2.82 3.589(7) 142.9 1_455 N3 H3B Se3 0.91 2.83 3.723(8) 166.0 3_766 N4 H4 Se1 0.92 2.87 3.650(7) 143.9 2_756 N5 H5 Se4 0.92 2.58 3.475(7) 163.9 1_455 N6 H6A Se3 0.91 2.90 3.663(8) 142.3 2_746 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.580 _refine_diff_density_min -1.191 _refine_diff_density_rms 0.210